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                                    FORMS SETUP

FORMS (Field Operations Record Management System) software is used to generate labels and
chains-of-custody for all samples. Familiarity with the FORMS program is required.

Equipment Required:

Computer with FORMS software installed.
Labels for Lazer printer (3 V^'x 15/16" computer labels).
Sample Tags numbered in sequential order.
Log books.

Information Required to Setup FORMS:

Project number (if samples will be sent to the Region IV BSD laboratory).
A list of sampling stations complete with station identification #'s (see below).
Type of samples to be collected (water, sediment, periphyton ...etc).
List analyses to be performed on  each sample type (THG, TOC, MeHg etc).
Name of each laboratory analyzing samples.
Which stations will require duplicate samples  (eg.  any station # ending in "0" ).
Which analyses and stations will  require an additional QA sample (eg. stations ending in "3").
List of laboratories that will be performing QA analyses.
rmat for sample identification #'s:
                                   PI-XXX-MTA
     PROJECT IDENTIFICATION
     EXAMPLES:
     Ml = MARSH STUDY # 1
     M2 = MARSH STUDY # 2
     C4 = CANAL STUDY # 4
 STATION NUMBER
 001-999
MT= MATRIX TYPE
EXAMPLES:
SW = SURFACE WATER
BW = BOTTOM WATER
SD = SEDIMENT
PF = PERIPHYTON FLOATING
PS = PERIPHYTON SOIL
HI = HELICOPTER 1 BLANK
H2 = HELICOPTER 2 BLANK
HB = HELICOPTER BLANK
BB = BOAT BLANK
OTHER IDENTIFIER
EXAMPLES:
A = ATHENS BSD
B = BATELLE
F=FIU
     Example 1:
                                     M2-001-SWA
     Marsh Study #2
Station #001
Surface Water     Analyzed by Athens BSD
                                           23
-------
                   BASIC CALIBRATION - HYDROLAB SCOUT 2
               Refer to diagram of Scout 2 display unit panel keys (below)
                           fc:K<'ir'a'^r::-^>iai^-..^-..^^..
-------
       F.      Press either the right or left arrow to change No to Yes.

       G.     Press Enter. The unit is now calibrated to the standardizing solution.

       H.     Remove cup from sonde, rinse probes with deionized water, attach next
              standardizing solution and repeat steps 4 A thru H.

5.      After calibrating to pH 7.00, calibrate to pH 10.00, then simply read and record the value
       for pH 4.00(or vice versa) (see attached HYDROLAB CALIBRATION FORM p. 14).
       (Note: if necessary, standardizing solutions can be reused for 4-5 days)

6.      Next calibrate to a conductivity of 718 via steps 4 A thru H, then read and record the
       value for the solution with a conductivity of 1413. (Note: Do not reuse solutions)

7.      Calibrate to Redox solution A via steps 4 A thru H, then read and record value for Redox
       solution B.  (Note: the values for Redox solutions A & B will vary each time the
       standards are  made, but the  exact value for each standard is  always marked on the bottle;
       the solution can be reused for 4- 5 days).

8.      Draw chlorine-free water from a 5 gal. bucket, perform two Winkler titrations, and record
       the mg/1 DO for each titration (see HYDROLAB CALIBRATION FORM).

9.      Attach the stirrer to the end  of the sonde, immerse the probes in the bucket of chlorine-
       free water, wait (several minutes) for the DO reading to stabilize, and then follow steps 4
       A thru H as before.

10.    Remove the sonde from the bucket of water. While exposed to the air, follow steps 4 A
       thru H to calibrate Depth to 000.0.

11.    When all calibrations are completed, disconnect stirrer, reattach cup of tap water, and
       turn OFF the  unit.

 *For more detail and for servicing  refer to instrument manual.
                                           25
-------
                                 SAMPLING WATER

Water samples are usually collected by submerging an open sample container beneath the surface
of the water. However, when collecting water for low-level mercury analysis, samples are best
collected with the aid of a vacuum apparatus ( see Fig. 1 below) consisting of a vacuum
chamber, teflon sampling wand, and a hand pump.

Procedure:

1.      Wearing latex gloves, drop an uncapped 2L polypropylene bottle into the vacuum
       chamber and secure the chamber lid by attaching the spring-loaded clamps.
2.
Place a fresh square of Nitex® screening over end of sampling wand and secure with the
magnetic ring (Fig. 2). Insert head of wand beneath surface of water and tie shaft of
wand to pontoon of helicopter or to gunwale of boat (strap is provided).
       Squeeze the hand pump until liquid starts to fill the bottle. When water level in bottle is
       about an inch deep, release the vacuum, remove the bottle, discard the water ( swirling
       the water to rinse the bottle as you dump), and replace the bottle in the vacuum chamber.

       Begin pumping again. When bottle is 3/4 full, release the vacuum, remove from
       chamber, and cap.
                                          26
-------
5.      From the 2L polypropylene bottle, fill labeled sample containers with classical nutrient
       samples, making sure to rinse each bottle three times with water from the 2L bottle
       before filling.

                     500 ml Storemore® bottle
                     125 ml polypropylene bottles with screw caps

6.      Place filled nutrient sample containers in a clean cooler for transport.

7.      When sampling for trace level mercury, wear shoulder-length polypropylene gloves (over
       latex gloves), remove 2L Teflon® bottle from its protective Ziploc® bag, record on a
       Field Data Sheet (see p. 10) the bottle number etched near the top of the bottle, and then
       carefully mark the station number on the colored label attached to the bottle using
       waterproof marker.

8.      Uncap the Teflon bottle and place bottle and cap into vacuum chamber.  Secure the
       chamber lid and begin pumping.

9.      Fill this bottle to overflowing, then release the vacuum, cap tightly, and return bottle to
       its protective bag.

10.    Place bottle and bag in a clean cooler for transport.
QA/QC

1.  Wear latex gloves when handling polypropylene sample containers.

2.  Wear polypropylene gloves over latex gloves when handling Teflon sample containers.

3.  Store Teflon bottles in a Ziploc® bag before and after collecting the sample, which in turn is
stored in a clean cooler lined with a clean plastic trash bag.

4.  Use only Teflon bottles that have been specially cleaned (FIU procedure).

5.  During transport from the field, store all samples in a ice chest (lined with a plastic garbage
bag) for protection.
                                           27
-------
          PREPARATION AND ANALYSIS OF SULFIDE SYRINGE SAMPLES

Mated al s/suppli e s

       60 ml plastic syringes with leur-loc tip
       ZnAcetate solution
       6N NaOH solution
       3-way valves with leur-loc
       Rack to hold syringes upright.

Procedure:

       1.      Remove cap from tip of syringe and then plunger and set parts aside on a "clean
              surface."

       2.      Attach 3-way valve to tip of syringe and turn stopcock on valve to block opening
              to the syringe. Place the syringe open end up in a rack.

       3.      Prepare a fresh batch of preservative by mixing 30 ml of ZnAcetate and 20 ml of
              6N NaOH in a 60 ml polyethylene bottle.  A precipitate (ZnOH) will soon form.
              Just before use (step 4 below) shake the bottle vigorously for a few seconds to
              evenly suspend the precipitate.

       4.      Transfer 0.5 ml of preservative to syringe.

       5.      Reinsert plunger, invert syringe (tip up), rotate stopcock on 3-way valve to open
              passage from the syringe, and carefully expell air, leaving only preservative in the
              syringe.

       6.      Close stopcock opening to the syringe, replace cap on the tip of the 3-way valve.
              The syringe is now ready for the field where the sample is taken.

       7.      The syringe is delivered to the laboratory with the preserved sample and the
              analyst pairs the surface and porewater samples and checks the pH.

       8.      If the pH is <10, drops of 6N Sodium Hydroxide are placed into the valve side
              port and the valve  set to allow the analyst to draw the NaOH into the sample.
              Once the samples have a pH >=10, the syringes are stood upright for at least 30
              minutes, but typically allowed to stand overnight.

       9.      After settling, the volume of supernatant is expelled from the syringe, and the
              same volume of DI water is drawn into the syringe. This step removes
              interferences from the samples, but retains the original concentration. The sample
              is now ready for analysis.

       10.     Each sample is matched with a pair of cuvettes.  One cuvette will contain 25 ml
              of DI water as a  blank, while the other cuvette will contain 25 ml of sample.  The
              cuvette pairs are placed on sheets of paper identifying the run order.
                                           28
-------
11.     The Hach DR/2010 Spectrometer is turned on, and analysis program 690 is
       recalled. If necessary, the wavelength dial is set to 665 nm. The analysis begins
       by adding 1 ml of Reagent 1 to each cuvette.

12.     The reagent and the water in each cuvette are mixed using transfer pipets. Then 1
       ml of Reagent 2 is added to each cuvette and the analyst then starts a 5 minute
       countdown timer and mixes using the transfer pipets.

13.     The blank cuvette is placed in the meter reading chamber and after 5 minutes the
       analyst presses the zero button on the meter.  The meter display will blink and
       indicate the meter is zeroing.

14.     When the blinking stops, the analyst removes the blank cuvette and replaces it
       with the sample cuvette.  The meter will then display the measured result of the
       sample.

15.     The analyst will store the result by pressing the store button and confirming the
       operation by pressing the enter button.  The sample may now be disposed.

16.     Following analysis of all samples the stored values are downloaded from the
       analyzer.
                                    29
-------
                                      SAMPLING
                         CHLOROPHYLL and PARTICULATES
Required supplies
140 ml plastic syringe
47mm 0.45 ^ membrane filters
filter holder for 47 mm filters

Procedure

1.      Draw site water into syringe and expel to rinse syringe.

2.      Draw water into syringe again and attach filter holder containing a fresh filter (see Fig. 1
       below).
3.      Apply steady pressure to the plunger to force the entire volume of water in the syringe
       through the filter.

4.      Disconnect filter holder and repeat steps 2 and 3.  Ideally, a total of three volumes of
       water should be filtered.  This is not always physically possible. If filter becomes totally
       clogged before filtering three volumes, record the actual volume filtered.

5.      After filtering three volumes of water (or less if the filter becomes totally clogged),
       remover the filter from the holder with clean forceps and stuff the filter into a microfuge
       tube (or small glass vial) and cap. This is the chlorophyll sample.  Store on ice in the dark
       for transport.

6.      Repeat steps 2-4, remove the filter from the holder with forceps, place in a glass vial,
       cap, and store for transport.  This is the particulates sample.

7.      In the laboratory, fill each microfuge tube with acetone and store at 4°C to await
       chlorophyll analysis.
QA/QC

1.  Wear latex gloves while collecting samples.
2.  Do not apply excessive force to the plunger of the syringe.  Excessive force can rupture the
membrane filter.

                                           30
-------
                                   SAMPLING SOIL

DEEP CHANNELS AND CANALS

1.      Collect and lift sediment to the surface with a Petit Ponar dredge.

2.      Homogenize sediment in a "clean" glass pan with a "clean" stainless steel or teflon-
       coated spoon.

3.      Spoon sediment into labeled containers.

4.      Store sediment samples in a cooler for transport.

MARSHES

1.      Collect soil/sediment samples using the coring device pictured below (Fig. 1).
2.      Collect three cores at each sampling station. Pore the floe trapped in the core top into a
       separate container.  Place the soil core samples in a 1-gallon plastic bucket with a tight-
       fitting lid.  Keep only the top 10 cm of sediment from each core.  A plunger (provided) is
       used to extrude longer cores from the coring tube until only the top 10 cm of core remain.

3.      Do not homogenize sediment cores in the field. Store gallon containers for transport and
       then process sediment in the laboratory at the end of the day (see  SEDIMENT
       PROCESSING p. 26).
QA/QC

1.      Wear latex gloves while collecting and handling sediments.
2.      Keep clean glass pans and stainless steel spoons wrapped in foil until needed.
3.      Rinse coring device with site water before collecting cores.
4.      Take a photograph of one of the three cores while still in the coring tube.
                                           31
-------
                             PERIPHYTON COLLECTION

Mat Samples

1.      Soil periphyton mat is collected off the top of all soil core samples taken at a site and
       placed in a 500 ml plastic container.

2.      Floating periphyton mat samples are collected with a stainless steel "cookie cutter" with a
       plexiglas sheet placed under the mat.  The cutter and soil core sampler both have the
       same 3-inch diameter.  The periphyton from atleast 3 samples is placed in a 500 ml
       plastic container.

3.      Cap and store at ambient temperature for transport.

4.      Upon returning from the field, process and freeze samples.

Epiphytic Samples

1.      Periphyton samples were collected from concentrations which were epiphytic on
       Utricularia where both occurred together.   The sample was placed in a separate 500 ml
       plastic container.

2.      Cap and store at ambient temperature for transport.

3.      Upon returning from the field, process and freeze sample.
QA/QC

1.  Wear latex gloves while collecting samples.
2.  Keep frozen until analyzed.
                                  FISH COLLECTION

Freshwater Marshes/Canals

The target species for freshwater marshes is the mosquito fish Gambusia sp. These small
ubiquitous fish are found throughout weedy areas of a marsh and along the edges of canals and
deep channels. They congregate around the pontoons of a helicopter or the hull of a boat and are
easily collected with a "clean" dip net.  The fish are handled with latex gloves., placed in a
Ziploc® bag, and packed in ice for transport back the laboratory. In the laboratory the fish are
frozen until they  are processed for analysis. For low-level mercury analysis a minimum of 20
fish is required and a an additional minimum of 20 fish were collected for stomach analyses.

Saltwater Marshes/Tidal Creeks

The target species for saltwater marshes is the mummichog Fundulus heteroclitus. The
distribution of these small, ubiquitous fish in the salt marsh is influenced by the daily cycle of
the tides. The following procedure has proven successful in locating and collecting this species:
                                           32
-------
1. Starting about 2 hours after high tide, locate small, V-notched channels (< 10 feet across) that
drain the marsh grass as the tide recedes.

2. Plant a minnow trap in the bottom of the V-notch in about 2 feet of water. If the bottom of
the notch is wider than the width of the trap, plant more than one trap so that by low tide the last
of the water draining the marsh grass must pass through the trap(s) (see  Fig. 1 below).  Note in
Fig. 1 that the traps are secured in place by tying them (before planting) to a length of steel
conduit stuck into the mud.  Set out traps at 2 to 4 small channels in the vicinity of each
sampling station.

3. As the tide recedes, return to the traps every 20 to 30 minutes to check for fish. If a trap is
exposed and does not contain fish, replant.

4. Wearing latex gloves, transfer fish from the traps to  a "clean" glass jar fitted with a Teflon lid
and then store on ice for transport back to the laboratory.  In the laboratory, fish are frozen until
they are processed for analysis. For organic analyses a minimum of 30 gm offish is required
(about 20 fish).

(Note: Fish can also be  collected on the rising tide by planting traps in exposed V-notch
channels ahead of the rising water.)
QA/QC

1.  Wear latex gloves when handling fish.
2.  Freeze fish within 48 hours of collection and keep frozen until processed for chemical
analysis.
                                            33
-------
                 DOWNLOADING GPS UNIT (Trimble® Pathfinder Pro)

1.     Disconnect data logger and antenna from the external battery pack and then connect
      external battery to charger.

2.     Connect logger to computer using appropriate pigtail connector.

3.     Turn "on" computer.  Exit to DOS (F8). When C:\> appears, type "pfmder" and hit
      ENTER. The PATHFINDER program will appear on screen. Hit Okay to accept.

      NOTE: Selections are made from a menu by highlighting and pressing ENTER or by
      hitting ALT followed by the underlined letter in the desired heading, (e.g. to accept
      Okay, hit ALT then O).

4.     Select Project and then Current files.  The filename (e.g. MARSH1) should be displayed.

5.     Now select Comm , highlight Data Files to PC, and then hit ENTER.  Computer will tell
      you that it is "Looking for data logger  on COM1**

6.     Turn "on" data logger. When main menu appears scroll down to selection #9 - DATA
      FILE MGMT (or simply hit 9 then ENTER).  Hit ENTER.

7.     Now under DATA FILE MGMT select  "0" TRANS SERVER and hit ENTER. (If the
      computer does not indicate that it is accepting data from the logger, hit ENTER on the
      logger again).  A list of files will appear on the computer screen.

      If you wish to download all files, hit Okay.

      If you wish to download only a select number of files, first tag the files.  Tagging is
      accomplished by highlighting a file and then hitting either ENTER or the space bar. To
      accept the tagged files, hit Okay.

      The computer screen will now indicate that each file in succession is being transferred,
      converted, and finally used in a calculation.

8.     After all files have been downloaded onto the computer, check the file (MARSH1) to see
      if they are there.  This is accomplished by returning to DOS and after C:\> appears, type
      pfmder\data\pfmder\ marsh 1 and hitting ENTER.

9.     If all downloaded files are present, copy files to a disc by inserting a disc into A drive
      and typing copy  *.SSF A: and hitting ENTER. Computer will diplay name of each file
      copied.

10.    After files have been copied,  ERASE files from data logger (select #9 then the #2 or
      #3).
                                         34
-------
               PROCESSING SOIL, PERIPHYTON, AND FLOC SAMPLES

Equipment/Supplies

       Osterizer 10-speed blender motor
       High Density Polyethylene (HOPE) blender jars - 500 ml (48)
       Polyethylene spoons (15)
       "Blade assembly" (knurled base, stainless steel blades, gasket)
       Deionized water supply
       Graduated cylinder or cup - 100 mis
       paper towels

Procedures:

       Soil

       1.     With a PE spoon chop sample cores in the sample container once or twice and
             then sniff the sample for traces of H2S. Record finding (yes/no, slight, strong).

       2.     After sniffing, continue  to chip and mix sample core while removing large sticks,
             rocks, and roots.  If necessary add DI water to the sample until the mixture
             becomes as slurry. Record the volume of water added.

       3.     Spoon mixed sample into a 500 ml HDPE jar until the jar is 3/4 full.

       4.     Attach blade assembly to the jar and blend for 30-60 seconds on "BLEND"
             setting until the sample is thoroughly homogenized.

       5.     Pour or spoon the homogenized sample into labeled, 120 ml specimen cups.
             Normally, there is enough sample to fill up to 5 cups !/2 to 3/4 full. (Do not fill
             cups more than 3/4 full because upon freezing they may burst the container).

       6.     Store specimen cups for FIU-AFDW (ash-free dry wt.) at room temperature.
             Store all other cups in a freezer.

       Periphyton

       1.     Briefly chop and  stir the sample with a PE spoon. If the sample is dry add DI
             water until the mixture is thoroughly wet and glistening.  Record the volume of
             water added.

       2.     Spoon mixture in a 500  ml HDPE blender jar until the jar is 3/4 full.

       3.     Attach blade assembly to the jar and blend for 30-60 seconds on "BLEND"
             setting until the sample is thoroughly homogenized.
       4.     Pour homogenized sample into labeled, 120 specimen cups as before.

       5.     Store all cups in freezer.

       Floe (collected in 500 ml polyethylene bottle)

                                          35
-------
       1.      Shake the collection bottle several times and then pour contents directly into a
              500 ml HOPE bender jar.

       2.      Attach blade assembly to the blender jar and blend for 30 to 60 seconds on
              "LIQUIFY" setting.

       3.      Pour liquified sample into labeled, 120 ml specimen cups as before filling the
              cups no more than 3/4 full.

       4.      Store all cups in freezer.

       Note:  To have enough floe to fill 3 to 5 specimen cups, the floe in the bottom of the
              collection should be at a depth of 1 to 1 /^ inches.
QA/QC

Wear latex gloves while processing sediment.
                                           36
-------
                       LABELING AND PACKAGING SAMPLES
Required Supplies:
Sample tags
Custody seals (signed and dated)
Appropriate size clear plastic bags for sample containers
Electrical tape

Procedure:

1.  After each label is generated using FORMS, place each label on a sample tag, taking special
care to match the number on the FORMS label with the number on the sample tag (see below).
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2.  Have the on-site project officer or the person who collected the sample sign the sample tag in
the appropriate box (see above).

3.  Seal samples if necessary. Example: water samples 500 ml Storemore® bottles should be
sealed with electrical tape stretched around the lid.

4.  Tie the sample tag onto the appropriate sample container.  Make sure that the suffix (matrix
type) on the sample identification # matches the sample type. Example: M2-001-SD tag is tied
to  a sediment sample.

5.  After the sample tag has been attached, fix a signed and dated custody seal  over the lid and
onto the jar or bottle.

6.  Place the sample  container with tag in a clear plastic bag and seal with electrical tape.  Then
place the sample in a holding container (eg. refrigerator at 4°C) or ship.
                                          37
-------
                                  SHIPPING SAMPLES

Required supplies:

Large clear plastic bags for bagging ice
Large trash bags to line shipping containers packing
Adequate  number of shipping containers (e.g. ice chests) for shipping samples
Strapping tape (or Duct tape)

Procedure:

1.  All shipping containers (ice chests) should be clean and dry.

2.  Place samples in a plastic trash bag inside the shipping container.  Add packing material such
as Vermiculite® to the bag if necessary, especially when shipping glass containers. Seal the bag
with electrical tape.  Allow enough room around the bagged samples for plenty of ice, if
required, or additional packing material.

3.  If ice is required, double bag all ice to insure no leakage.  Take special care to insure that
there is  no leaking water or moisture coming from the ice chest when shipping. Federal Express
is very particular about leaky ice chests and can and will stop shipment if a leak is detected.
Place double-bagged ice in a separate trash bag, seal with electrical tape, and place on top of
samples.

4.  Put chain of custody forms in a clean dry bag and tape to the inside lid of ice chest.

5.  Seal  the ice chest with strapping tape. Wrap tape around each end of ice chest.

6.  Place a custody seal on two opposite corners of ice chest.

7.  Attach shipping weigh bill to top of ice chest. If shipping more than one ice chest to the same
location label ice chest 1 of 3, 2 of 3...etc.
                                           38
-------
                                  TURBIDITY TESTS

       Turbidity tests are performed using an HF Scientific Inc. DRT-15C nephelometer.
Operating instructions are posted inside the lid of the instrument.

Procedure:

1.      Turn machine ON.

2.      Insert vial of standard (provided) into reading chamber.  Slowly rotate vial until the NTV
       digital readout displays a minimum value.

3.      Adjust NTV readout to 0.02 by turning the appropriate knob on the machine. Remove
       standard. Machine is ready to read samples.

4.      Mix sample by inverting 125 ml sample bottle 6-8 times. Immediately pour sample into
       clean vial (provided) and insert into reading chamber. Read NTV display and record.

Notes:

       Wipe vials clean of fingerprints and dirt before inserting into reading chamber.

       Read two subsamples (replicates) of each sample.

       Keep sample well mixed between replicate readings.

       Between samples, rinse vial with dH2O and then with an aliquot of the next sample.
                                          39
-------
                         ALKALINE PHOSPHATASE ASSAY

1.      Switch fluorometer (Guilford Fluoro IV model 1452 x 11) and printer "on" to warm up.

2.      Remove reagents (MF and MFP) from freezer and hold in hand or put in pocket to warm
       to room temperature. PROTECT FROM LIGHT!

             MF (ImM MF reagent in methanol) is used to generate standard curve (step 6).
             Stored in glass scintillation vial.

             MFP (ImM MFP in 100 ml Tris buffer ph = 8.7) is added to samples (step 7).
             Stored in plastic microfuge tube.

3.      Pipette 3 ml Trizma buffer into each of 4 clean styrene cuvettes.

4.      Set machine to read APtase. Start by placing one of the above cuvettes (from step 3) in
       position #2 in the machine (slide positioning lever to the 2 position).

             a.      Set wavelenth
                   Press "2" ENTER
                          excitation 430 ENTER
                          emmision 507 RETURN

             b.      Set response time
                   Press "3.5" ENTER
                          4 RETURN

             c.     Calibrate machine (w/ cuvette still in position #2)
                   Press "Calibrate" and wait for number to appear.
                   Press "3.2" ENTER
                          425 RETURN (sets high voltage)

5.      Move cuvette (and positioning lever) to position #1

       Press "Read Print" and see if readout (on printer) is zero.
       If not, press "Autoblank" until it reads  zero.

6.      Prepare standard curve.

       To the 4 cuvettes containing 3 mis Trizma buffer (from step 3) add:

       add 3.0 jA MF to 1st tube, mix w/ transfer pipette, "Read Print"
       add 7.5 (A MF to 2nd tube,
       add 15  jA MF to 3rd tube,    "           "   (continued on next page)
       add 30  ^1 MF to last tube

       (30 iA MF standard should read between 121.8 and 133.8)

       Fill-out log book
                                         40
-------
Run samples

Add 3 mis sample to a cuvette
Add 30 {A MFP to cuvette, mix w/ transfer pipette, "Read Print"

Place tube in incubator for 2 hours (minimum)
Read again.

(Note: for more than one sample, cuvettes are not labelled individually but are arranged
in cuvette box sequentially)
                                   41
-------
                 INTERSTITIAL SOIL WATER SAMPLING PROTOCOL:
               SOUTH FLORIDA ECOSYSTEM ASSESSMENT PROJECT
                                  (PHASE II) REMAP

                                         by

                              Jerry Stober and Phyllis Meyer
              USEPA, Region 4, SESD, Ecological Assessment Branch, Athens, Ga
                                          and
                              Leonard Scinto and Ron Jones
       Southeast Environmental Research Center, Florida International University, Miami, Fl

Introduction

       A component of the Everglades Ecosystem Assessment (Phase II) will include
experimental sampling of an array of interstitial soil (porewater) water samples at each spatially
distributed randomized site.  Approximately 125 sites will be sampled during the May (dry
season) and another 125 sites will be sampled during the September (wet season) survey.  This
protocol has been modified from that developed by L. Scinto and R. Jones, FIU/SERC for the
SERC Flume Project.

Objectives

       1. To modify and implement (in research mode) an interstitial soil water sampling
protocol which is compatable with the ecosystem scale REMAP probability sampling design.

       2. To determine the extent and magnitude of an array of interstitial soil water nutrients
(NH4, NO2, NO3, PO4), selected anions (Cl, Br, etc.), and sulfide.

       3. To establish a baseline porewater condition against which future monitoring and
assessment can be compared.

       4. To explore the existence and significance of porewater spatial gradients.

       5. To determine associations among porewater gradients and surface water gradients
taken at the same time.

       6. And, to determine, associations among constituents in porewater, surface water, soil
and plant indicator species responses occurring in the ecosystem.

Protocol

       Water Sample Containers
             Soil interstitial water (SI) is collected into clean 30 ml high-density polyethylene
(HOPE) bottles (Nalgene #2089-0001-Fisher Scientific, FS# 03-313-2A).

       Soil Interstitial Water Collection
             The soil interstitial water is collected via a soil interstitial water sampler (Sipper).
Sippers consist of a filter (nominal porosity = 60 um) (Porex 6810, Interstate Specialty Products)
held onto a male slip connector (Cole-Parmer #E-06359-05) with telfon tape. The slip connector

                                          42
-------
is attached to a hollow tube (1/16" ID x 1/8" OD, Tygon, FS# 14-169-1B) approximately 65 cm
in length, the distal end of which is connected to a capped female luer fitting (CP#E-063 59-25).
An array of five stainless steel sippers will be installed to a maximum depth of 10 cm with
individual insertion tools for each.  The array will be positioned so that the distance between
sippers is not less than 30cm. The insertion tool is the primary modification on the original
method to provide a fixed depth insertion with an associated soil surface sealing flange. The
sipper and insertion tool will remain in place until each sample has been collected.  The insertion
tool is also designed with water tight extensions to 120cm to prevent surface water from running
down the inside of the insertion tube during periods of high water.

Steps

1.  Load each insertion tool with a sipper with attached tubing.
2.  Locate five sites at least 30 cm apart which are relatively free of standing vegetation.
3.  Press the insertion tool into the soil firmly assuring the flange is tight against the soil surface
with the flange ring imbedded into the soil.  Note: A 9 cm diameter by 2.5 cm deep sharpened
ring was added to the bottom side of the flange to increase contact with the soil surface. In
addition a one way flapper valve was installed in the flange to allow surface water and gases to
exit the sampler during installation.
4.  Use the insertion rod to push the sipper into the undisturbed soil 4 cm to a depth of about 10
cm.
5.  Connect a syringe (60 ml) to the female luer fitting on each sipper.
6.  Apply suction and pull ten ml into the  syringe. The void volume of an empty sipper, with 65
cm tubing, is approximately 1.5 ml. Pulling slightly greater volumes than this assures flushing.
Disconnect syringe from luer fitting and attache a filter (Whatman GF/F, FS# 09-874-64 in
syringe filter-holder Gelman FS#09-730-2250).  Filter this water into the sample bottle in three 3
ml increments as rinse water discarding each in succession. Reapply suction to collect
approximately 30 ml of pore water.  If collection is difficult place binder clips on syringe such
that suction is held and allow time for sample to be obtained.
7.  Extract only one water sample from each of the five sippers for NO2, NO3, PO4; NH4;
selected anions; and sulfide. Four samples will be collected leaving the fifth sipper in reserve in
case a problem develops during sampling.
8.  The syringe used for the sulfide  sample will  be pre-loaded with a zinc acetate/sodium
hydroxide solution into which the sample will be drawn.  Once 30 ml has been drawn into the
syringe it will be disconnected, capped, labeled and placed in a cooler for transport.
9.  All samples will be stored on ice until  returned to the laboratory the same day.
10. Soil interstitial water samples (nutrients and anions) will be stored either in a refrigerator
and analyzed immediately (<24 h) or stored frozen until analyzed (<30 d).  Preserved sulfide
samples will be analyzed immediately upon return from the field.
11. If surface water depth exceeds the height of the insertion tube add extension at step 1 and
proceed as directed.  The amount of water for flushing will be increased to 15  ml when the
extension is used.
12. This procedure will be  repeated consistently across all randomly selected REMAP sample
sites in the ecosystem
                                           43
-------
Figure 1. Porewater sampler.
Figure 2. Sampler prior to
insertion in soil.
                                         44
-------
Figure 3. Design drawing of sampler.
               45
-------
               Attachment 4
Analytical Support Branch Operations and
Quality Control Manual - SESD, Region IV
-------
  ANALYTICAL SUPPORT BRANCH

OPERATIONS AND QUALITY CONTROL
             MANUAL
   ENVIRONMENTAL PROTECTION AGENCY
 SCIENCE AND ECOSYSTEM SUPPORT DIVISION
             REGION 4
       980 COLLEGE STATION ROAD
          ATHENS, GA 30605
-------
                             DISCLAIMER

The mention of trade names or commercial products in this manual is for
illustration purposes, and does not constitute endorsement or recommendation
for use by the Environmental Protection Agency.
-------
                        TABLE OF CONTENTS
Section
1.  INTRODUCTION	1-1

2.  BRANCH ORGANIZATION AND OPERATION  	  2-1

3.  CHAIN-OF-CUSTODY 	  3-1

    3.1. Introduction	3-1
    3.2. Sample Custody Forms	3-1
    3.3. Standard Operating Procedure - Sample Receipt/Custody .   .  3-1
    3.4. Audit of Custody Records	3-3
    3.5. Policy for Disposal of Laboratory Samples 	  3-3
    3.6. Special Sample Handling Instructions  	  3-4

4.  GENERAL LABORATORY PRACTICES 	  4-1

    4.4.  Laboratory Apparatus and Instruments 	  4-1
    4.5.  Laboratory Supplies  	  4-2
    4.6.  Laboratory Waste Disposal Practices  	  4-3
    4.7.  Procedures for Satellite Hazardous Waste Accumulation.   .  4-7
    4.8.  Guidelines for Disposal of Environmental Samples ....  4-8
    4.9.  Handling, Storage, Disposal and Reporting Procedures .   .  4-9

5.  LABORATORY EQUIPMENT MAINTENANCE AND SERVICES	5-1

6 .  LABORATORY SAFETY	6-1

    6.1. Introduction	6-1
    6.2. General	6-1
    6.3. Sample Receiving and Logging	6-2
    6.4. Compressed Gases	6-3
    6.5. Radioactivity	6-3
    6.6. Laboratory Waste Disposal Practices 	  6-3

7.  METHODOLOGY	7-1

8.  SAMPLE COLLECTION AND HANDLING 	  8-1

    8.1. Sample Collection - Water 	  8-1
    8.2. Sample Handling - Water	8-1
    8.3. Sample Collection and Handling Other Substances 	  8-1

9.  SAMPLE RECORDS AND DATA HANDLING	9-1

    9.1. Sample Accountability 	  9-1
    9.2. Chemical Sample Logging 	  9-1
    9.3. Central Laboratory Sample Logging 	  9-1
    9.4. Chemical Data Handling	9-1
    9.5  Computerized Analytical Data System 	  9-2

10. ORGANIC ANALYSIS, PERFORMANCE QUALITY CONTROL AND ANALYTICAL
     OPERATION	10-1

    10.2. General	10-1
    10.3. Organic Methodology	10-1
    10.4. Sample Prep,  of Semivolatile and Pesticide fractions .   . 10-1
-------
    10.5.  Surrogate Standards	10-4
    10.6.   Internal Standards	10-8
    10.7.   GC Analysis	10-8
    10.8.   GC/MS Analysis	10-18
    10.9.   Extract Storage	10-29
    10.10.  Preparation, Storage, and Use of Organic Standards. .   . 10-30
    10.11.  Data Reporting	10-35

11.  INORGANIC ANALYSIS, PERFORMANCE QUALITY CONTROL AND
     ANALYTICAL OPERATION	11-1

    11.2.  General	11-1
    11.3.  Custody	11-1
    11.4.  Metals	11-2
    11.5.  General Inorganic	11-11
    11.6.  QC Requirements for General Inorganic	11-11

12.  PERFORMANCE QUALITY CONTROL DATA HANDLING	12-1

13.  ANALYTICAL CORRECTIVE ACTIONS	13-1

14.  DATA QUALITY OBJECTIVES	14-1
-------
                                LIST OF FIGURES




                                                                     Page




Organizational Chart  (Fig 2-1)	2-2
-------
                                LIST OF TABLES
List of Organic Test Procedures  (Table 7-1)	7-2
Organic Method References, Region 4 Method Tracker  (Table 7-2)  .  .   7-6
Test Name and Reporting Units  (Table 7-3)	7-7
Recommended Sample Containers, Sample Preservation, Sample
 Holding Times, And Permissible Sample Type  (Table  8-1)	   8-3
Organic Method Number and Sample Type  (Table 10-1)  	   10-42
Standard Levels and Concentrations  (Table 10-2)	   10-43
Drinking Water Methods  (Table  11-1)	   11-4
NPDES Methods  (Table 11-2) 	   11-6
Nutrients/Classicals Capabilities and Methods  	  11-13
-------
                                 LIST OF FORMS
Chain-Of-Custody Seal  (Form 3-1)	3-8
Chain-Of-Custody Record  (Form 3-2)  	   3-9
Custody Room Sample Log  (Form 3-3)	3-10
Diagram of Custody Room  (Form 3-4)	3-11
Disposal Letter  (Form 3-5) 	   3-12
Water Extraction Log Book Form  (Form 10-1)	10-45
Solids/Waste Extraction Log Book  Form  (Form 10-2)	   10-46
Tissue Extraction Log Book Form  (Form  10-3)	10-47
GC Screen Log Book Form  (Form 10-4)	10-48
GC/MS Log Book Form  (Form 10-5)	10-49
Stock Standard Log Book Form  (Form  10-6)	10-50
Stock Summary Log Sheet  (Form 10-7)	10-51
GC Analysis Log Book Form (10-8)	10-52
Surrogate Recoveries Log Book Form  (10-9)	10-53
Master Log GC Analysis Log Book Form (10-10)	10-54
Pesticide QC Water Data A (Form 10-11)	10-55
Pesticide QC Water Data B (Form 10-12)	10-56
Pesticide QC Soil Data A  (Form 10-13)	10-57
Pesticide QC Soil Data B  (Form 10-14)	10-58
Dilution Standard Log Form (Form  10-15)	10-59
MQL Guidelines for Pesticides  (Form 10-16)  	   10-60
Vial Storage Location Form (Form  10-17)   	   10-61
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                                                Section:  1
                                                Revision: 1
                                                Date: December 1,  1997
                                                Page:  1
1.   INTRODUCTION


    1.1  This manual is designed to delineate the routine operation of the
    USEPA Region 4 Analytical Support Branch.  The primary purpose of this
    document is to establish and maintain uniform operational and quality
    control guidance for regional analytical chemistry activities, contractor
    laboratory monitoring/performance,  and quality assurance/quality control
    activities.  The establishment of,  and adherence to,  uniform elements of
    an intralaboratory quality control  program are essential to the production
    of reliable analytical data.

    1.2.   Coordination of Region 4 quality assurance activities and likewise,
    the Analytical Support Branch (ASB),  rests primarily with the Region 4
    Quality Assurance Officer (QAO).   The functions and responsibilities of
    the QAO are identified in the Region 4 Quality Assurance Program Plan.
    The QAO functions as a focal point  for the dissemination of information
    and provides program managers with  technical advice pertaining to the
    development, implementation, and operation of quality assurance
    activities.  Implementation of agency quality assurance policies
    applicable to the Analytical Support Branch laboratory is the
    responsibility of the Chief, Analytical Support Branch.

    1.3  While the implementation of quality assurance policy is a management
    function, each individual staff person has a responsibility for the
    operational aspects of the quality  assurance.  It is the individual
    responsibility of each analyst and  his/her supervisor to monitor quality
    control indicators and to provide for corrective actions when necessary.

    1.4  This manual and the quality control protocols described herein are
    not to be viewed as all inclusive.   Rather, they serve as a basic
    foundation on which to build a stronger quality assurance program within
    the Branch.  Methodologies and some quality assurance documents are
    included by reference.
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                                                    Section 2
                                                    Revision:  0
                                                    Date:  August 1990
                                                    Page 1
2. BRANCH ORGANIZATION AND OPERATION

    2.1. The Analytical Support Branch organizational structure is shown in
    Figure 2-1.

    2.2. The Branch is a technical support activity with the following
    functions:

        2.2.1.  Provides chemical laboratory services in support of all
        regional program needs.

        2.2.2.  Provides consultation and assistance to local, State,  and other
        agencies in matters of analytical methodology and laboratory quality
        assurance.

        2.2.3.  Provides personnel as regional representatives to national
        programs relating to selection, validation, and promotion of the use
        of official EPA analytical methods.

        2.2.4.  Participates in national and regional interlaboratory method
        evaluation studies.
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                                              Section:   2
                                              Revision:  1
                                              Date:  December 1,  1997
                                              Page:   2
                       SCIENCE AND  ECOSYSTEM

                          SUPPORT DIVISION
    OFFICE OF
     QUALITY
    ASSURANCE
   GARY BENNETT
  ANALYTICAL SUPPORT
     BRANCH
   CHARLES HOOPER
INORGANIC CHEHISTE
   SECTION
 JENNY SCXFRES
 ORGANIC CHEMISTRY
   SECTION
 BILL HCDANIEL
  RUSSELL WRIGHT, DIRECTOR
ALLAN ANTLEY, DEPUTY DIRE
  TECHNICAL ADVISOR (SEE)
  LEAD REGION COORDINATOR
    REGIONAL SCIENTIST
     ENFORCEMENT AND
   INVESTIGATIONS BR
      BILL BOKEY
  OFFICE OF PROGRAM
   AND  TECHNICAL
    OPERATIONS
   BETTY  KINNEY
   ECOLOGICAL
 ASSESSMENT BRANCH
BRANCH CHIEF -  VAi
                            Figure 2-1
-------
                                                    Section 3
                                                    Revision:  0
                                                    Date:  August 1990
                                                    Page 1


3. LABORATORY CHAIN-OF-CUSTODY

    3.1. Introduction

        3.1.1. Complete documentation of the sample collection and handling
        process is an extremely important aspect of a regulatory monitoring
        effort.  Formal chain-of-custody procedures provide for a written
        record of sample traceability,  accountability,  and serve to validate
        sample integrity.  All samples  received by ASB for chemical analysis
        are controlled by these procedures.  Field sample custody procedures
        are detailed in the Enforcement Investigations Branch, Standard
        Operating Procedures and Quality Assurance Manual.

        3.1.2. All custodial documentation on samples for ecological/
        biological analyses will be maintained within the records of the
        project biologist.  The Analytical Support Branch sample custodian
        will not maintain these records.

    3.2. Sample Custody Forms

        3.2.1. The following sample custody and disposal forms are shown in
        Form 3-1 through 3-5:

            3.2.1.1. Chain-of-Custody Seal (Form 3-1).

            3.2.1.2. Chain-of-Custody Record (Form 3-2).

            3.2.1.3. Custody Room Sample Log (Form 3-3).

            3.2.1.4. Diagram of Custody Room (Form 3-4).

            3.2.1.5. Disposal Memo Form (Form 3-5).

        3.2.2. In addition to these forms, custody information is maintained
        in the master logbooks, Data Management System,  computer sample log,
        the chemistry field logbooks, and in the individual analytical data
        books.

    3.3. Standard Operating Procedure - Sample Receipt/Custody

        3.3.1. Samples are received by  the sample custodian or a designated
        alternate.  The alternate must  be an EPA employee on the staff of the
        Analytical Support Branch.  Samples that arrive after hours will be
        secured in the custody room and the sample custodian will receive them
        the next business day.  At the  time of receipt,  the custodian or
        designee will perform the following actions:

            3.3.1.1. Sign the chain-of-custody form and record the date and
            time of sample receipt.

            3.3.1.2. Document whether the individual samples, boxes, or ice
            chests were sealed upon receipt;  also document unusual conditions
            of sample container in remarks section of the custody form.

            3.3.1.3. Log all samples into the Data Management System.

            3.3.1.4. Place sample numbers on all sample tags or containers and
            secure samples in the area  designated for new samples.  The
            designated area will be the middle shelf in the front entrance of
            each walk-in cooler.  Walk-in coolers will be labeled as follows:

                3.3.1.4.1. Metals/Organics:  Storage for metals samples,
                extractable organics and pesticide samples.
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                                            Section:  3
                                            Revision: 1
                                            Date: December 1, 1997
                                            Page:  2
        3.3.1.4.2. Ultra Low Level:   Storage for Metals, extractable
        organics, pesticide and classical ultra low level samples such
        as drinking water.  Note: In special cases some low level
        samples will be stored in refrigerators in the laboratories
        such as the low level mercury samples.

        3.3.1.4.3. Classical Inorganic/EAB:   Storage for samples for
        classical analyses and Ecological Assessment Branch samples.

        3.3.1.4.4. The walk-in freezer will  be divided equally between
        the ASB and EAB for frozen samples.

        3.3.1.4.5. Volatile organic  samples  will be stored in a
        secured refrigerator in the  GC/MS laboratory.

    3.3.1.5. After samples are placed in the area designated for new
    samples the following will be performed:

        3.3.1.5.1. As soon as possible,  the  analyst(s)  will move the
        samples onto their allotted  shelves  and place them in a manner
        that is functional for their team.  See Form 3-4.  Each team
        is responsible for keeping their area of the custody room
        secure, orderly, neat and maintaining space for incoming
        sample placement.

        3.3.1.5.2. It is the responsibility  of the sample custodian to
        insure that all areas of the custody room are maintained in a
        clean, orderly and secure manner.

    3.3.1.6. After sample logging is completed, computer data
    reporting information will be available  in the Database Management
    System for reference.

    3.3.1.7. The original field custody form, along with a computer
    printout of the requested analytical tests, will be maintained in
    the ASB files.  A copy of the field custody form and a copy of the
    computer print out will be sent  to the project leader responsible
    for sample collection.

3.3.2. Access to the main custody room area  will be by computer card
as authorized by the Chief of the Analytical Support Branch or Chief
of the Ecological Assessment Branch.

3.3.3. For an analyst to receive samples for analysis,  he/she must
assume legal custody of the samples  and the  following actions are
required:

    3.3.3.1. The analyst must complete the appropriate Custody Room
    Sample Log including their initials, listing the sample numbers,
    date and time.  Samples may be removed from the custody area only
    after performing the appropriate documentation transferring
    custody to the analyst.   There  will be  4 separate log books: 1)
    metals, 2)extractable and pesticide, 3)  volatile and 4)  classical
    and inorganics.  Records of samples to be stored by the Ecological
    Assessment Branch will be maintained in  logbook #4  (for classical
    and inorganic chemistry analyses.)

    3.3.3.2. The analyst will return the samples to the custody room
    when he/she is finished with the analysis.   In no case will the
    original samples (less aliquot required  for analysis) remain
    outside the custody room during  non-duty hours.  When the samples
    are returned, the analyst will note the  date and time returned in
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                                                Section:  3
                                                Revision: 1
                                                Date: December 1, 1997
                                                Page:  3


        the appropriate Custody Room Sample Log, returning custody back to
        the sample custody room.

        3.3.3.3. The Custody Room Sample Logs will be maintained as a
        permanent file.

3.4. Audit of Custody Records

    3.4.1. Audits of custody information will be performed by the Branch
    Chief or designee.  These audits will include an examination of
    custody documentation of randomly selected samples for traceability,
    completeness, and accuracy.  The results of these audits will reflect
    the general effectiveness of the custody procedures.

3.5. Policy for Disposal of Laboratory Samples

    3.5.1. No criminal investigation samples, extracts or sample
    containers will be disposed of until authorized by the appropriate
    officer of the court.   Due to the timing on litigation, criminal
    samples usually require long term storage.  Space limitations within
    the custody room make it necessary to store criminal samples within
    the HAZMAT facility using the following procedure:  1)  At the
    completion of all required analyses the "characterization report" will
    be generated, denoting the sample as to its hazardous or non-harzadous
    status.  2) A copy of the characterization report and custody of the
    samples will be transfered to the Divisional SHEM Officer.  3)  The
    SHEM Officer will maintain custody of the criminal samples while in
    storage and will coordinate disposal with all appropriate parties.

    3.5.2. Samples and their extracts that are not part of a criminal
    investigation will normally be disposed of within 90 days from the
    completion of the final laboratory data report.  The exception to this
    will be when a sample hold request is implemented.  The "Intent to
    Dispose of Samples Memo" (Table 3-5)  will be prepared and sent out by
    the Sample Custodian or designee as desingated below.

        3.5.2.1. Intent To Dispose Memo and Sample Hold Request

        30 Days after all laboratory analyses have been completed and the
        data reported, the sample custodian will submit the disposal memo
        (form 3-5) to the appropriate project manager.  The memo will be
        submitted via cc mail with receipt requested.  The sample
        custodian will maintain a file of receipts to document the notice
        received by the project manager.  To place samples on hold  (non-
        disposal) the project manager must so note on the form memo in the
        appropriate place, list why the hold is necessary,  and return the
        memo to the sample custodian.

        3.5.2.2. The sample custodian or designee will monitor samples
        requested for hold and the samples ready for disposal.   Samples
        ready for disposal will be entered into the Database Management
        System program which then generates a list of compounds found in
        each sample.  This "compound list" is used to  identify those
        samples that may be disposed of as ordinary environmental samples
        and those that are defined as "hazardous" by regulation.

        3.5.2.3. Samples that qualify as hazardous are documented within
        the Data Management System Program and a list is generated.  Those
        samples characterized as hazardous will be coordinated with the
        Science and Ecosystem Support Division  (SESD), Safety Health and
        Environmental Management (SHEM) Officer for disposal.  Refer to
        Chapter 4 for more details on hazardous waste disposal.
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                                                Section:   3
                                                Revision:  1
                                                Date:  December 1,  1997
                                                Page:   4
    3.5.3. For those samples characterized as non-hazardous (routine
    environmental),  a disposal report will be generated and provided to
    designated staff as appropriate.  Sample disposal of the routine
    environmental samples should be completed by the appropriate analyst
    within 2 weeks from disposal report distribution.  The routine
    environmental samples will be disposed of in the following manner:

            3.5.3.0.1. The tags are removed, sorted and sent to the sample
            collectors.

            3.5.3.0.2. Water samples are disposed of by pouring the water
            down the sink drain and rinsing the containers out with water.
             These containers will be recycled.  Preserved samples must be
            neutralized.  Each person disposing of samples must maintain
            an awareness of the status of the laboratory centralized
            neutralization system.  If  the neutralization system is under
            maintenanace and/or not functional, the preserved waters must
            be neutralized before flushing down the sink.

            3.5.3.0.3. Non-hazardous soil/sediment samples are disposed of
            in the dumpster.

3.6. Special Sample Handling Instructions

    3.6.1. Soils from Foreign Countries

        On occasion the Analytical Support Branch may receive requests  for
        analyses of foreign soil samples.  Such samples require special
        handling for labeling and disposal.  The following procedure
        should be followed:

        3.6.1.1. When booked into the data management system there must be
        a special notice of the fact that the samples are of "FOREIGN
        SOIL".

        3.6.1.2. When the samples are received at the laboratory the
        sample custodian or designee is responsible for labeling the tags
        with the notation "FOREIGN SOIL".  The tag must remain with the
        sample container until project completion and sample disposal.

        3.6.1.3. After the samples are tagged and logged they should be
        stored in the custody area per standard procedures.

        3.6.1.4. Unused original sample must be autoclaved prior to
        disposal for at least 30 minutes at 121 C and 15 psi.

        3.6.1.5. After autoclaving the samples may be disposed of using
        standard procedures for environmental samples.   NOTE:   ASB will
        not routinely accept foreign soil/sediment samples suspected to be
        hazardous as defined by statute.  However, in the unlikely event
        that the test results indicate that they are "hazardous",
        disposal should be coordinated with the SESD SHEM Officer.  Refer
        also to Chapter 4 for additional details of disposal of samples
        characterized as "hazardous".

    3.6.2. Handling Procedures for Potentially Hazardous Waste Samples  in
            the Laboratory

        A small percentage of samples received by ASB are characterized as
        concentrated waste.  In these instances field personnel are
        required to screen the waste materials to ensure safe
        transportation and handling of the samples.  Concentrated waste
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                                        Section:  3
                                        Revision: 1
                                        Date: December 1,  1997
                                        Page:  5
samples are not preserved and are not required to be cooled to 4
degrees C.

The waste samples should be in a primary container that has been
                            cleaned by field personnel to insure
                            no contamination to the exterior of
                            the container.  The samples should
                            then be tagged,  sealed and placed
                            within a plastic bag secured with
                            electrical tape.  Each sample will
                            then be placed within a 6-quart
                            plastic pail with a spill proof, tight
                            fitting lid and packed with
                            vermiculite as a secondary
                            containment.  There should be special
                            notations to the sample custodian as
                            to the hazardous nature of the
                            samples.  It is the Sample Custodian
                            responsibility to insure that the
                            hazardous nature of the samples is
                            communicated to all ASB staff.
                            Concentrated waste samples will be
                            stored within the hood of the custody
                            room.

3.6.2.1. When concentrated waste samples are received at the
Laboratory the following procedure should be followed for the
storage and handling:

    3.6.2.1.1. Samples will be signed out of the designated
    storage area and chain of custody maintained as with routine
    environmental samples.

    3.6.2.1.2. The samples will be transported unopened within the
    laboratory and placed in the appropriate preparation area
    within a fume hood.  Samples should never be transported
    outside a fume hood unless they are sealed within the
    secondary containment vessel.

    3.6.2.1.3. Once inside the hood, the secondary containment may
    be opened and the individual sample processing may begin.
    Care should be taken to keep the secondary containment vessel
    so that the original sample may be repacked after completion
    of the preparation for analysis.  All sample processing and
    manipulation should be accomplished within the hood.  At no
    time should the raw sample be removed from the hood without
    being properly repacked within the primary and secondary
    containment vessels.

    3.6.2.1.4. Personal Protective Equipment (PPE):  All initial
    preparation/aliquoting of the samples must be performed using
    the following personal protective equipment at a minimum: 1)
    Latex or other type of appropriate gloves;  2)  Lab Coat; 3)
    Safety glasses or safety face shield.  Higher levels of PPE
    may be required as determined by information received from
    field personnel, knowledge/experience of the analyst, or lab
    supervisor.  These determinations will be made by results of
    field screening and any additional knowledge of the sample
    matrix.  It is the responsibility of each analyst to insure
    that appropriate methods and safe laboratory practices are
    followed at all times.  If at any time an analyst has a
    concern about the preparation process, or if unsure about
    their ability to safely handle the samples,  they should
    immediately contact their supervisor.
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                                    Section:  3
                                    Revision: 1
                                    Date: December 1, 1997
                                    Page:  6
3.6.2.1.5. Any glassware or equipment such as spatulas,
pipets, droppers, etc. used in contact with the concentrated
waste must remain within the hood until cleaned or disposed of
in an appropriate fashion.  These may be placed in the
secondary containment container to be disposed of with the
samples.  Any solvents,  solutions, or materials (kimwipes,etc)
 used to clean waste from glassware or other equipment must be
collected and treated the same as the waste material.   Where
practical and prudent for the analytical method, choose items
that are disposable.  In all cases consult with the Divisional
SHEM Officer before removing and discarding any of the
contaminated materials.

3.6.2.1.6. At the completion of the sample processing the
original samples should be repacked into the primary and
secondary containment with care taken to insure that there is
no waste contamination on the exterior of the containment
vessels.  When properly repacked, the samples should be
returned to the custody room hood and custody is returned by
signing the appropriate logbook.  Refer to Chapter 4 for
details of the disposal of hazardous waste samples.
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                                    Section:   3
                                    Revision:  1
                                    Date:  December 1,  1997
                                    Page:   7
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           Chain-of-Custody Seal
                  Form 3-1
-------
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                                REGION 4
                 U.S.  ENVIRONMENTAL PROTECTION  AGENCY
                                                                CHAIN   OF   CUSTODY   RECORD
                                                                                                                                    ENVIRONMENTAL  SERVICES DIVISION
                                                                                                                                    COLLEGE  STATION ROAD
                                                                                                                                    ATHENS,  GEORGIA 30613-7799
                PROJECT NO.
                PROJECT NAME/LOCATION
                                                    PROJECT LEADER
                        ESD  SAMPLE  TYPES
                 1. SURFACE WATER
                 2. GROUND WATER
                 3. POTABLE WATER
                 4. WASTEWATER
                 5. LEACHATE

                 11. OTHER .
                                     S. SOIL/SEDIMENT
                                     7. SLUDGE
                                     fl. WASTE
                                     9 AIR
                                     10. RSH
                                                         STATION LOCATION/DESCRIPTION
                 ELINQUISHED BY:
                (PRINT)
                (PRINT)
                                                    SAMPLERS (SIGN)
RECEIVED BY:
(PRINT)	
                                                           RECEIVED BY:
                                                            (PRINT)	
                                                           (SIGN^
                                                                                              REMARKS
                                                                                             RELINQUISHED BY:
                                                                                             (PRINT)
                                 RELINQUISHED BY:
                                  (PRINT)
                          White and Pink copies accompany sample shipment to laboratory; Pink copy retained by laboratory;
                          White copy is returned to samplers; Yellow copy retained by samplers.
                                                                                                                              DATE/TIME
                                                                                                                              DATE/TIME
RECEIVED BY:
(PRINT)
RECEIVED BY:
(PRINT)	
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                                             Section:  3
                                             Revision: 1
                                             Date:  December 1,  1997
                                             Page:   9
                                                                 Book   15
CUSTODY ROOM
SAMPLE LOG
  SAMPLE #
PARAMETER
                                 OUT
DATE
TIM
 E
                              IN
DATE
TIM
 E
                          DATE
DISPOSED
NAME
                       Chain-of-Custody Form
                              Form  3-2
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                            Section:   3
                            Revision:  1
                            Date:  December  1,  1997
                            Page:   10
Custody Room Sample Log
        Form 3-3
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                                      Section:  3
                                      Revision: 1
                                      Date: December 1,  1997
                                      Page:  11
Organ ic/Motals
   Cooler
                       Ultrj
                  New Samples

                               New samples
                               New Samples
                               New Samples
                               New Semples
         Diagram of Custody Room
                 Form 3-4
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                                                    Section:  3
                                                    Revision: 1
                                                    Date: December 1, 1997
                                                    Page:  12
                              MEMO     FORM


    SUBJECT:    Notice of Intent to Dispose of Samples; (Sample Project
                Name; SESD project no., city, state)

    FROM:       Person sending memo  (i.e. sample custodian/coordinator);


    TO:         Project manager
    This memorandum is being sent as a reminder that the Analytical
Suppport Branch has completed all analyses on the subject samples.  Due to
our limited space for long term sample storage,  we must proceed with
sample disposal.  Please take note that within sixty (60) days of the date
of this memo the original samples will be disposed of following all
applicable and appropriate statutes.

    If there is any reason to hold these samples in custody for longer
than 60 days, you may activate a "hold" by so indicating below and
returning this memorandum via cc mail to Debbie Colquitt within the next
30 days.  Also, please state briefly the reasons for retaining these
samples in custody.

    Thank you for your cooperation in this request.
Date:

Project Manager Name:

Reason for Hold:
                           Disposal Memo Form
                                Form 3-5
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                                                    Section:  4
                                                    Revision: 1
                                                    Date: December 1,  1997
                                                    Page:  1
4.  GENERAL LABORATORY PRACTICES

    4.1. Intrinsic to the production of quality analytical data is the quality
    of laboratory services available to the analyst.  Without adequate quality
    control being exercised with regard to facilities, services,  laboratory
    environment,  instrumentation,  and laboratory supplies, an analyst cannot
    be expected to produce reliable analytical data.

    4.2. Recognizing the necessity of maintaining control over general
    laboratory operation, the subsequent sections outline provisions for
    maintaining the quality laboratory support services.

    4.3. All quality control checks listed in this section should be recorded
    in the appropriate logbook or file (printed or electronic).

    4.4. Laboratory Apparatus and Instruments

        4.4.1. Incubators and Waterbaths

            4.4.1.1. If an automatic temperature recorder is not  used, place
            calibrated thermometer on a central shelf and record  temperature
            at least once daily (more frequently if required) when the
            incubator is in use.

            4.4.1.2. Periodically check temperature variations when incubator
            or waterbath is loaded to capacity.

            4.4.1.3. Drain and clean waterbath as required and refill with
            laboratory pure water.

        4.4.2. Refrigerators and freezers

            4.4.2.1. Check and document temperature weekly.

            4.4.2.2. Clean periodically and discard outdated materials.

            4.4.2.3. Do not store food in any laboratory refrigerator or
            freezer.  There is a refrigerator in the lunchroom for storage of
            food.

        4.4.3. Autoclave and Hot Air Oven

            4.4.3.1. Record date,  and sterilization time, and temperature for
            each cycle.

            4.4.3.2. Operate hot air oven at a minimum of 170°C for
            sterilization.
        4.4.4. Balances

            4.4.4.1. Check with Class-S weights at least monthly and record in
            the QC log.

            4.4.4.2. Clean and level balances as required.
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                                                Section 4
                                                Revision: 1
                                                Date: December 1, 1997
                                                Page 2

        4.4.4.3. Maintain annual maintenance services contract.

    4.4.5. pH Meters

        4.4.5.1. Date all pH buffer solutions when opened.  Buffers that
        have reached the manufacturer's expiration should  be discarded and
        replaced.

        4.4.5.2. Standardize meter with pH 7.0 and pH 4.0 and/or pH 10
        buffer before each use,  or as required by regulated methods.

        4.4.5.3. Use pH buffer aliquot only once.

    4.4.6. Thermometers

        4.4.6.1. Unless otherwise specified by regulatory methodoloy,  it
        is the policy of ASB to use only non-mercury containing
        thermometers in all laboratory operations.  Check all  laboratory
        thermometers annually with a reference NIST thermometer.  Mark any
        necessary corrections on each thermometer and record in the QC
        logbook.

4.5. Laboratory Supplies

    4.5.1. Glassware

        4.5.1.1. Glassware used in general laboratory operations must  be
        of a high quality borosilicate glass, e.g.,  "Pyrex" or "Kimax."
        Volumetric glassware must be of a Class "A"  quality.

        4.5.1.2. Clean glassware in hot water with a suitable  detergent,
        rinse in hot water to remove detergent residue, and finally rinse
        in laboratory pure water.  Glassware used in special  analyses,
        e.g., metals and organics require more scrupulous cleaning, e.g.,
        acid and/or solvent washing.  Glassware must be oven-dried or
        drained thoroughly before use or storage.  Glassware  used in trace
        metals analysis should be air dried.  In some instances it may
        prove to be advantagous to store labware for ultrace  level metal
        analyses in a dilute acid solution.  In operations of  specific,
        low-level analyses glassware should be isolated and maintained
        only for these specific operations.

        4.5.1.3. If, at any time a new washing compound or cleaning
        application is introduced, it is imperitive that  tests be
        performed to assure that the glassware is free of intereferences
        before routine analyses are begun.

    4.5.2. Chemicals, Reagents,  Solvents, Standards, Gases, and Culture
          Media

        4.5.2.1. The quality of chemicals, reagents, solvents, standard
        gases, used in the laboratory is determined by the sensitivity and
        specificity of the analytical techniques being used.   Reagents of
        lesser purity than specified by a method will not be  used.

        4.5.2.2. Reagents, chemicals, solvents, and standard reference
        materials (excluding high-demand items) should be purchased in
        small quantities to minimize extended shelf storage.

        4.5.2.3. Date all reagents, chemicals, solvents,  and standard
        reference materials when received and when opened or  prepared, and
-------
                                                Section 4
                                                Revision: 1
                                                Date: December 1,  1997
                                                Page 3

        discard when outdated,  or when evidence of discoloration or
        deterioration is detected.

    4.5.3. Laboratory Pure Water

        4.5.3.1. The laboratory pure water system consists of a
        deionization supply followed in individual labs by exchange
        modules and other modules capable of supplying high quality (18
        megaohm) water suitable for the application.  The system is also
        equipped with a direct  reading resistivity meter.

        4.5.3.2. Change system modules as recommended by the manufacturer
        or as indicated by water quality.  Date modules when changed.

4.6. Laboratory Hazardous Wastes Handling and Disposal Procedures

    4.6.1. It is the policy of  the Analytical Support Branch to collect,
    store, package, label, ship and dispose of hazardous wastes in a
    manner which ensures compliance with all Federal, State and local
    laws,  regulations and ordinances.  These procedures are also designed
    to minimize employee exposure to hazards associated with laboratory
    generated hazardous wastes  and to afford maximum environmental
    protection.

    4.6.2. Policies and procedures for operation of the Division's
    environmental compliance program are detailed in the document, Safety
    Health and Environmental Management Program, Procedures and Policies
    Manual.   This manual is maintained by the Divisional Safety, Health
    and Environmental Managment (SHEM)  Officer.

    4.6.3. Regulatory Requirements

        4.6.3.1. ASB is subject to the Resource Conservation and Recovery
        Act  regulations as contained in the Georgia Rules for Hazardous
        Waste Management for the handling, storage and disposal of
        laboratory-related hazardous wastes.  Generally, the laboratory is
        subject to the rules applicable to generators of 100-1000
        kg/month.
    4.6.4. Waste Handling Practices

        4.6.4.1. Hazardous Waste Determination.  The determination of
        whether or not a waste is a regulated substance is made by the
        Divisional SHEM Officer.  Generally the following criteria apply
        either individually or in combination:

            4.6.4.1.1. Is the waste material listed in 40 CFR 261.30 -
            261.33(e)?

            4.6.4.1.2. Does the material conform to any of the listing
            characteristics specified in 40 CFR 261.20 - 261.24?

            4.6.4.1.3. Does the generator have personal knowledge of the
            hazardous nature of the material?

            4.6.4.1.4. Would disposal of the material as non-regulated
            waste pose an environmental threat and/or leave the Agency
            open to criticism?
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                                            Section 4
                                            Revision: 1
                                            Date: December 1, 1997
                                            Page 4

    4.6.4.2. Wastes which meet any of the above criteria must be
    handled and disposed of as a regulated waste.

4.6.5. Waste Minimization

    4.6.5.1. The Branch Chief is responsible for ensuring that staff
    adhere to all Region 4 waste handling and disposal requirements
    for all laboratory operations.  This includes the implementation
    of procedures (i.e., technical and/or management) designed to
    minimize the generation of hazardous wastes.

    4.6.5.2. Waste minimization should be a prime consideration of
    initial experimental design and investigation planning.  The degree
    to which waste minimization is achieved ultimately impacts the
    operational and cost effectiveness of our overall hazardous waste
    management program.

4.6.6. Tracking

    4.6.6.1. A tracking system is maintained to account for monthly
and annual hazardous waste generation.  This system is maintained by
the Divisional SHEM Officer.

    4.6.6.2. Jim Gray, SHEM Officer,  phone 355-8613, is responsible
for waste logging, acceptance for storage, and periodic shipments as
required by policies and procedures.

4.6.7. Waste Accumulation Limits

    4.6.7.1. As a small quantity generator, the laboratory is subject
    to the following waste accumulation limits:
        4.6.7.1.1. Hazardous waste

            4.6.7.1.1.1. Generate no more than 1000 kg/mo and
            accumulate no greater than 6000 kg of wastes.  Wastes must
            be disposed of within 180 days of the start of
            accumulation, or within 270 days if waste is transported
            more than 200 miles for disposal.

            4.6.7.1.1.2. Wastes generated in excess of these limits
            subjects the laboratory to the full generator rules (40
            CFR 262.34  (a)).

        4.6.7.1.2. Acutely Hazardous Waste

            4.6.7.1.2.1. Those wastes specifically listed in 40 CFR
            261.31 and 261.33 (e)(f) are considered acute hazardous
            waste.  The laboratory cannot generate more than 1 kg/mo
            of acute hazardous waste and retain its'  small quantity
            generator status.  The 180/270-day storage limit also
            applies to acutely hazardous wastes if less than 1 kg/mo
            is generated.

        4.6.7.1.3. Waste accumulation will be monitored to ensure that
        the applicable generation and accumulation (i.e.,
        quantity/time) limits are not exceeded.  Waste will be
        disposed of as required to ensure conformance with the
        regulatory limits (i.e.,  180 days) and at a minimum of twice
        per year.
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                                            Section 4
                                            Revision: 1
                                            Date: December 1,  1997
                                            Page 5
4.6.8. Waste Packaging and Labeling

    4.6.8.1. All hazardous wastes designated for temporary storage
    must be packaged in an appropriate container designed to avoid
    loss or spillage of the materials.  The determination of the
    hazardous nature of a waste is the responsibility of the SHEM
    Officer.

    4.6.8.2. Before transporting or offering a hazardous waste for
    storage the SHEM Officer must be consulted.  The SHEM Officer will
    ensure that all containers shipped off-site are properly packaged
    and labeled and that the transport vehicle is appropriately
    placarded and manifest documentation is complete.

4.6.9. Waste Storage

    4.6.9.1. Except for in-laboratory accumulation (i.e., satellite
    storage (40 CFR 262.34 (c)(1)), all hazardous wastes generated at
    the Region 4, College Station Road facility and accumulated for
    disposal will be stored in the Hazardous Materials (HAZMAT)
    Storage Facility .   The HAZMAT facility is located adjacent to and
    detached from the main SESD building.  The building is
    specifically designed for the storage of hazardous materials.

    4.6.9.2. Materials stored in the HAZMAT are segregated according
    to compatibility groups.
    4.6.9.3. The HAZMAT storage facility will be inspected on a weekly
    basis as required 40 CFR 265.15. These inspections and the
    required documentation thereof are the responsibility of the
    Divisional SHEM Officer.

    4.6.9.4. Inspection of emergency equipment and spill control
    equipment will be conducted at appropriate intervals by the SHEM
    Officer.

    4.6.9.5. Additional housekeeping and security inspections of the
    HAZMAT facility will be performed on a regular basis in
    conjunction with safety inspections conducted by the SESD Health
    and Safety Committee.  An inspection report will be provided to
    the SHEMP Officer and to Divisional Senior Management.

    4.6.9.6. Hazardous waste generated at EPA's leased space at the US
    Department of Agriculture, Russell Reasearch Laboratory will be
    stored in the SESD HAZMAT Facility.  This is appropriate due to
    the close proximity of the locations of the two laboratories.

4.6.10. Waste Disposal

    4.6.10.1.  Disposal of regulated laboratory wastes is the
    culmination of the waste management process.  As such, selection
    of a responsible waste transporter and disposal facility is
    vitally important.   The selection of a waste transporter must be
    predicated on their being permitted to transport hazardous wastes
    coupled with an absence of prior RCRA/DOT violations and a proven
    record of successful performance.

    4.6.10.2.  The method of waste disposal will, in part, dictate the
    selection of a waste disposal facility.  To the extent possible,
    it will be the policy of Region 4 to dispose of all hazardous
    wastes by incineration, and/or chemical treatment/fixation.
    Landfilling of hazardous wastes will be avoided if at all
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                                                Section 4
                                                Revision: 1
                                                Date: December 1,  1997
                                                Page 6

        possible.  Factors considered in the selection of a waste  disposal
        facility include:  current permit status,  compliance with  the EPA
        Off-Site Policy,  (SARA Sec. 121), past performance, effectiveness
        of treatment processes and ability to provide a certificate of
        disposal.  To the extent possible, all hazardous waste will be
        disposed of at facilities which comply with the EPA off-site
        policy.

        4.6.10.3. Non-regulated solid wastes will  be disposed of in the
        building dumpster.   Non-regulated aqueous  wastes will be flushed
        to the sewer system.  See Section 3.5.42.4.2 for proper disposal.
          Spent sample containers disposed of in the dumpster should have
        their labels removed or obliterated.

    4.6.11. Recordkeeping

        4.6.11.1. All records related to the generation and disposal of
        hazardous wastes  will be retained as permanent facility records.

        4.6.11.2. These records will be maintained in the files of the
        Divisional SHEM Officer.

    4.6.12. Contingency Measures

        4.6.12.1. As required by 40 CFR 265.50 - 265.56, a Hazardous Waste
        Contingency Plan  has been developed which  outlines facility
        emergency response procedures.

4.7. Procedures for Satellite Hazardous Waste Accumulation

    4.7.1. Many laboratory operations necessitate  the generation of
    hazardous wastes (e.g., solvents, acids, etc.)  which are routinely
    accumulated near the  point of generation.  The in-laboratory
    "satellite" accumulation of such waste should  be carefully controlled
    by the laboratory manager working with the SHEM Officer so as  to avoid
    creating an unsafe situation and also comply with RCRA temporary
    storage requirements.

    4.7.2. The RCRA regulations (40 CFR 262.34(c)(1)) permit the temporary
    accumulation of hazardous waste or acutely hazardous wastes at or near
    the point of generation.  Waste accumulated in this manner are
    considered to be in "satellite accumulation."

    4.7.3. Hazardous Wastes.  The following procedures apply to satellite
    accumulation of hazardous waste in ASB facilities:

        4.7.3.1. All waste containers must be clearly marked with  a red
        "Hazardous Waste" label.  These labels are available from  the SHEM
        Officer, Jim Gray,  at 355-8613.

            4.7.3.1.1.  The contents of the container must be marked on the
            label.  Be specific in the identification of the contents.

            4.7.3.1.2.  All satellite storage containers must be closed
            except during periods of waste transfer.  Some operations
            (e.g., AA,  LC,  ICP, etc.) may require  using a container lid
            with a hole for introducing the waste  via a tube.  Waste
            collection vessels requiring zero back pressure can be fitted
            with an open-to-the-air absorbent trap  (e.g., carbon filled).
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                                                Section 4
                                                Revision: 1
                                                Date: December 1,  1997
                                                Page 7

            4.7.3.1.3. The volume of waste accumulated in the laboratory
            should not exceed 8 gallons.  Exceptions would be instrument
            (i.e., AA, ICP)  waste acid reservoirs and TCLP process waste.

            4.7.3.1.4. Volatile and/or flammable wastes should be
            temporarily stored in laboratory fume hoods nearest the point
            of generation.

            4.7.3.1.5. Caution must be exercised by the analysts to avoid
            creating incompatible and/or reactive waste mixtures.

            4.7.3.1.6. Waste removed from "satellite" storage for disposal
            will be handled according to the procedures contained in the
            Safety, Health and Environmental Management Program,
            Procedures and Policies Manual.

        4.7.3.2. All satellite accumalation containers must be placed in
        secondary containment.

    4.7.4. Acutely Hazardous Wastes

        4.7.4.1. Acutely hazardous wastes are those listed in 40 CFR
        261.31-261.33 and must be accounted for separately from non-acute
        wastes.  The following procedures apply to the satellite storage
        of acutely hazardous wastes:

            4.7.4.1.1. The acute waste must be collected in separate
            containers from the non-acute hazardous waste and be labeled
            as containing acute waste.

            4.7.4.1.2. Accumulation of acute waste cannot exceed one (1)
            quart and remain in the laboratory.  Once the volume reaches
            one quart, the waste container must be dated and removed to
            the permanent hazardous waste storage area within three (3)
            days.

            4.7.4.1.3. Except for the labeling and accumulation limits,
            acute wastes will be handled in the same manner as hazardous
            wastes.

        4.7.4.2. Laboratory managers and supervisors should conduct
        periodic walk-through inspections to ensure the proper application
        of temporary waste accumulation procedures.

4.8. Guidelines for Disposal of Environmental Samples

    4.8.1. Samples submitted to the laboratory for analysis are excluded
    from regulation as hazardous waste under 40 CFR 261.4(d)  provided the
    samples are being transported to or from the laboratory,  or are being
    analyzed,  are being held for analysis, are being maintained in custody
    for legal  reasons.  However, once a decision is made to dispose of
    laboratory samples, the exclusion provisions of 40 CFR 261.4(d)  no
    longer apply.  Depending upon the characteristics and/or contents of
    such samples, they may be subject to regulation as a hazardous waste
    under RCRA or as a PCB-containing material under TSCA and must be
    handled accordingly.

    4.8.2. Not all samples are routinely subjected to characteristic
    testing and are not readily classified as a hazardous waste.  To
    address the problem of proper sample handling and disposal in the
    laboratory, guidelines have been developed to aid laboratory and
    environmental compliance personnel in making a decision whether or not
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                                                Section 4
                                                Revision: 1
                                                Date: December 1, 1997
                                                Page 8

    to handle a particular spent laboratory sample as either a RCRA
    regulated or non-regulated waste containing potentially hazardous/
    toxic substances or simply a solid waste.  Application of these
    guidelines provides an environmentally conservative approach to the
    disposal of spent laboratory samples and minimizes the potential for
    non-compliance with RCRA regulations.
    4.8.3. At the completion of each project, the laboratory generates a
    report from its laboratory information management system which
    describes each analysis performed on the individual samples together
    with a parameter by parameter listing of positive results.  The
    computer program has been designed to deliver a list of samples that
    are potentially hazardous as defined by statute. Samples that are
    indicated by the computer program as potentially hazardous are
    referred to the Divisional SHEM Officer who then makes the decision as
    to the proper disposition of the samples.

    4.8.4. Acidified water samples are subject to elementary
    neutralization and would be classified as "hazardous" solely upon the
    basis of pH.  See Section 3.5 for proper disposal.  This method of
    disposal is applicable to all water samples which are classified as a
    hazardous waste exclusively on the basis of corrosivity.

    4.8.5. All non-acidified water samples are disposed of via the
    laboratory sinks.

    4.8.6. All samples containing total PCB's greater than 50 mg/kg  are
    subject to TSCA provisions contained in 40 CFR 761 and are disposed of
    as PCB containing materials.

            4.8.6.0.1. Disposal of Foreign Soil- See Section 3.7

4.9. Handling, Storage, Disposal and Reporting Procedures for PCB
Containing Materials

    4.9.1. The handling, storage, disposal and reporting of PCB items,
    containers, and articles containing PCB's in concentrations greater
    than 50 ppm are regulated under the Toxic Substances Control Act
    (TSCA).  Applicable regulations are contained in 40 CFR Part 761.1.

    4.9.2. REGULATORY REQUIREMENTS

        4.9.2.1. Marking Requirements:  Any PCB article or container (40
        CFR 761.3) of PCB materials in a concentration greater than 50 ppm
        must be properly marked according to 40 CFR 761.40.

        4.9.2.2. Storage Requirements:  Any PCB containing material (i.e.,
        item, article, etc.) designated for disposal shall be  disposed of
        within 1 year from the date it was first placed in storage  (40 CFR
        761.65  (a).

    4.9.3. The storage facility shall comply with the requirements
    specified in 40 CFR 761.65  (b) (1) (e.g., roof, walls,  floor, curbing,
    location, marking, inspection, etc.).

        4.9.3.1. Temporary Storage:  PCB wastes stored in laboratories are
        considered to be in temporary storage as described in 40 CFR
        761.65  (c) without having to comply with the storage requirements
        provided that:  (1)  the wastes container displays a proper PCB
        label,  (2) contains the date accumulation started,   (3) are stored
        in a DOT specification container as described in 40 CFR 761.65
        (c)(6), and  (4) are not stored in the laboratory for more than 30
        days.
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                                        Section 4
                                        Revision: 1
                                        Date: December 1, 1997
                                        Page 9
4.9.3.2. Reporting and Records:  If at any time the facility
stores 45 kg (99.4 pounds) of PCB material with a concentration
greater than 50 ppm, the following information will be compiled in
an annual report:  volume of PCB's stored, storage dates,
disposal dates, and PCB source (40 CFR 761.180(a)).  An Annual
Report will prepared by the Divisional SHEM Officer.

4.9.3.3. Disposal Requirements:  Destruction of PCB containing
materials must be done in an incinerator which complies with the
requirements contained in 40 CFR 761.70.
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                                                    Section 5
                                                    Revision:  0
                                                    Date:  August 1990
                                                    Page 1
5. LABORATORY EQUIPMENT MAINTENANCE AND SERVICE

    5.1. Proper maintenance of laboratory instrumentation is a key ingredient
    to both the longevity of the instrumentation, as well as,  providing the
    analyst with equipment capable of producing reliable analyses.  Proper
    equipment maintenance requires an alert analytical staff which recognizes
    the need for equipment maintenance coupled with available support services
    provided either by in-house personnel or vendor specialists.

    5.2. Responsibility for maintenance and repair of all Branch laboratory
    equipment is shared by the analysts and on occasion, vendor specialists.

    5.3. The primary elements of the equipment maintenance program include:

        5.3.1. All major equipment receives a daily check for such things as:
        cooling fan operation, pump operation, indicator readings, mechanical
        checks, clean air filters, etc.

        5.3.2. Service schedules are established for performing routine
        preventative maintenance on all major equipment items.

        5.3.3. Records are maintained for all equipment repairs.

        5.3.4. Instrument utilization records; including operating, and
        downtime,  are maintained for all GC, AA, GC/MS and ICAP instruments.

        5.3.5. A conservative inventory of critical spare parts is maintained
        for high-use instrumentation.

        5.3.6. Vendor operation and maintenance manuals are maintained for all
        laboratory instrumentation.
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                                                    Section 6
                                                    Revision:  0
                                                    Date:   August 1990
                                                    Page 1
6.  LABORATORY SAFETY

    6.1.  INTRODUCTION

        6.1.1.  All Branch employees must accept the responsibility for acting
        in accordance with safety rules and practices and for reporting any
        observed safety hazard.   This section highlights some general
        guidelines and rules that specifically apply to the Analytical Support
        Branch.  Obviously no set of rules will cover all possible situations.
         Therefore,  in addition to adhering to these rules, each person is
        expected to exercise good judgement in all situations and to maintain
        a high level of safety consciousness.

        6.1.2.  The rules and guidelines listed in this section only supplement
        or highlight the following official publications:

            6.1.2.1. Safety and Health Manual, draft (proposed effective Feb
            1998) .

            6.1.2.2. EPA Occupational Health and Safety Manual,  October 1984.

            6.1.2.3. Laboratory Health Monitoring Requirements,  March 6, 1987.

    6.2.  General

        6.2.1.  Lab coats and safety glasses should be worn at all times in
        laboratories.  The only exception to this is when personnel are
        working at computer terminals or microscopes.  When working with
        corrosives and/or toxic substances, lab coats should be  left in the
        laboratory.

        6.2.2.  Open sandals and shorts will not be worn in laboratories.

        6.2.3.  When working in any of the laboratories, it is recommended that
        all jewelry be removed and that personnel wash their hands frequently.
        Always wash hands thoroughly when leaving the laboratory.

        6.2.4.  When working with flammable materials, nylon or other totally
        synthetic clothing should be avoided to minimize the possibility of
        static sparks.

        6.2.5.  All containers should be labeled as to contents,  with
        particular care to note corrosive or hazardous materials.

        6.2.6.  There will be no eating, drinking, or smoking in  any
        laboratory.

        6.2.7.  Glassware that is chipped but still usable, must  be fire
        polished before use; otherwise it must be discarded.

        6.2.8.  Never use any lab glassware as a container for food or drink.

        6.2.9.  An inventory of all chemicals maintained in the laboratory will
        be prepared and updated on an annual basis.

        6.2.10. Return all chemicals to their proper storage areas after use.

        6.2.11. Never pipet by mouth.
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                                                Section:   6
                                                Revision:  1
                                                Date:  December 1,  1997
                                                Page:   2


    6.2.12.  Designated personnel are to conduct a safety  inspection of
    their laboratory at least quarterly.

    6.2.13.  No perchloric acid or perchlorate salts will  be stored in the
    Analytical Support Branch.  If at any time these chemicals are
    required in a method, special precautions will be  necessary and should
    be coordinated with the Chief of the  Inorganic Chemistry or Organic
    Chemistry Section.

    6.2.14.  All work areas should be cleaned at the end of each work day.
    Spills should be cleaned up immediately.

    6.2.15.  Samples should be in laboratories only during preparation and
    analysis; otherwise,  keep them in the custody room, or proper  volatile
    organic  storage area.

    6.2.16.  All stock standards of a toxic nature should  be prepared in a
    hood and stored in designated areas.   Only experienced personnel
    should handle these standards.

    6.2.17.  Work of a hazardous nature will not be performed in a
    laboratory after normal business hours when only one  person is
    present.

    6.2.18.  New personnel must be familiarized with safety practices,
    location of safety equipment, and made aware of possible hazards in
    the areas in which they will be working.

    6.2.19.  When conducting routine maintenance of electrical equipment,
    observe  all shock hazard warnings displayed on instrumentation.

    6.2.20.  Use safety guards where appropriate when using electrical
    equipment or ventilation/fumehood systems.

    6.2.21.  Observe all cryoprotective warnings regarding cylinders and
    sample storage areas.

    6.2.22.  When using pressurized systems, take care  to  tighten
    restraints before pressurizing system and depressurize system  before
    loosening restraints.

6.3. Sample  Receiving and Logging

    6.3.1. When possible, determine the source of the  samples and  any
    special  hazards that  might be associated with them.  (Refer also to
    Section  3, Laboratory Chain-o£-Custody and Sample  Handling.)

    6.3.2. Some samples,  especially domestic waste when sealed in
    containers will build up pressure.  Care should be taken in handling
    these type samples.  Also, gloves should be used to handle these
    samples  during analysis, due to the possibility of the transmission of
    a variety of human enteric pathogens  that cause diseases.

    6.3.3. Broken samples should be handled with protective gloves and
    disposed of immediately according to  the waste disposal procedures.

    6.3.4. A small percentage of samples  received by ASB  would be
    characterized as concentrated waste.   These samples will require
    special  handling.  (Refer to Section  3.5.6.2 for Handling Procedures.)
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                                                Section:  6
                                                Revision: 1
                                                Date: December 1,  1997
                                                Page:  3
6.4.  Compressed Gases

    6.4.1.  Compressed gases should be handled in accordance with Chapter 3
    of the  Safety and Health Manual,  Science and Ecosystems Support
    Division.

    6.4.2.  It  is the responsibility of each Team to maintain current
    inventory  and status of compressed gases used within their respective
    areas.   Each Section Chief and/or Team must designate individuals to
    perform these inventories.

6.5.  Radioactivity

    6.5.1.  Electron Capture Detectors require wipe tests for radioactivity
    every six  months.

    6.5.2.  The Divisional SHEM Officer will be the person responsible for
    the wipe tests and to maintain documentation of the tests.

6.6.  Laboratory Waste Disposal Practices

    6.6.1.  ASB is subject to the Resource Conservation and Recovery Act
    (RCRA)  regulations as contained in the Georgia Rules for Hazardous
    Waste Managment for handling,  storage, and disposal of laboratory
    related wastes.  While knowledge of the hazardous waste handling and
    disposal regulations is the primary responsiblity of the Divisional
    SHEM Officer, each ASB staff member should become familiar with the
    basic policies and procedures for waste disposal as it pertains to
    his/her area.  ALL WASTE DISPOSAL MUST BE COORDINATED WITH THE SHEM
    OFFICER.  (Refer also to Section 4.6)
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                                                    Section 7
                                                    Revision:  0
                                                    Date: August 1990
                                                    Page 1
7.  METHODOLOGY

    7.1. A detailed listing and discussion of specific chemical methods  are
    not included in this manual.  Instead, lists containing the methods  (and
    analytical technique) used in this laboratory for organic analysis of  all
    sample types are listed in Table 7-1.  Table 7-1 contains the  method
    tracking number and method summary.  The method tracking number  is listed
    in extraction logbooks to identify the organic methods of extraction and
    analysis. (See Table 7-2.)  See Section 11 for references to inorganic
    methods.

    7.2. Details on the applications, limitations, precision, and accuracy are
    found within the listed methods.

    7.3. Reporting Units

        7.3.1. Table 7-3 lists the reporting concentration units for all
        parameters in waters, soil/sediments  (solids), fish  (tissue), air, and
        waste.  These units are always to be used unless sample matrix or
        methodology criteria require a change.  Changes in units must be
        coordinated between the Organic and Inorganic Chemistry Sections.
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                                                                 Section: 7
                                                                 Revision: 1
                                                                 Date: December 1, 1997
                                                                 Page: 2
   Method
Parameter
                   Method
                                           TABLE 7-1
                                  LIST OF TEST PROCEDURES
         Reference    Tracker #
                            Surface Water. Monitoring Wells. Wastewater

1.  Extractable Organics Capillary GC/MS          8270/625/CLP  47A

2.  Volatile Organics    Capillary GC/MS          8260/624/CLP  46A

                          Capillary GC/ECD
3.  Organochlorine
  Pesticides/PCBs

4.  Acid Herbicides
                        8081/608/CLP  55A,55


Capillary GC/ECD         8151/515.1    38A

                   8141       57
5.  Organophosphorus   Capillary GC/NPD
  Pesticides
6.  Formaldehyde       Capillary GC/MS          ASB Method   48A,48
              HPLC         FORM-10/83/8315
1.  Extractable Organics Capillary GC/MS

2.  Volatile Organics    Capillary GC/MS
3.  Organochlorine
  Pesticides/PCBs

4.  Acid Herbicides

5.  EDBandDBCP
                          Capillary GC/ECD


                          Capillary GC/ECD

                          Capillary GC/ECD
               Drinking Water

                525/8270     47A

                   524.2/8260    46A

                        508/8081     55A55
6.  Screening for PCBs  Capillary GC/ECD
                        515.1/8151    38A

                        504       52A

                   508A       62
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                                                                Section: 7
                                                                Revision: 1
                                                                Date: December 1, 1997
                                                                Page: 3
Parameter
                   Method
              TABLE 7-1 (cont.)

        LIST OF TEST PROCEDURES

        Reference    TRACKER #
                                                                    METHOD
1.  Extractable Organics Capillary GC/MS

2.  Volatile Organics    Capillary GC/MS

                          Capillary GC/ECD
                                        SEDIMENT/SOIL

                                             3550/8270/CLP  43,43A,54

                                             8260/CLP     43D,54B
3.  Organochlorine
  Pesticides/PCBs

4.  Acid Herbicides
                        3550/8080/CLP  43,43A,43B,
                                     43Q54
5.  Organophosphorus   Capillary GC/NPD
  Pesticides
Capillary GC/ECD         8151

                   3550/8141
                                                            51A
                                                         57
6.  Formaldehyde       Capillary GC/MS          ASB Method    48A,48
              HPLC         FORM-10/83/8315
7.  PCBSforTSCA
                          Capillary GC/ECD
1.  Extractable Organics Capillary GC/MS

2.  Volatile Organics    Capillary GC/MS

                          Capillary GC/ECD
3.  Organochlorine
  Pesticides/PCBs

4.  Acid Herbicides
                          Capillary GC/ECD
5.  PCBs in Waste Oil   Capillary GC/ECD
1.  Extractable Organics Capillary GC/MS
                         8270

2.  Volatile Organics    Capillary GC/MS
3.  Organochlorine
  Pesticides/PCBs
                          Capillary GC/ECD
                               8080
                        3540/8080     31A

                   WASTE

                   3580/8270     54A
                                  3550/8270    54C
                   8260       54B

                        3580/8080     54A
                             3550/8080    54C

                        8151       51A

                   600/4-81-045  35
                        8080

                   TISSUE

                   ASB Sonicator  44


                   ASB Method/8260 44

                        ASB Sonicator  44
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                                                               Section: 7
                                                               Revision: 1
                                                               Date: December 1, 1997
                                                               Page: 4
                                       TABLE 7-1 (cont.)

                                 LIST OF TEST PROCEDURES
                                                                  METHOD
Parameter	Method	Reference   TRACKER #

                                             AIR

1. Extractable Organics  Capillary GC/MS        PUFbyTOlS    50C
                                                    8270

2. Volatile Organics   Capillary GC/MS         Canister by   56
                                                    TO 14/8260

3. Organochlorine          Capillary GC/ECD        PUFbyTO4    50
  Pesticides/PCBs                                   8080

4. Formaldehyde      HPLC                    TrapbyTOll   59
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                                                                 Section: 7
                                                                 Revision: 1
                                                                 Date: December 1, 1997
                                                                 Page: 5
Method*        Descriptor      Sample Type

46 A           VLW     Volatile low water
43D           VLS      Volatile low soil/sed
54B           VMS      Volatile medium soil/sed
54B           VMW          Volatile medium waste
56             VAC      Volatile air canister
60       VTC   VOLATILE BY TCLP EXTRACTION

47             SLW      Semivolatile low water - separately funnel
47A           SLW      Semivolatile low water - continuous liquid ext.
43             SLG      Semivolatile low soil/sed w/GPC
43 A           SLS       Semivolatile low soil/sed wo/GPC
54             SMS      Semivolatile medium soil/sed
54A           SHW     Semivolatile high waste wo/son.
54C           SMW     Semivolatile medium waste w/son.
44             SLT      Semivolatile low tissue
SOB           SAP      Semivolatile air PUF
58             SCW      Semivolatile Cartridge ext. water
60             STC      Semivolatiles by TCLP extraction
31C    SSS   SEMIVOLATILE LOW SOIL WITH SOXHLET
55
55A
43
43A
43B
43C
44
44A
44B
SOB
54
54A
54C
52B
57
60
35
31A
31C
38
51
60
48
48
59
61
61
PLW
PLW
PLG
PLS
PSA
PSH
PLT
PTH
PTA
PAP
PMS
PHW
PMW
PCW
PNP
PTC
PWO
PCS PCB LOW
PSS PEST/PCB
HLW
HLS
HTC
FLW
FLS
FAC
CLW
CLS
Pesticide low water - separatory funnel
Pesticide low water - continuous liquid ext.
Pesticide low soil/sed w/GPC
Pesticide low soil/sed wo/GPC
Pesticide low soil/sed w/acid cleanup
Pesticide low soil/sed w/hex/acetone
Pesticide low tissue
Pesticide low tissue w/hexane
Pesticide low tissue w/acid cleanup
Pesticide air PUF
Pesticide medium soil/sed
Pesticide high waste wo/son.
Pesticide medium waste w/son.
Pesticide Cartridge ext. water
Pesticide low water nitrogen/phosphorous
Pesticides by TCLP extraction
PCBs waste oil
SOIL WITH SOXHLET
LOW SOIL WITH SOXHLET
Herbicides low water
Herbicides low soil/sed
Herbicides by TCLP extraction
Formaldehyde low water
Formaldehyde low soil/sed
Formaldehyde air cartridge
Carbamates low water w/HPLC
Carbamates low soil/sed w/HPLC
                                           Table 7-2
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                                                                  Section:  7
                                                                  Revision: 1
                                                                  Date: December 1, 1997
                                                                  Page:  6

                            METHOD SOURCES FOR TABLES 7-1 & 7-2

1.  1000-8000 Methods: USEPA, Test Methods for Evaluating Solid Waste. SW-846, 3rd Edition, 1986 plus the 1st
and 2nd Updates.

2.  500 Methods: USEPA, Methods for the Determination of Organic Compounds in Drinking Water. EPA/600/4-
88/039, Dec., 1988.

3.  600 Methods: USEPA. Guidelines Establishing Test Procedures for the Analysis of Pollutants Under the Clean
Water Act-40CFR Part 136. Federal Register of Oct. 26, 1984.

4.  TO Methods: USEPA, Compendium of Methods for the Determination of Toxic Organic Compounds in Ambient
Air. EPA-600/4-84-041, Apr. 1984 plus the Supplements of 1986 and 1988.

5.  CLP Methods: USEPA Contract Laboratory Program Statement of Work for Organics Analysis. Multi-Media.
Multi-Concentration. 1990.

6.  USFDA Methods: Pesticide Analytical Manual. Volumes I and II.

7.  Region 4 Methods: Adaptations of Published Methods when Official Methods are not Available.
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 7
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS   UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE WASTE    AIR
7736
4045
9999
1046
1028
5215
5205
5206
6105
6100
6716
4055
7051
3005
7015
7020
5867
5793
5794
5795
5005
3008
3009
3010
2125
5884
1008
5830
5791
3015
3016
3018
6160
2065
5878
5115
5095
5100
5085
5105
% ALCOHOL
% LIPIDS
% MOISTURE
% SOLIDS
% WATER
2,4,5-T
2,4-D
2,4-DB
ACENAPHTHENE
ACENAPHTHYLENE
ACETALDEHYDE
ACETATE
ACETONE
ACIDITY
ACROLEIN
ACRYLONITRILE
ALACHLOR (LASSO)
ALDICARB
ALDICARB SULFONE
ALDICARB SULFOXIDE
ALDRIN
ALKALINITY, BICARBONATE (AS CAC03 )
ALKALINITY, CARBONATE (AS CAC03 )
ALKALINITY, TOTAL (AS CAC03 )
ALUMINUM
AMBUSH (PERMETHRIN)
AMES TEST
AMETRYN
AMINOBENZIMIDAZOLE, 2- (2-AB)
AMMONIA
AMMONIA, DISSOLVED
AMMONIA, UNIONIZED (AS NH3 )
ANTHRACENE
ANTIMONY
ANTOR
AROCLOR 1016 (PCB-1016)
AROCLOR 1221 (PCB-1221)
AROCLOR 1232 (PCB-1232)
AROCLOR 1242 (PCB-1242)
AROCLOR 1248 (PCB-1248)
%


%
%
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
MG/L
UG/L
MG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
MG/L
MG/L
MG/L
UG/L
UG/L

UG/L
UG/L
MG/L
MG/L
MG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
%

%
%
%
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG
UG/KG
MG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG


MG/KG
MG/KG
UG/KG

UG/KG
UG/KG
MG/KG


UG/KG
MG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
%

%

%
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG


MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG


MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
%

%

%
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG


MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG


MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
UG/M3







UG/M3
UG/M3


UG/M3

UG/M3
UG/M3
















UG/M3







                                            Table 7-3
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 8
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS   UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE  WASTE    AIR
5090
5110
5111
5112
5895
2010
1005
1007
1006
5861
5781
1010
5894
2020
5789
5868
7105
6020
6190
6215
6210
6211
6235
6216
6220
6256
6795
6770
6241
6180
6765
2025
5020
5025
5035
5030
3012
6080
6040
6050
AROCLOR 1254 (PCB-1254)
AROCLOR 1260 (PCB-1260)
AROCLOR 1262 (PCB-1262)
AROCLOR 1268 (PCB-1268)
AROCLORS, TOTAL (PCBS)
ARSENIC
ASBESTOS (FIBROUS)
ASBESTOS, BULKED
ASH
ATRAZINE
AZODRIN (MONOCROTOPHOS)
BAC-T
BALAN (BENEFIN)
BARIUM
BENOMYL
BENOMYL (BENLATE)
BENZENE
BENZIDINE
BENZO (A) ANTHRACENE
BENZO(B AND/OR K) FLUORANTHENE
BENZO (B AND/OR K) FLUORANTHENE *
BENZO (B) FLUORANTHENE
BENZO (GHI) PERYLENE
BENZO (K) FLUORANTHENE
BENZO-A-PYRENE
BENZOIC ACID
BENZONITRILE
BENZOPHENONE
BENZYL ALCOHOL
BENZYL BUTYL PHTHALATE
BENZYLIC ACID
BERYLLIUM
BHC, ALPHA -
BHC, BETA-
BHC, DELTA -
BHC, GAMMA- (LINDANE)
BICARBONATE (AS HC03 ION)
BI S ( 2 - CHLOROETHOXY) METHANE
BIS(2-CHLOROETHYL) ETHER
BIS (2-CHLOROISOPROPYL) ETHER
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
F/L


UG/L
UG/L

UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
MG/L
UG/L
UG/L
UG/L
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG
UG/KG

%
UG/KG
UG/KG

UG/KG
MG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG
UG/KG
UG/KG
UG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG


MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
%
%
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
















UG/M3

UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3


UG/M3
UG/M3







UG/M3
UG/M3
UG/M3
                                            Table 7-3
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 9
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS   UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE  WASTE    AIR
6805
6185
2705
4004
4007
4005
4009
4006
4008
5885
2015
5862
2727
3017
7131
6810
7059
7085
7130
7030
6150
7737
5902
5801
7907
7905
7903
6173
6713
2030
2135
2136
5782
6295
5790
5904
7052
7080
4038
4037
BIS (2-ETHYLHEXYL) ADIPATE
BIS(2-ETHYLHEXYL) PHTHALATE
BISMUTH
BOD (LONG TERM)
BOD, 20 DAY
BOD, 5 DAY
BOD, 5 DAY (CARBONACEOUS)
BOD, 5 DAY (DISSOLVED)
BOD, 60 DAY
BOLSTAR (SULPROFOS)
BORON
BROMACIL
BROMATE
BROMIDE
BROMOBENZENE
BROMOCHLOROACETONITRILE
BROMOCHLOROMETHANE
BROMODICHLOROMETHANE
BROMOFORM
BROMOMETHANE
BROMOPHENYL PHENYL ETHER, 4-
BTEX
BUTACHLOR
BUTYLATE
BUTYLBENZENE, N-
BUTYLBENZENE, SEC-
BUTYLBENZENE, TERT-
BUTYLISOCYANATE, N- (BIG)
BUTYLISOCYANATE, N- (BIG)
CADMIUM
CALCIUM*
CALCIUM (LOW LEVEL)
CAPTAN
CARBAZOLE
CARBENDAZIM (MBC)
CARBOFURAN
CARBON DISULFIDE
CARBON TETRACHLORIDE
CARBON, PARTI CULATE ORGANIC
CARBON, PURGEABLE ORGANIC
UG/L
UG/L
UG/L
MG/L
MG/L
MG/L
MG/L
MG/L
MG/L
UG/L
UG/L
UG/L
UG/L
MG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
MG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
MG/L
MG/L
UG/KG
UG/KG
MG/KG






UG/KG
MG/KG
UG/KG
UG/KG

UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG
MG/KG
MG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/L

MG/KG
MG/KG
MG/KG






MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG


MG/KG
MG/KG
MG/KG






MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG



UG/M3












UG/M3

UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3


UG/M3
UG/M3
UG/M3
UG/M3





UG/M3


UG/M3
UG/M3


                                            Table 7-3
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 10
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS   UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE WASTE    AIR
3022
4035
4036
3013
5871
1076
2715
4010
4011
5787
2728
5080
5165
5155
5135
5140
5142
5145
5824
3020
3021
8005
2729
6270
6076
6803
7150
5880
5874
7040
7125
7065
7025
6095
6240
6760
6125
1082
1083
1081
CARBON , TOTAL
CARBON, TOTAL ORGANIC
CARBON, TOTAL ORGANIC (DISSOLVED)
CARBONATE (AS C03 ION)
CARBOPHENOTHION (TRITHION)
CATION EXCHANGE CAPACITY (CEC)
CERIUM
CHEMICAL OXYGEN DEMAND
CHEMICAL OXYGEN DEMAND, DISSOLVED
CHLORAMBEN (AMIBEN)
CHLORATE
CHLORDANE (TECH. MIXTURE) /I
CHLORDANE, ALPHA- /2
CHLORDANE, GAMMA- /2
CHLORDENE/2
CHLORDENE, ALPHA- /2
CHLORDENE, BETA- /2
CHLORDENE, GAMMA- /2
CHLORDIMEFORM
CHLORIDE
CHLORINE
CHLORINE, RESIDUAL
CHLORITE
CHLORO-3-METHYLPHENOL, 4-
CHLOROANILINE, 4-
CHLOROBENZALDEHYDE, 0-
CHLOROBENZENE
CHLOROBENZILATE
CHLOROBENZILATE *
CHLOROETHANE
CHLOROETHYLVINYL ETHER, 2-
CHLOROFORM
CHLOROMETHANE
CHLORONAPHTHALENE , 2 -
CHLOROPHENOL, 2-
CHLOROPHENOL, 4-
CHLOROPHENYL PHENYL ETHER, 4-
CHLOROPHYLL A (FLUORIMETER)
CHLOROPHYLL A (HPLC)
CHLOROPHYLL A (UV/VIS)

MG/L
MG/L
MG/L
UG/L
UG/L
UG/L
MG/L
MG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
MG/L

MG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
MG/KG
MG/KG

MG/KG
UG/KG
MQ/KG
MG/KG
MG/KG

UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG


UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG

MG/KG


MG/KG
MG/KG
MG/KG


MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG



MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
%
MG/KG


MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
%

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG























UG/M3
UG/M3

UG/M3


UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3

UG/M3



                                            Table 7-3
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 11
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS  UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE WASTE    AIR
5869
5792
7185
7180
7190
2040
2155
6195
2035
1090
1085
1100
1095
1018
1016
1015
1014
1020
2045
1025
1026
5863
3025
3026
3038
3039
3027
3028
3037
5803
5886
5783
5785
5858
5060
5857
5055
5856
5050
5859
CHLOROTHALONIL
CHLOROTHALONIL *
CHLOROTOLUENE, M-
CHLOROTOLUENE, 0-
CHLOROTOLUENE, P-
CHROMIUM
CHROMIUM, HEXAVALENT
CHRYSENE
COBALT
COLIFORM, FECAL MF/100ML
COLIFORM, FECAL MPN/100ML
COLIFORM, TOTAL MF/100ML
COLIFORM, TOTAL MPN/100ML
COLOR (ADMI @ ORIG. SMPL . PH)
COLOR (ADMI @ PH 7.6)
COLOR (APPARENT- PTCO)
COLOR (TRUE -PTCO)
CONDUCTIVITY
COPPER
CORROSIVITY (PH)
CORROSIVITY (STEEL)
CYANAZINE
CYANIDE*
CYANIDE (LOW LEVEL)
CYANIDE MICRODIFFUSION/METHOD 4282
CYANIDE WEAK DISSOCIABLE/METHOD 4500
CYANIDE, AMENABLE TO CHLORINATION
CYANIDE, FREE
CYANIDE, REACTIVE (AS HCN)
CYCLOATE
CYGON (DIMETHOATE)
DALAPON
DAS AN IT
ODD, 2,4'- (0,P'-DDD)
ODD, 4,4'- (P,P'-DDD)
DDE, 2,4'- (0,P'-DDE)
DDE, 4,4'- (P,P'-DDE)
DDT, 2,4'- (0,P'-DDT)
DDT, 4,4'- (P,P'-DDT)
DDT, TOTAL RESIDUES (TDDTR)
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L





ADMI
PTCO
PTCO
UMHOS
UG/L


UG/L
MG/L
UG/L
UG/L
UG/L
UG/L
UG/L

UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG
MG/KG
UG/KG
MG/KG









MG/KG

MM/YR
UG/KG
MG/KG
MG/KG
UG/KG
UG/KG
MG/KG
MG/KG
MG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG









MG/KG


MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG









MG/KG
PH
MM/YR
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG


UG/M3
UG/M3
UG/M3


UG/M3
































                                            Table 7-3
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 12
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS   UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE WASTE    AIR
5883
5839
5899
5825
5822
5819
1002
6165
6779
6205
5833
5860
6230
6111
5817
7908
5873
6811
7110
7720
7091
6772
5836
6806
6812
6035
7205
6025
7195
6030
7200
6200
5221
6714
6816
5881
7005
7055
DDVP
(2,2-DICHLOROVINYLDIETHYLPHOSPHATE)
DECACHLOROBIPHENYL (DCB)
DEBT
DBF
DELNAV (DIOXATHION)
DEMETON-S
DENSITY (20 DEC. C)
D I - N - BUTYL PHTHALATE
DI -N-BUTYLSEBACATE
DI -N-OCTYLPHTHALATE
DIALLATE
DIAZINON
DIBENZO (A, H) ANTHRACENE
DIBENZOFURAN
DIBROM (NALED)
DIBROMO-3-CHLOROPROPANE, 1,2-
DIBROMO-3-CHLOROPROPANE, 1,2- (DBCP)
DIBROMOACETONITRILE
DIBROMOCHLOROMETHANE
DIBROMOETHANE, 1,2- (EDB)
DIBROMOMETHANE
DIBUTYL TIN
DICAMBA
DICHLOROACETIC ACID
DI CHLOROACETONI TRI LE
DICHLOROBENZENE, 1,2- (EXTRACTABLE)
DICHLOROBENZENE, 1,2- (VOLATILE) *
DICHLOROBENZENE, 1,3- (EXTRACTABLE)
DICHLOROBENZENE, 1,3- (VOLATILE) *
DICHLOROBENZENE, 1,4- (EXTRACTABLE)
DICHLOROBENZENE, 1,4- (VOLATILE) *
DICHLOROBENZIDINE, 3,3'-
DI CHLOROBENZ I LATE
DICHLOROBENZOIC ACID
DICHLOROBENZOPHENONE, 4,4'-
( EXTRACTABLE) *
DICHLOROBENZOPHENONE, 4,4'-
(PESTICIDE)
DICHLORODIFLUOROMETHANE
DICHLOROETHANE, 1,1-
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
GM/ML
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG

UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
GM/ML
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG







UG/M3

UG/M3


UG/M3
UG/M3

UG/M3


UG/M3
UG/M3
UG/M3




UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3




UG/M3
UG/M3
                                            Table 7-3
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 13
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS   UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE WASTE    AIR
7070
7050
7061
7056
7060
6260
6261
5806
7090
7141
7057
6813
7076
7120
7095
5876
5045
6135
6003
5818
6110
7730
6255
6800
6275
6115
6120
5887
6775
6015
5810
1001
5842
5831
5896
5828
5889
5040
5070
DICHLOROETHANE, 1,2-
DICHLOROETHENE, 1,1-
(1, 1-DICHLOROETHYLENE)
DICHLOROETHENE, 1,2- (TOTAL)
DICHLOROETHENE, CIS- 1,2-
DICHLOROETHENE, TRANS -1,2-
DICHLOROPHENOL, 2,4-
DICHLOROPHENOL, 2,6-
DICHLOROPROP
DICHLOROPROPANE, 1,2-
DICHLOROPROPANE, 1,3-
DICHLOROPROPANE, 2,2-
DICHLOROPROPANONE, 1,1-
DICHLOROPROPENE, 1,1-
DICHLOROPROPENE, CIS- 1,3-
DICHLOROPROPENE, TRANS- 1,3-
DICOFOL (KELTHANE)
DIELDRIN
DI ETHYL PHTHALATE
DIETHYLENE GLYCOL MONOETHYL ETHER
DIMETHOATE
DIMETHYL PHTHALATE
DIMETHYLAMINE
DIMETHYLPHENOL, 2,4-
DINITROBENZENE, 1,3-
DINITROPHENOL, 2,4-
DINITROTOLUENE, 2,4-
DINITROTOLUENE, 2,6-
DINOSEB (DNBP)
DIPHENYL TIN
DIPHENYLHYDRAZINE, 1 , 2 -/AZOBENZENE
DIQUAT
DISTRIBUTION COEFFICIENT
DISULFOTHION (DISULFTON)
DISULFOTON
DISYSTON
DIURON
DURSBAN (CHLORPYRIFOS) (LORSBAN)
ENDOSULFAN I (ALPHA)
ENDOSULFAN II (BETA)
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L

UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG

UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3

UG/M3
UG/M3
UG/M3

UG/M3
UG/M3
UG/M3


UG/M3


UG/M3
UG/M3
UG/M3

UG/M3
UG/M3
UG/M3












                                            Table 7-3
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 14
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS   UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE WASTE    AIR
5075
5065
5125
5220
7725
5888
5811
5872
5843
7155
6001
4060
5854
5841
5882
1030
8015
6170
6130
3030
3031
5812
6715
1027
1048
1115
1120
5879
4051
4050
1035
1031
5010
5015
410
6784
409
424
6790
ENDOSULFAN SULFATE
ENDRIN
ENDRIN ALDEHYDE
ENDRIN KETONE
EPICHLOROHYDRIN
EPN
EPTC (EPTAM)
ETHION
ETHOPROP
ETHYL BENZENE
ETHYLENE GLYCOL
FDCC BLUE DYE
FENITROTHION (SUMITHION)
FENSULFOTHION
FENTHION
FLASH POINT
FLOW
FLUORANTHENE
FLUORENE
FLUORIDE
FLUORINE
FONOFOS (DYFONATE)
FORMALDEHYDE
FREE LIQUID
GEOTECH PARAMETERS
GROSS ALPHA, TOTAL
GROSS BETA, TOTAL
GUTHION
HALOGEN, PURGEABLE ORGANIC
HALOGEN, TOTAL ORGANIC
HARDNESS (AS CAC03 )
HEAT CONTENT (HEAT OF COMBUSTION)
HEPTACHLOR
HEPTACHLOR EPOXIDE
HEPTACHLORODIBENZODIOXIN (TOTAL)
HEPTACHLORODIBENZODIOXIN (TOTAL)
HEPTACHLORODIBENZODIOXIN,
1,2,3,4,6,7,8-
HEPTACHLORODIBENZOFURAN (TOTAL)
HEPTACHLORODIBENZOFURAN (TOTAL)
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
MG/L
UG/L
UG/L
UG/L

MGD
UG/L
UG/L
MG/L

UG/L
UG/L


PC/L
PC/L
UG/L
UG/L
UG/L
MG/L

UG/L
UG/L
NG/L
NG/L
NG/L
NG/L
NG/L
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG
UG/KG
UG/KG
UG/KG


UG/KG
UG/KG
MG/KG

UG/KG
UG/KG
ML /KG

PC/G
PC/G
UG/KG

UG/KG

BTU/#
UG/KG
UG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG


MG/KG
MG/KG
MG/KG

MG/KG
MG/KG




MG/KG




MG/KG
MG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
DEC C

MG/KG
MG/KG
MG/KG
%
MG/KG
MG/KG
ML /KG



MG/KG

MG/KG

BTU/#
MG/KG
MG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG




UG/M3




UG/M3







UG/M3
UG/M3




















                                            Table 7-3
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 15
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS  UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE WASTE    AIR
422
423
5190
5786
7910
6145
5200
6065
6090
408
6783
405
406
407
421
6789
417
418
419
420
6045
5185
6796
6712
6819
3023
5150
6225
2145
2146
2730
5840
6085
7733
7900
7906
2720
2060
HEPTACHLORODIBENZOFURAN,
1,2,3,4,6,7,8-
HEPTACHLORODIBENZOFURAN,
1,2,3,4,7,8,9-
HEPTACHLORONORBORNENE (HCNB)
HERBAN (NOREA)
HEXACHLORO- 1 , 3 -BUTADIENE
HEXACHLOROBENZENE (HCB) (EXTRACTABLE)
*
HEXACHLOROBENZENE (HCB) (PESTICIDE)
HEXACHLOROBUTADIENE
HEXACHLOROCYCLOPENTADIENE (HCCP)
HEXACHLORODIBENZODIOXIN (TOTAL)
HEXACHLORODIBENZODIOXIN (TOTAL)
HEXACHLORODIBENZODIOXIN, 1,2,3,4,7,8-
HEXACHLORODIBENZODIOXIN, 1,2,3,6,7,8-
HEXACHLORODIBENZODIOXIN, 1,2,3,7,8,9-
HEXACHLORODIBENZOFURAN (TOTAL)
HEXACHLORODIBENZOFURAN (TOTAL)
HEXACHLORODIBENZOFURAN, 1,2,3,4,7,8-
HEXACHLORODIBENZOFURAN , 1,2,3,6,7,8-
HEXACHLORODIBENZOFURAN , 1,2,3,7,8,9-
HEXACHLORODIBENZOFURAN, 2,3,4,6,7,8-
HEXACHLOROETHANE
HEXACHLORONORBORNADIENE (HCNBD)
HMX (EXPLOSIVE)
HYDROCARBONS, TOTAL PETROLEUM (TPHC)
HYDROCARBONS, TOTAL POLYAROMATIC (PAH)
HYDROGEN
HYDROXYCHLORDENE, 1- /2
INDENO (1,2, 3 -CD) PYRENE
IRON*
IRON (LOW LEVEL)
IRON, DISSOLVED
ISODRIN
ISOPHORONE
ISOPROPYL ETHER
ISOPROPYLBENZENE
ISOPROPYLTOLUENE, P-
LANTHANUM
LEAD
NG/L
NG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
NG/L
NG/L
NG/L
NG/L
NG/L
NG/L
NG/L
NG/L
NG/L
NG/L
NG/L
UG/L
UG/L
UG/L
MG/L
UG/L

UG/L
UG/L
MG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
NG/KG
NG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
UG/KG
UG/KG
UG/KG
MG/KG
UG/KG

UG/KG
UG/KG
MG/KG
MG/KG

UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG
MG/KG
NG/KG
NG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
NG/KG
NG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
%
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG




UG/M3
UG/M3

UG/M3
UG/M3











UG/M3






UG/M3




UG/M3
UG/M3
UG/M3
UG/M3


                                            Table 7-3
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 16
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS   UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE WASTE    AIR
4015
2726
2140
2141
5875
5901
6804
2130
5807
5808
2122
6002
2124
2123
2120
2121
5788
7732
5877
5175
7142
7058
7086
5865
6280
7045
6066
6243
6242
6244
5853
5780
5837
6999
5999
7999
5802
2050
6807
LINEAR ALKYL SULFONATE
LITHIUM
MAGNESIUM*
MAGNESIUM (LOW LEVEL)
MALATHION
MALI NATE
MALONONITRILE
MANGANESE
MCPA
MCPP
MERCURY, DIMETHYL- (AS MERCURY)
MERCURY, DIMETHYL- (EXTRACTABLE)
MERCURY, MONOETHYL- (AS MERCURY)
MERCURY, MONOMETHYL- (AS MERCURY)
MERCURY, TOTAL
MERCURY, TOTAL UTL
MERPHOS (FOLEX)
METHANE
METHOMYL (LANNATE)
METHOXYCHLOR
METHYL BUTYL KETONE (2-HEXANONE)
METHYL ETHYL KETONE (2-BUTANONE)
METHYL ISOBUTYL KETONE
( 4 -METHYL - 2 - PENTANONE )
METHYL PARATHION
METHYL-4, 6 -DINITROPHENOL, 2-
METHYLENE CHLORIDE
METHYLNAPHTHALENE , 2 -
METHYLPHENOL, (3 -AND/OR 4-)
METHYLPHENOL, 2-
METHYLPHENOL, 4-
METOLACHLOR
MEVINPHOS (PHOSDRIN)
MIREX
MISCELLANEOUS EXTRACTABLES
MISCELLANEOUS PESTICIDES
MISCELLANEOUS VOLATILES
MOLINATE
MOLYBDENUM
MONOBROMOACETIC ACID
MG/L
UG/L
MG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
NG/L
UG/L
NG/L
NG/L
UG/L
NG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
MG/KG
MG/KG
MG/KG
MG/KG
UG/KG
UG/KG
UG/KG
MG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG
UG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
UG/KG
MG/KG
UG/KG
UG/KG
MG/KG
UG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG


MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

















UG/M3


UG/M3
UG/M3
UG/M3

UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3



UG/M3
UG/M3
UG/M3



                                            Table 7-3
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 17
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS   UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE WASTE    AIR
6771
6808
6774
6055
6010
6140
6075
2055
3035
3036
3033
3034
6096
6121
6126
6060
6778
3032
3065
3066
6245
6290
5170
5160
5195
411
6785
425
6791
5855
1011
1012
4020
4025
5866
5805
5796
5850
5172
3019
MONOBUTYL TIN
MONOCHLOROACETIC ACID
MONOPHENYL TIN
N-NITROSODI -N- PROPYLAMINE
N-NITROSODIMETHYLAMINE
N-NITROSODI PHENYLAMINE/DIPHENYLAMINE
NAPHTHALENE
NICKEL
NITRATE/NITRITE NITROGEN
NITRATE/NITRITE NITROGEN, DISSOLVED
NITRATE/NITROGEN
NITRITE/NITROGEN
NITROANILINE, 2-
NITROANILINE, 3-
NITROANILINE, 4-
NITROBENZENE
NITRODIPHENYLAMINE, 2-
NITROGEN
NITROGEN, TOTAL KJELDAHL
NITROGEN, TOTAL KJELDAHL (DISSOLVED)
NITROPHENOL, 2-
NITROPHENOL, 4-
NONACHLOR, CIS- /2
NONACHLOR, TRANS -/2
OCTACHLOROCYCLOPENTENE (OCCP)
OCTACHLORODIBENZODIOXIN
OCTACHLORODIBENZODIOXIN
OCTACHLORODIBENZOFURAN
OCTACHLORODIBENZOFURAN
OCTACHLORONAPHTHALENE
ODOR (60 DEGREE C)
ODOR (ROOM TEMP)
OIL AND GREASE
OIL IDENTIFICATION
ORDRAM
ORTHENE (ACEPHATE)
OXAMYL
OXYCHLORDANE
OXYCHLORDANE (OCTACHLOREPOXIDE) /2
OXYGEN
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
MG/L
MG/L
MG/L
MG/L
UG/L
UG/L
UG/L
UG/L
UG/L

MG/L
MG/L
UG/L
UG/L
UG/L
UG/L
UG/L
NG/L
NG/L
NG/L
NG/L
UG/L
TOD
TOD
MG/L

UG/L
UG/L
UG/L
UG/L
UG/L

UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG
MG/KG

MG/KG

UG/KG
UG/KG
UG/KG
UG/KG
UG/KG

MG/KG

UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
NG/KG
NG/KG
NG/KG
NG/KG
UG/KG


MG/KG

UG/KG
UG/KG
UG/KG
UG/KG
UG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
NG/KG
NG/KG
NG/KG
NG/KG
MG/KG


MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
%
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
NG/KG
NG/KG
NG/KG
NG/KG
MG/KG


MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
%



UG/M3

UG/M3
UG/M3





UG/M3
UG/M3
UG/M3
UG/M3




UG/M3
UG/M3


















                                            Table 7-3
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 18
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS   UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE WASTE    AIR
8011
8010
5815
5870
1047
5813
6286
6817
404
6782
403
416
6788
414
415
6818
6285
8020
1013
1021
1019
1022
6155
6250
4030
5900
5816
3040
3070
3072
3060
5784
5898
2160
2161
5897
5829
5903
5864
5797
OXYGEN, DISSOLVED (ELECTRODE)
OXYGEN, DISSOLVED (WINKLER)
PARAQUAT
PARATHION, ETHYL-
PARTICULATE, TOTAL SUSPENDED
PEBULATE (TILLAM)
PENTACHLOROANI SOLE
PENTACHLOROBENZENE
PENTACHLORODIBENZODIOXIN (TOTAL)
PENTACHLORODIBENZODIOXIN (TOTAL)
PENTACHLORODIBENZODIOXIN, 1,2,3,7,8-
PENTACHLORODIBENZOFURAN (TOTAL)
PENTACHLORODIBENZOFURAN (TOTAL)
PENTACHLORODIBENZOFURAN , 1,2,3,7,8-
PENTACHLORODIBENZOFURAN , 2,3,4,7,8-
PENTACHLORONITROBENZENE
PENTACHLOROPHENOL
PH (FIELD)
PH (LABORATORY)
PH (METHOD 9040)
PH (METHOD 9045)
PH (METHOD 9045B)
PHENANTHRENE
PHENOL
PHENOLS (4AAP)
PHORATE (THIMET)
PHOSDRIN
PHOSPHORUS, ORTHO- PHOSPHATE
PHOSPHORUS, TOTAL
PHOSPHORUS, TOTAL (LOW LEVEL)
PHOSPHORUS, TOTAL DISSOLVED
PICLORAM
PIPERONYL BUTOXIDE
POTASSIUM*
POTASSIUM (LOW LEVEL)
PROMETON
PROMETRYNE
PROPACHLOR
PROPAZINE
PROPICONAZOLE (TILT)
MG/L
MG/L
UG/L
UG/L

UG/L
UG/L
UG/L
NG/L
NG/L
NG/L
NG/L
NG/L
NG/L
NG/L
UG/L
UG/L
SU
PHUN
PHUN
PHUN
PHUN
UG/L
UG/L
UG/L
UG/L
UG/L
MG/L
MG/L
UG/L
MG/L
UG/L
UG/L
MG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L


UG/KG
UG/KG

UG/KG
UG/KG
UG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
UG/KG
UG/KG
SU
PHUN
PHUN
PHUN
PHUN
UG/KG
UG/KG
MG/KG
UG/KG
UG/KG
MG/KG
MG/KG
UG/KG

UG/KG
UG/KG
MG/KG
MG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG


MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
MG/KG
MG/KG
SU



PHUN
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
UG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG


MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
NG/KG
MG/KG
MG/KG
SU
PHUN
PHUN
PHUN
PHUN
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
UG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
















UG/M3





UG/M3
UG/M3
















                                            Table 7-3
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 19
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS   UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE WASTE    AIR
7901
6777
5890
6175
6296
6802
1112
1110
1113
1111
6797
1049
5826
9998
5500
400
300
6000
5800
2000
3000
5001
5000
7000
2070
5891
5893
3046
3045
2005
5210
5827
2150
2151
1053
1051
1052
1040
1045
1050
PROPYLBENZENE, N-
PROPYLENE GLYCOL DINITRATE
PYDRIN (FENVALERATE)
PYRENE
PYRIDINE
QUINUCLIDINOL, 3-
RADIUM-226, DISSOLVED
RADIUM-226, TOTAL
RADIUM-228, DISSOLVED
RADIUM-228, TOTAL
RDX (EXPLOSIVE)
REACTIVITY PARAMETERS
ROZOL
SAMPLE WT
SCAN, DDT
SCAN, DIOXIN
SCAN, EP-TOX
SCAN, EXTRACTABLES
SCAN, HERBICIDES
SCAN, METALS
SCAN, NUTRIENTS
SCAN, PCB
SCAN, PESTICIDES
SCAN, VOLATILES
SELENIUM
SENCOR (METRIBUZIN)
SEVIN (CARBARYL)
SILICA (SI02)
SILICON (SI)
SILVER
SILVEX (2,4,5-TP)
SIMAZINE
SODIUM*
SODIUM (LOW LEVEL)
SOLIDS, % FIXED
SOLIDS, % TOTAL
SOLIDS, % VOLATILE
SOLIDS, SETTLEABLE
SOLIDS, TOTAL
SOLIDS, TOTAL (VOLATILE)
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
PC/L
PC/L
PC/L
PC/L
UG/L

UG/L


NG/L








UG/L
UG/L
UG/L
MG/L
UG/L
UG/L
UG/L
UG/L
MG/L
UG/L
%
%
%
MG/L
MG/L
MG/L
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
PC/G
PC/G
PC/G

UG/KG

UG/KG


NG/KG








MG/KG
UG/KG
UG/KG
MG/KG
MG/KG
MG/KG
UG/KG
UG/KG
MG/KG
MG/KG
%
%
%

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG




MG/KG

MG/KG


NG/KG








MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG






MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG




MG/KG

MG/KG


NG/KG








MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG




MG/KG
MG/KG
UG/M3


UG/M3
UG/M3


















UG/M3
















                                            Table 7-3
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 20
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS   UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE  WASTE    AIR
1065
1066
1070
1055
1060
1105
2080
7158
3050
3057
3055
3054
3056
5832
3024
4040
6780
6786
1074
1073
600
800
200
500
700
2732
2085
8025
1017
426
6792
5799
5820
6820
402
6781
401
413
SOLIDS, TOTAL DISSOLVED (105 DEGREE
C)
SOLIDS, TOTAL DISSOLVED (180 DEGREE
C)
SOLIDS, TOTAL DISSOLVED (VOLATILE)
SOLIDS, TOTAL SUSPENDED
SOLIDS, TOTAL SUSPENDED (VOLATILE)
STANDARD PLATE COUNT, 35C, 48HR/ML
STRONTIUM
STYRENE
SULFATE
SULFIDES (ION SELECTIVE ELECTRODE)
SULFIDES (METHYLENE BLUE METHOD)
SULFIDES, REACTIVE (AS H2S)
SULFITE
SULFOTEPP
SULFUR
TANNIN AND LIGNIN
TCDD, 2,3,7,8- (DIOXIN)
TCDF, 2,3,7,8- (DIBENZOFURAN)
TCLP (INORGANIC)
TCLP (ORGANIC)
TCLP SCAN, EXTRACTABLES
TCLP SCAN, HERBICIDES
TCLP SCAN, METALS
TCLP SCAN, PESTICIDES
TCLP SCAN, VOLATILES
TECHNETIUM
TELLURIUM
TEMPERATURE
TEQ (TOXIC EQUIVALENT VALUE, TCDD)
TEQ (TOXIC. EQUIV. VALUE, FROM
I-TEF/89)
TEQ (TOXICITY EQUIVALENT VALUE)
TERBUFOS
TERBUTRYN
TETRACHLOROBENZENE, 1,2,4,5-
TETRACHLORODIBENZODIOXIN (TOTAL)
TETRACHLORODIBENZODIOXIN (TOTAL)
TETRACHLORODIBENZODIOXIN, 2,3,7,8-
TETRACHLORODIBENZOFURAN (TOTAL)
MG/L
MG/L
MG/L
MG/L
MG/L

UG/L
UG/L
MG/L
MG/L
MG/L
MG/L
MG/L
UG/L

MG/L
NG/L
NG/L


MG/L
MG/L
MG/L
MG/L
MG/L

UG/L
DEC C
PPQ
NG/L
NG/L
UG/L
UG/L
UG/L
NG/L
NG/L
NG/L
NG/L






MG/KG
UG/KG
MG/KG
MG/KG
MG/KG
MG/KG

UG/KG


NG/KG
NG/KG


MG/L
MG/L
MG/L
MG/L
MG/L

MG/KG

PPT
NG/KG
NG/KG
UG/KG
UG/KG
UG/KG
NG/KG
NG/KG
NG/KG
NG/KG






MG/KG
MG/KG

MG/KG



MG/KG


NG/KG
NG/KG


MG/L
MG/L
MG/L
MG/L
MG/L

MG/KG

PPT
NG/KG
NG/KG
MG/KG
MG/KG
MG/KG
NG/KG
NG/KG
NG/KG
NG/KG






MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
%

NG/KG
NG/KG


MG/L
MG/L
MG/L
MG/L
MG/L

MG/KG
DEC C
PPT
NG/KG
NG/KG
MG/KG
MG/KG
MG/KG
NG/KG
NG/KG
NG/KG
NG/KG







UG/M3






























                                            Table 7-3
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 21
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS   UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE  WASTE    AIR
6787
412
7151
7135
7140
6291
6766
7735
6799
2095
3029
2075
2090
6798
7145
5120
1075
5892
5823
6773
6809
6814
7912
6710
7909
6070
6705
7075
7115
7100
7010
6266
6265
7175
6815
5798
7904
7902
6801
TETRACHLORODIBENZOFURAN (TOTAL)
TETRACHLORODIBENZOFURAN, 2,3,7,8-
TETRACHLOROETHANE , 1,1,1,2-
TETRACHLOROETHANE , 1,1,2,2-
TETRACHLOROETHENE
( TETRACHLOROETHYLENE )
TETRACHLOROPHENOL, 2,3,4,6-
TETRACHLOROPHENOL, 2,3,5,6-
TETRAHYDROFURAN
TETRYL (EXPLOSIVE)
THALLIUM
THIOCYANATE
TIN
TITANIUM
TNT (EXPLOSIVE)
TOLUENE
TOXAPHENE
TOXICITY (EP)
TREFLAN (TRIFLURALIN)
TRIALLATE
TRIBUTYL TIN
TRICHLOROACETIC ACID
TRICHLOROACETONITRILE
TRICHLOROBENZENE, 1,2,3-
TRICHLOROBENZENE, 1,2,3-
TRICHLOROBENZENE, 1,2,4-
TRICHLOROBENZENE, 1,2,4-
TRICHLOROBENZENE, 1,3,5-
TRICHLOROETHANE, 1,1,1-
TRI CHLOROETHANE , 1,1,2-
TRICHLOROETHENE (TRICHLOROETHYLENE)
TRI CHLOROFLUOROMETHANE
TRICHLOROPHENOL, 2,4,5-
TRICHLOROPHENOL, 2,4,6-
TRICHLOROPROPANE, 1,2,3-
TRICHLOROPROPANONE, 1,1,1-
TRIDEMORPH (CALIXIN)
TRIMETHYLBENZENE, 1,2,4-
TRIMETHYLBENZENE, 1,3,5-
TRINITROBENZENE, 1,3,5-
NG/L
NG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
MG/L
UG/L
UG/L
UG/L
UG/L
UG/L
MG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
NG/KG
NG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
MG/KG
MG/KG
MG/KG
MG/KG
UG/KG
UG/KG
UG/KG

UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
NG/KG
NG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
NG/KG
NG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG


UG/M3
UG/M3
UG/M3
UG/M3

UG/M3






UG/M3







UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3


UG/M3
UG/M3

                                            Table 7-3
-------
                                                              Section: 7
                                                              Revision: 1
                                                              Date: December 1, 1997
                                                              Page: 22
TEST
  #
   TEST
DESCRIPTION
UNITS  UNITS  UNITS  UNITS   UNITS
WATER  SOLIDS TISSUE WASTE    AIR
6776
1080
2731
2725
2100
5814
7054
7035
7156
7160
7157
7165
7170
2105
1084
2110
2115
TRIPHENYL TIN
TURBIDITY
URANIUM 234
URANIUM, TOTAL METAL
VANADIUM
VERNAM (VERNOLATE)
VINYL ACETATE
VINYL CHLORIDE
XYLENE, (M- AND/OR P-)
XYLENE, M-
XYLENE, 0-
XYLENE, 0- (MIXED)
XYLENES, TOTAL
YTTRIUM
ZEAXANTHIN A (HPLC)
ZINC
ZIRCONIUM
UG/L
NTU

UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L
UG/L

UG/L
UG/L
UG/L
UG/L
UG/L
UG/KG


MG/KG
MG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG
UG/KG

UG/KG
MG/KG
UG/KG
MG/KG
MG/KG
MG/KG


MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG


MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG
MG/KG

MG/KG
MG/KG
MG/KG
MG/KG
MG/KG






UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3
UG/M3




                                            Table 7-3
-------
                                                    Section 8
                                                    Revision:  0
                                                    Date:   August 1990
                                                    Page 1
8.  SAMPLE COLLECTION AND HANDLING

    8.1.  Sample Collection - Water

        8.1.1.  Water samples should be collected using standard field sampling
        techniques consistent with the parameter being determined.   Sampling
        procedures are followed that minimize the possibility of sample
        adulteration by either the sample collector or sampling device.  Field
        sample  collection procedures are detailed in the Environmental
        Investigations Branch, Standard Operating Procedures and Quality
        Assurance Manual.

        8.1.2.  Sample Containers and Sample Preservation:   Containers and
        preservation techniques used must be consistent with the
        recommendations contained in Table 8-1.

            8.1.2.1. Selection of sample container types and preservation
            techniques are further guided by the method being applied.
            Additional guidance is available in references,  e.g.,  Standard
            Methods for the Examination of Water and Wastewater, ASTM, Book of
            Standards, Volume 11.01 and 11.02 and EPA Methods for Chemical
            Analyses of Water and Waste.

            8.1.2.2. Samples must be accompanied by proper identification,
            e.g., tags, labels, and chain-of-custody forms.   Sample source,
            date of collection, time of collection, and analysis required must
            be  provided.

            8.1.2.3. Laboratory pure water blanks are prepared containing the
            preservative for each type of sample collected,  such as metals,
            nutrients, phenols, etc.  The same preservative  is used for both
            blanks and samples.  The blanks are then analyzed along with the
            samples for the constituents of interest.

    8.2.  Sample Handling - Water

        8.2.1.  Handling of samples must be done in a manner  that both insures
        the integrity of the sample and minimizes sample alteration.  Sample
        custody is handled according to the procedures outlined in Section 3
         of this document.

        8.2.2.  When samples are not analyzed within the recommended holding
        time,  a notation of this will be made in the final data report.

        8.2.3.  Intralaboratory sample control and handling is the
        responsibility of a project analyst.

    8.3.  Sample Collection and Handling - Other Substrates

        8.3.1.  Air, sediment, sludge, plant, and animal tissue samples, should
        be collected using techniques consistent with the  parameter being de-
        termined and with the recommendations contained in Table 8-1.
        Sampling procedures are followed that minimize the possibility of
        sample  adulteration either by the sample collector or sampling device.

        8.3.2.  Sediment and sludge samples for organic analyses must be
        collected in glass containers with Teflon or aluminum-foil-lined caps.
        Samples must be maintained at 4°C and analyzed as  soon as possible
        after collection.   Sediment samples for extractable  organic analyses
-------
                                            Section:  8
                                            Revision: 1
                                            Date:   December 1, 1997
                                            Page:  2

must be in 4 oz or 8 oz glass bottles.  Samples for VGA analyses must
be in 40 ml VGA vials or 4 oz wide mouth jars.

8.3.3. Sediment and sludge samples for nutrient and metal analyses
should be collected in glass or plastic jars and cooled to 4°C.

8.3.4. Tissues from specific organs of fish or whole fish specimens
should be frozen immediately after collection.

    8.3.4.1. If organic analyses are to be performed on fish tissue,
    the tissue should be wrapped in aluminum foil  (shiny side out)
    prior to freezing.

    8.3.4.2. For metal analyses, fish are wrapped in aluminum foil and
    then placed in plastic bags.  Past studies have indicated little
    or no problems due to aluminum contamination.
-------
                                                    Section:  8
                                                    Revision: 1
                                                    Date:   December 1, 1997
                                                    Page:  3
                         RECOMMENDED SAMPLE CONTAINERS,  SAMPLE PRESERVATION,  SAMPLE HOLDING TIMES,  AND
                                                    PERMISSIBLE SAMPLE TYPE
Parameter

Concentrated Waste Samples

Organic Compounds -
Extractable and
Pesticide/PCBs

Organic Compounds-
Purgeable  (VGA)
Metals and Other
Inorganic Compounds

EP Toxicity
TCLP Purgeable
Organics (VGA)
TCLP Extractable
Organics, Herbicides and
Pesticide/PCBs

TCLP Mercury
TCLP Metals except
mercury

Flash Point and/or
Heat Content
Container
8-oz. widemouth glass
 with Teflon liner
2-oz.(60-mL) VGA container
with Teflon lined Septum
 sealed caps

8-oz. widemouth glass
 with Teflon liner

8-oz. widemouth glass
 with Teflon liner

2-oz.(60-mL) VGA container
with Teflon lined Septum
 sealed caps1

8-pz. widemouth glass
 with Teflon liner1
8-pz. widemouth glass
 with Teflon liner1
Permissible
Preservative
None
ner None
m
None
None
ner None
Holding
Time
14 days
14 days
Not Speci-
fied
Not Speci-
fied
28 days2
Sample
G or C
G or C
G or C
G or C
G or C
Reference
A
A
A
B
A
None
None
Sample will be taken        None
from TCLP Mercury container1
8-oz. widemouth glass
 with Teflon liner
None
 54 days"



 56 days"


360 days"
Not Speci-
  fied
G or C



G or C


G or C


G
                                                 A
-------
                                                    Section:  8
                                                    Revision: 1
                                                    Date:   December  1,  1997
                                                    Page:  4
Parameter

Fish Samples

Organic Compounds
Metals and Other
Inorganic Compounds
                         RECOMMENDED SAMPLE CONTAINERS,  SAMPLE PRESERVATION,  SAMPLE HOLDING TIMES, AND
                                                    PERMISSIBLE SAMPLE TYPE
Container
 Wrap in aluminum foil
 (Shiney side out)

 Place in plastic zip-
 lock bag
Permissible
Preservative
Freeze
Freeze
Holding
Time
Not Speci-
fied
Not Speci-
fied
Sample
G or C
G or C
Reference


Water - Low to Medium Concentration Samples
Alkalinity500-ml or 1-liter poly-3




Acidity



Bacteriological



Static Bioassay
   Cool,  4°          14  days          G  or  C         C
 ethylene with polyethylene
 or polyethylene
 lined closure

 500-ml or 1-liter poly-3       Cool, 4°C        14 days       G or C
 ethylene with polyethylene
 or polyethylene lined closure

 250-ml glass with glass       Cool, 4°C          6 hrs.        G
 closure or  plastic capable
 of being autoclaved

 1-gal. amber glass             Cool,  4°C        48  hrs.     G or C
 (not solvent rinsed)
-------
                                                    Section:  8
                                                    Revision: 1
                                                    Date:   December  1,  1997
                                                    Page:  5
                         RECOMMENDED SAMPLE CONTAINERS,  SAMPLE PRESERVATION,  SAMPLE HOLDING TIMES, AND
                                                    PERMISSIBLE SAMPLE TYPE
Parameter
Container
Permissible
Preservative
Water - Low to Medium Concentration Samples  (contd)
Biochemical Oxygen
Demand (BOD)

Chloride
Chlorine Residual
Color
Conductivity
Chromium, Hexavalent
Cyanide
1/2-gal. polyethylene3      Cool,  4°C
with polyethylene closure

500-ml or 1-liter poly-3    None
ethylene with polyethylene
or polyethylene lined closure
In-situ, beaker or bucket
500-ml or 1-liter poly-3
ethylene with polyethy-
lene or polyethylene
lined closure

500-ml or 1-liter poly-3
ethylene with polyethy-
lene or polyethylene
lined closure

1-liter polyethylene with
polyethylene closure

1-liter or 1/2-gallon
polyethylene with poly-
ethylene or polyethylene
lined closure
     None
     Cool,  4°C
     Cool,  4°C
     Cool,  4°C
Holding
Time
                      48 hrs.
                       28  days
 Analyze
 Immediately

48 hrs.
 28 days
              G or C
              G or C
 G  or  C
G or C
                                                                                   (determine on
                                                                                 site if possible)
    Ascorbic Acid4'5
    sodium Hydroxide,
    pH >12
    Cool,  4°C
  24  hrs.
 14 days
Reference



  C


  C



  C


  C
              C


               C
-------
                                                    Section:  8
                                                    Revision: 1
                                                    Date:   December 1, 1997
                                                    Page:  6
                         RECOMMENDED SAMPLE CONTAINERS,  SAMPLE PRESERVATION,  SAMPLE HOLDING TIMES,  AND
                                                    PERMISSIBLE SAMPLE TYPE
Parameter
                                      Container
Permissible
Preservative
Water - Low to Medium Concentration Samples  (Continued)

                                      In-situ, beaker or bucket  None
Dissolved Oxygen
(Probe)

Dissolved Oxygen
(Winkler)
EP Toxicity


Fluoride




Hardness
                                      300-ml glass, BOD bottle
                                      1-gal. glass (amber)  with
                                      Teflon liner
  Fix on site,
  store in dark
  Cool,  4°C
                                      1-liter polyethylene or3    None
                                      1/2-gal. polyethylene with
                                      polyethylene or polyethy-
                                      lene lined closure
                                      500-ml or 1-liter poly-
                                      ethylene with polyethy-
                                      lene or polyethylene
                                      lined closure
  50% Nitric4
  Acid,  pH <2
Holding
 Time
Determine
On Site

8 hrs .
 (determine
on site if
possible)

Not Speci-
fied

28 days
 6  months
                         Reference
              G or C
                                   G or C
             G or C
LAS
                                      500-ml or 1-liter poly-3    Cool,
                                      ethylene with polyethylene
                                      or polyethylene lined closure
        4°C
48 hrs.
             G or C
-------
                                                    Section:  8
                                                    Revision: 1
                                                    Date:   December 1, 1997
                                                    Page:  7
                         RECOMMENDED SAMPLE CONTAINERS,  SAMPLE PRESERVATION,  SAMPLE HOLDING TIMES,  AND
                                                    PERMISSIBLE SAMPLE TYPE
Parameter
  Container
Water - Low to Medium Concentration Samples  (Continued)

Metals                                1-liter polyethylene
                                      with polyethylene lined
                                      closure
Metals, Dissolved
Nutrients6 1-liter polyethylene or
Oil and grease
Organic Compounds -

 Extractable and
 Pesticide Scan

 No Residual Chlorine
  Present
  1-liter  polyethylene
  with  polyethylene  lined
  closure
Permissible
Preservative
  50% Nitric4
  Acid,  pH <2


 Filter-on-site4
 50% Nitric
 Acid, pH <2
50% Sulfuric4          28  days           G or C
  1/2-gal.  polyethylene      Acid,  pH <2
  with  polyethylene  or poly- Cool,  4°C
  ethylene  lined  closure
  1-liter  widemouth  glass
  with  Teflon  lined  cap
 50% Sulfuric4
 Acid,  pH <2
  Cool, 4°C
  1-gal.  amber  glass  or
  2  1/2-gal.  amber  glass
  with  Teflon lined cap
  Cool,  4°C
 Holding
   Time
                                                 6 months
6 months
28 days
               G or C
47 days7     G or C
 Reference
A or C
-------
                                                    Section:  8
                                                    Revision: 1
                                                    Date:   December  1,  1997
                                                    Page:  8
                         RECOMMENDED SAMPLE CONTAINERS,  SAMPLE PRESERVATION,  SAMPLE HOLDING TIMES, AND
                                                    PERMISSIBLE SAMPLE TYPE
Parameter
Container
Water - Low to Medium Concentration Samples  (Continued)
 Residual Chlorine
  Present
Organic Compounds -
 Purgeable (VGA)

  No Residual Chlorine
  Present
  No Residual Chlorine
  Present
  Residual Chlorine
  Present
Organic Compounds -
Specified and
Pesticides (Non-
Priority Pollutants
such as Herbicides)
1-gal. amber glass or
2 1/2-gal. amber glass
with Teflon lined cap
3 40-ml vials with
Teflon lined septum
sealed caps

3 40-ml vials with
Teflon lined septum
sealed caps

3 40-ml vials with
Teflon lined
septum sealed caps
  Permissible
  Preservative
Add 3 ml 10%
sodium thiosulfate
per gallon
Cool, 4°C
4 drops 1+1
hydrochloric acid,
Cool, 4°C

Cool, 4°C
Footnote 8
1-gal. glass  (amber) or
2 1/2-gal. glass  (amber)
with Teflon lined closure
     Footnote 9
 Holding
  Time
 47 days7
 14 days
   7  days
14 days
47 days7
Sample
 Type
 G or C
G
G or C
Reference
  A or C
             A or C
              A or C
 A or C
 A or C
-------
                                                    Section:  8
                                                    Revision: 1
                                                    Date:   December  1,  1997
                                                    Page:  9
                         RECOMMENDED SAMPLE CONTAINERS,  SAMPLE PRESERVATION,  SAMPLE HOLDING TIMES, AND
                                                    PERMISSIBLE SAMPLE TYPE
                                                 Permissible
Parameter
Container
Water - Low to Medium Concentration Samples  (Continued)
   Holding
Preservative
Sample
 Time
           Reference
Organic Halides
Total  (TOX)
pH


Phenols



Phosphate-Ortho
Phosphorus, Total
Dissolved
Solids, Settleable
250-ml amber glass with
Teflon lined septum
closure

In-situ, beaker or
bucket

1-liter amber glass
with Teflon lined
closure

500-ml or 1-liter poly-
ethylene with polyethy-
lene or polyethylene
lined closure

500-ml or 1-liter poly-
ethylene with polyethy-
lene or polyethylene
lined closure

1/2-gal. polyethylene
with polyethylene
closure
   Cool,  4°C        28  days        G
   H2S04 to pH<2
   None
   50% Sulfuric
   Acid,  pH <2
   Cool,  4°C
 Analyze
 Immediately

 28  days
   Filter-on-site  48 hrs.
   Cool,  4°C
   Filter-on-site  28 days
   50% Sulfuric
   Acid,  pH <2
     Cool,  4°C
     Cool,  4°C
48 hrs.
G


G



G




G




G or C
A or E



 C


 C
-------
                                                    Section:  8
                                                    Revision: 1
                                                    Date:   December  1,  1997
                                                    Page:  10
                         RECOMMENDED SAMPLE CONTAINERS,  SAMPLE PRESERVATION,  SAMPLE HOLDING TIMES, AND
                                                    PERMISSIBLE SAMPLE TYPE
                                                         Permissible
Parameter
Container
Water - Low to Medium Concentration Samples  (Continued)
	       Holding
Preservative       Time
                          Reference
Organic Halides
Total  (TOX)
pH


Phenols



Phosphate-Ortho
Phosphorus, Total
Dissolved
Solids, Settleable
250-ml amber glass with
Teflon lined septum
closure

In-situ, beaker or
bucket

1-liter amber glass
with Teflon lined
closure

500-ml or 1-liter poly-
ethylene with polyethy-
lene or polyethylene
lined closure

500-ml or 1-liter poly-
ethylene with polyethy-
lene or polyethylene
lined closure

1/2-gal. polyethylene
with polyethylene
closure
   Cool, 4°C       28 days       G
   H2S04 to  pH<2
   None
   50% Sulfuric
   Acid, pH <2
   Cool, 4°C
Analyze
Immediately

28 days
   Filter-on-site  48 hrs.
   Cool, 4°C
   Filter-on-site  28 days
   50% Sulfuric
   Acid, pH <2
     Cool, 4°C
     Cool, 4°C
48 hrs.
G


G



G




G




G or C
A or E



 C


 C
-------
                                                    Section:  8
                                                    Revision: 1
                                                    Date:   December 1, 1997
                                                    Page:  11
                         RECOMMENDED SAMPLE CONTAINERS,  SAMPLE PRESERVATION,  SAMPLE HOLDING TIMES,  AND
                                                    PERMISSIBLE SAMPLE TYPE
                            Permissible
Parameter
Container
       Holding
Soil, Sediment or Sludge Samples - Low to Medium Concentrations
EP Toxicity
TCLP Purgeable
Organics (VGA)
TCLP Extractable
Organics, Herbicides and
Pesticide/PCBs

TCLP Mercury
TCLP Metals except
mercury

Metals
Nutrients Including:
Nitrogen, Phos-
phorus, Chemical
Oxygen Demand

Organics -8-oz. widemouth glass
Extractable
8-oz. widemouth glass
with Teflon\ lined
closure

Two 2-oz. (60-mL)  VGA
container with Teflon lined
Septum sealed caps1

8-oz. widemouth glass
with Teflon liner1
8-oz. widemouth glass
with Teflon liner1

Sample will be taken
from TCLP Mercury container

8-oz. widemouth glass
with Teflon lined closure

500-ml polyethylene with
polyethylene closure or
8 oz. widemouth glass
with Teflon lined closure

  Cool,  4°C         ASAP
with Teflon liner
Preservative
 Cool,  4°C
 None
 None
 None
 None
 Cool,  4°C
 Cool,  4°C
    G or C
Time
Type
Reference
Not
Speci- G or C
B
fied
28
54
56
360
days2 G or C
days2 G or C
days2 G or C
days2 G or C
6 months G or C
Not
fied
Speci- G or C

A
A
A
A
A
A

-------
                                                    Section:  8
                                                    Revision: 1
                                                    Date:   December 1, 1997
                                                    Page:  12
                         RECOMMENDED SAMPLE CONTAINERS,  SAMPLE PRESERVATION,  SAMPLE HOLDING TIMES,  AND
                                                    PERMISSIBLE SAMPLE TYPE
Parameter
Container
Permissible      Holding         Sample
           Preservative       Time
Soil, Sediment or Sludge Samples - Low to Medium Concentrations
Organics -2-oz.  (60 ml) VGA vial
Purgeable (VGA)

Other Inorganic
Compounds -
Including Cyanide
                        Cool, 4°C      14 days
                      w/Teflon lined septum seal

                      500-ml polyethylene
                      with polyethylene
                      closure or 8-oz.  wide
                      mouth glass with
                      Teflon lined closure
Municipal Sludge - Low to Medium Concentrations
Organics -0 - 30% Solids
Extractable &
Pesticide/PCBs
Organics -
Purgeables (VGA)
                        Cool, 4°C      47 days7
                      1- gal. amber glass or
                      4 qt wide mouth bottle
                      (depending on consistency)
                      with Teflon lined cap
                      > 30% Solids
                      8-oz widemouth glass jar
                      with Teflon lined cap

                      0-1% Solids
                      3 40-mL VGA vials with
                      Teflon lined septum
                      sealed caps

                      > 1% Solids
                      2 2-oz (60 mL)  VGA vials
                      w/ Teflon lined septum
                      sealed cap
                                     G or C
                                     Cool,  4°C
                                     G  or  C
                                                                    Cool, 4°C
                                     4 drops 1+1
                                     HC1 acid,
                                     Cool,  4°C
                                                                    Cool, 4°C
     Reference
Not Speci-
fied
                                                    47  days7
14 days
                                                    14  days
G or C
A
             G or C
 G or C
              G or C
NOTE;  The Analytical Support Branch should be consulted prior to making any changes to any of the above  sampling protocols.
-------
                                                    Section:  8
                                                    Revision: 1
                                                    Date:   December 1, 1997
                                                    Page:  13


                     RECOMMENDED SAMPLE CONTAINERS, SAMPLE PRESERVATION, SAMPLE HOLDING TIMES, AND
                                                PERMISSIBLE SAMPLE TYPE

Abbreviations:  G  = Grab                C  = Composite
                NS = Not Specified     ASAP = As Soon As Possible

Footnotes:

1. The TCLP method requires the leaching of 25 gm of solid for volatile organics and 100 gm of solids for all other
   parameters.  If the sample is low in solids, additional sample containers may be required to provide sufficient
   sample for the TCLP leach extraction.

2. These are total holding times for TCLP that cover sampling through analysis.  The holding times are broken down as
      follows:   TCLP  volatile  organics  -  14  days  from collection  to  TCLP extraction  plus  14  days  from leach  extraction
      to  analysis;  extractable organics,  pesticides  & herbicides  - 7  days  from  collection to TCLP  extraction plus  7
      days  to  solvent extraction of  leachate plus  40 days to  analysis of extract; mercury -  28  days  from  collection  to
      TCLP  extraction plus  28  days to analysis; metals  except  mercury -  180  days  from collection  to  TCLP  extraction
      plus  180  days  to analysis.

3. Use indicated container for single parameter requests or 1/2-gallon polyethylene container  for multiple parameter
   requests except those including BOD.  Use a 1-gallon polyethylene container for multiple parameter requests which
   include BOD.

4. Must be preserved  in the field at time of collection.

5. Use ascorbic acid only if the sample contains residual chlorine.   Test a drop of sample with potassium iodide-starch
   test paper; a blue color indicates need  for treatment.  Add ascorbic acid, a few crystals at a time, until a drop of
   sample produces no color on the indicator paper.  Then add an additional 0.6 g of ascorbic  acid for each  liter of
   sample volume.

6. May include nitrogen series (ammonia, total Kjeldahl nitrogen, nitrate-nitrite), total phosphorus, chemical oxygen
   demand and total organic carbon.

7. Samples must be extracted within seven days and  extract must be analyzed within 40 days.

8. Collect the sample in a 4 oz.  soil VGA container which has been pre-preserved with four drops of 25 percent ascorbic
   acid solution.  Gently mix the sample and transfer to a 40 ml VGA vial that has been prepreserved with four drops
   1+1 HC1, cool to 4°C.

9. See Organic Compounds - Extractable  (page 8 & 9  of 15).  The Analytical Support Branch should be consulted for any
   special organic compound analyses in order to check on special preservation requirements and or extra sample volume.
-------
                                                    Section:  8
                                                    Revision: 1
                                                    Date:   December 1, 1997
                                                    Page:  14


                  RECOMMENDED SAMPLE CONTAINERS,  SAMPLE PRESERVATION,  SAMPLE HOLDING TIMES,  AND
                                             PERMISSIBLE SAMPLE  TYPE
References
A.    US-EPA, Test Methods for Evaluating Solid Waste, SW-846, 3rd Edition, Office of Solid Waste and Emergency
      Response"! Washington,DC, Nov. 1986.


B.    US-EPA, Test Methods for Evaluating Solid Waste, SW-846, Office of Solid Wastes, Washington, DC,  1982.

C.    40 CFR Part 136, Federal Register, Vol. 49, No. 209, October 26, 1984.
D.    US-EPA, Region IV, Environmental Services Division, "Ecological Support Branch, Standard Operating
      Procedures Manual," latest version.

E.    EPA Interim Method 450.1, "Total Organic Halide," US-EPA, ORD, EMSL, Physical and Chemical Methods Branch,
      Cincinnati, Ohio, November 1980.

F.    US-EPA, Analytical Methods for the National Sewage Sludge Survey, Office of Water Regulations and
      Standards, Washington, DC, Aug. 1989.
-------
                                                    Section 9
                                                    Revision:  0
                                                    Date:  August 1990
                                                    Page 1
9.  SAMPLE RECORDS AND DATA HANDLING

    9.1.  Sample accountability through the analytical process can be divided
    into three major elements:  (1)  initial sample logging;  (2)  data
    acquisition,  and (3)  documentation/storage.  The laboratory location,
    i.e., field or central, and the analyses requested will  dictate the nature
    and location of the sample and data records.  In addition to the procedure
    discussed in Section 3 of this manual, the following sections outline
    current sample and data documentation procedures.

    9.2.  Sample Logging

        9.2.1. Field Laboratory Sample Logging

            9.2.1.1. Samples received at a field laboratory with accompanying
            identification are logged into the field sample logbook.  Samples
            are assigned sample ID and station ID.

    9.3.  SESD Laboratory Sample Logging

        9.3.1. Samples received at the SESD laboratory with accompanying iden-
        tification are logged into the Region 4 Laboratory Information
        Management System  (R4LIMS).   Samples are assigned consecutive log
        numbers and logged as described above.

        9.3.2. Also contained in the R4LIMS is a description of the dis-
        position of every log number used, whether in the field or SESD
        laboratory.

    9.4.  Analytical Data Handling

        9.4.1. General

            9.4.1.1. All raw analytical and instrument control data generated
            in the laboratory are entered into bound data books or kept as
            strip charts, or in instrument computer hardcopy,  tape, or disk.

            9.4.1.2. Information contained in these data logbooks includes the
            following:   project number, sample log number, parameter, date of
            analysis, analyst, and all pertinent instrument identification
            with analytical conditions.  For non-computerized instruments all
            calibration data, all readout data, calculation, final concen-
            tration, and quality control data should also be recorded in the
            log.

            9.4.1.3. Final results of all analyses are provided in a standard
            computerized report format and forwarded to the requester with
            cover memorandum.  Remarks should be used with reported data to
            alert the user to some specific condition that affects the data.


        9.4.2. More specific information on data handling is contained in
        Sections 10 and 11.

    9.5.   Computerized Analytical Data System

        9.5.1. Introduction
-------
                                            Section:  9
                                            Revision: 1
                                            Date: December 1,  1997
                                            Page:  2

    9.5.1.1.  The "Region 4 Laboratory Information Management System"
    (R4LIMS)  is a computerized data storage and laboratory information
    management system.   R4LIMS is utilized to store project
    information as well as analytical results for specific samples.

    9.5.1.2.  R4LIMS is  structured using the Oracle data base
    management system.   R4LIMS is a very flexible, interactive system
    that integrates a variety of data processing functions within the
    structure of one high level language.

    9.5.1.3.  R4LIMS is  located on an IBM compatible computer at the
    EPA, Region 4, Science and Ecosystems Technology Center in Athens,
    GA.   All  communication with R4LIMS is through the EPA Local Area
    Network (LAN)  or Wide Area Network (WAN).

    9.5.1.4.   The sample custodian or field engineers are responsible
    for logging new projects into the system.  The sample custodian
    logs sample related information into the system.  Individual
    analysts  are responsible for entering results and verifying their
    accuracy.   The analysts are also responsible for reporting these
    results to the requestor.

9.5.2.  System Description

    9.5.2.1.  Project Logging

        9.5.2.1.1. All  Analytical projects, when initiated by the
        requester, are  logged into R4LIMS by either the project leader
        or the sample custodian.  Four digit project numbers (prefixed
        by the two digit Fiscal Year) are assigned consecutively by
        R4LIMS starting with FY-0001 at the beginning of each fiscal
        year  (e.g.,FY=89, 90, etc).   This includes all identification
        information for the project such as:   project number,  name of
        project, location, date project to be conducted, requester and
        program element, account number,  time accounting information,
        etc.

        9.5.2.1.2. If the samples from the project are to be analyzed
        by the Contract Laboratory Program (CLP), the project is
        flagged as contract and pertinent information recorded such  as
        the contract laboratory name, case number, etc. are
        identified.

        9.5.2.1.3.  Project log also stores non-sample related project
        information from field investigations.

9.5.3.  Sample Logging

    9.5.3.1.   All samples to be analyzed or tracked by R4LIMS are
    logged into the system when received.  The samples are numbered  in
    chronological order.

    9.5.3.2.   Data entered identifies and describes each sample, the
    tests required, and the test numbers.  Test numbers are maintained
    in a file.   A copy  of the sample data log printout is filed in the
    project file and another copy is sent to the requester along with
    his copy  of the custody record.

9.5.4.  Analytical Data  Processing
    9.5.4.1.   All analysis results are entered into the analytical
    results data bases.
-------
                                            Section:   9
                                            Revision:  1
                                            Date:  December 1,  1997
                                            Page:   3


    9.5.4.2.   The majority of all data is transmitted electronically
    to the Computer system.

9.5.5. Other ADP Operations

    9.5.5.1.   Quality Control Data.   Data bases are available,  or will
    be developed, for entering,  storing and summarizing precision and
    accuracy data generated during sample analysis.  This may include
    percent RSD, matrix spike recovery data,  surrogate spike recovery
    data,  results of reference sample analyses, etc.   Entry and
    verification programs are available for this QC operation.
    Summary programs are available for QC reports  as  required.

    9.5.5.2.   Sample Custody Information.  Sample  custody information,
    such as custody room check-out and check-in information, sample
    disposal information, etc.,  is kept in a custody  log.  Information
    in this log and the sample log can be combined to give a complete
    documentation of chain-of-custody for all samples.  A module to
    store this information is under development.

    9.5.5.3.   Time Accounting Information.  A data base named ASBTIME,
    divided into fiscal years, is maintained for storage and
    manipulation of personnel time.   All personnel time is entered by
    employee,  pay period, activity,  account number and program
    element.   Summary reports can be generated based  on the specific
    elements required.

    9.5.5.4.   Accounting Reports.  Various reporting  modules are
    available sample tracking and counting.

        9.5.5.4.1.  Sample Counter - Listing of number of samples
        received by type, program element, and whether analyses were
        performed by EPA or a contract lab.

        9.5.5.4.2.  Analysis Counter - Listing of  analyses by
        parameter, sample type,  and whether analyses  were conducted by
        EPA or contract laboratory.
        9.5.5.4.3.  Total Accounting Report - Listing of analyses
        within each program element by parameter,  sample type and
        whether analyses were conducted by EPA or  contract laboratory.

    9.5.5.5.   Analytical Backlogs. Several types of backlogs can be
    produced that give information on completed projects, incomplete
    projects,  and projects scheduled for the future.   These are used
    for tracking progress of samples being analyzed and for planning
    analysis of samples not yet  received.  Tailor  made requests can be
     submitted to report as much information as needed, or as specific
    as needed.

        9.5.5.5.1.  Analytical Backlog/Inhouse Samples:  List projects
        in chronological order with name, project  number, program
        element, requester, receipt data  (actual or projected),
        projected completion date, number of samples  scheduled to be
        received or number of samples received broken down into
        analytical categories (inorganics, VGA, extractable organics,
        pesticides, metals, and EP).

        9.5.5.5.2.  Analytical Backlog/Contractor  Samples:  Same
        information as above except for contract samples.
-------
                                    Section:  9
                                    Revision: 1
                                    Date: December 1, 1997
                                    Page:  4

9.5.5.5.3. Detail Backlog:  Listing of all required analyses,
by parameter test code, sample type, project number and sample
number.  The listing separates in-house analyses from
contractor analyses if requested.
-------
                                                    Section:  10
                                                    Revision:  0
                                                    Date:  September 1990
                                                    Page:  1
10.  ORGANIC ANALYSIS,  PERFORMANCE QUALITY CONTROL AND ANALYTICAL OPERATION

    10.1.  Every element of environmental data acquisition,  from sample
    collection to final data reporting,  has associated with it degrees of
    error.   The primary purpose of a total quality assurance program is the
    optimization of conditions whereby the introduction of  error can be either
    precluded or substantially reduced.   The operating procedures and quality
    control checks practiced in this laboratory and outlined in this manual
    are implemented to minimize the total error associated  with data
    generation.  No number can be affixed to total error;  however,  analytical
    performance is measurable and thus definable.  Analyses are performed in
    support of EPA Programs such as RCRA, Superfund,  NPDES, Drinking Water,
    Air Toxics, CERCLA, and other initiatives.  The methods used in organic
    analysis are based primarily on RCRA guidance.  Modifications have been
    made to increase quality, efficency, and to support specific requests of
    the various programs.

    10.2.  General

        10.2.1. It is  the  policy of this Branch to apply the best laboratory
        practices, use approved methodology when mandated by regulation and
        use standardized methodology to meet quality requirements designated
        in the following paragraphs.  When approved methodology is  not
        applicable, fully  document all operations associated with the
        generation of  data.

        10.2.2. Safety precautions associated with the safe handling of toxic
        chemicals, reagents, solutions and samples will be  observed and
        regarded as a  first order responsibility of the analyst. The analyst
        will take the  necessary precautions to prevent exposure or  harm to any
        employee.

    10.3.  Organic Methodology

        10.3.1. Section 7  contains a listing of individual  analytical methods
        used.  Table 10-1  contains a listing of current analytical  descriptors
        associated with these methods. These descriptors are used in sample
        vial labeling  and  file naming conventions in GC and GC/MS computer
        systems as appropriate.

    10.4.  Sample Preparation of Semivolatile fraction and Pesticide fraction

        10.4.1. General Quality Control Requirements

            10.4.1.1.  All  glassware and glass wool is rinsed sequentially with
            methanol,  acetone, and the sample solvent, just prior to use.

            10.4.1.2.  A reagent blank is set up with each set of 20 or less
            samples when an extraction is performed or when simply  putting a
            chemical waste sample in solution.  Include all glassware and
            extraction equipment.
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                                            Section:  10
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        10.4.1.2.1.  Water sample - Use reagent grade water and all
        solvents.

        10.4.1.2.2.  Soil/Sediment/Tissue sample - Use the appropriate
        amount of  anhydrous sodium sulfate and all solvents and
        reagents.

        10.4.1.2.3.  Waste sample - Use anhydrous sodium sulfate (if
        used in the  samples)  and all solvents and reagents.

    10.4.1.3.  Duplicate matrix spikes (spike two portions of a sample
    expected to contain no organics or low levels) and/or duplicate
    method spikes  (media known to be organic free, i.e., reagent grade
    water or for solids, clean sand and anhydrous sodium sulfate).
    Duplicate  spikes are included with each set of 20 or less samples.

    10.4.1.4.  A gel  permeation chromatograph (GPC) calibration
    standard consisting of corn oil, bis(2-ethylhexyl)phthalate, 4-
    nitrophenol, perylene, and sulfur must be passed through the GPC
    system prior to  beginning cleanup of samples, once/month.  This
    must be done more frequently after repacking the column.  Adjust
    the collection volume to recover >_ 85% of the bis (2-
    ethylhexyl)phthalate.

10.4.2. General Extraction Protocols

    10.4.2.1.  Determination of percent moisture

        10.4.2.1.1.  Sediment/Soil - Percent moisture must be
        determined on all samples unless otherwise specified.

        10.4.2.1.2.  Waste - Determine percent moisture if the sample
        is primarily heavily contaminated soil or a dry solid.  This
        must be done in an oven located in a hood.  Waste that is
        primarily  a  non-aqueous liquid does not require a percent
        moisture determination.  See Section 3.5.6.2 for additional
        handling guidance.

    10.4.2.2.  Chlorinated water samples must be dechlorinated with
    sodium thiosulfate prior to extraction.

    10.4.2.3.  All  water samples extracted for pesticide analysis from
    compliance sampling inspections (CSI)  and toxic compliance
    sampling inspections  (XCSI), and all water extracts with color
    must be passed through the alumina microcolumn.

    10.4.2.4.  If the final extract volume is greater than 1 mL,
    transfer at least 1 mL to a GC vial.  The remainder is discarded.
     Never leave any extracts in volumetric flasks.
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                                            Section:  10
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    10.4.2.5.  Labeling Laboratory Sample Containers

        10.4.2.5.1.  One or more of the analytical descriptors  should
        be used as a suffix after each sample number recorded  on the
        sample vial  and in the extraction logbook (i.e. 10234SLS for a
        semivolatile low soil extract of sample 10234).  See Table
        10-1.

        10.4.2.5.2.  Record on the blank, spikes,  and surrogate
        included with the set the inclusive numbers of the samples
        that were extracted together.

            10.4.2.5.2.1. B  -  Blank, include inclusive sample
            numbers  after B (e.g. B05440-05461SLW)

            10.4.2.5.2.2. S  -Spike,  include sample designation and
            sample number spiked after S (e.g. S12440P for pesticide
            spike of sample 12440)

            10.4.2.5.2.3. X and Y - To designate duplicate
            extractions.

            10.4.2.5.2.4. R,  R2,  R3,  etc. - To designate when  re-
            extractions are required; designate them with an "RX"
            depending on the number of re-extractions required.

            10.4.2.5.2.5. A mark is placed on each sample vial to
            indicate the bottom of the meniscus when vialed.

            10.4.2.5.2.6. The final extract volume is recorded on all
            vials and in the extraction logbook.

10.4.3.  Extraction Logbook

    10.4.3.1.  All pertinent information requested on the sheet will be
    properly recorded prior to submittal to the GC and or GC/MS
    chemists.   See Forms 10-1, 10-2,  and 10-3.

    10.4.3.2.  List the blank and spike in the sample number column.
    Record the range of sample numbers that the blank and spike
    represent  (example: blank 01411-25; spike 01411-25).

    10.4.3.3.  Record the extract volume on the sheet.

    10.4.3.4.  Record the designation for extract type after the sample
    number.

    10.4.3.5.  Record unusual occurrences during sample preparation,
    e.g.,  unusual appearance of sample, problems during extraction,
    losses of  extract, precipitation and/or increase in viscosity
    during final evaporation,  etc.

    10.4.3.6.  All calculations must be checked by a second person and
    the  extraction sheet initialed by both analyst and checker.

    10.4.3.7.  Do not erase or use "Liquid Paper"  to correct any error.
     Put one line through the error with initials and date.


10.4.4.  Sample Vial  Handling
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        10.4.4.1.  Put all vials on one board or container that pertain to
        a set of samples that were extracted together,  and label the board
        with the projects' names.  The chemist  in charge of the extraction
        laboratory should check the labeling of all vials.  Do not put two
        separate extraction batches on one board.

        10.4.4.2.  Sample vials and copies of the extraction sheet should
        be given to the chemist in charge of the pesticide or semivolatile
        analysis.

        10.4.4.3.  Include a surrogate standard solution with each set of
        samples. This solution should be at the same concentration as in
        the sample extracts.

10.5.  Surrogate Standards

    10.5.1. A surrogate standard,  a chemically inert compound not expected
    to occur in an environmental sample, is added to each sample just
    prior to extraction or purging.   The recovery of the surrogate
    standard is used to monitor for unusual matrix effects,  gross sample
    processing errors,  etc.   Surrogate recovery is evaluated by
    determining whether the measured concentration falls within the
    statistical acceptance limits.
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                                            Section:  10
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10.5.2. Following are the surrogate standards and the corresponding
spike solution concentrations currently used by ASB:
Semivolatile-Base/Neutral
Nitrobenzene - d5
Terphenyl - d!3

Semivolatile-Acid
2,4,6-tribromophenol
phenol - d6

Volatiles-Water/Soil/Sed
toluene - d8
p-bromofluorobenzene
dibromofluoromethane
Sol'n Cone.
lOOOng/uL
lOOOng/uL

Sol'n Cone.
lOOOng/uL
lOOOng/uL

Sol'n Cone.
Method 8260
modifications
Spike Amt per Final
Extract Volume

50uL/lmL
Spike Amt per Final
Extract Volume

50uL/lmL
Spike Amt per Final
Purge Volume

Method 8260
modifications
Volatiles-Air Canister
Sol'n Cone.
Spike Amt per Final
Canister Volume
toluene - d8
p-bromofluorobenzene
dibromofluoromethane
TO-14
modifications
TO-14
modifications
Organo-chlorine
Pesticides and PCBS
dibutylchlorendate (DEC)
2,4,5,6 tetrachloro-
 meta-xylene (TCMX)

Phenoxy Herbicides
Sol'n Cone.


40ng/uL

20ng/uL

Sol'n Cone.
Spike Amt per Final
Extract Volume

25uL/lmL
Spike Amt per Final
Extract Volume
DCAA (2,4 -Dichlorophenyl-
 Acetic Acid)                   20ng/uL

Organonitrogen/phosphate
Pesticide                       Sol'n Cone.
                IQOuL/lOmL
                Spike Amt per Final
                Extract/Purge Volume
2-Nitro-m-xylene (NMX)
250ng/uL
50uL/lmL
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                                            Section:  10
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10.5.3. Calculation of Acceptance Limits (All calculations are
performed by the laboratory's computer data system).

    10.5.3.1. Calculate average recovery (R) and standard deviation
    (S),  in percent recovery, for each surrogate standard using the
    entire data base over a set period of time, e.g. annually.

    10.5.3.2. Values greater than 3 standard deviations are eliminated
    from the data base as outliers. The limits are then re-calculated
    as above.

    10.5.3.3. Calculate method performance criteria and define the
    performance of the laboratory for each surrogate standard being
    used.

    10.5.3.4. Calculate upper and lower control limits for method
    performance and surrogate standard recovery:

    Semivolatiles and Pesticides:

            Upper Control Limit  (UCL)  = R + 2 S

            Lower Control Limit  (LCL)  = R - 2 S

    Volatiles:

            Upper Control Limit  (UCL)  = R + 3 S

            Lower Control Limit  (LCL)  = R - 3 S

    10.5.3.5. Surrogate limits are calculated annually.

10.5.4. Analysis of Surrogates

    10.5.4.1. Purgeable and Extractable Organics - All samples and
    blanks are to be analyzed by GC/MS.  The GC/MS analyst is
    responsible for calculating recovery, recording the data in the
    GC/MS logbook and transferring it to the PC data base using
    appropriate software.

    10.5.4.2. Pesticides/PCBs - Most samples and blanks will be
    analyzed by GC/EC or GC/NP for pesticides/PCBs.   The analyst is
    responsible for keeping a hardcopy of the pesticide surrogate data
    in the project file as well as transferring the data to the
    computer data system.  See Form 10-9.

        Percent Surrogate Recovery = Od X 100
                                        Qa

        Where Qd = Quantity determined by analysis
              Qa = Quantity added to the sample
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                                            Section:   10
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10.5.5.  Evaluation of Surrogate QC Data
    10.5.5.1.  Purgeable Organics - If surrogate standard recovery of
    any one surrogate is out of limits in a blank or a sample,  proceed
    with corrective action.

    10.5.5.2.  Extractable Organics - If recovery of two surrogates
    from the same sample pH fraction are out of limits, proceed with
    corrective action.   See below for action on blanks and matrix or
    method spikes.

    10.5.5.3.  Pesticide/PCB - Since GC/EC data is much more subject to
    interference than GC/MS, two surrogate standards are added to each
    sample: Dibutylchlorendate (DEC) and 2,4,5,6-tetrachloro-meta-
    xylene (TCMX).    DEC is the primary surrogate and should be used
    whenever possible.   However,  DEC is subject to acid and base
    degradation so, if DEC recovery is low or compounds interfere with
    DEC, then the TCMX should be evaluated for acceptance.  Proceed
    with corrective action when both surrogates are out of limits for
    a sample.  See below for action on blanks and matrix or method
    spikes.

    10.5.5.4.  At present there are no QC limits for the herbicide and
    organo-nitrogen/phosphorus surrogates.

    10.5.5.5.  Corrective Action

        10.5.5.5.1. Check for instrumental problems and make any
        necessary corrections.  Redilute the extract (if necessary),
        and then rerun the sample.  This also applies to blanks and
        matrix or method spikes.

        10.5.5.5.2. If no instrumental problems exist,  the sample
        should be re-extracted and re-analyzed.  However,  if the
        sample data from the first analysis has to be reported, report
        the data from the first analysis and flag it with a "J".   If
        surrogates  from extractable or pesticide blanks exceed the
        above criteria, but one or more samples in the set have
        acceptable  surrogate limits, evaluate the blanks carefully to
        see if they still provide sufficient information to determine
        the presence of contaminants in the samples. For  matrix or
        method spikes which are already prepared in duplicate,  no re-
        extraction  is required.  If both duplicates are out,
        indicating  a matrix effect, record matrix surrogate recovery
        data for both.

        10.5.5.5.3. If the surrogates are still outside the acceptance
        limits after repurging or re-extraction, the data should be
        reported and flagged with a "J".
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                                                Section:   10
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    10.5.6.  Reporting Surrogate Data
        10.5.6.1.  All surrogate data must be transferred to the computer
        data system except for surrogate data that is known to be in
        error;  i.e.,   acid was not added to water prior to water
        extraction, valve on GPC instrument was leaking caused cross-
        contamination,   purge and trap system contamination,  etc.  DEC
        data whose pH is outside neutral range during extraction or
        cleanup should also not be recorded.

10.6.  Internal  Standards
    10.6.1.  Internal standards,  compounds not expected to occur in an
    environmental sample,  are added to each sample just prior to
    instrumental analysis.

    10.6.2.  Following are  the internal standards and the corresponding
    spike solution concentrations currently used by ASB:
        Semivolatile                Sol'n Cone.
        1,4-Dichlorobenzene-d4      lOOOng/uL
        Naphthalene-dS              lOOOng/uL
        Acenaphthene-dlO            lOOOng/uL
        Phenanthrene-dlO            lOOOng/uL
        Chrysene-dl2                lOOOng/uL
        Perylene-dl2                lOOOng/uL

        Volatiles-Water/Soil/Sed    Sol'n Cone.
                    Amt per Final
                    Extract Volume

                    IQuL/lmL
                    Spike Amt Per
                    Final Volume
        Difluorobenzene
        Chlorobenzene-d5
        1,4-Dichlorobenzene-d4

        Volatiles-Air Canister
Method 8260
modifications
Sol'n Cone.
Method 8260
modifications
Spike Amt Per
Final Volume
        Difluorobenzene
        Chlorobenzene-d5
        1,4-Dichlorobenzene-d4
TO-14
modifications
TO-14
modifications
10.7.  GC Analysis

    10.7.1 GC Screening

        10.7.1.1 It is suggested that a GC Screening of all samples be
        conducted before the GC Analytical run.  The following set-up is an
        example for screening all types of matrices.

            10.7.1.1.1 Begin with an Evaluation Mix and a lOOx dilution of
            the Surrogate standard or the dilution that is required for
            the surrogate to be within the standard curve range.

            10.7.1.1.2 Make a 100X dilution of all extracts and run them
            next including the blank and spike.   Include a standard and an
            Evaluation Mix after each 20 samples.

            10.7.1.1.3 Repeat the 100X dilution of the Surrogate  standard
            at the end of the screening run.
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                                            Section:  10
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    10.7.1.2 This run of 100X dilutions may be used to calculate the
    Surrogate recovery if the following procedures were done:

        10.7.1.2.1 An Evaluation Mix is run both at the beginning and
        at the end of the run.

        10.7.1.2.2 A QC curve of the Surrogate standard is run before
        or immediately after the screening run.

10.7.2. GC Logbook

    10.7.2.1. Be sure all pertinent information requested on the sheet
    is properly recorded.  See Form 10-8.  An analyst should keep
    track of projects on a master log sheet.  See Form 10-10.

    10.7.2.2. All analysts that participated in making dilutions and/
    or loading the auto-sampler must record their names. This includes
    analysts that add extracts at the end of the run to verify or
    check on samples from other sets of samples.

    10.7.2.3. Record inclusive sample numbers for each blank and
    spike.

    10.7.2.4. Record the level of concentration of standard and the
    name of the standard (e.g., Red Pest Mix VI).

    10.7.2.5. Record all information that is needed to identify the
    sample vial (see Table 10-1) .

    10.7.2.6. Record all dilutions with dilution factor, times sign,
    and original volume  (example:  10 X 1 mL or 10,000 X of 25 mL).

    10.7.2.7. A copy of the logbook page should be kept in the project
    file.

10.7.3. Follow the procedure for setting up instruments for data
analysis, i.e., for collecting, processing, analyzing, and reporting
data,   using a PC with a pesticide analysis software program. Make
sure that the correct time and date are on all QC runs and reports.
This can be done by making sure that the processing PC and the
acquiring GC are set to the correct time and date.

    10.7.3.1. Build a new method or edit an existing one that is
    suitable for the analysis as required by the software program
    being used.  This will include developing or updating the
    instrument, processing and calibrating parameters for the method.
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    10.7.3.2.  Create a report format for the method.

    10.7.3.3.  Create a new Sequence file for each GC run.  The
    sequence should include information to identify the sample,  vial,
    and method used.

        10.7.3.3.l.Give the sequence file a singular name associated
        with the project name.

    10.7.3.4.  Download a sequence or method file to the interface.

    10.7.3.5.  Set  the GC conditions for the run and then start the GC
    which will begin data collection.

    10.7.3.6.    After collection, process the data using a pesticide
    analysis software protocol.

    10.7.3.7.  Build summary reports for QC linear curve, surrogate,
    and sample results.

    10.7.3.8.  Archive and back up all files associated with an
    analytical run.

10.7.4. Dilutions  and Sample Vials.

    10.7.4.1.  The  GC chemist is  responsible for all sample extract
    vials received from the extraction lab.  The chemist is
    responsible for the vials until GC analysis is complete,  and the
    vials have been stored in proper order or have been discarded.

    10.7.4.2.  Re-mark all vials  at the meniscus after dilutions  or GC
    analysis.   Do  not allow original vials to remain in auto-samplers
    over the weekend.

    10.7.4.3.  One  sample from every set of samples requiring dilutions
     will be analyzed in duplicate.  Select the sample requiring the
    greatest dilution that has usable data.  If the original  dilution
    was made using the auto-diluter, then its duplicate should be made
    manually,  or by a different  auto-dilute, or by another analyst.

    10.7.4.4.  Record the QC dilutions in the GC Logbook.

    10.7.4.5.  The  duplicate shall be made and analyzed as soon as
    possible after the initial dilutions are analyzed.

    10.7.4.6.  Data from duplicate of the greatest dilution containing
    usable peak(s)  shall agree within 10% RSD.
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                                            Section:   10
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    10.7.4.7.  If data difference is greater than 10%  RSD,  resolve the
     problem before continuing by:

        10.7.4.7.1. Re-diluting the sample extract in  question.

        10.7.4.7.2. If unsatisfactory results are  obtained,  then all
        samples shall be re-diluted from the original  extracts and
        analyzed again.

    10.7.4.8.  The auto-diluter must be rinsed at least 5 times when
    diluting sample extracts known or suspected of containing high
    compound concentrations.  Rinsing 3 times is satisfactory for most
    routine samples.

10.7.5.  Labeling Chromatograms and/or Data Packet.

    10.7.5.1.  The data packet should contain the following
    information: Logbook number and page,  project  name, who  calculated
    the  data,  who checked the calculation, and when and who  recorded
    the  data and QC.

    10.7.5.2.  Individual chromatograms should contain  information to
    identify the sample analyzed,  volume and dilutions, and
    calculations used.

    10.7.5.3.  Do not erase or use  "Liquid Paper" to correct  any
    errors.  Put one line through  the error with initials  and date.

10.7.6.  Retention Time (RT)  Windows

    10.7.6.1.  Retention time window size

        10.7.6.1.1.  Make a minimum of 1 injection of  all  single
        component mixtures,  multi-response pesticides, and PCBs  at 24-
        hour intervals throughout  the course of a  72-hour  (3 days)
        period.  However, 1 injection at 24-hour intervals throughout
        the course of a 120-hour (5 day)  period is preferred.

        10.7.6.1.2.  Calculate the standard deviation  of three
        (preferably five) absolute retention times for each  single
        component pesticide.  For  multi-response pesticides/PCBs,
        choose one major peak from the group of peaks  and  calculate
        the standard deviation of  the retention time  of that peak.

        10.7.6.1.3.  Three times the standard deviation of the
        retention time for each pesticide/PCB will be  used to
        establish the retention time window or, (+/-)  0.03 min for
        capillary columns; however, the experience of  the  analyst
        should weigh heavily in the interpretation of  chromatograms.
        For multi-response pesticides/PCBs, the analyst should utilize
        the retention time window  but should primarily rely  on pattern
        recognition.  If the standard deviation of any compound is
        zero,  use the standard deviation of any compound near the same
        retention time.

        10.7.6.1.4. The laboratory must calculate  retention  time
        windows for each pesticide/PCB on each GC  column used at the
        beginning of any new GC instrument setup or whenever a new GC
        column is installed.

    10.7.6.2.  Daily retention time windows
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                                            Section:   10
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        10.7.6.2.1.  Inject all individual standard mixes and all
        multi-response pesticides/PCBs.   To establish  the RT window
        for the  pesticides/PCBs of interest,  use  the  absolute RT from
        the above chromatograms as the midpoint,  and (+/-)  three times
        the standard deviation calculated in Section 10.7.5.1.3. as
        the range or (+/-) 0.03 min for capillary  columns.

        10.7.6.2.2.  Intersperse a standard mixture after every 20
        samples but  no less than every 12 hours as a minimum to verify
        that standard retention times are falling  within the windows.
         Any pesticide outside of its established  time window requires
        immediate investigation and correction before  continuing the
        analysis.  New absolute retention time windows must be
        established, unless instrument maintenance corrects the
        problem.  Then re-inject all samples following the last
        standard meeting the criteria.  If no target compounds are
        present in the samples, and the surrogate   recovery is within
        limits, no re-injection is necessary  and  MQLS may be
        calculated.

10.7.7.  Calibration

    10.7.7.1. The gas chromatographic system should be calibrated
    using the external standard technique for all  columns used for
    quantitation and after a new column is installed.

        10.7.7.1.1.  Prepare calibration standards  at a minimum of
        three concentration levels (preferably five)  for each compound
        of interest.  One level of the external standards should be at
        a concentration near,  but above,  the MDL and the other
        concentrations should define the working range of the
        detector.  This should be done on each quantitation column,
        each new instrument, and whenever the new  calibration
        verification standard falls outside of accepted criteria.  See
        SW-846, 8000 methods.  See Table 10-2.

        10.7.7.1.2.  Using injections of 1 to 5 uL  of each calibration
        standard, tabulate peak height or area responses against
        amount injected.  The results can be used  to prepare a
        calibration curve for each compound.

        10.7.7.1.3.   If the run is for confirmation (no quantitation)
        or for MQLs, the linearity check is not required.  For MQLs,
        however, a standard at the MQL level of QC-1 is required.
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                                            Section:  10
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        10.7.7.1.4.  The %RSD is calculated on representative compounds
        of interest  (e.g.,  Lindane,  Endrin,  p,p'-DDT, and
        Methoxychlor).   If  the %RSD is (
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                                        Section:  10
                                        Revision: 1
                                        Date: December 1, 1997
                                        Page:  14

Percent BD   =  Total  DDT degradation peak area  (DDE + ODD)  x 100
for 4,4'-DDT     Total DDT peak area  (DDT + DDE + ODD)

Percent BD for Endrin =

Total Endrin degradation peak areas  (E. Aid. + E. Ketone) x 100
Total Endrin Peak Area (Endrin + E. Aldehyde + E. Ketone)

See suggested maintenance in Section 10.7.8. if degradation
exceeds 20%.

10.7.8.3. All calculations for percent breakdown must be part of
the data package.

10.7.8.4. For calibration verification target analytes required in
the project plan must be injected at the beginning of each 12 hour
period with the following exception for the Aroclors.  For sites
that require PCB analysis include only the Aroclors that are
expected to be found at the site.  If PCBs are required but it is
unknown which Aroclors may be present, the mid-concentration
Aroclors 1242/1260 mixture only need be injected.  However, if
specific Aroclors are found at the site during the initial
screening, it is required that the samples containing Aroclors be
reinjected with the proper mid-concentration Aroclor standards.
See SW-846, 8000 methods.

10.7.8.5. Intersperse a mid-point calibration standard after every
 20 samples but no less than every 12 hours as a minimum. It is
recommended that a calibration standard be included after every 10
samples for highly contaminated samples to minimize the number of
repeat injections.  The calibration factor of a specific standard
compound shall not exceed a 20% difference from the initial
    response when screening samples or more than  (+/-) 15% for any
 standard used for quantitating.  When one or more of the
compounds are greater than +/- 15%, take the average % of all
compounds.  If the average % is less than +/- 15%, the calibration
verification is considered acceptable.  See SW-846, 8000 methods.

                    Calibration Factor =    Total Response of
Peak*                                   Amount injected  (in
nanograms)
               *For multi-response pesticides/PCBs use the
response of the major peaks used for quantitation.

            Percent Difference= R1-R2  X 100
                             Rl
    Where   Rl = Calibration Factor from first analysis and
        R2 = Calibration Factor from succeeding analysis.

    10.7.8.5.1. All calculations for percent difference must be
    included in the data package.
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    10.7.8.6.  Check retention time windows by analyzing a calibration
    standard after every 20 samples but no less than every 12  hours
    and compare it to the standard at the beginning of the 12  hour
    shift.  If  retention time is outside of calibrated window (see
    10.7.6.2.)  (+/- .03min or 3 standard deviations) check the GC for
    problem (i.e., septum and/or column leaks,  bad syringe,  etc.)

    10.7.8.7.  Check for peak tailing and take corrective action if
    necessary.

    10.7.8.8.  The %RSD may be calculated using 3 to 5 concentration
    levels.  However,  any peaks quantitated must fall within the
    linear range and the required minimum quantitation limits  must be
    met.  The calculation for % RSD for the representative compounds
    must  be included in the chromatogram package.

10.7.9. Suggested Maintenance

    10.7.9.1.  Corrective measures may require any one or more  of the
    following  remedial actions:

        10.7.9.1.1. Capillary columns-Turn off both oven and injection
        ports.   Clean and deactivate the glass  injector port  insert
        or replace with a cleaned and deactivated insert.  Remove the
        analytical column when the oven has cooled.  Break off the
        first  few inches of the column (up to one foot)  on the
        injector port side and then reconnect the column.  If  these
        procedures fail to eliminate the degradation problem,  it may
        be necessary to deactivate the metal injector body and/or
        replace the column.

        10.7.9.1.2. Metal Injector Port-Turn off the oven and
        injection port heaters and remove the analytical column when
        the oven and the injection port heaters have cooled.  Remove
        the glass injection port insert (in instruments with off-
        column injection).   Inspect the injection port and removed any
        noticeable foreign material.

            10.7.9.1.2.1. Place a beaker beneath the injector  port
            inside the GC oven.  Using a wash bottle, serially rinse
            the entire inside of the injector port with acetone,
            toluene and then iso-octane,  catching the rinsate  in the
            beaker.

            10.7.9.1.2.2. Use a solution of deactivating agent  (Sylon-
            CT or its equivalent) following manufacturer's directions.
            After all metal surfaces inside the injector body have
            been thoroughly coated with the deactivation solution,
            serially rinse the injector body with toluene, methanol,
            acetone, and hexane.  Reassemble the injector and
            reconnect the column.
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10.7.10. Qualitative Analysis
    10.7.10.1. Identification of compounds by retention times must be
     performed by experienced gas chromatographers because slight
    shifts in retention times require judgment  decisions.  Observe
    retention time shifts of standards throughout a day's run to
    evaluate retention time shifts in samples. Utilize the daily
    retention time windows for compound identification.

    10.7.10.2. Confirm all compounds  (pesticides/PCBs) on a second
    different column, or different detector (other than  FID),  unless
    the compound has been confirmed by GC/MS.

    10.7.10.3. It is suggested that at least one sample from a set be
    confirmed by  GC/MS, if concentration permits.  It is the
    responsibility of the GC analyst to report any  pesticides/PCBs
    confirmed by GC/MS.  This must be properly noted on the data
    sheet.  Confirmation by GC/MS is shown by adding the letter C to
    the amount of the compound being reported.  Alpha-BHC, gamma-BHC,
     Endosulfan I and II, and Endrin must be confirmed on the
    pesticide extract from water rather than the BNA extract  (these
    compounds are unstable at the basic pH).

    10.7.10.4. Reporting Chlordane-Weathering and/or different
    fomulations of chlordane may modify the technical chlordane
    pattern.  If the chlordane pattern in a sample is similar to
    technical chlordane, use a technical chlordane standard for
    quantitation.  ("similar" means all constituents are present,
    including heptachlor, in about the same ratio as a standard of
    technical chlordane.) If the pattern is different but gamma and
    alpha chlordane and other chlordane constituents are present, use
    the individual chlordane constituent standards for calculation.
    Report the individual constituents on the data reporting sheet.
    Report a total of all constituents listed on the data sheet,
    except heptachlor, when the total is requested.  Heptachlor is
    reported separately in these situations.

10.7.11. Calculation and Project Wrap-up (Also see Section 10.11 on
Data Reporting)

    10.7.11.1. For calculation of components in a sample two options
    are available:

        10.7.11.1.1.  Use a one-point mid-level red mix standard either
        manually or by acceptable computer program; or,

        10.7.11.1.2.  Use a three (preferably five)-point linear curve
        by acceptable computer program.

        10.7.11.1.3.  For samples with no analytes found use the MQL
        guidelines for different matrices.   See Form 10-16.
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10.7.11.2. To simplify the checking of calculations, everyone may
use the formulas for calculating concentrations:

For response factor (K):
	uL injected	X (mL, mg or gm extracted) = K
(Volume extract in uL) (dilution)

For amount in sample:

Pk ht or area of sample X(ul inj)(cone.of std.,ng/ul)
Pk ht or area of std.          K                  = Concentration

10.7.11.3. Calculation of off-scale peaks using peak height or
area is allowable if it has been shown that response is linear in
the concentration range of the off-scale peak and no interfering
or rising baseline exists.

10.7.11.4. All calculations must be checked by someone other than
the person who performed the original calculation.  The
chromatogram with the appropriate standards and QC showing the
calculations for the reported data should be given to the checker.
 A hardcopy of the chromatogram should be put in the project file.

10.7.11.5. The checker should check for accuracy of the
transcription of data to the data report sheets.

10.7.11.6. Diluted samples and all standards should be discarded
at the completion of each project.

10.7.11.7.  All vials that are ready for disposal should be placed
in a waste safety can, keeping vials with PCBs in a separate waste
safety can.  These vials must be treated as hazardous waste and
disposed of accordingly.  (See Section 4.6.)

10.7.11.8. All original sample vials should be stored in vial
storage boxes in a refrigerator and placed in a secure area for
permanent storage after completion of analysis.  See Section 10.9.
for instructions on vial storage.

10.7.11.9. The project chemist is responsible for calculating
surrogate and matrix spike recoveries and recording the results on
the appropriate data sheets and/or transmitting all results to the
proper computer data system.  Unusual results on QC data should be
reported to a pesticides' senior staff specialist.  See Forms 10-
11, 10-12, 10-13, and 10-14.

10.7.11.10. Samples having greater than or equal to 50 ppm PCBs
should be reported to the extraction lab Senior staff specialist.
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10.8.  GC/MS ANALYSIS

    10.8.1. GC Screen and GC/MS Logbook

        10.8.1.1. Record all pertinent information requested on the
        logbook sheet. The electronic version of these forms are available
        from the forms custodian.  The designated person at this time is
        Sallie Hale.  See Forms 10-4 and 10-5.

        10.8.1.2. Record file name under sample number column as it exists
        on the disk.

    10.8.2. GC Screen

        10.8.2.1. Volatile Organics

            10.8.2.1.1. All samples may be screened by GC/PID/ELCD to
            determine the approximate concentration level prior to GC/MS
            analysis.  Dilutions for GC/MS analysis are to be determined
            from this screen analysis.

        10.8.2.2. Semivolatile Organics

            10.8.2.2.1. All samples may be screened by GC/FID, GC/ELCD,
            GC/PID,  or any combination of these necessary to determine the
            approximate concentration level prior to GC/MS analysis.
            Dilutions for GC/MS analysis are to be determined from this
            screen analysis.

    10.8.3. File Name Labeling

        10.8.3.1. Use the following format for file names for volatile
        blanks and standards.

            10.8.3.1.1. S0128R1 - Rl  (or R2,  R3,  ect.)  represents the
            standard run number, B for blanks, followed by date of ana-
            lysis .

        10.8.3.2. Use the following format for file names for semivolatile
        blanks.

            10.8.3.2.1. B00736SLW    - B for blank, followed by ASB log
            number for first sample in the set that blank applies to,
            followed by appropriate analysis designations.

        10.8.3.3. Use the following format for file names for semivolatile
        standards.

            10.8.3.3.1. S01997SLW - Surrogate standard. S for standard,
            followed by ASB log number for first sample in the set that
            standard applies to, followed by appropriate analysis
            designations, followed by the day of the month if the
            instrument allows that length for file names.
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        10.8.3.3.2. S093020 -  First four digits date designations,
        followed by concentration level in ng/ul.  Surrogate compounds
        are normally included in the daily standard.

    10.8.3.4. Sample file name.  Use the ASB log number followed by
    the proper analytical descriptor if the instrument allows that
    length for file names  (ie 42361SLW).  See Table 10-1.

    10.8.3.5. Current instrument designations are:

            50  -  INCOS 50 - EPA
            52  -  INCOS 50 - EPA
            53  -  INCOS 500 - EPA
            71  -  HP5971 - EPA - VGA
            72  -  HP5972 - EPA - VGA
            73S -  HP5973 - ESAT - BNA
            73B -  HP5973 - ESAT - VGA
            73A -  HP5973 - EPA - BNA

    10.8.3.6. Add the following designations between the SESD number
    and the analytical descriptor   (ie. 40849XDSLS):

        10.8.3.6.1. X and Y - for duplicates.

        10.8.3.6.2. D - Dilution (Indicate D2,  D3, etc. for subsequent
        dilutions)

        10.8.3.6.3. R, RS,  R3, etc. - Designates a re-extraction of a
        sample or reinjection or a purging of a replicate VGA sample.

        10.8.3.6.4. If other designations are needed, record their
        meaning in logbook.

    10.8.3.7. NOTE: Some software may limit the file name to eight
    characters.

10.8.4. Title Information as Follows:

    10.8.4.1. File name.

    10.8.4.2. Instrument designation.

    10.8.4.3. Sample volume information (including dilution
    information).

    10.8.4.4. GC Column type and conditions as 50-210 X 8, 12 F12
    where 50-210 are initial and final temperatures, X8 is program
    rate, 12 is initial hold time,  F12 is final hold time.
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10.8.5.  Mass Scale Calibration Using FC43

    10.8.5.1.  Tune instrument using the following guidance:

        10.8.5.1.1. Admit FC43 with carrier flow entering source as
        appropriate for the individual instrument.

        10.8.5.1.2. Adjust resolution to achieve the desired
        parameters.

        10.8.5.1.3. Make appropriate tuning adjustments to achieve the
        following ion intensity ratios as nearly as possible.

                Mass 219 15-40% of Mass 69

                Mass 220  > Mass of 70

                Mass 414 50-125% of Mass 220 (for semi-volatiles)

                Mass 131 + 80-120%of Mass 219

    10.8.5.2.  Acquire at least 5 scans of FC43  data scanning a mass
    range of 20-650 amu (or as appropriate).

    10.8.5.3.  Run calibration routine.

    10.8.5.4.  Instrument should calibrate from at least 28 - 502 amu.

10.8.6.   Zero the Instrument

    10.8.6.1.  Set instrument zero consistent with manufacturer's
    specifications and/or to a proven, reliable setting (if this is
    necessary).

10.8.7.  Instrument Tuning Performance Test

    10.8.7.1.  A tune performance check must be  performed every 12
    hours during analysis.

    10.8.7.2.  Analyze 50 ng of Decafluorotriphenylphosphine (DFTPP)
    for extractables or 50 ng of p-Bromofluorobenzene (BFB) for
    volatiles.

    10.8.7.3.  Other concentrations or compounds may be used as
    required by the analytical protocols.

    10.8.7.4.  Operating Conditions

            10.8.7.4.0.1.  Mass Spectrometer parameters same as
            analysis planned for the twelve hour shift.

            10.8.7.4.0.2.  The reference compound should elute so that
            compounds of interest are resolved.
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        10.8.7.4.1.  The mass spectrum must be acquired in the
        following manner:  Three scans (the peak apex scan and the
        scans immediately preceding and following the apex)  are
        acquired and averaged.   Background subtraction is required,
        and must be  accomplished using a single scan within 10 scans
        prior to the beginning of elution of the performance compound.

        10.8.7.4.2.  Compare the ion intensity ratio of those of
        published criteria.

        10.8.7.4.3.  If the required criteria are not met, the
        instrument must be retuned until the spectra meets the
        specified criteria.

        10.8.7.4.4.  Check retention time and peak shape of reference
        compound to  determine if they are consistent with prior
        results.

        10.8.7.4.5.  Check the peak intensity (by peak height or area)
        to determine if the sensitivity is adequate.

        10.8.7.4.6.  Print a list of masses and intensities,  a copy of
        the chromatogram with areas of each peak printed, and maintain
        in a folder.

10.8.8.  GC/MS Linearity Check

    10.8.8.1. Initial Calibration

        10.8.8.1.1.  The GC/MS system must be initially calibrated with
        all compounds of interest at a minimum of three concentrations
        (5 levels are recommended).  Using the response factors (RF)
        from the initial calibration, calculate the percent relative
        standard deviations (% RSD)  for all compounds.

            10.8.8.1.1.1.  A system performance check must be met for
            all compounds. A minimum response factor of 0.100 for the
            volatile compounds and 0.05 for the semivolatile compounds
            is required. If this criteria is not met, corrective
            action must be taken.

            10.8.8.1.1.2.  The % RSD for each compound must be less
            than 15  percent. If this criteria is not met, corrective
            action must be taken. This might require instrument
            maintenance, new standards preparation, and/or repeating
            the analysis of the curve.  If after corrective action
            some compounds exceed 15 percent, the analyst may proceed,
            but any  positive results for these compounds must be
            reported with a J flag.

                10.8.8.1.1.2.1. Thirty percent RSD is acceptable for
                the  following semivolatile compounds: 4-nitrophenol,
                4-chloro-3-methylphenol, 2,4-dinitrophenol,  2-
                methyl,4,6-dinitrophenol, pentachlorophenol, 3,3-
                dichlorobenzidine,  2-nitroaniline, 3-nitroaniline, 4-
                nitroaniline.   Thirty percent RSD is acceptable for
                the following purgeable compounds: vinylchloride,  1,1-
                dichlorothene,  chloroform,  1,2-dichloropropane,
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            toluene,  and ethylbenzene.   If these  analytes  are of
            specific  importance to the  project,  corrective action
            may be necessary.   Otherwise,  these compounds  must be
            flagged as estimated (J)  if the %RSD  is greater than
            15%.

            10.8.8.1.1.2.2.  The RF for  each compound in each
            concentration level of the  curve must  be compared to
            the average RF of  the curve to determine if any
            individual point on the curve  is an outlier.  Calculate
            the percent difference between the average response
            factor from the curve and the  response factor  from the
            individual concentration level in the  curve.  If the
            percent difference for any  compound is greater than
            25%, corrective action may  be  necessary. This  usually
            means re-analyzing the bad  point on the curve.

10.8.8.2.  Daily Calibration Check

    10.8.8.2.1. A standard mixture containing all  volatile or
    semivolatile compounds of  interest  must be analyzed every 12
    hours  of operation.

        10.8.8.2.1.1.  A system performance check  must be met for
        all compounds. A minimum response  factor  of 0.100  for the
        volatile compounds and 0.05 for the semivolatile compounds
        is required.  If this criteria is not met,  corrective
        action must be taken.

        10.8.8.2.1.2.  A calibration check  of the  initial
        calibration curve is made for each target  compound.
        Calculate the  percent  difference between  the average
        response factor from the initial calibration and the
        response factor from the current standard. If the  percent
        difference for any compound is  greater than 25%,
        corrective action may  be necessary. The analyst must
        immediately judge the  impact on the data  generated for
        that day.  Any compounds with %D greater  than 25%  should
        be flagged as  estimated (J).  If more than  25% of the
        compounds are  greater  than 25%D, corrective action must be
        taken.  This  may require generation of a  new curve.
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                      Difference  =  RF:-  RFc   X  100
                                        RF:


                RFj  - Average  response  factor  for  initial  curve

                RFc  -  Response factor from current standard mixture

            10.8.8.2.1.3.  Continuing without corrective action may be
            prudent  if the outlier compounds are not of interest to
            the project.  The Senior Staff Specialist or Organic
            Section  Coach must be consulted before continuing without
            corrective action. In this case, the corrective action may
            be to report  these compounds as not analyzed or with an
            estimated  flag.

            10.8.8.2.1.4.  A file of the results from the initial and
            continuing calibration checks must be maintained.
            Continuing calibration files are part of the daily
            standard chromatograms and are to be filed with the
            appropriate project.

10.8.9.  Analyze Standard Mixture

    10.8.9.1.  Analyze  standard mixtures and performance compounds at
    least every 12 hours  (purgeable standards should be at room
    temperature before analysis).

    10.8.9.2.  Use GC conditions and MS parameters consistent with
    sensitivity requirements and equal to those planned for the
    shift's operations.

    10.8.9.3.  Incorporate internal standards where feasible.

    10.8.9.4.  Perform  system performance check and daily calibration
    check.

    10.8.9.5.  Record area count of the quantitation ion for at least
    one  of  the internal standards.

    10.8.9.6.  The surrogate standard is normally part of the BNA
    standard.

10.8.10. Analyze Laboratory Blank

    10.8.10.1. Utilize internal standards where feasible.

    10.8.10.2. Record  integrations for the same internal standards
    recorded in standard.
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        10.8.10.2.1. If the area count is not within - 50% to + 100%
        of those in Standard Mixture, rerun.

        10.8.10.2.2. Internal standard retention times must be within
        +_ 10 scans or 10 seconds of standard, whichever is greater.

    10.8.10.3. Check for carryover from standard injection.

    10.8.10.4. Compute surrogate recovery.

    10.8.10.5. Section 10.11.3 gives further guidance on use of
    blanks.

10.8.11. Analyze Samples

    10.8.11.1. If area count of internal standard is not within - 50%
    to +100% of the standard, rerun.

    10.8.11.2. Internal standard retention times must be within +_ 10
    scans or 30 seconds of standard, whichever is greater.

    10.8.11.3. Disperse field or lab blanks throughout the day as
    necessary.

    10.8.11.4. Disperse standard mixtures between at least every 12
    hours of analysis.

    10.8.11.5. Utilize internal standard where feasible.

    10.8.11.6. Compute surrogate recovery and record in GC/MS Log.

10.8.12. Analyze at least one check sample monthly.

10.8.13. Drinking water samples with positive results should be
verified by analyzing a replicate sample whenever possible.  The
Senior Staff Specialist or Organic Section Chief should be contacted
if deviations from this policy are necessary.

10.8.14. TCLP analysis: The GC/MS data generated for VGA,  BNA, and
Pesticide analysis is reviewed with the Extraction Laboratory Chemist
and a decision made whether any samples could fail the TCLP test.  If
it potentially could fail, then the TCLP test is performed and the
results reported.  If the sample cannot fail the test, this
information is reported.

10.8.15. Data Processing

    10.8.15.1. Plot total ion current profiles.

    10.8.15.2. Using the peak finding algorithm and the total ion
    current profile, place scan numbers in scan list. The parameters
    should be set to find all peaks at approximately 10% of instrument
    MQL (This is usually set to 10% of the area of an internal
    standard response.)
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    10.8.15.3.  Print a copy of spectra and library search (best 3
    match graph,  ranked on purity).   Use both NIST and Wiley library
    in search if  available.

        10.8.15.3.1. If peaks are asymmetrical,  print  a spectra with
        the background manually subtracted.

    10.8.15.4.  Compare the spectra of the unknown with the 3 best
    matches and see if one is a logical match.

    10.8.15.5.  Check for presence of molecular ion and isotopic
    clusters.

    10.8.15.6.  Check the data printed with the best entries from the
    library search as an aid to the visual comparison  of an unknown
    spectra to the library spectra.

    10.8.15.7.  If no reasonable match, check other published data
    bases,  as needed.

10.8.16.  Qualitative Analysis

    10.8.16.1.  Target compounds shall be identified by comparison of
    the sample mass spectrum to the mass spectrum of a standard of a
    reference spectra of suspected compound.  Two criteria must be
    satisfied to  verify the identifications:  (1)  elution of the
    sample component at the same GC relative retention time as the
    standard component, and (2) correspondence of the  sample component
    and standard  component mass spectra.

        10.8.16.1.1. For establishing correspondence of the GC
        relative  retention time (RRT) , the sample component RRT must
        compare within -F 0.06 RRT units of the RRT of  the standard
        component.  For reference,  the standard must be run within 12
        hours of  the sample.  The RRT should be assigned by using
        extracted ion current profiles for ions unique to the
        component of interest.

        10.8.16.1.2. The requirements for qualitative  verification by
        comparison of mass spectra are as follows:

            10.8.16.1.2.1. All ions present  in the standards mass
            spectra at a relative intensity  greater than 10% (most
            abundant ion in the spectrum equals 100%)  must be  present
            in the sample spectrum.

            10.8.16.1.2.2. The relative intensities of ions specified
            above must agree within plus or  minus 20%  between  the
            standard and sample spectra.  (Example: For an ion with an
            abundance of 50% in the standard spectra,  the
            corresponding sample ion abundance must be between 30 and
            70 percent.)
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        10.8.16.1.2.3. Ions greater than 10% intensity in the
        sample spectrum but not present in the standard spectrum
        must be considered and accounted for by the analyst making
        the comparison.  Do not report any compounds with a
        calculated value below 0.1 of the MQL.

10.8.16.2. A library search shall be executed for Non-Target
sample components for tentative identification.  The most recent
available version of the NIST and Wiley Mass Spectral Libraries
should be used.

    10.8.16.2.1.  Do not report any compounds with a calculated
    value below the MQL.  Only after visual comparison of sample
    spectra with the nearest library searches will the mass
    spectral interpretation specialist assign a tentative
    identification.  Computer generated library search routines
    should not use normalization routines that would misrepresent
    the library or unknown spectra when compared to each other.

    10.8.16.2.2.  Guidelines for making tentative identification:

        10.8.16.2.2.1. Relative intensities of major ions of the
        reference spectrum (ions greater than 10% intensity of the
        most abundant ion)  should be present in the sample
        spectrum.

        10.8.16.2.2.2. The relative intensities of the major ions
        should agree within •+• 20%.  (Example:  For an ion with an
        abundance of 50% in the standard spectra, the
        corresponding sample ion abundance must be between 30 and
        70 percent.

        10.8.16.2.2.3. Molecular ions present in reference
        spectrum should be present in sample spectrum.

        10.8.16.2.2.4. Ions present in the sample spectrum but not
        in the reference spectrum should be reviewed for possible
        background contamination or presence of coeluting
        compounds.

        10.8.16.2.2.5. Ions present in the reference spectrum but
        not in the sample spectrum should be reviewed for possible
        subtraction from the sample spectrum because of background
        contamination of coeluting compounds.  Data system library
        reduction programs can sometimes create these
        discrepancies.

        10.8.16.2.2.6. If in the opinion of the mass spectral
        specialist, no valid tentative identification can be made,
        the compound should be reported as unidentified compound.
         The mass spectral specialist may give additional
        classification of the unknown compound, if possible (i.e.
        unknown phthalate,  unknown hydrocarbon, unknown acid type,
        unknown chlorinated compound).
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            10.8.16.2.2.7. Non-Target compounds identified in samples
            will be reported using the NIST and Wiley Libraries name
            of the best probable match.  The best probable match is
            selected by the mass spectroscopist from the best matches
            as chosen by the library search routine ranked by purity.
             The analysts interpretation may supersede the computer
            matching algorithm.

            10.8.16.2.2.8. The NIST or Wiley Library nomenclature
            should be stripped of numbers or letters that would make
            the reported compound a specific isomer  (e.g.  1,2-
            dibromoethane should be reported as dibromoethane).

            10.8.16.2.2.9. Where more than one isomer of a compound is
            identified, they should be reported under one name.  The
            total concentration should be reported with this one name
            and the number of isomers should be reported in paren-
            thesis.  The isomer name chosen for one sample of a
            project should be used in all samples for the project,
            where no distinguishable spectral differences are present
            (e.g.  If the best match for C3alkyl  benzenes is  methyl
            ethyl benzene instead of trimethyl benzene, or propyl
            benzene, report as methyl ethyl benzene in all samples of
            the project where this is true).

            10.8.16.2.2.10. Name alkyl substituted analogs of Target
            compound isomers using the earlier eluting of the
            isomers(e.g. methylfluoranthene, not methylpyrene).

10.8.17.  Quantitation

    10.8.17.1. Target components identified shall be quantified by the
    internal standard method. The internal standard used shall  be the
    one nearest the retention time to that of a given analyte.   The
    EICP area of characteristic ions of analytes are used.  The
    response factor (RF) from the daily standard analysis is used to
    calculate the concentration in the sample.  Secondary ions  may be
    used if interferences are present.  The area of a secondary ion
    cannot be substituted for the area of a primary ion unless  a
    response factor is calculated using the secondary ion.

        10.8.17.1.1. Any compound that had a %RSD in RF of greater
        than 30 in the initial calibration curve must be reported with
        an estimated value flag (J).  Similarly,  any compound that had
        a % difference in RF of greater than 25 between the RF  from
        daily standard mixture and the average RF from the initial
        curve must be reported with an estimated value flag  (J) .

    10.8.17.2. An estimated concentration for Non-Target components
    tentatively identified shall be quantified by comparison to an
    internal standard free of interferences. The following order of
    preference for internal standards to use as a reference for
    extractables is D10Phenanthrene, D8Naphthalene,  D10Acenaphthylene,
    D12Chrysene, D12Perylene,  and D4 Dichlorobenzene.  The internal
    standard nearest in retention time to the Non-Target compound may
    be used to estimate concentration.  Total area counts or peak
    heights from the total ion chromatograms are to be used for both
    the compound to be measured and the internal standard. A RF of one
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    (1)  is to be assumed.   The value from this quantitation shall be
    qualified as estimated.  This estimated concentration should be
    calculated for all tentatively identified compounds as well as
    those identified as unknowns.

10.8.18.  GC/MS Data Transfer

    10.8.18.1.  Initial Reports - After the data is processed by the
    GC/MS data system, it  is transferred to another computer.   The
    data  is then adjusted  taking into account sample dilution,  amount
    purged or extracted,  and dry weight, when applicable.  Hard-copies
    are then produced.  After corrections or additions are made to the
    data  based on further  analysis of the chromatograms and mass
    spectra, the final data product is transferred to  the R4LIMS
    computer.

    10.8.18.2.  Final Reports

        10.8.18.2.1.  When no more alterations are necessary,  the
        final data can be  transferred to the R4LIMS system.

        10.8.18.2.2. The data is then printed out  in final production
        format and proofed for errors.  Any corrections are made and
        the corrected data sheet is printed.  A memo is also printed,
        the appropriate number of copies (include  one  file copy)  are
        made and the report is signed by the project chemist and given
        to the Organic Section Chief for review.

10.8.19.  Archiving Data

    10.8.19.1. All samples and standards must be archived by copying
    to nine-track mag tapes using the EPA program  or using other
    electronic storage devices.

10.8.20.  General Responsibilities

    10.8.20.1. The GC/MS chemist is responsible for verifying that all
    sample extract vials were received from the extraction lab or GC
    analyst.  The chemist  is then responsible for  the  vials until
    GC/MS analysis is complete, and the vials have been stored or have
    been  discarded. The extract vials should be stored in the
    refrigerator designated for semivolatile extracts  when not in use.

    10.8.20.2. Recap all vials that are to be retained as soon as pos-
    sible after puncturing the septum.  Remark the volume on the vial
    label after injection  or dilution.

    10.8.20.3. Diluted samples and standards should be discarded
    immediately following  injection to avoid unnecessarily cluttering
    up the lab and extract boards.
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        10.8.20.4.  All vials that are ready for disposal  should be placed
        in the "Oily Waste Safety Can."  Vials must be disposed of
        according to the procedures outlined in Section 4.6.  Dispose of
        standard and sample vials containing PCB's and other listed
        compounds in a separate waste container.

        10.8.20.5.  All original sample vials are placed in boxes and are
        to be stored in a  locked custody room upon completion of
        analysis.  See Section 10.9 for instructions on vial storage.

        10.8.20.6.  The project chemist is responsible for  calculating
        surrogate and matrix spike recoveries and recording the results on
        the appropriate computer data sheet. Unusual results on QC data
        should be reported to the Senior Staff Specialist  and/or the
        Organic Section Chief.

        10.8.20.7.  GC/MS Files - Chromatograms should be  filed numerically
        according to sample numbers.  Files should be labeled with the
        series of sample numbers on first line.  Project  name(s)  should be
        listed under this.  Chromatograms and each file should be  arranged
        as follows:

            10.8.20.7.1. Extraction sheets and data sheets.

            10.8.20.7.2. Standards analyzed in order of date run.

            10.8.20.7.3. Blanks analyzed in order of date  run or sample #
            of blank series.

            10.8.20.7.4. Samples analyzed in numerical order.

            10.8.20.7.5. Pertinent GC screening Chromatograms.

        10.8.20.8.  Any pesticides/PCBs confirmed by GC/MS  must be  reported
        to the Pesticides Senior Staff Specialist to be noted on the
        pesticide/PCB data sheet. Chromatograms from Pesticide and PCB
        confirmation are sent to the GC unit to file with  their
        Chromatograms.

        10.8.20.9.  Keep GC screen Chromatograms for samples that did not
        require GC/MS analysis.  All other GC screen Chromatograms should
        be discarded.

10.9.  Extract Storage

    10.9.1. Sample  extracts are to be stored in storage containers after
    final reporting of data.  These containers will be kept in their
    respective areas of the GC Lab and the GC/MS Lab in a  refrigerator,
    based on the type of sample.  As soon as possible, the containers
    should be disposed of.  Some criminal and other samples may need to be
    stored for extended periods of time.  The sample storage custodian
    will furnish information on disposition of samples in  a timely manner.
     Record sample  extracts placed in storage containers  on Form 10-17.
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10.10.  Preparation,  Storage,  and Use of Organic Analytical Standards

    10.10.1.  Standard Sources

        10.10.1.1.  Primary Standards: Commercial sources are available,
        request the  purest grade available.

            10.10.1.1.1.  Prepared standards: Commercial sources.

            10.10.1.1.2.  QC Standards: second source other than primary
            standards.

            10.10.1.1.3.  Prepared standards: commercial.  Commercially
            prepared stock standards can be used at any concentration if
            they are certified by the manufacturer or by an independent
            source.   If the purity of these standards is questionable,
            report  the  data based on these standards as estimated.

    10.10.2.  Glassware, Equipment, and Solvents:

        10.10.2.1. Analytical balance, capable of an accuracy of +_ 0.1 mg.

        10.10.2.2.  Spatula, stainless steel.

        10.10.2.3.  Transfer class "A" pipets and Pasteur disposable pipets
        or suitable  syringes.

        10.10.2.4.  Flasks, volumetric, 25, 50, 100 and 200 mL.

        10.10.2.5.  Bottles, Teflon-lined caps 60 mL.

        10.10.2.6.  Small  glass funnels, and bent paper clip.

        10.10.2.7.  Refrigerator, explosion-proof.

        10.10.2.8.  Pesticide grade solvents:  ethyl acetate, toluene,
        acetone, isooctane, hexane,  methanol, and carbon disulfide.

    10.10.3.  Safety  Precautions and Operating Procedures

        10.10.3.1.  Gloves should be used when handling reference
        materials.

        10.10.3.2.  Standards used for quantitating samples are to be made
        by a chemist.

        10.10.3.3.  Hoods  should be used when weighing toxic standards or
        diluting with organic solvents.

        10.10.3.4.  Rinse  all glassware prior to use with methanol,
        acetone, and isooctane and let air dry in hood.

        10.10.3.5. Always perform a balance check with Class-S weights
        each day the balance is used.  Record the balance check on the
        Standard Sheet.  Check calculations on solutions to be made up.
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    10.10.3.6.  Do not store any standards in volumetric glassware.
    Transfer to a 60-mL screwcap bottle with Teflon8 liner if  the
    solution is to be stored.   Use phosphate tubes or vials,  with
    TeflonR  liners,  for short  term storage.  All  standards  must be
    properly labeled.

    10.10.3.7.  Always rinse used glassware with acetone before washing
    in dishwasher with other glassware.  Rinse pipets out  with acetone
    immediately after use.

    10.10.3.8.  Keep all standards in refrigerator or freezer when not
    in use.

    10.10.3.9.  Always let standards and solutions come to  room
    temperature before opening.

    10.10.3.10. Check new working standard against old standard.  Old
    standard may be slightly more concentrated due to evaporation of
    solvent  from repeated openings.

    10.10.3.11. Transfer waste standards to a waste bottle.  Rinse the
    empty bottle several times with acetone.  Add the rinsate to the
    waste bottle and discard the standard bottle.

    10.10.3.12. Provide a large waste beaker located in a  hood for
    rinsing  all used glassware and pipets before washing with soap and
    water.  Transfer the wash solvent to a waste bottle.

    10.10.3.13. Volumetric  flasks and storage bottles used for
    standards must be rinsed several times with distilled  water to
    remove any alkaline residue.  Alkaline residues cause  degradation
    of certain organics and pesticides.

10.10.4.  Standards:

    10.10.4.1.  Replace stock standards and "non-working" standards
    every year.

        10.10.4.1.1. Suggested procedures for preparation  of stock
        standards follow.  We also suggest procedures found in SW-846,
        8000 methods.

            10.10.4.1.1.1.  Weigh 50.0 mg of primary standard into a 50
            mL beaker using a small spatula for solids or  a disposable
            pasteur pipet for liquids.  It may be necessary to aid
            dissolution by adding as small amount of solvent  (e. g.
            ethyl acetate or toluene).

            10.10.4.1.1.2.  Some standards may require placing the
            beaker in an ultrasonic cleaning device or on  a steam bath
            for complete dissolution.
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    10.10.4.1.1.3. Transfer through a glass funnel into a 50
    mL volumetric flask, washing with an appropriate solvent.
     Dilute to volume with the least volatile of the
    appropriate solvents and mix.  Calculate the concentration
    in micrograms per microliter.  When compound purity is
    assayed to be 96% or greater, the weight may be used
    without correction to calculate the concentration of the
    stock standard.  If the purity is less than 96%, the
    weight must be adjusted for purity.

    10.10.4.1.1.4. Transfer to 60 mL screw capped bottles with
    orange labels.  Old bottles that contain the same standard
    may be reused if rinsed with isooctane.

10.10.4.1.2. Calibration Standards - This consists of a set of
five standards with concentrations covering the linearity
range for each detector used for quantitative analysis.

10.10.4.1.3. Intermediate and working standards, (blue,
yellow, silver, and red) are diluted with a high boiling
solvent such as isooctane.  Working standards are diluted to
give even numbered concentrations if possible, from
intermediate and working standards (i.e. 10 ng/uL vs 11
ng/uL) .  Discard working standards after six months.  Some
standards are unstable and must be made up more frequently.
Working solutions should be checked at least quarterly against
available Cincinnati QC samples or a check standard.  New
working solutions should be checked against the old standard.
 Percent difference must not exceed 10% for each compound
checked.

                                    RI -  RZ
            Percent Difference        R2     X   100

                        Total area of peak* _
            R  =        Amount injected  (in nanograms)

10.10.4.1.4. For multicomponent pesticides/PCB' s , use the
total area of all peaks used for quantitation.

        RI  =   relative response  from working standard

        R2  =   relative response  from (second vendor)
                QC standard

        Mixes Used      Detector     Concentrations (ng/uL)
        Blue            FID/MS             5   -  100
        Yellow          Hall, N/P        0.2   -   10
        Silver          Hall            0.05  -    2.5
        Red             EC              0.005 -    0.25
        Green       (Spike solutions for all parameters)

    10.10.4.1.4.1. All standards must be stored in
    refrigerator when not in use.
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10.10.4.2. Spike Solution - All spike solutions are made from
stock or intermediate solutions and diluted with acetone or
methanol.

10.10.4.3. Volatile standard solutions - Stock standard solutions
may be prepared from pure standard materials or purchased as
certified solutions.  Prepare stock standard solutions in methanol
using assayed liquids or gases as appropriate.  Because of the
toxicity of some of the organohalides, primary dilutions of these
materials should be prepared in a hood.  A NIOSH/MESA approved
toxic gas respirator should be used when the analyst handles high
concentrations of such materials.

    10.10.4.3.1. Place about 9.8 mL of methanol into a 10 mL
    ground glass stoppered volumetric flask.  Allow the flask to
    stand, unstoppered, for about 10 minutes or until all alcohol
    wetted surfaces have dried.  Weigh the flask to the nearest
    0.1 mg.

    10.10.4.3.2. Add the assayed reference materials as described
    below:

        10.10.4.3.2.1. Liquids - Using a 100 uL syringe,
        immediately add 2 or more drops of assayed reference
        material to the flask, then re-weigh.  The liquid must
        fall directly into the alcohol without contacting the neck
        of the flask.

        10.10.4.3.2.2. Gases - Introduced from lecture bottle.
        Flow rate is controlled with a valve through a teflon tube
        to top of the meniscus.

    10.10.4.3.3. Re-weigh, dilute to volume, stopper, then mix by
    inverting the flask several times.  Calculate the
    concentration in micrograms per microliter.  When compound
    purity is assayed to be 96% or greater, the weight may be used
    without correction to calculate the concentration of the stock
    standard.

    10.10.4.3.4. Transfer the stock standard solution into a
    Teflon sealed screw-cap bottle.  Store, with minimal head-
    space, at -10°C to -20°C and protect from  light.

    10.10.4.3.5. When stored under the above conditions, those
    standards should be replaced if comparison with QC check
    samples indicates a problem.  Gases are replaced after 3
    months and all others after 6 months.

    10.10.4.3.6. Intermediate standards -  Using stock standard
    solutions, prepare intermediate standards in methanol that
    contain the compounds of interest, either singly or mixed
    together.  The intermediate standards  should be prepared at
    concentrations such that the aqueous calibration standards
    will bracket the working range of analytical system.
    Intermediate standards should be diluted to give calibration
    standards of approximately 30 ng/uL.
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        10.10.4.3.7.  Intermediate standards are prepared as needed and
        should be stored in a freezer with minimal headspace.   They
        should be checked frequently for signs of  degradation  or
        evaporation,  especially prior to preparation of calibration
        standards.   Quality control check standards used to determine
        the accuracy of calibration standards may  be obtained  from
        commercial  sources.

        10.10.4.3.8.  Internal/Surrogate standard spiking solution -
        The solution may be prepared as described  above or with a
        dilution of a commercial standard.  The intermediate surrogate
        solution is prepared as needed.  The stock standard is good
        for a minimum of 6 months.   The first compound is a good
        barometer of the solution;  if it appears to be much smaller in
        size than the other two in a GC/MS run, the stock solution
        should be discarded and another one made.

10.10.5. Records

    10.10.5.1. Stock Standards.  Enter the weight  of the primary stan-
    dard and other  requested information on the stock standard sheet
    in the Quality  Control Standards Logbook (See  Form 10-6).   Also,
    record the requested information on the summary log sheet  at the
    beginning of the section (See Form 10-7), and  on the label of the
    standard bottle.

    10.10.5.2. Each stock solution is assigned a discrete number that
    identifies that particular stock solution.   Whenever a new stock
    solution of the same compound is made up, the  original number
    should be retained.

    10.10.5.3. Blue,  Yellow, and Red Mixes.  Record the parent color,
    dilution number and date of preparation on the standard sheet.
    See Form 10-15.

    10.10.5.4. A new standard sheet must be prepared when one  or more
    ingredients or  the concentrations in a mixture changes. Retain the
    old mix bottle  number on the new mix.  Select  a new number when a
    completely new  mix or standard is made up.   Retire the number when
    a mix or standard is no longer needed.

    10.10.5.5. In GC and GC/MS Logbook, enter name of  the standard
    plus the color  code if applicable.

    10.10.5.6. There are three Quality Control Standards Logbooks.
    Volume 1 is for stock solutions (orange label). Volume 2 is for
    intermediate, working, and spike standards. Volume 3 is for
    outdated sheets.
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10.11.  Data Reporting

    10.11.1. General
        10.11.1.1.  No data will be reported until all QC data has been
        evaluated and data determined to be valid.

        10.11.1.2.  In certain situations where % moisture is not
        determined or used,  the data should be reported on a wet weight
        basis.

        10.11.1.3.  Report parameter concentration in units as in Table 7-
        4.

        10.11.1.4.  Waste samples and % moisture - Calculate and report
        waste samples on a dry weight basis if they are primarily heavily
        contaminated soil or dry solid.  Waste that is primarily
        nonaqueous liquid should be reported using the weight as received
        or wet  weight basis.

        10.11.1.5.  Use the following designations on the data sheet:

            10.11.1.5.1. U - The analyte was analyzed for but not
            detected. The value preceding the "U" is the "minimum
            quantitation limit (MQL)".

                10.11.1.5.1.1. Minimum Quantitation Limit (MQL)  -- Every
                sample has a concentration level below which the variance
                of the results for a particular analyte (element or
                compound) exceeds the acceptable quality control criteria.
                 This level  is the MQL and is reported as the value
                preceding the "U".  The MQL is based on the lowest
                quantitative data point of the instrument calibration
                curve.  The  MQL is derived using this data point and other
                factors such as:  sample size, dilution required, sample %
                moisture, and sample interferences.  The value often
                varies from analyte to analyte within a sample.   Analytes
                are often detected at levels below the MQL and are
                reported as  estimated values (J).  Generally, analytes
                identified below the MQL will only be reported if the
                concentration is greater than one tenth of the MQL.

            10.11.1.5.2. J - The identification of the analyte is
            acceptable, but  the quantitative value is an estimate. The
            value preceding the "J" is the "estimated value".

                10.11.1.5.2.1. Estimated Value — Every sample analysis has
                quality control criteria associated with the quantitative
                data which have been established based on similar
                analyses. When these criteria are exceeded,  the value for
                that analyte or similar analytes is reported as an
                estimated value.  Examples are:

                    10.11.1.5.2.1.1. Calculated values are below or above
                    an appropriate linear range
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        10.11.1.5.2.1.2. Calculated values are below the MQL
        of an analyte.

        10.11.1.5.2.1.3. Analytical holding times for analysis
        are exceeded.

        10.11.1.5.2.1.4. Surrogate recovery limits are
        exceeded.

        10.11.1.5.2.1.5. There are no known quality control
        criteria for an analyte.

10.11.1.5.3. N - There is presumptive evidence that the
analyte is present but it has not been confirmed. The analyte
is "tentatively identified".

    10.11.1.5.3.1. Tentative Identification--There is an
    indication that the analyte reported is present. The
    quality control requirements necessary for confirmation
    were not met. Examples are:

        10.11.1.5.3.1.1. A specific list of compounds is
        analyzed for in every organic analysis by gas
        chromatography/mass spectrometry (GC/MS).  Other
        compounds are often present and their spectra are
        compared to published mass spectral data.  If a
        qualitative determination is made,  the compound is
        reported as tentatively identified.

        10.11.1.5.3.1.2. The presence of analytes is often
        indicated, but there is evidence of possible
        interferences. There is presumptive evidence that the
        analyte is present, therefore, it is reported as
        tentatively identified.

10.11.1.5.4. C - The analyte is determined to be present. The
presence of the analyte was "confirmed by GC/MS".

    10.11.1.5.4.1. Confirmed by GC/MS - Pesticides are
    routinely analyzed by gas chromatography with an electron
    capture detector  (GC/EC).  When identified by GC/EC
    analysis in sufficient concentrations,  pesticides are
    confirmed on the mass spectrometer by comparing the
    spectra of the analyte with the spectra of a particular
    pesticide.  If a good spectral match is obtained, the
    pesticide identification is considered to be confirmed.
    The concentration is quantitated by GC/EC.

10.11.1.5.5. A - The analyte was analyzed in replicate. The
value preceding the "A" is an "average value" of the
replicates.

    10.11.1.5.5.1. Average Value--Samples are often analyzed
    in replicate  (usually in duplicate). Aliquots of the same
    sample are analyzed and the values are averaged. Sometimes
    replicate samples are analyzed and the values are reported
    as an average.

10.11.1.5.6. K - The analyte is determined to be present. The
actual  value is known to be "less than" the value preceding
the "K".
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        10.11.1.5.6.1.  Less Than Values — The analyte is present,
        but the amount  of the analyte is determined to be below an
        acceptable level for quantitation.  The concentration can
        not be calculated,  but is determined to be less than the
        value given.  Example: 10K means that the analyst has
        determined that the analyte is present at some
        undetermined amount less than 10.

    10.11.1.5.7.  L -  The analyte is determined to be present.  The
    actual value  is known to be "greater than" the value preceding
    the "L".

        10.11.1.5.7.1.  Greater Than Values — The analyte is
        present,  but  the amount of the analyte is determined to be
        above an  acceptable level for quantitation. Example:  500L
        means that the  analyte is present at some undetermined
        amount greater  than 500.

    10.11.1.5.8.  R -  Data is "rejected" and should not be used.

        10.11.1.5.8.1.  Rejected Data - Some or all of the quality
        control data  for the analyte were outside criteria.  The
        presence  or absence of the analyte  can not be determined
        from the  data.  Resampling and reanalysis are necessary to
        confirm or deny the presence of the analyte.

    10.11.1.5.9.  UJ - This  is a combination of the "U" and "J"
    codes. The analyte  is not present and the value preceding "UJ"
    is an estimated MQL.

    10.11.1.5.10. JN -  This is a combination of the "J" and "N"
    codes. The analyte  is tentatively identified and the value
    preceding the "JN"  is estimated.

    10.11.1.5.11. JR -  This is a combination of the "J" and "R"
    codes. The analysis indicated the presence of the analyte. The
    data is rejected and the value preceding "JR" is estimated.
    Resampling and reanalysis are necessary to confirm or deny the
    presence of the analyte.

    10.11.1.5.12. UR -  This is a combination of the "U" and "R"
    codes. The analysis did not indicate the presence of the
    analyte. The  data is rejected and the value preceding "UR" is
    the MQL. Resampling and reanalysis are  necessary to confirm or
    deny the presence of the analyte.

    10.11.1.5.13. NAI - Not analyzed due to interference.

    10.11.1.5.14. NA  - Not analyzed for.

10.11.1.6. The number precedes the code letter in all cases.
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10.11.1.7. When adding one or more J values to real values  (e.g.,
for DDTR), J the total if the J values are equal to ^ 10% of the
total value.

10.11.1.8. Rules of rounding.  Round off by dropping digits that
are not significant.  If the digit 6,7,8, or 9 is dropped,
increase preceding digit by one unit; if the digit 0,1,2,3, or 4
is dropped, do not alter preceding digit.  If the digit 5 is
dropped, round off preceding digit to the nearest even number:
thus 2.25 becomes 2.2 and 2.35 become 2.4.

10.11.1.9. Reporting estimated minimum quantitation limits  (MQL) -
The MQL is reported to 2 significant figures.

10.11.1.10. Reporting target compounds below the MQL - Report the
actual calculated value  (to 2 significant figures) with a J for
any concentration below the MQL.  Anything below 1/10 of the MQL
and/or less than a 3mm peak height is reported as not detected.

10.11.1.11. If dilutions of the sample extract are required, the
MQL is raised by the same factor as the dilution.

10.11.1.12. Determine from the analytical request if a specific
limit of quantitation is required.  This is especially important
when analyzing samples for compliance monitoring, spill
investigations, and drinking water investigations.

10.11.1.13. Calculate the MQL for the blank using the lowest
sample weight or sample volume.

10.11.1.14. Report all non-target (library search compounds) data
to 1 significant figure.

10.11.1.15. Inorganic compounds.  Do not report sulfur, H2S, S02,
etc .

10.11.1.16. Reporting duplicate data - Calculate and report the
average with an A flag.  If a compound is detected on one
duplicate and not the other, do not report the compound.
-------
                                            Section:  10
                                            Revision: 1
                                            Date: December 1, 1997
                                            Page:  39

10.11.2.  Nomenclature for Library Search Compounds

    10.11.2.1.  Spaces in chemical names - Be careful where spaces are
    used in nomenclature especially when rearranging CAS names.   Where
    there are dashes, always attach the words.  Where there are
    spaces, always leave them.

        10.11.2.1.1.  Caution!  Location of spaces, brackets,  and
        parentheses are very important when entering names and should
        be entered consistently.

    10.11.2.2.  Names  should be entered in all caps.

    10.11.2.3.  Isomers.  Report as METHYLBIPHENYL  (2 ISOMERS).   Make
    sure spacing is strictly adhered to.

    10.11.2.4.  Isomers of Target Analytes:    TRICHLOROBENZENE (NOT
    1,2,4-) (2  ISOMERS).

    10.11.2.5.  Specified compounds:  Enter as 6275*SPECIFIED COMPOUND
    NAME.

    10.11.2.6.  ESAT should send a copy of final edited data to the
    work assignment monitor.

    10.11.2.7.  Acids.   Always precede acids with a space, same  for
    esters, acetates, oxides, etc. (i.e. BENZOIC ACID).

    10.11.2.8.  Isomers and/or rearranged names, 2-HEXANONE, 5-METHYL-
    3-METHYLENE -, rearrange and combine to METHYLMETHYLENEHEXANONE.
    Dashes indicate no space when the name is rearranged.

    10.11.2.9.  Alkyls. No space.

    10.11.2.10. Esters.  Do not rearrange esters  (i.e., DODECANOIC
    ACID, METHYL ESTER not METHYL ESTER OF DODECANOIC ACID).

    10.11.2.11. Truncated names in data system.  The current GC/MS
    data system library only stores the first 70 characters.  Long
    names with odd looking endings should be looked up to verify the
    complete name.  The HS library display truncates if the name
    extends beyond where the scan number is printed.

    10.11.2.12. Unidentified compounds.  Report as 5 UNIDENTIFIED
    COMPOUNDS,  5 equals the number of compounds.

    10.11.2.13. Hydrocarbon series.  Report homologous hydrocarbon
    series as "PETROLEUM PRODUCT" with an "N" flag in the result
    field.
-------
                                            Section:  10
                                            Revision: 1
                                            Date: December 1, 1997
                                            Page:  40

    10.11.2.14. Common names vs CAS names.  The following commonly
    found compounds are changed from CAS names to common names:

            All pesticides recognized as such
            2-PROPANONE TO ACETONE
            2-PROPANOL TO ISOPROPANOL
            2- BUTANONE TO METHYL ETHYL KETONE
            2-PENTANONE TO METHYL PROPYL KETONE
            3 METHYL-2-BUTANONE TO METHYL ISOPROPYL KETONE
            4 METHYL-2-PENTANONE TO METHYL ISOBUTYL KETONE
            THIOBISMETHANE TO METHYL SULFIDE
            ACETIC ACID ETHYL ESTER TO ETHYL ACETATE
            1,1'-OXYBISETHANE TO ETHYL ETHER
            2,2'-OXYBISPROPANE TO ISOPROPYL ETHER
            1,2-BENZENEDICARBOXYLIC ACID TO PHTHALIC ACID
            ETHENYLBENZENE TO STYRENE

10.11.3.  Laboratory Contaminants

    10.11.3.1. The following organics are frequently detected in
    blanks in trace concentrations.  Therefore, special precautions
    need to be taken when reporting positive findings of these
    compounds.  Do not subtract blank values from sample values  unless
    specified by the method.

        10.11.3.1.1. Volatile Organic Analysis

            10.11.3.1.1.1. Do not report compounds unless they are 5
            times the blank value.

            10.11.3.1.1.2. Background contamination by methylene
            chloride, methylethylketone, and acetone may yield higher
            than normal values.  Therefore, do not report these
            compounds unless they exceed 10 times the blank value.

        10.11.3.1.2. Extractable Organic Analysis

            10.11.3.1.2.1. Report phthalates only if above the MQL.

            10.11.3.1.2.2. Do not report these compounds unless  they
            are present at 5 times the blank value:  bis(2-ethylhexyl)
            phthalate, diethyl phthalate, dibutyl phthalate,  n-
            nitrosodiphenylamine, the xylenes, silicones, and phthalic
            acid.

            10.11.3.1.2.3. Butoxyethoxyethanol and related compounds
            are common contaminants of tubing used in automatic
            samplers. Therefore, if these compounds are detected in
            the sampler blank, report them in sampler blank and  all
            samples where identified.

    10.11.3.2. Reporting of Data when Considering Other Possible
    Contaminants

        10.11.3.2.1. Use the following criteria when evaluating  the
        validity of a positive identification  (see aslo SW-846,  8000
        methods):

            10.11.3.2.1.1. If the compound in question is in the blank
            and in the sample but the concentration in both is 
-------
                                Section:  10
                                Revision: 1
                                Date: December 1, 1997
                                Page:  41
10.11.3.2.1.2. If a compound in question is detected in
the blank at greater than the usual MQL and is in a sample
at £ the blank, report the sample value as the MQL for the
sample.

10.11.3.2.1.3. If the compound in question is in the blank
at MQL, then the analyst must
use professional judgement in determining its validity.

10.11.3.2.1.4. In general, it should be >2 times the blank
value before reporting.  The same is true if the compound
in question is present in both the blank and sample, and
>MQL.   If the compound is reported with a U, the MQL
should be adjusted to the level found in the sample.

10.11.3.2.1.5. Natural organics in fish - Do not report
cholestanol or related compounds.
-------
                                Section:  10
                                Revision: 1
                                Date: December 1,  1997
                                Page:  42

Method*
46A
43D
54B
54B
56
56B
60
47
47A
43
43A
54
54A
54C
44
SOB
58
60
31C
55
55A
43
43A
43B
43C
44
44A
44B
SOB
54
54A
54C
52B
57
60
35
31A
31C
38
51
60
48
48
59
61
61

Descriptor
VLW
VLS
VMS
VMW
VAC
VAC
VTC
SLW
SLW
SLG
SLS
SMS
SHW
SMW
SLT
SAP
sew
STC
SSS
PLW
PLW
PLG
PLS
PSA
PSH
PLT
PTH
PTA
PAP
PMS
PHW
PMW
PCW
PNP
PTC
PWO
PCS
PSS
HLW
HLS
HTC
FLW
FLS
FAC
CLW
CLS
ANALYTICAL DESCRIPTORS
Sample Type
Volatile low water
Volatile low soil/sed
Volatile medium soil/sed
Volatile medium waste
Volatile air canister
Volatile air canister
Volatile by TCLP Extraction
Semivolatile low water - separatory funnel
Semivolatile low water - cont . liquid ext .
Semivolatile low soil/sed w/GPC
Semivolatile low soil/sed wo/GPC
Semivolatile medium soil/sed
Semivolatile high waste wo/son.
Semivolatile medium waste w/son.
Semivolatile low tissue
Semivolatile air PUF
Semivolatile Cartridge ext. water
Semivolatiles by TCLP extraction
Semivolatiles low soil with soxhlet
Pesticide low water - separatory funnel
Pesticide low water - cont. liquid ext.
Pesticide low soil/sed w/GPC
Pesticide low soil/sed wo/GPC
Pesticide low soil/sed w/acid cleanup
Pesticide low soil/sed w/hex/acetone
Pesticide low tissue
Pesticide low tissue w/hexane
Pesticide low tissue w/acid cleanup
Pesticide air PUF
Pesticide medium soil/sed
Pesticide high waste wo/son.
Pesticide medium waste w/son.
Pesticide Cartridge ext. water
Pesticide low water nitrogen/phosphorous
Pesticides by TCLP extraction
PCBs waste oil
Pesticide low soil/sed w/sohxlet
Pesticide/PCB low soil/sed w/sohxlet
Herbicides low water
Herbicides low soil/sed
Herbicides by TCLP extraction
Formaldehyde low water
Formaldehyde low soil/sed
Formaldehyde air cartridge
Carbamates low water w/HPLC
Carbamates low soil/sed w/HPLC
10.11.3.2.1.6. Do not report chlorinated and brominated
cyclohexenes,  cyclohexanes,  and cyclohexanols if
chlorinated water was extracted with methylene chloride.
-------
                                Section:  10
                                Revision: 1
                                Date: December 1, 1997
                                Page:  43

The sampler should verify that it was chlorinated water
and write a memo to the Chemistry Section, so stating.
Standard Levels and Concentrations

GDI Components
TCMX
g- BHC (Lindane)
Aldrin
Heptachlor
Kept. Epoxide
Endosulfan I
Endosulfan II
Dieldrin
p,p' -DDT
Endrin
Methoxychlor
DEC
GDI I Components
TCMX
a- BHC
b- BHC
d- BHC
Aldrin
p,p' -DDT
p,p' -DDD
p,p' -DDE
Endrin Aldehyde
Endrin Ketone
Endosulfan
Sulfate
DEC
Multi Component
Compounds
Toxaphene
Technical
Chlordane
Chlordane
Constituents I
a-Chlordane
b-Chlordene
g-Chlordane
Chlordane
Constituents II
Chlordene
a-Chlordene
g-Chlordene
Oxy Chlordane
Cis Nonachlor
Trans Nonachlor
PCB's
AR 1242
AR 1248
Red Level
Concentratio
ns

0.005
0.010
0.008
0.010
0.010
0.020
0.010
0.025
0.020
0.050



0.005
0.010
0.010
0.010
0.025
0.020
0.010
0.025
0.025
0.025


0.500
0.075

0.010
0.010
0.010

0.005
0.010
0.010
0.010
0.010
0.010

0.15
0.15
Linear Curve Concentration
Level QC-1
0
0.001
0.002
0.0015
0.002
0.002
0.004
0.002
0.005
0.004
0.010
0.00313

0.0013
0.001
0.002
0.002
0.002
0.005
0.004
0.002
0.005
0.005
0.005
0.00313

0.200
0.0125

0.0025
0.0025
0.0025

0.0013
0.0025
0.0025
0.0025
0.0025
0.0025

0.025

Level QC-2
0.0025
0.002
0.004
0.0030
0.004
0.004
0.008
0.004
0.010
0.008
0.020
0.0063

0.0025
0.002
0.004
0.004
0.004
0.010
0.008
0.004
0.010
0.010
0.010
0.0063

0.400
0.025

0.005
0.005
0.005

0.0025
0.005
0.005
0.005
0.005
0.005

0.050

Level QC-3
0.005
0.004
0.008
0.0060
0.008
0.008
0.016
0.008
0.020
0.016
0.040
0.013

0.0050
0.004
0.008
0.008
0.008
0.020
0.016
0.008
0.020
0.020
0.020
0.013

0.600
0.050

0.010
0.010
0.010

0.005
0.010
0.010
0.010
0.010
0.010

0.100

Level QC-4
0.01
0.008
0.016
0.0120
0.016
0.016
0.032
0.016
0.040
0.032
0.080
0.025

0.0100
0.008
0.016
0.016
0.016
0.040
0.032
0.016
0.040
0.040
0.040
0.025

0.800
0.100

0.020
0.020
0.020

0.01
0.020
0.020
0.020
0.020
0.020

0.200

Level
QC-5
0.02
0.016
0.032
0.0240
0.032
0.032
0.064
0.032
0.080
0.064
0.160
0.050

0.0200
0.016
0.032
0.032
0.032
0.080
0.064
0.032
0.080
0.080
0.080
0.050

1.000
0.200

0.040
0.040
0.040

0.02
0.040
0.040
0.040
0.040
0.040

0.300

-------
                Section:   10
                Revision:  1
                Date:  December 1,  1997
                Page:   44
Standard Levels and Concentrations

GDI Components
TCMX
g- BHC (Lindane)
Aldrin
Heptachlor
Kept. Epoxide
Endosulfan I
Endosulfan II
Dieldrin
p,p' -DDT
Endrin
Methoxychlor
DEC
GDI I Components
TCMX
a- BHC
b- BHC
d- BHC
Aldrin
p,p' -DDT
p,p' -DDD
p,p' -DDE
Endrin Aldehyde
Endrin Ketone
Endosulfan
Sulfate
DEC
Multi Component
Compounds
AR 1254
AR 1260
AR 1268




Red Level
Concentratio
ns

0.005
0.010
0.008
0.010
0.010
0.020
0.010
0.025
0.020
0.050



0.005
0.010
0.010
0.010
0.025
0.020
0.010
0.025
0.025
0.025


0.15
0.25
0.25




Linear Curve Concentration
Level QC-1
0
0.001
0.002
0.0015
0.002
0.002
0.004
0.002
0.005
0.004
0.010
0.00313

0.0013
0.001
0.002
0.002
0.002
0.005
0.004
0.002
0.005
0.005
0.005
0.00313


0.025





Level QC-2
0.0025
0.002
0.004
0.0030
0.004
0.004
0.008
0.004
0.010
0.008
0.020
0.0063

0.0025
0.002
0.004
0.004
0.004
0.010
0.008
0.004
0.010
0.010
0.010
0.0063


0.050





Level QC-3
0.005
0.004
0.008
0.0060
0.008
0.008
0.016
0.008
0.020
0.016
0.040
0.013

0.0050
0.004
0.008
0.008
0.008
0.020
0.016
0.008
0.020
0.020
0.020
0.013


0.100





Level QC-4
0.01
0.008
0.016
0.0120
0.016
0.016
0.032
0.016
0.040
0.032
0.080
0.025

0.0100
0.008
0.016
0.016
0.016
0.040
0.032
0.016
0.040
0.040
0.040
0.025


0.200





Level
QC-5
0.02
0.016
0.032
0.0240
0.032
0.032
0.064
0.032
0.080
0.064
0.160
0.050

0.0200
0.016
0.032
0.032
0.032
0.080
0.064
0.032
0.080
0.080
0.080
0.050


0.300





Table 10-2
-------
                                                 Section:   10
                                                 Revision:  1
                                                 Date: December  1,  1997
                                                 Page:  45
                                                                  BOOK
                                  EXTRACTION OF WATER
Project
Analysts
Extraction Solvent & Volume
Spike Solution, Volume & Solvent Method/Matri
Pesticide
Acid
Base/Neutral
Herbicide
Surrogate
Spike
BNA
Pest
Pesticide
Acid
Base/Neutral
Herbicide




Comments:
Method No:
Start date:
Start time:
SAD #


















BNA
VOL SAMPLE


















FINAL
VOL


















STOP DATE:
TIME:
FINAL PROG CHECK


PESTICIDES
VOL SAMPLE


















FINAL
VOL























HERBICIDE
VOL SAMPLE


















FINAL
VOL
























VOL
SAMPLE


















FINA
L
VOL





















                                       Form 10-1
-------
                                                    Section:   10
                                                    Revision:  1
                                                    Date: December  1,  1997
                                                    Page:  46
                                      BOOK
                                 EXTRACTION  OF  SOLIDS/WASTE
Proj ect	
Analysts_
                                  DATE
Extraction Method#_

Extraction Device:
Soxhlet
_B/N      Acid      VGA

           Sonicator
                                       Pest.
      Herb.
Surrogate Spike Added   BNA
            Florisil
                   5%
151
50%
Cleanup /Separation
Acetonitrile
Sulfuric Acid
Auto Prep

Esterification:
Pest
Spike Solution
Extraction Solvent & Volume Volume/Solvent Method/Matrix
Pesticide
Acid
Base/Neutral
Herbicide

Diazomethane
Pesticide
Acid
B/N
Herbicide
PCB's






COMMENTS:

SAD
NUM.










CRUC
SURR
ADD
SURR










GROSS
WT.










DRY
WT.










TARE
WT.










DRY WT
WET WT




















%
SOLID










WET WT
EXTRACT










DRY WT
EXTRACT










FINAL
VOL










  Calculations
   Checked
                                          Form 10-2
                              Completed Date 	
                            Final Project Check
-------
                                                    Section:   10
                                                    Revision:  1
                                                    Date: December  1,  1997
                                                    Page:  47
                                      BOOK
                               EXTRACTION OF BIOLOGICAL TISSUE
Proj ect	
Analysts_
                                                     DATE
Extraction Method#	

Extraction Device:   Sonicator_


Surrogate Spike Added   BNA	
                    B/N
Acid
Pest.
PCB
                      Pest
Cleanup/Separation
Extraction Solvent & Volume
      Volume/Solvent
                 Method/Matrix
GPC
Alumina
Sulfuric Acid
Pesticide
Acid
Base/Neutral
Pesticide
Acid
B/N
PCB's




COMMENTS:
SAD
NUM












GROSS
WT












TARE
WT












WEIGHT
OF OIL












%
LIPID












WET
WEIGHT












FINAL
VOL












COMMENTS












  Calculations
   Checked
                                       Completed Date 	
                                     Final Project Check
                                          Form 10-3
-------
INSTRUMENT
                                                    Section:  10
                                                    Revision: 1
                                                    Date: December 1, 1997
                                                    Page:  48

                                                              BOOK/PAGE 105 /
     GC ANALYSIS

DETECTOR
    COLUMN TYPE
     HP 5890
Hall/PID
DB624  30m x 0.53mm ID x 3um FT
RESTEK 30m X 0.53mm ID x 3um FT
HP 5890 Hall/PID DBS 30m x 0.32mm ID x lum FT
Sw
In
At
PS
eep :
it :
ten :
I:
FID
min ml/min
°C Final
Hall
Other
Split: min ml/min Makeup:
: °C Rate: °C/min
PID FID
ml/m
Init. Hold: Final Hold
Other


Volume Inj :

RUN tt



















PROJ tt




















SAMPLE




















VOLUME




















DIL



















COMMENTS




















DATE




















ANAL



















                                         Form  10-4
-------
                                                           Section:   10
                                                           Revision:  1
                                                           Date: December  1,  1997
                                                           Page:   49
                                         GC/MS ANALYSIS
                                                                      BOOK/PAGE  135/_
                                                                      DATE      	
                                                                      ANALYST    	
                                                                      TRANSFERRED
PROJECT(S).
                                  _5973S _5973V _
                                     DB 624 FSCC
                                       _5973B _JL5200 	5390
                                       	Other (Specify)	
                                                       METHOD*:
                                                                                     V
INSTRUMENT: _5971_5972.
COLUMN:   X DB5MS-FSCC
Meters: _30_ ID: _^25 mm FT:^25_um Purge Temp/Flow: __/__ ACQU TIME:	 EMV:	
Pulse Splitless: ^5_minisPSI   Vent:  .6 min 60 ml/min  EPC/He:_L2 ml/min Makeup:	ml/min
Init. PC/Hid: j4Q_/_2_  Rate 1:_35_  Init. 2 °C/H:J30_/_Q_  Rate 2:  12   Final °C/H: 300 / 8
SS#1 DSPhenol SS#2 D5Nitrobenzene SS#3 Tribromophenol  SS#4  D14Terphenyl
   SLOT#
   TIME
SS#1
SS#2
                SS#3
SS#4
M
MAG
TAPE
FILE NAME
VOL
INJ.
COMMENTS
INT. STD.
  AREA
                                               Form 10-5
-------
   Section:  10
   Revision: 1
   Date: December  1,  1997
   Page:  50

PREPARATION OF STOCK STANDARD

SOL.
NO.
1
2
3
4
5
6
7
8
9
10




DATE














INT














COMPOUND
SOURCE














LOT
NO.














PURITY














BOTTLE NO.
COMPOUND

NET
WEIGHT














ADJUSTED
NET
WEIGHT*














SOLVENT















DILUTION
VOLUME
ml














FINAL
CONC.
ng/ul














BALANCE
CHECK
ACTUAL/-
FOUND














COMMENTS














       Form 10-6
-------
                                                      Section:   10
                                                      Revision:  1
                                                      Date:  December  1,  1997
                                                      Page:   51
                                        SUMMARY LOG SHEET
SECTION
                                              B - Bottle Number
                                         D - Dilution Number
     Name of Standard or Mix
                                         Date
                                                            Date
                                                                             Date
                                                                                               Date
-------
         Section:   10
         Revision:  1
         Date:  December  1,  1997
         Page:   52
Form 10-7
-------
                                                            Section:   10
                                                            Revision: 1
                                                            Date:  December 1,  1997
                                                            Page:   53
                    GC ANALYSIS
             BOOK-PAGE
PROJECT(S) _
ANALYST(S).
ANALYSES:
	Pesticide Quantitation
	Organic Quantitation
	PCB Quantitation
	Herbicide Quantitation
   Confirmation
                   DATE
     INSTRUMENT:
    	HP5890-1
. HP5890-2
     	HP5890-3
. HP5890-4
. HP5890 ESAT
. HPLC/Fluorescence
        HPLC/PDA
        DETECTOR:
       	Electron Capture NI63
	Nitrogen/Phosphorus Thermionic
        	Fluorescence
    PDA
GC COLUMN TYPE:
C18HPLC
DB5-FSCC
DB608-FSCC
	 DB1701-FSCC
DB1301-FSCC
DB210-FSCC
DB1-FSCC
Temperature: Iso
Attenuation: A
B
COLUMN INFORMATION:
1. Capillary Length m ID
2. Capillary Length m ID

STANDARD MIX:
Red Zip File:
Yellow
°C. for min. Program: Initial °C
l.Vol. Ini. ul. Level 1 oQ for
2.Vol.ini. ul. Post Value °C.
Film Thickness
Film Thickness

. for min.
min. (a),
for min.
um
um

°C/min.

i
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23

24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46

47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
SAD#
TYPE ANALYSIS























DILUTION























FINAL
VOLUME























QC























REMARKS























-------
              Section:   10
              Revision:  1
              Date:  December  1,  1997
              Page:   54
Form 10-8
-------
                                                                       Section:   10
                                                                       Revision:  1
                                                                       Date:  December  1,  1997
                                                                       Page:   55
PESTICIDE / HERBICIDE

DATE ANALYZED	

SAMPLE TYPE
SURROGATE RECOVERIES (%)
                                                                    Ext. org.
                                                                                      Pest.*
                                                                                                     VGA
                                                                                                                 Pest
          SAMPLE NO.
                             METHOD
                                            INSTRUMENT
                                                                                                 10
                                                                                                      11
                                                                                                            12
                                                                                                                  13
       1) Phenol-DS
       2) 2,4,6-Tribromophenol
       3) Nitrobeiizene-DS
       4) Terphenyl-D14
       5) 1,2,3,4-TCDD
      * DCAA = 2,4-Dichlorophenyl Acetic Acid
                              6) Dibutylchlorendate
                              10) D4-l,2-Dichloroethane
                              11) p-Difluorobenzene
                              12) p-Bromofluorobenzene
                              13) 2,4,5,6 Tetrachloro-m-xylene
                      * NMX = 2-Nitro-m-xylene
                                                       Form 10-9
-------
                                                               Section:    10
                                                               Revision:  1
                                                               Date:  December  1,  1997
                                                               Page:   56
                                                            MASTER LOG-GC ANALYSIS
Sample Type
W-Water
S-Sediment
F-Fish
B-Biological Material
P-Plant
WA-Waste
AP-Air Puffs
O-OU
MLW-Midlevel Waste
X-Others
Project











Ext
Sht

















Project #

















Sample
Type

















Date
Received
(GC Lab)

















Projected
Completion
Date

















Analysis Type
Pest

















PCB

















Herb

















Other

















Analysis Progress
GC
Screen

















Calc

















Calc
Check

















Date

















Data
Recorded

















Project File
Progress
Project Archive
Name



















































                                                                     Form  10-10
-------
                                                         Section:   10
                                                         Revision:  1
                                                         Date:  December 1,  1997
                                                         Page:   57
Sample #_
Std PC Types
	Reference Ref#_
	PE Sample PE#
	NEIC PRP
	Method Spk
Other
                                 PESTICIDE QC DATA REPORTING SHEET
                                         H20 PEST MATRIX A
                                                P27
Chemist	
Instrument_
Vol/Wt.	
Remarks
Date	
Method_
Vol/Wt.
Test#
5030
5010
5005
5015
5075
5045
5175
5050
5070
5125

















Compound
Gamma-BHC
Heptachlor
Aldrin
Heptachlor Epoxide
Alpha-Endosulfan
Dieldrin
Methoxychlor
P, P-DDT
Beta-Endosulfan
Endrin Aldehyde

















Dup 1



























Dup2



























Spike
Added
500
1000
1000
1000
1000
1000
1000
2000
2000
2500

















%Rec 1



























%Rec 2



























                                          Form  10-11
-------
                                                        Section:   10
                                                        Revision:  1
                                                        Date:  December  1,  1997
                                                        Page:   58
SAMPLE #	
Std PC Types
	Reference Ref#_
	PE Sample PE#
	NEIC PRP
	Method Spk
Other
                                   PESTICIDE QC DATA REPORTING SHEET
                                            H20 PEST MATRIX B
                                                  P28
Chemist
                              Date
Instrument_
Vol/Wt.
Method_
Vol/Wt.
                                     Remarks
Test#
5020
5025
5035
5005
5055
5065
5165
5155
5060
5075


















Compound
Alpha-BHC
Beta-BHC
Delta-BHC
Aldrin
P, P-DDE
Endrin
Alpha-Chlordane
Gamma-Chlordane
P, P-DDD
Endosulfan Sulfate


















Dup 1




























Dup2




























Spike Added
500
1000
1000
1000
1000
1000
1000
1000
2000
2000


















%Rec 1




























%Rec 2




























                                              Form  10-12
-------
                                                         Section:   10
                                                         Revision:  1
                                                         Date:  December 1,  1997
                                                         Page:   59
Sample #	
Std PC Types
	Reference Ref#_
	PE Sample PE#
	NEIC PRP
	Method Spk
Other
                                   PESTICIDE QC DATA REPORTING SHEET
                                           SOIL PEST MATRIX A
                                                  P29
Chemist	
Instrument_
Vol/Wt.	
Remarks
Date	
Method_
Vol/Wt.
Test#
5030
5010
5005
5015
5075
5045
5175
5050
5070
5125
















Compound
Gamma-BHC
Heptachlor
Aldrin
Heptachlor Epoxide
Alpha-Endosulfan
Dieldrin
Methoxychlor
P, P-DDT
Beta-Endosulfan
Endrin Aldehyde
















Dupl


























Dup2


























Spike
Added
1250
2500
2500
2500
2500
2500
2500
5000
5000
6250
















%Rec 1


























%Rec 2


























                                              Form  10-13
-------
                                                 Section:   10
                                                 Revision:  1
                                                 Date:  December  1,  1997
                                                 Page:   60
Sample #_
Std PC Types
	Reference Ref#_
	PE Sample PE#
	NEIC PRP
	Method Spk
Other
                            PESTICIDE QC DATA REPORTING SHEET
                                    SOIL PEST MATRIX B
                                           P30
Chemist
Instrument_
Vol/Wt.	
Remarks
Date	
Method_
Vol/Wt.
Test#
5020
5025
5035
5005
5055
5065
5165
5155
5060
5075

















Compound
Alpha-BHC
Beta-BHC
Delta-BHC
Aldrin
P, P-DDE
Endrin
Alpha-Chlordane
Gamma-Chlordane
P, P-DDD
Endosulfan Sulfate

















Dupl



























Dup2



























Spike
Added
1250
2500
2500
2500
2500
2500
2500
2500
5000
5000

















%Rec 1



























%Rec 2



























                                      Form  10-14
-------
        Section:   10
        Revision:  1
        Date:  December 1, 1997
        Page:   61
A=COLOR CODE B=BOTTLE NUMBER C=DILUTION NUMBER
NAME SOLVENT




BOTTLE# COLOR CODE

COMPOUND

Parent
Sol. ID
A-B-C

Cone.
Parent
ng/ul

AH.
Vol.
ml

Fin.
Cone.
ng/ul

Fin.
Vol.
ml


1J1LU11UN Llrtlb INlllrtLo
BOTTLE# 	 COLOR CODE 	
1.
2.
3.
4.
5.
COMPOUND





Parent
Sol. ID
A-B-C







Dilution #1
Date
Initials


2

Cone.
Parent
ng/ul







3

Ali.
Vol.
ml







4


5

Fin
Cone.
ng/ul





Fin
Vol.
ml






BOTTLE# 	 COLOR CODE 	
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
COMPOUND









Parent
Sol. ID
A-B-C










Cone.
Parent
ng/ul










Ali.
Vol.
ml










Fin.
Cone.
ng/ul










Fin.
Vol.
ml










Dilution #
1
Date
Initials
2


3


4


5


6


7


8


9


10


Form 10-15
-------
                                           Section:   10
                                           Revision:  1
                                           Date:  December 1,  1997
                                           Page:   62
MQL1 GUIDELINES FOR DIFFERENT MATRICES
COMPONENT
Aldrin
Heptachlor
Kept. Epoxide
alpha-BHC
beta-BHC
gamma-BHC
delta-BHC
Endosulfan- 1
Dieldrin
pp-DDT
pp-DDE
pp-DDD
Endrin
DW
ug/1
(ppb)2
0.10 U
0.10 U
0.10 U
0.10 U
0.10 U
0.10 U
0.10 U
0.10 U
0.10 U
0.10 U
0.10 U
0.10 U
0.10 U
WATERS
(other)
ug/1
(ppb)2
0.50 U
0.50 U
0.50 U
0.50 U
0.50 U
0.50 U
0.50 U
0.50 U
0.50 U
0.50 U
0.50 U
0.50 U
0.50 U
SED
ug/kg
(ppb)3
SOU
SOU
SOU
SOU
SOU
SOU
SOU
sou
sou
sou
sou
sou
sou
WASTE
mg/kg
(ppm)4
0.20 U
0.20 U
0.20 U
0.20 U
0.20 U
0.20 U
0.20 U
0.20 U
0.20 U
0.20 U
0.20 U
0.20 U
0.20 U
FISH
mg/kg
(ppm)5
0.050 U
0.050 U
0.050 U
0.050 U
0.050 U
0.050 U
0.050 U
0.050 U
0.050 U
0.050 U
0.050 U
0.050 U
0.050 U
    2  Based on an extraction of  1L and a  final  concentration  vol.  of  1.0ml.

    3  Based on an extraction of  approx. 25gm(dry weight)  and  a  concentration
vol. of 4.0ml.

    4  Based on an extraction of  1.0gm(wet weight)  and a  final concentration
vol. of 10ml.

    5  Based on an extaction of 25gm(wet weight)  and a final concentration  vol
of 4.0ml.
                     DW = drinking water     SED = sediments
                                  Form 10-16
-------
                                Section:   10
                                Revision:  1
                                Date:  December 1,  1997
                                Page:   63
MQL1 GUIDELINES FOR DIFFERENT MATRICES
Endosulfan -II
Endosulfan- SO4
Endrin Ketone
Methoxychlor
Tech. Chlordane
PCB
Toxaphene
0.10 U
0.10 U
0.10 U
0.25 U
0.25 U
0.50 U
5.0 U
0.50 U
0.50 U
0.50 U
1.0 U
1.0 U
2.0 U
20 U
SOU
SOU
SOU
200 U
200 U
500 U
3000 U
0.20 U
0.20 U
0.20 U
0.50 U
0.50 U
1.0 U
8.0 U
0.050 U
0.050 U
0.050 U
0.20 U
0.20 U
0.50 U
3.0 U
BOX NO.
STORAGE LOCATION

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
48
49























































































50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
80
81
82
83
84
85
86
87
88
89
97
98






















































































                       Form 10-17
                  Form  10-17
-------
                                                    Section:  11
                                                    Revision:  0
                                                    Date:  September 1990
                                                    Page:  1
11.  INORGANIC ANALYSIS, PERFORMANCE QUALITY CONTROL AND ANALYTICAL OPERATION

    11.1.  Every element of environmental data acquisition,  from sample
    collection to final data reporting,  has associated with it degrees of
    error.   The primary purpose of a quality assurance program is the
    optimization of conditions whereby the introduction of  error can be either
    precluded or substantially reduced.   The operating procedures and quality
    control checks practiced in this laboratory and outlined in this manual
    are implemented to minimize the total error associated  with data
    generation.  No number can be affixed to total error;  however, analytical
    performance is measurable and thus definable.  This section is limited to
    a discussion of the analytical operation and procedures used in this
    laboratory to measure and record analytical performance.

    11.2.  General

        11.2.1. During the course of generating data on samples for inorganic
        parameters, it is the policy of the Analytical Support Branch (ASB) to
        apply the best laboratory practices, use approved methodology when
        mandated by regulation, use standardized methodology,  if possible,
        when approved methodology is not applicable, fully  document all
        operations associated with the generation of data and to meet certain
        quality requirements that will be designated in the following
        paragraphs.  It should be noted, however, that occasionally certain
        matrices and samples present analytical challenges, or are not
        amenable to standardized methodology.  In these instances
        modifications to standard protocols may have to be  made to produce a
        high quality analysis.  When this occurs, any deviations from standard
        operating procedures will be fully documented.

        11.2.2. Safety precautions associated with the safe handling of toxic
        chemicals, reagents, solutions and samples will be  observed and
        regarded as a first order responsibility of the analyst.  The analyst
        will take the necessary precautions to prevent exposure or harm both
        to himself and his fellow workers.

        11.2.3. Water used to prepare calibration standards, spike solutions,
        standard reference solutions or any sample dilutions or mixtures must
        meet or exceed the requirements for Type II grade water as specified
        by the American Society for Testing and Materials  (ASTM); Standard
        Practice D 1193.   This grade water is equivalent to Type II water as
        specified in Standard Methods 1080.  The parameter  measured to verify
        the quality of water is resistivity, with a requirement of 1 megohm-cm
        at 25°C or better.   See also section 2.2  of Handbook for Analytical
        Quality Control in Water and Wastewater Laboratories (EPA 600/4-79-
        019, March 1979), and any future updates of the manual.  Reagent water
        used for trace metals determinations must meet or exceed the
        requirements for Type I grade water as specified by ASTM.  The
        parameter monitored to verify the quality of water  is resistivity,
        with a requirement of 18 megohms-cm at 25°C or better.   This  grade
        water is equivalent to Standard Methods Type I water.

        11.2.4. Reagents must be ACS reagent grade quality  or better.  All
        reagents will be dated upon receipt, and will be properly disposed of
        when the shelf life has been reached.
-------
                                                Section 11
                                                Revision: 1
                                                Date: December 1, 1997
                                                Page 2
11.3. Custody
    11.3.1. The EPA Region IV Science and Ecosystem Technology Center is a
    "controlled access" facility.  Entry to the facility is restricted to
    employees and is controlled by keycards.   All visitors to the facility
    must enter through the guard station at the main entrance and be
    escorted by a host when in the facility.   Additionally, access to the
    custody room is controlled by keycard.  Only employees with legitimate
    reason for access to samples have keycard access to the custody room.
     All samples removed from the custody room must be signed out.  When a
    sample is signed out,  the signee is legally assuming custody of the
    sample and is responsible for its integrity and accountability during
    possession.  Custody is relinquished only when the samples have been
    returned and signed back to the custody room.  Aliquots taken from the
    original samples for analysis will be accounted for by entering sample
    ID in the proper log books during preparation and analysis.

11.4.  Metals  Metals analyses are performed in support of various agency
programs.  Some programs mandate methods  (e.g. Drinking Water at 40CFR
Part 141 ff. and NPDES at 40 CFR Part 136), while others publish methods
strictly as guidance (e.g. RCRA except for the Characteristic Tests at
40CFR Subpart C Part 261.20 ff.)  Subject to the restrictions in 11.2.1,
mandated methodology will be used for those analyses requiring them.
Guidance methods will be closely adhered to with the possibility of minor
changes which do not change the chemistry of the procedure.  In any event,
all procedures will be fully documented.  The following programs are
supported by laboratory analyses:

    11.4.1. Drinking Water

        11.4.1.1. Regulatory Authority:  National Primary Drinking Water
        Regulations are found at 40 CFR Part 141.  National Secondary
        Drinking Water Regulations are found at 40 CFR Part 143.  In
        general these regulations apply to Public Water Systems which are
        defined as "a system for the provision to the public of piped
        water for human consumption, if such system has at least fifteen
        service connections or regularly serves an average of at least
        twenty-five individuals at least 60 days out of the year."
        Historically, this laboratory has analyzed few samples from public
        water systems as the states have been delegated the authority for
        monitoring public water supplies within their boundaries.
        However, this laboratory does often analyze samples from
        individual private potable wells.  While not legally obligated to
        adhere to the requirements of 40 CFR Part 141 for these samples,
        this lab has chosen to follow the requirements Part 141 whenever
        possible when analyzing private potable wells.

        11.4.1.2. Identification of Samples:   Drinking water samples from
        public water systems will be logged into the data system with the
        program element HOH.  The requirements of 40 CFR Part 141 must be
        adhered to for the analysis of these samples.  Samples from
        individual potable wells may be received under any program
        element, the most common being RCRA or Superfund (SSF or NSF).
        The samples will be identified on the sample log sheets as
        "Potable Well", code PW.  Requirements of 40 CFR Part 141 will be
        met whenever practicable.

        11.4.1.3  Preparation and Analysis of Drinking Water Samples:  Any
        or all of the following methods in Table 11.1 may be used by this
        laboratory for the analysis of drinking water and potable well
        samples.  Prior to analysis samples will be digested using the
        procedure in the approved method.  The digestion step may be
-------
                                        Section 11
                                        Revision: 1
                                        Date: December 1, 1997
                                        Page 3

omitted on those samples with a turbidity of less than 1
nephelometric turbidity unit  (NTU) and a "direct analysis" may be
performed. (Technical Notes on Drinking Water Methods, EPA 600/R-
94-173, October 1994 as referenced in 40CFR 141.23.)
-------
                                                    Section 11
                                                    Revision: 1
                                                    Date: December 1,
                                                    Page 4
1997
                       Table  11.1  Drinking Water Methods
ANALYTE
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Lead
Mercury
Nickel
Selenium
Thallium
MCL (mg/L)
0.0061
0.0502
2.01
0.0041
0.0051
0.101
0.0153
0.0021
0.101
0.0501
0.0021
ICP4

200.7
200.7
200.7
200.7
200.7


200.7


Graphite
Furnace4
200.9
200.9

200.9
200.9
200.9
200.9

200.9
200.9
200.9
Graphite
Furnace5
3113B
3113B
3113B
3113B
3113B
3113B
3113B

3113B
3113B

ICP-MS4
200.8
200.8
200.8
200.8
200.8
200.8
200.8
200.8
200.8
200.8
200.8
CVAA4 ' 6







245.1
245.2



Footnotes:
1   40CFR 141.23
2   40CFR 141.11
3   40CFR 141.80
4   ICP method 200.7, Graphite Furnace Method 200.9, ICP-MS Method 200.8 and
    Mercury CVAA Method 245.1 are in "Methods for the Determination of Metals
    in Environmental Samples-Suppplement 1", EPA-600/R-94-111,  May 1994.
    Available from NTIS, PB 94-184942;  (800) 553-6847.
5   Graphite Furnace Method 3113B is in 18th Edition of Standard Methods  for
    the Examination of Water and Wastewater, 1992, American Public Health
    Association.  Available from American Public Health Association,  1015
    Fifteenth Street NW, Washington DC.
6   Mercury CVAA Method 245.2 is available from US EPA, NERL, Cincinnati, OH
    45268.   The identical method was formerly in "Methods for Chemical
    Analysis of Water and Wastes", EPA-600/4-79-020, March 1983 which is
    available from NTIS, PB84-128677;  (800)  553-6847.

            11.4.1.4.  NPDES Monitoring:  The National Pollutant Discharge
            Elimination System (NPDES) is the national system for the issuance
            of permits under section 402 of the Clean Water Act (CWA) of 1977
            as amended.  Test procedures for the analysis of pollutants are
            found at 40CFR Part 136.

            11.4.1.5.  Identification of Samples:  Samples received by this
            laboratory will be logged into the data system under one of three
            program elements; ICSI  (Industrial Compliance Sampling
            Inspection) , MCSI (Municipal Compliance Sampling Inspection) or
            XCSI (Toxic Compliance Sampling Inspection).

            11.4.1.6.  Preparation and analysis of NPDES samples:   Samples
            received in support of the NPDES program will be prepared and
            analyzed in accordance with the requirements at 40CFR 136.  Table
            11.2 lists approved test procedures for metals analyses that may
            be used by this laboratory.  Digestion is required prior to
            analysis for all metals.
-------
                                                    Section 11
                                                    Revision: 1
                                                    Date: December 1, 1997
                                                    Page 5
                           Table 11.2 NPDES Methods
Analyte
Aluminum
Antimony
Arsenic
Barium
Beryllium
Boron
Cadmium
Calcium
Chromium VI
Chromium
Cobalt
Copper
Hardness
Iron
Lead
Magnesium
Manganese
Mercury
Molybdenum
Nickel
Potassium
Selenium
Silica
Silver
Sodium
Thallium
Tin
Titanium
Vanadium
Zinc
ICP

200. 71
200.
200.
200.
200.
200.
200.
200.

200.
200.
200.
200.
200.
200.
200.
200.

200.
200.
200.
200.
200.
200.
200.
200.
200.

200.
200.
7
7
7
7
7
7
7

7
7
7
7
7
7
7
7

7
7
7
7
7
7
7
7
7

7
7
GFAA Other CVAA-HG
3113B2
3113B
3113B
3113B
3113B

3113B

3500-Cr D2
3113B
3113B
3113B

3113B
3113B

3113B
245. I1
245.2
3113B
3113B

3113B

3113B

279. 21
3113B1
283 .21
286. 21
289. 21
Footnotes:
-------
                                                    Section 11
                                                    Revision: 1
                                                    Date: December 1, 1997
                                                    Page 6

1   Methods for the Determination of Metals in Environmental Samples-
    Suppplement 1,  EPA-600/R-94-111, May 1994.
2   Standard Methods for the Examination of Water and Wastewater.  American
    Public Health Association,18th  Edition,1992.

            11.4.1.7. Other Waters:   Monitoring well, ambient water,  effluents
            and other water samples  are digested with nitric-hydrochloric
            acids according to Method 200.2.  All digests are scanned by ICP.
             Where the detection/quantitation technique is specified by
            program requirements, positive elements from the ICP scan will be
            verified by atomic absorption to satisfy the appropriate
            requirement.  Mercury analyses are performed according to MCAWW1-
            245.1 or 245.1-Region 4  Modification or 245.7 CVAF depending on
            detection limit requirements.   (245.1-Region 4 Modification
            consists of an autoclave digestion instead of a water bath
            digestion.  The autoclave digestion of waters has proven effective
            and allows for greater throughput than the water bath digestion.
            All other method parameters remain the same.)

            11.4.1.8. Soil and Sediment:  A 50 g aliquot (approximately) is
            taken from a well mixed  sample and weighed in a crucible.  The
            sample is dried overnight at 60°C  for a % moisture determination.
              The dried sample is ground to fineness and a 1 g subsample is
            taken for analysis.  Sample digestion is conducted according to
            Method 200.2 or Method 30502 for those samples  containing large
            amounts of organic matter and made up to 100 mLs for analysis.

            11.4.1.9. Final low level data for thirty elements is generated by
            ICP (Method 200.7), Graphite Furnace  (Method 200.9 or 3113B) or
            ICP-MS (Method 200.8, 6020, or 1638).

            11.4.1.10.  Mercury analysis of sediments will be conducted
            according to method 245.5 - Either water bath digestion or Section
            11.3 (autoclave digestion)  in Methods for the Determination of
            Metals in Environmental  Samples, or by CVAF Region 4 method for
            those samples requiring  lower levels of detection.

            11.4.1.11. Fish:  Whole  fish are initially prepared with dry ice
            grinding followed by preparation by Method 200.3  (Methods for the
            determination of Metals  in Environmental Samples, Supplement 1:
            EPA/600/R-94/111.)

            11.4.1.12. Requests for  analysis of individual organs or tissue
            can be satisfied by using the sample in its entirety or sub-
            sampling to obtain the maximum weight required for the analysis.
            The tissue should be kept frozen during sub-sampling and weighing
            to prevent fluid migration or drainage.

            11.4.1.13. Mercury analyses on fish tissue are performed according
            to Region 4 modification of Method 245.5.
            11.4.1.14. Digestion of  tissue for multielement analyses is con-
            ducted according to Method 200.3  (nitric/peroxide) followed by ICP
            detection.  Detection limit requirements are satisfied by
            manipulation of sample weight, final volume of digestate and in
            certain instances,  detection by HGAA graphite furnace.

            11.4.1.15. Other Tissue:  Generally, other tissues will be
            prepared and analyzed the same as fish tissue with the additional
            precaution during preparation to observe closely and add
            additional reagents as required to thoroughly digest the sample.
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                                            Section 11
                                            Revision:  1
                                            Date: December 1,  1997
                                            Page 7

    11.4.1.16.  EP/TCLP Extracts:  Waste samples for EP Toxicity
    determinations will be extracted according to Method 1310A in SW-
    846 and subsequent clarifications of the methodology as received
    from Office of Solid Waste.  The extract may be acid digested
    (Method 3010A SW-846)  and scanned by ICP for the usual 26
    elements.   If any of the drinking water parameters are above the
    fail level  in EP extracts,  the parameter(s) will be confirmed by
    the method  of standard additions, Method 6010.  (Figure 2-6,
    Chapter Two,  SW-846.)   TCLP extracts will be prepared per  Method
    1311,  optionally digested by Method 3010A and analyzed by  Method
    6010.

    11.4.1.17.  Oil and Oily Samples: Oil emulsions and oil samples
    will be prepared in one of two ways on a wet weight basis.  Those
    oil samples which are thin enough to disperse on heating,  yet not
    cover the  entire surface of the digestion fluid resulting  in a
    superheated solution will be prepared by Method 3050A.  Those
    samples not amenable to Method 3050A will be prepared by the
    following method:  The oil phase is weighed  (1 g)  into a small
    crucible.   The crucible is transferred to a muffle furnace and
    brought up  to 125°C for 1  hr.   Increase  temperature  175°C  for 1
    hr.  Increase to 250°C for  1 hr.   NOTE:   Do not  open furnace
    during the  procedure and until furnace has cooled to 100°C.   The
    sample is  ashed overnight at 450°C maximum temperature.  One mL  of
    concentrated nitric acid and 1 mL of concentrated hydrochloric
    acid is added to the ash and warmed until ash is in solution.
    This solution is diluted to volume and is ready for analysis by
    ICP.

    11.4.1.18.  High Volume Filters:  Air filters are prepared  with a
    digestion  fluid as outlined in 40 CFR Part 50, Appendix G.  The
    digestion  fluid is prepared by combining 167 mL of HN03  and  77 mL
    of HCL and  diluting to 1 Liter.  The resulting digestion fluid is
    2.6 M HN03  and 0.9M HC1.   The Federal  Register method uses an
    ultrasonic  extraction; however, an oscillating hot plate
    extraction  is also acceptable.  Typically, a 1x8 inch strip of a
    "high vol"  filter is digested with a final volume of 100 mL, or a
    1x4 inch strip is digested to 50 mL final volume.   For the
    preparation of "saturation" filters, typically the entire  filter
    is digested because of its small size.

    11.4.1.19.  Special Samples:  Samples received for analysis which
    are not amenable to the standard digestion techniques will be
    prepared according to the best judgement of the analyst.  These
    cases will  require additional documentation as to methodology,
    quality control,  and justification of the method used.

11.4.2. QC Requirements for Metals:

    11.4.2.1.  Sample Preparation

        11.4.2.1.1. A blank solution will be prepared with each group
        of samples to monitor for contamination of reagents, glassware
        and the laboratory.  Detectable blank levels up to ten percent
        of sample concentration are permissable and are not an
        indication of an out of control sample.

        11.4.2.1.2. A spike solution, prepared from standard reference
        materials  (or laboratory standards that have been confirmed by
        SRM) will be prepared with each group of samples.   (A  group is
        defined as any batch of samples prepared together in the same
        hood at the same time and with the same reagents).  This
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                                        Section 11
                                        Revision: 1
                                        Date: December 1, 1997
                                        Page 8

    solution verifies instrument calibration and monitors the
    digestion procedure.

    11.4.2.1.3. All projects will have at least one sample
    duplicated and spiked.  Projects with large numbers of samples
    will be duplicated and spiked at the rate of ten percent.

11.4.2.2. Calibration Standards: Commercial single element or
multielement standard solutions will be used for the preparation
of instrument calibration solutions.  These standards will be
dated when received and their concentration verified with standard
reference materials from NIST, commercial sources where available,
or reference samples from NERL-Cincinnati, QA Branch.  All
commercial standards will undergo additional examination for trace
contamination of elements other than the specified element.   Mixes
of these single element standards are prepared according to the
requirements of the instrument being used.

11.4.2.3. Instrument Calibration:  All instruments will be cali-
brated with working standards diluted from commercial stock
solutions that have been verified to contain their stated
concentration.  Instruments will be calibrated to cover the range
of concentrations found in the samples or the samples may be
diluted to fall within the calibration range. (The following
acceptable alternate technique is used in multi-element analyses
(ICP or ICP/MS) when an analyte exceeds the high standard:  A high
level single element standard may be run to demonstrate that the
linear calibration range has not been exceeded and that no inter-
element interferences are presented by the higher level of the
analyte.)  An initial calibration check solution should be run as
specified in the method.  Calibration must be verified during each
set of samples at a frequency that will validate all data
generated for that set.  Reference samples can also be considered
as calibration check samples.

11.4.2.4. Instrument Log Books:  Will be maintained to record all
service and maintenance records.

11.4.2.5. Sample Analysis Records:  Log books will be maintained
to record preparation of samples to include records of duplicates,
spikes, sample numbers, dates, analyst, etc.

11.4.2.6. Log Books: Will be maintained at each instrument to
record instrumental conditions and settings during the analysis of
samples.

11.4.2.7. Data Records:  All raw data from instrumentation will be
retained for future reference in either hard copy or electronic
storage.

11.4.2.8. QC Data:  Data generated from sample duplicates, sample
spikes, preparation blanks and SRM preparations will be compared
with historical data for that particular sample type and, if found
to be within acceptable limits, will be added to the QC data base.
 If the data are not within acceptable limits, the samples will be
re-analyzed or will the data will be flagged.  If, after a second
analysis, the data still remains outside acceptable limits,  data
will be flagged and reported.

11.4.2.9. Glassware and Equipment:  All glassware/teflon vessels
will be placed into a detergent soak immediately after use and
must not be allowed to dry while dirty.  After thoroughly soaking,
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                                        Section 11
                                        Revision: 1
                                        Date: December 1, 1997
                                        Page 9

all detergent is removed by rinsing, followed by a 20% nitric acid
rinse and finally a thorough rinsing with DI water.  Allow to
drain on its side and seal with parafilm or a glass stopper before
storage in an upright position. Pipets are rinsed immediately
after use and placed in a detergent soak until moved to an
automatic rinser with DI water.  Labware used in ultra-trace
analyses may require more rigorous specialize cleaning.

Footnotes:
1   MCAWW - Methods for Chemical Analysis of Water and Wastewater.
     EPA 600/4-79-020,  March 1979.  (Revised March 1983),  and any
    future updates.

2   SW846 - Test Method for Evaluating Solid Waste, EPA 1982, and
    any future updates.
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                                                Section 11
                                                Revision:  1
                                                Date:  December 1,  1997
                                                Page 10
11.5.  General Inorganic
    11.5.1.  Preparation and Analysis:  A large portion of the samples that
    require  analysis for nonmetal inorganic constituents (commonly
    referred to as Nutrients/Classicals)  are NPDES Projects.  These
    samples  are analyzed according to acceptable methods listed in 40 CFR
    Part 136.   In addition to these methods, other methods  are used as
    appropriate for programs other than NPDES.  The current approved
    versions of all methods are used for regulatory purposes.   Guidance
    methods  will be closely adhered to with the possibility of minor
    changes  which do not change the chemistry of the procedure.  In any
    event,  all procedures will be fully documented. Table 11.3 lists
    parameters routinely analyzed in this laboratory and methods of
    analysis.   In addition to these parameters, the lab is  capable of or
    is in the process of developing capability for analysis of dermal
    corrosion, heat of combustion, and trace level analysis for several
    parameters.

11.6.  QC Requirements for General Inorganic

    11.6.1.  Sample Preparation

            11.6.1.0.1. A blank solution will be prepared with each group
            of samples to monitor for contamination of reagents, glassware
            and the laboratory.

            11.6.1.0.2. All projects will have at least one sample
            duplicated and spiked.  Projects with large numbers of samples
            will be duplicated and spiked at the rate of ten percent.

        11.6.1.1. Instrument Calibration:  All instruments  will be cali-
        brated with working standards diluted from commercial  stock
        solutions that have been verified to contain their  stated
        concentration when these commercial solutions are available and
        use  is appropriate.  Instruments will be calibrated to cover the
        range of concentrations found in the samples or the samples may be
        diluted to fall within the calibration range.  An initial
        calibration check solution should be run as specified in the
        method.   Calibration must be verified during each set  of samples
        at  a frequency that will validate all data generated for that set.
         Reference samples can also be considered as calibration check
        samples.

        11.6.1.2. Instrument Log Books:  Will be maintained to record all
        service and maintenance records.

        11.6.1.3. Sample Analysis Records:  Log books will  be maintained
        to  record preparation of samples to include records of duplicates,
        spikes,  sample numbers, dates, analyst, etc.

        11.6.1.4. Log Books: Will be maintained at each instrument to
        record instrumental conditions and settings during  the analysis of
        samples.

        11.6.1.5. Data Records:  All raw data from instrumentation will be
        retained for future reference.  Where readings are  read directly
        from an instrument, these readings are considered raw data and are
        recorded in the appropriate log book.

        11.6.1.6. QC Data:  Data generated from sample duplicates, sample
        spikes,  preparation blanks and SRM preparations will be compared
        with historical data for that particular sample type and, if found
        to  be within acceptable limits, will be added to the QC data base.
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                                        Section 11
                                        Revision: 1
                                        Date: December 1, 1997
                                        Page 11

 If the data are not within acceptable limits,  the samples will be
re-analyzed.  If, after a second analysis, the data still remains
outside acceptable limits, data will be flagged and reported.

11.6.1.7. Reference materials: Sources outside the lab will be
used for reference materials when available.  As of November 1997,
the following parameters do not have commercial sources known to
this lab:  color, settlable solids, acidity, and TVSS.
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                                         Section 11
                                         Revision: 1
                                         Date: December 1, 1997
                                         Page 12

Table 11.3 Nutrients/Classicals Capabilities and Methods
Analyte
Acidity
Alkalinity
Ammonia
BOD
Chloride
Chlorine,
Residual
COD
Color, ADMI
Color, Apparent
Color, Pt Co
Conductivity
Cyanide
Fluoride
Hardness
Nitrate/Nitrite
Nitrite
Oil and Grease
% Solids or
Moisture
PH
Phenols
Phosphorus
Phosphorus ,
Ortho
Solids
Sulfates
Sulfides
Method Other than 40 CFR Part
136 and Comments


Sedmt-EPA Region 4 method: 1
similarly to aqueous samples
g sample distilled

NPDES Methods and Method 3001






Sedmt digested according to note in Std Mthds2 p. 4 -19
2.b.

Summation of Ca+Mg carbonates
Method 353. 2M- formal request
Test Procedure 11/97
Sedmt-EPA Region 4 method: 1
dilute acid
(ICP)
submitted for Alternate
g sample leached into

Method 1664- interim approval
821-B-94-0046
4/96, Document # EPA-

SW-846 Method 9040 or 9045

Sedmt-EPA Region 4 method: 0.
similarly to aqueous samples
2 g sample digested


NPDES Methods and Method 3001
Sedmt distillation3 followed by methylene blue color
development
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                                                    Section 11
                                                    Revision: 1
                                                    Date: December 1, 1997
                                                    Page 13
TKN
TOG
Turbidity
MCAWW 351.2-Cu
compound
Sedmt -Method 42
compound substituted
4, pp3-22
for Hg digestion


Footnotes:
1   Methods for the Determination of Inorganic Substances in Environmental
    Samples.  EPA/600/R-93/100,  August 1993.
2   Standard Methods for the Examination of Water and Wastewater.  American
    Public  Health Association, 18th Edition, 1992.
3   Chemistry Laboratory Manual  "Bottom Sediments".  Great Lakes  Region
    Committee on Analytical Methods, EPA-FRQA, December 1969.
4   Procedures for Handling and Chemical Analysis of Sediment and Water
    Samples.  USEPA/Corp of Engineers.
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                                                    Section:  12
                                                    Revision: 1
                                                    Date: December 1, 1997
                                                    Page:  1


12.  PERFORMANCE QUALITY CONTROL DATA HANDLING

    12.1. All performance quality control data (Section  10, and 11) are trans-
    ferred from the data books and forms to the appropriate quality control
    logs or data entry forms.  Quality control logs or forms are maintained
    for inorganic parameters, organics and pesticides, metals and
    microbiological parameters.

    12.2. The following subsections contain the techniques used to measure
    analytical performance:

        12.2.1. Precision Data

            12.2.1.1. Organic -  Precision is expressed as percent relative
            standard deviation and is calculated by the  formula:

                            % RSD  =    S  x 100
                                        X
                        Where:  £3 = Standard Deviation
                                X = Mean

            12.2.1.2. Inorganic  - Precision is expressed as relative percent
            difference and is calculated by the formula:

                            % RPD  =    D  x 100
                                        X
                        Where:  D = Difference between measurements
                                X = Mean

        12.2.2. The estimated standard deviation may be  calculated by the
        following equations fpr duplicate analysis:

                            S =  +  (Xx -  X2) 0.89

                    Where:  Xx and X2  = individual  observations.

            For replicate analysis (any number >2)

                     	          NOTE:  Automatic calculators
                S =
+n E X2  -  (EX)2                   may be used to deter-
              \|  n(n-l)                             mine S if this formula
                                               is used.
                Where:  X = individual observations.
                        n = number of observations.

                       Do not use this formula for n=2.
    12.3. Accuracy Data

        12.3.1. Accuracy is expressed as percent recovery and calculated by
        the formula:

                                     Z  -  X
                        % Recovery =     T       (100!
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                                                Section:  12
                                                Revision: 1
                                                Date: December 1,  1997
                                                Page:  2


            Where:   X = concentration in unspiked sample.
                    Z = concentration in spiked sample.
                    T - True concentration of spike added.

12.4.  Annual Analytical Performance Summary

    12.4.1.  At the  end of each fiscal year, a summary report of the
    Branch's analytical performance is prepared.  Contained in this report
    are:   the precision data (average percent RSD or RPD, upper warning
    and control limits),  and accuracy data (average total percent  recovery
    of spiked samples, AQC reference samples, and performance audit
    samples  where possible).   This summary will contain all parameters for
    which adequate  quality control data have been generated during the
    year.

    12.4.2.  Participation in EPA Performance Evaluation Studies.

        12.4.2.1. The Branch will participate in announced EPA performance
        Evaluation  Studies.   Performance on these studies further
        indicates the effectiveness of the laboratory's day-to-day quality
        control procedure.
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                                                    Section 13
                                                    Revision:   0
                                                    Date:  August 1990
                                                    Page 1
13.  ANALYTICAL CORRECTIVE ACTIONS

    13.1.  Corrective action will be taken at any time during the analytical
    process when deemed necessary based on analyst judgement or when quality
    control data indicate a need for action.  Generally,  corrective action
    will be triggered by such things as:  poor analysis replication, poor
    recovery,  instrument calibration problems, blank contamination, etc.   (See
    previous sections for specifics).

    13.2.  Corrective actions will include, but not necessarily be limited to:
    reanalysis,  calculation checks, instrument recalibration,  preparation of
    new standards/blanks, re-extraction/digestion, dilution, application of
    another analysis method, additional analysts training,  etc.  Most
    frequently,  these corrective actions will be initiated by the analyst at
    the time of analysis.  However, some corrective actions are initiated
    subsequent to analysis based on evaluations performed by quality assurance
    or laboratory management personnel.

    13.3.  All  data corrective actions  will be noted on the appropriate log,
    chromatogram, strip chart or data  report.
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                                                    Section 14
                                                    Revision:   0
                                                    Date:   August 1990
                                                    Page 1
14.  DATA QUALITY OBJECTIVES

    14.1. During the planning phase of a project requiring laboratory support,
    the data user must establish the quality of data required from the
    investigation.  Such statements of data quality are known as Data Quality
    Objectives (DQO's).   The DQO's are qualitative and quantitative statements
    of the quality of data required to support specific decisions or
    regulatory actions.   The laboratory is responsible for producing data of
    known quality and consistent with that prescribed in the DQO.

    14.2. The laboratory will select analytical methods, instruments,
    parameter detection limits,  etc. which are capable of producing data of
    the quality required by the  DQO.  The quality of a data set is defined in
    terms of:  precision,  accuracy, representativeness, completeness and
    comparability.  The significance of each of these measures differs
    according to their applicability to the laboratory and to a particular
    data set.  A brief explanation of the above measures are as follows:

        14.2.1. Precision and accuracy.  These are quantitative measures that
        characterize the amount  of variability and bias inherent in a given
        data set.  Precision refers to the level of agreement among repeated
        measurements of the same characteristic.  Accuracy refers to the
        difference between an estimate based on the data and the true value of
        the parameter being estimated  (See Section 13).

        14.2.2. Representativeness.  Refers to the degree to which the data
        collected accurately reflect the population, group or medium being
        sampled.

        14.2.3. Completeness.  Refers to the amount of data that is
        successfully collected with respect to that amount intended in the
        study design.

        14.2.4. Comparability.  Refers to the ability to compare data from
        different sources with a degree of confidence.
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                Attachment 5
Battelle Quality Assurance Management Plan
-------
Battelle
Marine
Sciences
Laboratory
Quality Assurance
Management Plan
January 2000
-------
   GBaneiie
     . . .  Putting Technology To Work
     Marine Sciences Laboratory
        Quality Assurance Management Plan


Introduction

The purpose of the Battelle Marine Sciences Laboratory (MSL) Quality Assurance
Management Plan is to describe the Quality Program implemented at the facility. This
plan summarizes the elements of the quality assurance program and discusses the
quality control activities routinely used for MSL work. The objective of the Quality
Program is to obtain accurate and precise data consistent with project objectives. The
MSL QA Program has evolved over time to meet client needs but its roots are from the
U.S. Environmental Protection Agency's Quality Assurance Management Staffs
requirements specified in QAMS 005/80 which has been updated to the "EPA
requirements for Quality Management Plans", EPA QA/R-2.  While this plan sets forth
Quality Program requirements, project plans and work plans are used to define  project-
specific customer requirements.

This QA Management Plan is divided into three volumes:

  Volume 1  MSL administrative and management requirements
  Volume 2  Marine and Environmental Chemistry QC and technical requirements
  Volume 3  Marine Ecological  Processes QC and technical requirements

Implementation of the policies and requirements specified in the MSL Quality Assurance
Management Plan and the associated MSL procedures will provide defensible and
credible data enhancing the quality of MSL products and services.
R.M. Ecker
MSL Manager
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 OBaltelle
  . . . Putting Technology To Work
  Marine Sciences Laboratory
  QUALITY ASSURANCE MANAGEMENT PLAN
                  VOLUME 1
May 2000
              Battelle Marine Sciences Laboratory
                1529 West Sequim Bay Road
                Sequim, Washington 98382
                   (360)681-3645
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                      Battelle Marine Sciences Laboratory
                 QUALITY ASSURANCE MANAGEMENT PLAN
                                VOLUME 1

                         Concurrences and Approvals
D. Coffey                                     Date
Quality Assurance Officer
360-681-3645
E.A. Crecelius                                 Date
Marine and Environmental Chemistry
Technical Group Manager
360-681-3604
R.M. Thorn                                    Date
Ecosystem Processes and Restoration
Technical Group Manager
360-681-3669
J.A. Ward                                     Date
Ecotoxicology and Risk Assessment
Technical Group Manager
360-681-3669
R. M. Ecker
MSL Manager
360-681-3602
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                     Battelle Marine Sciences Laboratory
                QUALITY ASSURANCE MANAGEMENT PLAN
                              VOLUME 1
                               Contents

                                                      Issue Date Rev.
1.0   INTRODUCTION	1/2000   2
     1.1    QUALITY ASSURANCE MANAGEMENT PLAN
     1.2    POLICY STATEMENT
     1.3    OVERVIEW OF PROGRAM
     1.4    SCOPE

2.0   ORGANIZATION AND PERSONNEL	 1/2000   3
     2.1    ORGANIZATION
     2.2    RESPONSIBILITIES
     2.3    PERSONNEL QUALIFICATIONS AND EXPERIENCE
           2.3.1  Responsibilities
           2.3.2  Training
           2.3.3  Documentation
           2.3.4  Improper, Unethical or illegal Actions

3.0   FACILITIES AND EQUIPMENT	5/2000   4
     3.1    FACILITIES
     3.2    EQUIPMENT

4.0   PROCUREMENT AND CONTROL	5/2000   4
     4.1    MATERIAL PROCUREMENT AND CONTROL
     4.2    SUBCONTRACTORS

5.0   PROJECT PLANNING DOCUMENTS	 1/2000   1
     5.1    RESPONSIBILITIES
     5.2    CONTENT AND FORMAT
     5.3    APPROVAL AND DISTRIBUTION
     5.4    DATA QUALITY OBJECTIVES

6.0   STANDARD OPERATING PROCEDURES	 1/2000   2
     6.1    SCOPE AND PURPOSE
     6.2    CONTENT AND FORMAT
     6.3    RESPONSIBILITIES
     6.4    REVIEWS AND APPROVALS
     6.5    DISTRIBUTION AND CONTROL
     6.6    MODIFICATION AND REVISION

7.0   LABORATORY  DOCUMENTATION AND RECORDS	1/2000   1
     7.1    DOCUMENTATION
     7.2    RECORDS
8.0   SAMPLE CONTROL	1/2000   2
     8.1    PROCEDURES
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     8.2   RESPONSIBILITIES

9.0   QUALITY CONTROL	5/2000
     9.1   INTERNAL QUALITY CONTROL CHECKS
     9.2   APPROVALS BY OUTSIDE AGENCIES
           9.2.1 Certifications
           9.2.2 Performance Evaluation

10.0  DATA REDUCTION, REPORTING, AND VALIDATION	1/2000
     10.1   DATA REDUCTION
     10.2   REPORTS
     10.3   DATA VALIDATION
     10.4   MSL DATA AUDIT PROCESS
     10.5   CONFIDENTIALITY

11.0  VERIFICATION ACTIVITIES	5/2000
     11.1   ASSESSMENTS
     11.2   DATA AUDITS
     11.3   QA REPORTS TO MANAGEMENT
     11.4   CORRECTIVE ACTION
12.0  QUALITY IMPROVEMENT	1/2000
     12.1   TECHNICAL PERFORMANCE
     12.2   ASSESSMENT ACTIVITIES
                             APPENDICES

A    LIST OF ACRONYMS	1/2000   0

B    BATTELLE MSL PERSONNEL	5/2000   4

C    BATTELLE MSL STANDARD OPERATING PROCEDURES	5/2000   4
                                  in
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                                                                           Section: 1
Battelle Marine Sciences Laboratory                                               Revision: 2
Quality Assurance Management Plan                                              Date: January, 2000
Volume 1                                                                    Page 1 of 3

                                    1.0  INTRODUCTION

1.1 QUALITY ASSURANCE MANAGEMENT PLAN

The purpose of this Quality Assurance (QA) Management Plan (QAMP) is to describe Battelle's QA
Program as implemented within the Marine Science Laboratory (MSL). This QAMP summarizes
elements of quality assurance and the quality control (QC) activities routinely used to perform work by
collecting accurate and precise data consistent with project objectives. This QAMP has been designed to
meet the requirements of many of the MSL's clients and addresses elements of the Environmental
Protection Agency's (EPA's) Quality Assurance Management Staffs (QAM's) "EPA Requirements for
Quality Management Plans", EPA QA/R-2, the Navy QA Program and the requirements for the National
Environmental Laboratory Accreditation Program (NELAP). While this plan establishes the quality
assurance program requirements, Quality Assurance Project Plans (QAPjPs), sample analysis plans and
"kits" assembled at the time of sample receipt, are used to define any project specific quality requirements
not contained in this plan.

A copy of this QAMP is available to each staff member, who is expected to be aware of, and perform his
or her assignments in accordance with, the QA requirements stated in this document. The signature
page at the front of the QAMP indicates MSL  management's review, consensus and approval.

To ensure that the QAMP remains current, it is reviewed annually and updated as needed.  If major
changes are needed, the entire document is re-issued; if only minor changes are  needed, only the
affected sections are updated. The document control header in the upper right hand corner of each page
signifies that the document is controlled.  Upon revision of the document (or selected sections), the
effective date is updated and the revision number incremented by one. The revisions are reviewed and
approved as described below and distributed  to the staff. The QAMP will be issued by the MSL Quality
Assurance Officer.

1.2 POLICY STATEMENT

The commitment of Battelle to quality assurance is reflected in the following statements from the Battelle
Pacific Northwest National Laboratory (PNNL) policies:

   •   We are committed to provide services and products of the highest quality consistent with the needs,
      expectations, and resources of our customers.

   •   We are committed to continuously improving our processes, systems and capabilities so that we
      can increase the technology-based value of products delivered to our customers.

In accordance with these principles, the MSL  has developed a QA Program to assure that all activities
affecting the quality of data or products produced for clients are thoroughly planned and coordinated by
project teams.  The policy of the MSL is to ensure that all data generated, processed, or used in
completing each task are scientifically valid, legally defensible, and of known and acceptable quality. As
part of PNNL, the MSL is committed to the corporate policy of providing quality products and services and
committed to their clients to ensure that sampling and analytical procedures are properly executed,
sample integrity is not compromised, all QC procedures are implemented and recorded, and only valid
data is reported. To attain this goal, the MSL has implemented the QA Program summarized in section
1.3.
1.3  OVERVIEW OF PROGRAM
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                                                                             Section:  1
Battelle Marine Sciences Laboratory                                                Revision: 2
Quality Assurance Management Plan                                               Date: January, 2000
Volume 1                                                                      Page 2 of 3

The objective of the MSL's QA Program is to provide clients with quality products and services. A critical
element in providing quality products is the maintenance of a QA Program that provides for conducting
activities in a planned and controlled manner, thereby permitting the verification of quality performance.
The consistent delivery of products of acceptable and documented quality requires commitment and
adherence to QA and QC principles and procedures throughout the performance of each task. A
commitment to quality is an integral part of every employee's job at the MSL.  In addition, the MSL
recognizes that formal functions are necessary to assure Battelle Management and it's clients that the
work performed and the technical products produced meet client needs and conform with their specific
data quality objectives and requirements.  These formal functions are QA and QC. QA  includes all
systems designed to assure MSL management and the client that data were collected, processed, and
interpreted in accordance with the requirements of the planning documents; that all aspects of work
performance,  including data generation and analysis  are adequately documented; and that all data are
accurate and fully traceable. For this system to be effective,  each individual must understand his or her
role in implementing the program. The responsibilities, authorities,  and accountabilities with the MSL QA
Program are defined in Section 2.0. QC functions  include all activities that are designed to assess or
control precision and accuracy of measurements and data. QC functions involve performance of
procedures necessary to attain and document the prescribed standards of performance in all
measurement and data collection processes.

One of the first steps of the planning process is the development of data quality objectives (DQOs) (refer
to Section 5.4).  DQOs provide the criteria needed  to design a study, and once determined, become part
of the project planning documents (Section 5.0). In addition to the objectives, the project planning
documents define the methods, personnel, schedule, and deliverables associated with the project. The
project planning documents are supported by standard  operating procedures (SOPs), which are detailed
documents that describe the approved methods for instrument calibration, data collection,  processing,
reduction and reporting (Section 6.0).  Planning also involves ensuring that staff members are fully
qualified and trained to perform their responsibilities (Section 2.0) and that facilities and  equipment are
adequate and appropriate for their use (Section 3.0).  Procurement  of qualified subcontractors (Section
4.0) is also a key consideration during  the project planning stage.

A major component of the work performed by the MSL  involves the  collection and analysis of samples for
chemical, biological, and physical parameters. A sample control system is essential to ensure that the
history of each sample is documented  and verifiable (Section 8.0).  QC activities are implemented during
the performance of the work to measure and control the quality of the product (Section 9.0). Additional
methods of quality assessment are data validation  and  document reviews (Section 10.0) and QA
verification activities (Section 11.0). Deficiencies noted during the assessment process  are reported to
management who take the necessary remedial action to bring the system into compliance (Section 11.3).
Quality improvement processes are implemented to ensure that problems identified are  solved, and do
not recur (Section 12.0).

1.4 SCOPE

Battelle MSL comprises three technical groups: Marine  and Environmental Chemistry, Ecotoxicology and
Risk Assessment, and Ecosystem Processes and Restoration. These groups provide a wide range of
contract research services related to environmental programs, primarily related to the marine
environment.  The QA program defined in this document applies to all projects performed by Battelle
MSL,  both for external clients and other components of Battelle.

The services and products provided by Battelle MSL are used by our clients for a variety of purposes,
including defining  baseline environmental  conditions,  assessing environmental effects, as evidence in
litigation, and  as the basis for regulatory decisions. The diversity of projects demands a flexible QA
program that is cost-effective, yet meets the needs of the client and the standards of Battelle MSL. This
document describes the framework of Battelle MSL's QA Program and defines the minimum standards
that apply to all  projects.  This QAMP is supplemented by SOPs and project planning documents (i.e.,
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QAPjPs, work plans, toxicity testing plans). MSL procedures provide detailed descriptions of QA
activities, as well as the QC requirements for routine technical procedures. Project planning documents
define the specific quality objectives for projects and describe the procedures necessary to attain those
objectives.

This QA Management Plan is divided into three volumes:

   Volume 1    MSL administrative and management requirements
   Volume 2    Marine and Environmental Chemistry QC and technical requirements
   Volume 3    Marine Ecological Processes QC and technical requirements
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                           2.0 ORGANIZATION AND PERSONNEL

This section describes the organization of the MSL and defines the associated responsibilities,
authorities, and accountabilities.

2.1 ORGANIZATION

QA at MSL is an interdisciplinary line management function. MSL's responsibility assignments are that 1)
quality is achieved and maintained by those who have been assigned responsibility for performing work,
and 2) quality achievement is verified by those not directly responsible for performing the work. The
organization of Battelle MSL is illustrated in Figure 2.1.

The QA Officer has the authority and organizational freedom to identify quality problems, to initiate,
recommend or provide solutions, and to verify implementation.  All verification activity reports are made
available to line and project management. Line and project management are responsible for identifying
and assuring implementation of corrective action to all deficiencies.

Any MSL employee can initiate a stop work on the basis of a safety or quality concern.  The  immediate
supervisor shall be immediately notified of the concern and the shall initiate investigative activities or
initiate implementation of corrective actions.

2.2 RESPONSIBILITIES

Quality Assurance Officer

The QA Officer provides overall direction to, and management of, all Battelle MSL QA activities. Specific
responsibilities include

   •   Developing the QAMP and updating it, as needed, to reflect Battelle MSL policies and procedures

   •   Developing project budgets for QA activities and reviewing proposals for adequate and appropriate
      QA requirements

   •   Assisting project managers in defining the QA/QC procedures to be used during  a project

   •   Administering  a training program  related to QA policies and procedures

   •   Scheduling, planning, and conducting verification activities (assessments, data audits) of projects
      and facilities

   •   Preparing written reports summarizing the results of verification activities for distribution to project
      managers and MSL management

   •   Participating in, or coordinating, inspections and audits conducted by clients and regulatory
      agencies

   •   Preparing periodic status reports  of QA activities and verification results for MSL management

   •   Reviewing and approving technical procedures, project planning documents, and reports

   •   Preparing SOPs of QA activities
   •   Scheduling annual SOP review, distributing SOPs, maintaining  an SOP log, and archiving historical
      SOPs
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   •   Conducting training sessions on QA functions and activities.

The MSL QA Officer is part of the Battelle Process Quality Department located in Richland, WA and
reports to the supervisor of that Department. The MSL QA Officer does not report to anyone at the
Sequim facility, thereby attaining independence.

Marine Sciences Laboratory Manager

The MSL Manager provides overall management of the MSL and has responsibility for all the laboratory's
operations.

Technical Group Leader

Technical Group Leaders are responsible for ensuring the quality of products produced within their group.
Specific responsibilities include

   •   Ensuring that all activities related to meeting the data quality objectives defined in the MSL QAMP
      are being performed

   •   Providing sufficient resources, including both time and staff, to meet project and laboratory
      objectives

   •   Ensuring that all products produced from their group are reviewed and approved according to
      Battelle MSL policy before being released

   •   Ensuring that all projects have adequate project planning documents prior to initiation

   •   Promptly and appropriately correcting deficiencies noted during QA verification activities

   •   Ensuring that any SOPs that are required within the group are written, reviewed, and revised
      accordingly

   •   Identifying and addressing training  needs

Project Manager

The Project Manager has overall responsibility for the management of project activities. Specific
responsibilities include

   •   Administering and supervising all project tasks to ensure that all project objectives are met, on time,
      within budget, and of appropriate quality

   •   Preparing project planning documents and ensuring that the plans are reviewed and approved
      according to MSL policies

   •   Ensuring that the project objectives are communicated to project personnel and that project
      personnel are trained to perform any procedures unique to the project

   •   Reviewing all project reports and deliverables

   •   Addressing project-specific deficiencies that are identified during verification activities
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Laboratory Supervisor

Laboratory supervisors provide the day-to-day oversight activities of the laboratory.  Specific
responsibilities include

   •  Organizing equipment, staff, and materials

   •  Providing technical direction in the performance of tasks

   •  Resolving day-to-day problems, including instrument operation, calibration and use concerns and
     ES&H issues

   •  Reviewing records and data associated with the tasks under their direction for accuracy, validity
     and completeness

   •  Communicating with the project manager and advising him/her of problems, progress and needs

Staff Member

Each staff member has the following responsibilities:

   •  Performing work to the specified procedures in  conformance with the project planning documents,
     applicable SOPs,  and Battelle MSL policies, including ethical and legal responsibilities

   •  Identifying safety and quality concerns and informing the appropriate supervisor

   •  Communicating to the appropriate manager any deviation from established procedures or issues
     requiring corrective action

   •  Defining  appropriate QA requirements for purchased items and services

Contracts/Business  Representative

   •  Providing acquisition, contracts, and related business support to the MSL that assists in meeting
     the strategic goals and objectives of the  MSL and its clients

   •  Assisting staff in ensuring that the proposal preparation process  meets the goals of the MSL

   •  Ensuring that QA  requirements are specified  in  procurement documentation

ES&H Representative

   •  Overseeing and implementing core ES&H support services (Environmental Compliance, Safety,
     Health, and Training) to ensure laboratories and staff compliance with regulations

   •  Ensuring and assessing that proper waste handling, safety measures, and training are being
     performed by and for staff in conjunction with work performed at the MSL.

Environmental and Safety Engineer and Radiation Safety Officer

   •  Managing laboratory water and ventilation supply and discharge systems in compliance with
     environmental and health  regulations and in support of lab missions
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   •   Managing lab radiation safety program in compliance with regulations and in support of lab
      missions

2.3  PERSONNEL QUALIFICATIONS AND  EXPERIENCE

The quality of MSL products depend, in part, on the competence and expertise of the staff involved. It is
MSL policy that all individuals involved in the conduct or supervision of projects (including laboratory
technicians, field personnel, toxicolegists, analysts, data-processing personnel, supervisors, project
managers, and QA staff) must have the necessary education, training, or experience to perform their
assigned tasks. This objective is achieved by hiring personnel with the appropriate qualifications and
providing continual training and opportunities for  professional growth.

A summary of experience and qualifications is  documented on the Qualification and Training form and
placed in the individual's training file.  In addition, a list of personnel and an associated biosketch is
maintained for each employee and are shown in  Appendix B of this QAMP. Biosketches are revised as
needed.

2.3.1  Responsibilities

The MSL Manager is ultimately responsible for ensuring that appropriately qualified personnel are hired,
resources for training are allocated, and that appropriate training and professional growth are provided,
and records of training are maintained. Within  a  group, these responsibilities rest with the Technical
Group Leader.

Each individual's supervisor is responsible for identifying specific training needs,  ensuring that the
employee receives the necessary training to perform his/her assigned tasks, and assigning personnel to
project tasks in accordance with their experience and skill.

Each individual  is responsible for completing required training and submitting training records and
certificates to their supervisor, for updating their biosketch as needed, and for identifying and completing
additional training that may be required, but was  not assigned.

2.3.2  Training

Specific training requirements are contained in procedure, MSL-A-006, Marine Sciences Laboratory
Training. Training begins the first day of service  and continues throughout a staff member's term of
employment.  Introductory seminars on Battelle policies and organization, QA,  ethical and legal
responsibilities,  and Environment, Safety, and Health (ES&H) are presented during  an orientation
program.  Technical training begins prior to work being performed, through reviews  of procedural
documents and  demonstrations by experienced personnel.  Introductory courses are augmented by
general and project-specific train ing that is conducted periodically. All personnel assigned to projects
receive training to acquire the necessary skills  to perform their responsibilities. Technical training is
accomplished through a variety of approaches, including
   •   Direct hands-on training. Training is accomplished by reviewing procedural documents (e.g.,
      SOPs, project work plans), proficiency testing, and supervision by experienced personnel. Each
      MSL procedure includes the training requirements associated with that procedure, including any
      proficiency tests.

   •   Project kickoff meetings. Kickoff meetings  ensure that all project personnel are aware of the project
      objectives and the methods to be used to accomplish the objectives. This also includes field safety
      training at the beginning of each sampling  period.
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   •   In-house technical seminars. These seminars, which are available to all personnel, are conducted
      by MSL staff or guest speakers and generally cover current projects or related research programs.

   •   Continuous education through a tuition reimbursement program.

   •   Attendance of professional meetings and outside workshops.

ES&H training is provided to each employee who works in the laboratory or whose responsibilities expose
them to potential risk or hazard. Training includes chemical, physical, biological, radiological, and
mechanical hazards. Training is conducted and coordinated by the MSL ES&H Representative.

QA training is conducted by the QA Officer. Briefings and one-on-one training on general or  project-
specific topics related to QA (e.g., sample custody, data validation, Good Laboratory Practices [GLPs])
are conducted as needed.  A Battelle on-line training module titled, Quality Program Training (course
#1366) is available. The employee completes the training activity and prints a training completion  form
that must be signed  and submitted to the training department to obtain credit. The signed form is
evidence that the employee has read; acknowledges, and understands their personal QA responsibilities.

2.3.3 Documentation

Records of training and qualifications include the following:

   •   MSL training assignments
   •   Certificates attesting to the attendance or completion  of external courses
   •   Resumes and biosketches
   •   ES&H Records

Original records of training and qualifications are maintained by the Technical Group Managers. Copies
of technical training records are forwarded  to the QA Officer.

2.3.4 Improper, Unethical or illegal Actions

Training courses in ethical and legal responsibilities including the potential punishments & penalties for
violations are provided by Battelle via on-line computer training. The applicable course title and number
are Battelle Standard of Business Ethics and Conduct, course number 1062.  The employee  completes
the training activity and must score 80% or better. The module allows the successful employee to print a
training completion form that must be signed and submitted to the training department to obtain credit.
The signed form is evidence that the employee has read; acknowledges, and understands their personal
and legal responsibilities including potential punishments & penalties for violations; and provides the
required training documentation.
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Battelle Marine Sciences Laboratory
Quality Assurance Management Plan

    iBaflelle
     Putting Technology To Work
     Marine Sciences Laboratory
                                                                 Section: 2
                                                                 Revision: 3
                                                                 Date: January, 2000
                                                                 Page 1 of 6
                                               Marine Sciences Laboratory
                                                       Manager
                                                      R.M. Ecker
                                  ES&H
                                D.S. Coffey
                         Business Administration
                              J. H. Slater
                                                                       Quality Assurance
                                                                       D.S. Coffey
                                                                    Facilities and Operations
                                                                         J.A.Nimmo


Marine and Environmental
Chemistry
E.A. Crecelius





Business Development
Ecotoxicology and
Risk Assessment
TBD





Ecotoxicology
J.A. Ward


Data Management
   C.R. Suslick
     Inorganic Laboratory
         C. W. Apts
                                                             Ecosystem Processes
                                                                & Restoration
                                                                 R.M. Thorn
                         Mercury Laboratory
                            B.K. Lasorsa
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                             3.0  FACILITIES AND EQUIPMENT

Pacific Northwest National Laboratory is a research and development laboratory operated by Battelle
Memorial Institute, Pacific Northwest Division (Battelle), a non-profit organization. Among the entities that
operate Department of Energy (DOE) National Laboratories, Battelle is the only entity that holds a Use
Permit contract with the U. S. Department of Energy in addition to its operating contract.  Battelle is the
only DOE Management and Operating Contractor that actually owns a significant amount of our own land
and buildings, rather than occupying exclusively government-owned property. The method of obtaining
contract research business under the Use Permit is to prepare and submit technical or research
proposals to potential clients. Battelle MSL  is part of the  PNNL, operated for the U.S. DOE by Battelle
Memorial Institute under Contract DE-AC06-76RLO.

3.1 FACILITIES

Battelle MSL is located in Sequim, WA on 125 acres fronting Sequim Bay, and consists of 40,000 square
feet of laboratory and office space housed in two buildings - a beach facility containing bioassay
laboratories, and an  upland facility for analytical laboratories and office space.  The facilities support
approximately 40 scientists and support staff and about 15 on-site contractors and graduate research
students.

Biological  Laboratories

Two bioassay laboratories provide 5,300 sq  ft of space for studies requiring flowing seawater. Four
separate distribution systems supply seawater and/or freshwater to the laboratories.  High quality, Class
AA seawater is obtained from Sequim Bay through an all-PVC system with two independent intakes.  A
redundant system of three pumps provides a continuous supply of filtered and unfiltered seawater to
experimental tanks.  An emergency diesel generator ensures continuous seawater supply and other
essential services in the event of electrical failure.  Furthermore, the system is checked daily every 2 to 4
hours while experiments are in progress. A  16,000-gal reserve tank provides filtered seawater to the wet
laboratories for up to 18 hours in the event of failure of all three pumps.  Seawater at ambient
temperature (9-11 °C) can be provided at a rate of 250 GPM, and  up to 20 GPM of seawater can be
supplied at temperatures ranging from 0-38°C through a chiller and gas-fired heat exchange system.
Fresh water is also supplied to the laboratories  from uncontaminated groundwater reservoirs.

Holding and breeding facilities fora variety offish, shellfish, and freshwater, estuarine, and marine  plants
are provided in these laboratories and in outdoor tanks. All water leaving the seawater laboratory is
passed through a treatment system to ensure no impact is made on the receiving environment.

Analytical  Chemistry Laboratories

Analytical laboratories in the beach facility consist of two general purpose bioassay preparation
laboratories occupying approximately 1,000  sq  ft. These laboratories provide space and  equipment for
conducting measurements supporting the bioassays, such as water quality parameters, pH, dissolved
oxygen, temperature, and salinity. They also provide work stations for microscopy and space for sample
storage and  preservation.

Analytical laboratories in the upland facility consist of two  banks of five fully-equipped  chemistry
laboratories, each occupying 600 sq ft.  The chemistry laboratories are equipped with  state-of-the-art
instrumentation and supplies, including an array of mass spectrometers, chromatographs, analytical
balances, rotary evaporators, freeze-driers, microwave digestion systems, sonicators, freezers,
refrigerators, and drying ovens. The following are some of the specialized purposes that these
laboratories serve:

General Laboratory for Rceipt of Smples and Peparation for Analysis:
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General Organic Chemistry Laboratories for preparation of sample extracts for gas chromatography and
mass spectroscopy, and analysis for physical properties of sediment. A high-performance liquid
chromatography (HPLC) system, with variable-wavelength UV detector, fluorescence detector, auto
injector, fraction collector,  integrator, and data reduction system is available for specialized sample
preparation.

Analytical Services

Gas Chromatography and Mass Spectroscopy Laboratory for conducting specialized cleanup procedures
and analyses of oil and grease, polynuclear aromatic hydrocarbons, phenols, polychlorinated biphenyls
by congener or Aroclor,  pesticides, and organotin compounds.  The laboratory contains three
microprocessor-controlled high-resolution gas chromatographs: two Hewlett-Packard Model 5890A, and
one Model 5890 Series 2 equipped with a mass spectrometer.  Detectors available include
flame-ionization detection  (FID), flame photometric detection (FPD), and electron-capture detection
(ECD). The laboratory also contains a VG Fison Model TRIO 1000 GC/LC/Mass Spectrometer.

Metals Chemistry Laboratory for preparation of samples for metals analyses and determination of basic
chemical and physical properties of samples such as pH,  salinity, grain size, total volatile solids, and
percent dry weight, as well as instrumentation for counting radioisotopes used in age-dating sediments.

Inorganics Laboratory for metals analyses using  a Perkin  Elmer Elan 5000 Inductively Coupled Plasma
Mass Spectrometer and two atomic absorption spectrophotometers:  a  Perkin-Elmer Model 5000 and a
Perkin-Elmer3030 equipped with a background corrector, graphite furnace or flame capability,
autosampler, and printer and rapid-response  recorder.

Specialized Mercury Analysis Laboratory for ultra-trace level (picogram/liter) analysis of mercury in water
samples, and parts per trillion analysis of total and methylmercury in water, tissue, and sediment using
analytical methods developed at Battelle MSL.

Specialized Sulfide Analysis Laboratory for trace level determination of inorganic sulfur compounds in
water and sediment using  gas generation, purge and trap, and gas chromatography coupled with flame
photometric or photoionization detection.

Physical Oceanography Laboratory for gas exchange research, contains a whitecap simulator with  two
large tanks, a Dantec laser-doppler velocity and particle analyzer, electronics shop, computer-controlled
data loggers, and extensive test equipment and chemical  instrumentation.

Computer Facilities

Battelle MSL staff use PC, Macintosh, and UNIX-based computer systems connected via a local area
network. The systems are linked to other on-  and offsite hardware composed of some 6700 workstations
and servers, minicomputers, database and file repositories, Web servers, and supercomputer facilities.

Battelle MSL has access to the numerous online databases accessible through Dialog Information
Services. Commercial databases such as BIOSIS (Biological Abstracts),  Chemical Abstracts, Oceanic
Abstracts, Enviroline,  and  many others can all be accessed quickly by computer at MSL.  Other
databases such as Aquatic Sciences and  Fisheries Abstracts, National Technical Information Service, ad
ToxChem (Toxicology and Chemistry) are accessible through the University of Washington libraries.
Through such access to information, literature searches can be conducted efficiently at MSL.

Safety and Security
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The safety of MSL employees is of paramount importance. Therefore, the MSL buildings are equipped
with structural safety features (e.g., fire doors and extinguishers, emergency lighting systems), alarm
systems which serve to alert the staff in the event of emergencies (e.g., fire/smoke alarm), and
engineering controls designed to minimize exposure to potential hazards (e.g., fume hoods).

The security of the facility is an important consideration because of the type of work performed by the
MSL.  Access to the MSL grounds and buildings is controlled through a card-access and lock and key
system. During business hours, all visitors must enter through the main lobby and sign in with the
receptionist. Selected areas within the facility are secured at all times and their access limited to
authorized personnel.  These areas include the walk-in cold room used for sample storage, the records
storage area, the solvent shed, and the GLP data archives.  Procedure, MSL-A-011, MSL /Access
Control, describes the process in detail.

Computer security is a function of the PNNL network and is administered from facilities located in
Richland, WA. Staff have individual responsibility to back up files, instruments and data bases at
regularly scheduled  intervals which are described in the MSL procedure, MSL-D-004,  Data Reporting,
Reduction, Back Up, and Archiving.

3.2 EQUIPMENT

The quality of MSL products is directly related to the validity of the data produced. To produce valid data,
equipment must be properly operated, maintained, and calibrated. Preventive maintenance and primary
maintenance is  provided through the Battelle Facilities and Operations staff located in Sequim, but
located organizationally in Richland, WA. The MSL maintains a wide variety of equipment related to the
collection and analysis of chemical, biological, and physical oceanographic parameters. To support the
generation of data of known and acceptable quality, the following general guidelines are implemented

   •   The appropriate and necessary equipment,  instruments, and supplies must be available in
      adequate quantities to perform the proposed work.  Spare parts for critical components are
      maintained to  minimize downtime.

   •   Measuring and testing equipment is properly handled and stored to maintain accuracy.

   •   All equipment involved in the collection and analysis of environmental data is operated, maintained,
      and calibrated according to approved procedures and specified schedules.

   •   Equipment is serviced regularly by qualified individuals, either trained in-house personnel or
      through service contracts with the manufacturer or an authorized representative. For example,
      balances  are cleaned  and calibrated by a Battelle Preferred-Supplier, and analytical instruments
      have service contracts with manufacturers such as Perkin-Elmer. Most support equipment (e.g.,
      ovens, refrigerators, freezers, hoods) servicing is done internally by Battelle Facilities and
      Operations staff.  When problems arise that can not be corrected internally, external contractors or
      manufacturer's representatives are contacted.

   •   Written records of all instrument maintenance, calibration, testing, and inspection are maintained.
      Maintenance records  contain a description  of the operation or problem, the remedial action taken (if
      necessary), date, and the  person responsible.

   •   When  equipment or instrument maintenance is required, equipment is monitored by facilities to
      ensure correct operation.  Analytical instrument operation after maintenance is monitored by the
      responsible analyst by running a calibration curve and assessing results of standard reference
      materials  (SRMs) .

   •   All calibrated equipment is suitably marked to indicate calibration status.
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      Written direction on equipment operation (e.g., operating manual, manufacturer's instruction, and
      SOPs) are maintained with the equipment and are available to personnel using the equipment.

      All balances are calibrated annually orsemi-annually by an approved metrology laboratory. All
      balances are checked daily prior to use with certified weights by a designated laboratory technician.
      These performance checks are documented in balance logbooks.

      All cold-storage facilities are monitored daily with a calibrated or certified thermometer. Acceptable
      temperature ranges for refrigerators is 4 ±2 °C and for freezers is -20 ±10 °C. The ultra-low freezer
      is maintained at -68 + 5 °C.
Specific equipment lists for the Marine and Environmental Chemistry Group are contained in Volume 2.
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                           4.0  PROCUREMENT AND CONTROL

4.1 MATERIAL PROCUREMENT AND CONTROL

Examples of items that generally have a significant influence on the quality of MSL work, and therefore
generally need defined quality requirements are the following:

•   Standards and reference materials
•   Reagents, chemicals and solutions
•   Animals and feed
•   Computer software and hardware, and
•   Some miscellaneous items such as designed equipment

Procurement activities at MSL are guided by procedure, MSL-A-012, Procurement, which should be
consulted to determine appropriate QA requirements before initiating procurement actions.

Miscellaneous Procurements

Miscellaneous procurements of items that have a significant influence on the quality of MSL work,
generally need defined quality requirements. When the purchaser does not know if quality requirements
should be specified, the  rule is to request the MSL Quality Assurance Officer or representative to make
this determination and document it as a note, letter or email.

Material Receiving Inspection

When the MSL orders materials that require certification (i.e., standard or certified reference materials
(SRMs, CRMs), standards,  precleaned sample containers, etc.), a request for certifications shall be made
on the purchase order. Standards and reference materials must be traceable to the National Institute of
Standards and Technology  (NIST; formerly the National Bureau of Standards or NBS) or other nationally-
recognized standard (e.g., American Society for Testing Materials [ASTM]).  The traceability must be
documented  by a certificate or label that verifies this link.  The traceability documentation must be
received and found to be acceptable by MSL staff before material use.  Acceptance of these items and
certifications shall consist of verifying that the lot numbers on the certifications and the jar and/or boxes
are the same. Approval shall be indicated by a signature and date of signature on the certificate.
Pending receipt of this documentation and its acceptance, affected material must be segregated to
prevent inadvertent use.  Certifications received will be maintained in the Project or Central files.

Reagent and Standard Inventory  Procedures

The procurement of reagents, chemicals and solution should include requirements for shipping stocked
 inventory materials with the longest period to the expiration date (i.e., the freshest material) possible, with
 lot numbers specified. In some cases where extremely high purity material is requested, a request for
 purity documentation may be necessary.

Procurement procedures should require that a manufacturer's recommended expiration date  be provided
with every standard material. If manufacturer's expiration dates are not provided, the laboratory must
assign an appropriate expiration date, based on professional judgement and in consideration of the shelf
life for similar materials at similar concentrations.  The technical basis for each such determination must
be documented in the project file by the responsible analyst, and approved by the Project Manager.

MSL follows the Pacific Northwest National Laboratory's (PNNL's) Standards-Based Management
System (SBMS) requirements for logging in reagents, chemicals and solutions into the associated
Chemical Management System (CMS). This system provides the PNNL Laboratory with policies and
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procedures regarding tracking and inventory, storage, and disposal of completed samples and analytical
wastes as well as chemical use and disposal. The CMS is used to provide an up-to-date inventory to
facilitate emergency response, monitor the location of various classes of materials and identify situations
where acceptable limits for the building/facility determined by the assigned chemical hazard group and
fire zone might be exceeded before a violation occurs.  An assigned Sample Inventory Coordinator
provides bar codes  for each chemical item when it is received and assigns it to a location. The item then
is tracked  in the CMS until disposal.  The system is also used to ensure that facility limits based on the
chemical hazard group and the assigned fire zone determination are not exceeded.

Organisms and Feed

The procurement of organisms and feed for bioassays should include requirements for chain of custody
of animals during shipping and documentation of any available feed analyses, feed storage
recommendations, and expiration dates so that feed quality can be monitored.  Animal shippers should be
requested  to document conditions of animals and environmental parameters (temperature) at the time of
shipping for comparison with conditions encountered at the time of receipt. In some cases, it might be
important to include QA requirements for a minimum/maximum thermometer or temperature strip in the
cooler at the time of shipping. Requirements regarding common carriers, Saturday delivery acceptability
and locations, and other details might also be specified in QA requirements documents.

Computer Software and Hardware

QA requirements for the procurement of hardware must ensure that hardware is compliant for periods
where clock or time information settings provided by the manufacturer might affect future hardware
operation.  QA requirements for the procurement of software should follow some general guidelines:

•  Commercial software that has been developed under the manufacturer's QA Program and fully tested
   before release is preferable to other types of software developed under lesser or no QA Program
•  Documents necessary to demonstrate that software was developed using a Life Cycle approach such
   as User's Manuals shall be requested when software is ordered.
•  Licenses that come with the software and original documentation should be requested, obtained and
   protected.
•  Software that requires a signed site license agreement can only be purchased by individuals with
   appropriate delegations.
•  Hardware/Software that exceeds $5,000 can only be purchased with appropriate management
   approvals.
•  Software procured as a product under a subcontract must specify detailed QA requirements for
   software development and use, and provide plans for testing, verification and validation tests and
   include acceptance criteria.

Solvent Storage  Policies

Solvents used in the laboratory are in containers of 4 liters or less. On receipt they are logged in, bar-
coded, and tracked, as are all chemicals. No more than a working day's supply of flammable or
combustible solvents is permitted out of flammable storage in a laboratory; at the end of the day, these
materials must be returned to flammable storage. Large flammable storage cabinets, located in an area
separate from the building, are used for storage of solvents that exceed the lab's storage capacity.

Waste Disposal

Hazardous wastes at the MSL are managed in accordance with Washington State Department of
Ecology's Chapter 173-303 WAC, "Dangerous Waste Regulations." The MSL is a "less the 90-day
storage" facility and a medium-quantity generator and, as such, fulfills all the requirements outlined in the
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regulation regarding proper labeling, designating, inspections, and timely disposal of hazardous waste.
Staff who generate/handle waste are trained annually in waste management procedures.

Section 1.3 of Volumes 2 and 3 of this QAMP addresses specific requirements for sample disposal.

4.2 SUBCONTRACTORS

MSL policy for sending to work to subcontractors is that MSL routinely does not subcontract analyses that
can be performed  in house.  In some situations this could occur, if the capacity of the laboratories is not
adequate to meet  a project deadline. MSL does contract project analyses when this approach is a
project-specific requirement.  All staff are expected to clearly and completely specify appropriate
requirements for purchased goods and services consistent with project needs. This is done by developing
a statement of work that includes, number of samples, sample matrix, required procedure, applicable
holding times, quality control sample requirements and project data quality objectives, and data
deliverables.  Materials, equipment,  and  services shall be delivered at reasonable costs, with  delivery
times consistent with the specific project and business needs of the Laboratory. Costs and commitments
will be recorded in a timely and accurate manner. Battelle MSL is ultimately responsible for the quality of
work performed by its subcontractors.  Therefore, procedures have been established to ensure that
subcontractors involved in environmental data collection programs are qualified to perform their
responsibilities,  that project objectives, methods, and responsibilities are clearly defined and
communicated,  and the work performed  is monitored to assess conformance to the project specifications.

The approved supplier list maintained  by the WA DOE is one source for identifying appropriate
subcontractors to provide performance evaluation samples (refer to Section 9.2). PNNL also  maintains a
list of approved  suppliers for analyses, and this list is used as a starting  point to define subcontractors.  If
the subcontractor  is not on an approved  list, then the subcontractor must have demonstrated  or provided
proof of the necessary technical capabilities, facilities, resources, and experience to perform the specified
tasks. The contract specifies the costs, technical services, QA requirements, deliverables, and schedule
of performance. The contract must include a Statement of Work (SOW) in sufficient detail so  that the
scope of work, methods, quality assurance requirements, responsibilities, deliverables, and due date are
clearly understood by the MSL and the subcontractor.

In terms of QA, each subcontractor must have a written description of its QA program, that defines the
policies, procedures, and responsibilities implemented to ensure the quality of the data or other products
provided to the MSL. More detail may be found in procedure, MSL-A-012, Procurement. In addition, it is
expected that the following standards will be met.

   •   If appropriate, the subcontractor must have an  internal QC  program. Analysis of internal QC
      samples (the type and frequency to be specified in the SOW) must be performed in conjunction with
      analysis of MSL samples and the results reported with the sample data.

   •   Written descriptions of all procedures involving environmental data collection and generation must
      be available and implemented.

   •   Equipment used to generate data must be maintained, calibrated, and operated according to written
      procedures.
   •   Subcontractor personnel must be properly trained and qualified.

   •   Adequate procedures for record management and reviewing documents and data products must be
      in place and implemented.

Whenever deemed appropriate by the Project  Manager and the MSL QA Officer,  the MSL QA Officer
shall perform audits of subcontractors. These audits may include data audits, inspection of facilities, or
inspection of project activities.
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                                                                            Section:  5
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                          5.0 PROJECT PLANNING DOCUMENTS

Project planning documents (e.g., work plans, QAPjPs, toxicity testing plans, health and safety plans, field
sampling plans) are documents that describe the objectives of a project and the methods, organization,
and QA and QC activities necessary to meet the goals of the project.  It is Battelle MSL policy that each
project conducted by the MSL must have a planning document that adequately describes the work to be
performed, has been approved by the Project Manager, and is in place prior to the start of work.

5.1 RESPONSIBILITIES

It is the responsibility of the Project Manager to:

   •   Ensure that a project work plan, QAPjP or both  is  prepared prior to work initiation and that it meets
      the requirements of the MSL, the client, and any applicable regulations

   •   Approve the plan and to obtain any other necessary approvals

   •   Ensure that the planning documents are made available to project personnel

   •   Ensure that project participants are adequately trained to perform the assigned work and that the
      training is documented as required.

Each staff member involved in the project is responsible for performing his/her task(s) in conformance
with the planning documents.  MSL staff members are also responsible for notifying their supervisor or
the appropriate manager of any deviations to the procedures/methods specified in the planning
documents.

The QA Officer is responsible for reviewing project planning documents for conformance to relevant
regulations and MSL policies.

5.2 CONTENT AND FORMAT

A significant amount of the work performed by the MSL  is conducted for the U.S. EPA. EPA requires that
all environmental data-collection activities conducted for the EPA must be covered by a QAPjP.
Therefore, all  project planning documents prepared for the EPA must adhere to  specific content and
format requirements, as dictated by the EPA office involved.  Protocols written for studies conducted
under Food and Drug Administration (FDA) or EPA GLP standards must adhere to the specifications of
21 Code of Federal Regulations (CFR) Part 58 (FDA), 40 CFR Part 160 (EPA/ Federal Insecticide,
Fungicide, and Rodenticide Act [FIFRA]), or 40 CFR Part 792  (EPA/Toxic Substances Control Act
(TSCA), as applicable.

In the absence of client-driven requirements, the MSL has established minimum standards for project
work plans. These are, as applicable

   •   A descriptive title, client name, Battelle project number,  and effective date

   •   The identities of the project manager, task leaders, and  other key project personnel, including
      subcontractors
   •   A statement of the general goals and the specific  DQOs of the project

   •   A description of the experimental design and procedures

   •   A description of the QA and QC procedures that will be  applied to the project tasks
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   •   The project schedule, including milestones and deliverables

   •   A description of the types of data to be recorded

   •   A statement of deliverable requirements

5.3 APPROVAL AND DISTRIBUTION

At a minimum, the planning documents must be approved by the Project Manager. Additional approvals
may be required by MSL policy or by the client.  All planning documents shall be approved before work is
started on the project.

The project planning  document is distributed, or made available to, all key personnel involved in the
project and  to the QA Officer.  It is expected that all work will be conducted according to the planning
documents.  Modifications to approved planning document procedures should be made only with the
concurrence of the Project Manager.

5.4 DATA QUALITY OBJECTIVES (DQO)

DQOs are defined as the criteria needed to design an environmental data collection program. DQOs are
developed from a multi-step, reiterative process that involves,  project management, technical staff, and
the individuals who will be  using the data to make decisions. The DQO process entails

   •   Stating the problem to be resolved, including limitations  of time and resources

   •   Identifying the decision that will be made using the data

   •   Identifying inputs to the decision, including the environmental measurements needed and the
      criteria for taking action

   •   Specifying how the results will  be summarized and used

   •   Specifying acceptable error rates (i.e., limits on uncertainty)

The objective of the DQO development process is to design a cost-effective program that will provide the
necessary amount and type of sufficient-quality data.

During the development of DQOs, the parameters of accuracy, precision, completeness, comparability,
representativeness, and sensitivity are commonly considered when measuring data quality. These
qualitative and quantitative parameters are described below.


   Accuracy is a measure of the bias of a system or measurement.  It is the closeness of agreement
   between an observed value and an accepted value.

   Precision is the degree of mutual agreement among individual measurements of the same property
   obtained under similar conditions.

   Completeness is the amount of data collected as compared to the amount that was needed to ensure
   that the uncertainty or error is within acceptable limits.

   Comparability is  a measure of the confidence with which one data set can be compared to another.
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   Representativeness is the degree to which data accurately and precisely represent a characteristic of
   a population.

   Sensitivity is the capability of methodology or instrumentation to discriminate among measurement
   responses for quantitative difference of a parameter of interest.

Once the acceptable error rate has been defined, the program's QA requirements are developed in
response. The specific types of QC samples used to measure data quality are discussed in Section 9.0
ofthisQAMP.

Further definitions and applications of DQOs for chemical and biological analyses are contained in
Volumes 2 and 3 of this QAMP.
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                        6.0  STANDARD OPERATING PROCEDURES

6.1 SCOPE AND PURPOSE

Battelle MSL's policy requires that SOPs be written for all routine environmental measurement
procedures that are associated with data collection and analysis and related QA/QC activities.
Procedures that are not routine, or are unique to a project, are described in project planning documents
or in written protocols included  in the project files.  Subjects that are covered in SOPs include, but are not
limited to:

   •   Sample collection
   •   Sample handling, preservation, and storage
   •   Chain-of-custody procedures
   •   Sample analysis
   •   Bioassay toxicity testing
   •   Equipment use, maintenance, and calibration
   •   Record management
   •   Data reduction, processing, and validation
   •   QA verification activities

SOPs are  documents that describe procedures that must be followed to ensure the integrity and quality of
data.  SOPs serve a multi-purpose function, including to

   •   Reduce the introduction of errors and variables by  ensuring the consistent use of appropriate
      procedures

   •   Communicate to the necessary people (e.g., client, project personnel) how the work will be
      conducted

   •   Increase the effectiveness of training by clearly and consistently communicating the approved
      method of performing a procedure

   •   Provide a historical record of the work performed

   •   Provide a basis for data comparability

   •   Provide a basis for maintaining  reproducible results and producing defensible data.

A list of all MSL procedures is contained in  Appendix B of Volume 1 of this QAMP.

6.2 CONTENT AND FORMAT

Each SOP must be clearly written and include sufficient detail to clearly describe the operation to be
carried out so that a qualified individual can perform the procedure. However, it should be flexible
enough to accommodate expected variations while maintaining the integrity of the procedure and the
quality of the data being generated. SOPs  covering equipment must include descriptions of calibration,
operation, and maintenance requirements.  Procedural SOPs must contain sections on preparation,
procedures, calculations, and quality control.  Equipment and procedural SOPs must also include a
discussion of the safety concerns associated with the equipment or procedure. All SOPs must state the
objective or application of the SOP topic and must stipulate the requirements for the successful
completion of training. Specific requirements for content and format are stipulated in SOP, MSL-A-003,
Guidelines for SOP Format and Control.
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6.3 RESPONSIBILITIES

Each Technical Group Leader is responsible for ensuring that the routine procedures needed within their
group are written and for providing resources for their preparation. The Technical Group Leader also is
responsible for approving all procedures produced within his/her group.

The individual preparing the SOP is responsible for ensuring that the SOP completely and accurately
describes the procedures, is based on sound scientific principles or recognized procedures, and conforms
to the MSL standards for procedure documentation as specified in MSL-A-003, Guidelines for SOP
Format and Control).

The QA Officer is responsible for

   •   Assigning each SOP a unique number and entering it into the SOP controlled document log
   •   Reviewing and approving all SOPs
   •   Distributing approved SOPs
   •   Maintaining historical files of SOPs

6.4 REVIEWS AND APPROVALS

Draft procedures must go through a formal review and approval process. At least one technical reviewer
of record is assigned.  Additional technical reviewers are encouraged for new procedures. The MSL QA
Officer and the Technical Group Manager are also reviewers and provide final signature approval. Users
should be included in the review process to ensure that the procedure is accurate and able to be
implemented. Review comments for all reviewers can be submitted to the procedure file.  Review
comments and any documentation of comment resolution by the technical reviewer of record (who
provides signature approval) should be submitted to the QA Officer to be maintained in the procedure file.
The SOP is reviewed, and when satisfactory, is signed and dated, at a minimum, by the following people:

•  Author - who becomes the procedure subject matter expert
•  Technical Reviewer - should be someone who will be able to assure that the procedure is technically
   adequate, complete and correct.
•  MSL Quality Assurance Officer (not required for safety procedures)
•  MSL Manager for non-technical procedures or the appropriate Technical Group Manager for technical
   procedures.

6.5 DISTRIBUTION AND CONTROL

Copies of all current MSL procedures are kept in the QA Office and are available to all MSL staff upon
request. In addition, MSL Procedure Manuals, which contain copies of all current MSL Procedures are
issued to managers and professional-level staff and are located in areas that are accessible to all staff
requiring their use. All procedures used  at the MSL will be controlled by the QA Officer.  Original SOPs,
both current and historical versions, are maintained  by the QA Officer.

6.6 MODIFICATION AND REVISION

Changes to SOPs must be controlled to ensure documentation and traceability to the modification.  SOP
modifications fall into three categories: one-time modifications, interim changes, and major changes.


One-Time Modifications
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A "one-time" modification is used when the change is for a one-time use of the procedure.  This situation
is often guided by a customer request.  It is not intended to result in modifications to other copies or future
uses of the procedure.
If the change is significant, then the user should document the modification and associated justification,
obtain the approval of the project manager, and proceed with the modified work activity.

If the change is not significant, then the user should document the modification and associated
justification, proceed with the modified work activity, and later have the change reviewed by the project
manager.

The modification and justification shall be documented  in an  appropriate place such as the data sheet,
daily log or other raw data documentation.

Interim Changes

An interim change may be  made when a procedure requires a modification and formal revision is not
prudent or timely. This can be used for minor changes (minor procedural changes, typographical errors,
etc.) or changes of a more substantive nature.  The user should document the interim change; and the
line or project manager who required the procedure should approve the change. The interim change
should be communicated to all users of the procedure,  and the user should then initiate the review and
approval  process to revise the procedure if the change is substantive or permanent.

Major Changes

Major changes (e.g., new equipment specifications, maintenance procedures, and major procedural
changes) require a revision of the procedure.  Major revisions must go through the writing of a formal
review draft and receive approval consistent with the requirements specified in  Section 4.3 above.,
before being implemented. All revised procedures retain their original  number assignments but are
issued a new revision number.
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                   7.0  LABORATORY DOCUMENTATION AND RECORDS

A critical component in the generation quality products is proper record keeping and the maintenance of
the records after project completion. Documentation must be sufficiently detailed so that the data are
traceable and program data could be reconstructed  based on the project records. These records must be
maintained in a secure location and must be identifiable and retrievable.

7.1 DOCUMENTATION

It is Battelle MSL policy that data generated during the course of a project must be capable of
withstanding challenges to its validity, accuracy, legibility and traceability. To meet this objective, data
are recorded in standardized formats and in accordance with prescribed procedures.  All staff members
whose responsibilities include recording data must be aware of, and adhere to, the procedures during the
performance of their work.  Briefly, data must be entered onto data sheets or in project notebooks directly,
promptly, and legibly. All entries must be made in reproducible ink, and must be initialed  and dated by
the person making the entry.  Changes or corrections to data must not obliterate the original entry, but
must be indicated with a single line through the original entry.  All changes or corrections  must be
accompanied by the initials of the person making the change, the date, and when not obvious, an
explanation of the change. Specific requirements for documentation are included in procedures MSL-D-
001, Recording Data on Data Sheets and Laboratory Notebooks and MSL-D-004, Data Reporting,
Reduction, Back Up, and Archiving.

7.2 RECORDS

The MSL data archive system is designed to ensure that materials are stored in an orderly manner under
secure conditions, and may be easily and promptly retrieved should the need arise. Specific details are
found in procedures MSL-D-003, Archiving of Records, data, and Retired SOPs and in MSL-D-004, Data
Reporting, Reduction, Back Up, and Archiving.

All material generated during a project conducted  by the MSL must be archived upon completion of the
project. All records necessary for the interpretation  and evaluation of project data, including planning
documents, raw data and other documentation, correspondence, and reports, should be retained.  The
Project Manager is  responsible for ensuring the project materials are collected, organized, and forwarded
to the archives at the end of the project.  MSL policy is to retain electronic data files for five  years, unless
otherwise specified by customer request. Hard copy data are stored indefinitely as per MSL procedure
MSL-D-003, Archiving of Records, Data, and  Retired SOPs which primarily addresses GLP requirements.
Archives are controlled access (locked) storage rooms. Data are stored and retrieved by project number.
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                                  8.0 SAM RLE CONTROL

Sample control is the formal system designed to provide sufficient information to reconstruct the history of
each sample. This system involves procedural, record keeping, and organizational components and is
critical for any environmental program that is generating data that may be used for regulatory decisions or
in support of litigation.

8.1 PROCEDURES

The MSL sample control system encompasses the following elements

   •   Upon collection or preparation, each sample is assigned and  labeled with a unique identification
      code that allows it to be tracked through analysis and reporting. Assignment of identification
      numbers is on a group or project-specific basis.

   •   Standard forms are used to document the history of each sample, including collection, storage,
      preservation, processing, and analysis.

   •   Samples are received, logged in, stored, and archived according to SOP MSL-A-001, Sample Log-
      in Procedure.

   •   Samples are stored in controlled or secure areas.

   •   Transfer of the custody of samples (both within the MSL and to  outside agencies) and the removal
      of samples in and out of storage is documented in accordance with SOP MSL-A-002, Sample
      Chain of Custody.

Specific sample custody requirements for the Marine Chemistry and Ocean Processes Group and the
Marine Ecological Processes Group are addressed in Volumes 2 and  3 respectively.

8.2 RESPONSIBILITIES

Sample custody responsibilities must  be clearly defined  and understood by all personnel  involved for the
system to be effective. Samples are considered to be in a person's custody if

   •   The samples are in a person's actual possession
   •   The samples are in a person's view after being in that person's  possession
   •   The samples were in a person's possession and then were locked or sealed to prevent tampering
   •   The samples are in a secure area

The sample collector is responsible for the proper collection, preservation, and labeling of samples, and
for documentation of sample history and custody in the field. The sample collector also is responsible for
packaging the samples for shipment and for arranging for transportation to the laboratory.

Responsibilities of the laboratory sample custodian include  receiving and inventorying the samples,
placing them in storage, and completing the documentation associated with these  procedures. The
laboratory sample custodian also is responsible for informing the Project Manager of the samples' arrival
and for promptly notifying him/her of any broken, missing, or compromised samples.
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                                  9.0 QUALITY CONTROL

QC activities are performed by technical personnel during the conduct of the project. The purpose of
these functions is to measure the quality of the data and if necessary, adjust the measurement system so
that the specified level of quality is attained.

9.1  INTERNAL QUALITY CONTROL CHECKS

The following are common types of QC procedures implemented by the Battelle MSL Marine Chemistry
and Ocean Processes Group.

   Method blanks - Method (or procedural) blanks are prepared in the laboratory using the same
   reagents, solvents, glassware, and equipment as the field samples and accompany the field samples
   through analysis.  Method blanks serve as a means to measure contamination associated with
   laboratory processing and analysis.

   Matrix spikes - Matrix spike  (MS) samples are field samples that are spiked in the laboratory with
   target analytes and analyzed under the same condition as the field samples. Matrix spikes provide a
   measure of the recovery efficiency of the analytical method and are generally analyzed in duplicate
   (matrix spike/matrix spike duplicate [MSD]).

   Blank spikes - Blank spikes  are similar to matrix spikes but are prepared by spiking the target
   analytes into a clean  matrix (e.g., deionized water).  Blanks spikes also are used to  measure the
   recovery efficiency of the analytical method, but without the interference of the matrix.

   Laboratory replicates - Laboratory replicates consist of splitting a single sample or compositing and
   splitting two or more samples in the laboratory, and  subsequently processed and analyzed as separate
   samples.  Laboratory replicates serve as a measure of the error associated with the analytical process.

   Standard reference  materials (SRM) - SRMs are materials for which certain properties have been
   certified by a recognized authority.

   Reference samples  - Reference samples are samples for which selected properties are  known,
   generally through historical analysis.  Reference samples are used as a benchmark for similar
   analyses.

QC samples may also be collected  in the field to monitor contamination and to assess sampling error.
Common field-related QC samples include

   Equipment blanks - Equipment blanks are prepared in the field using the freshly decontaminated
   sampling equipment.  Deionized water is poured over and through the equipment, collected in an
   identical sampling  container,  and shipped to the laboratory for processing and analysis. Equipment
   blanks measure the contamination associated with the entire sampling and analytical process.

   Split samples - Split samples are obtained by compositing sample material in the field and dividing
   the material into separate containers for processing and  analysis.  Split samples are used to assess
   the total error associated with sampling and analysis.  If split samples are sent to separate laboratories
   for analysis, intelaboratory variation may also be obtained.
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   Field replicates - Field replicates are two or more separate samples that have been collected from the
   same sampling point.  Field replicates also serve to measure the error associated with the entire
   sampling and analytical process, including variation inherent in the sampled media.

QC checks are associated with biological toxicity testing (independent recounting of sample, reference
toxicity tests, establishment of acceptable water quality measurement ranges) and data processing
(proofing or double entry/comparison programs). The specific QC procedures, frequency of performance,
and criteria for acceptance for all environmental data  collection procedures are defined in SOPs or in the
project planning documents.

The immediate monitoring of QC results allows the data collection process to be  continually compared to
pre-established  acceptance criteria and corrected as  necessary.  In addition, assessment of QC results is
a critical component of the data validation process (Section 10.0) and is used to interpret the
accompanying sample data and to judge its acceptability and usefulness with regard to the project DQOs.
QC results are reported with the project data.

Within the Marine and Environmental Chemistry and Ecotoxicology and Risk Assessment Groups, control
charts have been established for selected QC analyses (i.e., inorganic and organic analytes and
reference toxicity results).

See Volumes 2  and 3 of this QAMP for specific requirements for quality control samples, quality control
criteria and control charts.

9.2 APPROVALS BY  OUTSIDE AGENCIES

MSL is accredited by the states listed below. As part of the state accreditation programs, MSL
participates in several chemistry laboratory intercomparison and certification programs that require
analysis of performance evaluation samples and also participates in inter-laboratory toxicology
comparisons whenever offered. Battelle MSL also is  routinely audited by its clients.
State
Florida
New Jersey
South Carolina
Washington
Wisconsin
Accreditation Organization
Department of Environmental Protection (DEP)
Department of Environmental Protection (DEP)
Department of Health and Environmental Control (DHEC)
Department of Ecology (WA DOE)
Department of Natural Resources (DNR)
Accreditation through the Navy QA Program and NELAP are in progress.  In the past, MSL has
participated in the following Performance Evaluation Studies:

   EPA - Water Pollution (WP) Laboratory Performance Evaluation Study
   EPA - Water Supply (WS) Laboratory Performance Evaluation Study
   Mercury Intercomparison Program (MIP)
   International Atomic Energy Agency (IAEA) - World Wide Intercomparison for Trace Elements
   National Oceanic and Atmospheric Administration (NOAA) National Status and Trends


In many cases these programs have ended (e.g., WP, MIP), and have not been replaced by new
programs. Currently PE samples are purchased from an approved vendor on the list maintained by the
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WA DOE. MSL is currently participating in the CalFed Mercury QA Program, a study to demonstrate
comparability among laboratories. Results are expected in early 2000.

9.2.1 Certifications

Certification programs are based on the demonstration of a function quality program, the existence of
planning documents and procedures, the successful analysis of external performance samples at least
twice per year, and in some cases, periodic on-site assessments. Specifics of MSL certification is
described in MSL-A-013, Laboratory Accreditation and PE Sample Analysis.  MSL maintains the following
documentation to meet these requirements:

               •      Quality Assurance Management Plan
               •      Comprehensive QA Plan (for the State of Florida)
               •      Procedures in the following general areas (numbers of procedures)
                  .   Quality Assurance
                  .   Administration
                  .   Documentation, Records, and Reports
                  .   Organic Chemistry
                  .   Inorganic Chemistry
                  .   Conventional Chemistry
                  .   Water Quality Instrumentation
                  .   Toxicological Testing
                  .   Facilities,
                  .   Safety, and
                  .   Work Practices

MSL participates in performance  studies at the required frequency as per MSL procedure,  MSL-A-013,
Laboratory Accreditation and Performance Evaluation Sample Analysis.  Customers are provided with the
results of recent performance studies on request.

9.2.2 Performance Evaluations

MSL analysts are degreed staff operating analytical instruments on a daily basis. The dedication of
analytical staff to the specific procedures for which they are responsible, their level of training and, daily
QC assessments of proficiency through the analysis of blank samples, sample replicates, SRMs, and
MSs combine to make the results produced by MSL highly defensible, accurate, precise, and repeatable.
MSL is a  specialty laboratory, providing its customers with relatively low detection limits for environmental
samples.  Daily proficiency is monitored at the bench level, at the level of data assessments performed on
sample sets by the analyst and the MSL Data Coordinator (data validation), and at the level of the MSL
QA Officer who provides data quality verification. Internal PE samples may be provided as blind or
double blind samples to the analyst by a Project Manager, the Marine and Environmental Chemistry
Manager, or the MSL QA Officer.  The source for internal PE samples is generally previously analyzed,
archived PE samples.  Internal PE samples provide an indication of analyst proficiency and instrument
performance and are used to return serviced equipment to full operation, or to provide an instrument
check when preventive maintenance has been performed.  Blind internal PE samples are also used to
test initial method/instrument proficiency when training new staff.

External PE sample results are used at MSL as an  external verification of analyst proficiency and as a
means of comparison with ones peers.  An "Unacceptable" data evaluation through the PE sample


program is taken seriously and the entire system is reviewed for anomalies.  If an "Unacceptable" data
evaluation is obtained, various parts of the analytical process (e.g., digestion, dilution, instrument
injection)  are investigated using the archived PE  sample. In addition, once the results from the previous
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study are received, then that archived sample has a known certified mean and range and can be used (if
used < 6 moths from sample receipt) as an internal PE sample or a QC verification sample. Most
available external PE samples that can be purchased are aqueous. MSL participates in programs to
analyze sediment and tissue samples (e.g., NOAA Trace Metals Intercomparison) whenever offered.
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                 10.0  DATA REDUCTION, REPORTING, AND VALIDATION

10.1  DATA REDUCTION

Reduction of raw data shall be accomplished using established techniques. The calculations required to
perform the reduction of data may be performed manually or with the aid of automated data processing
systems. In either case, the procedures for the testing and analysis of samples or the QAPjPs will specify
the calculations and the mode for raw data processing.  If manual processing is to be used for data
validation, then the procedure or QAPjP will provide the calculation method and the units for reporting
derived values. In order to reduce the potential of errors in data transcription the manual transfer of data
will be minimized.  All calculations performed manually will be checked for accuracy by someone other
than the person who performed the original calculation.  Data validation checks shall be documented by
the signature and date of the reviewer.  Separate documentation is acceptable, provided traceable
records are maintained. For automated data reduction methods, the accuracy of calculations will be
verified through the use of standards or test case inputs with known resultant values.

10.2  REPORTS

Technical reports are the primary product produced by the MSL. To ensure the quality of the reports, two
mechanisms are used: (1) the selection of technical staff with the appropriate mix of technical and writing
skills to produce data products and reports, and (2) a formal system of review and correction.

MSL policy requires that all deliverables prepared for clients must be submitted to an internal review
before being released to the client. The document is then reviewed as per MSL-Q-002, Quality
Assurance Audits of Reports, for technical content, conformance to QA policies and procedures, and
editorial correctness.

The purpose of the technical review is to evaluate the document for technical quality (including scientific
validity and logic),  conformance to client expectations, and for agreement with MSL policies.  This review
is performed by a senior technical staff member selected for familiarity with the technical discipline of the
work being reported.  The QA review is conducted by the QA Officer and encompasses  accuracy,
completeness, adequacy of QA issues, and conformance to applicable standards, including federal
regulation (when applicable), project planning document requirements, and MSL policies. Editorial review
addresses grammatical correctness and consistency of style and format.

The reviewer's comments are communicated in writing to the author who revises the document, if
necessary. The revised document is then sent to the Technical Group Leader or designee for final
approval  prior to its release.

10.3  DATA VALIDATION

Prior to their use, data must be validated. Validation is defined  as the process through which data  are
accepted or rejected and consists of proofing, verifying, editing, and technical reviewing activities.  At the
MSL,  data validation is described in MSL-D-004, Data Reporting, Reduction, Back Up, and Archiving, and
it is considered a technical function and must occur prior to the data being audited by the QA Officer
(Section 11.2).

Data validation occurs at multiple levels as data are collected and processed:

   •   Individuals recording data during field or laboratory operations are responsible for reviewing their
      work at the end of the day to ensure that the data are complete and accurate.
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   •   Analysts and instrument users are responsible for monitoring the instrument operation to ensure
      that instrument has been properly calibrated.

   •   Laboratory Supervisors and Project Managers are responsible for reviewing analytical results and
      supporting documentation to assess sample holding times and conditions, equipment calibration,
      and sample integrity. As an additional measure of acceptability, the results of QC samples are
      compared to the project  DQOs.

   •   Technical staff are responsible for reviewing the data for scientific reasonableness.

   •   All  manual entries into databases and spreadsheets are verified, either through proofing or by
      double entry/comparison programs.

   •   All  calculations performed by hand are checked for accuracy.

Data that do not meet the pre-established criteria for acceptance may be flagged, not reported, or
reported with an explanation of the limitations, at the discretion of the Project Manager.

10.4  MSL DATA AUDIT PROCESS

The MSL data audit process is primarily a data verification activity that is described in MSL-Q-005, Quality
Assurance Data Audits. However, verification of validation activities also  occurs. Complete data
packages including all kit information, hard copies of instrument outputs, and summary data sheets are
provided  to the MSL QA Officer or designee for review. Analytical data packages are reviewed to a
checklist.  Project notebooks, because of their variability,  are not reviewed to a checklist. However, the
review process is essentially the same. Data are reviewed to ensure that the data are accurate,
traceable, defensible, and complete, as compared to the planning documents and/or project
requirements. The audit procedure is a randomized  check that involves comparing selected reported
values to the original data. This check  can either be performed randomly or on  a statistical basis. Results
of the data audit are documented either on the checklist from MSL-Q-005 or in  a summary statement.
Concerns that can be corrected will be corrected before the data are released.  Deviations are required to
be summarized and provided to the customer.

10.5  CONFIDENTIALITY

MSL policy does not allow the  release  of customer data or project-related information to anyone except
the customer unless expressly directed by the customer or an authorized  representative.
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                             11.0  VERIFICATION ACTIVITIES

One of the policies of the MSL is to assure that the products generated, and the services performed by
the MSL meet the standards established by Battelle and its clients. The Self Assessment Program (SAP)
is the  MSL's performance measurement system. The SAP

    provides MSL staff and  management accurate technical, business and operational performance
       information that promotes early identification and resolution of problems that may impact
       achievement of the  MSL critical outcomes and objectives

    verifies conformance to  established requirements

    verifies effective conduct of activities to protect the environment and the health and safety of workers
       and the public

    contributes to ongoing improvement in performance.


The first process of the performance measurement system is determining the MSL's critical outcomes and
performance objectives and indicators.  The MSL's critical outcomes and associated performance
objectives and indicators are established by PNNL's Environmental Technology Division (ETD) and MSL
staff on an annual basis. The key performance objectives and indicators resulting from this process drive
the development of self assessment plans.

The second process of the performance measurement system is developing and implementing an
assessment plan. The MSL develops an annual assessment plan as part of ETD's self assessment
program. The assessment plan describes the assessment activities that the MSL performs to ensure that
plans  and controls are in place to achieve its objectives.

The third process of the performance measurement system is the overall evaluation of the MSL's
performance and is described in section 11.1.  The primary mechanism for evaluating this performance
measurement system is assessment activities. Assessment activities refer to the verification of
conformance to the MSL's SAP and include  line management assessments, QA assessments, and data
audits. During a QA assessment or data audit, the agreement between data and data quality objectives
or indicators with QA policy  documents  (e.g., QAMP, SOPs, project planning documents) is evaluated,
deficiencies are identified, and corrective action is taken.

The final step in the performance measurement system is to implement the  key improvement
opportunities that the evaluation processes identified (See Section 12). Improvement areas requiring
action are implemented as determined by the MSL Manager, Technical Group Leader and/or QA Officer.

11.1  ASSESSMENTS

As part of the MSL SAP, assessments are performed in accordance with the SBMS subject area,
Conducting and Using Results From Operational Assessments, by staff and line management to evaluate
the performance of the MSL. Assessment methods include, but are not limited to, walkthroughs,
procedure and program reviews, staff feedback, and safety, health, and environmental evaluations.

In addition, the QA Officer conducts QA assessments to assess that facilities, equipment, personnel,
methods, practices, records and quality control are in conformance to approved planning documents,
procedures, regulations, client requirements and Battelle policy. QA assessments are scheduled based
on a request from the MSL Laboratory Manager, the definition of critical phase  inspections by project
managers or MSL customers, and by scheduling by the MSL QA Officer when a new procedure  is
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implemented or significantly revised, when a new study type is initiated, or when data quality reviews
indicate technical systems problems.  At least 25 assessments per annum are the target.  External
assessments of suppliers are conducted through the Battelle Quality Process Division in Richland, WA
and are related to qualifying preferred suppliers.

QA assessments are formal or informal verification activities that are performed in accordance with
procedure MSL-Q-002, Quality Assurance Inspections ofMSL System and Study Activities and subject
area,  Conducting and Using Results From Operational Assessments. The  purpose of a formal QA
assessment is to determine verification with a requirement and includes formal corrective action and
follow-up.  If the assessment is determined to be informal, the purpose is to determine the status and to
report the factual evidence and is not intended to be a verification activity with formal corrective action
response, follow-up, etc.  Informal assessments are generally requested by MSL management to assess
the status of a particular activity.

A schedule of all QA assessments, which are not part of the MSL's self assessment plan, will be
completed by the QA Officer and, as needed, issued quarterly to the MSL Manager and the Technical
Group Leaders. This schedule will include verifications based on client needs, management requests
and routine internal verifications (i.e., checking standards logs, sample preparation forms,  QC checklists,
equipment calibration and maintenance, etc.).

11.2  DATA AUDITS

MSL policy requires that all environmental measurement data produced by the Technical Groups  must be
audited prior to their final release. The reported data are audited, using a process that ensures that the
data are complete, accurate, traceable, and defensible. Details of the data auditing process is
documented in SOP MSL-Q-005, Quality Assurance Data Audits.

11.3  QA  REPORTS TO  MANAGEMENT

Upon  completion of the QA assessment activity, the QA Officer prepares a  written report that specifies the
basis  of the assessment activity, identifies the type of assessment activity and phase covered, and
summarizes the results of the assessment activity. The report is signed and dated by the  QA Officer and
forwarded to the appropriate manager, who reviews assessment results and determines corrective action.
Each  deficiency must be addressed in writing. The Project Manager (when appropriate) and the
Technical Group Leader then sign and date the report and return it to the QA Officer for verification of the
responses.

Quarterly, the QA Officer will submit to the Technical Group Leaders and the MSL Manager a summary of
the past quarters QA activities. Subjects to be covered in the quarterly QA report as addressed in MSL-
Q-008, QA Reports to MSL Management, and shall include, but not be limited to, results of assessment
activities, results of performance evaluation samples, trends of deficiencies, and other important QA-
related issues.

11.4  CORRECTIVE ACTION

Typical corrective actions for exceeding the project-specified DQOs for chemistry analyses and bioassay
and aquatic toxicology tests are summarized in Section 5 of volumes 2 and 3 of this document. This topic
is also addressed in Section 12 below. In addition, individual  analytical procedures may contain
appropriate corrective actions for various routine problems. MSL procedure MSL-A-005, Deviations from
Established Requirements,  addresses an approach to differentiate between acceptable deviations that
will be reported to the client and formal deviations  requiring a greater level  of investigation to determine
the root cause, documentation and verification of corrective action implementation and the effectiveness
of
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actions designed to prevent recurrence. Deviations may be found during routine data validation or
verification activities, during an assessment or identified by any project participant. In most cases, the
MSL QA Officer and the Project Manager have the primary responsibility for evaluating the impact of the
deviation on data quality, and defining required corrective actions.  In some cases the client may also be
involved in this assessment.  Deviations and deficiencies and the assigned corrective actions are
documented on a Quality Problem Report (QPR, referto Exhibit 12.1 in the following chapter). It is the
Project Manager's responsibility to ensure completion of the identified corrective action by the expected
completion date, and to request independent verification (when required).

When there has been an impact on data, the Project Manager shall assure that there is a cross reference
in the raw data that indicates there is an associated QPR (i.e., referto the QPR on each of the impacted
data sheets, in the  laboratory record book, and in any other documents used to transcribe the information
or data).

Once a quarter, the MSL QA Representative shall present to MSL Management a summary of all QPRs,
any significant control limit data deficiencies, and an analysis of trends or recurring deficiencies as part of
the quarterly QA Report to Management.
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                               12.0 QUALITY IMPROVEMENT

Quality improvement is a critical aspect of the MSL Self Assessment Program and involves both
corrective action to identified deviations and continuous improvement processes.

The corrective action process involves determining, implementing, approving, and verifying the
appropriate remedial action. Corrective actions may be identified by technical personnel during the
course of work performance, or may be in response to assessment activities.

The continuous improvement process involves determining and prioritizing improvement areas,
implementing improvement action and documenting the disposition of each action.

12.1  DEVIATIONS

Each individual engaged in project activities should be alert to problems, deviations from approved
procedures, out-of-control events, or other issues that may require corrective action.  The appropriate
response is determined  by the event. SOP MSL-A-005, Deviations  from Established Requirements
provides methods for addressing deviations from MSL procedures, planning documents, and client
requirements.

Briefly, deviations are identified either as observations or quality problems as follows.

   Observations are defined as  incidences that require action or correction but are not considered
   ongoing, operational  problems.

   Quality Problems are defined as situations where the quality and usability of data, a process, or item
   are indeterminate (i.e., no objective evidence is available to substantiate data quality or to indicate that
   established procedures/requirements were met). Quality problems can be (1) repeated incidences of
   an observation, (2) repeated errors due to a flaw in the data generation or validation process, or (3)
   assessment issues that require a change in laboratory procedures or processes.

It is MSL  policy that all issues that may impact the quality of the data must be documented. The
documentation must clearly state the event and the corrective action taken in response, and must be
approved by the appropriate management representative. Acceptance of data that exceeds pre-
established criteria also  must be documented and justified.

Depending on the severity of the  deviation, the MSL QA Officer and the Project Manager will determine
how the deviation will be documented (i.e., through use of a  Quality Problem Report form (Exhibit 12.1)
per MSL-A-005, Deviations from Established Requirements. The MSL QA Officer and the Project
Manager will determine  if there is a formal deviation when one or more control limits are exceeded in a
data set.  In some cases, the customer may be involved in these discussions. Deviations from project
control limits will be identified in the narrative accompanying the data set or package or in a letter to the
customer, and the impact of the deviation addressed. The following are guidelines to resolving
deviations:

   •   All deviations from approved procedures, project planning documents or this QAMP will be
      documented.

   •   Issues that affect  cost, schedule, or performance of the project will be reported to the Project
      Manager. The Project Manager will then be responsible for evaluating the overall impact to the
      project and implementing the necessary corrective actions.

   •   Deficiencies identified through QA assessment activities will be brought to the attention of the
      Project Manager and the Technical Group Leader. Implementation of corrective action will be the
      responsibility of the Project Manager.
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   •   See Section 5 of Volumes 2 and 3 of this QAMP for additional information regarding corrective
      action of identified deviations.

12.2  ASSESSMENT ACTIVITIES

For all assessment activities, a system of notification and verification of corrective action is in place. An
assessment report is prepared and submitted to the appropriate Manager (Project Manager or Technical
Group Leader). The Manager reviews the assessment results to determine overall impact and  risk and
then determines corrective action and prioritizes the actions.  The Manager assigns the corrective actions
to individuals.  The  Managers ensures that the corrective action is tracked to completion and  as part of
completion, documentation is included that describes the justification for completion of the corrective
action. Issues that  in the manager's judgement require significant corrective action should be scheduled
for verification of that corrective action at a subsequent assessment.

Issues that in  the manager's judgement require process improvement instead of, or in addition to,
corrective action, are identified as such and any improvement actions are implemented and documented.
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                     EXHIBIT 12.1 Quality Problem Report Form
Originator: Date: QPR Number:
Project Number:
_ . _ _



Project Title:
Purchase Order Number/SOP/Work Plan:
10CFR830. 120 Related? Yes or No
Statement of the Deviation
Impact of the Deviation
Steps to Prevent Inadvertent Use of the Item or Process
Cause of Events Leading to the Problem
Planned Corrective Action for the Immediate Problem/Independent Verification Required? Yes or No
Planned Corrective Action to Prevent Recurrence/Independent Verification Required? Yes or No

Person Responsible for the Corrective Action

Last Name, First, MI


Approval of Planned Corrective Action

Cognizant Manager or Designee


Closing the Problem

Actions Completed as Planned

Name Date

Independent Verification Has Been Completed (if
required)

MSL QA Representative Date
Intermediate Distribution:
Final Distribution:
MSL QA Office
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                                   APPENDIX A
                                 List of Acronyms

ANWAP      Arctic Nuclear Waste Assessment Project
APDC        Ammonium pyrrolidinedithiocarbamate
AVS         Acid Volatile Sulfide

CCV         Continuing Calibration Verification
CFR         Code of Federal Regulations
CHP         Certified Health Physicist
CMS         Chemical Management System
CoC         Chain of Custody
CREM        Coastal Resource and Ecosystem Administrative Management
CRM         Certified Reference Material

DEP         Department of Environmental Protection
DHEC        Department of Health and Environmental Control
DO          Dissolved Oxygen
DOE         Department of Energy
DNR         Department of Natural Resources
DQO         Data Quality Objective

ECD         Electron-capture Detector
EPA         Environmental Protection Agency
ES&H        Environment, Safety, and Health
EPRI         Electric Power Research Institute

FDA         Food and Drug Administration
FID          Flame-ionization Detector
FIFRA        Federal Insecticide, Fungicide, and Rodenticide Act
FPD         Flame Photometric Detector

GC          Gas Chromatography
GFAA        Graphite Furnace Atomic Absorption
GPM         Gallons Per Minute
GLP         Good Laboratory Practices

HMC         Hazardous Materials Coordinator
HPLC        High-Performance Liquid Chromatography
HVAC        Heating Ventilation and Cooling System

IAEA         International Atomic Energy Agency
ICP-AES     Inductively Coupled Plasma - Atomic Emissions Spectrometry
ICP-MS      Inductively Coupled Plasma (Emissions) - Mass Spectrometry
ICV          Initial Calibration Verification
ID           Identification
MDL
Method Detection Limit
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                                   APPENDIX A
                                  List of Acronyms

MIP          Mercury Intercomparison Program
MS          Mass Spectroscopy
MSL         Marine Science Laboratory

NAUI         National Association of Underwater Instructors Technical Diving International
NBS         National Bureau of Standards
NELAP       National Environmental Laboratory Accreditation Program
NIST         National Institute of Standards and Technology
NOAA        National Oceanic and Atmospheric Administration

NPDES       National Pollutant Discharge Elimination System
NRCC        National Research Council  of Canada

PAH         Polycyclic Aromatic Hydrocarbon
PCB         Polychlorinated Biphenyls
PNNL        Pacific Northwest National Laboratory
PSEP        Puget Sound Estuary Program
PVC         Polyvinyl Chloride

QA          Quality Assurance
QAMP        Quality Assurance Management Plan
QAMS        Quality Assurance Management Staff
QAPjP        Quality Assurance Project Plan
QC          Quality Control
QPR         Quality Problem Report

REM         Registered Environmental Manager
RPD         Relative Percent Difference
RSD         Relative Standard Deviation
RSO         Radiation Safety Officer

SBMS        Standards Based Management System
SEM         Simultaneously Extracted Metals
SESP        Surface Environmental Surveillance Project
SIC          Sample Inventory Coordinator
SOP         Standard Operating Procedures
SOW        Statement of Work
SRM         Standard Reference Material

T            Temperature
TBT         Tributyl Tin
TDI          Technical Diving International
TSCA        Toxic Substances Control Act
UV
VIS
Ultraviolet (light)

Visible (light)
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WA DOE     State of Washington, Department of Ecology
WHP        World Hydrographic Global Measurement Program
WIPP        Waste Isolation Pilot Plant
WP          Water Pollution
WS          Water Supply
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                                    APPENDIX B
                           BATTELLE MSL PERSONNEL

The following is a list of MSL personnel and a summary of their current position, and length of
relevant experience. Educational background and work experience are documented on the
Qualification and Training form which is a part of each person's training file.

     Mr. Liam Antrim, has over 21 years experience in environmental science.  He has worked
on a variety of aquatic toxicity projects, focusing on acute and chronic toxicity testing of
industrial effluents,  the effects of contaminants in near-shore and urban sediments on marine
and freshwater organisms, and collection and toxicity testing of the sea-surface microlayer.  He
has participated in numerous sample collection projects in Puget Sound, the Gulf Stream,
Chesapeake Bay, and southern California for federal and industrial clients.  Mr. Antrim is
currently the MSL Dive Officer.

     Mr. Chuck Apts has been working on trace metal research at MSL for more than 29
years, contributing to studies involving the bioavailability of trace metals in marine ecosystems
and effects of trace metals in the sea-surface microlayer.  He has managed numerous projects
in the field of metal analysis, ranging from sedimentary samples from the Beaufort Sea prior to
oil-well drilling to the determination of the effects of dredging around  Oakland Harbor, CA.
Through  his work on these studies, Mr. Apts has gained considerable experience in field
sampling and trace metal analytical techniques using ICP/MS.

     Ms. Blythe Barbo is the MSL Marketing Information Specialist. She has nearly 9 years
experience at the MSL. Some of her duties include proposal coordination  and production,
marketing materials development, capability information organization, business intelligence
tracking,  database research, information distribution services, media and public relations, and
market and proposal communications.

       Mr. Michael Blanton specializes in the areas of water quality and ecotoxicology.  Other
areas of expertise include strategic planning, experimental design, and ecological
surveys/evaluations. Mr. Blanton participated in the Columbia River Comprehensive Impact
Assessment, which modeled fate and exposure of contaminants to various trophic levels in the
ecosystem and to humans; he has also participated in environmental exposure and risk analysis
programs for the Surface Environmental Surveillance Project (SESP), Hanford, Washington. He
recently investigated the potential injury to fall Chinook salmon from  exposure to  chromium
releases  to the Columbia River and the development of an Information Management System to
aid in ESA compliance under FIFRA for new agricultural chemical product registration. He is
currently the project manager for an Evaluation of the Environmental Effects of Synthetic -
Based Drilling Fluids on Coastal and Marine Waters. Mr. Blanton has 7 years of  experience at
Battelle Richland and joined MSL in October 1999.

       Ms. Susan Blanton joined MSL in October 1999.  She previously supported the Pacific
Northwest National Laboratory for 6 years as a Science & Engineering Associate II in the
Ecology Group within Environmental Technology Division. Her research has focused on
diverse salmonid issues in the Columbia and Snake River Basins. She has evaluated fish
screening facilities in the Yakima River Basin, supported hydroacoustic fish passage research
efforts at Snake and Columbia River hydroelectric projects,  studied the effects of gas
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supersaturated water on salmonids, contributed to preparation of environmental impact
statements, and conducted teacher workshops on numerous aspects of aquatic ecology.

     Ms. Elisabeth Smolski Barrows has over 22 years experience working environmental
science encompassing project management, analytical organic and inorganic chemistry, marine
and freshwater toxicity testing, and field work. She is currently involved with the environmental
assessment of dredged material disposal options in New York. She is currently managing
projects for the U.S. Army Corps of Engineers.  Ms. Barrows has been with Battelle for 15
years, with 9 of those years at MSL.

     Dr. Peter Becker, is a physical oceanographer who specialized in the description,
analysis, and modeling of physical processes in freshwater distribution and transport in the
Arctic Ocean. He is currently a post-doctoral research associate at the MSL, working on the
Arctic Nuclear Waste Assessment Project (ANWAP) for the Office of Naval Research.  During
his position as oceanographic consultant at the University of Washington, from 1974 to 1989,
his duties included head oceanographer on over 35 field projects.

     Ms. Linda Bingler, marine chemist, has been at MSL for 9 years and serves as a project
manager and provides support for sample digestion, distillation, and extraction. She has
researched the effective removal of contaminants by thermal and hydrocyclone processing.  As
part of the World Hydrographic Global Measurement Program (WHP), she managed Battelle's
portion of a 60-day cruise from Dutch Harbor to  New Caledonia to collect CTD and high-
accuracy measurements of anthropogenic and natural tracers. Ms. Bingler has taken shipboard
measurements of TCO2 in seawater using the SOMMA/coulometric system and participated in
World Ocean Circulation Experiment cruises as  part of the WHP global measurement program.
Ms. Bingler has also researched rare earth element nutrient complexation in seawater,
determination of formation constants for metal-nutrient complexation, and phytoplankton uptake
of rare earth elements over time.

     Ms. Amy Borde has been with the MSL since 1995. Her research has focused on
wetland ecology, specifically marine habitat assessment and restoration. She has conducted
reviews of wetland ecology and policy issues for EPA, contributed to long-term studies of habitat
change in PNW estuaries, supported eelgrass restoration efforts in Puget Sound,  provided GIS
support for numerous studies, and has acted as a teachers assistant for wetland ecology and
restoration classes.

       Ms.  Deborah Coffey is the MSL QA Officer and ES&H Representative. She has more
than 16 years of quality assurance experience supporting U.S. EPA and NQA-1 QA Programs
at the Corvallis Environmental Research Laboratory, and at Sandia National Laboratories
supporting the  Waste Isolation Pilot Plant (WIPP) program.  She joined Battelle in September
1999. She is responsible for overseeing all QA/QC aspects of the MSL's project performance,
such as developing QA planning documents, assessing and improving processes, ensuring that
all protocols are followed, and that data are accurately presented. She is an NQA-certified and
Lead Auditor and routinely conducts internal QA assessments to verify procedural compliance
and data acceptability.  Ms. Coffey reports to the Process Quality Department of the Battelle
Quality Division and is therefore, independent of MSL.
     Dr. Eric Crecelius, the Technical Group Manager of the Marine and Environmental
Chemistry Group, has over 20 years of experience in freshwater and marine geochemistry
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                                                                      Appendix B
Battelle Marine Sciences Laboratory                                           Revision: 4
Quality Assurance Management Plan                                           Date: May, 2000
Volume 1                                                               Page 7 of 7

studies with an emphasis on concentrations, fates, and effects of trace metals. Dr. Crecelius is
internationally recognized in the field of marine pollution and trace metal chemistry. He is
frequently an invited participant or session chairman for workshops or scientific meetings that
deal with arsenic speciation, marine monitoring, and the fate of contaminants in coastal waters.

     Dr. Val Cullinan, specializes in the statistical design, analysis, and interpretation of results
from multidisciplinary experimental research. Her research has addressed marine resources,
as well as agricultural systems, terrestrial  and aquatic ecosystems.  She specializes in
developing statistically efficient sampling designs to detect ecological change at landscape
levels of spatial heterogeneity.

     Ms, Mary Ann Deuth, is a technical specialist responsible for ongoing analyses for trace
amounts of mercury in tissue, sediment, and water.  She has been at the MSL for 5 years and
she is currently developing  proficiency with new mercury analyzers.

     Ms. Ann  Skillman Drum, has 20 years experience conducting research on biological
mechanisms of marine invertebrates and fist infectious diseases and cancer, environmental
pathology and toxicology, parasitology, and aquatic animal health management, disease
diagnosis and prevention.  Her areas of specialization include health management of salmon
and invertebrates, relationship of animal health to resource management, development of new
aquaculture techniques and aquatic animal drug registration studies conducting  under GLP.

       Mr. Richard Ecker returned to MSL in March 1999 to serve as the MSL  Manager. He is
the Associate Director of (CREM) Coastal Resource and Ecosystem Administrative
Management,  a joint venture of Battelle Duxbury and the MSL. He is also a Battelle Product
Line Manager for the Resource and Ecosystem Management Product Line, which  is dedicated
to finding solutions to complex environmental issues.  Prior to his current position as Product
Line Manager,  he was the Department Manager of the Water and Land Resources Department
and Product Line in the Environmental Technology Division managing a department of over  180
staff. He also previously managed the  Battelle Marine Sciences Laboratory for 6 years.  Dick
started with Battelle in 1978 and has been involved  in all aspects of the business;  business
development and marketing, deployment of technology, technical research and line
management.  Before his career with Battelle, Dick served with the Army Corps  of Engineers,
San Francisco District where he directed environmental projects.

     Mr. Paul  Farley, is responsible for high resolution acoustic survey and precision seafloor
mapping programs. He has formal training and more than 20 years of experience in side scan
sonar operations, high resolution seismic data acquisition,  interpretation and bathymetric
survey, and satellite and microwave navigation systems. He also supervises the
electronics/instrumentation shop where duties include trouble-shooting and repair  of various
analog and digital instrumentation and to design and construct various equipment  as needed.

     Mr. Tim Fortman is a technical specialist in organic chemistry who has participated in  a
variety of environmental pollution monitoring projects such as NOAA's status and trends, the
Exxon Oil Spill Herring study, and the EPA's Great Lakes assessment program. He also has
worked on all aspects of trace metal and organic contaminant analysis, and set up an
automated gel  permeation chromatography system  used as an advanced cleanup of organic
environmental analysis. In addition, he trains and supervises several technicians.  Mr. Fortman
is the MSL Acid Neutralization Drum Custodian and has been at MSL for 14 years.
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                                                                       Appendix B
Battelle Marine Sciences Laboratory                                            Revision: 4
Quality Assurance Management Plan                                            Date: May, 2000
Volume 1                                                                Page 7 of 7

     Mr. Brian Gruendell's expertise is in biologic oceanography.  His recent research has
focused on bioaccumulation and toxicity testing using amphipods and bivalve larvae, dredged
material evaluation, and field sampling efforts for private and Federal agencies. He also serves
as the MSL Hazardous Materials Coordinator (HMC).

     Mr. Tom Hausmann recently joined the staff of MSL after 2 years as a Bioremediation
Research Assistant Fellow at MSL under the Associated Washington Universities program.  He
is completing his thesis in Environmental Engineering and he will be providing support for
GC/MS analyses for the Marine and Environmental Chemistry Group.  Mr. Hausmann is a QA
Representative who is trained to perform data reviews.

     Mr. Lyle Hibler specializes in studies of contaminant transport in rivers, estuaries, the
open ocean, and groundwater.  He has developed and applied numerical computer models and
processing codes, and has been involved in the statistical and uncertainty analysis  associated
with numerical algorithms used by these types of models.

     Dr. Michael Huesemann, is involved in bioremediation research and project
management. His areas of specialization are hazardous waste soil and groundwater
bioremediation, including field applications of composting,  bioventing, and air-sparging
technologies.

       Ms. Lara Johnson joined MSL in December of 1999 as a Scientist Engineer Associate
I.  For the prior 7 months she has supported MSL toxicity tests of marine sediments as an intern
through the Associated Western Universities (AWU) program. During her internship she was
involved in numerous bioassay and bioaccumulation tests on sediments from various parts of
the world. Her experience is shared between technical laboratory skills, data processing, and
data analysis. Ms. Johnson is currently working closely with project managers on the same type
of testing activities.

     Ms. Rhonda Karls,  a laboratory supervisor in the toxicology testing laboratory, is
responsible for preparation of the laboratory for testing, maintaining water quality instruments,
ordering supplies, animal  care and maintenance of test organisms,  and the conduction of the
actual test.

     Ms. Nancy Kohn, research scientist, has  experience in conducting sediment evaluation
studies for the U.S. Army  Corps of Engineers and other clients.  She has  participated in
laboratory bioassays and  has served in a project management role  with the responsibility for
planning and leading field sampling efforts and for coordinating sample preparation tasks and
laboratory testing schedules. Her recent research has concentrated on understanding the
effects of ammonia to benthic organisms,  primarily amphipods, under varying environmental
conditions.
     Ms. Brenda Lasorsa, senior research scientist, supervises the mercury analytical
laboratory.  She has helped develop methods for total and methyl mercury analysis by cold-
vapor atomic fluorescence; sulfide analysis using gas chromatographic techniques, and an acid
volatile sulfides analysis system.  Ms. Lasosa has been at the MSL for 10 years.
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                                                                      Appendix B
Battelle Marine Sciences Laboratory                                            Revision: 4
Quality Assurance Management Plan                                           Date: May, 2000
Volume 1                                                               Page 7 of 7

     Ms. Mary McGahan, a technician in the Marine and Environmental Chemistry Group, has
over 15 years of experience.  Her experience includes sample log in and performing preparation
and analysis of tissue, water and soil samples.

     Ms. Laurie Niewolny, research scientist, is experienced at identifying algae, zooplankton,
aquatic insects, and fish and organizing and completing field data collection of water, sediment,
and biota. She is also proficient in most laboratory procedures for standard chemical and
toxicological water and sediment quality analyses and maintains laboratory records,  equipment,
chemical solutions, food supplies, water supply, and test organism cultures.  Ms. Niewolny has
been at the MSL for 4 years, and within the last year supports mercury lab analyses. She is a
QA Representative who is trained to perform data reviews.

     Mr. James Nimmo is the Manager for Facilities and Operations; he has over 30 years
experience in facility operations, and facility and  building management.  Mr. Nimmo has been at
MSL since 1967 and has served as the Project Manager and/or field engineer representative on
most MSL construction projects. He has a background in electronics, specializing  in airborne
radar, navigation, and weapons systems.  Mr. Nimmo was previously an electronic and
pneumatic instrument specialist for nuclear facilities.  He has numerous course completion
certificates in environmental engineering, air and hydronic balancing, property conservation
(relative to fire and flood construction practices and natural disasters), pneumatic control
systems for building heating, ventilation and cooling (HVAC), steam systems, crane-hoist
rigging techniques, and safety including national SCUBA certification and boat operation.

     Ms. Peg O'Neill, technical specialist, is experienced in the operation of inorganic analytical
equipment including atomic absorption and ICP/MS.  She is also proficient in distillation and
acid digestion (hot plate, water bath, and microwave) sample preparation techniques.

     Ms. Meg Pinza, research scientist, has a background in  aquatic toxicology.  She is
currently involved in field sampling and sediment evaluation studies conducted for several
district offices of the U.S. Army Corps of Engineers. She has also conducted bioassays on pulp
mill effluents to determine effluent quality and compliance with discharge permit standards,  and
is currently part of the team developing biotechnology for remediation of contaminants in various
matrices.

     Ms. Jeni Franklin Ross is the point of contact for shipping and receiving and in this role,
assigns bar codes for chemical solutions to implement the Chemical Management  System
(CMS). She has 7 years of experience at  MSL and supports travel,  accounts payable, and
security through the badging process.

     Mr. Jan Slater is the Manager for Business Administration. He has been at MSL for 3
years.  Prior to that he supported the Pacific Northwest National Laboratory for 7 years as
Manager and Sr. Technical Team Lead in various US Department of Energy Programs including
the privatization of the Tank Waste Remediation Systems, the Tritium Target Qualification
Program, ADPE Procurement, the Global Studies Program, and the Environmental
Management Operations.  Prior to coming to PNNL, he worked as Bonneville Power
Administration as a Sr. Contract and Financial Specialist.

     Mr. John Southard, joined MSL in December 1999. He  is part of the MSL Dive Team and
has been certified since 1993.  He is an active SCUBA instructor with National Association of
Underwater Instructors (NAUI) and Technical Diving International (TDI). He is familiar with
underwater survey activities and has used lines,  quadrats, and linear count methods, and has
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                                                                      Appendix B
Battelle Marine Sciences Laboratory                                           Revision: 4
Quality Assurance Management Plan                                           Date: May, 2000
Volume 1                                                               Page 7 of 7

experience with underwater species identification.  Mr. Southard is a collection diver for the
State of WA and the Arthur Feiro Marine Laboratory in Port Angeles, WA.

     Ms. Karen Steinmaus  has 15 years experience in remote sensing and image processing
for both environmental and national security applications. From 1983-1987, Karen worked for
the Defense Mapping Agency (currently NIMA) in NTM Image Exploitation. At the Pacific
Northwest National Laboratory, Karen has focused on the development and application of
remote sensing and geographic information system (GIS) technologies for a very wide variety of
government and commercial clients.  Throughout her career, Karen has emphasized
multidisciplinary problem solving, and multisensor data fusion and integration. Karen has
contributed to, managed, and developed business for basic, applied, and technology transfer
R&D projects, resulting in a very unique opportunity to understand client needs,  technology
gaps, and future trends in the areas of hyperspectral/multi-spectral image exploitation and
multisensor data fusion. Karen holds DOE, DOD and SCI clearances.

     Mr. Monte Sula is a Registered Environmental Manager (REM) and a certified Health
Physicist (CHP). As the MSL  environmental engineer he is in charge of Environmental Waste
Operations at MSL.  He is also the MSL Radiation Safety Officer (RSO). Mr. Sula has been at
MSL for 7 years, and at the Pacific Northwest National Laboratory for the past 20 years.  He is
responsible for all activities associated with liquid and airborne discharges at the MSL and for
work conducted under the laboratory's radioactive materials license.

     Ms. Carolyn Suslick is the Data Coordinator for the Marine Chemistry and Ocean
Processes Group and the Sample Inventory Coordinator (SIC). She is the custodian of and
manages the chemistry data central filing  system. She creates and formats data tables and
control charts from  raw data, tracks data for projects, and assists  Program Managers in
preparing and editing reports.

     Dr. Ronald Thorn, a senior research scientist, has 21 years of professional experience as
an algologist, wetlands ecologist, toxicologist and fisheries biologist.  Dr. Thorn specializes in
environmental impacts of navigation and marina dredging and dredged material  disposal;
habitat construction and restoration of marine and estuarine systems; and ecology of fisheries
resources in nearshore systems.  He also serves as the Technical Group Manager for the
Marine Ecological Processes Group.
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                                                                      Appendix B
Battelle Marine Sciences Laboratory                                            Revision: 4
Quality Assurance Management Plan                                           Date: May, 2000
Volume 1                                                               Page 7 of 7

     Dr. Susan Thomas, senior research scientist, is part of the biotechnology team in
remediation research that is using fungal organisms for the degradation and removal of
contaminants from natural matrices. She has worked in environment assessment and reporting
and as environmental impact statement coordinator. She also has laboratory experience in
radiation biology, olfactory/taste chemistry, and human DMA synthesis and repair.

     Mr. Jeffrey Ward, senior research scientist, has  over 15 years experience in
environmental studies. He provides management and technical expertise for projects  involving
toxicity testing, dredged sediment evaluations, analyses of benthic community structure, and
environmental impact assessments. He has coordinated and participated in numerous field
sampling efforts,  and is experienced in a variety of field sampling procedures.  Mr. Ward is
currently the Technical Group manager for the Toxicology and Risk Assessment Group.

     Dr. Dana Woodruff currently conducts research  in benthic habitat mapping using side-
scan sonar and underwater video.  Her background is  in remote sensing of coastal and
estuarine waters, specializing in optical water quality modeling, in-situ spectral characterization,
and remote estimation of water clarity using satellite imagery.  She received her Ph.D. in 1996
from the University of North Carolina, where she developed algorithms to predict turbidity in
Pamlico Sound, NC, using satellite imagery. Dr. Woodruff recently completed a National
Research Council Research Associateship with the National Marine Fisheries Service  and has
also served as the Southeast Regional Manager for NOAA's CoastWatch Program. Her
previous marine research experience has included primary productivity studies from coastal
North Carolina to the Sargasso Sea, sewage pollution  assessments of coastal sediments using
bacterial indicators, king and tanner crab feeding ecology studies in the Bering Sea, and
behavioral research  on fish and crustaceans relative to oil contamination. Dr. Woodruff was at
MSL from 1976 to 1988, when she left to resume her studies.  She returned in 1998, and has a
total of 13 years at MSL.

     Ms. Jordana Wood has been at  MSL for 1 year.  She supports analyses using the ICP-
AES; GFAA; and FIAS for selenium, mercury,  and arsenic. Prior to her position at MSL, she
was a Supervisor at  Battelle Duxbury for ICP-AES and GFAA analyses.  She has 4 years of
experience as a Supervisor at the EPA's laboratory facilities in Las Vegas,  NV and 3 years
experience at ICF Kaiser for the same  set of analyses.
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                                                                        Appendix C
Battelle Marine Sciences Laboratory                                             Revision: 4
Quality Assurance Management Plan                                            Date: May, 2000
Volume 1                                                                 Page 1 of 4

                                      APPENDIX C

                BATTELLE MSL STANDARD OPERATING PROCEDURES

QUALITY ASSURANCE

MSL-Q-001     Maintaining the Master Schedule Sheet
MSL-Q-002     Quality Assurance Inspections of MSL System and Study Activities
MSL-Q-003     Quality Assurance Audits of Reports
MSL-Q-004     Quality of Testing Water and Feed
MSL-Q-005     Quality Assurance Data Audits
MSL-Q-006     Procedures for Control Charting
MSL-Q-007     Procedure for Determining Method Detection Limits
MSL-Q-008     QA Reports to Management
MSL-Q-009     Method Development, Validation, and Implementation

ADMINISTRATION

MSL-A-001     Sample Log-In Procedure
MSL-A-002     Sample Chain of Custody
MSL-A-003     Guidelines for SOP Format and Control
MSL-A-004     Guidelines for Protocol Preparation and Assignment of Study Numbers
MSL-A-005     Deviations From Established Requirements
MSL-A-006     Marine Sciences Laboratory Training
MSL-A-008     Control of Reagents/Solutions, Test/Control Articles and Specimens
MSL-A-009     GLP Study Initiation Requirements
MSL-A-010     Document Control
MSL-A-011     MSL Access Control
MSL-A-012     Procurement
MSL-A-013     Laboratory Accreditation and PE Sample Analysis
MSL-A-014     Sample Container Requests

DOCUMENTATION, RECORDS, REPORTS

MSL-D-001     Recording Data on Data Sheets and Laboratory Notebooks
MSL-D-002     GLP Records Management
MSL-D-003     Archiving of Records, Data and Retired SOPs
MSL-D-004     Data Reporting, Reduction, Back Up, and Archiving


ORGANIC CHEMISTRY

MSL-O-001     Butyltin  in Sediments and Tissues
MSL-O-002     Butyltin  in Water
MSL-O-003     Identification and Quantification of Polynuclear Aromatic Hydrocarbons by Gas
              Chromatography/Mass Spectrometry
MSL-O-004     Analysis of Polychlorinated Biphenyls and Chlorinated Pesticides by Gas
              Chromatography with Electron Capture Detection
MSL-O-005     Stock and Standard Solution Preparation
MSL-O-006     HPLC Cleanup of Sediment and Tissue Extracts for Semivolatile Pollutants
MSL-O-007     Determination of Lipid Content in Tissues
MSL-O-008     Operation and Maintenance of Gas Chromatographs (GC) and Gas
              Chromatograph/Mass Spectrometer (GC/MS) Systems
MSL-O-009     Extraction and Clean-up of Sediments and Tissues for Semivolatile Organics following
              the Surrogate Internal Standard Method
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                                                                           Appendix C
Battelle Marine Sciences Laboratory                                               Revision:  4
Quality Assurance Management Plan                                              Date:  May, 2000
Volume 1                                                                    Page 2 of 4

MSL-O-010    Extraction and Clean-up of Water for Semivolatile Organics following the Surrogate
              Internal Standard Method
MSL-O-011    HOC Sampling Media Preparation and Handling; XAD-2 Resin and GF/F Filters
MSL-O-012    Extraction and Cleanup of Resin Cartridges for Polychlorinated Biphenyls and Trans-
              Nonachlor
MSL-O-013    Extraction and Cleanup of Glass Fiber Filters for Polychlorinated Biphenyls and Trans-
              Nonachlor
MSL-O-014    PCB Congener Analysis of XAD Resins and GFF Filters Using GC/ECD
MSL-O-015    Identification and Quantification of Polynuclear Aromatic Hydrocarbons by Gas
              Chromatography/Mass Spectrometry Following EPA Method 8270B Quality Control
              Criteria
MSL-O-016    Analysis of Polychlorinated Biphenyls and Chlorinated Pesticides by Gas
              Chromatography with Electron Capture Detection Following EPA Method 8080A Quality
              Control Criteria
INORGANIC CHEMISTRY
MSL-
MSL-
MSL-
MSL-
MSL-
MSL-
MSL-
MSL-
MSL-
MSL-
MSL-
MSL-
MSL-
Spectrometry
MSL-
MSL-
MSL-
MSL-
MSL-
MSL-

MSL-
MSL-
MSL-
MSL-
•001     APDC Extraction for Trace Metals in Water
•003     TAMU Sediment and Tissue Digestion
•004     Sediment Evaporation Digestion
•005     Hot Nitric Acid Digestion of Sediments and Tissues
•006     Mixed Acid Sediment Digestion
•007     Nitric Acid and Hydrogen Peroxide Tissue and Sediment Digestion
•011     Total Mercury in Solids by CVAF
•012     Easily Reducible Mercury in Water by CVAF
•013     Total Mercury in Aqueous Samples by CVAF
•014     Methylmercury in Aqueous Samples by CVAF
•015     Methylmercury in Tissues and Sediments by CVAF
•016     Total Mercury in Tissues  and Sediment by CVAA
•019     Determination of Trace Elements in Water by Stabilized Temperature GFAA
•020      Trace Elements in Sediment and Tissues by GFAA
•021      Arsenic Speciation in Aqueous Samples
•022      Determination of Elements in Aqueous and Digestate Samples by ICP/MS
•023      Selenium Speciation in Aqueous Samples
•024      Mixed Acid Tissue Digestion
•025      Methods of Sample Preconcentration: Cobalt/APDC Co-precipitation and Borohydride
         Reductive Precipitation for Trace Metals Analysis in Water
•026      Use of Laboratory Refrigerators and Freezers
•027      Determination of Metals in Aqueous and Digestate Samples by ICP/AES
•028      Navy Sample Analysis Plan
•029      Determination of Metals in Aqueous and Digestate Samples by GFAA
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                                                                         Appendix C
Battelle Marine Sciences Laboratory                                              Revision: 4
Quality Assurance Management Plan                                            Date: May, 2000
Volume 1                                                                 Page 3 of 4

CONVENTIONAL/GENERAL CHEMISTRY

MSL-C-001     Acid Volatile Sulfide (AVS) and Simultaneously Extracted Metals (SEM) in Sediments
MSL-C-002     Total Volatile Solids
MSL-C-003     Percent Dry Weight and Homogenizing Dry Sediment, Soil, and Tissue
MSL-C-004     pH in Water
MSL-C-005     Total Dissolved Solids
MSL-C-006     Grain Size
MSL-C-007     Total Suspended Solids
MSL-C-008     Total Solids
MSL-C-009     Use and Performance Checks of Balances
MSL-C-010     Calibration  and Use of Pipettes
MSL-C-011     Glassware and Equipment Cleaning Procedures
MSL-C-012     Pb210 Dating Digestion and Analysis
MSL-C-013     137Cs Analyses by Gamma Counting
MSL-C-015     Preparation of Sediment Porewater for Analysis of Organic Compounds and Metals

WATER QUALITY/INSTRUMENTATION

MSL-W-001     Calibration  and Use of pH Meters
MSL-W-002    Calibration  and Use of Dissolved Oxygen Meters
MSL-W-003    Calibration  and Use of Thermometers
MSL-W-004    Calibration  and Use of Refractometers
MSL-W-005    Calibration  and Use of LI-COR Light Meter, Model LI-185A
MSL-W-006    Operation of Atlas CFA-3232 Incinerator
MSL-W-007    Determination of Ammonia
MSL-W-008    Routine Water Quality Measures for Toxicity Tests
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Battelle Marine Sciences Laboratory
Quality Assurance Management Plan
Volume 1

TOXICITY/BIOLOGICAL TESTING
                                                            Appendix C
                                                            Revision: 4
                                                            Date: May, 2000
                                                            Page 4 of 4
MSL-T-001     Water and Tissue Sample Collection
MSL-T-002     Animal Receipt, Acclimation, and Holding
MSL-T-003     Test Organism Observations
MSL-T-004     Sediment Bioaccumulation Testing
MSL-T-005     Acute Sediment Toxicity Testing Using Amphipods
MSL-T-006     Solid Phase Flow-Through Bivalve and Worm Test
MSL-T-007     Suspended Particulate Phase Preparation
MSL-T-008     Suspended Particulate Phase Bivalve Larvae Test
MSL-T-009     Suspended Particulate Phase Fish Test
MSL-T-010     Suspended Particulate Phase Mysid Test
MSL-T-012     Sediment Preparation for Chemical and/or Biological Evaluation
MSL-T-013     Suspended Particulate Phase Echinoderm Larvae Test
MSL-T-020     Preparation of Sediment Porewater
MSL-T-021     Preparation of Sediment Porewater for Sulfide Analysis
MSL-T-022     Collection and Handling of Aquatic Surface Microlayer Samples
MSL-T-023     Collection and Handling of Fish Samples Using a Backpack Electroshocker
MSL-T-024     Sediment Bioassay Testing Using Mysidopsis bahia
MSL-T-025     Bivalve Larvae Test
MSL-T-026     45-Day Sediment Bioaccumulation Testing
MSL-T-027     Supplemental Feeding for Oysters and Clams
MSL-T-028     Sediment and Water Dosing for GLP Study Number SS-00-0001
MSL-T-029     Use of Hemacytometer
MSL-T-030     Collection of Sediment, Tissue, and Water Samples for Good Laboratory Practices Study
              SS-00-0001
MSL-T-031     Calibration and Use of Extech Heavy Duty Light Meter
MSL-T-032     Receipt, Holding, and/or Testing of Fish
FACILITIES

MSL-F-001
MSL-F-002
MSL-F-003
Seawater and Freshwater System Maintenance
Wastewater Discharge Permit Monitoring Procedures
Beach Facility Wastewater Control Procedure
SAFETY

MSL-S-001
Safe Diving Practices
WORK PRACTICES

Biological Hazards
Handling, Storing, and Disposing of Samples
Neutralization of Waste, Acid Solutions
Exposure Control Plan
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                                   Appendix C
Battelle Marine Sciences Laboratory                      Revision: 4
Quality Assurance Management Plan                      Date: May, 2000
Volume 1                                Page 1 of 4
 llBaffeiie
  . . . Putting Technology To Work
  Marine Sciences Laboratory
  QUALITY ASSURANCE MANAGEMENT PLAN
VOLUME  2
Marine and Environmental Chemistry
May 2000
             Battelle Marine Sciences Laboratory
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                                                                          Appendix C
Battelle Marine Sciences Laboratory                                              Revision: 4
Quality Assurance Management Plan                                              Date:  May, 2000
Volume 1                                                                   Page 2 of 4

                               1529 West Sequim Bay Road
                                Sequim, Washington  98382
                                      (360) 681-3645
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                                                              Appendix C
Battelle Marine Sciences Laboratory                                       Revision: 4
Quality Assurance Management Plan                                     Date: May, 2000
Volume 1                                                       Page 3 of 4

                      Battelle Marine Sciences Laboratory
                 MARINE AND ENVIRONMENTAL CHEMISTRY
                 QUALITY ASSURANCE MANAGEMENT PLAN
                                 VOLUME 2

                         Concurrences and Approvals
D. Coffey                                      Date
Quality Assurance Officer
360-681-3645
E.A. Crecelius                                  Date
Marine and Environmental Chemistry
Technical Group Manager
360-681-3604
R. M. Ecker
MSL Manager
360-681-3602
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                                                           Appendix C
Battelle Marine Sciences Laboratory                                     Revision: 4
Quality Assurance Management Plan                                    Date: May, 2000
Volume 1                                                      Page i of 4

                     Battelle Marine Sciences Laboratory
                MARINE AND ENVIRONMENTAL CHEMISTRY
                QUALITY ASSURANCE MANAGEMENT PLAN
                               VOLUME 2

                                 Contents

                                                        Issue Date Rev.

1.0   SAMPLE CONTROL	5/2000    4
     1.1   SAMPLE RECEIPT AND LOG-IN
     1.2   SAMPLE TRACKING
     1.3   SAMPLE ARCHIVING AND DISPOSITION

2.0   ANALYTICAL PROCEDURES	5/2000    4

3.0   EQUIPMENT MAINTENANCE AND CALIBRATION	5/2000    4
     3.1   PREVENTATIVE MAINTENANCE
     3.2   EQUIPMENT CALIBRATION

4.0   QUALITY CONTROL	5/2000    4
     4.1   LIMITS OF DETECTION
     4.2   DATA QUALITY OBJECTIVES
           4.2.1  Precision
           4.2.2  Accuracy
           4.2.3  Representativeness
           4.2.4  Comparability
           4.2.5  Completeness
     4.3   HOLDING TIMES AND PRESERVATION
     4.4   CONTROL CHARTS

5.0   CORRECTIVE ACTION	5/2000    4
     5.1   DEVIATIONS
     5.2   CORRECTIVE ACTION FOR
           DATA OUTSIDE OF CONTROL LIMITS

6.0   DATA REPORTING	5/2000    3

7.0   REFERENCES	5/2000    3
                               APPENDICES

      LIST OF EQUIPMENT	5/2000
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Battelle Marine Sciences Laboratory                                                Section: 1
Marine Chemistry and Ocean Processes Group                                        Revision: 4
Quality Assurance Management Plan                                                Date: May 2000
Volume 2                                                                      Page 3 of 3


                                  1.0 SAM RLE CONTROL

Sample handling and tracking with the Marine and Environmental Chemistry Group is covered by two
procedures: MSL-A-001, Sample Log-in Procedure and MSL-A-002, Sample Chain of Custody.  The
processing of data collected from these activities discussed in procedure MSL-D-004, Data Reporting,
Reduction, Back Up, and Archiving.  The following is a description of the procedure used for receipt and
tracking of samples, as well as chain of custody procedures.

1.1 SAM RLE RECEIPT AND LOG-IN

Samples or test organisms are logged in when received in the shipping area.  If a Chain of Custody (CoC)
form accompanies the samples or test organisms, this form is used to document the date and time of
sample receipt and condition.  If a CoC form is not shipped with samples, an MSL form will be initiated.
For test organisms, a shipping form can be signed and dated and the condition of organisms noted.
Cooler temperatures are taken and recorded on the CoC.  The sample labels are compared to the CoC
and assigned an identification code plus sequential numbering of samples upon arrival. If sample
preservation  is indicated by the type of analysis or customer specification, samples may be pH adjusted
or the pH of a set of subsamples measured to ensure that samples needing to be at a pH of < 2 pH  units
are acidified.  This is recorded on the CoC.  If samples require filtration,  they will be filtered and this
information recorded on the CoC form.  Samples are counted and assigned an MSL project number (i.e.,
a central file  number and sequential numbering of the set of samples that were received).  In some cases
samples in a set may arrive on different days depending on the customer's needs and direction.
For analytical samples, an electronic spreadsheet is generated (Login Sheet) listing the customer or
sampling  identification (ID) number, (sponsor code), the MSL sample ID Number (Battelle code), the
sample matrix, the parameters requested, the date of sample collection, and the initials of the person
logging in the samples (the Sample Custodian or Designee). The location of sample storage until
preparation is also noted.

The "kit" is initiated at this time and generally includes:
•   kit initiation date
•   assigned central file number
•   client name
•   project title
•   data due date
•   work package  number (charge code)
•   any holding  time specifications1
•   expected sample concentration level, if known (high, moderate, low)
•   expected number of samples
•   blank correction instructions
•   matrix and summary of requested preparation activities, digestions,  and analyses
•   hazardous material designation
•   sample disposal instructions
•   project manager signature and date
•   Project Workplan Sheet - page 2; specifies sample preparation instructions
•   Metals - page 3; specifies matrix and analysis method(s)
•   QA/Quality Control (QC) Requirement Sheet - page 4; specifies precision (number of replicates,
    number of spiked replicates), and accuracy (standard reference material [SRM] type and frequency,
    number of matrix spikes and concentrations levels] method detection limit [blank and blank spike
    frequency] and initial calibration verification (ICV) and continuing calibration verification [CCV])
    sample frequencies. Project control limits may also be specified or attached. When the customer
    does not specify project control limits, MSL default limits will be used.
       In the absence of customer-specified holding times, holding times defined in standard methods
(e.g., EPA 1600 series methods; U.S. Army Corps of Engineers, 1994. Inland Testing Manual. EPA-823-
B-94-002. U.S. EPA, Office of Water. Washington, D.C.) may be assigned by the MSL Project Manager.
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Battelle Marine Sciences Laboratory                                                Section: 1
Marine Chemistry and Ocean Processes Group                                       Revision: 4
Quality Assurance Management Plan                                               Date: May 2000
Volume 2                                                                     Page 3 of 3

•   The CoC forms are appended to the last sheet of the kit.

An addendum is prepared for anything that is added to the kit.  Additions might include the receipt of
another sample set to be included in the project sample set, changes to the analysis request, or deletion
of some samples to be analyzed.

The kit and any addedums are copied and distributed by the Project Manager to all analysts involved.
The original pages of the kit become part of the Chemistry Central File System.

1.2 SAM RLE TRACKING

Sample tracking while samples are in the laboratory is the responsibility of the individual Laboratory
Supervisors and the Project Manager. It is the responsibility of the Project Manager to ensure that the
samples are given the appropriate priority in the laboratory and that the proper analyses and methods are
being performed.

1.3 SAMPLE ARCHIVING AND DISPOSITION

The Project Manager is responsible for proper disposal of leftover sample material. Sample disposition
takes three forms:  1) dispose of by appropriate means depending on sample content; 2) return to client;
or 3) archive  indefinitely. Unless arrangements have been made previously, the samples are generally
disposed  of by Battelle MSL.

When samples are disposed of by a subcontractor laboratory:

   If the subcontractor laboratory or testing facility is  responsible for disposing of the samples,
     the subcontractor is asked to notify the MSL Project Manager before final disposition.  The
     MSL Contact will notify the originator that the samples are scheduled to be destroyed, or
     will define customer requirements for an extended period of storage.

   After destruction of samples, the subcontractor laboratory or testing facility is asked to return
     a copy of the Chain-of-Custody Form to the MSL Contact for placement in project files.
     The originator may be forwarded a copy of the final Chain-of Custody documentation if
     requested.

    The MSL Contact records the date of receipt on the Chain-of-Custody Form in the "Received by"
    section of the form space and indicates the samples were destroyed ending the chain of possession.

When samples are disposed of by the Marine Sciences Laboratory (MSL):

     If the laboratory or testing facility is not responsible for disposal of the samples, MSL personnel will
     obtain custody of the samples from the subcontractor laboratory or testing facility along with the
     Chain-of-Custody Form.

For returned samples or samples that have never left MSL custody, the MSL Contact will notify the
     originator that the samples are scheduled to be destroyed, or will define customer requirements for
     an extended period of storage. If extended storage is not requested, then MSL will dispose of the
     samples following the guidelines specified in the Pacific Northwest National Laboratory's (PNNL's)
     Standards-Based Management System (SBMS).  This system provides a framework for logging in
     reagents, chemicals and solutions into the associated Chemical  Management System (CMS).  This
     system provides the PNNL Laboratory with the policies and procedures regarding tracking and
     inventory, storage and disposal of completed samples and analytical wastes, as well as chemical
     use and disposal.  The CMS is used to provide an up-to-date inventory to facilitate emergency
     response,  monitor the location of various classes of materials and identify situations where
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Battelle Marine Sciences Laboratory                                              Section: 1
Marine Chemistry and Ocean Processes Group                                      Revision: 4
Quality Assurance Management Plan                                              Date: May 2000
Volume 2                                                                   Page 3 of 3

     acceptable limits for the building/facility determined by the assigned chemical hazard group and fire
     zone might be exceeded before a violation occurs.

After destruction of samples, MSL personnel responsible for sample destruction returns a copy of the
     Chain-of-Custody Form to the MSL Contact and the Sample Disposal Log Book entry is updated.
     The MSL Contact records the date of receipt on the Chain-of-Custody Form in the "Received by"
     space next to the Sample Custodian's signature and indicates the samples were destroyed  ending
     the chain of possession.

When samples are returned to the customer for disposal:

                 Samples may be returned to the customer (or the sampling site) by customer
                 request. Samples are shipped to meet Department of Transportation
                 regulations.  Generally, the samples are shipped in the same way that they
                 were initially shipped to MSL. Sample disposition should be documented in the
                 central file of each project. The MSL Contact shall ensure that completed
                 Chain-of-Custody Forms are filed in the appropriate project files. The
                 originator may be forwarded a copy of the final  Chain-of Custody
                 documentation if requested.
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Battelle Marine Sciences Laboratory                                                Section:  1
Marine Chemistry and Ocean Processes Group                                       Revision: 4
Quality Assurance Management Plan                                                Date: May 2000
Volume 2                                                                     Page 3 of 3


                             2.0 ANALYTICAL PROCEDURES

All routine analytical laboratory activities are directed and controlled by internal MSL procedures. Where
possible, U.S. Environmental Protection Agency (EPA) and consensus methods (e.g., NOAA Status and
Trends) are used where the technique is applicable to the sample matrix and the overall objective of the
analysis. Table 2.1 lists the analytes and applicable SOPs associated with metals and ancillary
measurement analysis.  Table 2.2 lists the analytes and applicable SOPs associated with organic
analysis. Table 2.3 is a list of the MSL Chemistry procedures and the corresponding EPA or other
reference methods upon which the SOPs are  based.
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Battelle Marine Sciences Laboratory
Marine Chemistry and Ocean Processes Group
Quality Assurance Management Plan
Volume 2


Analyte
METALS (1)
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Copper
Lead
Manganese
Mercury
Methyl Mercury
Nickel
TABLE 2.1 List of Analytes
Sed/Tiss
Preparation
Method(s)

MSL-I-003/004/006/024/C-003/01 5
MSL-I-003/004/006/024/C-003/01 5
MSL-I-003/004/006/024/C-003/01 5
MSL-I-003/004/006/024/C-003/01 5
MSL-I-003/004/006/024/C-003/01 5
MSL-I-003/004/006/024/C-003/01 5
MSL-I-003/004/006/024/C-003/01 5
MSL-I-003/004/006/024/C-003/015
MSL-I-003/004/006/024/C-003/015
MSL-I-003/004/006/024/C-003/015
MSL-l-003/004/006/024/ C-003/015
MSL-l-015
MSL-I-003/004/006/024/C-003/01 5
Selenium MSL-I-003/004/006/024/025/C-003/01 5
Silver
Tin
Thallium
Vanadium
Zinc
MSL-I-003/004/006/024/C-003/01 5
MSL-I-003/004/006/024/C-003/01 5
MSL-I-003/004/006/024/C-003/01 5
MSL-I-003/004/006/024/C-003/01 5
MSL-I-003/004/006/024/C-003/01 5
Section: 1
Revision: 4
Date: May 2000
Page 3 of 3
and SOPs for Metals and Ancillary Measurements
Sed/Tiss
Analysis
Method(s)

MSL-l-022/020/027
MSL-l-022/020/027
MSL-l-022/020/027
MSL-l-022/020/027
MSL-l-022/020/027
MSL-l-022/020/027
MSL-l-022/020/027
MSL-l-022/020/027
MSL-l-022/020/027
MSL-l-022/020/027
MSL-l-016
MSL-l-015
MSL-l-022/020/027
MSL-l-022/020/027
MSL-l-022/020/027
MSL-l-022/020/027
MSL-l-022/020/027
MSL-l-022/020/027
MSL-l-022/020/027
Water
Preparation
Method(s)

I-025
I-025
I-025
I-025
I-025
MSL-I-001/-025
I-025
MSL-l-001/025
MSL-l-001/025
I-025
MSL-l-012/013
MSL-l-014
MSL-l-001/025
I-025
MSL-l-001
I-025
I-025
MSL-l-001
I-025
Water
Analysis
Method(s)

MSL-l-022/1-01 9/027
MSL-I-022/I-01 9/029
MSL-l-022/1-01 9/021/027/029
MSL-l-022/1-01 9/027
MSL-l-022/1-01 9/027
MSL-l-022/1-01 9/027
MSL-l-022/1-01 9/027
MSL-l-022/1-01 9/027
MSL-l-022/1-01 9/027/029
MSL-l-022/1-01 9/023/027
MSL-l-012/013
MSL-l-014
MSL-l-022/1-01 9/027
MSL-l-022/1-01 9/023//029
MSL-l-022/1-01 9/027/029
MSL-l-022/1-01 9
MSL-l-022/1-01 9/029
MSL-l-022/1-01 9/027
MSL-l-022/1-01 9/027
ANCILLARY MEASUREMENTS
Total Lipids
Grain Size
Percent Moisture
AVS
TVS
(1) List is a partial listing




- additional metals can be analyzed
MSL-O-007
MSL-C-006
MSL-C-003
MSL-C-001
MSL-C-002











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Battelle Marine Sciences Laboratory
Marine Chemistry and Ocean Processes Group
Quality Assurance Management Plan
Volume 2
TABLE 2.2 List of Analytes and SOPs for Organics
Sediment/Tissue

Analyte
ORGANICS
PAHs
Acenaphthene
Acenaphthylene
Anthracene
Fluorene
Naphthalene
Phenanthrene
Benzo(a)anthracene
Benzo(a)pyrene
Benzo(b)fluorene
Benzo(g,h,i)perylene
Benzo(k)fluoranthene
Chrysene
Dibenzo(a,h)anthracene
Fluoranthene
lndeno(1 ,2,3-cd)pyrene
Acenaphthylene
Phthalates
Dimethyl Phthalate
Diethyl Phthalate
Di-n-butyl Phthalate
Butyl benzyl Phthalate
Bis(2-ethylhexyl)Phthalate
Di-n-butyl Phthalate
PCB Congeners (1)
8(2,4')
18 (2,2', 5)
28(2,4,4')
44 (2,2', 3,5')
49 (2,2', 4,5')
52 (2,2', 5,5')
66 (2,3', 4,4')
87 (2,2', 3,4,5')
101 (2,2', 3,5,5')
105 (2,3,3', 4,4')
118(2,3',4,4',5)
128(2,2',3,3',4,4')
138(2,2',4,4',5,5')
153(2,2',4,4',5,5')
170(2,2',3,3',4,4',5)
180(2,2',3,4',5,5',6)
183 (2,2', 3,4,4', 5',6)
Preparation
Method(s)


MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009

MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009

MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
Sediment/Tissue
Analysis
Method(s)


MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015

MSL-O-003
MSL-O-003
MSL-O-003
MSL-O-003
MSL-O-003
MSL-O-003

MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
Water
Preparation
Method(s)


MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010

MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010

MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
Section: 1
Revision: 4
Date: May 2000
Page 3 of 3
Water
Analysis
Method(s)


MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015
MSL-O-003/015

MSL-O-003
MSL-O-003
MSL-O-003
MSL-O-003
MSL-O-003
MSL-O-003

MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004
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Battelle Marine Sciences Laboratory
Marine Chemistry and Ocean Processes Group
Quality Assurance Management Plan
Volume 2
Section: 1
Revision: 4
Date: May 2000
Page 3 of 3
TABLE 2.2 Continued

Analyte
PCB/Aroclors(2)
1242
1248
1254
1260
Organotins
Tributyltin
Dibutyltin
Monobutyltin
Pesticides
Aldrin
-Chlordane
Trans nonachlor
Dieldrin
p,p'-DDT
o,p'-DDT
p,p'-DDD
o,p'-DDD
p,p'-DDE
o,p'-DDE
Endosulfan I
Endosulfan II
Endosulfan sulfate
Heptachlor
Heptachlorepoxide
Lindane
Sediment/Tissue
Preparation
Method(s)

MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009

MSL-O-001
MSL-O-001
MSL-O-001

MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
MSL-O-006/009
Sediment/Tissue
Analysis
Method(s)

MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004

MSL-O-001/016
MSL-O-001/016
MSL-O-001/016

MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
Water
Preparation
Method(s)

MSL-O-010/012
MSL-O-010/012
MSL-O-010/012
MSL-O-010/012

MSL-O-002
MSL-O-002
MSL-O-002

MSL-O-010
MSL-O-010
MSL-O-010/012
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
MSL-O-010
Water
Analysis
Method(s)

MSL-O-004
MSL-O-004
MSL-O-004
MSL-O-004

MSL-O-002/016
MSL-O-002/016
MSL-O-002/016

MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
MSL-O-004/016
(1)  List is a partial listing - up to  100 congeners can by analyzed
(2)  List is a partial listing - additional aroclors can be analyzed
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Battelle Marine Sciences Laboratory
Marine Chemistry and Ocean Processes Group
Quality Assurance Management Plan
Volume 2
                         Section: 1
                         Revision: 4
                         Date: May 2000
                         Page 3 of 3
             TABLE 2.3 List of Chemical Analytical Methods Proposed and
                          Their Similar or Equivalent Methods
MSL Procedure
Method Used as Basis for Procedure
MSL-C-001, Acid Volatile Sulfide (AVS) and
Simultaneously Extracted Metals (SEM) in
Sediments
and Aqueous Samples

MSL-C-002, Total Volatile Solids

MSL-C-003, Percent Dry Weight and
Homogenizing Dry Sediment, Soil, and Tissue

MSL-C-004, pH in Water

MSL-C-005, Total Dissolved Solids

MSL-C-006, Grain Size

MSL-C-007, Total Suspended Solids

MSL-C-008, Total Solids

MSL-C-015, Preparation of Sediment
Porewater for Analysis of Organic
Compounds and Metals

MSL-l-001, APDC Extraction for
Trace Metals in Water

MSL-l-003, TAMU Sediment and
Tissue Digestion

MSL-l-004, Sediment Evaporation Digestion

MSL-l-005, Hot Nitric Acid Digestion
of Sediment and Tissue

MSL-l-006, Mixed Acid Sediment Digestion

MSL-l-007, Nitric Acid and Hydrogen Peroxide
Tissue and Sediment Digestion
Allen et.al., 1990




Standard Methods 1995 (Method 2540 E)

EPA 1979 (Method 160.3)


EPA 1979 (Method 150.1)

Standard Methods 1995 (Method 2540 C)

Plumb, 1981

Standard Methods 1995 (Method 2540 D)

Standard Methods 1995 (Method 2540 B)

NA



EPA 1996c (Method 1640)


NOAA1993


NA

NA


Kostas, O'Conner, and Crecelius 1997

EPA 1991 (Method 200.3)
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Battelle Marine Sciences Laboratory
Marine Chemistry and Ocean Processes Group
Quality Assurance Management Plan
Volume 2
                         Section:  1
                         Revision: 4
                         Date: May 2000
                         Page 3 of 3
                                   TABLE 2.3 Continued
MSL Procedure
Method Used as Basis for Procedure
MSL-l-011, Total Mercury in Solids by CVAF

MSL-l-012, Easily Reduceable Mercury in Water
by CVAF

MSL-l-013, Total Mercury in Aqueous Samples
by CVAF

MSL-l-014, Methyl mercury in Aqueous
Samples by CVAF

MSL-l-015, Methylmercury in Tissues and
Sediments by CVAF

MSL-l-016, Total Mercury in Tissues and
Sediments by CVAA

MSL-l-020, Trace Elements in Sediments
and Tissues by GFAA

MSL-l-021, Arsenic Speciation in Aqueous
Samples

MSL-l-022, Determination of Elements in
Aqueous and Digestate Samples by ICP/MS

MSL-l-023, Selenium Speciation in Aqueous
Samples

MSL-l-025, Methods of Sample Preconcentration:
Cobalt/APDC Coprecipitation and Borohydride
Reductive Precipitation for Trace Metals
Analysis in Water

MSL-l-027, Determination of Metals in Aqueous
and Digestate Samples by ICP/AES

MSL-l-029, Determination of Trace Elements
in Water by Stabilized Temperature GFAA

MSL-O-001, Butyltins in Sediment and Tissue

MSL-O-002, Butyltins in Water
Bloom and Crecelius, 1983

Bloom and Crecelius, 1983
Bloom and Crecelius, 1983; EPA 1996b
(Method 1631)

Bloom, 1989; EPA 1998a (Method 1630)
Bloom, 1989
EPA 1991 (Methods 245.5 and 245.6)
EPA 1991 (Method 200.9)
EPA 1998b (Method 1632)
EPA 1991 (Method 200.8), EPA 1996d
(Method 1638)

EPRI 1986
Brugmann et. al., 1983
EPA 1994 (EPA 200.7); EPA 1997 (SW-846 Method
6010B)

EPA 1991 (Method 200.9)
Linger et. al., 1986

Linger et. al., 1986
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Battelle Marine Sciences Laboratory
Marine Chemistry and Ocean Processes Group
Quality Assurance Management Plan
Volume 2
                          Section: 1
                          Revision: 4
                          Date: May 2000
                          Page 3 of 3
                                   TABLE 2.3 Continued
MSLSOP
Method Used as Basis for SOP
MSL-O-003, Identification and Quantification of
Polynuclear Aromatic Hydrocarbons by GC/MS

MSL-O-004, Analysis of PCBs and Chlorinated
Pesticides by GC/ECD

MSL-O-006, HPLC Cleanup of Organic Extracts

MSL-O-007, Determination of Lipid Content
in Tissues

MSL-O-009, Extraction  and Cleanup of Sediment
and Tissue for Semivolatile Organics following the
Surrogate Internal Standard Method

MSL-O-010, Extraction  and Cleanup of Water
for Semivolatile Organics following the
Surrogate Internal Standard Method

MSL-O-012 Extraction and Cleanup of Resin
Cartridges for Polychlorinated Biphenyls and
Trans-Nonachlor

MSL-O-016, Analysis of PCBs and Chlorinated
Pesticides by GC/ECD Following EPA Method
8080A Quality Control Criteria
EPA 1996a (Method 8270C)


EPA 1996a (Method 8081 A)


Krahn et. al., 1988

Bligh & Dyer, 1959


NOAA1993



NOAA1993



EPA 1986



EPA 8080A
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Battelle Marine Sciences Laboratory                                        Section:  4
Marine Chemistry and Ocean Processes Group                                      Revision: 4
Quality Assurance Management Plan                                              Date: May, 2000
Volume 2                                                                    Page 1 of 11

                   3.0 EQUIPMENT MAINTENANCE AND CALIBRATION
3.1 PREVENTATIVE MAINTENANCE

Equipment is serviced regularly by qualified individuals, either trained in-house personnel or through
service contracts with the manufacturer or an authorized representative.  Written records of all instrument
maintenance, calibration, testing, and inspection are maintained. Maintenance records contain a
description of the operation or problem, the remedial action taken (if necessary), date, the person
responsible, and where applicable, documentation of the instrument's return to analytical control. Each
major instrument listed in Appendix A has it's own logbook used to document the preventative
maintenance.

3.2 EQUIPMENT CALIBRATION

Calibration procedures are performed on each piece of analytical equipment prior to use. Requirements
for specific levels and frequency of calibration are described in the procedures specific for the equipment
and methods that are being used. These criteria are summarized in Table 3.1.  Note that these are the
minimum requirements and project specific requirements may be different. All raw calibration data are
kept in the data files and are traceable to sample runs.  Corrective actions when calibration criteria are
not met are described in section 5.0 of this document and  in the specific procedures.

Initial Calibration Verification

After instrument calibration, an initial calibration verification (ICV) sample should be  run to verify
instrument control.  Normally, this check will consist of running a standard reference material  (SRM) or
one of the same standards that were used for the initial calibration.  For samples that are to be analyzed
for the Navy, or when requested by a client, a secondary source ICV shall be run prior to running any
samples. This ICV will be a standard from a different source than those used in the  initial calibration.

Continuing Calibration Verification

Continuing calibration verification (CCV) samples shall be run at the frequency described in the SOP for
each method. Analysts will attempt to  run CCVs such that they bracket the analytical range of the
samples run in the analytical batch.  If CCVs do not bracket the samples, the data will be flagged.
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Battelle Marine Sciences Laboratory
Marine Chemistry and Ocean Processes Group
Quality Assurance Management Plan
Volume 2
PID
                                                    Section: 4
                                                           Revision: 4
                                                           Date: May, 2000
                                                           Page 1 of 11
                             TABLE 3.1  Marine and Environmental Chemistry Calibration Procedures
Equipment
GC/ECD
GC/MS
GC/FPD
HPLC
GFAA
ICP/MS
ICP/AES
CVAA
CVAF
SOP No./Section
MSL-O-0047 Sec. 4.1.1
MSL-O-003/ Sec. 5.1.1
MSL-O-001/002/Sec. 5.1 and 6.1
MSL-O-006
MSL-l-029/Sec 5.4.2
MSL-l-022/ Sec 5.0
MSL-l-027/Sec. 5.4.2
MSL-l-016/ Sec. 4.4.1 and 5.1
MSL-l-01 2/01 3/01 4/01 5
Parameters
PCBs, chlorinated pests
PAH, phthalates
Butyltins
Semivolatile clean-up
Metals in water, sediment
and tissue
Metals in water, sediment
Metals in water, sediment
value and tissue
Total Hg in sediment and tissue
Total Hg in water and MeHg in
Description (a)
4 pt calibration
3 pt calibration
4 pt calibration
only set collection
windows
3 pt calibration
3 pt calibration
1 pt. calibration
4 pt calibration
4 pt calibration
Criteria
The RSD(b) of the RRF(C) <_30%
for each analyte
The RSD of the RRF <_30%
for each analyte
The RSD of the RRF <_30%
for each analyte
Not used for quantitation
r2> 0.995
r2> 0.995
ICV within 10% of concentration
r2> 0.995
r2> 0.995
MSL-C-001
                                                   water, sediment and tissue
Acid Volatile Sulfides
3 pt calibration
r2> 0.99
(a)  Minimum number of calibration points
(b)  RSD = relative standard deviation
(c)  RRF = Relative Response Factor
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Battelle Marine Sciences Laboratory                                         Section: 4
Marine Chemistry and Ocean Processes Group                                       Revision: 4
Quality Assurance Management Plan                                               Date: May, 2000
Volume 2                                                                     Page 1 of 11

4.0 QUALITY CONTROL

The characteristics used to define data quality are accuracy, precision, completeness, comparability,
representativeness and sensitivity (limits of detection).  The definition and application of these parameters
are discussed below.

4.1 LIMITS OF DETECTION

Method detection limits (MDLs) are determined for all parameters for a number of different matrices. The
matrices generally used for MDL studies are freshwater collected from the in-house deionized water
system, filtered seawaterfrom Sequim Bay, Sequim Bay or other clean sediment, and Macoma tissue.
The method used to determine MDLs is covered in procedure MSL-Q-007, Procedure for Determining
Method Detection Limits. Briefly, MDLs are determined by spiking a minimum of 7 replicate matrices with
low levels of the analytes of interest. MDLs are calculated by multiplying the standard deviation of the
replicate results by the student t value (99th percentile) for the number of replicates analyzed.  Limits of
quantitation may also be reported on request as more conservative estimates of detection limits and are
defined as 10 times the standard deviation of the replicate analyses. MDL studies should be performed
annually.

Tables 4.1 and 4.2  show representative MDLs for the majority of parameters analyzed at Battelle and for
a variety of matrices.  Since MDLs change yearly and sometimes are performed specifically for individual
projects, these exact MDLs are not used to report all data, however; they give a good approximation of
the level of detection capable for the various parameters using the methods specified.  Because the types
of matrices actually analyzed at Battelle vary quite significantly, the MDLs determined on representative
matrices may only be estimates of actual detection limits achievable.  In addition, MDLs will change if
insufficient sample  is received by the MSL, if sample matrix interference dictates higher detection limits,
or if modifications to existing methods are requested by the client.
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Battelle Marine Sciences Laboratory
Marine Chemistry and Ocean Processes Group
Quality Assurance Management Plan
Volume 2
                   Section: 4
                          Revision: 4
                          Date: May, 2000
                          Page 1 of 11

TABLE 4.1  Typical Inorganic MDLs
SEDIMENT ( a/a drv wt.)
METALS
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Copper
Lead
Manganese
Mercury
Methyl mercury
Nickel
Selenium
Silver
Tin
Thallium
Vanadium
Zinc
ICP/MS
1.0
0.05
0.60
0.10
0.10
0.024
0.50
0.70
0.75
0.65
NA
NA
1.2
0.25
0.02
0.05
0.02
1.0
3.3
GFAA
1.0
0.50
1.0
10
0.30
0.03
0.50
0.10
0.50
0.50
NA
NA
0.50
0.27
0.02
1.0
0.50
NA
1.0
CVAA/F
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
0.009
0.00006
NA
NA
NA
NA
NA
NA
NA
TISSUE ( a/a drv wt.)
ICP/MS
1.8
0.04
0.04
0.04
0.2
0.03
0.25
0.014
0.02
0.63
NA
NA
0.02
0.12
0.03
0.0
0.02
0.10
0.10
GFAA
2.0
0.2
0.03
2.0
0.10
0.10
0.10
0.10
0.10
0.10
NA
NA
0.10
0.40
0.05
0.50
0.20
NA
0.50
APDC/
CVAA/F
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
0.02
0.005
NA
NA
NA
NA
NA
NA
NA
WATER ( a/L)
ICP/MS
0.06
0.009
0.04
0.006
0.05
0.02
0.04
0.01
0.005
0.001
NA
NA
0.03
0.39
0.004
0.02
0.004
0.02
0.04
ICP/MS
NA
NA
0.003
NA
NA
0.003
NA
0.03
0.03
NA
NA
NA
0.06
NA
0.005
NA
NA
NA
NA
GFAA
2.0
2.9
1.0
5.0
0.20
0.05
0.10
0.50
1.0
0.50
NA
NA
1.5
0.78
0.50
2.0
1.0
NA
0.55
CVAA/F
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
0.0002
0.00004
NA
NA
NA
NA
NA
NA
NA
APDC     Ammonium pyrrolidinedithiocarbamate
ICP/MS    Inductively Coupled Plasma Mass Spectrometry
GFAA      Graphite Furnace Atomic Absorption
CVAA/F:    Cold Vapor Atomic Absorption/Fluorescence
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Battelle Marine Sciences Laboratory
Marine Chemistry and Ocean Processes
Quality Assurance Management Plan
Volume 2
Group
Section:
4
Revision: 4
Date: May, 2000
Page 1 of 11
TABLE 4.2 Typical Organic MDLs

PARAMETER
PAHS
Naphthalene
Dimethyl Phthalate
Acenaphthylene
Acenaphthene
Diethyl Phthalate
Fluorene
Phenanthrene
Anthracene
Di-n-butyl Phthalate
Fluoranthene
Pyrene
Butyl benzyl Phthalate
Benzo(a)anthracene
Chrysene
Bis(2-ethylhexyl) Phthalate
Di-n-octyl Phthalate
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(e)pyrene
Benzo(a)pyrene
Perylene
lndeno(1 ,2,3-cd)pyrene
Dibenzo(a.h)anthracene
Benzo(g,h,i)perylene
SEDIMENT
(|j,g/kg dry wt)

0.23
10.8
0.43
0.39
24.5
0.53
3.51
0.72
21.4
0.45
0.52
15.3
0.19
0.52
45.0
24.1
0.63
0.44
1.17
0.85
1.30
0.84
0.51
0.55
TISSUE
(l-ig/kg wet wt)

1.85
2.91
0.55
1.39
76.6
1.28
2.67
2.25
7.68
3.10
2.79
6.02
0.90
1.74
17.0
5.64
1.14
1.50
1.30
1.28
1.35
1.53
1.22
1.07
WATER
(ng/L)

2.8
NA
30.7
3.6
NA
8.8
15.7
17.0
NA
8.7
7.9
NA
3.2
3.4
NA
NA
14.5
14.8
19.5
7.5
2.9
11.8
13.1
11.4
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Battelle Marine Sciences Laboratory
Marine Chemistry and Ocean Processes Group
Quality Assurance Management Plan
Volume 2
TABLE 4.2

PARAMETER
PESTICIDES
Hexachlorobenzene
a-BHC
G-BHC
Heptachlor
Aldrin
b-BHC
d-BHC
Heptachlor Epoxide
2,4'-DDE
Endosulfan 1
g-Chlordane
a-Chlordane
Trans Nonachlor
4,4'-DDE
Dieldrin
2,4'-DDD
Endrin
4,4'-DDD
Endosulfan II
4,4'-DDT
Endrin Aldehyde
Endosulfan Sulfate
Methoxychlor
Mi rex
Endrin Ketone
T-Chlordane
Toxaphene
Typical Organic MDLs
SEDIMENT
(|j,g/kg dry wt)

0.64
0.45
0.28
0.08
0.27
0.45
0.45
0.39
0.85
0.45
0.45
0.64
0.29
0.18
0.26
0.26
0.45
0.33
0.45
0.94
0.45
0.45
0.45
0.28
0.45
5.0
20
Section:
(continued)
TISSUE
(l-ig/kg wet wt)

0.13
0.18
0.13
0.19
0.13
0.18
0.18
0.13
0.26
0.18
0.18
0.10
0.15
0.19
0.52
0.25
0.18
0.26
0.18
0.15
0.18
0.18
0.18
0.20
0.18
5.0
20
4
Revision: 4
Date: May, 2000
Page 2 of 11

WATER
(ng/L)

1.18
2.00
1.23
1.02
0.76
2.00
2.00
2.14
0.74
2.00
2.00
1.93
0.57
0.84
0.36
0.98
2.00
0.28
2.00
0.50
2.00
2.00
2.00
6.29
2.00
5.0
20
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Battelle Marine Sciences Laboratory Section:
Marine Chemistry and Ocean Processes Group
Quality Assurance Management Plan
Volume 2
TABLE 4.2 Typical Organic MDLs (continued)
SEDIMENT TISSUE
PARAMETER (ng/kg dry wt) (l-ig/kg wet wt)
PCB/CONGENERS
Range 0.06 - 3.05 0.06 - 0.28
AROCLORS
1242 3.16 6.95
1248 3.16 6.95
1254 3.16 6.95
1260 3.16 6.95
BUTYLTINS
Tributyltin 0.48 0.37
Dibutyltin 0.56 1.39
Monobutyltin 1.82 1.97
4
Revision: 4
Date: May, 2000
Page 3 of 11

WATER
(ng/L)

0.17- 1.15

NA
NA
NA
NA

3.07
12.0
10.8
NA = Not Applicable
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Battelle Marine Sciences Laboratory                                        Section: 4
Marine Chemistry and Ocean Processes Group                                      Revision:  4
Quality Assurance Management Plan                                              Date:  May, 2000
Volume 2                                                                    Page 4 of 11

4.2 DATA QUALITY OBJECTIVES

The quality control (QC) measurements that are performed during the chemical analysis of the sediments,
waters and tissues are outlined in each applicable analytical SOP.  The precision and accuracy objectives
specified in the SOPs are based on standard method performance information (when available)  and
historical laboratory performance but may change based on project specific criteria. When required by
the client or MSL project manager, other QC checks for accuracy, precision, comparability and
completeness shall be applied to each batch of samples.  Corrective actions when data quality objectives
(DQOs) are addressed in Section 5.0.

4.2.1  Precision

Precision measures the similarity of individual measurements of the same property, usually under
prescribed similar conditions.

Within the Marine Chemistry and Ocean  Processes Group, measures of analytical precision will be
determined by the analysis of laboratory replicates or matrix spike/matrix spike duplicate recoveries.
Duplicates are normally performed unless more are requested by the client. Laboratory replicates will be
prepared by homogenizing and splitting a sample in the laboratory, and carrying the subsamples through
the entire analytical process.  Precision can be expressed in terms of relative percent difference (RPD) or
relative standard deviation (RSD).


For replicates where duplicates are performed, RPD will be used:

                             RPD = _C^C2__  x  100
                              where RPD = relative percent difference
                                     C-| = larger of the two observed values
                                     C2 = smaller of the two observed values
For replicates where triplicates or more are performed, RSD (coefficient of variation) will be used:

                             RSD = (s)x 100
                                    m
                            where RSD = relative standard deviation
                                     s = standard deviation of replicates
                                    m = mean of replicates

4.2.2 Accuracy

Accuracy is a measure of the bias of a system or measurement. It is the closeness of agreement
between an observed value and an accepted value.

Within the Marine and Environmental Chemistry Group, accuracy of chemical analysis will be determined
[for each matrix of interest (sediment, tissue and seawater)] through the analysis of matrix spikes,
surrogate internal standards, method blanks and, when available, SRMs.  SRMs are materials that have
been certified by a recognized authority [e.g., National Institute of Standards and Technology (MIST)] and
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Battelle Marine Sciences Laboratory                                         Section: 4
Marine Chemistry and Ocean Processes Group                                       Revision: 4
Quality Assurance Management Plan                                               Date: May, 2000
Volume 2                                                                     Page 5 of 11

which are treated and analyzed as an actual sample. Matrix spikes will be performed by adding a known
quantity of target analytes into a sample and preparing and analyzing the sample the same as a regular
sample.  Surrogate internal standards will be spiked into each sample for organics analyses just prior to
extraction and will be used to monitor the  method performance.  Method blanks will be used to measure
contamination associated with laboratory processing and analyses.


For measurements where matrix spikes are used, percent recovery will be used to assess accuracy:

                             %R= S-U  x100
                                      Csa

                             where  %R = percent recovery
                                      S = measured concentration in spiked aliquot
                                      U = measured concentration in  unspiked aliquot
                                      Csa = actual concentration of spike added
For situations where a SRM is used, percent difference or percent recovery will be used:

                             PD = C1^C2 x100
                                    ~C2  "

                             where   PD = percent difference
                                     C-| = measured value
                                     C2 = certified or consensus value

                             %R = C1 x100
                                  C2

                             where   %R = percent recovery
                                     C-| = measured value
                                     C2 = certified or consensus value

4.2.3 Representativeness

Representativeness expresses the degree to which data accurately and precisely represent a
characteristic of a population, parameter variations at a sampling point, a  process condition, or an
environmental condition.

Representativeness will be addressed primarily by the proper handling  and storage of samples and
analysis within the specified holding times so that the material analyzed reflects the material collected as
accurately as possible.  Representativeness of data  will be discussed, when appropriate, in deliverable
reports.

4.2.4 Comparability

Comparability expresses the confidence with which one data set can be compared to another.
Comparability will not be quantified, but will be addressed through the use of laboratory methods that are
based on EPA or other recognized methods. The use of standard reporting units also will facilitate
comparability with other data sets.  Comparability of other data will be discussed, when appropriate, in
deliverable reports.

4.2.5 Completeness
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Battelle Marine Sciences Laboratory                                        Section: 4
Marine Chemistry and Ocean Processes Group                                       Revision: 4
Quality Assurance Management Plan                                               Date: May, 2000
Volume 2                                                                     Page 6 of 11
Completeness is a measure of the amount of valid data obtained from a measurement system compared
to the amount that was expected to be obtained under normal conditions.

Target completeness values are 100% for chemical sample analysis.
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Battelle Marine Sciences Laboratory
Marine Chemistry and Ocean Processes Group
Quality Assurance Management Plan
Volume 2

4.3 HOLDING TIMES AND PRESERVATION
                                   Section: 4
                                          Revision: 4
                                          Date: May, 2000
                                          Page 7 of 11
Holding times for analytical chemistry typically begin with the day of sample collection. These holding
times and requirements are listed in Table 4.3.  Because MSL can not control the fate of samples prior to
receiving them, MSL calculates holding times from the time of sample receipt.  However, sample
collection data are recorded and holding times can be assessed from both the date of sample collection
and the date of sample receipt, depending on customer preference.
                   TABLE 4.3 Sample Holding Times and Preservation
          Analysis
  Preservation
     Holding Time
Sediment*
       Metals (except Hg)

       Mercury

       Organic Compounds
       Grain Size
Tissue*
       Metals (except Hg)
       Mercury
Water
       Metals (except Hg)
       Organic Compounds
freeze dried at room temp.
or frozen at-20°C
freeze dried at room temp.
or frozen
4 °C /-20 °C

4°C

freeze dried at room temp.
or frozen at-20 °C
freeze dried at room temp.
or frozen
       Organic Compounds    4 °C / -20 °C
<2 pH with HMOs/room temp.
4°C
6 months

28 days(a)

30 daysC3) to extraction; 40 days
(to analysis after extraction)
6 months

6 months

28 days(a)

30 daysC3) to extraction; 40 days
(to analysis after extraction)

6 months (Hg 28 days)
7 days to extraction; 40 days (to
analysis after extraction)
(a)  If samples are freeze dried, then samples can be held for up to 6 months.

(b)  TWO references state that if sediments and tissues are held frozen (-20 °C), then holding times for
chemical analysis may be extended up to 6 months:  (1) Puget Sound Estuary Program, Recommended
Guidelines for Measuring Organic Compounds in Puget Sound Sediment and Tissue Samples, EPA,
December 1989; and (2) EPA, Analytical Methods for U.S. EPA Priority Pollutants and 301 (h) Pesticides
in Estuarine and Marine Sediments, EPA, May 1986.
*  After receipt at the laboratory, sediment and tissue samples for analysis of metals will be held
refrigerated (4 °C ± 2 °C) until freeze dried.
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Battelle Marine Sciences Laboratory                                         Section: 4
Marine Chemistry and Ocean Processes Group                                       Revision: 4
Quality Assurance Management Plan                                               Date: May, 2000
Volume 2                                                                     Page 8 of 11

4.4 CONTROL CHARTS

Control charts are used to assess quality control (QC) efforts in the laboratory by graphically presenting
the variability overtime of the various analyses performed. The control charts produced are theoretically
based on normally-distributed measurements and short-term variation. The data that are presented in a
control chart may vary with the analysis, information sought, the amount of data available, and customer
specifications. Details of the control charting process used at the MSL are covered in procedure, MSL-Q-
006, Procedures for Control Charting.  A brief description of the methods used, the criteria used for
assessing out of control events, and the administration of the control charts is presented here.

4.4.1  Control Chart Methodology

The control charts produced are based on normally distributed measurements and short-term variation.
Precision is charted overtime by calculating a mean recovery for the control sample parameters and then
establishing upper and lower warning and control limits.  The warning limit is defined as ±2o and the
control limits are defined as ±3o .  The control samples used for organic parameters are blank spikes and
for inorganic parameters results from the analyses of a standard reference material are plotted. A
minimum of 20 points are used to set the initial control limits for each parameter.

SRMs used as inorganic control samples are generally obtained from either NIST or the National
Research Council of Canada (NRCC).  All certificates of accepted values for the SRMs are kept in a
central SRM log book by inorganic laboratory supervisor. Inorganic SRMs are available for water,
sediment and tissue and separate control charts for each SRM analyzed will be maintained.

4.4.2 Criteria for Assessing Out  of Control Events

The laboratory process for a particular analyte will be considered out of control whenever, as a minimum,
any one of the following conditions is demonstrated:

1.    Any one point is outside of the control limits;
2.    Any three consecutive points are outside of the warning limits;
3.    Any eight consecutive points are on the same side of the centerline;
4.    Any six consecutive points are such that each point is higher or lower than its immediate
     predecessor;
5.    Any obvious cyclic pattern is seen in the points.

When any one of the situations listed above occurs, it is the responsibility of the appropriate laboratory
supervisor to  notify the MSL QA Officer and Project Manager so that appropriate corrective actions can
be determined and  the situation documented by filling out a Quality Problem Report form and attaching a
copy to the control chart. Details regarding the procedure and information required on a Quality Problem
Report form are described in procedure MSL-A-005, Deviations  from Established Requirements.

4.4.3 Administration of Control Charts

One set of control samples (e.g. one set of blank spikes for organic parameters and one SRM for
inorganic parameters)  is analyzed with each batch of samples, with a batch consisting of no more than 20
samples. Control charts are produced quarterly by the data manager and distributed to the laboratory
supervisors and appropriate project managers. Project-specific  requirements may have a greater
frequency, or may require that control be prepared only for control  samples run with project-specific
samples. Table 4.4 lists the minimum numbers of parameters to be charted.

Note that control charts are only used for monitoring blank spikes and SRMs.  Control limits for matrix
spikes, replicate analyses, blank analyses etc. are generally defined  by the project guidelines.  If
available, standard EPA control limits are used. Additional or alternate compounds may be charted if
necessary.
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Battelle Marine Sciences Laboratory
Marine Chemistry and Ocean Processes Group
Quality Assurance Management Plan
Volume 2
                                Section:  4
                                      Revision: 4
                                      Date: May, 2000
                                      Page 9 of 11
                        TABLE 4.4 Control Chart Parameters
         Matrix
QC Sample
    Analyte and/or Method
Matrix
Water or Sediment/Tissue
Blank Spikes
 ORGANICS

   Parameter
   PAHs
   PCBs
   PCBs
   Pesticides
   Butyltins

INORGANICS
Compounds
Anthracene, Benzo(a)pyrene
Aroclor 1254
2 Congeners or Total PCB
Dieldrin
Tributyltin
Matrix
Water (fresh)
Sediment (estuarine)
Tissue (shellfish)
   Metals/ Method
   Cd, Cu, Zn, Pb/ ICP-MS,
   Cd, Cu, Zn, Pb/ ICP-MS or GFAA, Hg/CVAA
   Cd, Cu, Zn, Pb/ ICP-MS or GFAA, Hg/CVAA
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Battelle Marine Sciences Laboratory                                               Section:  5
Marine Chemistry and Ocean Processes Group                                       Revision: 4
Quality Assurance Management Plan                                               Date: May, 2000
Volume 2                                                                     Page 1 of 1

                                 5.0 CORRECTIVE ACTION

The need for corrective action may be identified by the technical staff during the course of their work or
through assessments or data audits. Each individual performing laboratory or data processing activities
will be responsible for notifying the appropriate supervisory personnel of any circumstance that could
affect the quality or integrity of the data.

5.1 DEVIATIONS

All deviations from approved procedures, project planning documents or this QAMP will be documented.
Depending on the severity of the deviation, the MSL QA Officer and the Project Manager will determine
how the deviation will be documented through

        use of a Quality Problem Report (QPR) form (Exhibit 12.1 of Volume 1) per MSL-A-005,
        Deviations  from Established Requirements;

        documented as part of the narrative summary provided to the customer, and

        documented directly on the raw data.

The MSL QA  Officer and the Project Manager will determine if there is a formal deviation when one or
more control limits are exceeded in a data set. In some cases, the customer may be involved in these
discussions.  Deviations from project control limits will be identified in the narrative accompanying the
data set or package or in a letter to the customer, and the impact of the deviation addressed. The
following are guidelines to resolving deviations identified within the Marine and Environmental Chemistry
Group:

        When sample integrity is compromised or questionable (e.g., mislabeling, broken or leaking
        sample containers, improperly preserved samples, expiration of sample holding times), it is the
        responsibility of the staff who identify the problem to bring it immediately to the attention of the
        Project Manager or Technical Group Leader for resolution.

        In the event of an instrument problem, it is the responsibility of the operator to attempt to correct
        the problem (e.g., recalibrate the instrument). If the problem persists or cannot be  identified, the
        issue should be brought to the attention of the Technical Group Leader for resolution.

        Corrective actions for results outside established DQOs are addressed in section 5.2.

5.2 CORRECTIVE ACTION FOR DATA OUTSIDE OF CONTROL LIMITS

It is the responsibility of the analyst to monitor QC sample results.  Results outside the established criteria
in method procedures or project specific criteria will  be brought to the attention of the Laboratory
Supervisor and Project Manager who will determine  and document the appropriate corrective action. The
corrective actions may include, but are not  limited to, review of data and calculations, flagging of suspect
data (flagging requirements are addressed  in Section 6.0) or re-extraction and/or re-analysis of individual
or entire batches of samples. Documentation may take the form of flagging the QC data and/or sample
data in the report.  The form  of documentation is project specific, but at a minimum, the QC data that is
outside the established criteria shall be flagged. In addition, during the process of data review performed
by the MSL QA Officer or representative as per procedure, MSL-Q-005, Quality Assurance Data Audits,
the QC data of concern my be required to be addressed in the narrative to the customer accompanying
the sample data.
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Battelle Marine Sciences Laboratory                                         Section: Appendix A
Marine Chemistry and Ocean Processes Group                                       Revision: 4
Quality Assurance Management Plan                                                Date: May, 2000
Volume 2                                                                      Page 2 of 2

                                    6.0 DATA REPORTING

All reported data will be validated and verified in accordance with Section 10 of Volume  1. Chemistry
data and all accompanying QC data will be reported as tables of validated data points for analysis.
Reporting limits are defined as MDLs or, when required by a client, target detection limits.  When
reporting data, the following example data flags will be used where appropriate:

    U   Analyte not detected  at or above the detection limit shown

    J   Analyte detected below the detection limit; concentration reported may be an estimate

    B   Analyte detected in sample is less than 5 times the blank value

    E   Analyte concentration estimated because of matrix interference in sample

    X   Analyte quantified outside of the calibration range of the instrument

    D   Analyte determined from diluted sample

In addition, all QC data that falls outside established control limits will be flagged.
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Battelle Marine Sciences Laboratory                                        Section: Appendix A
Marine Chemistry and Ocean Processes Group                                      Revision: 4
Quality Assurance Management Plan                                              Date:  May, 2000
Volume 2                                                                    Page 2 of 2

                                     7.0 REFERENCES

Allen, H.E., G. Fu, and B. Deng. 1990.  Development of Analytical Method for the Determination of Acid
Volatile Sulfide (AVS) in Sediment. Department of Civil Engineering.  University of Delaware.  Newark,
Delaware. September 1990.

Bligh, E.G., and W. J. Dyer.  1959. A Rapid Method of Total Lipid Extraction and Purification.  Canadian
Journal of Biochemistry and Physiology. Vol 37 No. 8.  pp. 911-917.

Bloom  and Crecelius. 1983. Determination of Mercury in Seawater at Sub-nanogram Per Liter Levels.
Marine Chem.  14:49-59.

Bloom  and Crecelius. 1984. Determination of Silver in Seawater by Coprecipitation with Cobalt
Pyrrolidinedithiocarbamate and Zeeman Graphite Furnace Atomic Absorption Spectrometry. Anal. Chim.
Acta 156:139-145.

Bloom  1989. Determination of Picogram Levels of Methylmercury by Aqueous Phase Ethylation,
Followed  by Cryogenic Gas  Chromatography with Cold Vapor Atomic Fluorescence Detection.  Can. J.
Fish. Aquat, Sci.,  Vol. 46, 1989.

Brugmann, L., L.G. Danielsson, B. Magnusson, and  S. Westerlund. 1983. Intercomparison of different
methods for the determination of trace metals in seawater. Mar. Chem. 18:327-339.

Cutter,  G.A.  1978. Species Determination of Selenium in Natural Waters. Anal. Chim. Acta. 98:59-66.

EPA.  1979.  Revised (1983).  Methods  for the Chemical Analysis of Water and Wastes. EPA-600/4-79-
020. U.S. EPA, Environmental Monitoring Systems Laboratory, Cincinnati, OH.

EPA.  1986.  The Determination of Polychlorinated Biphenyls - Cleaning Methods for XAD-2 Resin and
Filters,  in Quality Assurance Plan - Green Bay Mass Balance Study. EPA 660/4-86-045.

EPA.  1991.  Methods for the Determination of Metals in Environmental Samples. EPA-600/4-91-010.
Environmental Services Division, Monitoring Management Branch.

EPA, 1994 (revised). Methods for Chemical Analysis of Water and Wastes.  EPA/600/5-94. U.S. EPA,
Cincinnati, Ohio.

EPA.  1995.  Method 1637.  Determination of Trace Elements in Ambient Waters by Chelation
Preconcentration  with Graphite Furnace Atomic Absorption.  EPA 821-R-95-030. April 1995. U.S. EPA,
Office of Water. Washington, D.C.

EPA.  1996a. Test Methods for Evaluating Solid  Waste. U.S. EPA, Office of Solid Waste and Emergency
Response, Washington, D.C. (SW846)

EPA.  1996b. Method 1631. Mercury in Water by Oxidation, Purge and Trap, and  Cold Vapor Atomic
Fluorescence Spectrometry. EPA 821-R-96-012. July 1996.

EPA.  1996c. Method 1640. Determination of Trace Elements in Ambient Water by On-Line Chelation
Preconcentration  and Inductively Coupled Plasma-Mass Spectrometry. January 1996.

EPA.  1996d. Method 1638. Determination of Trace Elements in Ambient Water by Inductively Coupled
Plasma-Mass Spectrometry. Draft, January 1996.

EPA, 1997. Test Methods for Evaluating Solid Waste. EPA/SW-846. U.S.  EPA, Office of Solid Waste
and Emergency Response.  Washington, D.C.
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Battelle Marine Sciences Laboratory                                       Section:  Appendix A
Marine Chemistry and Ocean Processes Group                                      Revision: 4
Quality Assurance Management Plan                                             Date: May,  2000
Volume 2                                                                    Page 2 of 2

EPA.  1998a.  Method 1630.  Methyl Mercury in Water by Distillation, Aqueous Ethylation, Purge  and
Trap, and CVAFS. Draft. March 1998.

EPA.  1998b.  Method 1632.  Chemical Speciation of Arsenic in Water and Tissue by Hydride Generation
Quartz Furnace Atomic Absorption. Draft, Revision 2.0, March 1998.

EPRI, 1986.  Speciation of Selenium in Natural Waters and Sediments: Volume 1; Selenium Speciation.
EPRIEA-4641. Electric Power Research Institute.  Norfolk, Virginia.

Kostas, D.D., O'Conner, T.P., Crecelius,  E.A. 1997. Evaluation of Digestion Procedures for Determining
Silver in Mussels and Oysters. Environ. Sci. Technol. 1997, 31, 2303-2306.

Krahn et al. 1988.  New HPLC Cleanup and Revised Extraction Procedures for Organic Contaminants.

NOAA Technical Memorandum NMFS F/NWC-153.  1988.

NOAA 1993. NOAA Status and Trends Technical Memorandum, NOSORCA71, July 1993.

NOAA Technical Memorandum NOS ORCA 130 "Sampling and Analytical Methods of the National Status
and Trends Program Mussel Watch Project: 1993-1996 Update". G.G Lauenstein and A.Y. Cantillo, eds.

Plumb, R.H., Jr. 1981.   Procedure for Handling and Chemical Analysis of Sediment and Water Samples.
Tech. Rep. EPA/CE-81-1. Prepared by Great Lakes Laboratory, State  University College at Buffalo,
Buffalo, NY, for the U.S. EPA/U.S. Army  Corps of Engineers Technical  Committee on Criteria for Dredged
and Fill Material. U.S. Army Corps of Engineers, Waterways Experiment Station, Vicksburg, MS.

Rafter, T.A. 1950. Sodium Peroxide Decomposition of Minerals in Platinum Vessel. Analyst  1950.
Volume 75, pp. 485-492.

Standard  Methods 1995.  Standard Methods for the Examination of Water and Wastewater. 19th Edition.
American Public Health Association, American Water Works Association, Water Environment Federation.

Unger, M.A., W.G. Maclntyre, J. Greaves, and R.J. Huggett. 1986.  GC Determination of Butyltins in
Natural Waters by  Flame Photometric Detection of Hexyl Derivatives with Mass Spectrometric
Confirmation.  Chemosphere 15(4):461-470.
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Battelle Marine Sciences Laboratory
Marine Chemistry and Ocean Processes Group
Quality Assurance Management Plan
Volume 2
Section: Appendix A
       Revision: 4
       Date: May, 2000
       Page 2 of 2
                                        APPENDIX A
                            MARINE CHEMISTRY EQUIPMENT LIST

The following is a list of the major pieces of equipment in both the organic and inorganic chemistry
laboratories. This list is intended to demonstrate the types of equipment available and will be revised
when the QAMP is revised, but not each time equipment or instruments are added or deleted.
Balances
Make
Sartorius
Mettler
Fisher/Denver
Denver
Ohaus
Mettler
Sartorius
Mettler
Sartorius

Model
B3100P
AE50
XL300
XP-300
CT200
PE3600
BP3100S
AC100
LC1200S

Serial Number
40019183
M21198
09630
990131
CD03172
D56329
50806575
A89515
10606711

Location
MSL5
118
118
126
126
126
215
223
231
231
ORGANIC CHEMISTRY
EQUIPMENT
Measures
Determination of TBT,
alkanes, phosphorus
and sulfur compounds
PAHs and phthalates
Chlorinated compounds,
PCBs and pesticides
Presently idle
Sample clean up, Gel
permeation
chromatography,
explosives, and PAHs
Sample clean up, Gel
permeation
chromatography,
explosives, and PAHs

Description
Hewlett Packard 5890 Gas Chromatograph/
Flame Photometric Detector/ Flame lonization
Detector
Hewlett Packard 5890 Gas
Chromatograph/Model 5970 Quadropole Mass
Selective Detector
Varian Star 3600 CX Gas
Chromatograph/Electron Capture
Detector/Flame lonization Detector
VG Fison Model TRIO 1000 Gas
Chromatograph/Liquid Chromatograph/Mass
Spectrometer with Thermospray/Plasmaspray
Interface
High Performance Liquid Chromatograph
(HPLC) system with autosampler,
UV/Florescence Detector
High Performance Liquid Chromatograph
(HPLC) system with autosampler,
UV/Florescence Detector

Serial or ID
Number
WB73809
N821982
N830047
N828035
WD28663
N828182

Location
MSL5
223
215
223
215
223
114
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Battelle Marine Sciences Laboratory
Marine Chemistry and Ocean Processes Group
Quality Assurance Management Plan
Volume 2
Section: Appendix A
       Revision: 4
       Date: May, 2000
       Page 2 of 2
INORGANIC
CHEMISTRY
EQUIPMENT
Measures
Metals
Mercury and
Methylmercury
Mercury and
Methylmercury
Mercury and
Methylmercury
Metals
Metals
Metals
Atomic Absorption
Spectrometers
Metals
Metals
Mercury (back up only)
Mercury (back up only)
Mercury (back up only)
Mercury

Description
Perkin-Elmer Elan 5000 inductively coupled
plasma mass spectrometer (ICP-MS)
Perkin-Elmer Elan 6100 inductively coupled
plasma mass spectrometer (ICP-MS)
Cold Vapor Atomic Fluorescence Unit - In-
house design - #1
Cold Vapor Atomic Fluorescence Unit - In-
house design - #2
Cold Vapor Atomic Fluorescence Unit - In-
house design - #3
Perkin-Elmer Optima 3000 ICP-AES
GFAA Perkin-Elmer 5100 ZL graphite furnace
Dionex4500i, Ion Chromatograph, autosampler,
conductivity detector and UV/VIS Detector

Perkin-Elmer Model 5100 Zeeman-effect
graphite furnace
Perkin-Elmer Model 5000 with Zeeman-effect
graphite furnace
Cold Vapor Atomic Absorption Units - Lab Data
Control - #1
Cold Vapor Atomic Absorption Units - Lab Data
Control - #2
Cold Vapor Atomic Absorption Units - Lab Data
Control - #3
Thermo Separation Products (TSP) 3200
Automated Mercury Analyzer

Serial or ID
Number
WD08519
PT06550
PT08031
N830368
R101823
N830377
N830371
WB67819

N830372
WB73815
WA71764
WA26316
N822042
R101553

Location
MSL5
227
126
126
126
114
114
114

222
222
126
126
126
126
GFAA   Graphite Furnace Atomic Absorption
HPLC    High Performance Liquid Chromatograph
ICP-MS  Inductively Coupled Plasma (Emissions) - Mass Spectrometry
ICP-AES Inductively Coupled Plasma -Atomic Emissions Spectrometry
PAH     Polycyclic Aromatic Hydrocarbons
PCB     Polychlorinated Biphenyls
TBT    Tributyl Tin
UV      Ultraviolet (light)
VIS      Visible (light)
-------
 <|Baiteiie
  . . . Putting Technology To Work
Marine Sciences
Laboratory
 QUALITY ASSURANCE MANAGEMENT PLAN
 MARINE ECOLOGICAL PROCESSES GROUP

            VOLUME 3
January, 2000
-------
                       Battelle Marine Sciences Laboratory
                         1529 West Sequim Bay Road
                          Sequim, Washington 98382
                               (360)683-4151
                      Battelle Marine Sciences Laboratory
                 MARINE ECOLOGICAL PROCESSES GROUP
                 QUALITY ASSURANCE MANAGEMENT PLAN
                                VOLUME 3

                         Concurrences and Approvals
D. Coffey                                     Date
Quality Assurance Officer
360-681-3645
R.M. Thorn                                    Date
Ecosystem Processes and Restoration
Technical Group Manager
360-681-3669
J.A. Ward                                     Date
Ecotoxicology and Risk Assessment
Technical Group Manager
360-681-3669
R. M. Ecker
MSL Manager
360-681-3602
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                    Battelle Marine Sciences Laboratory
                MARINE ECOLOGICAL PROCESSES GROUP
                QUALITY ASSURANCE MANAGEMENT PLAN
                              VOLUME 3
                               Contents

                                                     Issue Date  Rev.
1.0   SAMPLE CONTROL	1/2000    1
     1.1   SAMPLE RECEIPT AND LOG-IN
     1.2   SAMPLE TRACKING
     1.3   SAMPLE ARCHIVING AND DISPOSITION

2.0   BIOLOGICAL PROCEDURES	1/2000    1

3.0   EQUIPMENT MAINTENANCE AND CALIBRATION	1/2000    1
     3.1   EQUIPMENT CALIBRATION
     3.2   PREVENTATIVE MAINTENANCE

4.0   QUALITY CONTROL	1/2000    1
     4.1   HOLDING TIMES AND PRESERVATION
     4.2   WATER QUALITY MONITORING
     4.3   REFERENCE TOXICANT TEST
     4.4   TOXICITY TESTS
     4.5   CONTROL CHARTS

5.0   CORRECTIVE ACTION	1/2000    1
     5.1   DEVIATIONS
     5.2   CORRECTIVE ACTION FOR DQO EXCEEDENCES

6.0   DATA REPORTING	1/2000    1

7.0   REFERENCES	1/2000    1

                             APPENDICES

A    LIST OF EQUIPMENT	1/2000    0
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Battelle Marine Sciences Laboratory                                             Section: 1
Marine Ecological Processes Group                                              Revision:  1
Quality Assurance Management Plan                                             Date: January, 2000
Volume 3                                                                    Page 1 of 1

                                  1.0 SAM RLE CONTROL

Sample handling and tracking with the Marine and Environmental Chemistry Group is covered by two
procedures: MSL-A-001, Sample Log-in Procedure and MSL-A-002, Sample Chain of Custody. The
processing of data collected from these activities discussed in procedure MSL-D-004, Data Reporting,
Reduction, Back Up, and Archiving. The following is a description of the procedure used for receipt and
tracking of samples, as well as chain of custody procedures.

1.1 SAM RLE RECEIPT AND LOG-IN

Samples or test organisms are logged in when received in the shipping area.  If a Chain of Custody (CoC)
form accompanies the samples or test organisms, this form is used to document the date and time of
sample receipt and condition.  If a CoC form is not shipped with samples, an MSL form will be initiated.
For test organisms, a shipping form can  be signed and dated and the condition of organisms noted.
Cooler temperatures are taken and recorded on the CoC. The sample labels are compared to the CoC
and assigned an identification code plus sequential numbering of samples upon arrival. Chain of Custody
forms (if present) are compared to  sample container labels and sample containers are inspected for
sample integrity (e.g., broken seals, broken or cracked containers, spilled samples, sample temperature).
Any discrepancies are brought to the attention of the Project Manager who is responsible for contacting
the client as well as returning a signed copy of the custody form.  If the samples are not immediately
prepared for testing, they are stored at approximately 4 °C until used.

See Section 4.1  for holding times for suspended sediment, sediment, effluent, and elutriate samples.
1.2 SAM RLE TRACKING

Sample tracking, while samples are in the laboratory, is the responsibility of the individual Laboratory
Supervisors and the Project Manager.  It is the responsibility of the Project Manager to ensure that the
samples are given the appropriate priority in scheduling and that the proper tests and methods are being
performed.

1.3 SAMPLE ARCHIVING AND DISPOSITION

The Project Manager is responsible for proper disposal of leftover samples material.  Sample disposition
takes three forms: 1) dispose of by appropriate means depending on sample content; 2) return to client;
or 3) archive  indefinitely.  Unless arrangements have been made previously, the samples are generally
disposed of by Battelle.  If samples are to be disposed of by Battelle, the Project Manager notifies the
Health  and Safety Officer who then completes a Chemical  Disposal Recycle Request form in accordance
with Subject Area, Managing Nonradioactive Chemical Waste.  The Health and Safety Officer then must
determine the appropriate disposition and approve the form prior to sample disposition. A copy of this
form is maintained in the appropriate project central file.
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Battelle Marine Sciences Laboratory
Marine Ecological Processes Group
Quality Assurance Management Plan
Volume 3
Section: 2
Revision:  1
Date:  January, 2000
Page 1 of 3
                              2.0 BIOLOGICAL PROCEDURES
All routine, repetitive biological laboratory activities are directed and controlled by internal Standard
Operating Procedures (SOP). Where possible, U.S. Environmental Protection Agency (EPA) and
consensus methods are used where the technique is applicable to the testing matrix and the overall
objective of the analysis. Table 2.1 lists the more routine toxicity tests performed at the MSL along with
the corresponding methods and SOPs associated with each of those tests. Table 2.2 lists the test
organisms and type of tests that are performed at the MSL.

All toxicity tests are controlled by some type of planning document, generally in the form of a Test Plan.
Other project planning documents such as work plans are occasionally used. Table 2.3 is an example of
a test conditions table that would  normally be included in a Test Plan.

          TABLE 2.1  List of  Biological Tests and Associated Methods and SOPs
Test
Amphipod
Echinoderm, Embryo - Larval
Echinoderm, Fertilization
Echinoderm, Sediment
Fish, Acute
Bivalve, Sediment
Bivalve, Embryo - Larval
Inland Silverside, Acute
Inland Silverside, Chronic
Microtox
Microtox, Sediment
Mysid, Acute
Mysid, Chronic
Polychaetes, Sediment
Holmesimysis
Bioaccumulation
Method
EPA 600/4-90/027F; ASTM 1367-92
EPA 600/R-95/136; ASTM E-1 563-95
EPA 600/R-95/1 36 (Method 1008.0)
PSEP 1995
EPA 600/4-90/027F
PSEP 1995
EPA 600/R-95/136 (Method 1005.0); ASTM E-
724-94
EPA 600/4-90/027F
EPA 600/4-87/028; 600/4-91/003
Microbics Corporation
PSEP 1995
EPA 600/4-90/027F
EPA 600/4-87/028; 600/4-91/003
PSEP 1995
EPA 600/R-95/136; EPA/503/8-91/001
EPA 503/8-91/001
SOP
MSL-T-005
MSL-T-013
MSL-T-01 1
MSL-T-018
NA2
MSL-T-006
MSL-T-008
MSL-T-01 7
MSL-T-01 6
NA
NA
MSL-T-01 4
MSL-T-01 5
MSL-T-006
MSL-T-01 0
MSL-T-004
2 NA   Not available
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Battelle Marine Sciences Laboratory
Marine Ecological Processes Group
Quality Assurance Management Plan
Volume 3
Section: 2
Revision: 1
Date: January, 2000
Page 2 of 3
                 TABLE 2.2  Test Organisms Commonly Used by the MSL
Appropriate Use of
Test Organism
Scientific Name
Acropora elseyi
Ammodytes hexapterus
Amphiprion clarkii
Arbacia punctulata
Capitella capitata
Champia pan/a
Citharichthys stigmaeus
Clupea pallasi (eggs, larvae,
adults)
Crassotrea gigas
Cyprinidon vulgaris
Daphnia spp.
Dendraster excentricus
Dinophilus spp.
Holmesimysis spp.
Isochrisis spp.
Selenastrum spp.
Menidia beryllina
Mysidopsis bahia
Mytilus spp.
Onchorhynchus spp.
Oryzias latipes
Penaeus spp.
Photobacterium phosphoreum
Strongylocentrotus purpuratus
Ampelisca abdita
Corophium spinicorne
Eohaustorius estuarius
Grandidierella japonica
Hyallella azteca
Leptocheirus plumulosus
Neanthes arenoceodentata
Panopea generosa
Rhepoxynius abronius
Abarenicola pacifica
Macoma nasuta
Nephtys caecoides
Nereis virens
Common Name
Coral
Sandlance
Clownfish
Sea Urchin
Polychaete
Algae
Sanddab
Pacific Herring
Oyster
Sheepshead Minnow
Water Flea
Sand Dollar
Polychaete
Mysid
Algae
Algae
Inland Silverside
Mysid
Mussel
Salmon
Medaka
Shrimp
Microtox
Sea Urchin
Amphipod
Amphipod
Amphipod
Amphipod
Amphipod
Amphipod
Polychaete
Clam, Geoduck
Amphipod
Polychaete
Clam, Bent Nose
Polychaete
Polychaete
Test Type
Acute
Acute
Acute
Acute/Chronic
Acute/Chronic
Acute/Chronic
Acute/Chronic
Acute/Chronic
Acute/Chronic
Acute/Chronic
Acute/Chronic
Acute/Chronic
Acute/Chronic
Acute/Chronic
Acute
Acute
Acute/Chronic
Acute/Chronic
Acute/Chronic
Acute/Chronic
Acute/Chronic
Acute
Acute/Chronic
Acute/Chronic
Acute
Acute
Acute
Acute
Acute
Acute/Chronic
Acute/Chronic
Acute
Acute
Acute
Chronic
Acute/ Chronic
Acute/ Chronic
Aquatic
Phase
^
^
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Battelle Marine Sciences Laboratory
Marine Ecological Processes Group
Quality Assurance Management Plan
Volume 3
Section: 2
Revision:  1
Date:  January, 2000
Page 3 of 3
        TABLE 2.3  Example of a Test Conditions Table Established for a Test Plan
Paramet
er
Test Type
Water Quality
Temperature
Salinity
PH
Dissolved Oxygen (DO)
Photoperiod
Test Chamber
Test Solution Volume
Life Stage of Organisms
# of Organisms per
Chamber
# of Replicate Chambers
per Treatment
Feeding
Reference Toxicant
Concentration Series
Dilution Water
SPP Prep Water
Dilution Series and
Concentrations3
Test Duration
Endpoint
Conditio
ns
M. beryllina
Water-column, static
H. costata
Water-column, static
M. galloprovincialis
Water-column, static
Temperature, pH, salinity, and DO will be monitored on all replicates on Day 0 and
Termination Day and in one replicate on remaining days
20 °C ± 2 °C
30%o ± 2%o
7.30-8.30 pH units
20 °C ± 2 °C
30%o ± 2%o
7.30 -8.30 pH units
>40% saturation; aeration provided to all chambers only
if DO is <40%
16L8D
500 mL glass jar
300 mL
< 5 days
10
5
Concentrated Artemia
nauplii, fed daily
CuatO, 150,200, 300,
400 ng/L
NH3atO, 10,30,60, 90
mg/L
0.45 urn-filtered Sequim
Bay seawater
dredging site water
0%, 10%, 50%, and 100%
SPP
96 h
Survival (LC^Q)
16L8D
400 mL glass jar
200 mL
5 days
10
5
Concentrated Artemia
nauplii, fed daily
CuatO, 50, 100, 150,200
ng/L
NH3atO, 20, 40, 60, 80
mg/L
0.45 urn-filtered Sequim
Bay seawater
dredging site water
0%, 10%, 50%, and 100%
SPP
96 h
Survival (LC^Q)
15°C±2°C
30%o ± 2%o
7.30-8.30 pH units
>60% saturation
16L8D
500 mL glass jar
300 mL
4 hours
4500 to 9000 embryos per
chamber
5
None
CuatO, 1, 4, 16, 64 ng/L
NH3atO, 1,4,8, 16, 32
mg/L
0.45 urn-filtered Sequim
Bay seawater
dredging site water
0%, 10%, 50%, and 100%
SPP
48 to 72 h
Survival (LCsg) and
normal development
(EC50)
       A 1% SPP dilution may be added if low-level affects are anticipated.
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Battelle Marine Sciences Laboratory
Marine Ecological Processes Group
Quality Assurance Management Plan
Volume 3
                                                    Section:  2
                                                    Revision: 1
                                                     Date:  January, 2000
                                                     Page 4 of 3
 Test Acceptability
90% Survival in control
90% Survival in control
  90% Survival and 70%
normal development in the
        controls
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Battelle Marine Sciences Laboratory                                        Section: 3
Marine Ecological Processes Group                                               Revision:  1
Quality Assurance Management Plan                                              Date:  January, 2000
Volume 3                                                                    Page 1 of 1

                   3.0 EQUIPMENT MAINTENANCE AND CALIBRATION

Instruments used for routine measurements of chemical and physical parameters, such as pH, dissolved
oxygen (DO), temperature, salinity, and ammonia, are calibrated and standardized prior to use. All
calibration and  preventative maintenance data are documented.

3.1 EQUIPMENT CALIBRATION

Calibration procedures are performed on each water quality instrument prior to use. Requirements for
levels and frequency of calibration are described in procedures specific to each water quality instrument:
              •   MSL-W-001 Calibration and Use ofpH Meters
              •   MSL-W-002 Calibration and Use of Dissolved Oxygen Meters
              •   MSL-W-003 Calibration and Use of Thermometers
              •   MSL-W-004 Calibration and Use of Refractometers
              •   MSL-W-007Routine Water Quality Measures for Toxicity Tests, and
              •   MSL-W-008 Determination of Ammonia

All calibration records are kept in the data files and must be traceable to date and standards. Corrective
actions to be taken when calibration criteria are not met, are described in section 5.0 of this document
and in the specific procedures.

3.2 PREVENTATIVE MAINTENANCE

Instruments are serviced regularly by trained in-house personnel. Written records of all instrument
maintenance, calibration, testing, and inspection  are maintained. Maintenance records contain a
description of the operation or problem, the remedial action taken (if necessary), date, the person
responsible, and where applicable, documentation of the instrument's return to acceptable use.
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Battelle Marine Sciences Laboratory                                        Section: 4
Marine Ecological Processes Group                                               Revision:  1
Quality Assurance Management Plan                                              Date:  January, 2000
Volume 3                                                                    Page  1 of 2

                                  4.0 QUALITY CONTROL

Quality control in toxicity tests consists of establishment of criteria for water quality, test acceptability,
reference toxicant tests, replication, control treatments, etc. Each toxicity test has its own quality control
criteria that are included as part of the test design established in project planning documents. See Table
2.3 for an example of an established test conditions table.

4.1 HOLDING TIMES AND PRESERVATION

Holding times for toxicity tests typically begin the day of sample collection. Holding times and
preservation requirements are listed in Table 4.1.


                    TABLE 4.1  Sample Holding Times and Preservation
Matrix
Sediment
Effluent
SPP/Elutriate
Preservation
4 °C ± 2 °C/dark/airtight
4 °C ± 2 °C/dark/airtight
4 °C ± 2 °C/dark/airtight
Holding Time
2 weeks is recommended; up to 6 weeks is acceptable
36 hours from sample collection 0)
24 hours from preparation
0) Every effort must be made to initiate the test with an effluent sample on the day of arrival in the
laboratory. The holding time should not exceed 36 hours unless a variance is approved by the client.
4.2 WATER QUALITY MONITORING

Acceptable criteria for water quality (pH, DO, salinity, temperature, ammonia) measurements are
established for each test and are identified in project planning documents, such as a test conditions table.

4.3 REFERENCE TOXICANT TEST

Reference toxicant tests (positive controls), are performed to demonstrate that test organisms used are
appropriately sensitive and that the laboratory procedures and techniques are appropriate and
repeatable. A reference toxicant test is normally performed with each test, or at a minimum, once with
each batch of test organisms.

4.4 ACCEPTABILITY OF TOXICITY TESTS

Each test method contains specific test acceptability criteria for controls, reference toxicant results, test
conditions, etc. See Section 5.2 for corrective action when criteria are not met.

An individual test may be conditionally acceptable if temperature, DO, or other specified conditions fall
outside specifications, depending on the degree of the departure from the specified conditions and the
overall impact on the test.  The acceptability of the test will depend on the professional judgment of the
laboratory supervisor and project manager. Any deviation from test specifications must be noted when
reporting data.
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Battelle Marine Sciences Laboratory                                         Section: 4
Marine Ecological Processes Group                                                 Revision: 1
Quality Assurance Management Plan                                                Date: January, 2000
Volumes                                                                      Page 2 of 2

4.5  CONTROL CHARTS

Control charts are used to asses QC efforts in the laboratory by graphically presenting the variability over
time of the various analyses performed. Details of the control charting process used at the MSL are
covered in procedure MSL-Q-006, Procedures for Control Charting. A brief description of the methods
used, the criteria used for assessing out of control events, and the administration of the control charts is
presented here.

4.5.1 Control Chart Methodology

The control charts are based on normally distributed measurements and short-term variation. Precision is
charted overtime by calculating an 1050 and EC^Q for the reference toxicity tests and then establishing
upper and lower warning and control limits. The warning limit is defined as ±2a and the control limits are
defined as ±3a. A minimum of 10 points, but preferably 20, are used to set the initial control limits for
each parameter.

Reference toxicity tests are run concurrently with the majority of toxicity tests.  Separate control charts are
maintained for each reference toxicant for each species.

4.5.2 Criteria for Assessing Out of Control Events

The laboratory process for a particular analyte will be considered out of control whenever, as a minimum,
any one of the following conditions is demonstrated:

1.     Any one point is outside of the control limits;
2.     Any three consecutive points are outside of the warning limits;
3.     Any eight consecutive points are on the same side of the centerline;
4.     Any six consecutive points are such that each point is higher or lower than its immediate
      predecessor;
5.     Any obvious cyclic pattern is seen in the  points.

When any one of the situations listed above occurs, it is the responsibility of the appropriate laboratory
supervisor to notify the MSL QA Officer and Project Manager so that appropriate corrective actions can
be determined and  the situation documented by filling out a Quality Problem Report form  and attaching a
copy to the control chart.  Details regarding the procedure and  information  required on a Quality Problem
Report form are described in procedure MSL-A-005, Deviations from Established Requirements.

4.5.3 Administration of Control Charts

A minimum of one reference toxicant test is run with each toxicity test or at a minimum, once with each
batch of test organisms. Therefore, control results will be tracked after no more than 20 sequential
sample analyses.  It is the responsibility of Project Managers to provide data after each test to the control
chart administrator. Control charts are produced on at least a quarterly basis by the control chart
administrator, and this information is passed on to the Laboratory Supervisor and Project Managers, as
appropriate. If specific projects require it, more frequent updates and reviews of control charting will be
performed.
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Battelle Marine Sciences Laboratory                                                Section: 5
Marine Ecological Processes Group                                                Revision:  1
Quality Assurance Management Plan                                               Date: January, 2000
Volume 3                                                                     Page 1 of 2

                                 5.0  CORRECTIVE ACTION

The need for corrective action may be identified by the technical staff during the course of their work, and
through assessments or data audits.  Each individual performing laboratory or data processing activities
will be responsible for notifying the appropriate supervisory personnel of any circumstance that could
affect the quality or integrity of the data.

5.1 DEVIATIONS

All deviations from approved procedures,  project planning documents or this QAMP will be documented.
Depending on the severity of the deviation, the MSL QA Officer and the Project Manager will determine
how the deviation will be documented through

        use of a Quality Problem Report (QPR) form (Exhibit 12.1  of Volume 1) per MSL-A-005,
        Deviations from Established Requirements;

        documented as part of the narrative summary provided to  the customer, and

        documented directly on the raw data.

The following are guidelines for resolving  deviations identified within the Marine Ecological Processes
Group:

        The  response to technical problems in the field,  such as broken equipment, weather delays, or
        inability to sample specific locations, is the responsibility of Field Task Leader.  This individual
        determines the appropriate action, in conjunction with the  Project Manager and/or client
        representative.

        The  need for corrective action at the laboratory level, for events such as broken samples or
        improper instrument calibration, will be addressed by the Laboratory Supervisor or Project
        Manager.

        Corrective actions for results outside established DQOs are addressed in section 5.2.

5.2 CORRECTIVE ACTION FOR DQO EXCEEDENCES

DQO deviations are defined as deviations that are outside of test specific criteria addressed in Section 2.
Out-of-compliance data may be due to deviations from test protocols or deficiencies associated with
toxicological tests.  Examples of DQO deviations in toxicological tests are shown in Table 5.1.  Poor
control survival, out-of-range water quality measurements, out-of-range reference toxicant results, or
mishandling  of test organisms or test sediment/water may result in a decision to retest; minor episodes of
out-of-range water quality conditions, incomplete test monitoring information, or broken  or misplaced test
containers may only require that data be flagged and qualified. A summary of typical test deviations and
suggested corrective actions is presented in Table 5.1.

Corrective actions relative to toxicological tests may include, but are not limited to, review of data and
calculations, flagging and/or qualification of suspect data, or possible retesting. A review that provides a
preliminary check of all "out of limit" events should be performed as soon as the data  for a given
parameter or test is tabulated and verified for accuracy.
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Battelle Marine Sciences Laboratory
Marine Ecological Processes Group
Quality Assurance Management Plan
Volume 3
Section: 5
Revision:  1
Date:  January, 2000
Page 2 of 2
           TABLE 5.1 Summary of Test Deviations and Suggested Responses
Suggested Responses
Deviation
Lack of test array randomization
Testing was not blind
Required references or controls were not tested
Test chambers not identical
Test container(s) broken or misplaced
Test organism mortality in controls exceeds acceptable limits
Excessive test organism mortality in a single replicate of a control
Test organisms were not randomly assigned to test chambers
Test organisms were not from the same population
Test organisms were not all from the same species (or species
complex)
Test organism holding times were exceeded
Test organism sensitivity out of acceptable control chart range
Water quality parameters consistently out of range
Brief episodes of out-of-range water quality problems
Test monitoring was not documented
Test monitoring was incomplete
Sediment/testing water holding times were exceeded
Sediment/testing water storage conditions deviated from acceptable
ranges
Retesting
Required
S
S
S
S

S
S
S

S


S

S

V^(2)

Retesting May
Be Required
(1)




S



S

S
S

S

S

^(2)
0) If retest not completed, data may have to be qualified.
(2) Unless evidence is provided to show that sediment quality (geochemistry and contaminant
levels) has not been affected
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Battelle Marine Sciences Laboratory                                                Section:  6
Marine Ecological Processes Group                                                Revision: 1
Quality Assurance Management Plan                                               Date:  January, 2000
Volume 3                                                                     Page  1 of 1
                                   6.0  DATA REPORTING
All reported data will be validated in accordance with Volume 1, Section 10 of this QAMP. Reduced or
summarized data from the toxicity tests will be reported to the client. The following is a list of data that is
typically reported.
    description of test sediment or water; it's handling, manipulation, storage, and disposal
    description of test organisms; scientific name, age, size (when applicable), life stage, source, and
       their handling, culturing, and acclimation
       toxicity test method used
    date and time test started and terminated
    percent survival for each  test treatment
    control treatment survival
    results of water quality measurements (may be reported as mean, range of measurements, number
       of times criteria limits were exceeded)
    number of organisms used per test chamber
    number of replicate test chambers per treatment
    summary of statistical endpoints (mortality, growth, LC50, no observed effect concentration [NOEC],)
    gender determinations (when appropriate)
    growth (when appropriate)
    reproduction (when appropriate)
    summaries of biological observations
    summaries of reference toxicant evaluations
    summary of any problems encountered and corrective actions
    description of any deviations from  prescribed laboratory protocols
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Battelle Marine Sciences Laboratory
Marine Ecological Processes Group
Quality Assurance Management Plan
Volume 3
                                              Appendix A
                                                     Revision: 1
                                                     Date: March, 2000
                                                     Page 1 of 2
                                     7.0 REFERENCES
 ASTM 1367-92
 ASTM E-724-94
 ASTM E-1563-95
 EPA 503/8-91/001
 EPA 600/4-87/028
 EPA 600/4-90/027F
 EPA 600/4-91/003
 EPA 600/R-95/136
 PSEP 1995
1992 - Standard Guide for Conducting 10-Day Static Sediment Toxicity Tests
with Marine and Estuarine Amphipods. American Society for Testing and
Materials, Philadelphia, Pennsylvania.

1994 - Conducting Static Acute Toxicity Tests Starting with Embryos of Four
Species of Saltwater Bivalve Mollusks. American Society for Testing and
Materials, Philadelphia, Pennsylvania.

1995 - Conducting Static Acute Toxicity Tests with Echinoid Embryos.
American Society for Testing and Materials, Philadelphia, Pennsylvania.

Evaluation for Dredged Material Proposed for Ocean Disposal - Testing
Manual. U.S. Environmental Protection Agency (EPA) and U.S. Army Corps
of Engineers. U.S. EPA, Office of Water,  Washington D.C.

Short-Term Methods for Estimating the Chronic Toxicity of Effluents and
Receiving Waters to Marine and Estuarine Organisms.  May 1988. U.S. EPA.
Office of Research and Development, Cincinnati, Ohio.

Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters
to Freshwater and Marine Organisms. Fourth Edition. September 1991. U.S.
EPA. Office of Research and Development, Washington, D.C.

Short-Tern Methods for Estimating The Chronic Toxicity of Effluents and
Receiving Water to Marine and Estuarine  Organisms. Second Edition.  July
1994. U.S. EPA. Office of Research and Development, Washington,  D.C.

Short-Term Methods for Estimating the Chronic Toxicity of Effluents and
Receiving Waters to West Coast Marine and Estuarine Organisms. August
1995. U.S. EPA. Office of Research and Development, Washington DC.

Puget Sound Estuary Program (PSEP). 1995. Recommended Guidelines for
Conducting Laboratory Bioassays on Puget Sound Sediment. Prepared for
the U.S. EPA, Region 10, Seattle, WA..
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Battelle Marine Sciences Laboratory
Marine Ecological Processes Group
Quality Assurance Management Plan
Volume 3
Appendix A
       Revision: 1
       Date: March, 2000
       Page 1 of 2
                                        APPENDIX A
                    MARINE ECOLOGICAL PROCESSES EQUIPMENT LIST

The following is a list of the major pieces of equipment in the MSL bioassay wet laboratory. This list is
intended to demonstrate the types of equipment available and will be revised when the QAMP is revised,
but not each time equipment or instruments are added or deleted.
Water Quality Measures
Ammonia


Combined Measures
DO, pH, T, salinity

Individual Measures
T








Salinitiy


DO Meter


pH Meter


Other Equipment
Light Intensity

Microscopes



Centrifuge


Orion 900A ph Meter
Orion 900A ph Meter
Various ammonia probes

YSI Meter Environmental
Monitoring System 610-DM/ Data
Logger
Sonde 600 probe

NIST-traceable thermometer
Fluke 52 K/J thermometer
Fluke 52 K/J thermometer
Fluke 52 K/J thermometer
Fluke 52 K/J thermometer
Fluke 52 K/J thermometer
Fluke 52 K/J thermometer
Fluke 52 K/J thermometer

Reichert Refractometer


YSI Model 57
YSI Model 57

Orion SA250
Orion SA250
Orion SA250

Licor 185-A
Extech Instruments Light Meter
407026
Leica Wild M3Z
Wild Heerbrugg 28003
Nikon Labophot

Bock Extractor


SN 039388
SN 039548


312188R
SN 991 10867

A-09618
4986664
4655092
480056
5000160
5425282
5305158
5025363

10212-8
10392-8

37222
15679(TBT)

7335
7428
6478


E002938
Z-050-262
28003
100476-89

9183-P

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Battelle Marine Sciences Laboratory
Marine Ecological Processes Group
Quality Assurance Management Plan
Volume 3
Appendix A
        Revision:  1
        Date: March, 2000
        Page 1 of 2
Weight/Balances
AND FX3000
AND FX3200
ANDER120A
Mettler PE3600
Mettler P2010
Mettler AE163
Ohaus DS4
Ohaus DS4


5213125
5314791
3502726
D07416
633034
QC03126
60919
77927


0-3000 g
0-3000 g
0-100 g
0-3000 g
0-2000 g
0-150 g
0-20 g
0-20 g

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                                  Attachment 6
SERF Comprehensive QA Plan (Analytical and Mercury Laboratories)
-------
COMPREHENSIVE QUALITY ASSURANCE PLAN
              Prepared by and for:

     Southeast Environmental Research Program
          Florida International University
                Miami, Florida
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                                                                                         Section 1
                                                                                    Date: 11/25/98
                                                                                       Page 1 of 1
                        COMPREHENSIVE QUALITY ASSURANCE PLAN

                                        Prepared by and for:

                              Southeast Environmental Research Program
                                   Florida International University
                                             OE148
                                          University Park
                                       Miami, Florida 33199
                                          (305) 348-3095
                                       FAX: (305) 348-4096
Ronald D. Jones, Ph.D.                                      Date
SERF Director and Professor
Doraida Diaz                                         Date
SERF Quality Assurance Officer
Laboratory Certification Program                        Date
Department of Health
                                               1- 1
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TABLE OF CONTENTS

Section       Title

1.0           Title Page

2.0           Table of Contents

3.0           Statement of Policy

4.0           Organization and Responsibility
              4.1    Capabilities
              4.2    Key Personnel

5.0           Quality Assurance Obj ectives (Preci si on, Accuracy,
              and Method Detection Limits)

6.0           Sampling Procedures
21
                                                                                             Section 2
                                                                                        Date: 11/25/98
                                                                                           Page 1 of 5
Date

11/25/98

11/25/98

11/25/98

11/25/98



11/25/98


11/25/98
              6.1    Sampling Capabilities
              6.2    Sampling Equipment and Cleaning Procedures
                    6.2.1   Sampling Equipment
                    6.2.2   Sampling Equipment Laboratory Cleaning Procedures
                    6.2.3   Sampling Equipment Field Cleaning Procedures
              6.3    Sample Containers and Cleaning Procedures
                    6.3.1   Sample Containers
                    6.3.2   Sample Container Cleaning
              6.4    Sampling Protocols
                    6.4.1   Surface Water Sample Collection
                    6.4.2   Field Measurements
                    6.4.3   Pore Water Sample Collection
                    6.4.4   Soil and Sediment Sample Collection
                    6.4.5   Tissue Sample Collection
              6.5    Sample Documentation and Identification
              6.6    Documentation
              6.7    Sample Preservation, Holding Times and Sample Volume
              6.8    Sample Dispatch
              6.9    Reagent Storage and Waste Disposal
                    6.9.1   Reagent Storage
                    6.9.2   Waste Disposal
                                                 2- 1
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                                                                                                 Section 2
                                                                                           Date: 11/25/98
                                                                                               Page 2 of 5
Section       Title                                                           Pages         Date
7.0           Sample Custody                                                21            11/25/98
              7.1    Field Custody
              7.2    Laboratory Custody
              7.3    Electronic Data Records

8.0           Analytical Procedures                                           5             11/25/98
              8.1    Laboratory Method Modifications
                     8.1.1   Autoanalyzer Methods
                     8.1.2   Total Nitrogen in Water S ampl es
                     8.1.3   Alkaline Phosphatase Activity
                     8.1.4   Total Phosphorus
                     8.1.5   Silica
                     8.1.6   Chlorophyll a
       8.2    Laboratory Operations
                     8.2.1   Laboratory Glassware Cleaning
                     8.2.2   Reagent and Chemical Storage
                     8.2.3   Waste Disposal

9.0           Calibration Procedures and Frequency                            17            11/25/98
              9.1    Instrument Lists
              9.2    Standard Receipt and Traceability
              9.3    Standard Sources and Preparation
              9.4    Instrument Calibration
                     9.4.1   Field Instruments
                            9.4.1.1 Salinity/Conductivity/Temperature
                            9.4.1.2  pH
                            9.4.1.3 Dissolved Oxygen
                            9.4.1.4 Turbidity Meter Calibration
                            9.4.1.5 Light Meter Calibration
                            9.4.1.6 CTD Calibration
                     9.4.2   Laboratory Instruments
                                9.4.2.1  Alpkem Rapid Flow Autoanalyzer
                                9.4.2.2  Total Organic Carbon Analyzer
                                9.4.2.3  Total Nitrogen Analyzer
                                9.4.2.4  Fluorometer
                                9.4.2.5  Carlo Elba
                                9.4.2.6  Balances
                                9.4.2.7  Pipettes
                                                   2-2
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Section
Title
                   Section 2
              Date: 11/25/98
                 Page 3 of 5


              Date
10.0
11.0
Preventive Maintenance
10.1   Routine Maintenance
10.2   Maintenance Documentation
10.3   Contingency Plans

Quality Control Checks and Routines to Assess
Precision Accuracy and Calculation of MDLs
11.1   Field QC Checks
11.2   Laboratory QC Checks
11.3   Routine Method Used to Assess Precision
       and Accuracy
11.4   Method Detection Limits
              11/25/98
                                                                                        11/25/98
12.0
13.0
Data Reduction, Validation, and Reporting
12.1   Data Reduction
12.2   Data Validation
12.3   Data Reporting
12.4   Data Storage

Corrective Action
              11/25/98
              11/25/98
14.0
15.0
Figure
No.
Performance and System Audits
14.1   Field Audits
14.2   Laboratory Audits
Quality Assurance Reports
Figure
Title
                                          LIST OF FIGURES
Page
No.
              11/25/98
              11/25/98
Date
4.1           SERF Organization Chart
7.1           Centralized Sample Receipt Log-in Form
7.2           Chain-of Custody/Sample Log-in Form
       11/25/98
7.3           Surface Water Field Data Sheet
7.4           Lysimeter Field Data Sheet
7.5           Soil/Sediment Field Data Sheet
       11/25/98
7.6           Tissue Field Data Sheet
       11/25/98
                                                             4-2
                                                             7-3
                                                             7-5
                                                             7-6
                                                                    7-4
                                                                    7-7
              11/25/98
              11/25/98
              11/25/98
              11/25/98
                                                 2-3
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                                                                                           Section 2
                                                                                      Date: 11/25/98
                                                                                         Page 4 of 5
7.7          Field Instrument Sheet                                        7-9           11/25/98
7.8          Sample Checklist                                             7-10         11/25/98
7.9          TOC-5000 Log Book                                         7-11         11/25/98
                                                2-4
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Figure        Figure
No.           Title

7.10          RF A Nutri ent Analyzer Log B ook
7.11          RFA Total Phosphorus Log Book
7.12          RFA Silica Log Book
7.13          Antek Nitrogen Analyzer
7.14          Fluorometer
7.15          Total Phosphorus Preparation Form
7.16          Total Nitrogen Preparation Form
7.17          Refrigerator/Freezer Temperature Log
7.18          Oven Temperature Log
       11/25/98
9.1           Standard and Reagent Logb ook
9.2           Balance Calibration Log
9.3           Pipette  calibration Log
9.4           Daily Pipette Calibration Instructions
12.1          Final Data Report
14.1          Field Audit Checklist
14.2          Laboratory Audit Checklist
                                          LIST OF TABLES

Table         Table
No.           Title

5.1           Quality Assurance Obj ectives
              Field Measurements
5.2           Sample Preparation Methods
5.3           Quality Assurance Obj ectives
              Laboratory Measurements
6.1           SERF Sampling Capabilities
6.2           Field Sampling Equipment
6.3           Field Equipment Checklist
6.4           Sample Containers, Sizes, Preservation
              Holding Times
6.5           Field Reagent Storage
8.1           Reagent and Chemical Storage
       11/25/98
9.1           Instrument List
9.2           Standard, Source, Preparation, and Storage
9.3           Field Instrument Calibration
9.4           Laboratory Instrument Calibration
10.1          Laboratory Equipment Preventive Maintenance
       11/25/98
Page
No.

7-12
7-13
7-14
7-15
7-16
7-17
7-18
7-20
Page
No.

5-2
6-21
9-2
9-5
9-8
9-10
       7-21
       8-5
     Section 2
Date: 11/25/98
   Page 5 of 5


Date

11/25/98
11/25/98
11/25/98
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9-4
9-15
9-16
9-17
12-4
14-2
14-4
1 1/25/98
1 1/25/98
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1 1/25/98
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Date
11/25/98
5-3
5-4
6-2
6-3
6-7
6-10
1 1/25/98
1 1/25/98
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1 1/25/98
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       10-2
                                                 2-5
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                                                                                            Section 2
                                                                                       Date: 11/25/98
                                                                                          Page 6 of 5
10.2          Field Equipment Preventive Maintenance                         10-3          11/25/98
11.1          Quality Control Checks                                              11 -2
       11/25/98
                                                2-6
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Table
No.
13.1
13.2
Table
Title
Correi
Correi
             Corrective Actions for the Laboratory
             Correction Actions for the Field
                                                            Page
                                                            No.

                                                            13-2
                                                            13-3
                  Section 2
             Date: 11/25/98
                Page 7 of 5


             Date

             11/25/98
             11/25/98
                                           APPENDICES
Appendix    Appendix Title
A
B
D
Method Validation for Micromolar Concentrations
of Total Nitrogen in Natural Waters

Results of QC Check Samples for Total Phosphorus
in Soils/Tissue.
Solorzano L. and J.H. Sharp. 1980. Determination of
Total Dissolved Phosphorus and Paniculate Phosphorus
in Natural Waters. 25(4). pp. 754-758.

The Effect of Frozen Storage of Open-Ocean Seawater
Samples

An Equivalency Study on the Preservation of Total
Organic Carbon Samples With and Without Acid
No. of
Pages
18
Date
4/25/94
16
11/01/94
                                                                                             11/16/95
            11/16/95
              SERF Standard Operating Procedures
                                                            46
           12/04/97
                                                2-7
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                                                                                 Section 3
                                                                            Date: 11/25/98
                                                                               Page 1 of 1
3.0    Statement of Policy
The  Southeast Environmental  Research Program (SERF) is made up  of university research
professors and their staff from Florida International University (FIU). FIU is one of the nine State
University System (SUS) universities and all SERF personnel are employees of the State of Florida.
 The goals of SERF are  to  advance scientific  research,  the understanding  of biogeochemical
processes, and to publish results in high  quality refereed scientific publications. Pertinent to these
goals, is the  need to collect accurate,  high quality,  and reproducible  data, which  can only be
obtained through strict internal  and external quality assurance practices.  SERF is committed to
follow sound quality assurance/quality control (QA/QC) practices for the purposes of producing
verifiable quality data.

The professors associated  with  SERF have been involved  in monitoring surface water quality in
Florida Bay, Biscayne Bay, the Everglades, other areas of South Florida,  and the world's oceans for
over 15  years. The data collected by SERF to date is considered to be of excellent quality, and has
been used by FDEP, South Florida Water Management District  (SFWMD), the National Park
Service, Department of Interior, Department of Justice, and the EPA.

Research  conducted by SERF is  mainly  focused  on water quality nutrients  (nitrogen  and
phosphorus),  which are important influences  to South  Florida's  ecosystem.   In support of
interpreting  the  nutrient data,  SERF also  measures other water  quality and  physiochemical
parameters such  as salinity, temperature,  turbidity and chlorophyll.  Nutrients commonly measured
by SERF typically occur in surface waters of South Florida at relatively low concentrations (parts
per billion).   Often the nutrients occur at concentrations below typical contract laboratory method
detection limits;  however, small changes in these surface  water nutrients can have  a significant
effect on the ecology of South  Florida.  As a university research  facility, SERF is committed to
obtaining the most  accurate measurements as well as obtaining the lowest possible method
detection limits for these nutrients.  To obtain low level detection and calibration, SERF has had to
modify  and optimize analytical  methods and equipment for detection of nutrients in freshwater,
brackish waters, and  seawater.   SERF has also had  to modify  equipment decontamination
procedures to ensure contamination-free sampling for low concentrations of nutrients.  Many of the
analytical and sampling methods employed by SERF have been included in scientific publications.

This Comprehensive Quality  Assurance  Plan (CompQAP) describes the sampling and analytical
methods used by SERF personnel to ensure the integrity and accuracy of field and laboratory data
collection and analysis.   The  CompQAP has been prepared in accordance with the  Florida
Department  of Environmental  Protection (FDEP) guidelines.   Project-specific objectives and
sampling protocols will be described in more detail in Quality Assurance Project Plans  (QAPPs).
                                           3- 1
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                                                                                  Section 4
                                                                             Date: 11/25/98
                                                                                Page 1 of 2
4.0    Organization and Responsibility

4.1    Capabilities

The research group at SERF conducts both field sampling and laboratory analysis.  SERF performs
field sampling of surface water, pore water (water in soils and sediments), soils, sediments, and
plant tissue.  Analyses performed in the laboratory include inorganic nutrients, organic nutrients,
and physical parameters of surface waters, ground waters, pore waters,  soils, sediments, and plant
tissue.  SERF is fully capable of analyzing nutrients in fresh water, brackish water and sea water.

4.2    Key Personnel

Dr. Ronald D. Jones is the director of the Southeast Environmental Research Program  (SERF) at
Florida International University (Figure  4-1).  As director, Dr. Jones supervises all laboratory and
field operations and personnel. He provides a final review of all data and documents produced.

Mr. Pete Lorenzo is the chief laboratory  chemist and the field operation manager.  In this role, he is
responsible  for the proper execution of the daily field and laboratory operations.  He provides
scheduling of field and laboratory personnel, and is responsible for the collection, custody, storage,
and analysis of all samples.

Ms. Pura Rodriguez de la Vega is the SERF Data manager. She is responsible for checking all the
data produced in the lab according with QC criteria and for the preparation of the final data reports.

Ms. Doraida Diaz  is the SERF  QA officer.   She is responsible  for preparing all QAPs,  and
overseeing that the field  and laboratory  operations are performed according to the QAPs.  She is
also responsible for a final check of all data produced with respect to  QC criteria, initiating and
conducting audits, and preparing QA reports.

Sample collection, analysis, and data entry is performed by technicians and graduate students at
SERF under the direction of Dr. Jones and Mr. Lorenzo.  They are trained in the proper procedures
for sample collection, preservation, transportation, and analysis.
                                           4- 1
-------
                                                                         Section 4
                                                                    Date: 11/25/98
                                                                       Page 2 of 2
                  Figure 4.1 SERF Organization Chart
                           Dr Ronald D. Jones
                                Director
            Field Operations
Laboratory Operations
    Pete Lorenzo
  Field Operation
    Manager
Technicians:
Jeff Absten
Sean Gilhooly
Bill Gilhooly
Braxton Davis
Sean O'Brian
Steve Parthemore
Cristina Covas
Pierre Sterling
Giselle Bansee
Todd Shipman
Frank Tarn
                              Doraida Diaz
                             QA/QC Officer
                            Pura Rodriguez de
                                la Vega
                             Data Manager
            Pete Lorenzo
            Chief Lab.
             Chemist
        Technicians:
        Jeff Absten
        Sean Gilhooly
        Bill Gilhooly
        Braxton Davis
        Sean O'Brian
        Steve Parthemore
        Cristina Covas
        Pierre Sterling
        Giselle Bansee
        Todd Shipman
        Frank Tarn
        Elaine Kotler
                                      4-2
-------
                                                                                 Section 5
                                                                            Date:  11/25/98
                                                                               Page 1 of 5
5.0    Quality Assurance Objectives (Precision, Accuracy, and
       Method Detection Limits)

All sampling  and analytical work is performed  to  obtain  accurate,  reproducible  data using
consistent standard curves and extremely low method detection limits.  The SERF laboratory is
equipped with state-of-the art analytical equipment.  All students and staff are trained on proper use
of the equipment and supervised during all phases of sample collection and analysis by Dr. Jones.
In general, the people responsible for sample collection are also performing the laboratory analysis
of the samples, thereby, maintaining control of all aspects of sample collection and analysis.

Parameters routinely measured in the field are listed on  Table 5.1  and include temperature,
salinity/conductivity,  dissolved oxygen, pH, and turbidity.  Matrices analyzed include surface
waters,  pore  waters, ground waters,  soils, sediments and plant  tissue.   Laboratory precision,
accuracy,  and method  detection limits  (MDLs)  for specific  parameters in each  matrix  are
summarized in Table 5.2. The listed precision, accuracy, and MDLs are determined using in-house,
historically generated data.

Analytical procedures performed by SERF are listed in Table 5.2.  In general, SERF follows
analytical procedures described in Methods for Chemical Analyses of Water and Wastes, EPA-
600/4-79-020, Revised March 1983 and in  Standard Methods for the Examination of Water and
Wastewater, 18th Edition, 1989.  For solid samples SERF follows the methods described in the
Annual Book of ASTM Standards,  Volume  4.08, Procedures for Handling and Chemical  Analysis
of Sediments and Water Samples, May 1981, EPA/CE-81-1 and Methods of Soil Analysis, Part 2-
Chemical and Microbiological Properties, Second Edition, American Society of Agronomy, Inc.
Soil Science Society of America, Inc., 1982.
                                           5- 1
-------
TABLE 5.1
Quality Assurance Objectives
Field Measurements
                                                                                  Section 5
                                                                            Date: 11/25/98
                                                                                Page 2 of 5
Method No.
EPA 170.1
SM 2520 (B)
EPA 120.1
EPA 360.1
EPA 150.1
EPA 180.1
Photosynthetically Active
Radiation (a)
Pressure Transducer,
Depth Sounder (b)
Matrix
Surface Water,
Pore Water
Surface Water,
Pore Water
Surface Water,
Pore Water
Surface Water,
Pore Water
Surface Water,
Pore Water
Surface Water,
Pore Water
Surface Water
Surface Water
Parameter
Temperature
Salinity
Conductivity
Dissolved Oxygen
pH
Turbidity
Light Attenuation Coefficient
Depth
EPA =        U.S. Environmental Protection Agency.  Methods for Chemical Analysis
              Water and Wastes, Revised March 1983.
SM =         Standard Methods for Examination of Water and Wastewater, 1989, 18th
              Edition.
ASTM=       Annual Book of ASTM Standards, Vol 11.01.

EPA/Corps  of Engineers,  Procedures for Handling and  Chemical  Analysis of Sediments and Water
Samples.  May 1981. EPA/CE-81-1 Page 3-52.

(a)     See Section 6 for method details.

(b)     Pressure transducer method is used on the SEA-BIRD CTD; depth sounder method is used when
       the CTD is not used.
                                           5-2
-------
TABLE 5.2
Sample Preparation Methods
                                                                             Section 5
                                                                        Date: 11/25/98
                                                                           Page 3 of 5
Sample Prep. Method
Number
ASTMD 463 8(7.4)
ASTMD 4638(9.2)
Description
Evaporation
Dry Ashing
Matrix
Water
Water, Soil,
Sediment, Tissue
Sample Prep, for
these Methods
EPA 365.1
EPA 365.1
Method References:

EPA Methods for Chemical Analysis of Water and Wastes, Revised March 1983.

Annual Book of ASTM Standards, Vol 11.01.

Solorzano L. and J.H. Sharp.  1980. Determination of Total dissolved Phosphorus and Particulate
Phosphorus in Natural Waters. Limnol. Oceanogr. 25(4), pp. 754-758. See Appendix B.
                                         5-3
-------
TABLE 5.3
Quality Assurance Objectives
Laboratory Measurements
                                                                                      Section 5
                                                                                 Date: 11/25/98
                                                                                    Page 4 of 5
Analyte
Ammonium-N
Nitrite - N
Nitrate - N
Soluble Reactive
Phosphate
Dissolved Silica
Total
Nitrogen
Total
Phosphorus
Total Organic
Carbon,
Dissolved
Organic Carbon
Chlorophyll a
Alkaline
Phosphatase
Activity
Bulk Density
Total Nitrogen
Total Carbon
Moisture Cont./ %
Solids
Ash Free Dry
Weight
Total Phosphorus
(m)
Matrix
SW,
GW,PW
SW,
GW,PW
SW,
GW,PW
SW,
GW,PW
SW, GW, PW
SW, GW, PW
SW,
GW,PW
SW, GW, PW
SW
SW
S, SED
S, SED, T
S, SED
S, SED
S, SED, T
Analytical
Method
EPA350.1(d)
EPA 353.2 (d)
EPA 353.2 (d)
EPA365.1(d)
EPA370.1(d)
(g)
EPA 365.1(e)
EPA415.1(h)
SM 10200H (i)
CD
ASTMD4531-86
MSA 29-2.2.5(1)
EPA/CE-81-1
SID, S3, 2
ASTMD22 16-80
ASTMD2974-87
EPA365.1(e)
Precision
(RPD) (a)
<20 %
<20 %
<20 %
<20 %
<20 %
<20 %
<20 %
<20 %
<20 %
<20 %
<20 %
<20 %
<20 %
<20 %
<20 %
Cone.
Range (b)
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
Accuracy
(%R) (a)
78-128
84-107
84-107
78-110
85-123
75-108
79-125
85-118
80-120
80-120
80-120
80-120
80-120
80-120
96-118
MDL (c)
(|imol/l,
unless noted)
0.06
0.05
0.02
0.02
0.05
0.05
0.02
0.04
0.07 (i)
2.1
0.01
0.01
10.00
NA
0.01
|jmol/l.hr -1
NA
NA
NA
1.7|jrnol/kg(k)
0.97 |jrnol/kg (k)
MDL (c)
(mg/1,
unless noted)
0.0008
0.0007
0.0003
0.0003
0.0007
0.0007
0.0006
0.0012
0.002 (f)
0.03
0.0003
0.0003
0.12
0.0001
NA
0.001 g/cc (k)
10mg/kg(l)
3 % (k)
0.02 mg/kg (k)
0.03 mg/kg (k)
                                             5-4
-------
                                                                                                             Section 5
                                                                                                       Date: 11/25/98
                                                                                                           Page 5 of 5
TABLE 5.3 Continued
Quality Assurance Objectives
Laboratory Measurements

(a)      QA targets for precision and accuracy determined from in-house, historical data.

(b)      Concentration Range: L = lower 20% of linear calibration or range.
                           M = from 20% to 80% of linear calibration range.
                           H = The upper 80% of linear calibration range.

(c)      Method Detection Limits (MDLs) determined by EPA procedure described in 40 CFR Part 136, Appendix B, revision  1.11.

(d)      Ammonium, nitrite, nitrate, soluble reactive phosphate, and silica of water samples are determined on an ALPKEM 305
        Rapid Flow Analyzer and ALPKEM 501 autosampler.

(e)      Total phosphorus of water and solid samples is determined on an ALPKEM 305 Rapid Flow Analyzer and ALPKEM
        501 autosampler using the automated method of EPA 365.1, with the samples prepared according to a modification of
        Solorzano and Sharp (1980; see Section 8.1.4 and Appendix B), instead of persulfate digestion.

(f)      Theoretical MDL for the method.  The actual MDL for silica for our laboratory has not yet been determined.

(g)      Total Nitrogen of water samples is determined using an ANTEK Instruments Model 7000N Total Nitrogen Analyzer.
        Method validation package included as Appendix A.

(h)      Total Organic Carbon of water samples is determined by high temperature catalytic combustion with a Shimadzu 5000
        Total Organic Carbon Analyzer with autosampler.

(i)      Chlorophyll a is determined using a modification of SM 10200H as outlined in Section 8.1.6.

(])      The  analytical method  for Alkaline Phosphatase  Activity is currently under experimental research.  This method is
        described in more detail in Section 8.

(k)      Values represent minimum reportable quantities.

(1)      Total nitrogen and total carbon of solid samples determined using a Carlo Erba Model  1500 N/C  analyzer. Minimum
        reportable quantity of 0.01 % based upon a sample size between 0.5-100 mg.

(m)     The results of quality control check samples are summarized in Appendix B.

SW-Surface Water; PW-Pore Water; GW-Ground Water; S-Soils; SED-Sediments; T-Tissue

Method References:

EPA Methods for Chemical Analysis of Water and Wastes, Revised March 1983.
EPA/Corps of Engineers, Procedures for Handling and Chemical Analysis of Sediments and Water Samples.  May 1981. EPA/CE-81-1.
Standard Methods for the examination of Water and Wastewater, 17th edition. 1989.
Annual Book of ASTM Standards, Method D4531-86, Volume 04.08, 1989.
Methods of Soil Analysis, Part 2-Chemical and Microbiological Properties, Second Edition, 1982.
                                                         5-5
-------
                                                                                 Section 6
                                                                            Date: 11/25/98
                                                                              Page 1 of 21
6.0    Sampling Procedures

6.1    Sampling Capabilities

SERF performs  sampling of surface water, pore water, soil and sediments, and plant tissue for
determination of the field and laboratory analytical parameters listed in Table 6.1.

6.2    Sampling Equipment and Cleaning Procedures

6.2.1   Sampling Equipment

Preceding a trip to the field, the personnel responsible for collection of the samples are required to
ensure that everything  is prepared for the expedition.  This entails making sure that all sample
containers are clean and properly labeled, and that all sampling and field measurement equipment
are properly cleaned, charged and functioning within acceptable limits.  Table 6.2 lists the field
sampling equipment used for sampling  each  matrix, while Table 6.3 is an equipment checklist
prepared for the sampling team.

In general, sampling equipment used is dictated by a  specific project.  Surface water sampling
equipment may include plastic sample containers, syringes, filter holders, and buckets.  Pore water
samples are collected from lysimeters using a peristaltic pump or a syringe equipped with tygon
tubing.  Soil  and  sediment  samples are collected  using plastic core tubes or by hand.  Tissue
samples are generally collected by  hand and stored in plastic, sealable bags.

6.2.2   Sampling Equipment Laboratory Cleaning Procedures

All reusable  field  sampling and measurement equipment  is  subjected to precleaning in the
laboratory prior to transportation to a field site according to the following procedures:

       a.      Wash all surfaces thoroughly with hot, tap water.  Use a brush to remove large or
              stubborn particles.
       b.      Rinse thoroughly with analyte free water (deionized water).
       c.      Let air dry completely, or  dry with Kimwipes.
       d.      Wrap equipment in plastic bags for storage and transportation.

Note, the above cleaning procedure does not include the use of soaps or acids as recommended by
DEP. The concentrations of the nutrients of interest (phosphate, ammonium and nitrate) can be
significantly affected by the use  of these  cleaning solutions.  The  cleaning procedures used by
SERF in the  last ten years have produced non-detectable concentrations of the analytes  listed in
Table 6.1 in equipment blanks, and historical data supporting this is available upon request.
                                           6- 1
-------
                                                                      Section 6
                                                                  Date: 11/25/98
                                                                    Page 2 of 21
TABLE 6.1
SERF Sampling Capabilities
Parameter Group
Inorganic Anions and Nutrients
Ammonium
Nitrite
Nitrate
Phosphate
Silica
Total Nitrogen
Total Phosphorus
Organics
Total Carbon
Dissolved Organic Carbon
Chlorophyll-a
Alkaline Phosphatase Activity
Field Parameters
Temperature
PH
Salinity/Conductivity
Dissolved Oxygen
Turbidity
Light Attenuation Coefficient
Other
Bulk Density
Percent Mineral Content
Ash Free Dry Weight
Sample Source
Surface Water, Pore Water
Surface Water, Pore Water,
Surface Water, Pore Water,
Soils, Sediments, Tissue
Soils, Sediments, Tissue

Surface Water, Pore Water,
Soils, Sediments, Tissue
Surface Water, Pore Water
Surface Water
Surface Water, Pore Water,
Soils, Sediments, Tissue
Surface Water, Pore Water
Surface Water
Soils, Sediments
                                     6-2
-------
                                                                                                    Section 6
                                                                                               Date: 11/25/98
                                                                                                 Page 3 of 21
TABLE 6.2
Field Sampling Equipment
Equipment
Surface Water
Sampling Equipment
Syringes
Bottles
Bottles
Microcentrifuge
Tubes
Bucket
Niskin Sampler
Field Filtration

In-line Filter Holders
Filters
Construction


140 ml plastic (HDPP)
60 ml plastic (HOPE)
125 ml plastic (HOPE)
1.8 ml plastic (HOPE)
2-5 gallon plastic
(LDPE)
2.5 L PVC

2.5 cm plastic
(Gelman)
2.5 cm Whatman GF/F
glass fiber
Use


Collection
Collection
Collection
Filter storage
Collection
Collection

Filtration
Filtration
Parameter Groups


Soluble nutrients,
Suspended matter
Chlorophyll
Soluble nutrients
Total nutrients, organics
Suspended matter,
Chlorophyll
All surface parameters
All surface parameters

Soluble nutrients,
Suspended matter,
Chlorophyll
Soluble nutrients,
Suspended matter,
Chlorophyll
Restrictions,
Precautions, Notes.


None
Filtered samples only, 2 per
location
2 per location
2 per location, preserve
with acetone
None
None

Attach to end of syringe
Use filter forceps to place
into and remove from filter
holder
                                                    6-3
-------
                                                                                                 Section 6
                                                                                            Date: 11/25/98
                                                                                              Page 4 of 21
TABLE 6.2 Continued.
Field Sampling Equipment
Equipment
Pore Water
Sampling
Equipment
Peristaltic Pump
In-line Filter
Syringe
Soils, Sediments
Spade, Spatula
Core Tubes
Wildco Eggshell Core
OO
Eckman Dredge
Plant Tissue
Bags
Construction

Tygon Tubing
Plastic, 2.5 cm Whatman
GF/F glass filter
120 ml plastic (HDPP)
with Tygon Tubing

Stainless Steel
Polycarbonate or PVC
Stainless Steel
Stainless Steel

Plastic
Use

Purging, Sampling
Filtration
Purging, Sampling

Sample collection,
cutting
Sample collection
Corer
Penetration

Sample collection
Parameter Groups

All parameters
Soluble nutrients
All parameters

All parameters
All parameters
All parameters
All parameters

All parameters
Restrictions,
Precautions, Notes.

Use new tubing prior to each
sampling event.
None
Use new tubing prior to each
sampling event.

None
None
None
None

None
                                                  6-4
-------
                                                                                                     Section 6
                                                                                                Date: 11/25/98
                                                                                                  Page 5 of 21
TABLE 6.2 Continued.
Field Sampling Equipment
Equipment
Miscellaneous
Equipment
Acetone
Disposable pipettes
Ice (wet)
Coolers
DI water
Field notebook
Pens
Labeling tape
Site charts
Construction

90%, ACS grade
Plastic (polyethylene)

Plastic
1 L plastic (LDPE)
250 ml plastic (LDPE)
squeeze bottle
Field data sheets
Instrument calibration
sheets
Field equipment
checklist
Waterproof
Waterproof
Waterproof
Use

Preservation
Dispensing
Preservation
Transportation
Equipment blanks
Rinsing
Documentation
Documentation
Documentation
Reference
Parameter Groups

Chlorophyll
Chlorophyll
Soluble nutrients
Chlorophyll
Tissue samples
All parameters
All parameters
All parameters
All parameters
All parameters
All parameters
Restrictions,
Precautions, Notes.

Store in a 25 Oml HOPE
bottle in a ziploc bag
None
Need sufficient quantity to
ensure even temperature
distribution
None
None
None
None
None
None
                                                    6-5
-------
TABLE 6.2 Continued.
Field Sampling Equipment
                                                                                                    Section 6
                                                                                                Date: 11/25/98
                                                                                                  Page 6 of 21
Equipment
Miscellaneous
Equipment
Field instruments
pH buffers
S/C check standard
Construction

DO meter
SCT meter
pH meter
CTD
7.00 and 10.00 pH
solutions
Gulfstream seawater
Use

Field measurements
Meter calibration
Calibration check
Parameter Groups

All parameters
All parameters
All parameters
Restrictions,
Precautions, Notes.

None
None
None
                                                    6-6
-------
                                                                               Section 6
                                                                         Date: 11/25/98
                                                                            Page 7 of 21
TABLE 6.3
Field Equipment Checklist
Surface Water Sampling Equipment
1.      Labeled and cleaned sample bottles (narrow-mouth plastic)
              60 ml (2 per site)
              125 ml (2 per site)
2.      140 ml clean plastic syringes
3.      Mi crocentrifuge tub es
4.      2.5 cm in-line filter holders
5.      2.5 cm Whatman GF/F glass fiber filters
6.      Filter forceps
7.      2-5 gallon plastic bucket
8.      Niskin sampler

Pore Water Sampling Equipment
1.      Peristaltic pump or 120 ml plastic syringes
2.      Tygon tubing
3.      Water level indicator

Field Measurement Equipment
1.      pH meter
2.      S/C/T meter
3.      Dissolved oxygen meter
4.      CTD
5.      Light meter
6.      pH Buffers (7.00 and 10.00)
7.      Salinity/Conductivity check standard
8.      Plastic beaker

Sample Preservation
1.      100% Acetone
2.      Disposable polyethylene pipettes
3.      Ice
4.      Coolers
5.      DI water (1L) for equipment blanks

Soil, Sediment & Sampling Equipment
1.      Labeled sampling bottles
2.      Spatula
3.      Spade
4.      Measuring rule
5.      Core tubes
                                         6-7
-------
                                                                             Section 6
                                                                        Date: 11/25/98
                                                                          Page 8 of 21
TABLE 6.3 Continued
Field Equipment Checklist

Tissue Sampling Equipment

1.     Labeled sample bags
Boat Supplies

1.     Depth finder
2.     GPS (Magellan 5000 D)
3.     VHP Radio
4.     PFD's (adequate for number for passengers)
5.     Boat hook
6.     Emergency flares
7.     Charts
8.     Tool box
9.     Fire extinguisher

Miscellaneous Equipment

1.     Clipboard with waterproof field data and calibration sheets
2.     Pencils
3.     Waterproof label tape and waterproof pens
4.     Deionized water squeeze bottle (filled)
5.     Watch
6.     CompQAP (available in the field for reference)
                                         6-8
-------
                                                                                  Section 6
                                                                            Date: 11/25/98
                                                                               Page 9 of 21

Two types of analyte-free water  are produced in the laboratory:  deionized-distilled water and
double-deionized water.  In general, the deionized-distilled water is used for washing equipment
and glassware, while the double-deionized water is used as reagent water.  Tap water is  first
deionized using a Culligan system containing activated carbon and 2-mixed bed ion exchange beds
followed by filtering through a 0.45 |om polypropylene filter cartridge.  The water is then either
distilled through a Corning Mega-Pure 11 Liter Automatic Water Still to produce the deionized-
distilled water or  further deionized  with a Barnsted model D8911  HN Ultrapure mixed  bed
deionization cartridge to produce the double-deionized water. Both types of water have proven to
be analyte-free for the nutrients analyzed.  The quality of this water is frequently checked with
laboratory method and field equipment blanks.  Containers used to store analyte-free water are kept
dedicated to this use, therefore, cleaning of these containers is not necessary.

6.2.3   Sampling Equipment Field Cleaning Procedures

In the field, all field equipment used for  collection of surface and  pore water sampling is triple-
rinsed with sample water prior to sample collection or field  measurement.  New tygon tubing is
replaced  on the peristaltic pump or syringe at the beginning  of each pore water sampling event.
Between sampling locations,  the tygon tubing is rinsed  with analyte-free water.  Reusable field
equipment used to collect soil and sediment equipment is cleaned between sampling locations by
rinsing with analyte-free water. If the sampling equipment is used only once in the field, and not
cleaned in the field, the equipment is tagged with the sample location and cleaned according to the
laboratory cleaning procedures described in Section 6.2.1.   The  probes of field instruments are
wiped if necessary to remove large particles, rinsed with DIW, and allowed to air dry for as long as
possible before using at the next station.  The cleaning  procedures for all field  equipment used
during a  sampling  event are documented in the field notebook and  include which equipment was
cleaned, the procedure used, and the date and initials of the person  performing the procedure.

If samples containing high concentrations are suspected of being collected during an event (such as
surface waters downgradient of a landfill), then the sampling program will be performed to collect
samples from lowest suspected concentration to highest suspected concentration.  Any equipment
suspected of contamination from these sampling events, will by thoroughly cleaned; any equipment
that can not be cleaned is discarded.
                                           6-9
-------
TABLE 6.4
Sample Containers, Sizes, Preservations and Holding Times
                                                                                                              Section 6
                                                                                                         Date: 11/25/98
                                                                                                          Page 10 of 21
Sample
Type/Parameter
Water Samples
Ammonia
Nitrite
Nitrate
Soluble Reactive Phosphate
Silica
Total Nitrogen
Total Phosphorus
Total Organic Carbon,
Dissolved Organic Carbon
Chlorophyll-a
Alkaline Phosphatase
Activity
Container/Size

Plastic, 60 ml
Plastic, 60 ml
Plastic, 60 ml
Plastic, 60 ml
Plastic, 125 ml
Plastic, 125 ml
Plastic, 125 ml
Plastic, 125 ml
Plastic, 60 ml
GF/F Glass Fiber filter, 1.8 ml
HDPE Microcentrifuge Tube
Plastic, 125 ml
Preservative

Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
Acetone, Freeze, -15°C,
Store in the Dark
Store in the Dark
SERF Holding Time

24 hours
24 hours
24 hours
24 hours
28 days
28 days
28 days
7 days
7 days
12 hours
Maximum Allowable
Holding Time (a)

28 days (b)
28 days (b)
28 days (b)
28 days (b)
28 days
28 days
28 days
28 days
21 days
N/A (c)
                                                        6- 10
-------
TABLE 6.4  Continued
Sample Containers, Sizes, Preservations and Holding Times
(a)     According to U.S. EPA, 1983, methods for chemical analyses of Water and Wastes.
(b)     If SERF maximum holding times are exceeded for these parameters, then samples are frozen and analyzed within the maximum allowable holding time.
(c)     Not Applicable.
                                                                                                                                       Section 6
                                                                                                                                 Date: 11/25/98
                                                                                                                                  Page 11 of 21
Sample Type/Parameter
Turbidity
pH
Temperature
Salinity/
Conductivity
Dissolved Oxygen
Light Attenuation
Coefficient
Soils Sediments
All Parameters
Tissue
All Parameters
Container Size
Plastic, 125 ml
None
None
None
None
None
Plastic core tubes, plastic wide-
mouth specimen cups
Plastic Bags
Preservative
Cool, 4°C
None
None
None
None
None
Cool, 4°C, dark
Dry, grind, and store in
desiccator
Freeze, -15°C, dark
Freeze, -15°C, dark
SERP Holding Time
12 Hours
Analyze Immediately
Analyze Immediately
Analyze Immediately
Analyze Immediately
Analyze Immediately
48 hours
48 days
48 days
lYear
Maximum Allowable
Holding Time (a)
48 hours
Analyze Immediately
Analyze Immediately
28 days
Analyze Immediately
Analyze Immediately
48 hours
Indefinitely
Indefinitely
N/A (c)
                                                                     6- 11
-------
                                                                                  Section 6
                                                                            Date: 11/25/98
                                                                             Page 12 of 21
6.3    Sample Containers and Cleaning Procedures

6.3.1   Sample Containers

Sample containers, preservation methods, and appropriate holding times are listed in Table 6.4.
Three types of sample containers are used for surface water nutrient sampling: 60 ml HDPE screw-
cap bottles for filtered water samples; 125 ml HDPE screw-cap bottles for unfiltered water samples;
and Whatman GF/F glass fiber filters, stored in 1.8  ml microcentrifuge polypropylene tubes with
caps for suspended matter samples. Sample containers used for pore water samples are the same as
those used for surface water samples except that chlorophyll-a is not collected.  Soil and sediment
samples are collected in plastic core tubes or wide-mouth plastic specimen cups.   Plant tissue
samples are stored in plastic, sealable bags.

6.3.2   Sample Container Cleaning

Similar to the field equipment cleaning protocols, no soaps or acids are used in cleaning of sample
containers, since  we have found  these cleaning  solutions have the potential to  contaminate the
sample containers for the nutrients listed in Table 6.1.  All surface water and pore water sample
bottles are further cleaned in the field by triple  rinsing with  sample water.  Each  surface water
sample is collected in duplicate in the field, providing for a quality assurance check of possible
container contamination.  Any sample container suspected of being contaminated is discarded. The
equipment blank results are documented with the  corresponding sample set runs so it is possible to
track potential  bottle  contamination. The  water  sample bottles can be  re-used  after the proper
cleaning procedure during 2 years (after they were used for the first time) for sampling purposes
and after this period of time they are discarded independently from how many times they were used.

6.3.2.1 Surface Water  and  Pore Water  Sample  Containers  for  Filtered
              Nutrient Analyses

HDPE sample bottles  used for collection of filtered nutrient analyses are cleaned by the following
methods:

       a.      Remove all labels,  and wash all surfaces thoroughly with hot, tap water. Use a brush
              to  remove large or stubborn particles.
       b.      Rinse thoroughly (at least three times) with analyte-free water.
       c.      Rinse once with acetone to aid in drying,  and to remove organics.
       d.      Shake dry then cap.
       e.      Store sample containers in plastic bags for transportation to the field.
       f      In  the field, triple rinse with sample water prior to sample collection.

6.3.2.2 Surface Water  and Pore  Water  Sample Containers  for Unfiltered
              Nutrient Analyses

Sample bottles used for collection of non-filtered samples are cleaned following the procedures
described in Section 6.3.2.1, except they are not rinsed with acetone, and they are allowed to air dry.

                                          6-  12
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6.3.2.3 Surface Water Sample Containers for Suspended Matter (Chlorophyll
              Analyses)

Both the Whatman GF/F glass fiber filters and the 1.8 ml tubes used for storage of suspended
matter sediments are obtained clean directly from the manufacturer, used once, then discarded.

6.3.2.4 Soil and Sediment Sample Containers

The polycarbonate or PVC core tubes and specimen cups used for soil and sediment collection are
washed according to the following procedures:

       a.      Remove all labels, and wash all surfaces thoroughly with hot, tap
              water. Use a brush to remove large or stubborn particles.
       b.      Rinse thoroughly (at least three times) with analyte-free water.
       c.      Allow to air dry.

6.3.2.5 Tissue Sample Containers

The plastic bags used to store tissue samples are used once, then discarded.

6.4    Sampling Protocols

Specific sampling locations are  chosen based on criteria described in  the  appropriate Quality
Assurance Project Plans. In general, surface water, sediment, and plant tissue samples are collected
from a boat, helicopter, airboat or by a SCUBA diver. To ensure collection of undisturbed samples,
the boat is advanced toward a sampling  station from  the downstream direction.   Surface water
samples are collected as grab samples from the bow of the boat, away from the outboard engine.
Sediment and tissue samples are collected by SCUBA diver or by wading upgradient of the anchor,
if one is used, or upgradient of the bow if an  anchor  is not used.  If surface water samples and
sediment and/or tissue samples are to be collected at one location, then the surface water samples
will be collected prior to the collection of sediment or  tissue samples.  In  areas of suspected high
concentrations, such as downgradient of a landfill,  samples are collected in order of suspected low
concentration to higher concentration.

6.4.1   Surface Water Sample Collection

SERF generally collects three types of surface water samples are collected:  suspended  matter
samples, filtered, and unfiltered, samples in that order. Each of these types of samples are collected
in duplicate by collecting from successively collected volumes.  The quantity of each subsample
collected is recorded in the field  notebook.  Surface water samples  are collected according to the
following procedures:

I.      Suspended Matter Samples for Chlorophyll Analysis
       a.      Use clean 140 ml polypropylene  syringes to collect suspended matter
              samples.
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                                                                                   Section 6
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                                                                              Page 14 of 21
       b.      Place the syringes to draw water  10 cm below the surface of the water into the
              direction of water flow (if applicable).
       c.      Partially fill the syringe and rinse with sample water three times.
       d.      Completely fill the syringe.
       e.      Using filter forceps, put a 25 mm Whatman GF/F glass fiber filter into a 25 mm in-
              line filter holder.
       f.      Attach the filter holder to the end of the syringe.
       g.      Force a known amount of sample water (50 - 200 ml) through the filter (Do not
              rinse the filter first). Discard Filtrate.
       h.      Record the amount of water filtered in the field notebook, along with date and time
              of sample collection.
       i.      Transfer the filter, with the filter forceps, to a 1.8 ml microcentrifuge tube.
       j.      Add 1.5 ml of acetone to the tube with a disposable polyethylene pipet.   Acetone
              extracts the chlorophyll from the cells collected on the filter.
       k.      Check that tube is properly labeled.
       1.      Place the tube immediately in the cooler on ice and in the dark.

n.     Filtered surface water samples for inorganic nutrient determinations
       a.      Use clean 140 ml polypropylene syringes to collect filtered surface water samples.
       b.      Place the syringes to draw water  10 cm below the surface of the water into the
              direction of water flow (if applicable).
       c.      Partially fill the syringe and rinse with sample water three times.
       d.      Completely fill the syringe.
       e.      Using filter forceps, put a 25 mm Whatman GF/F glass fiber filter into a 25 mm in-
              line filter holder.
       f.      Attach the filter holder to the end  of the syringe and force about 10 ml of sample
              through the filter to rinse.
       g.      Use the remaining filtrate from syringe to rinse a 60 ml HOPE sample bottle three
              times.
       h.      Fill syringe with sample water again (if necessary),  and re-attach filter holder with
              filter.
       i.      Fill sample bottle to neck and cap. Multiple syringe volumes may contribute to a
              single sample bottle.
       j.      Repeat steps a through h to collect a duplicate sample.
       k.      Check that the sample bottles are properly labeled.
       1.      Record date and time of sample collection in the field notebook.
       m.     Place the samples in a cooler with ice.

HI.     Unfiltered surface water samples for total nitrogen, phosphorus, and carbon  and alkaline
       phosphatase activity determinations:
       a.      Unfiltered  surface water samples are collected directly into clean 125 ml HOPE
              bottles.
       b.      Submerge the bottles neck first to about 10 cm below the surface of
              the water.
       c.      Invert the bottle with neck upright and pointing into the direction of water flow (if
              applicable).
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       d.      Partially fill the bottle (at least 25 percent filled) cap, and shake, and pour the rinse
              water downstream of the sampling location.
       e.      Repeat this procedure two more times for a total of three rinses.
       f.      Fill the bottle to the neck and cap.
       g.      Repeat procedures a through/to collect a duplicate sample.
       h.      Check that the sampl e b ottl es are properly 1 ab el ed.
       i.      Record date and time of sample collection in the field notebook.
       j.      Place the  samples in a  cooler in the dark.  Alkaline phosphatase
              activity is  a microbiological parameter, therefore,  these samples can
              not be  stored on ice.  Once alkaline phosphatase activity has  been
              determined on the samples, the  remaining sample for the inorganic
              parameters are stored in a refrigerator.

When access to the surface water can not be made by boat or wading,  such as from a bridge or side
of canal, then a clean plastic bucket attached to  a line is used to collect the surface water sample in
bulk.  This bucket is rinsed with sample water three times, with the rinse water poured downstream
of the sampling location, prior to collection of the sample.  Sample bottles, syringes, and filters are
then rinsed and filled  from the water collected in the bucket following the procedures described
above.  If necessary, split samples are collected from consecutive sample volumes from the same
sample device.

When water samples are to be collected from depths below the water surface, a Niskin sampler is
used. The sampler is cocked open,  then lowered from the boat to the appropriate depth, closed at
depth, and returned  to the surface.  Sample bottles, syringes, and filters are then rinsed and filled
from the  water collected in the bucket following the procedures described above.   For good
comparability between duplicate samples and all parameters, it is important to fill all sample bottles
for a location from one cast of the Niskin sampler.  If for some reason all of the bottles cannot be
filled from one cast, as may happen if the Niskin sampler does not fill completely or that some of
the sample water is lost due to spillage, then any sample already put into bottles needs to be rinsed
and filled again with water collected from a new cast of the Niskin sampler.

6.4.2   Field Measurements

Temperature, salinity/conductivity, pH,  dissolved  oxygen,  and  light attenuation coefficient are
measured  directly in the field  at each sampling location using properly calibrated (Section 9)
portable electronic meters and/or a SEA-BIRD Model 19-03 CTD.  These measurements are taken
contemporaneously with the sample collection to ensure direct correlation of laboratory results with
field measurements. Temperature, salinity/conductivity and dissolved oxygen are measured both at
the surface and at the bottom of the water column; pH is measured at the surface.

The water depth is determined from a depth finder on the boat and/or the pressure transducer on the
SEA-BIRD CTD.  Meter probes are attached 10 cm from the bottom of the weighted line to obtain
bottom water measurements.

6.4.2.1. Temperature

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                                                                                Section 6
                                                                           Date: 11/25/98
                                                                            Page 16 of 21
Surface   temperature   is   measured   (in   °C)   by   submersing   the   probe   of   the
salinity/conductivity/temperature (SCT) meter  10 cm under water.   After the digital  readout
stabilizes (less than 5 minutes), the temperature is recorded in the field notebook. The probe is then
lowered to 10 cm from the bottom of the water column. After the digital readout stabilizes, the
bottom temperature is recorded in the field notebook.  Temperature can also be measured by the
thermistor on the SEA-BIRD CTD.

6.4.2.2. Salinity/Conductivity

Surface salinity and conductivity are measured  in units of parts per thousand (ppt).  Surface and
bottom salinity are measured contemporaneously with temperature. The probe of the SCT meter is
submersed 10 cm under water. After the digital readout stabilizes (less than 5 minutes), the surface
salinity is recorded in the field notebook.  The probe is then lowered to 10 cm from the bottom of
the water column. After readout stabilization, the bottom salinity is recorded in the field notebook.
 Salinity and conductivity can also be measured by the SEA-BIRD CTD.

6.4.2.3. pH

An automatic temperature compensation (ATC) probe on the pH meter adjusts the pH reading for
temperature differences between standards and samples. A sample of surface water is collected in a
clean, 400 ml polyethylene beaker after it is rinsed three times with sample water. The pH probe
and ATC probe are submersed in the beaker,  and the pH is recorded in the field  notebook.
Successive aliquots  of surface water are collected until the pH of three successive aliquot agrees
within 0.02 pH units.

6.4.2.4. Dissolved Oxygen

Automatic temperature, atmospheric pressure and salinity corrections are made by the Orion model
840 Dissolved Oxygen meter.  Switch the salinity compensation on, and use the Mode Key Pad to
select the Cal mode. The last salinity entered in the system is displayed. Adjust the salinity display
with the up and down arrow keys to match the previously-measured  station salinity.   Dissolved
oxygen (DO) concentration, in mg/1, is determined from the surface water by submersing the probe
10 cm.  The probe is gently agitated to approximate a velocity of 15 cm/sec past the membrane.
After a brief equilibration time, the meter displays a  stable DO reading.  Once the surface DO is
recorded in the field notebook, the probe is then lowered to 10 cm from the  bottom and gently
agitated to approximate a flow of 15 cm/sec past the membrane. After a stable reading is reached,
the DO of the bottom water is recorded in the field notebook.  Dissolved oxygen can also be
measured by the dissolved oxygen sensor (SB23B) on the SEA-BIRD CTD.

6.4.2.5 Light Attenuation Coefficient

Light attenuation coefficient is a measurement of the attenuation  of photosynthetically active
radiation (PAR) as measured by two spherical quantum light sensors (LI-COR model LI-193SA) at
different depths in the water. The two light sensors are mounted on two extensions, each 90° apart,
from a PVC pole, such that one probe is held just below the water surface, while the other is 0.5 or
1 m below (depending on water depth). The measurements are made and the ratio of light at depth
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                                                                                Section 6
                                                                           Date: 11/25/98
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(lz)/ light near surface (10) is calculated by a LI-COR model LI-1000 DataLogger. After a stable
reading is reached, the ratio value and distance (z, 0.5 or 1 m) are recorded in the field notebook.
The light attenuation coefficient is then calculated as In(lz/l0)/z*-l.  Light attenuation coefficient can
also be calculated by PAR measured by quantum light sensor on the SEA-BIRD CTD.

6.4.3  Pore Water Sample Collection

SERF collects pore  water from  either  temporary or permanently placed  lysimeters.  Prior to
sampling, the water level and bottom of the lysimeter  are measured to determine the volume of
water in the lysimeter. Using either a peristaltic pump or a syringe, the lysimeter is purged of three
volumes of standing water or pumped dry. The volume of water removed is recorded in the field
notebook. Specific conductance, temperature, and pH are monitored  while purging if the lysimeter
produces sufficient volume of water.  If the lysimeter  does not produce enough water then it is
pumped dry and sampled immediately following recovery. Since SERF does not sample hazardous
water, the water purged from the lysimeter is allowed to drain on the ground but away from the
lysimeter. Pore water is collected in sample bottles according to  the procedures  for surface water
outlined in Section 6.4.1.

6.4.4   Soil and Sediment Sample Collection

SERF collects  surface and subsurface soils  and sediment  samples according  to the following
protocols.

6.4.4.1 Surface Soil Samples

Surface soil samples are collected from  the upper 10 cm of an undisturbed location.  Surface
detritus is removed prior to sample collection.   The surface  soil samples are  collected with a
stainless steel trowel,  spade, PVC core, polycarbonate core or by hand and placed into plastic, wide-
mouth specimen cups.   The physical parameters of the soil, including color, moisture  content,
presence of biota, and texture are described in the field notebook if  required to satisfy the project
objectives.  The sample depth, date and time of sample collection, and the amount of sample (or
subsamples) collected are also recorded in the field notebook. Roots may or may not be removed
from the soil samples depending upon the project objectives.

Soil samples are homogenized either in the field or in the laboratory, depending upon the project
objectives.  If homogenized in the field, the soil sample is placed  into a polypropylene mixing tray
and homogenized by slicing, mixing, and remixing of the sample.  The homogenized soil sample is
then placed into a wide-mouth specimen cup and stored in a cooler in the dark for transport to the
laboratory.  In the laboratory, soil samples are homogenized  by mixing the entire sample in a
blender.

6.4.4.2 Subsurface Soil Samples

Subsurface soil samples are collected using either polycarbonate or PVC core tubes, pushed into the
soil or sediment by hand by twisting the tube in a circular clock-wise and then in a counterclock-
wise movement. The depth of the soil surface on the outside and on the inside of the  core tube is
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measured and recorded to determine compaction.

Once the core is extracted, plastic caps or neoprene rubber stoppers are inserted and taped to the
end of the tube to prevent slippage and spillage. The top direction of the core tube is marked on the
tube along with the sample number and the tube is stored in an upright position during transport to
the laboratory.  In the laboratory, the soil or sediment is extracted from the core tube and using a
stainless steel knife, a sample for analysis is collected from the center of the tube, away from the
sides.  The physical characteristics of the soil  are described in the field notebook, along with the
approximate amount of sample (or subsample collected).

In general, soil  sample compositing or  splitting  in the field  is not preferred due to potential
contamination concerns; the collection of duplicate samples in the field by collecting soil from the
same sample source and  homogenization of the samples in the laboratory with  a blender, is
preferred. If samples are to be homogenized in the field, then the samples will  be extracted from
the core tube onto a polypropylene tray and mixed with a stainless steel or Teflon spatula.  The
homogenized samples are then placed into plastic, wide-mouth specimen cups and  stored in a
cooler in the dark for transport to the laboratory.
6.4.4.3 Sediment Sample Collection

Sediment is collected using either polycarbonate or PVC core tubes or with an Ekman Dredge. The
sediment sample  is removed from the tubes or  dredge  and placed in a polypropylene tray.  A
stainless steel knife is used to collect a section of soil from near the center of the sample container.
These samples may be homogenized in the field by mixing with a spatula or homogenized in the
laboratory using a blender.  Samples are stored in plastic wide-mouth specimen cups and stored in a
cooler in the dark for transport to the laboratory.  The amount of sediment collected, all equipment
used, the method of homogenization, and the amount of sample stored are documented in the field
notebook.

6.4.5  Tissue Sample Collection

Plant tissue samples are collected by gathering the plants by hand and placed into plastic bags. The
plant samples are kept in a cooler on ice until transported to the laboratory.

6.5    Sample Documentation and Identification

All sample bottles are  pre-labeled in the laboratory prior to transport to the field site.  Labels of
colored tape are attached to the side of the bottle.  Water-proof ink pens are used to mark the labels
with a unique sample number  (Section 7).   Sample  containers  used for  the suspended matter
samples, sediment samples and tissue samples are used only once, and are marked with water-proof
ink pens directly on the outside of the  sample container.  The collection of all samples is recorded
in the field notebook.

6.6    Documentation

                                           6-  18
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                                                                                Section 6
                                                                           Date: 11/25/98
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The following is a list of the field records that are maintained:
       1.     Field Equipment Checklist
       2.     Fi el d Noteb ook with the fi el d data sheets.
       3.     Field Instrument calibration Sheet.
       4.     Chain of Custody Form.

6.7    Sample  Preservation, Holding Times, and Sample Volume

Sample containers, sizes, preservatives, and maximum holding times, by parameter are included in
Table 6.4.  Note, there are two columns listing sample holding times prior to analysis.  SERF
recognizes that  samples should  be analyzed as soon as possible after sample collection and the
holding times are defined  from date/time of sample collection.  SERF has instituted  its  own
maximum holding times as goals.  In almost all cases, the SERF holding times are more stringent
than those established by EPA (Table 6.4).  The SERF holding times are almost always met. In the
case of filtered soluble nutrients,  however, if the SERF  holding times are exceeded, then the
samples are frozen and analyzed within the maximum holding time.  Every effort is made to ensure
that the EPA holding times are not exceeded, but, should a sample be analyzed after the  maximum
holding time, the data for that sample will be marked with a qualifier code in the data report.

In the event that filtered samples need to be frozen, then  each sample bottle  is examined to
determine that there is adequate space for expansion (i.e. the sample bottle can only be 3/4 full). If
needed, sample  is removed from the bottle so that it is no more than 3/4 full.  Prior to analysis the
sample bottles are allowed to thaw slowly (2-3 hours) to room temperature then shaken well to
ensure that all constituents are re-distributed evenly throughout the sample as they were at the time
of sample collection.  Clementson and Wayte (1992) have demonstrated that freezing of water
samples results in no  change  in  dissolved nutrient concentrations for at  least  4  months  (See
Appendix C).  SERF has also demonstrated that freezing water samples has no effect on soluble
nutrient concentrations,  including ammonia, for at least 35 days (See Appendix C).

Samples are preserved  in the field, immediately following sample collection.  For the  most  part,
sample preservation requires placing the sample in a  cooler with ice, and in  the dark.  Suspended
matter samples collected for chlorophyll-a determination are preserved in the field by adding 1.5 ml
of acetone to the HDPE microcentrifuge tube with  a  disposable pipet.  The chlorophyll-a samples
are then stored in a cooler in the dark on ice.  Equipment blanks  for chlorophyll-a determination are
preserved with the same amount of acetone and stored in the dark on ice.  Any additional chemical
used to augment preservation in the field will be from the same source  as the chemical used to the
preserve the sample and any additional preservative  added to the samples is documented on the
field data sheet.  The acetone preservative used is of ACS reagent-grade or  better; obtained  fresh
from the laboratory stocks on a daily basis; and transported to the field in an HDPE bottle.

SERF does not  use  acid preservatives for ammonia,  total nitrogen, total phosphorus, and organic
carbon samples.  The addition of even small amounts of acid to a sample bottle collected for
ammonia  determination  enhances the uptake of ammonia into the sample  bottle  from the
atmosphere.  The concentrations of ammonia most commonly  determined in the  waters sampled
and analyzed by SERF are less than 0.05 ppm (3.6 |JVI).  At these low concentrations, even the
smallest uptake  of ammonia into a sample from the atmosphere will be detected  and produce an
                                         6- 19
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                                                                                  Section 6
                                                                            Date: 11/25/98
                                                                             Page 20 of 21
anomalous high result.

Samples collected for total phosphorus and total nitrogen are processed immediately upon receipt in
the laboratory (within 12 hours of sample collection) according to the sample handling procedures
for these methods (Appendix A and B), therefore, preservation with acid is not required. Samples
collected for total organic carbon are refrigerated, without acidification, until analysis.  SERF has
demonstrated that there is no difference in TOC concentrations between samples preserved with or
without acid for at least 33 days (See Appendix D).

6.8    Sample Dispatch

For most projects, samples are stored on wet ice in coolers and delivered  to the laboratory by the
field personnel on the same day of sample collection.  SERF performs its own laboratory analyses;
however, if samples must be sent to an out-side laboratory they will be shipped on the same day of
sample collection to the laboratory using a common carrier and  overnight delivery.  These samples
will  be  carefully packaged with bubble  wrap or  styrofoam to prevent breakage.  Individual or
duplicate samples will be placed in individual plastic, sealable, bags to prevent cross-contamination
if the sample bottles break.  Insulated coolers will be used for sample shipment. The lids and drain
ports of the coolers will be securely sealed with shipping tape to avoid opening. The samples will
be preserved in the coolers with wet ice, if appropriate.

6.9    Reagent Storage and Waste Disposal

6.9.1  Reagent Storage

The  type  of reagents  typically  transported to the field by SERF  are  limited  to pH buffers,
salinity/conductivity standard and acetone. The storage and transport procedures for these reagents
are listed in Table 6.5.

6.9.2  Waste Disposal

Field generated wastes are kept to a minimum since soaps, acids, and solvent compounds are not
used during equipment decontamination procedures. In addition, SERF does not perform sampling
of hazardous waste sites. The only wastes generated during sampling include calibration standards
for pH and acetone.  The field  calibration standards are taken  back to the laboratory, neutralized
and/or diluted then flushed down the sanitary sewer.  Any acetone that may be remaining on the
pipet tips is allowed to evaporate, then the pipet tips are disposed in trash receptacles.
                                          6-20
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TABLE 6.5.
Field Reagent Storage
  Chemical
  pH Buffers
  Salinity\conductivity
  standard
  Acetone
                                                                                  Section 6
                                                                             Date:  11/25/98
                                                                              Page 21 of 21
Method of Storage
Stored in original containers in the
laboratory and transferred to 60 ml HDPE
bottles in ziplock bags for transport to the
field.
Stored in their original containers in the
laboratory and transferred to 250 ml HDPE
bottles for transport to the field.
Stored in original steel container in a vented
cabinet designed for flammable storage.
Cabinet in laboratory is locked and labeled
as containing flammable substances.
Transferred to a 250 ml HDPE squeeze
bottles in ziplock bags for transport to the
field.
                                           6-21
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                                                                                 Section 7
                                                                           Date: 11/25/98
                                                                             Page 1 of21
7.0    Sample Custody

Sample custody is the responsibility of the sampling team and of the Chief Chemist.  The sampling
team is responsible for labeling, collecting, documenting  in the field notebook and transporting
samples to the  laboratory.  The Chief Chemist is responsible for proper storage of the samples
within the laboratory, and that the samples are analyzed within their appropriate holding times.
Figure 7.1 shows the centralized receipt log form used for any incoming sample set at SERF. This
centralized receipt log form is maintained in a loose leaf notebook at the Chief Chemist office.
Samples  are not discarded  until the analytical results are checked and approved by the Quality
Assurance Officer. All documentation/logs are signed/initialed by appropriate personnel.

Currently, all analyses of all samples collected by  our laboratory are performed by our laboratory.
However, should the need arise to  send samples via courier to another laboratory for analysis, then
the SERF sample chain-of-custody form (Figure 7.2) and/or one supplied by the contract laboratory,
including all necessary information, will be used.  This form will be included  within the sample
cooler and protected within  a plastic, sealable bag.  A copy of the form will be retained by SERF in
project specific files.  Upon  receipt of the samples, the receiving laboratory will be requested to sign
the sample chain-of-custody form and  send a copy  of the signed form via mail or facsimile to
SERF. The QA officer will be in charge of ensuring that a copy of the  signed chain-of-custody
form is obtained from the receiving laboratory.

SERF  also often  receives  samples (surface water,  ground  water, soils, sediments, and tissue)
collected by other researchers for analysis.   A completed SERF chain-of-custody form will be
required  to accompany the samples and will  be  signed by the QA  officer or SERF  technician
receiving the samples.   These samples will be  inspected  by the SERF QA officer  or  SERF
technician  for  integrity  and  completeness according  to  the chain-of-custody  form.   Any
discrepancies between  the samples  received  and  the  chain-of-custody form  and/or missing
information will be reported immediately to the researcher that collected the samples. Any samples
with visible contamination, leaks, damage, or odors will be noted on the form.  A copy of the chain-
of-custody form will be kept in the project specific files. Records of shipping receipts for outgoing
and incoming samples are maintained indefinitely at SERF office. Sample personnel responsible for
sample delivery are identified  in the chain of custody form as well as common  carriers that might
have been used in the process.

Each sample container is labeled with a unique sample identification number as indicated below:

                                     AAA###-###XX.

The first letters in the sample identification number (AAA) refer to the client or program name.  For
example, the three letters FBY would be used to  designate SERF samples collected from Florida
Bay.  The first set of numbers (###) can vary from 1 to 999 and refers to the survey or batch
number.  The second set of numbers  (###) is the  site number or bottle number.  The last letters
(XX)  refer to  the  type  of  sample   (U=unfiltered,  F=filtered,  S=soil/sediments,   T=tissue,
C=chlorophyll a) and the duplicate letter (A or B, not applicable for some clients' samples).

Sample numbers are recorded on sample containers, the  field data sheet, and sample chain-of-
                                          7-  1
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                                                                                 Section 7
                                                                            Date: 11/25/98
                                                                              Page 2 of 21
custody/log-in form.  When we receive samples collected by other researchers, a SERF technician
will assign the unique code to each bottle at the time of receipt, and record it on the bottle and
chain-of-custody/log-in form.  An example of a sample label is included below:
                                      FBY77-10UA

7.1    Field Custody

Loose-leaf field notebooks are used for all field documentation.  Once QA checked, the sheets are
removed from the notebooks and kept in project-specific files.  All field notebook entries are made
in waterproof ink and include the following: name and number of sampling trip; date of sampling
trip; general weather and water conditions (waves and tides); name of individuals in sampling team;
location and number  of sample; and time of sample collection. For the collection of surface water
samples, additional recorded information includes the water temperature (both surface and bottom),
salinity/conductivity (both surface and bottom), pH, dissolved oxygen, the volume of water filtered,
the depth of sample  collection, the amount of preservative added, and a description of the water
clarity (Figure 7.3).  For pore water sample collection,  additional information recorded in the field
notebook includes the water level in the lysimeter, the bottom depth of the lysimeter, the volume of
water removed during purging, and the specific conductance, temperature, and pH during purging
(Figure 7.4).  For soil and sediment samples, additional information recorded in the field notebook
include  the depth of sample collection,  physical characteristics  of the soil, and  method  of
homogenization  (Figure  7.5).  For tissue  samples, identifying characteristics of the plant are
included in the field notebook (Figure 7.6).  Each notebook page is signed by the sampling team. If
an error is made in the field notebook, corrections are made by drawing a line through the error and
entering the correct information next to the error.

In addition to  the field notebook,  the field sampling team  keeps a field instrument sheet (Figure
7.7). On this sheet is recorded the number of each field instrument and probe, as well as instrument
calibration check information.  All  sampling equipment and  decontamination procedures are
recorded, along with the use of any fuel powered units (boats, generators, or pumps).

7.2    Laboratory Custody

Upon transport of the samples to the  SERF laboratory at FIU, the field sampling personnel  log-in
the samples on the  Sample Checklist (Figure  7.8).  All of the sample bottles are inspected for
integrity, proper  documentation (labelling), and preservation (cooler with wet ice). Any  samples
bottles found broken, leaking, not properly marked or not properly preserved are rejected from
analysis, and noted on the bottom of the Sample Checklist.  Samples are stored in the appropriate
conditions, refrigerator or freezer, in a locked room,  with access to the  room limited to SERF
employees.  Standards are stored separately from samples.

The Sample Checklist serves to track the samples collected from a sampling event through sample
analysis, data validation,  and sample disposition.  The Sample Checklist is stored in the project
files.  These files are checked on a daily basis by the chief Chemist and the QA Officer to ensure
that samples are analyzed within their appropriate holding times.  The checklist includes the date of
sample  collection, initials of field sampler(s), date of receipt in the laboratory, and requested
analyses.                                                                           Special
                                           7-2
-------
                                                                                                                          Section 7
                                                                                                                     Date: 11/25/98
                                                                                                                       Page 3 of21
Figure 7.1
Centralized Sample Receipt Log-in Form
                                                  ANALYSES REQUIRED AND MAXIMUM ALLOWABLE HOLDING TIMES
DATE
REC'D



















PROJECT



















SAMPLE
#'S



















#OF
REPLICATES



















MATRIX



















APA
12hrs



















TURB
48hrs



















CHLA
21 days



















TOC
28 days



















TN
28 days



















TP
28 days



















NUTR
28 days



















SI
28 days



















TSI
28 days



















DOC
28 days



















                                                               7-3
-------
                                                                                                                                                          Section 7
                                                                                                                                                    Date: 11/25/98
                                                                                                                                                      Page 4 of21
Figure 7.2
Chain-of-Custody/Sample Log-in Form
                                                          SOUTHEAST ENVIRONMENTAL RESEARCH PROGRAM

                                                       OE 148 (office)A/H 321 (lab), University Park, Miami, FL 33199, 305-348-3095
                                                                  Chain of Custody Record/Sample
Page.
of
CLIENT/PROJECT NAME:
DELIVERED BY:
ACCOUNT NO.: AUTHORIZATION:
RECEIVED BY:
RECEIPT ASSESSMENT/COMMENTS:
BOTTLE
ID

















SAMPLE
ID

















MATRIX
FW/SW

















H2SOR
ODORS ?

















COLLECTION
DATE TIME


































#OF
REPLICATES

















DATE AND TIME:
ICE IN COOLERS?:
ANALYSES REQUIRED*
APA

















CHLA

















TOC

















TN

















TP

















NUTR

















SI

















TSI

















DOC

















SAMPLE COMMENTS

















 : Analyses and methods APA (Alkaline Phosphatase Activity); CHLA (chlorophyll a, SM 10200H); TOC, DOC (Total and Dissolved Organic Carbon, EPA 415.1); TN (Total Nitrogen, Antek);

  TP (Total Phosphorus, EPA 365.1); nutr (Soluble NO3, NO2 [EPA 353.2], NH4 [EPA 350.1], PO4 [EPA 365.1]); SI, TSI (Soluble and Total Silica, [EPA 370.1])
                                                                               7-4
-------
Figure 7.3
Surface Water Field Data Sheet
                                                                               Section 7
                                                                          Date: 11/25/98
                                                                            Page 5 of21
Sampling Event

Station
No.















Station
Name















Date

Time















Dept
h















Names

Temp















Salinity















D.O















Z(l;0.5)















Weather Conditions

Iz/Io















Volume
Filtered















Comment















                                          7-5
-------
Figure 7.4
Lysimeter Field Data Sheet
                                                                             Section 7
                                                                        Date: 11/25/98
                                                                          Page 6 of21
Sampling Event

Station
No.















Station
Name















Date

Time















Water
Level















Names

Total
Dept















Specific
Cond.















Temp















pH















Weather Conditions

Sample
Volume















Preservativ.















Comment















                                         7-6
-------
Figure 7.5
Soil/Sediment Field Data Sheet
                                                                              Section 7
                                                                         Date: 11/25/98
                                                                           Page 7 of21
Sampling Event

Station
No.















Station
Name















Date

Time















Depth















Names

Sample
Volume















Homogenization















Weather Conditions

Description















                                         7-7
-------
Figure 7.6
Tissue Field Data Sheet
                                                                                   Section 7
                                                                             Date: 11/25/98
                                                                               Page 8 of21
Sampling Event
            Date
               Names
                            Weather Conditions
Station
No.
Station
Name
Time
Description
                                            7-
-------
Figure 7.7
Field Instrument Sheet
                                                                             Section 7
                                                                        Date: 11/25/98
                                                                          Page 9 of21
Sampling Event
Date
Names Comments

Instrument
Name












Instrument
Number












Probe Number












Time












Calibration Check












                                         7-9
-------
Figure 7.8 Sample Checklist
Sample Checklist
                                                                                        Section 7
                                                                                   Date: 11/25/98
                                                                                   Page 10 of 21
                  Sampling Event:
                   Sampling Team
             Sampling Date / Time:
                Lab Receipt Date:
                                  Sample Nos.:
                                 Sample Matrix:
                              Sample Disposal Date:
                                    Initials:
            Analyses
Analysis
Date/Init
  SOP/
Issue Date
Data Entry
 Date/Init
QA Check
Date/ Init
             Salinity
              D.O.
             Temp.
         Alkaline Phosp.
            Turbidity
              TOC
            Nutrients
             Total P
             Total N
           Chlorophyll
                  Other Analyses:
                                              7- 10
-------
                                                         Section *
                                                      Dae  11/25.^1
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Figure 7 9
TOC-SOOO Log Book


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Figure 7 10
RFA Nutrient Analyzer Log Book
                                                                        Section. ?
                                                                   Dale: I U25/98
                                                                        ^- of 21
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-------
                                                      Section
                                                 Date- I I/ZS/Q
                                                  Pane 13 of 2
Figure 7 1 1
RFA Total Phosphorus
Book
-------
Figure 7. 12
RFA Sica Log
                                                                     Section "
                                                                 Oaie  11/25/98
                                                                 Page 14 of: I
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-------
                                                                    Section "
                                                                Dite  I1/25TO
                                                                Page 15 of 21
Figure 7 I J
Antek Nitrogen Analyzer Log Book
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                                    7- 15
-------
                                                       Seclaon '
                                                   Date: 11/25/98
                                                    Page 16 ofZ i
Figure 7 14
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                             7-
-------
Figure 7.15
Total Phosphorus Preparation Form
                                                                                                      Section 7
                                                                                                Date: 11/25/98
                                                                                                Page 17 of 21
                                                                  TOTAL PHOSPHORUS-WATER
                                                                  SERF TP SOP 001-98
                                                                  Tray contents:
                                                                  Prep (100 ^1 0.17 N MgSO4 + 5 ml sample per
                                                                  vial) and put in oven
                                                                  (80 °C):
                                                                  (Date MgSO4 was made	)
                                                                     Date      Time

                                                                  Taken out of oven:
                                                                                        Init
                                                                     Date      Time     Init

                                                                  Put in muffle oven (550 °C)

                                                                     Date      Time     Init

                                                                  Taken out of muffle oven:
                                                                     Date      Time

                                                                  Did the pellet melt? _
                                                                                        Init
                                                                  Add acid (5 ml HC1), shake, and put in oven
                                                                  (80 °C):
                                                                  Acid added:	
                                                                  ( Date acid was made:	)
                                                                  (L=0.06N, M=0.12N, H=0.18N; if varied put
                                                                  the letter in each circle)
                                                                     Date      Time

                                                                  Taken out of oven:
                                                                                        Init
                                                                     Date      Time

                                                                   Second shake:
                                                                                        Init
                                                                     Date      Time

                                                                  Analyzed:
                                                                                        Init
                                                                     Date      Time

                                                                  Vials discarded:
                                                                                        Init
                                                                     Date      Time     Init
                                                                  Comments or problems:
                                                     7- 17
-------
Figure 7.16
Total Nitrogen Preparation Form
                                                                          Section 7
                                                                     Date: 11/25/98
                                                                      Page 18 of 21
         Tray Contents:

  Prepared by:	
                        TOTAL NITROGEN PREPARATION LOG
Date/time:
HC1 added?
                                                                             10
    A
    B
    C
    D
                                      7- 18
-------
                                                                                 Section 7
                                                                            Date: 11/25/98
                                                                             Page 19 of 21
preservation of samples is noted in the comments  section of the checklist.  Once the required
analyses are performed on all of the samples collected in one sample event, the Sample Checklist is
initialed  and dated by  the sample  analyst.   Sample analysis  are  also tracked  in  individual
instrumentation notebooks and include sample handler name and sample number.  Figures 7.9 -
7.14 are copies of pages from instrument logbooks for the TOC-5000, RFA nutrient analyzer, RFA
total phosphorus analyzer, RFA  silica analyzer, Antek total nitrogen analyzer, and fluorometer.
Preparation of water and sediment/soil samples for total phosphorus and water for total nitrogen are
recorded on sample preparation forms (Figures 7.15 and 7.16).

Ovens, refrigerators and freezers  have digital temperature readouts that are monitored daily having
the temperature  recorded on the log posted  on each oven (Figures  7.17  and 7.18).  All oven,
refrigerator, and freezer monitoring thermometers will be checked annually against a NIST-certified
thermometer and the result of these checks and any  necessary corrections will be recorded on the
daily temperature logs.

The field notes, chain-of-custody/log-in form,  sample checklist, and raw instrument data printouts
for each  sampling  event are included in individual project files and kept indefinitely. These files
are stored in a locked file cabinet. Once the laboratory data is entered into the computer data base
and checked by the QA officer, the samples containers are directed to be either cleaned or discarded
and the date is recorded in the sample Checklist form.  Once the samples are discarded, the sample
checklist is dated and initialed.

7.3 Electronic Data Records

Data from field measurements and laboratory  analyses are  compiled and  summarized in computer
spreadsheet format. We currently use Quattro Pro (Lotus  123 compatible) and Microsoft Excel.
Separate spreadsheets for each sampling event are kept, and a compilation of all  data to date is
made.  Spreadsheets are  stored both on the hard drive of the computer, as well  as onto write-
protected floppy disks. In the event of computer equipment failure, the data files on the floppy
disks are used as backup.  The access to this electronic records is password protected.  A hard copy
of the spreadsheets are stored in the project files indefinitely.

All deletions or corrections will be documented on a hard  copy of the  spreadsheet and the person
making the corrections will initial any changes.

Records of all aspects relating to changes, updates,  problems and maintenance of the instrument
and database software will be maintained in the instrument logbooks.
                                          7- 19
-------
Figure 7.17  Refrigerator/freezer temperature Log
                     Daily refrigerator / Freezer temperature Log
                           Room	refrigerator
                                                                         Section 7
                                                                     Date: 11/25/98
                                                                     Page 20 of 21
              Date
Temp (UC)
Date
Temp (UC)
Date
Temp (°C)
                                      7-20
-------
Figure 7.18 Oven temperature Log
                                                                      Section 7
                                                                 Date: 11/25/98
                                                                  Page 21 of 21
                       DAILY OVEN TEMPERATURE  LOG

                              ROOM         OVEN
              Date
Temp (UC)
Date
Temp (UC)
Date
Temp (°C)
                                    7-21
-------
                                                                                 Section 8
                                                                           Date: 11/25/98
                                                                               Page 1 of 5
8.0    Analytical Procedures
Section 5 includes the parameters and their corresponding analytical method numbers
followed by SERF.

8.1    Laboratory Method Modifications

8.1.1  Autoanalyzer Methods

The methods for the inorganic nutrients (ammonium, nitrite, nitrate, and  soluble  reactive
phosphate) are modified  to be analyzed simultaneously by wet chemical analysis using a four-
channel Alpkem RFA-300 (Rapid Flow Analyzer) Nutrient Analyzer (Alpkem Corp., Clackamas,
OR) following the procedure for each inorganic nutrient as suggested by the Alpkem Corporation.
The Alpkem methods for ammonium, nitrite, nitrate, and soluble reactive phosphate are listed in
Table 5.2.  Total phosphorus of water and solid samples are also determined on the Alpkem RFA
following  evaporation then dry ashing according to ASTM D-4638-86(9.2).  Dissolved silica are
also determined on the Alpkem RFA using method USGS 12700-85 (a slight modification of EPA
method 370.1).

When  determining concentrations of inorganic nutrients  in seawater, SERF  uses  stock Sargasso
Seawater or Gulf Stream water as analyte-free water in preparing method blanks  and calibration
standards.  Prior to its use, the Sargasso Seawater or Gulf Stream water is analyzed to demonstrate
levels of analyte less than 20% of the MDL (meaning it is not detectable).

8.1.2  Total Nitrogen in Water Samples

SERF  prefers not to use  Total Kjeldahl Nitrogen plus nitrate and nitrite for the determination of
total nitrogen in water samples,  because of the imprecision,  insensitivity and tediousness of the
procedure.  Instead,  SERF determines Total Nitrogen using an ANTEK 7000 Elemental Analyzer.
This method was developed by Dr. Jones and ANTEK and involves injecting a small volume (5
|oL) of sample into an oxidation furnace, where all combined nitrogen is converted to Nitric Oxide
(NO).  NO is then reacted with ozone to form Nitrous Oxide (NzO), which is a chemiluminescent
reaction. The light emission is detected and quantified by a photomultiplier tube. This method has
been determined to produce results comparable to the Total Kjeldahl Nitrogen plus nitrate method
with better estimates of precision  and accuracy. A detailed description of this method along with a
method validation package are included in Appendix A.

8.1.3  Alkaline Phosphatase Activity

The alkaline phosphatase activity (APA) assay measures the  activity of alkaline phosphatase, an
enzyme used by bacteria to mineralize phosphate from organic compounds (Hashimoto, Kitao, and
Keiichiro,  1985. Relationship between alkaline phosphatase  activity and orthophosphate in the
present Tokyo Bay. Environ. Sci. Health, A20(7), 781-908). The determination of APA is currently
under research by SERF in an effort to determine if APA can be used as a biological indicator.  The
assay is performed  by adding  a  known concentration of an  organic phosphate compound (3-c-
                                           8- 1
-------
                                                                                Section 8
                                                                           Date: 11/25/98
                                                                              Page 2 of 5

methylfluorescein phosphate (MFP)) to an unfiltered water sample.  Alkaline phosphatase in the
water sample cleaves the phosphate from the MFP, leaving 3-o-methylfluorescein (MF), a highly
fluorescent compound.  The concentration of MF at the end of the assay is proportional to the APA
of the sample.

APA measurements are made within  12 hours of sample collection.  Duplicate 3 ml subsamples
from each sample bottle are pipetted into disposable cuvettes, and 30 |ol of MFP solution are added
to each. The MFP solution is prepared by dissolving 0.05255 g of anhydrous 3-o-methylfluorescein
phosphate in 100 mM Tris buffer, pH=8.7. The concentration of the final stock solution is 1  mM.

The fluorescence of the subsamples are immediately measured using  a Gilford Fluoro IV or
Shimadzu RF-1501  Spectrofluorometer (excitation = 430 nm,  emission = 507 nm) or Shimadzu
RF-Mini 150 Fluorometer (filters) and recorded.  The subsamples are then incubated for 2 hours in
an incubator at 25 degrees Centigrade, and then the fluorescence of the samples is measured again
using the same excitation and emission wavelengths.  The amount of MF produced in  2 hours is
quantified by comparison to a standard curve.

A stock standard solution  of 3-o-methylfluorescein is diluted to make working standards that
bracket the concentration of MF in the APA assays after 2 hours. Working standards are made up
from standard  stock solution and the fluorescence of the working standards is measured each day
that the analyses are performed.  Standard stock solution of 3-o-methylfluorescein is prepared by
dissolving 0.0346 g of 3-o-methylfluorescein in 100 ml of methanol for a resulting concentration of
1 mM.  Working standards  of 0, 1, 2.5, 5 and 10 |JVI 3-o-methylfluorescein are then prepared by
diluting the standard stock solution in analyte-free water.

8.1.4  Total Phosphorus

For the determination of total phosphorus in water, soil, sediment, and tissue samples, SERF does
not use the  typical ammonium persulfate digestion because of the explosive hazards and  special
handling requirements associated with the use of this chemical.  Instead, SERF uses the  sample
preparation  methods described by Solorzano and Sharp (1980. Determination of total dissolved
phosphorus andparticulate phosphorus in natural waters. Limnol. Oceanogr., 25(4), pp. 754-758;
see Appendix B). Total phosphorus is determined in water, soil, sediment, and tissue samples by
oxidizing  and  hydrolyzing  all of the phosphorus-containing compounds in a sample  to  soluble
reactive phosphate, and determining  the soluble reactive phosphorus  concentration by the EPA
Method 365.1.  For water samples, 100 ml of 0.17 N MgSCH is added to 5 ml of the water  sample
in a 8 ml glass scintillation vial and evaporated to dryness in a 80°C oven (usually overnight). Once
dry, the sample is ashed at 550°C in a muffle furnace for 3.5 hours and allowed to cool overnight.
The sample is then hydrolyzed with the addition of 5 ml of hydrochloric acid. The normality of the
acid is dependent on the salinity of the sample, ranging from 0.06 N HCL for freshwater samples to
0.12 N HC1 for seawater samples. The samples are then shaken, put into an 80°C oven for 3 hours,
shaken again, then allowed to cool in the oven overnight.

Soil, sediment and tissue samples are prepared in the same manner as the water samples except they
are first dried in an 80°C oven for 2 days then ground.  Approximately 25 mg of sample is put into
                                          8-2
-------
                                                                                Section 8
                                                                           Date: 11/25/98
                                                                              Page 3 of 5

a 20 ml glass scintillation vial with 1 ml of DIW and 200 jj] of 0.17 N MgSO4, then dried and ashed
as described for water samples, except they are hydrolyzed with 10 ml of 0.24 N HC1.

SERF  has analyzed NIST standard  reference material 1572 (citrus leaves) as well as replicate
samples of sawgrass according to the method described above.  The results of these samples are
included in Appendix B. The concentration of phosphorus in the NIST standard is reported as 1300
|ig/gm ± 200 |ig/gm, depending upon the analytical method. SERP's analysis of the NIST standard
resulted in an accuracy range of 99% to 101% recovery. Precision ranged between 1 and 3% RSD.
8.1.5   Silica

For the determination of silica in water, SERF uses USGS method 12700-85 (a modification of the
EPA 370.1 method) using the protocol outlined by Perstorp Analytical Environmental for analysis
on  an Alpkem RFA.   This  modification involves the addition  acidified  (with sulfuric acid)
ammonium molybdate and oxalic acid to the water sample, subsequent reduction with ascorbic
acid, and the spectrophotometric measurement of the resulting color development at 660 nm.

8.1.6   Chlorophyll a

A modification of the  SM 10200H  chlorophyll  a method is used by SERF.  Each sample is
collected according to the protocol given in Section 6.4.1.  Saturated magnesium carbonate is not
added to each filter as preservation is  not necessary since acetone is immediately added to the
filters. Extraction of the pigment is done in a microcentrifuge tube with 1.5 ml of acetone, in the
dark,  at -20DC, for several days.  Before analysis on a spectrofluorometer, each filter is pushed
down into the tip of the tube with a stirring rod, and centrifuged for 3  minutes. In a glass cuvette,
0.75 ml of the sample and 2.25 ml of acetone are combined and the relative fluorescence at an
excitation of 435 nm and emission of 667 nm is recorded.
8.2    Laboratory Operations

8.2.1   Laboratory Glassware Cleaning

All laboratory glassware is cleaned by rinsing with hot tap water, washing within Liquinox in hot
tap water, rinsing with hot tap water, rinsing with 10% HC1, then rinsing three times with analyte-
firee (deionized water) water.  Glassware used for determination of total  and dissolved organic
carbon analyses are also soaked in RBS35 (a dichromate-sulfuric acid mixture substitute) for 12
hours prior to rinsing.  Once dried, all glassware is stored in one area of the laboratory in cabinets
separate from reagents and standards.  Class A volumetric glassware is not baked.

8.2.2   Reagent and Chemical Storage

All reagents and chemicals used in the laboratory are listed on Table 8.1. The method of storage for
each reagent is also included on Table 8.1.  Small quantities of reagents to satisfy a month or two of
                                          8-3
-------
                                                                                  Section 8
                                                                             Date: 11/25/98
                                                                                Page 4 of 5

analyses are kept in the laboratory.  Each class of chemical is kept in its own dedicated storage area.
 Larger quantities of reagents are kept in a locked,  outside storage area, with limited access. While
being used in the laboratory, compressed gas cylinders are secured upright with straps or chains.
New and empty compressed gas cylinders are also secured upright in an outside storage area that is
locked with limited access. As each reagent or chemical is received it is dated and initialed by the
person unpacking it. When the container is opened for the first time it is dated again and initialed
by the opener.

8.2.3   Waste Disposal

Wastes produced in the laboratory include liquid acids, bases, salt mixtures and acetone. Many of
these  reagents  are spent during sample prep and analysis.  Any remaining waste acids and bases are
neutralized then washed  down the sink to the  sanitary sewer.  Non hazardous salt mixtures are
diluted and washed down the sink.  Small quantities of acetone is washed down the sink with large
volumes of water.  Empty reagent bottles are rinsed with hot  tap water and  disposed  in  trash
receptacles.  SERF never stores wastes; therefore, segregation and storage protocols are not needed.
 Since all wastes are either put down the drain or in trash receptacles, no documentation of waste
disposal is needed. Bade County sewer discharge requirements and restrictions are followed.
                                             -4
-------
TABLE 8.1
Reagent and Chemical Storage
                                                                                                                                                  Section 8
                                                                                                                                            Date: 11/25/98
                                                                                                                                                Page 5 of 5
Chemical
Laboratory Chemicals
Mineral Acids (a)
Liquid Bases (a)
Liquid Oxidizers (a)
Organic Solvents (a)
Compressed Gases
Dry Chemicals
pH Buffers
Method of storage

Stored in original glass containers in a cabinet dedicated to acid storage.
Stored in original glass containers in a cabinet dedicated to corrosive substances.
Stored in original plastic container in a dedicated cabinet.
Stored in original glass containers in a vented cabinet designed for flammable storage.
Cabinet in laboratory is locked and labeled as containing flammable substances.
Secured upright in laboratory and in outside, locked, storage area.
Stored in original containers in alphabetical order in a dry cabinet.
Stored in original containers in dedicated cabinet.
(a) Small quantities are stored in dedicated cabinets within the laboratory. Larger quantities are stored in an outside storage area that is kept locked with limited access.
                                                                              -5
-------
                                                                                   Section 9
                                                                             Date: 11/25/98
                                                                                Page 1 of 17
9.0    Calibration Procedures and Frequency

9.1    Instrument Lists

Laboratory and field instrumentation are listed in Table 9.1.

9.2    Standard Receipt and Traceability

Primary  standards traceable to NIST reference standards  are purchased from reliable scientific
supply firms.  The standards are received by  the Chief Chemist, inspected,  dated, initialed, and
stored in the appropriate storage area for that  standard (desiccator, refrigerator, or freezer).  Once
opened, the standards are  dated  and initialled again.    The manufacturer's  certificates for each
standard received are kept on file in a central location.

9.3    Standard Sources and Preparation

The source, preparation, and storage of standards are included on Table 9.2. Primary standards are
prepared by dissolving the source standard into analyte-free deionized water.  Secondary and
working standards are prepared by diluting the primary standards in deionized water.  Standard
preparation methods are detailed in the  laboratory SOP.  The date, concentration, chemical vendor,
lot number, and technician's initials for all standards made are recorded in the standard and reagent
preparation logbook (Figure 9.1). Once prepared, the standard bottles are dated and initialed, then
preserved according to the methods summarized  in  Table 9.2.   Preservation method,  storage
location, and expiration date are  also  recorded on the  standard bottles.   Primary standards are
produced at least quarterly, while working standards are produced daily.  As no new standard or
reagent is  prepared until the previous one has been  either completely used or  expired  and
discarded, the logbook records link the preparation with every specific analysis.

9.4    Instrument Calibration

All field and  laboratory instruments are calibrated,  and  checked for proper function prior to
analysis. Table 9.3 summarizes the calibration procedures for field instruments,  while Table 9.4
summarizes calibration  procedures for  the laboratory  instruments.  Calibration procedures for all
instruments are described below.

9.4.1  Field Instruments

Field  instrument calibration checks are recorded on the Field Instrument Calibration Sheet included
as Figure 7.2. These sheets are kept in project specific files.
                                            9- 1
-------
TABLE 9.1
Instrument List
                                                                                                                 Section 9
                                                                                                             Date: 11/25/98
                                                                                                               Page 2 of 17
Manufacturer
Laboratory Equipment
Alpkem
ANTEK
Shimadzu
Gilford Instruments
Carlo Erba
Fisher
Hewlett Packard
Allied
Blue
HF Scientific
Model

4-channel RFA 300 Rapid Flow
Analyzer.
7000 Elemental Analyzer
TOC-5000 Total Organic Carbon
Analyzer
RF-1501 Spectrofluorometer
RF-Mini 150 Fluorometer
Fluoro IV Spectroluorometer
1 500 CHN Analyzer
Models 255G and 255D IsoTemp Ovens
Model 5890 Oven
Model 7303DA Balance
LabHeat Muffle Furnace
DRT-15CTurbidimeter
Parameters

Ammonium, Nitrate, Nitrite, Ortho-
phosphate, Total Phosphorus, Silica
Total Nitrogen
Total Organic Carbon, Dissolved Organic
Carbon
Chlorophyll, Alkaline Phosphatase
Activity
Alkaline Phosphatase Activity
Chlorophyll, Alkaline Phosphatase
Activity
Total Carbon, Total Nitrogen
Total Phosphorus
Total Carbon, Total Nitrogen
Bulk Density
All Parameters
Total Organic Carbon
Turbidity
Matrix

SW, PW, SED
SW,PW
SW,PW
SW,PW
S, SED, T
SW,PW, S, SED
S,SED
S, SED
All Matrices
S, SED
SW,PW
                                                           9-2
-------
Table 9.1 Continued
Instrument List
                                                                                                                     Section 9
                                                                                                                Date: 11/25/98
                                                                                                                   Page 3 of 17
Manufacturer
Field Equipment
Orion
Orion
Orion
LI-COR
SEA-BIRD
Model

140 Conductivity/Salinity/
Temperature Meter
840 Oxygen Meter
SA 250 Meter and Ross
Combination Electrode
LI-1000 Datalogger
LI-193SA Quantum Light Sensors
SEACAT SEE 19-03
Conductivity/Temperature/
Depth Meter
Parameters

Salinity
Temperature
Dissolved Oxygen
pH
Photosynthetically Active
Radiation/Light Attenuation
Coefficient
Temperature Conductivity/Salinity
Dissolved Oxygen
Turbidity
Photosynthetically Active Radiation
Depth
Matrix

SW,PW
SW,PW
SW,PW
sw
sw
                                                             9-3
-------
Figure 9 I Standard and Reagent Logbook
                                                           Seenon ^
                                                       Date' ! 1/25/98
                                                         Pane 4 of 17


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                                                          56
                                9-4
-------
                                                                                                                     Section 9
                                                                                                                Date: 11/25/98
                                                                                                                  Page 5 of 17
TABLE 9.2
Standard, Source, Preparation, and Storage.
Instrument/Parameter

Alpkem RFA Auto-
Analyzer




Ammonia
Nitrite
Nitrate
Phosphate
Total Phosphorus
Silica







Shimadzu
TOC-5000 Total
Organic Carbon Analyzer


ANTEK 7000 N Total
Nitrogen Analyzer
Total Nitrogen
Standard
Sources
Fisher
Scientific, Inc.





NIST











Fisher
Scientific, Inc.



Fisher
Scientific, Inc.

How Received

Dry, ACS Reagent Grade
powder




....Solids 	

Dry Soil and Plant
Standards









Dry, ACS Reagent Grade
powder



Dry, ACS Reagent Grade
powder

Source Storage

Room Temperature






Desiccator Room
Temperature










Room Temperature




Room Temperature


Preparation from source

Primary from source:
5 |omol/ml NFL|+
1 |^mol/ml NC>2
10|amol/mlNO3"
1 Nmol/mlPC>43"

5 |^mol/ml SiC>2

Mixed from primary (for
dissolved nutrients):
1.56|amol/mlNH4+
1.25|amol/mlNO3"
0.31|amol/mlPO43"
Working from mixed standard
Working from primary for NC>2
, SiC>2, and Total Phosphorus
(see attached SOPs for lab /
field nutrient analysis and for
Total Phosphorus)
Primary from source: 10,000
mgC/1

Working from primary:
0,5,10,20 mgC/1
Primary from source:
2mgN/l

Lab Stock
Storage
Room
Temperature
with
Chloroform




Room
Temperature
with
Chloroform


Not Applicable




Refrigerate


Not Applicable

Room
Temperature w/
chloroform
Preparation
Frequency
Quarterly







Quarterly or as
needed




Daily




Quarterly


Daily

Quarterly or as
needed

                                                            9-5
-------
TABLE 9.2 Continued.
Standard, Source, Preparation and Storage
                                                                                                                    Section 9
                                                                                                               Date: 11/25/98
                                                                                                                 Page 6 of 17
Instrument/Parameter
Fluorometer Chlorophyll
Alkaline Phosphate
Activity

Carlo Erba
Total Carbon
Total Nitrogen
Turbidity
Standard
Sources
Sigma, Inc.


Fisher Scientific, Inc.
NITS
HF Scientific, Inc.
How Received
Dry, ACS Reagent Grade
powder


Dry ACS
Reagent Grade
SRM
Sealed 0.02 NTU reference
standard sent with
Instrument (calibrated in
each applicable range)
Source Storage
Dessicator
Freezer


Room Temperature
Desiccator
Room Temperature
Room Temperature
Preparation from source
Primary from source:
5 mg/1 chl a in acetone
Working from primary:
8 standards: 0-0.5 mg/1
Primary from source:
1 mmol/lMF
Working from primary:
0,1,2. 5,5, 10 nmolAMF
Used Directly
Used Directly
Not Applicable
Lab Stock
Storage
Freezer
Not
Applicable
Freezer
Not
Applicable
Desiccator
Desiccator
Not
Applicable
Preparation
Frequency
Quarterly or as
needed

Daily
Daily
Daily
Replace
annually
                                                            9-6
-------
                                                                                                                    Section 9
                                                                                                               Date: 11/25/98
                                                                                                                 Page 7 of 17
TABLE 9.2 Continued.
Standard, Source, Preparation and Storage
Instrument/Parameter
Orion pH Meter
PH
Orion Model 840 DO meter
Analytical Balances
Pipetman and Eppendorf
Pipets
Standard
Sources
Fisher
Scientific, Inc.
Orion
Troemner
DI Water
Weight
checked
How Received
pH 4.0, 7.0 and 10.0
solutions
Calibration Sleeve with
Instrument
Stainless Steel
(Class S weights)
In-house
Source Storage
Room Temperature
Room Temperature
Room Temperature
Room Temperature
Preparation from source
Not Applicable
Not Applicable
Not Applicable
Not Applicable
Lab Stock
Storage
Not Applicable
Not Applicable
Not Applicable
Not Applicable
Preparation
Frequency
Replace on
expiration
Not Applicable
Daily,
Semiannual
Service
Calibration
Daily, factory
calibrated as
needed
                                                            9-7
-------
                                                                                                                    Section 9
                                                                                                               Date: 11/25/98
                                                                                                                 Page 8 of 17
TABLE 9.3
Field Instrument Calibration
Instrument

Orion S/C/T Meter


Salinity/Conductivity
Temperature

Orion Dissolved Oxygen
Meter



Orion pH Meter



HF Scientific
Turbidimeter



Calibration Type




Continuing Check
Continuing Check

Initial


Continuing

Initial

Continuing

Initial


Continuing

No. of Standards




o
J

1
1


1

2

1

1


2

Type of Curve




Linear
Linear

Linear


Linear

Linear

Linear

Linear


Linear

Acceptance/
Rejection Criteria

Salinity or conductivity
within 5% of standard
value
Temperature within 0. 1
degrees of NIST
thermometer value
Slope must be within
0.7-1.2

Result within +1-5% of
Winkler titration
Reading must be with
0.05 pH units.
Reading must be within
0.05 pH units.
Reading within 0.01
NTU

Reading within 0.01
NTU
Frequency


Daily, prior to use,
every 4 hours, and end
of each use.

Daily
Daily, prior to use,
every 4 hours, and end
of each use.
Annually

Daily, prior to use.

Every 4 hours, and end
of each use.
Daily, prior to use,
every 4 hours, and end
of each use.
Quarterly

                                                            9-8
-------
                                                                                                                    Section 9
                                                                                                                Date: 11/25/98
                                                                                                                  Page 9 of 17
TABLE 9.3
Field Instrument Calibration
Instrument
LI-COR Light Meter
SEA-BIRD CTD

Calibration Type
Continuing Check
Continuing Check

No. of Standards
0
1
1
Type of Curve
Log
Linear
Linear
Acceptance/
Rejection Criteria
Reading between
0.95-1.05 over a
non-reflective
surface in air.
Salinity or
conductivity within
5% of standard value
Temperature within
0.1 degrees of NIST
thermometer value
Frequency
Daily, prior to use,
every 4 hours, and
end of each use.
Daily, prior to use,
every 4 hours, and
end of each use.
Daily
                                                            9-9
-------
                                                                         Section 9
                                                                    Date: 11/25/98
                                                                     Page 10 of 17
TABLE 9.4
Laboratory Instrument Calibration
Instrument/
Analysis

Alpkem Rapid
Flow Analyzer
NH4+
NO2
NO3"
PO43"
Total P
Si02
Shimadzu Total
Carbon
Analyzer




ANTEK
Elemental
Analyzer
Total Nitrogen




Gilford and
Shimadzu
Spectro-
fluorometers

Carlo Erba
Total Carbon,
Total Nitrogen
Calibration
Type

Initial + Final



Continuing



Initial



Continuing


Initial



Continuing



Initial


Continuing

Initial

Continuing
No. of
Standards

5



1 Blank

1 Intermediate

4


1 Blank


IHigh
5



1 Blank
IHigh


5


1 -Intermediate

1

IHigh
Type of
Curve

Linear







Linear






Linear







Linear




Linear


Acceptance/
Rejection
Criteria
R>995



Value of zero

90-110%ofexp.
value
R>995




90% -110% of
value
R>0.99



Value of zero
90% -110% of
value

R>995


90% -110% of
value.


90%-110%of
value.
Frequency


Daily, Prior to
use .


Every 20
samples
Every 20
samples
Daily, Prior to
use .

Every 20
samples
Every 20
samples
Annually or
upon placement
ofpyrolysis
tube
Daily, prior to
use, every 20
samples, and
end of run
Daily, prior to
use.

Every 20
samples.
Daily, prior to
use, every 20
samples, and
end of run.
                                      9- 10
-------
                                                                                 Section 9
                                                                            Date: 11/25/98
                                                                             Page 11 of 17
9.4.1.1. Salinity/Conductivity/Temperature

The Orion model 140 Salinity/Conductivity/Temperature meter, with a 014010 4-electrode probe,
is factory calibrated and compensated for temperature.  Salinity and/or conductance is checked daily
with a solution of known salinity or conductance, while temperature is checked daily  against an
NIST thermometer. The S/C/T meter probe and the NIST thermometer is inserted into 25 ml of the
salinity and/or conductance  standard.   A conductivity and/or salinity reading within  5% of the
standard value, and a temperature within 0.1 degrees are considered acceptable.  Values outside
these acceptance criteria will require the unit to be factory calibrated.

9.4.1.2. pH

The pH meter/probe is  calibrated before each  field day.   We  use  an automatic temperature
compensation (ATC) probe to adjust for differences in temperature between standards and samples.
 Standard pH buffers (pH 7.00, cat. no.  SB108-500; and 10.00, cat. no. SB116-500) are  purchased
from Fisher Scientific. The two-point calibration procedure is as follows:

       1.      Choose pH 0.01 mode.
       2.      Rinse probes (pH combination and ATC) in DIW. Blot dry. Rinse with ca. 2 ml of
              pH 7.00 buffer. Immerse probes in pH 7.00 buffer.
       3.      Press  Cal button.  The meter will display ".1." and  the pH value of the buffer; the
              meter automatically recognizes the pH of the buffer solution.  When pH stabilizes,
              press Enter. The display will freeze for 3 seconds, and then display ".2.".
       4.      Rinse probes in DIW.  Blot dry. Rinse with ca. 2 ml of pH 10.01 buffer. Immerse
              probes in pH 10.00 buffer.
       5.      Wait for pH display to stabilize, and press Enter.  Display now will say "PH" and be
              ready for sample measurement.
       6.      Rinse probe in DIW, place probe in  pH 7.00 buffer,  and check that  pH  meter
              reading is within 0.05 pH units.

The response of the pH meter is checked with the pH 7.00 buffer after 4 hours of use and at the end
of each use.  If the response is outside 0.05 pH units, the two-point calibration is repeated.

In case of low pH level samples, the pH 4.00 and pH 7.00 standards will be used in the calibration
procedure.

9.4.1.3. Dissolved Oxygen

The probe  of the Orion model 840 Dissolved  Oxygen meter is continuously polarized when
attached to the meter; if it has been disconnected for over 1 h it requires 50 min to repolarize.  No
readings or calibration should be attempted within 50  min of connecting the probe. Calibration is
preformed at the  beginning of every field day. A one point calibration is done, there  is no zero
current on the probe.  The calibration procedure is as follows:

       1.      Saturate the sponge in the calibration sleeve with deionized water.
       2.      Switch the meter on and wait 20 min for equilibration.
                                          9- 11
-------
                                                                                  Section 9
                                                                             Date:  11/25/98
                                                                              Page 12 of 17
       3.      Depress and hold the Mode Key Pad until the display cursor is at Cal.
       4.      Depress quickly and release the Mode Key Pad.  The display will show three dashes
              (—) and the slope of the  electrode/membrane system.  If the  slope is outside the
              range 0.7 -1.2, the probe must be serviced.
       5.      Remove  the calibration sleeve.   The  probe can  now  be used to make field
              determinations of dissolved oxygen concentration.

In addition, the response of the D.O. meter is checked against a Winkler titration on an annual
basis.

9.4.1.4 Turbidity Meter Calibration

A 0.02 NTU reference  standard, EPA approved  and shipped with the instrument,  is  used to
calibrate the instrument before each day's analyses.  Additionally, higher  turbidity standards,
prepared from a 4000 NTU stock Formazin solution, are used to check the instrument calibration
annually. The stock Formazin is purchased from HF Scientific, Inc., Ft. Meyers, FL.

Calibration is accomplished by inserting the 0.02 NTU standard cuvette into the instrument in the
proper orientation  and the  Reference Adjust Knob on the instrument is turned until the readout
displays 0.02. The standard cuvette must be clean and unscratched.  The cuvette is wiped with lint-
free wipers and inserted so that the index line on the cuvette matches the instrument's index line.

9.4.1.5 Light Meter Calibration

The calibration of the LI-COR instrument is checked on a daily basis.  The instrument is held in an
upright position in the air over a non-reflective surface such as still water, pavement, or grass (not a
white boat or concrete dock).  The instrument calibration reading is recorded and should  be
between 0.95 to 1.05.

9.4.1.6 CTD Calibration

Salinity/conductance is  checked  daily with a solution of known  salinity/conductance, while
temperature is checked daily against a NIST thermometer.  A conductivity reading within 5% of the
standard value, and a temperature within 0.1 degrees are considered acceptable.  Values outside
these acceptance criteria will require the unit to be factory calibrated.  The  unit is also factory
calibrated on an annual basis.

9.4.2   Laboratory Instruments

9.4.2.1 Alpkem Rapid Flow Autoanalyzer

The autoanalyzer is calibrated daily, using a five-point calibration standards of ammonium, nitrate,
nitrite,  and  phosphate.   Total phosphorus and  silica  are each analyzed separately on  the
autoanalyzer, also  using a five-point calibration.  Standards  are  prepared in  the matrix to  be
analyzed (i.e. freshwater or seawater).  The five-point calibration is checked at the beginning of
each run.  A linear calibration with an R square of greater than 0.995 is considered acceptable.
                                           9- 12
-------
                                                                                  Section 9
                                                                             Date: 11/25/98
                                                                              Page 13 of 17
Blanks are inserted after every 10 samples to monitor and correct for baseline drift. A log book is
kept to monitor the calibration curve parameters.  The instrument is recalibrated if accuracy is not
within 90 and 110  percent.   If continued attempts at calibration  do not meet the accuracy
requirements, then the instrument is cleaned and overhauled.

9.4.2.2 Total Organic Carbon Analyzer

A four-point standard curve consisting of 0, 5, 10, and 20 mgC/1 standards is run prior to every run.
 A linear calibration with an R square of greater than 0.995 is considered acceptable.  A log book is
kept to monitor the instrument calibration.  The instrument is recalibrated if accuracy is  not within
90 and 110 percent.  If continued attempts at calibration do not meet the  accuracy requirements,
then the instrument is cleaned and overhauled.

9.4.2.3 Total Nitrogen Analyzer

A five-point calibration  of the ANTEK Total  Nitrogen Analyzer is  conducted annually (see
Appendix A), or upon replacement of the pyrolysis tube. A two-point calibration is prepared daily
prior to every run using a 2.0 mgN/1 standard.  Due to the nature of the Total Nitrogen Analyzer,
zero total nitrogen has a signal of 0.  Intra-run drift in the calibration curve is monitored by insertion
of additional 2.0 mgN/1 standards after every 10 samples and at the end of the run.

9.4.2.4 Fluorometer

Calibration of the fluorometer for  chlorophyll determination  is done using solutions  of known
chlorophyll content dissolved in acetone.  Chlorophyll standard  is made from purified chlorophyll-a
obtained from Sigma Chemical Co.  The concentration of the  standard solutions  are measured
spectrophotometrically, and  a series of chlorophyll standards are prepared that bracket the range
from 0  to 0.5  mg/1.  Fluorescence of  these standards is determined,  and a standard curve is
generated.

A five-point standard  curve of 3-o-methylfluorescein is used to  calibrate the  fluorometer for
alkaline phosphatase activity (APA), prior to and at then end  of every run.  An R square of greater
than 0.995 is considered acceptable.  Values outside this range require recalibration.

9.4.2.5 Carlo Erba

The  Carlo Erba  is  calibrated with one  standard of known total  carbon and total nitrogen
concentrations. The  standard is run prior to every run,  after every 10 samples, and at the end of a
run.  An accuracy between 90 a 110 % is considered acceptable.

9.4.2.6 Balances

The balances are calibrated daily using 10 mg,  1 g, and 100 g weights and these calibration checks
are recorded in a logbook (Figure 9.2).

9.4.2.7 Pipettes
                                          9- 13
-------
                                                                                   Section 9
                                                                              Date: 11/25/98
                                                                               Page 14 of 17

Pipettes are checked following the procedure in Figure 9.3 and the results of these checks are
recorded in a logbook (Figure 9.4). If the pipette fails to achieve a weight / volume value within the
specified range, it is recalibrated with the appropriate tools. Any needed recalibration is recorded in
the logbook.
                                           9- 14
-------
Figure 9.2 Balance Calibration Log
                                                              Section 4>
                                                          Date: 11/25/98
                                                           Page 15 of 17
                       U,
  7ih i
' G Q 9
   J
|OO.Oo?
            D.OIO?
 !D5£)Of
                                       o
/OH   (.003
       I.
    1  1
                                                                  PL
tOO-CI
ICD-DC-
  J/ff/fB^f^  1.0*75 |o».o0{   fl'0|a  |.
  " jT I f™"/' * /*V  d. -*. • j •   tl    «%. ™*
                                                          ^1     JL
                                9- IS
-------
                                                                Section ^
                                                            Date: 11/25/98
                                                             Pige Idol" II
Figure <> 3 Pipctie Calibration Log
                         Jif
             .f/(W0       J:
                                                  Ji^r
                                     , 010 I      a^J-**^  p^
              PIG         3?4       i°"
                                     o-
             ifyaso      '2»f*         6
                                                            M, *J


                                                            WAJ
                                                             PL
             |f-5soo
                         ^irfr       vaot^-       ^       t^~
                              %        ,looi        *"        ^^~
                                       coit,i        ^"        P^
             r           v  •          ', J
-------
                                                                   Section 9
                                                              Dale: IU2S/°B
                                                               Page 17 of 1 ?
Figure 9 4  Daily Pipette Calibration Instructions
               DAILY PIPETTE CALIBRATION INSTRUCTIONS

  1.  Record the data,  pipttt* model  (ju«T P-SQMi,  P-100, etc.), and
  pipette ID (i.e.  321A, 316 prep, etc,I,

  2.  Sat  the pipette on the highest  setting  (e.g*  20-0 pi for a
  P-200^ .   Always dial SJQ.WH to th* setting (dial up a  little p«at the
  eatting,  then dial down).

  3.  Dispense that volya* of DIM into m  tarad  w*igh cup,

  4*  If the weight  is within the acceptable rang« (••• chart below or
  on  th*  balance),  th*n  record the w«igtit, put  a diack th* OK eodttmn,
  and initial,

  5,.  If  the weight is QH£ within the acceptable rang*,  try at  least
  two more tines.   If  the weight is still not acceptable, record the
  last u*ight obtained,  put an x in the OK column, initial, and  faring
  th* bad pipette to the QA Officer.
                      Accuracy  rangei
                                 4,5700  - 5.0300
                      P-1000     0,9920  - 1.0080
                      P-^QO      Q»l§§4  - 0.2016
                      P-lOO      O.OS9J  - O.IOO8
                      V~?,Q       O.Olffi  - 0,0101
                      P-10       0.0099  - 5,0101
                                     - 17
-------
                                                                                Section 10
                                                                            Date: 11/25/98
                                                                               Page 1 of 3
10.0   Preventive Maintenance

10.1   Routine Maintenance

Preventive maintenance is an essential part of a properly  functioning laboratory.    For field
equipment, general maintenance includes cleaning, proper storage, check batteries and keeping the
instruments fully charged.  In addition, all probes are checked and replaced as necessary.  The
laboratory equipment receives thorough cleaning after every use. A more detailed summary of the
maintenance procedures conducted on  each  piece of laboratory equipment is presented in Table
10.1, while field equipment is presented in Table 10.2.

10.2    Maintenance Documentation

Log books are kept on each piece of equipment.  Instrument response to calibration standards, the
number of samples run, and the hours of instrument use are recorded in each log book. In addition,
all maintenance activities for each instrument are recorded in the log book. A record of service
performed by the manufacturer or other service contractor is kept in the instrument files.

10.3    Contingency Plans

SERF maintains a stock of spare parts for all analytical instruments.  Instruments which can not be
fixed by SERF personnel are sent to the manufacturer or other service contractor.  If  equipment
failure occurs,  SERF  will either operate backup equipment at its  laboratory, or it has access to
backup  equipment in  other laboratories at FIU.  In any event, sample holding time will not be
jeopardized.
                                          10- 1
-------
TABLE 10.1 Laboratory Equipment Preventive Maintenance
                                                                                          Section 10
                                                                                     Date: 11/25/98
                                                                                         Page 2 of 3
  Instrument
Activity
Frequency
  AlpkemRFA
Clean and inspect tubing and fittings
Clean Platens
Wash manifold/flow cell
Check cadmium column
Inspect filters
Change tubing
Recondition pump rollers
Service Maintenance
Daily
Daily
Daily
Daily
Every 200 hours
Every 200 hours
Every 200 hours
Semiannually
  Shimadzu TOC Analyzer
Check 1C reagent level
Check DIW level
Check gases
Replace tubing
Replace needles
Change columns
Daily
Daily
Daily
As needed
As needed
Every 2000 samples
  Carlo ERBA
Check gas flow
Monitor Voltage
Reduce copper column
Repack water trap
Repack oxidation column
Daily
Daily
Every 150 samples
Every 150 samples
Every 350 samples
  ANTEK 7000N Nitrogen
  Analyzer
Replace autosampler septa
Replace column septa
Monitor vacuum pressure (25 inHg)
Change combustion column
Every 80 Samples
Every 40 Samples
Daily
As Needed
  Fluorometer
Clean and inspect sample chamber
Daily
  Analytical Balances
Clean weighing compartment
Clean interior/exterior
Check calibration
Factory service calibration
Daily
Monthly
Daily
Semiannually
  Ovens, Refrigerators, and
  Freezers
Check temperature
Calibrate with NIST thermometer
Daily
Annually
                                               10-2
-------
                                                                              Section 10
                                                                          Date: 11/25/98
                                                                             Page 3 of 3
TABLE 10.2 Field Equipment Preventive Maintenance
 Instrument
Activity
Frequency
 pH meter
Check batteries - recharge
Check liquid in probe
Replace probes
Rinse with analyte-free water
Daily
Daily
Every 6 to 9 months
Before and after each use
 Dissolved oxygen meter
 and S/C/T meter
Check batteries - recharge
Check probes
Daily
Daily
 Turbidimeter
Check battery - recharge
Check light source
Check cuvettes are scratch-free
Daily
Daily
Daily
 LI-COR Light Meter
Check battery - recharge
Check calibration
Factory service calibration
Daily
Daily
Annually
  SEA-BIRD CTD
Check battery - recharge
Check Tygon tubing is secure and
filled with DIW
Check all probes and connections
Check calibration
Factory service calibration
Daily
Daily

Daily
Daily
Annually
                                         10-3
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                                                                               Section 11
                                                                           Date: 11/25/98
                                                                              Page 1 of 5
11.0   Quality Control Checks and Routines  to Assess Precision, Accuracy and
       Calculation of MDLs

SERF uses both field and laboratory QC check samples.  Each of these QC check samples are
included on Table 11.1.

11.1   Field QC Checks

SERP's  field quality control includes the  collection of a duplicate  sample for each  parameter
analyzed at every sampling location.  In addition, according to FDEP-QA-001/90, one equipment
blank is prepared for every 20 samples.  This blank is  prepared in the field prior to sampling by
pouring or rinsing using analyte-free water on each piece of precleaned field sampling equipment.
Equipment blanks for surface water samples are collected by pouring DIW into a syringe then into a
sample bottle.  For analyses requiring filtration, the equipment blank is prepared by running DIW
through the  filter.  For pore water samples, the equipment blank is prepared by  running DIW
through the peristaltic pump then into sample bottles.  For  soil and sediment samples,  the
equipment blank is prepared by pouring DIW over the sampling equipment and into the appropriate
sample bottles.  All duplicate and blank samples are placed in appropriate bottles and preserved
according to each analysis. The collection of blank  samples are recorded in the field notebook.  For
field equipment cleaned in the field, an additional equipment blank is prepared following the field
cleaning procedures at a frequency of one per sampling event or one every 20 samples, whichever is
greater.  The time and number of all equipment blanks are recorded in the field notebook.

Field instrument checks are  completed prior to each sampling event, once  every  four hours of
operation and at the end of the  field sampling event.  The results of the field QC checks  are
recorded on  the Field Instrument Calibration Sheet (Figure 7.2).  Field equipment not functioning
properly are not used to collect data until they are brought back to the laboratory for maintenance.
Duplicate field equipment and probes are kept on hand in the laboratory if needed.

If problems arise with the Dissolved Oxygen (D.O.) meter, and D.O. is an important parameter of
the specific project, then the field sampling should be discontinued until the D.O. meter is brought
back to  the laboratory for maintenance.  If problems arise with the S/C/T meter, samples can be
collected in clean 125 ml bottles and brought back to the laboratory for  salinity/conductivity
determination within 24 hours. Temperature can be determined in the field with the D.O. meter.
Since the D.O. meter needs to be manually adjusted for salinity, take all D.O. measurements  at a
salinity of 0 ppt, and record this in the field notebook. D.O. measurements are later adjusted to the
sample salinity determined in the laboratory.
                                          11 - 1
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                                                                                                                                                                  Section 11
                                                                                                                                                             Date: 11/25/98
                                                                                                                                                                 Page 2 of 5
Table 11.1
Quality Control Checks
  Type
  Field
  Equipment Blank (non-
  field cleaned equipment)
  Equipment Blank (field
  cleaned equipment)
  Field Duplicate
  Field Measurements

  QC Check Standards



  pH meter
Description
Fill or rinse all pre-cleaned sampling equipment
(tubing, syringes, filter holders, etc.) with analyte-
free water, fill appropriate sample containers and
preserve according to each analysis.
If equipment is cleaned on-site, then prepare
additional equipment blank sample by filling or
rinsing the field-cleaned equipment with analyte-
free water, filling the appropriate sample containers
and preserve according to each analysis.
A duplicate sample collected and analyzed for the
same parameters as the original sample.
Record the results of calibration check standards for
all field measurement equipment.

Record two or more pH readings in field notebook
until sequential values are within 0.02 pH units.
No. of Samples
per event	
1 or more
1 or more
1 or more
Frequency (all parameter groups)
                     1 prepared on-site at the beginning of the sampling event

                     1 prepared on-site at the beginning of the sampling event, and
                     after every 20 samples or 5% whatever is greater
                     1 at the end of the sampling event
                                                                                                    1 after every 20 samples or 5% whatever is greater
Every sample is collected in duplicate
Beginning of each sampling event, once every four hours, and
again at end of the sampling day.

Every sample.
TABLE 11.1 Continued.
                                                                                    11 -2
-------
Quality Control Checks
                                                                                                                                                                   Section 11
                                                                                                                                                              Date:  11/25/98
                                                                                                                                                                  Page 3 of 5
  Type
Description
No. of Samples
per Event
Frequency (All parameters)
  Laboratory
  Method Reagent blank
Analyte-free water: DIW for freshwater samples,
and Gulf Stream  for seawater samples
1 or more
samples
1 at beginning of a run, after every 20 samples, and at the end.
  Replicate Samples
Re-analysis of a sample
1 or more
samples
Every sample is analyzed in replicate.
  Matrix Spikes
One sample from a set (not blanks) is split in two,
and one of the duplicates is spiked with a known
concentration prior to sample preparation.
1 or more
samples
1 sample in a set or at a frequency of 5%, whichever is greater.
  Continuing Calibration
  Standards
One intermediate standard and one high standard.
1 or more
samples
Analyzed at the beginning of each run, and at a frequency of 5%,
thereafter.
  Quality Control Check
  Standards
Standards from an  independent source that  are
certified and traceable (i.e. NIST standards).  Can
be  interchanged  as  one  of  the  continuing
calibration check standard.
1 or more
samples
Analyzed at the beginning of each run to check the initial
calibration of the standard curve.
  Quality Control Check
  Samples
Samples of known analytical concentration that are
submitted blind to the analyst. These samples are
either prepared in house  or obtained  from an
independent source
1 or more
samples
Analyzed in duplicate quarterly.
                                                                                     11 -3
-------
                                                                                Section 11
                                                                            Date: 11/25/98
                                                                               Page 4 of 5
11.2   Laboratory QC Checks

SERP's standard laboratory QC checks includes blanks, replicates, and QC standards and QC check
samples.  Method reagent blanks consisting of analyte-free water (DIW for freshwater samples, and
Sargasso Seawater or Gulf Stream water for seawater samples) are prepared exactly like a sample
and run prior to each instrument calibration, and after every 20 samples.  For the autoanalyzer,
method reagent blanks are run between every sample.

As standard practice SERF collects all field samples in duplicate (see Section 11.1). In addition,
SERF analyzes  all samples in replicate, thereby, producing four data points for one sample location.
 This QA protocol allows for easy identification of unusual sample results, and provides a constant
check of analytical precision and accuracy.

Continuing calibration standards (CCS) consisting of one intermediate standard and  one high
standard  are run at the beginning of each run and at a frequency of 5% thereafter. The  first CCS
should be 90-110 % of expected value and the following ones should fall in a 90-110 % range of
the original CCS.

Quality control check standards are  certified standards from an independent source that are
analyzed at the  beginning of a run to check the calibration of the standard curve. The %  Recovery
(%R) related to the expected  Quality control check standard concentration is calculated and
recorded. The control limits for the  %R are +/- three standard deviations of the historical average  ,
with warning limits set at +/- two  standard deviation of the historical average. New limits (both
control and warning) based on historical data are calculated  on a quarterly basis . These  standards
may be run in the place of one of the continuing calibration standards.

Matrix spikes samples are prepared by splitting a sample  from the set (not a blank) into two
duplicates and spiking one of the duplicates with a  known concentration. The concentration from
the unspiked duplicate is subtracted from the spiked result and the percent recovery by comparing
the remainder to the known spike concentration.  Quality control check samples are prepared in-
house or from an NIST certifying source.  These samples are submitted blind to the analyst on a
quarterly basis to check instrument and user performance. If the blind QC check sample result is
not acceptable, the results will be reported in the QA report to FDEP.

11.3   Routine Method Used to Assess Precision and Accuracy

Precision and accuracy of each analytical parameter determined in the laboratory is determined on  a
daily basis. Precision is defined as the agreement or closeness of two or more results.   As stated
above, SERF collects all field  samples in duplicate, and performs a duplicate analysis on each
sample, thereby, producing four results for one sample location.  SERF determines the mean (X)
and standard deviation (SD) of  these four data points and estimates precision in terms of percent
relative standard deviation (% RSD) using the following equation:

                     %RSD=  SD  * 100
                                 X

                                          11 -4
-------
                                                                                Section 11
                                                                            Date: 11/25/98
                                                                                Page 5 of 5
The control limits for precision are set at +/- two standard deviations of the mean.

The Relative Percent Difference (RPD) is  another parameter used to monitor the precision of our
analytical results  and  it is calculated for Matrix Spike duplicates and/or  sample duplicates. The
acceptance criteria is usually RPD <= 20 %.

Accuracy is  defined as the agreement between the analytical results and the known concentration.
Accuracy is  determined by running matrix spikes  (MS) and/or standard reference materials (SRM)
and is determined as percent recovery (% R) according to the following equations:

                     %R=  Cs-Cu  * 100.
                     MS      S
Where:
         Cs  = concentration of spiked sample
         Cu = concentration in unspiked sample
         S  = expected concentration of spike in sample
        %R = percent recovery
                     % R =  Sample Concentration * 100
                     SRM    True Value
The control limits for accuracy are +/- three standard deviations of the historical percent recovery
average , with warning limits set at +/- two standard deviation.

The results obtained for each quality control check  are compared to their acceptable limits for
precision and accuracy on a daily basis. New limits (both control and warning) based on historical
data are calculated on a quarterly basis .

11.4   Method Detection Limits

Method detection limits (MDLs) have been determined according to the EPA procedure described
in 40 CFR Part  136, Appendix B, revision 1.11.  Specifically, seven or more replicate  samples
containing an analyte at a known low concentration are analyzed according to the appropriate
analytical procedure for that analyte.  A standard deviation for the replicates is determined and the
MDL is computed as 3 times the  standard deviation.  The practical quantitation limit (PQL)  is
defined as 12 times the standard deviation.  MDLs and PQLs are verified/updated once a year.
                                           11 -5
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                                                                                    Section 12
                                                                                Date: 11/25/98
                                                                                   Page 1 of4
12.0   Data Reduction, Validation and Reporting

12.1   Data Reduction

Data reduction is not necessary for field data, as field measurements are read directly from the field
instruments in their appropriate reportable units.  The pH meter, SCT meter, and dissolved oxygen
meter are automatically compensated for temperature.  Salinity read from the SCT meter by the field
technician and then input to the D.O. meter by the field technician, where the D.O. is automatically
corrected for both salinity and temperature.  Each technician is responsible for data entry of field data
from the field notebook into Quattro Pro (Lotus 123 compatible) spreadsheets.

All data reduction is performed according to the protocols specified by the analytical methods listed in
Section 5. Laboratory data  reduction is mainly completed by computers associated with the laboratory
instruments. Calculation of standard curves and sample results in comparison to the standard curves is
determined by the analytical instrument computer.  Analytical runs are recorded in the instrument
computer under the project name and  sampling  event number.  If a sample is outside of the standard
curve, the analytical instrument automatically performs the required dilution, and calculates the sample
result based on the dilution.  If a  sample is suspected of being far beyond the  standard curve, the
laboratory analyst may perform the dilution themselves.  In this case, the laboratory analyst records the
dilution in the instrument log book, as well as on the instrument printout. All instrument printouts are
identified by their project name and sampling event number.   In addition,  any analytical conditions
(i.e. voltage setting, wavelength, flow rate, injection volume, etc.) that deviate from those listed in the
SOP are recorded on the instrument printout and logbook in detail.

Replicate sample results are further reduced to provide one data point per sampling location.  SERF
collects duplicate samples for all analyses at every sampling location. In addition, SERF completes a
duplicate or triplicate analysis of each duplicate sample,  producing at least four  replicate results for
each sampling location. Each of the four data points are input to a Quattro Pro or Excel spreadsheet by
the analyst and the mean and standard deviation of each sample result is calculated.  Any replicate
result that is two standard deviation away from the mean (+ or -) is removed from  the replicate data
set, by crossing out the value on the instrument printout, as well as from the input spreadsheet.

12.2    Data Validation

The Chief Chemist and analytical technicians are responsible for the collection, custody, storage, and
analysis  of  all of the samples.  It is their responsibility that the samples are  analyzed within the
appropriate holding times.   They are also responsible for the proper maintenance of all equipment and
cleaning of laboratory  glassware.  They provide the first check on  field and laboratory instrument
calibration,  method blanks, and equipment blank results, and ensure that all method specifications
have been met.  If problems arise during an analysis, such as failure of proper equipment calibration,  or
unusual sample results, it is their responsibility to verbally notify the laboratory director as  soon  as
possible.

The QA Officer is responsible for a second check of instrument calibration (both  laboratory and field
instruments) by comparing  the present instrument responses to historical values.  In addition, the QA
officer checks the results of method blanks, equipment blanks, and sample replicates and determines
                                                 12- 1
-------
                                                                                    Section 12
                                                                               Date: 11/25/98
                                                                                   Page 2 of4
that the instrument precision and accuracy is within the QA objectives listed in Section  5. Obvious
anomalous results are subject to re-analysis.

Dr. Jones, the director, is responsible for the final review of all data and documents that are submitted
to the client (FDEP; SFWMD). Due to his extensive experience in analytical chemistry, Dr. Jones can
apply both objective and subjective techniques to  data review.  From his knowledge of nutrient
chemistry, Dr. Jones can interpret the data in  its environmental context.  In addition,  through his
collection of historical data in South Florida, Dr. Jones can identify potential outliers in a data set.

12.3   Data Reporting

Once the instrument calibration and sample results  have been validated, they are entered into input
data files. The laboratory technicians  are responsible for providing a first check of data  entry.  Data
reports are prepared in Quattro Pro or Excel  spreadsheets.

When using Quattro Pro, a standard input file is used for data entry of all field and raw laboratory data
(secondary standards, sample results,  and sample replicates).  A second  spreadsheet file performs
calculations for data reduction, such as determination of replicate means and standard deviations, and
conversion of sample results into reportable units of interest (i.e. moles/1,  mg/1, ppm,  etc.).   A third
spreadsheet file is then produced as output from the second  spreadsheet and is the final data report in a
client (FDEP; SFWMD) requested format.

The Excel workbooks consist of three sheets:  one for the data input, a second one where raw data is
filtered eliminating those individual values that are outside the mean +/- 2 SD acceptance  range, and a
third one where the  final printout steps  are performed. The second sheet contains two Visual Basic
macros that perform all the calculations, unit conversions and format adjustments needed for the data
report, producing the final report printouts that are sent to the customer.

For data reports issued to the client for DEP-related work, or for reports issued directly  to DEP, the
following information will be included:

       a.      Laboratory name, address, and phone number
       b.      Client name and/or site name
       c.      CompQAP number
       d.      Client or field identification number
       e.      S ampl e i dentifi cati on numb er
       f      Method number of each analysis
       g.      Analytical result with applicable data qualifiers
       h.      Date of sample preparation
       i.      Time of sample preparation if holding time is in hours
       j.      Date of sample analysis
       k.      Date and time of sample collection
       1.      Identification of all laboratories providing analytical results, including their CompQAP
              number

The  QA officer provides a second check of the input data, spreadsheet calculations, and output file
                                                  12-2
-------
                                                                                    Section 12
                                                                                Date:  11/25/98
                                                                                   Page 3 of4
formats.  Once all of the data has been validated, the QA officer will provide a written statement of
validation along with the data report. An example of a final data report form is included as Figure
12.1.

12.4   Data Storage

Data input files and final report files are stored on hard drive and write-protected floppy disks  using
names that readily identify a  sampling event. Files labeled by sampling event are stored in a locked
file cabinet with limited access by SERF employees only.  These files contain hard copies of the file
input and output as well as all raw laboratory data sheets and field notebook sheets.  Raw laboratory
output data sheets are  identified with a date, analysis, analyst initials, and sampling event number.
SERF plans to maintain all records indefinitely, but will at minimum comply with the Chapter 62-160
F.A.C. requirement of 3 years.
                                                  12-3
-------
Figure 12.1
Final Data Report

Southeast Environmental Research Program
Florida International University OE 148
Miami, Florida 33199
Phone: (305) 348-3095
                                                                                    Section 12
                                                                                Date: 11/25/98
                                                                                   Page 4 of4
                                 Client Name:_
                                 Site Name:	
                                 CompQAP #:_
                                 Project Code:
Sample ID






















Field No.






















Station
Code






















FQC
Code






















Sampling
Date






















Time






















Sampling
Depth (m)






















Parameter/
SOP#






















Store!
Code






















Method
Name






















Sample Prep
Date






















Time






















Sample Analysis
Date






















Time






















PQL






















MDL























Result

Unit






















Remark






















   Other Laboratories providing analytical results:
   Lab :	       CompQAP # :
                                 Analyses:
   Lab:
CompQAP #:
Analyses:
   Lab:
CompQAP #:
Analyses:
                                                    12-4
-------
                                                                                  Section 13
                                                                              Date: 11/25/98
                                                                                 Page 1 of 3
13.0   Corrective Action

Corrective action is taken whenever the  quality assurance objectives have not been met.   A
summary  of the corrective actions for the laboratory and for the field are included in Tables 13.2
and 13.3, respectively.

The analyst, either the Chief Chemist or the technicians, are responsible for providing a first check
for compliance, and initiating corrective action procedures as described in Table  13.1. The QA
officer is responsible  for a  second check for compliance, and initiating  corrective action  as
appropriate.  If problems continue, then the analyst and/or  QA officer will notify the laboratory
director immediately, who may initiate further steps in solving the problem.

Any corrective action taken will  be documented  in the instrument log books, sample reanalysis
sheets, and/or sample checklist within the project-specific files.

FDEP recommended corrective action will be initiated as a result of systems or performance audits,
split samples, or data validation review.
                                           13- 1
-------
                                                                                            Section 13
                                                                                        Date: 11/25/98
                                                                                           Page 2 of 3
TABLE 13.1
Corrective Actions for the Laboratory
  QC Activity
Acceptance Criteria
Recommended Corrective
Action
  Initial Instrument Blank
Instrument response 0.995
Reanalyze standards, if same
response, reoptimize instrument, if
same response, prepare new
standards, notify Dr. Jones and
QA Officer
  QC Check
  Continuing Calibration Standards
Historical average +/- 3 SD
90-110 % from initial calibration
Reanalyze check standard, if same
response, prepare new check
standard, if same response,
prepare new primary and
calibration standards, notify Dr.
Jones and QA Officer.
  Matrix Spikes
Historical average +/- 3 SD
Reanalyze matrix spike, if same
response, prepare and run new
matrix spike, is same response,
notify Dr. Jones and QA Officer.
  Replicate Sample
RPD < 20 %
Determine cause: baseline drift,
carryover, etc. Reanalyze all
samples between duplicates,
notify Dr. Jones and QA Officer.
  Duplicate Sample
RPD < 20 %
Reanalyze duplicates, reanalyze
all samples between duplicates;
notify Dr. Jones and QA Officer
                                                 13-2
-------
TABLE 13.2
Corrective Actions for the Field
                                                                                             Section 13
                                                                                         Date: 11/25/98
                                                                                            Page 3 of 3
  QC Activity
Acceptance Criteria
Recommended Corrective
Action
  Initial Calibration Standards
Value within +/- 5% of expected
value
Reanalyze standards, if same
response, optimize instrument, if
same response, use new standards;
notify
Dr. Jones and QA Officer.
  QC Check Standards
Value within +/- 3 standard
deviations of the historical value
Reanalyze QC check standard, if
same response, prepare new QC
check standard, if same response,
recalibrate; notify
Dr. Jones and QA Officer.
  Equipment/Trip Blank
Value 
-------
                                                                                Section 14
                                                                            Date: 11/25/98
                                                                               Page 1 of 5
14.0   Performance and System Audits

Dr. Jones supervises all aspects of field and laboratory activities. He requires the laboratory and all
instrumentation to be clean and working at optimum conditions.  He is knowledgeable on the inner-
workings of each instrument and checks on their performance as well as on the performance of the
laboratory personnel continually.

14.1   Field Audits

An internal system audit is conducted on an annual basis by the QA officer. During these audits,
the QA officer will review and evaluate the various components of the measurement system  to
determine their proper selection and use. Specifically, the auditor will review  sampling technique,
field instrument calibration, and field notebook documentation.  The checklist included as Figure
14.1 will be used during the audit, and any discrepancies or deviations will be noted in the checklist
and corrected immediately.  At the end of the audit, the QA officer will date and sign the checklist
stating that the audit was completed, and a copy of the checklist will be put in the project-specific
files.

14.2   Laboratory Audits

Internal laboratory system audits are conducted on a semiannual basis by the QA officer. This audit
is  conducted with the use of the checklist included as Figure 14.2. In addition to these audits,
instrument performance is checked continually by the analyst with analysis  of standard curves,
sample replicates, method blanks, and equipment blanks. The QA officer checks the instrument log
books  on  a monthly basis to check that  instruments are  running within  their appropriate QA
objectives.   Many of the analyses are performed and  checked within 24 hours to seven  days  of
sample collection, allowing for any deficiencies to be corrected and samples re-analyzed if needed.
Documentation associated with each audit including the  checklist,  calculation checks  of standard
curves, sample replicates, equipment blanks, spikes, and QA check samples and standards are kept
in  the QA officer notebook.

Laboratory performance audits are conducted on a quarterly basis. The performance audit  consists
of at least two of the following samples:

• blind samples prepared by the QA Officer
• split samples with another laboratory
• QC samples from an independent certifying source (NIST)
• blind spike samples

Currently, SERF is not involved in a regular external audit program; however, we are available  to
receive on-site audits by FDEP at any time.
                                          14- 1
-------
Figure 14.1 Field Audit Checklist
       Auditor:
                                                                            Section 14
                                                                        Date: 11/25/98
                                                                           Page 2 of 5
Field Audit Checklist
                Date of Audit:
Y










Y









N










N









Sample Collection
* Sampling equipment & bottles rinsed 3 times before
samole collected.
* Samples collected near the bow of the boat away from
the engine.
* Samples collected for dissolved constituents are filtered.
* Filter is sparged with at least 30 ml of air prior to
removal from filter holder.
*Filters are placed in microcentrifuge tube and acetone is
added to the too line of the tube.
* Microcentrifuge tubes are stored in the dark in a cooler
with ice.
* Dissolved nutrient bottles kept in a cooler with ice.
* Total nutrient bottles stored in the dark in a cooler
without ice.
* The appropriate number of QC samples are collected at
the aDDrooriate times.
* Samples are collected at the correct project locations.
Field Notebook
The following are recorded in the field notebook:
* Names of the field crew
*Weather conditions
* Time of sample collection
* Time of QC sample collection
*Temperature, Salinity, D.O.
* Volume of water filtered
*Date
* Station names
Comments










Comments









                                        14-2
-------
Figure 14.1 Field Audit Checklist (Continued)
       Auditor:
Field Audit Checklist  (cont.)
                    Date of Audit:
                                                                             Section 14
                                                                         Date: 11/25/98
                                                                            Page 3 of 5
Y








Y

N








N

Field Instruments
* Meter number and probe number recorded on the field
instrument sheet.
* The D.O. meter is turned on at least 50 minutes prior to
first reading.
* Slope of the D.O. meter is checked with the sleave on and
the results are recorded.
* Salinity/Conductivity meter checked against Sal/Cond.
Standard with results recorded.
* Instrument calibration is checked at the beginning of the
dav. 4 hours later, and at the end of the dav.
* Spare instruments are available in the field.
* D.O. meter repair kit is available in the field.
* Temperature checked against NIST thermometer.
Other
* Main office (and NFS Dispatch) is notified before and
after samolins trio bv ohone or radio.
Comments








Comments

                                         14-3
-------
Figure 14.2 Laboratory Audit Checklist
                              Laboratory Audit Checklist
       Auditor:                                  Date of Audit:
                                                                           Section 14
                                                                       Date: 11/25/98
                                                                          Page 4 of 5
Y










Y




Y






N










N




N






Instrument Response
* Instrument notebook is up to date.
* High standard within 10 % of expected value.
* Calibration curve correlation coefficient better than
OQQ5
* Instrument blank is less than MDL.
* QC check standard within control limits.
* Matrix Spike samples within control limits.
* Replicate samples show RPD < 20%
* Duplicate samples show RPD < 20%
* Instrument maintenance up to date.
* Equipment Blank samples less than MDL.
Sample Tracking
* Sample Checklist is filled out correctly.
* Samples are kept in proper storage
* Samples are analyzed within holding times.
* Samples are not discarded until QA checked.
Labware
* Reagents are stored appropriately.
* Waste is disposed properly.
* Glassware and bottles are cleaned appropriately.
* Check the age of sample bottles.
* Standards are properly labeled and stored appropriately.
* Check dates of standards.
Comments










Comments




Comments






                                        14-4
-------
Figure 14.2 Laboratory Audit Checklist (Continued)
                                                                            Section 14
                                                                        Date: 11/25/98
                                                                           Page 5 of 5
       Auditor:
Laboratory Audit Checklist (cont.)
                       Date of Audit:
Y






N






Data Management
* Project Files up to date.
* Data input up to date and correct.
* Calculations performed correctly.
* Output files in correct format.
* Data values within 2 standard deviations of historical
mean.
* Data reports up to date.
Comments






                                        14-5
-------
                                                                                Section 15
                                                                            Date: 11/25/98
                                                                                Page 1 of 1
15.0   Quality Assurance Reports
SERF will submit quality assurance reports for all Quality Assurance Project Plans at a frequency
according to Table V of Appendix D of the QA Manual.  The Quality  Assurance Officer is
responsible for the preparation of these reports. In general, if no audits were performed and no
significant QA/QC problems have been identified, then SERF will prepare a brief letter stating
these facts in lieu of a detailed quality assurance report.

A detailed QA report will be prepared when:

       1.      Activities were conducted in a manner other than those described by the CompQap
              or QAPP.
       2.      Preservation or holding requirements were not met.
       3.      Quality control checks were unacceptable.
       4.      Precision, accuracy, or MDL objectives were not met.
       5.      Corrective action was taken.
       6.      Internal or external audits were conducted and discrepancies were noted.

According to FDEP guidelines, these QA reports will include the following:

       1.      Title Page including the time period of the report, the QA Project Plan Title and
              Plan number, the laboratory name, address and phone number, and the preparer's
              name  and signature.
       2.      Table of contents if the report is over 10 pages long.
       3.      The results of performance or system audits to include, date of audit, system tested,
              name  of auditor, parameters analyzed, results of tests, deficiencies or failures, and
              an explanation of the problem and the corrective action taken.
       4.      Significant QA/QC problems.
       5.      Corrective actions taken.
                                           15- 1
-------
                            APPENDIX A
       validation  for Miaraolar Concentration* of  Xetel tfitrog«a
                         in  Natural  Waters

                   Limited Us* Method Validation
                       'Prepared by and for:

             Southeast Environmental Raaiearchi Program
                 Florida International University
                              OE 14S
                         University Park
                       Miami, Florida 331S9
                          (305) 348-3095
                        PJUC: (305)348-4096
RSnaM 0, JQIWS,
SERP Director and
Professor
                                                           />"f
Rene* H. Price, P.O.
SBRP Qyality Assurance Officer
FDEP QJi Officer
-------
                                                        Appendix &
                                                        Revision 0
                                                    Date:  04/25/94
                                                      Page 2  of 18
1.0  scope and Application

This method covers the determination of total nitrogen in fresh and
saline surface waters.   The method ia capable of  measuring  total
nitrogen at concentrations  between 2.1 jjaol/1 (0.03 mg/l» to 2 SO
Mfflol/1  (3,500 jig/1)  at  an  precision of  5%  relative  standard
deviation (%RDS)  or better,  and an accuracy between 91  and  1051.
The method is  also  applicable for analysis o£ dissolved nitrogen of.
filtered water samples.

2.0  Summary of Method

The procedure is  a  modification  of  the olaMical Duma*  (1831)
method of determining nitrogen by conbuatlon technique with the
addition of cheni luminescence .  The method Involves converting all
forms of  nitrogen into  nitric oxide  (HO>  upon  combustion  of  a
sanple with oscygen at a temperature in  excess  of 100O"C.  The HO ia
reacted with  ozone  (O,J  to fom  a matastmble form of  nitrogen
diojelde (NCk"! . A«  the mwtaatable form  of  nitrogen dloauda decays,
a quanta of light is  emitted in an amount  directly proportional to
the amount of  nitrogen  in  the  sample,    Thm chemi luminescent
emission  is  detected  by a photonultiplier  tuba  at  a  specific
wavelength.
     R-H * 0, ~ — '">  Ho  *
     NO 4> Oy — ' — > MO," «• QS — — >

An WITEK Instruments, Inc.  Model 7000M nitrogen  toalyzer  (Figure
A-l}  is used  to determine  total nitrogen of  Sjil of *  preserves!
watar sample.  The instrument is run according to tfaa Installation/
Operation/ Service Manual provided by  AMTEK  Insteuments,  Inc.r
exctpt that Oseygen gas is used  as a carrier gas instead of Argon to
proaota complete recovery  of  the  nitrogen  in the water samples,
Total nitrogen  is determined  on unfiltered samples, while  total
dissolved  nitrogen  is  determined  on   filtered  samples.     .An
autoaanpler is used to  inject  the  samples into the analyzer.

3.i  interferences

There are no known interferences  with this procedure as long as all
olassware ia cleaned  properly,  and  deionlxed water (DPI)  is used to
naka the standards.  The emission wavelength is completely specific
for  nitrogen,  therefore,  there is no   interference  with  other
compounds.  In  addition, the  method is  specific for  chemically
bound  nitrogen  and  does  not detect  dinitrogen  (H) .    Matrix
interferences are eliminated by  analyzing only water samples.

Care must be  taken  not to  contaminate samples  or  laboratory
glassware.   Given  the small  si^e of   the  autoanalyzer  vials,
-------
                                                        Appendix A
                                                        Revision 0
                                                    Data: 04/25/94
                                                           3 of 18
 cleaning Is  not:  practical,  therefore,  autoanalyzar  vials  are
 obtained clean  directly from the  manufacturer,  used once,  then
 discarded.  All  laboratory glassware used for standard preparation
 are  washed  with hot  tap water and liquinox, rinsed with  hot tap
 water,  rinsed with hydrochloric  acid,  then  triple rinsed  vith
 analyte-free  water.  The Inside of all glassware,  sample bottles,
 autoanalyzer  vials or the autoanalyzer injection needle should not
 be touched  since  human  contact  can contaminate tne samples  with
 nitrogen.

 4.0  safety Precautions

 In general, this method  is environmentally safe.  Strong chemicals
 or acids are  not used, and no  hazardous wastes are produced.   The
 use of fume hoods  or protective clothing Is not required.  Care is
 advised during handling  of the high pressure gases as  well as the
 pyrotech tube.   All gas  lines, regulators,  gas filters,  etc,  need
 to be specified for high pressure  oxygen  gas.  In addition,  the
 pyrotech tube operates at combust ion temperatures of over 1000*cr
 and  care should  be  taken  during  maintenance to avoid  serious
 thermal burns.

 5.0  Apparatus JUid Materials

 An ANTEK Instruments, Inc. Model  7000M Nitrogen Analyzer equipped
 with the following:
     Autosampler
     Qiemi luminescent nitrogen Detector
     Gas/Liquid Inlet System
     Pyro Tech, Furnace and accessories
     Printer
     Oxygen Supply regulated to 20  psig

 Standard laboratory glassware is used for preparation of standards.
 Glass vials, l.S^j:, with teflon/silicon septa crimp seals are  used
 for the aiatoanalyier,                                           . ^

 ft.fi  Reagents

 leagents are United to primary standards,  secondary standards, and
 hydrochloric  acid   (used as  a preservative}.   All standards  are
 prepared with DIW.

 6.1  primary standards

 Primary standards  are made  by dissolving  0.3612  g  of  anhydrous
 Potassium nitrate  (KNO,)  In 100 ml  of  DIW in a volumetric  flask,
This  primary  standard has a nitrogen  concentration  of  500 mg/1.
 Preserve with 1 ml of  chloroform and store at room temperature for
 no more than one year.
-------
                                                        Appendix A
                                                        Revision 0
                                                    Data: 04/25/94
                                                      Page 4 Of 18
 6.2   Secondary Standards

 Using microliter  pipeta, add  the  required  volumes of  primary
 standard  Into 100 »1  flasks and dilute to  the »arJt with  DIW to
 produce the following  secondary  standards:
 Volume of  Primary Standard
 added fco l^Q «1  flask
Concentration of II in
Secondarv Standard
     0
     100
     200
     400
     1000
0 mg/1
0.5 ng/1
1.0 ng/1
2.0 119/1
9.0 ng/1
CO jCMOl/1)
(3S.7 jiaol/1)
(71.4 JMOl/1)
(1+2.9 Mfflol/1)
(357.1 jiaol/1)
These secondary standards are used to check instrument calibration
on an annual basis or upon replacement of  the pyrolysis tub®.

i.3  Working and Continuing Calibration Standard*

A  working standard  of  2.0  ng/1  (described  above)  is  prepared
identical to  samples.   Specifically, 1.5  ml of this  standard  is
placed Into a glass autoanalyrer sample vial and acidified with lo
Ml of  3  H  HCl.   Duplicate vials of tills standard  are run  in
triplicate prior to  each run,  after every 20  samples,  and at  the
and of the run to check  instrument calibration.

6.4  Hydrochloric Acid

ACS reagent grade 3 Iff 1C1 is  Bade by adding 125 ml  of concentrated
12 If HCl into a 500 ml flask and diluting  to the mark with DIW.

7.0  calibration

Low level calibration curves  have been performed in triplicate  for
both freshwater and soawater and yield the following results;

Low Level Calibration
flX
Cone en tra t ions
0
0.5
1.0
2.0
5.0
Instrument Counts
Freshwater
204, 193, 199
1002, 993, 974
2304, 2403, 2311
4686, 4688, 4803
10101, 10591, 10181

Instrument Counts
Seavetsr
1003, 987, 1003
2113, 1987, 2223
3034, 3081, 3003
5396, 5383, 5203
11201. 11903, 11514
-------
                                                        Appendix &
                                                        Rev la ion 0
                                                    Data: 04/25/94
                                                      Page 5 of IS
 Low  level   linear  calibration  curves  determined  by  plotting
 instrument  response count  against  standard  concentration  are
 Illustrated on  Figure A-2.  Mote that the slopes of the curves for
 frisnwater and  seawater are  similar with correlation coefficients
 of greater than 0.99.

 Rlgti  level  calibration curves prepared in  triplicate for  both
 freshwater and  seawater yield the following results:

 Hiati Level Calibration
|tM
Cone «n t r a t ions
0
25
50
100
125
150
200
Inatrua*nt Count*
Freshwater
794,656,600
45808,48213,48218
99403, §3619,96219
192390, 190000, 187230
239200,248870,233380
287070,297870,291080
389000,315330,382110
Instrument Count*
Seawater
715tS82»701
47541,46822,47849
94880,97103,96847
186458, 188999,
190506
238024, 242743,
241527
293001, 290901,
292006
380841, 387848,
387095
High, level linear calibration carves are illustrated on Figure A-3
and indicate identical  elopes  (5.17 X IO*)  for both. matrices with
correlation coefficients  of  0.9999.

Liimarity of  instrument response only  needs to be checked  on an
animal basis or whenever the pyrolysis tube is replaced.  Once the
instrument  calibration i« determined  to  be linear  (regressioir
coefffficient >0.91Jf then only a one-point instrument calibration is
required on a dally basis. The ABTEK instrument i* programmed such
that m zero nitrogen concentration produces an instrument response
of sera.  The one-point calibration curve  is obtained with a high
working standard, usually 2.0 mgir/1 (143 jiM M).  Prior to each run,
duplicate vials of  this standard are run  in triplicate.   Hie Bean
and standard deviation  of the siac results  are determined.   If the
precision of  these results is less  than  5 tESO, then  a standard
curre is  determined by using  the mean of the high  standard and
forcing the intercept through zero.
-------
                                                        Appendix A
                                                        Revision 0
                                                    Date: 04/25/94
                                                      Pago 6 of 18
 8.0  Quality control

 t.l  Calibration Check Standards

 Calibration  check standards are run  at the beginning  ami end of
 each  run,  with  each run consisting of  no  more than  20 samples.
 Calculate  accuracy and determine It to be within 95  to 105%.   If
 results fall outside thin acceptable range, then all samples within
 the run must  be  analyzed again.

 •.2 Duplicate and aaplleata Analyses

 Every sample  is  collected in duplicate  and  analyzed lit triplicate
 to  produce six results  for each sample.   Triplicate  analysis is
 recommended given the snail injection volume (5 |tl)  as veil as the
 possibility of injacting an air bubble Into the instrument,  A Bean
 and standard deviation of the six replicate  results  Is determined,
 and any replicate  result determined  to  be  beyond  1  standard
 deviation  away from  the  mean Is  discarded.  A  sample precision of
 5  tESD  Is  considered acceptable.     Values  outside this  range
 results in a  re-analysis of the  samples.

 9.0  Sample Collection,  Preservation, and Eaadliag

 Surface water samples are collected  directly  Into  clean,  120 ml
 plastic sample  containers.   Prior to  sample  collection,  sample
 containers are triple-rinsed with  the sample water.   Samples  are
 stored in  the dark: until delivery  to the laboratory,   within 12
 hours of sample collection, 1.5 ml of sample is placed into a glass
 autoanalyzer sample vial and acidified with 10  pi of 3 H HC1.  the
 vial is  sealed with a teflon/silicon lined crimp cap and, stored in
 a refrigerator  at  2*C until  analyzed.    Mien preserved by  this
 method,   samples  have  a  shelf  life  of  three months  without
deterioration;  however,   sample  analysis   within  28   days   is
recommended.

 1§. 0 Sample BJE tract ion/Preparation

Other than th« preservation procedures dmscrJJbad above,  there  are
no sample  extraction or  preparation procedures.

11.0 Sample Cleanup and  Separation

There are  no additional sample cleanup or  separation  protocol
necessary   to  separate  the nitrogen  from the sample  matrix.
Combustion of the sample  and its reaction with ozone Is completed
by the ANTEK Instruments, Inc. Model 7000M nitrogen Analyzer.
-------
                                                        Appendix A
                                                        Revision 0
                                                    Date: 04/25/94
                                                      Page 7 of IS
 12.9  Sample Analysis

 The JUfTEK  Instruments,  Inc.  Model  7QQQW  Nitrogen  Analyzer  is
 generally operated at the following conditions:

 Pyralysis Temperature         1100*C
 Pyrolysis Oxygen  flows         2,0 psig
 Oxygen to ozone flow:          2.0 psig
 System Pressure:               1.0 psig
 Vaeayn:                        25 in/Eg,
 PUT Voltage:             •      800
 Gain:                          X50 HI
 Sample volume:                 5  jil

 Using pipets,  2  al of  sample  is put into autoanalyzer vials and
 capped.  The  first two  vial*  consist of the blank  wat«r that is
 used  to rinse the  Instrument.    The  next  two  vials  are  high
 standards followed by a vial of blank water.   Samples are loaded
 into the following vials separated by vials containing blanks to
 rinse the  injection  system between samples.   The autoanalyzer
 collects  §j*l  from each sample  vial  and  injects  it  into  the
 instrument.  The  instrument is programmed to perform a triplicate
 analysis of each sample.  A calibration check standard is analyzed
 at  the end of every run,  which does not  exceed 20 samples.

 13.1 Calculations

 Mo  special  calculations are  required.    Instrument  peak height
 values  ars  converted  directly  to  sample   concentrations  by
 comparison to the standard curve.  Method precision, accuracy, and
 detiction limit are determined  according  to the equations presented
 in Section 11.  An eaeanple  of  the instrument raw data is attached
 along  with  determination  of  precision,,  accuracy,  and  method
 detection limit for that run.

 14 .§ Confirmation

 Confirmation of  tha presence  of nitrogen In  each  sample can  be
 confirmed by performing Total Kjeldhal nitrogen method plus nitrate
 or toy 0V persulfat* digestion.

 15.1 Method Performance

This method  measures  total nitrogen  of fresh  and  saline water
sanpl«s at concentrations between  2.1 pmol/1  {0.03  ag/1)  to 250
pmol/1  (3,300 pg/1)   at a precision   of  5%  relative  standard
deviation (%raJJ§)   or batter, and an accuracy between 35 and 1051.
There are no interferences with this method.  In addition, there is
no required sample extraction  procedure  and  sample preparation is
minimal.
-------
figur* &-1,
                            Appendix ...
                            lavision o
                         Date; 04/15/94
                             • of is
Flow Diagram Antek Nitrogen System

trogen                -         Ve"'
lector
         Membran
— —  —  -« Dryer
             Reaction
             Chamber
                     Pyrotube
    _ Z^T  _ _ — J
                                  Flowmeter
-------
Figur* A-a
     Calibration Data (High  Level)
                 Freshwater & Seawater
        Revision 0
    Data; 04/25/94
      Pmqm 9 of is
                                         ASeawater:
                                         correlation coefficient:
                                          r=0,9999
                                         slope:
                                          m =5.1787x10-4
                                         y-intercept:
                                          b=3,0418x10-1

                                         •Freshwater:
                                         correlation coefficient:
                                          r=0.9999
                                         slope:
                                         y-intercept:
 0        100,000

          .. „„   Counts
  ii            e
INSTRUMENTS
-------
-1
                                                     Appendix I
                                                     Revision 0
                                                 D»t«i  04/25/94
       Calibration Data  (Low Level)
                   Freshwater & Seawater
                                                      10 of
                                          ASeawater:
                                           correlation coefficient;
                                            r=0,9988
                                           slope:
                                            m= 4,7401
                                           y-intercept:
                                         •Freshwater:
                                          correlation coefficient
                                           r=0.iS80
                                          elope:
                                           m =4.8840 X10'4
                                          y-intercept:
 0  1,000 2,000 3,000 4|MO 5,000 i.OOQ 7.0M 8,000 S.OJO 10,00011,000
                   Counts

-------
I
                       Appendix  A
                       Revision  0
                    Date:  04/25/94
                     Page  11 of 18
       Table A-l-
       Instrument Raw Data

       High Standard
Height
32806S
126476
315434
307124
307802
I Coaf . s
sample
Me.
18
18
18
18
18
18
19
19
If
19
IS
19
20
20
20
20
20
20
21
21
21
21
21
21
22
22
22
22
22
22
Mean
316981




6.31E-06
VMfc
H.ight
68059
73595
76348
72947
53989
S6782
63046

631S1
58140
56652
69S79
101584
88086
93045
S3§43
103294
88642
143391
129645
§7297
146675
143873
124534
143131
126648
129014
124290
122970
117537
                           fl.D.
                           S961
                             Cone.
                              0.43
                              0.46
                              0.48
                              0,46
                              0.34
                              0.36

                              0.40

                              0.40
                              0.37
                              0-36
                              0.44

                              0.64
                              0.56
                              0.59
                              0.59
                              0.65
                              0.56

                              0.90
                              O.S2
                              0.55
                              0.93
                              0.91
                              0.79

                              0.90
                              0.80
                              o.ai
                              0.78
                              0.78
                              0.74
                                       M«an
0.46
0.06
0.39
0.03
0.59
0.04
0.80
0.14
0.83
0.05
-------
                                                        Appendix &
                                                        Revision O
                                                    Date:  04/11/94
                                                     Page  12 of 18
T»ULm  ft-l  Continued.
Instrument Raw Data
Sanplc
Mo.
23
23
23
13
23
23
24
24
24
24
24
24
35
25
25
25
25
25
26
26
26
26
26
26
27
17
27
27
2?
27
28
18
28
28
28
28
peak Cone.
Height
113338
97275
109933
114808
85867
109311
10316S
101434
89431
98077
94929
95829
5149S
50899
48765
46430
48899
51564
5189$
54313
50917
56950
53244
S5425
3755?
36379
36302
36827
38671
126059
64364
60120
56844
62889
60725
52691
•9/1
0.72
0.61
0.69
0.72
0.54
0.69
0.65
0.64
0.56
0.62
0.60
0.60
0.32
0.32
0.31
0.29
0.31
0.33
0.33
0.34
0.32
0.36
0.34
0.35
0.24
0.23
0,23
0.23
0.24
0.80
0.41
0.38
0.36
0.40
0.38
0.33
                                M»mm
s.a.
                                0.69
                                0.62
                                0.31
                                0,34
                                0.23
0,07
0.03
0.01
0.01
0.23
                                0.39
0.03
-------
                                                        Appendix &
                                                        Revision 0
                                                    Data:  04/25/94
                                                     Page  13 of IS
Table 1-1 Continuad.
Lastrujient law Data
Samp la
Wo.
29
29
29
29
39
29
30
30
30
30
30
30
31
11
31
31
31
31
32
31
32
32
32
32
33
33
33
33
33
33
34
34
34
34
34
34
Male
B*igbt
97467
95358
9414S
94593
89004
96449
113388
120673
105595
§7972
113795
115067
161965
199033
171121
164179
173619
170957
142926
138120
130054
136164
131559
129145
159314
144694
168716
179937
186718
165233
150115
1599S5
153592
145461
154167
157292
Cone.
»f/l
o.ii
0.60
0.59
0.60
0.56
0.61
0,72
0.76
0.17
0.56
0.72
0.73
1,02
1.26
1.11
1.04
1.10
l.OS
0.90
0.87
0.83
0.86
0.77
0,81
1.01
0.91
1.06
1.14
1.13
1,04
0.95
1.01
0.97
0.92
0,97
0.99
                                H«an
8.D.
                                0.60
0.02
                                0.67
0.07
                                1.11
0.08
                                0.86
o.os
                                1.03
0.09
                                0.96
0.03
-------
                                                        Appendix A
                                                        Revision 0
                                                    Data:  04/25/94
                                                     Page  14  of 18
Tab la  A-l  Continued.
           law Data
 Continuing  Calibration
 Chide    Standards
    V*aJt      Cone.
    Height    «g/l
   130196      2.09
   111059      1.96
   124867      2,OS
   J15S23      1.99
   329304      2.08
-------
I
                  Appendix &
                  Revision 0
              Data: 04/25/94
               Page 15 of 18
       Tibia A~2.
       tuple and QC caloulationa

        High atandmrd
Peak
bight
328068
326476
315434
307124
307802
Corf * of
Sample
NO.
18
18
18
18
18
18
19
19
19
19
19
19
20
20
20
20
20
20
21
21
21
21
21
21

Mean
316981




6.31E-06
P«aJc
Height
68059
73i§5
76348
72947


63046

63181
58140
56652


88086
9304S
93943

88642
143391
12964S

146675
143873


fl.D.
9961





Cone.
•g/1
0.43
0.46
0.48
0.46


0,40

0.40
0.37
0.36


0.16
0.59
0.59

0.56
0.90
0.82

0.93
0.91

Continuing Calibration
ChacJc    standards
Pea*
Height
330896
311059
324867
315522
329304
Cone.
•9/1
2.09
1.96
2.05
1.99
2.08

Accuracy
104
98
102
100
104
                                       Mean
    8.D. Precision
                                       0.46
    0.02
                                       0.39
    0.02
                                       0.58
    0.02
                                       0.88
    0.05
-------
                                                       Appendix A
                                                       Revision 0
                                                   Date:  04/25/94
                                                    Page  16 of 18
TiM* A-2.
Sanpl* and  QC Calculations
sample
Ho.
22
22
22
22
22
22
23
23
23
23
23
23
24
24
24
24
24
24
25
25
25
25
25
25
26
26
26
26
26
26
27
27
27
27
27
27
Peak
Haight

126648
129014
124290
122970
117537
113338

109933
114808

109311
103 168
101434

91077
94929
95829
51495
50899
48765
46430
48899
51564
51896
54313
50917
56950
53244
55425
37557
36379
36302
36827
38611

Cone.
•g/1

0.80
0*81
0.7S
0.7§
0.74
0.72

0.69
0.72

0.69
0.65
0.64

O.S2
0,60
0.60
0.32
0.32
0.31
0.29
0.31
0.33
6.33
0.34
0*32
0.36
0.34
0.35
0.24
0,23
0.23
0.23
0.34

                               Jtoaa
3.D. Pracision
                               0.80
0.03
                               0.71
0.02
                               0.64
0.02
                               0.31
0.01
                               0.34
0.01
                               0.23
0.01
-------
I
              Appendix &
              Revision 0
          Data:  04/25/94
           Page 17 of IS
       aupl*  and QC  Calculations
sup 1*
No.
28
28
28
28
28
28
29
29
29
29
29
29
30
30
30
30
30
30
31
31
31
31
31
31
32
32
32
32
32
32
33
33
33
33
33
33
!•«* Cone*
Height mg/1
64364
60120
56B44
62889
60725

97467
953SS
9414S
94593
89004
96449
113388
120673
105595

113795
115067
161965

175726
164179
173689
170957
142926
138120
130854
136164

129145
159314

168716


165232
0.41
0.38
0.36
0.40
0.38

0.61
0.60
0.59
O.iO
0.56
0.61
0.72
0.76
0.67

0.72
0,73
1.02

1.11
1,04
1.10
1.08
0.90
0.87
0.83
0,86

0.81
1.01

1.06


1.04
                                       Mean
B.D. Precision
                                       0.39
                                       0.60
                                       0.71
                                       1.06
                                       0.86
                                       1.03
0.02
0.02
0.03
0,04
0.04
0.03
-------
.
m
                                                       Appendix A,
                                                       Revision 0
                                                   Date; 04/25/94
                                                    Page IS of IS
Iftbla A-I.
Suple  and  QC calculations
   Bajnpl«      l**k    Cone,
     Me.   Might    •g/l      M«u     i.D.  lr«ei«ie»
       34   150819    i.SS
       34   159985    1.01
       34   153592    0.97
       34   145461    0.92
       34   154 1S7    Q.§7
       34   157292    0,99      0,§6     0.03         3
       P«t«atiott bimit  for  th« rm «*tttBia^ w tto «npl« with
 lowest concentration.

           FeaJt     Come*
           Might    ag/1      lto«m     ••»•      «» (1*«.D.)
      27     37S57    0.24
      27     3«379    0-23
      27     3«302    o.aa
      27     36827    0,23
      27     3§i7l    0.24
      27                        0.23     0.01      0.03
-------
                                                                                 Section 15
                                                                            Date: 11/25/98
                                                                                Page 1 of 1
15.0   Quality Assurance Reports
SERF rail submit quality assurance reports  for all Quality Assurance Project Plans at a frequency
according to Table V of Appendix D of the QA Manual. The Quality Assurance Officer is responsible
for the preparation of these reports. In general, if no audits were performed and no significant QA/QC
problems have been identified, then SERF will prepare a brief letter stating these facts in lieu of a
details! quality assurance report,

A detailed QA report will be prepared when:

       1.      Activities were conducted in a manner other than those described by the CompQap or
              QAPP
       2,      Preservation or holding requirements were not met.
       3.      Quality control checks were unacceptable,
       4.      Precision, accuracy., or MDL objectives were not met.
       5.      Corrective action was taken.
       6,      Internal or external audits were conducted and discrepancies were noted.

According to FDEP guidelines, these QA .reports will include the following:

       1.      Title Page including the time period of the report., the QA Project Plan Title and Plan
              number, the laboratory name, address and phone number, and the prepared name and
              signature,
       2.      Table of contents if the report is over 10 pages long.
       3.      The results of performance or system audits to include, date of audit, system tested,
              name of auditor,  parameters analyzed, results of tests, deficiencies or failures,  and an
              explanation of the problem and the corrective action taken.
       4.      Sigpifieant QA/QC problems,
       5,      Corrective actions taken.
                                           15- I
-------
                        APPENDIX B

              Results off QC Check Samples for
              Total Phosphorus IB ffoil/Tisaua


Bol6rzano L. and J.H. Sharp. 1980.  Datermination of Total
          Phoaphonia and Particulata Phosphorus IB Natural
              Waters.  25(4). pp. 754-758.
-------
 Attached are  the results  of  SERF'a  analysis of  HIST  standard
 r«£«rence 'Haterial 1572  (citrus  leaves 1  and sawgrass leaves  for
 total phosphorus.   Each of  the sample* were  prepared  according to
 tint preparation procedure* described in Section i  and  developed by
 Solonano and Sharp  (1980?  see attached).   Following the  sample
 prtparation,   total   phosphorus  concentrations   were determined
 according to  'the  OTA  Method 365,1.

 Eight  HIST standards  (CL1  -  CM)  wer« prepared  each  day  and
 unilyzed  in replicate,  while three  samples of  the sawgrass  leaves
 (Ll - L3)  wera prepared each day and analysed .in replicate.   The
 mean values of each data set are summarized below along  with  the
 resulting accuracy and  precision  estimates.
Sample Mean
Citrus Leaves
1378
139S
13S4
1381
13 63
X-138L
Sawgrass
Leaves
178O
1747
1748
17S1
1727
X-1750
Standard
Deviation

46
31
20
18
20
S.D-* 13


18
IB
37
20
10
S.D.- 19
Accuracy %R

99.7
101
100
100
99.0



98.3
99. a
99.9
100
98.7

Precision
%RSD

3
2
1
1
1
%RSD-1


1
1
2
I
1
lRSD-1
The HIST  sample  is certified  to  1300  pf/g»  t 20O  pg/g»
enclosed certificate of analysis) for an accuracy range of  85%  to
115% recovery.  SERF'S accuracy for the HIST standard  ranged  from
99 to  101%  recovery,  is  well within the  HIST  limits.   For the
sawgra»« leaves, SERF'* accuracy ranged from 98  to 100% recovery.
Precision for both the HIST standard and the sawgrass  leaves  varied
between 1 and 3% RSD.
-------
 Total rtiospnonts SMliMMtS    RFA



Citrus Umm




Ottei             Niy 22, 1999


iiwie
Sill
QJ

CL2

QJ

QL4

15

Ha

OJ

ota

u

L2

U

M§i«tk «
lOQufl ST»-30f7^l
Bed i sent Bin
Bry Ml. (FIT
0,0094 0

0.0098 0

0.0111 0

0,0913 0

d,ww o

0.0105 a

0,0100 0

0.0093 *

0.0099 0

0.0109 0

0.0109 0

4
44,11
m
wr
27.00
27, »
2?.50
29.50
U.uO
13.00
26.25
2A.Z5
.27.00
25.75
29.75
29.50
a. 75
29.00
27.75
27,73
31.30
36.50
41,75
40.25
40.75
W.7|
Baseline
STI Mfl
Cor
ftvf

27. 00

29.50

33.00

26*3

2A.3B

29.i>3

28. SB

27,73

36.^)

41.00

40.73
offset 3 0
It * M,f
P04 Cone.
(ug F/pi

1371

1437

1419

1347

1235

1373

1371

1314
_— .
1710

1711

1785
-------
Total Ptwspherus Sediaevts    RFfl




Citrus Uuvn - I




Dlttl             Ity 22, 19M


SdMlt
Silt
HI

CL2

QJ

QU

CL5

(LA

OL7

OJ

LI

LZ

U

» Blank :
lOOyHSW
Sequent
Dry HI.
O.(30?4

0.01 IV

0.1)100

0,0106

0.0122

0.01 10

0.3100

0,0105

0.0120

0.iX)98

«.00%

•

law
DFIT
0

0

0

0

0

0

9

0

0

0

0

0
•i 64.ee
m
mi
2B.3
29,9
B.2S
32,3
29.25
29.00
29.75
30.00
41.00
a. 75
31.J5
3?. 00
30,3
J3.ZS
11.00
31.3
45.25
43.50
3i.OO
33.73
34,73
34, 73
Bawlim
STB het^
Ccr
A*f

21,31

32.25

29.13

B.as

3B.3

31.83

30.3

31,13

M^a
**fQ

15.88

14,75
I crflsct * 0
^it » M.i
rat Gone.
(119 P/pl

1411

14w

13M

1S45

ISii—

13K

1444

1413
—
17oS

1741

1721
-------
 Foul PhMMonis Smimmtn   fif A

Citrus LMvtt - I



W U«fc *          0   Butlim offnt
ICftJ* STIKQffiig/l  45.00  SID (Might *
5j«>le
Sin
ai

CL2

QJ

0.4

as

cu

CLI

OJ

ii

L2

a

Seoioent
Dry lit.
O..J105

O.U096

0.00f4

'J.^101

O.OOT4

0.0914

O.MM

O.OW3

O.J119

0.0109

O.OU3

lasi
OFST
a

a

0

0

0

0

a

0

0

0

0

PK
HOT
31. M
11.00
27.29
27,50
27.79
27,73
2B.75
28.75
27.3
28.00
27.3
27.»
29.90
3§. 30
27.00
27.09
M.S0
44, 90
3I.7S
40.9)
+0.50
40, 3fc
Cdr
*fl

J:. L>O

27.38

Z7.75

2B.79

3.43

17.3

30.00

27,00

44,50

40.13

40.50
we
(U9P

1407

1399

t«7

1SI

14W

I3fl8

IS74

1313

ITS!

1794

1706
-------





iivk
Silt
0,1

DL2

03

0.4

OS

CL6

CL7

QJ

LI

11

y

fol*l rtiospfiorvts
Citrus Leaves
tata
W ilwk *
IWuH Slh2W7u5/;
• Sediment BAM
Dry it. VST
'UU
-------
; i
                        Total PhQfpMftH Stdiwits   RFA

                        Citrus Leavn

                        OaliE            Illy 23,  19B9

                        W Blank a
                 Bast
Site    Dry Hfc.   QF5T

 HI     0.0095      0

 O2     O.OW7      0

 QJ    0,0©f4      0

0.4    0.0104      0

OS
a*
0.7
OJ
u
L2
L3
0.0112
O.W3
O.OM
0,0114
0.09W
0.0111
0
0
0
0
0
0
                            0   teiirw offset
                                STD htight  »
  BC
  WT
                                                    Cor
 27.25
 me®    ».o   i34i
 moo
 29,«)    2?-00   1336
 ZF.23
 27.23    27.3   13*4
 30.73
 30,73   30.73   1371
 21.00
 28.00   28.00   1352
 33.30
 33.50    33.50   13B7
 27.50
 ^.73    27.43   1377
 ZB.25
2B.23    29.25   1336
42.90
42.73    42,43   1733
                                                 36. t3   1715
                                         41.53
                                         4i.9b   41.9ft   1733
                                                                         tA»m
-------
                                                     u£
                          Ccriiftorft  of
                  Standard Reference Material 15 72
                                     Citrus  Leaves
 Hit Standard leferenee Material (S1MJ « intended primarily fo» use in calibrating; io«nuantutien and
 the reliaMliiy of analytical method* for the determination of iMior, minor. and t«ee dcaeau in imankaJ
 •Iflculiaral food product*, and similar matrices,

 Ccnifieil V»lma of Ccnrtlumi Bemeat«  The eerti&d v.Ju« for the co^utuent ckacnd are 5ho*n in TiMe I  T>
 •re burnt on raulu obtaiarf «th«- by ddiniiiw methods of known accuracy or by two ^ more imfepntfeat
   rls. Non-c«iir«d valim, which ate given for in/ormafion aofy. appear in Ttfcte Z

      and
then, purchaiers will be notified by NBS.

        The material shoaW bt kepi
                      ; This ««ificwion is m*m&4 5 yean tlier th* sUpeiiii date. Should il be invUwJaietl
                                         bo«t(e and stored M tempcracurw bctw^n I&-30 *C It should no, i
«pese«l to .mcnsc SOurca of nduuion. IdetJJy, the botttc jhould be kepi tithtiy dosed in t desiccator in tHe dart al y
temperature indicated.
        *«>"^ should l» sh«ken weJl before each UM. A tmrumum jampJc of 500 BI of ite dried tntteml im Itmnu
uoni for Oryini» ihoiiJd be used for any analytical dctcrminai.on to be rcUced in th* ctnifled vmiiM of this ccnificai i
Siaiaiieai contultaiioR was provided by IL Kafadar of the StamucaJ EnKinefring Ditmon.

The overill direoioa and ceerdwaiioa of the analyses leadini to tins cmificai.on were performed under tie ehairrau
thipof EL, Caraer, CbM of the J nor game Analytical Research Oivuion.

The tcchaical »nd support aipeai involved in the prepmrmion, cevtiJIenioii. and issuance of tttit Siaiidmrd Rcfcnne
Mattriai were coord maied through the Office of Standard Reftraiee Maieruh by  IL
Washmp.on, D.C 20234
December 20, 1912
(Revision of Certificate
 daied 2-22-821
                                                                    George A, Unano, Chief
                                                              OfHa of Standard Reference Material
-------
I
                                   Table 1.	Cerrified Valuesof Comtituem Elements
        Major mil Minor Conamucnti
                                                                 CkHjtm,1
                                                               (Wt. Percent)
                                                               us ±ai§
                                   Mipwritta
                                   Phwphonji                   ai3  ±0.02
                                   Pwtwwin*                   !.«  ±0.06
                                  iSulfur
       Trace Coimnuenti	
       Element ___                 Can tent.  >tg/g                  Bcmcnt    .                Conient,1
       AJurainum                 92   ± 15               ^      MM^HMWI             '      23   i 2
       Araena:                    II  ±  OU         ^           Mucaff                      O.M ± 0.02
       Barium                   21   ±3                     MoiyMeniiai •                 0.17 ± 0.09
       Ca4nnuin                  0.03 ±  QMl                   Nicfed                        0,6 ± §J
       Ourommm                  ttJ  ±  §J     _               RuMdiuB*                    4.84 ±
       Copper                   l&J  ±  IJ                    Sodium                     110   ±20
       lodte                     1.84 ±  0.03                   Suwriufli*      •            tOO   ± 2
       Iron                      90   ±10                     OB                        2f   ± 2
       Lead*                    13.3  ±  2,4
       Mtlnow Muciuli hi
-------
                                   . j.._ Noiir-cmilled. Values far , Coa«Ftuenl EteBMtti

   NOTE: The following values *re «« certified because they are not basedon iheraulu ofathcr » definmve metho.
   known accuracy or two or more independent methods. These values are iododed for information only.
   Major Constituent

                                                                   OjBlCOC,
                                                                 (Wt Percent)
                                                              Element
 Ejement_                  Content,' «t/n;_

 Antimony                     {  0.04 )                      Samanun
 Bromine                      (   8L2  >                      Scandium
Cerium                        (   0.28 )                      Selenium
Cesium                        (   0.098)         •            TeJlurium'
Chlorine                      (414   >                      Thallium
Cobalt         .               (  a02 }                       Tia
Europium                      (* 0.01 )                       Uranium
Lanthanum                    (  flLlff )
'An»iyiu:al »iuci tn bucd o* ibt ~», under ihe direetniB of A. Brynjotfuon.
-------
I
            Analytical Methods Used and Afttiytat	

               Analytical Methods:

                 A.  Atomic absorption spcciromeiry
                 i.  Atomic emission specfrometry, flame
                 C.  Atonic emission spcciromctry, inductiveiy coup Jed plaitaa
                 0  Ion chramatography
                 E  Isotope dilution thermal source amm spectra ntetrjr
                 F,  Iioiope dilution spark source mass ipectromctry
                 G.  Xjeldahl meihod for nitrogen
                 H. Neutron activation
                 1.  Photon activation
                 J   Potarogriphy
                 K. Specirophoiotnetry

               Analysts,
                 inorfaflic Analytical Research Division, National Bureau of Standards

                 I, I.L Barnes                           14. R.M. Ltndstrom
                2. tS, S»ry                           '3. GJ. Lutt
                'J. lt,A. Irteic                          IB. LA. MieWm
                C T.A.  Suiter                           IT. EJ.  Mauailul
                1 I.R.  Daurdorff                       II. J.R. Moody
                '&, J.W.  Grminlkh                        1». TJ.  Murphy
                ?. R.R.  Cncnberi                      20L PJ.  PmKlMHi
                S. 5. Hanamura                        11. LJ.  PoweU
                ». 6.F, HeaM                          21 T.C RUM
               JO. W.R. iCeUy                          23. T.A. Ruih
               IL H.M, Hiiiploii                       24 P.A. Stalk
               12. W.F.  Koeb                          25. R.L. Wawers, Jr.
               U,  G.M- Lamben                       26. H. Zeisler

              Cooperating AnaJvsts:
           i. M  Ihnat. Chemiitry and Biology Research Insiitute, AgncuJiure Canada. Ottawa, Canada,
           1 U- Gilionnt, E. Orviru, and M. DiCawu Consigho Hazionak dclle Pacerche, Ccntroda Radioclnmtcac Analisj p(
             Attivwionc prrsso I'lnitituto di Chimica GcneraJe dell* Univcrsita,  Pmvia, Italy,
           J. L Ko«a. A, R. Byrne, and A. f*ros*ne, lnst«in« -Josef Sidkii,** yuW^n". Yupwlavim.
          4 J  B.  Jones, Jr., Depwimeni of Horticulture, University of Gtorpa, Albcm, Ceorjia..
          1 L M, CuwyiLK Department of Sidopcai ScMri«a» Uinweraky of Piiisbu^* Pirabuf|h, Pennsylvania.
-------
  nc acid to Kycirol>rie poly-
    phoiphatei  and  th* arthophosphate  ii
    mnuufwd by th« motjrbdat* method. The
    method gin* 100* racowny wtth refectory
   phosphorus compound*, ii tuabJn on untiirut-
   ad sitnpJej with up 
-------
                                        Notes
                                     755
  used potassium persulfate as the axidant
  of organic phosphorus. Oxidation  to  or-
  thophosphate is  also  die mechanism in
  Cbtt ultraviolet irradiation method  (Arm-
  strong et d.  1966). All  these methods.
  measuring total phosphorus, also detect
  initially  nonreactive  phasphortii  com-
  pounds that are not necessarily organic.
  The last two methods arc used at present
  in seawater analysis. We have found in-
  complete yield  with  the  UV method
  when  adenosine-5*-trfphosphate  (ATP)
  was used as m test compound and poor
  precision with the persulfate method.
  The UV  method  requires high intensity
  ultraviolet lamps and heat  for efficient
  yield of phosphate from ATP (Armstrong
  and Tibbitts  1968; Goonen and Hoos-
  lerboer 1978|.
   We  have developed procedures suit-
  able for both total dissolved phosphorus
  and total particulate  phosphorus. Our
  separation between particulate and dis-
  seised  is arbitrary (set  Soloraano and
  Sharp  1980), The  method is essentially a
  hi«h  temperature combustion  of dried
  samples  (Assoc.  Official Agric.  Chem,
  1936) that has been used for particulate
  matter  from freshwater  (Stockner and
 Armstrong 1871).  The procedure for par-
 ticulate phosphorus is mud i Red from that
 of Stockner and Armstrong  because we
 foynd  poor recovery of orthophosphate
 without die siddition of magnesium sul-
 fate. The procedure for total dissolved
 phosphorus was developed from the par-
 ticulate one. A somewhat similar method,
 without MgSO«» was used by Levine et
 a!. (1955K Since the forms of the samples
 are different and different concentrations
 of reagents are required, the dissolved
 and particulate methods are described
 separately. In both eases, reagent grade
 chemicals and high  quality  distilled
 water must be used {we used reverse os-
 rno:,is/deionized water from a Mfllipore-
 Mllli-RO/Mflli-Q system).
  This work and that on dissolved organ-
ic nitrogen (Solorzano  and Sharp 1980)
are offered us simple, accurate, and  pre-
cise methods for routine use  on samples
from fresh, estuarine, or oceanic waters.
The difficulties with the UV method and
 the special equipment it requires justify
 the method presented here.

       Total tti$iolvett phosphorus

   Magnesium ml/at*. 9.17 ,V — dUsidve 10 g of
 MKSO« (or 21 g of MgSO, -7H.O) In 900 ml of di*.
 tilled watte and add I ml at coned tftSQ*. Thii so-
 lution can he slewed for months in * glass bottle.
   Hydrochloric aad. 0.75 M—diluJ* 68 ml of coned
 HCI to 1 liter with distilled wmtur. Tliii solution can
 be stored (or  moothi in a ijlass bottle.
   Mixed jY«*mfr- 4hii i» th« miied twsflemi from
 ihc itanrfard method (or soluble neaciiv* phoi-
 pAonu (Murphy and fUley  1962) a MMJlntd by
 Strickland und Pandas  (1972). Am specified by
 Strjcfcbnd and RUMMI. it should be w»de imme-
 duleiy betoFf use and not stored lor more than
 about § h.
   Th« proe«du» gfrwn it far »a*J dtaiolved pkm-
 phorui on lampJo with > 15*. ulinMy: for sampl«
 of lower Mdifnlty, the variation JTJVCO below should
 be used.  Oiuoivcd urjpunc pinnphonjf ti deter*
 mined 'by lubtracttn* th« amhtr at sotuble reoctiv*
 phosphonu rancentratioM bom the measured total.
   The simple should tw filtered to remove  panic
 uJate matter.  W* IIM puctmtKJ CF/C Hllen («r
 Wow). Moisure 10 ml of sample iolo * small Pyw*
 container jmd add Oi «l trf a 17 M MgSO, Tl.e
 ideal container {• • 4O* « SO-mm weigh in« bMtle
 «ridi cwtside  pWHrtd gl«*  covw. Evaporate  ih*
 MHipJ* to ilrynesi in a clean oven at 95*C, this step
 talees about 2-5 K. Transfer the wciehinK bottle to
 m muffle fiunwc» aad W» irt. 43T-5WPC ftw t h.
 After codinK.  add 3 ml of 0.73 M HO and heal the
 ujnpte in tun ov«i at 8ETC fcr SJ miw. Tl»e» «H t
 ml of distilled wBtnr and continue hoiinp;  for an
 additional 10  min. The (ivapornrtoo step »ho«ld b«
 don* without (he covers, the baking Ttep should be
 don* with loose  coven, and hydrolysis must lw
 don* with covers on tightly. After Kydjolv-sis. cool
 and transfer the sample to • tw t tube, add I ml of
 the mixed rcntfent and aAer 10 mm read the jbsix-
 tunce  nt 885 nm in a I- or 10-cm cuvette.
  For  samples with salinity < IWU a modiflmtiofi
 must b* wsrf to emur* cseiplete recovery of pho»-
 ptae. AAer addlnf the 3 ml of acid, bv*t the s*m
 pies without coven in a WC water bath for 10 .mo.
 Then add 7 ml of distilled water and heat the IIUB-
 pJei without coweo Car am additional 19 min. After
 cooling ttamfer ixinples to a graduated cylinder
 and Itrtnii the voliww to 10 ml. Thereafter, treat the
 sample of above.
         Paniculate
  Sodium tmtfate, O.It M— «Uisol« 11 g »f *"»hv-
drous N%S0., in SOO ml of distlltwi water, Tlito so-
Uition can be stored fw month j 1* a «b« bottle.
     , in I liter of distilled VW»*K. This solution
CBB he atond for mondui in * «!"» hottle.
  Htfdrof Marie ticid, 0,3 .M— dilute 18 ml of voiwd
HCI ta I, li*tr with distilled water. Thii JoJution tan
be stored for months in a i^asJ battle.
-------
     756
                                         Nott*
      Tahfe I.  yield of phosphate from organic and
     inornaoic ulti with (MfSOj ind without (no
     MlSOJ iidditlon of iruj?i>esium mJfate and with
     fhydml) and widiovt (no hydrol)  finaj jcidic hy-
     draf yiii ittp. All yields ai pttcenteite oTthcorctlcaJ
         100 indicate* theoretical yield! (9S-LOS%>,
                            NB
                                     HyrfJ
    Sodium
     miMKiliiuM:
    Ki>n>H.ivm ph
    Phaspliwyl cfdonde
   ATP
   DfeoclNiin pJicnylphniphate
                           IS
                           29
                           53

                           10
                           12
                           16
 90
 Si
 66
 90

too
 40
 SI
loo
loo
100
100
100
100
100
too
    Collet* ill* (urtkiildl* nutter on a, pnttnotmd
   Jiiifiii method, the evaporation itep \houJd lie
  d«w wuh fiotdcs unseilad and the Iwdting mnd liy-
  dntlvti* » ,>t MS nm
 in a i- or  Id-cm cuiwlt*,

   Solutions of varying concentrations   „.„ ^m. ^ ^^ mva UMm K ^ ,„„ ,es
 of guanosine-5 -monophosphate,  gun-   from a redreulahnff swiwmter system (sa-
 nosme-5 ~diphi,spho^ucmet adenosine-   Unity ca, 30*^ with phosphate concen-
 5 -trtphosphttte (ATP)f deoxynboniicleic   traMons ranging from 0.30 to 3,70 aM and
 uc-id, riboflavin phosphate, potassium   dissolved organic phasphorxij eoTcenta-
 glycerophosphttte, sodium glycerophos-   rJons ranging from Q,0§ to OJS M
 phute. glucoauunine-S-phoiphitte. phos-    Because the particu/ate phoaphoros
 p uienul  pynivate, dbpdium phenyiphos-  determintrion fdlowi iw same steps ai
 phate, trjs-p.nitrophenyl  phosphate,  that  for dissolved organic phosphoms it
 detunieraitone phosphate  phosphoryl  Is also considered  to  be accurate.  The
chliiridc,  po(a»ium orthophosphate  thoroughness aad precision  of this rneth-
(immobiuicK iincl sodium orthophosphnte  od have been checked by analysis of fil-
(Eti>th inonolMuicr  and dibasic salts) huve  ten on which varying voJuinei  were col-
hi-rii ointt^ed by the dissolved  urnanic  lected of cultures of the marine diatoms
            method  at concentrations   Skefetan^ms cmtatum  md
                                                     The linearity (r*
   of phosphate from  these IS compounds
   were 95-103%; this indicates that the
   method is accurate. Five replicates of 6
   /iM ATP were ran which gave a relative
   standard error of the mean (1 SO) of 1%.
-  When  magnesium  sulrate was omitted
   from distilled water samples of phos-
   phorus compounds, recovery was vari-
   able. Table I shows yields of a series of
   standards with and  without the  .vigSO,
   addition .and with and without the final
   hydrolysis.  The  MgSO«  is  used as an
   acidic solution (after addibon to the sea-
   water sample, die pff was  about 3) to
   minimize silicate leaching from the glass-
  ware during evaporation. The acid and
  hemrJng ins  necessary to  faydrafyze any
  condensed phosphates in the final mix-
  ture. The modification for freshwater and
  low salinity  samples is needed because
  without it the acidity of the sample can
  retard color  development  of the phos-
  phomolybdale complex. We  found this
  problem some what evasive at first be-
  cause  of the variability in strength of
 coned  HC1 in older botries of the acid,
 Seawater sails apparently butter the re-
 hydrated sample sufficiently, and the par-
 tial evaporation IQ the modification also
 places the pH In the correct range f >0.7)
 tor optimal color development
   We haiw used the  procedure for dis-
 solved phosphorus on  estuarine to ocean-
 ic samples (salinity 0-36%)  with ambient
 phosphate concentrations ranging front
 <0,OS to  3,0 jtM»  and dissolved organic
 phosphorus concentrations from <0.05 to
 0.8 juM. We have also used it on samples
                                                                                              \
fntm 0.12 to 18.0 jiM phosphorus. Yields
-------
                                          No tea
                                       757
   was  similar  to that found  with varying
   concentrations of ATP. Absorbance from
   a reagent blank and  from a filter blank
   were 0,015  and 0.020  in  10-em path-
   length cells,
     Far work at sea, we have  found it con-
   venient to use liquid scintillation  vials
   for both dissolved and participate phos-
   phorus samples, processing the samples
   through the drying step and then storing
   them capped at room temperature far lat-
  er analysts on land,
    As  with all  organic  analyses, special
  care including prior acid-washing is re-
  quired with the glassware. The glassware
  should be used only for the organic phos-
  phorus determinations.  The  weighing
  bottles should be used only for the evap-
  oration. baking, and hydrolysis step! with
  transfer before the mixed reagent  is
  added. Disposable scintillation vials can
  be  used  throughout  the  procedure
  (capped with foil for the baking step).
    We 'thank A. C. Frake and C. B  Hillier
  for experimenting with the methods  and
 A. C. Frake, L. EL Fox, and P. A. Under-
 bill for comments on the manuscript. Re-
 search on  the  part icu late  phosphorus
 method was begun by  L.  S. at the Oun-
 staJFnane Marine  Laboratory (Scotland)
 and was supported there by the National
 Research Council of the United King-
 dom.
                         Lucia Solorzana1
                     Jonathan H. Sharp*
 College of Marine Studies
 University of Delaware
 Lewes 19958
AnMsrrwjNC, F. A.. ANO 5. TMMTTS. 196ft. Photo-
  .  cttemkfiJ comlniiMon of organic mutter in s*m»
    water, lor nilrojten, pituiphorus ami carbon de-
    terminations. J. Mar, Blot. Aiioc. U.K. 4*i M3-
    152-
— • — ..  P. M. WILLIAMS. AND  J. D. STRICKLAND.
    1966, Phtiln-uilichtfMl  285-295.
  CORRCUL, O. U 1965. Pelagic phosphorm roetah-
      dim in Antarctic watm. UmnoL OceaMgr.
      lOi J64-J70.
          J, T., AMI |, C. Kucsatm
      Oetenni nation of phosphate* in natural
      wane waMti after photochemical
      Mm and add bydrolysi* sf organic phatphwui
     compound*. Anal. Cbem. SOi TOT-TIL
         A. L, AND R. J, ROBWSCW. 1953. The
     determination of organic pfwphamf in iea-
     water with  perch toric odd oitdalion  f, Mir.
     Acs, 12; 31-42.
  HAHVEY. W. H.  1948. The «ttnuthm of pboiphate
     and of total photphoruj In smwatar. |, Mar.
     Biol. Asaoc. U.K. 27,  337^159.
 —	. 1953, Note on the abawrption of organic
     phmphorut eomp«Minds by iWtueM* etati*r>-
     mm in the dark. J. Mar Biol, AJMJC, U.K. 31:
     473-476,
 HOUM-KAMSEH, O.. f. D.  STRICILAND. AND P. M.
     WiuuAtm.  1966. A deMlcdl andyiii of fiiolo^-
     ically important ^ubitancei in a profile off
     southern California.  Limnol. OceafMfir. tli
     S48MMIL
          B. H., N. CoRvnn, AND D. J. KEEN.
     1955. The lignlficBitce, of organic pho^phorui
     detemuoatioos in ocean waters, Deep-Sea Res.
     Xi 172-Lfil.
         H,, J,  f. Bovm, AND F.  s. GMMAUH,
         Molybdenum bin* reaction and deter-
     mination of  phiMphoru* in wotctv ctmtaioinK
           ilKcon, ind BBrmanjum. AnaL diem.
 McGiLL, D. A^ N. Oonwm, AI«> B, H.
    1964. Otapnic pbospJioru* in th« d**p water of
    the weshrm North Atlantic. Umnaj.
 MENZEL, O, W.. AM» N, COR WIN. 1965. The
    Mcemeni of total phcupborus in .tnwater hai«l
    on the liberatkm of onjaniqajly bound fractioni
    by penul£ite oxidation. LimnoJ. OceiUKKp. 10i
    280-282.
          ^ AKD f, P. RIUEY,  1962, A nuxiifint
    •untie sdutton method for ihe dotcnninatlwi of
             in natural water*. AnaL Oiem. Acta
  1 Present .iddrejw:  liutltuta tl*  Inveitdtucinnv*
yuunit'iis, Univenldad tie Cnay. A. C. H. P. SMITH, AND 8.  H. Kcr>
    onni. 1137, The cycle of organic phosphorus
    in the Gulf of Mate*. Bid. Bull 73.  121-443
SOLdRZAJMO. L. AND J. H, SHAlV.  1980. Deler-
    minnlion of total Ui»uived rMtrogen in aiitunJ
    wateu. Umnol. Ocewiotpr. 2S: 751-754.
Srocxxnt. J. C.. AND F,  A. AKMSTWOWC. 1971,
    Prnphvton nf the  EipefimentaJ Likn Airi.
    northwestern Ontario.  J,  Fish,  flci  Sd. dn.
    28: 21S-2S9.
STMCKLA.ND. |. O., ANO K. H, AUSTIN. I960. Q«
    the iortnv Iwlancv and cycle of phunphomi irfi-
-------
TSS
   served In *. ooutaJ Mid mule w»tan of tfi«      M4T4 fa H. BMW fedL Smn»

                   " ''     to* M Ci*' lf *
                                                  .
  — . AMD T, R. PAHSOIW, 1§72. A practical hand-   WATT, W. O,, AWO F. R ,H*f» MSI. T»«r mtdhr
   took of MMtr nulyUi. ftri •d. enil. Pith,       «f ft, ph^Jjonw ^|. ta m M^T. Uwillilj.
   ««. BdL Ciin. 181.                              Owtwpi Si «i-SW.                        «
    , AND L SQUJHIAMO. 106&  D»twmlMtfoil             -,  ,  .„  , „_ _     ,    .^^    *   f
   of moi»«si»ffai* kydrafynbb ^mpJiatr «id             Sulwiilfai' 27 Dtcemlmr I §73    ,   \
                     jctivny m icaxtrmter,  p.               Accepted: 29 February 193O       |
-------
                          APPENDIX C
          An EqnivftlaBoy ftudy on tha Vmarvatien
       of Nutrient Samples  by Praeiing or R«frig«ration
 ClMMBtioa, L.&. «u« •.•• W»yt«. lit 2. »* Bff»ct of Fro««i
•tormga of op«n-Qe»«a fl«aimt«r S*api«» om t'M»  eoBeaBfer«tioa of
           Phosphate and Nitrate.  Water Resources Research.
                    26(9). pp. L171*117f.
-------
                                                       Appendix C
                                                       Revision 0
                                                   Date:  11/16/95
                                                      Page 2 of S
MTIODOCTIOH

on January  5, 1995, Florida Department of Environmental Protection
aoorowd SEKP's  Comprehensive Quality  Assurance  Fro jeet  Plan
fCo»QM»l    The approval did not  include the  freealng of samples
forTwwnimi analysis.  PDEF recommends storage of ammonium samples
at ?C   in response  to their  comment,  SHIP  has completed  an
emiivalancy study demonstrating no significant  difference in the
ralta of ammonium following storage by freezing or refrigeration.
The results of  this study are presented herein.
KETEODB
on  2  larch  1995 ,   two  2 -liter bottles  of  surface water  were
r«ni isetiad from Florida Bay  station  16  (Murray ley* .   The bottles
Seamed according to the protocol, de^ribed in SEEP*. CompQAP.
SDeJif ieally,  the bottles were rinsed three times with .ample water
p?lS to being  filled.   The bottles were then stored  in a dark
cooler with ice and transported to  SERF'S laboratory on the same
day o£ sample collection.

m the laboratory each bottle was vacuum-filtered through a Whatman
GF/F  gl*«  fibi filter.   Prom  each  filtered sample,  10 €0-ml
«mile bottles  were  filled,  for a total  of 20  nilMUplM (   ( W
"billed as F for frozen, and 10 labelled a* R for refrigerated >.
Each of  the sample  bottles were rinsed  three times with  the sample
prior to Tilling.  THe  10  F samples were stored in »"••*•*  Jf*
thi  10  R  sample*  were stored in   a  refrigerator  at  4*C until
analyzed.

Sample analysis was per formed  according to  EPA  method ;"0.l*«
described in SffiP's CompQAF.  Frozen samples  were allowed to thaw
sl^lv to roo« temperature and shaken thoroughly prior to analysis,
SoS * f ro«n and Refrigerated sample were analysed over the course
of 35 days from sample  collection.

RESULTS

A»oniu« concentrations varied from l.iS to  3.19 uM <****•  C-l).
n^ired t-test was used to test the null hypo thesis that there is
no difference between the ammonium concentrations of th*. froaen and
           d  samples  (that   they  are   from  th«   same  «««J
              ^results  of tto paired t-test conf irmed the null
            at   the  0.05  probability  level  (t— 0.09r  P-0-").
        nq no difference between the amaonium  concentrations of the
  row  and  refrigerated  samples.    In  addition,   ttere was no
aimificant difference between  the concentrations of  the frozen md
refriaerated  samples  for nitrate+nitrita (t-0.il» p-O.SSJ , nitrite
™   71  p-0.49); and soluble reactive  phosphorus (trt.10. p-0-07) ,
-------
T*bl« C-l.
R*siiltB
                                                                                Appenu^x
                                                                                Revision 0
                                                                            Date;  11/16/95
                                                                               Page 3 of 9
sampl*
i
2
3
4
S
fi
7
a
9
10
i — mti
Day»
0
6
7
20
21
24
25
26
27
35
^_^— .^ ^^^
D*t«
Q3-Mar-95
OS-Mar-iS
iO-Mar-SS
23-M*r-§5
24-Mar-S5
2?-Mar-95
2i-H«r-i5
2i-«ar-95
30-M»r-95
07-Apr-95
KH4-R
(PH)
2.09
2.58
2.37
3.01
2.73
2.60
1.98
2.05
2.10
2.74
NH4-F
IPM)
2.06
2*64
2.92
2,23
3.19
2.31
2. IS
2.13
2.19
a, so
H+N-R
(MM)
1.44
1.42
1.56
1,67
1.51
1.53
1.48
1.50
1.47
1.48
M+M-F
(MM)
1.40
1.41
1.61
1*4S
1.54
1.51
1.50
1.50
1.50
1.49
N02-R
fpM)
0.25
0.25
0.34
0.32
0.25
0.30
0.37
0.26
0.27
0.24
N02-P
(PHI
0.25
0.24
0.38
0.26
0.25
0.26
0.27
0.25
0.2S
0,26
BRP-R
(MM)
0.06
0.12
0.07
0.09
0.04
O.OB
0.08
0.04
0.14
O.OS
6RP-P
(MM)
0.06
0.10
0.06
0.09
0.07
0.03
O.OS
0.03
0.09
0,06
-------
I
                        I.. «r»  V,A ;iN«. f, pi. 11II-117/1 jt|}
                       ••niUMl Ml t.iril 8fll.li* • -  •
                               THE  EFFECT  OF FROSN STORAGE OF OPEN-OCEAN
                               SEA WATER SAMPLES ON THE CONCENTRATION OF
                                        DISSOLVED  PHOSPHATE  AND NITRATE
                                                     A. Cimmmatt* ind S*u,i- E W*nt
                                   CSIRO Diw«,fl rf Futeiiea, G.P.O. Boi |JH. HMnn, Taimaaia IBM. Awiralw
                                                 samples «h>ck wen itotctl at -
                                  to . «.«,««, rf 24 m,,,,,^ fta ^^ fo, „,„„.
                                          of ihr
                            nyutenii
                                                                                           b* r jpUintd ji
                                                   I»M * *M not dlM 10 ttw AetS Of Wife* adHMflMM..

                                                    r«ie« iMtait. mnp HIM. Hurtaa idMMpaon, nitrat* pht«ptw;c,
                                     "NTBOUI.CTTOfl

                      Bw iioraic of semwaiar sampiei for nuincnt analyses
                      lut been a problem ihat has pVagucd re^archm Tot
                      more ih»n 40 yean, Hayrwey |IW|> wu tme ufihc nm
                      fKca,rehc« lo deal with the pcoWem. Ideally lampka
                      ihould be analyud immediaidy after collection; tew-
                      ewr» LMi 11 not alwayi possiMe, and wftea iruJyiicaJ
                      cquiptnmt Hills dunn| an iruenuv* (fcJd profram ar
                      umpte ojHeclion it froiB • vcmoic location, simple*
                      (HUM be  norcd.  Qceanopiphk  viudicj urn *m
                      oampte of an intenim htlJ pregraw whem Kmited
                      pcnonnel, mfyfficknl imw  10 amiyjc lampla be-
                     tween sampte cnir«aioBii and weitlw condinonj may
                     ill mean ihai samples ha1** to IK Horrd. It is therefore
                     ntreeiwry to ttorc SMnpha  n» as to minimue any
                     drama in the conccniniiooj of nuiricnu wiUi lime.
                       Tlw liieraiiwi OB iiorage  ttdmiquei foe autmat
                     jwnples dcvrnba an array «f uduiiqiia. Some «rf
                     these techniques and the corresponding rrjulu are
                     w«««riTOi In Tabfa  i. Samples h,ve ten «oml by
                     ftteam. quick frecanf widi dry ice and the *dd.tl«rar*
    sunn of this uwdy wm to determine hw««" |,»n,.
 Mmplti can be storol from without aff«tu»f  .he
 reliability of analyrical mute foe Mtme ana ph,,%
         » awnm the dfccit,  if any. ,«' oinia»nrr
             area on chan|ct m nuinent cunftn.
           MATEM US AND MCTIN)»S
  Tfct
                               Tae
                        tkt «Ub*ii% 41
JJIIC Tht iB^phr WM ccritactcd in rhrre Jt'l. f»\T
bwilet MI a CID raMM and cmpM into s, 31
wtatod. mm
                          ID *hoin at) conrtsponteiet ihould he
              niAer cdbcom
    rj » Milbpore 0,4$ pm Miner thai hjj
W* MQ wlutioo, Appraiimmirii 6M»m( %H
water wai lUtcnm and divauded More ih.
nliwri aad rtUMtd (w 
-------
                                                                                            M*» ikr
Amfcun
                       KMrv*. •il}itil
                                                      lipc
                                                                                                                       tnurt
                                                                                                                                M^I

                                                                                                                                -ll
a*i  w**ck   «ij, NO,
                        I;  , NO,
                  , NO, ,
                                         apMwt«ilui«t3nilO41*ii MiftfMtl
                                                        100.
                                                                                         Ham
                                                                                         F«un.
M) M |«IH.  |lttL
Hurt
                                                                                                                                 M >
                                                                                                              Tdkr*  iMl |ii
                      N, P
                                                                                      fimnn.
                                                                                          Clin,
                                                          Fi»lui>uaKd hiiuJ    Own*  IfuWfl,
                                                          M'                   Mmp
                                                                                CltD,
                                                                                                              Ida ail
                                                                                         0»rt. ^ C
                                                                                                   NiF
                                                                                                   CHQ,
                                                                                         jrJ T>|CO,i-
                                                                                                                                                     I!A.ICJ«   -iih
                                                                                                                                                    L mi«J  uUi]4^
                                                                                                                                                                4r
                                 t .wtaii uagifa itwinl
                                 ^P WHiVMlHr %(M (JHPHF
                                 IIH IHM * Atpl Fnwi*
                                                                                                                                              IkMhiiiieMtc
                                                                                                                                                HUC  Jl|fcl
                                                                                                                                             ui  NO,

                                                                                                                                                       MIIIWIH
                                                                                                                                                       i j| jM
                                i* i|wct (iihmi
                                ••Mh tKO,  i» 114*4*
                                .-«nJli  ten  itt*n  in
                                franw   w  imrraj
-------
                                'Tic citicn of fn

        boUin [hithJmuir  polwihyVnc wMh InA proof
  wM »nd KRV tip (Kmrtctn. mrfaoi •m/volum . fljjfc
  171 -'-Oinl  bank* (aa  for I;  iwfae* irtuvoluow - I 4ft
  ill »ml   idftiiiUiioa  mala |hi|ln)rri
  •Mb   polypropylene   tern*  cap  fKarteMJj

  piufc-4M cap (Ditpotaob Producu  Awmlitlc  lurfcc
  jreaftoJumr - 1;H| Except for the 15 ml tuba, all cmn»,n-
  cii had been toafcrd in 10% HO wluiion for n  Icajt «| h,
  ontcd 3 times «ith w»ur friMi a Miiiporc MilU RO/Mtlli-Q
  lywtai and nnwd (WWE *nh tht Alumt «a*ilCT uaplc.
  'Tbe lube, wm tuoally u«u « mnml from the nunufac-

 i*«re wnh  the Mrcrcd vjwuer iampk. Two KpNcaiti fw
 ««ch conntnrr for  eack  iterant period wet* ukot The
 onniaMwa *«« WW at randnm md lr> only  7/| of ihtir
 iM*l voliMie. After M cnntiMien tat ibj ennn opmmat
 h*d born HIM ifcey ww* Irtan u -40TC in • Man freeier
 All conuwtr* w*r«  in the frtcm* tmata 1
 collection After (he cruti* iht wbumph

 toom UTT,peT»«uir a«r  1-J h i»d •nalyic4 for niirat* Jd
 phoiphair-wnrun m Further J-4 *> *JV» 9  I&. la  AT  JUIM
                                                of  OM  iwUkwii  we  tlttOIjtM  for  niua.c  .mj
                                                flU S ± 001 nM for ptaifkMt.
                                                 TIB rawfw wra» mbjrai to a t*»-f»ewif »n»l>ii».,rf,
                                                wwunfit mih tm F \ot (m Knew irenrt M cUv Tie iinrjr
                                                IIWl M leMMi  ipmi IMM tqiurc ««• «e*utHi«n rrom
                                                         macr ibM ite  mdnal  ntcm %e^ut hetaiiv
                                                                     of rMHtBdif *houl ihc re-
                                                          u •
                                                                     ibc ptM»phu<       niiM r*f*n i,§
                                                             « l»u iquam funcnon niitnK ruttiiiNr I Miller
                                                                      10 fil • two pJuic timnkr „»„,« „, |(|e
                                                                 •E5LLTS
                                                                             OtSCUSKlN
                                                      Tht vmrutiioo in conocntration of nitrite jrxl phu«»
                                                    ptele In frozen oceuuc satwiicr wmpki «-iih time u
                                                    ihown « Ftp 1 uui I Brforr I he «siniical ajuJ^iih
                                                        perfcvmcd. om "rBmtwielE"* data po,m ^aj ' re.
                                                          fne« the dat* KI m OBrf cuniammat
                                                                   for ii_
  Phoiprt»ic ind aitraie were drirtimntd
3020 Row iM|toi0a »*mly**t with • T«awt M1J
l»lMMam«rr md . H«wlE«-P»ek*riJ TI2JA cK«i
Tl* method for miraur arulywt »n |ij«d on ihn«
           by Arnlcnon  {|97V| and  JuJwwwn  ind
           20
           13
                                                 Til* total mraUily in the data frwn uorage
                                               uodici u due (a the cdrabtnaimn of xvcral fnuim
                                               in» MM 10 «ora§e lime ar tjfpe aJone fMacOunaU
                                               and McLauKhlin, I9«2. KronKn| and Wcnek  I486)
                                               Tfc« imal v.nabiLty (3^) » «1"*J » the vanabiln>
                                               *i«n « fraup of rrpJkun (5.) piu% the v^nai
                                                       idmiieai wmplei aitalywd o« difl^rvni
                          2SO ml boilhi
                                                                  SO nri bom*
          TO
                     30 ml sdniWaitofi vtal
              *  I
                              40O
                                               MO
                                                                  IS ml lute
                                                         it
                                                             200
                                                                 4m
                                                               12
                                                                              600     HDD

                                                                                   24 months
F,. ,
                                                rim* «ti v>i
                    i.
                                         and
                                                   am.
                                                                                     »..*«•« i _•
-------
                           ISO nru o 011 It:
                                \
             ,) J •;
                                                                   sominottt*
    3      |     *0 ml SCMII illation wul
    III*.,    .
            0(1
            00
                   Son
                   i
                  s
 400

12
                                                                   IS ml luto«
                                             24 months
                                           Sloragr Hrm ((Uv>»
                                                                        4aa
                                                                      t2
600      MO

    24 ntonins
         ip .'  Varuunn *n cancenrunon ofdithilvtd photpluutmilk itanft umc (OT botlln of different volume
                                            mil mclase area.
 r^i-  ;hr  \ari4hiliiv tiuc  in
iyj i)|v • f, i
                                         lime  and
                 V.» - V  - f. +• ^
  Che u'lhin-rrplicaie \-irur»M> is cqtuJ lo ihe arulyti-
 «.il pri-*i%nihi'tjid rcmjin ihc umc  ihrnughoul the
 !'pej (F-tesi (f ) • 2.66;
     cn   oi'   Freedom   (d.fj-l.50;   probafcuhty
      H05J The difference in concern rat ion between
            w« signtfieam (F - 13,91; dX • 12.50;
^ < 0001 >. but ai  ihe coneeatrmiion did not chmp
linearly  with  uorage nme  (F-0.134;  d.t. «I,J|;
/* > 0 U5>.  and ihe  ilora§e l>pc» rciponded simihrty
Jt  each  %«»m|B droe (no  ii|nific»ni interaclion:
f - I  *l d.f. -  3S.JO. P > 0 05), this difference mu«
be due ia the d*y to da* vanabtliiy
                       The  v»ftabiluy  due ta calibration eflccii rangri
                     from 0.3 to 1.2%  of the twngr concentration The
                     o (nerved vanaWNty in cooccntfation n greater than
                     1,1%.  thus the day to day wrubibiy  is  mostly
                     mnkrtn»b(e to factors otter than calibration uncer-
                     tainty  The variability tn nrnpiet docs not appear to
                     increase with 51 or age time aj found by other workers
                     (MiicDoiuld awl  Mclaughlin, 1912; KrcmJini and
                     Wenct,' I9I6*.
                       The  overaU iJope  cjdmatc from the  regrnttom
                     of nitrauc  concentration on  time  wu  -OOO025
                     (SE - 0 000323). This implies * dtcreaie  in  niirai*
                     coneentraiion  uf 1.2% ovet (he 729 diyt of the siudy,
                     Givta the lorei of vanabihty in thti dam.  a dope of
                     -0.0006) or t drop in eoiweniniiioB of 3% should
                     have been observed lo detect a statistically Mgmfkam
                     decrraie in nitrate concentration with  nor age time.
                                                The difference in  concentratioD between  $tora§e
                                              time* w(, hi^ily jtgn.ficam (f - 201.83; d.f. - 12.30:
                                              f < 0,0011, ind this *n l»rgtly aitnbuuWe to a
                                              ugmikaiii  linear  trend  owr  lime  (f-IItIM;
                                              d,.f, -l.ll; F. A rwn si jnificant iniennio*
                                              {F - 1.5* d.f. - 34,»; f > 0,05) ibowett that itont*
                                              iypa  rtspoBded imniiarly over line, figure 2 show»
                                              thai the data for all stomp types, except the 1 5 mi
                                              tube,  fetl into three distinct phases;  lb« phosphate
                                              conDefuration renamed  constant for •pprontmateiy
                                              ihe first 200 dayi and 
  off M
  phoxp
  be dei
  bilun
  sampii
  that id
  «nd st;
  I ration
  afier :
  nine, li-
  ra i ios
  i ration
  * possi
   The
 cant  j
 d.r - j
 enii/rJv
 phate c
 ihennt»
 to ihe i
 indicate
 deereasi
 behaves
 'arnplej
 grcatesi
 phiispila
because
cri. Ho«
wa* mad
-------
  , ion The
  Her (ham
  %  mostly
  • n. uncer-
  , ppear to
   .reuion
  i nuraie
  ne utidy
        of
 igftificant
 Age lime.
 n storage
 '. - 12.50:
[Jbie  (o  a
 - MM 76.
 the  1 5 mi
                                                     The effect of fi
                                                                     itonp
  lime before jppesnng 10  rarnin relatively caruum
  lot I he remainder of ihc study. One of the prime aim*
  of ihn uudy *n to find out how long uunpla could "
  be noret frosen without cbtnfo in phosphate con-
  centration.  Therefore tt was important  to determine
  i he storage tune  at  which the phosphate coaccn-
  trauon sinned to  decrease rather than  »ry and fil a
 model to i he enure set of data points  For liiu reason
 the data points corresponding la 590,  §45 and 773
 davi storage lime were omitted from further analyst*
 Ithcic were (he data point! that appeared to remain
 conn ant at  j lower concentration). To determine the
 point at which the concentration began  id decrease a
 model comiiiing  of two straight bnei,  the Hut with
 xcro slope.  <*»» Ailed to the data (w*  Rg. 2X The
 estimated times. Tor cadi itonp treatment, u which.
 i he  phosphate concentration begin 10 decrease and
 their uindard errors ore  shown in Table 2, These
 results indicate that in the 130 ml boitlc. 3H ml bonk
 and the nomination vial,  the  phosphate concen-
 tration remained unchanged for the firu 210 dayt of
 frozen  Morale and then  steadily  decreased at Hie
 vimc rate with increasing Horace lime until levelling
 off at appro*. 400 days. The exact time at whkh the
 phosphite concentration slopped decreaung cannot
 be deternunrd from thit uudy, Due to equipment
 failure  there was  a period of 200 days in whkh no
 samples were analysed and it wat during thii penod
 that the photphale concentration stopped decreasing
 jnti started to remain ai st, rclativriy constant canon*
 inttcHt.  The decreaie in  phosphate concentration
 after 1(0 dayi cannot be eipUmed  at ihc preient
 lime, Ho wrvcr, as the different suifacc area to volume
 raoot «jf the coniainert did not  :iffcci the conccn-
 tranuni. w«U adsorplinfi efTecls can be (Jiwrountcd :u
 a pofuble reason for  the tusi of phosphate.
   The jnalviu-of-varuncc also indicated  a ugmrV
 cani  iJirTcrrnce between  iioragc  types (/"»4.55;
 d.r, - 1.50; f <0,(JI), hut r-testi showed tlm to be
 entirely due to the tube having a tower mean phos-
 phate concentrauon than the other containers.  Fur-
 thermore a linear model (/?'=• 0 89) was the ben fit
 to the data  points Tor the tube (ice Fig.  2) which
 indicates that  the phosphate  concent ration bepn
4ecreasin| immediately on Ocean§.  Why  the  tube
 behave*  differently in  the  storage  of phosphite
iamplei is uncertain. Although the  lube had  the
greatest surface area to volume ratio, the early la« of*
phoiphaie cannot  be  attributed to wall adiorption
because this effect tnu not round in the other contain-
ers However, the lube w»s the only container whkh
was made of polypropylene rather ihan  high-denuiy
                                                                                      and «J» tu4 not  been iod «
                                                                         befon tha nut of th* experiment. Potublv  one or
                                                                         both of litoa facton are mponubk for the njnifi
                                                                         tautf dJfemx found ia ttortng  samples for phos-
                                                                         phate amrrm m the lubej rather than the other
   Kremlint tad Wenck (1986) iuggest that phos-
phite OHM be Ukco wp during  the  freeing and
thawing  pexiodi fcy  pfohFermuiig  ifucro^nrgmsins
that ttlach thonselv« ifl the walli of the contunrn
However, it n not known why the mitu-^Fjrw.m-,
temtJil in a "dormant " itatc  for approi  2111 Jjv^
before pffoliGntini and then later rttunt to »  .U.f-
Hunt" lute. If they uuch themvclvci to the
Ll» conmoer when proliferating, ihii stwh.
contwnen of djAcrent turface  area 10 volume ratim
wet* uaed. ihouM h»ve ihown wxrving phovphaic l^ni
with uimfe type.
   Tli« above uatiiucat  reiulu jppty only  m the
oceanic teawaier lampln.  but simiLar icsurti were
abiauwd for the Hunpiea from the coastal MIC. Nn
linear trend wis found between nitrate concetttration
and StOtagt time. For phosphate • significant linear
trend WH found to exist between c^ncentr jutm jnil
ttorage IMK,
   Im an attempt to resolve the ht-havinur of pho\
t>h>ie im ttorrd wmptd a second  expcnmcni ^a-,
initiated. Sunptes WCR collected in  April I9X1) irorn
•pproximitely the same powtion (41 40'S  I4« n F»
•nd depth as tho*e collected in July 1 at ihcrc
had ban no dilference between the  Bflml. MI ml
bottles and the soBuMation via* m the im  earx-t.
iment, only 50 ml bottle and tubes were used in ihc
second experiment. Tic  bottles and lubei
vided {MO two Ktc those thai  had been und
u prrrtouily dcicnbcd and those that *cre
recci*^ from ihe nwmifaeturer. The container*
Riled and stored m ihe »mc manner m the coniu
in the tint experiment and were analy led -Met  I ft  iti
a. n, iia im iw, ZH. 241 a*ui 1*7 **„
   M M the Im experiraeiK the analyi.i*-.i.r-urami
mdkcalcd  that the  cooccnirauon of pho^ptutr  n
ipcmded  dificrattly  owr lime for  the -i
50ml bottJe and  the acid-wuhcd iuN-
d.r*9JOc  001 < f < e.flSI,   For the
tnaiys»-of.vinance showed it  significant
betwe« storage time and  wid washtnp i f * •< M
i.f. -§»» F .Qmt tHittlt
Tube
nmi
(i m*
.• ^nu
_ — _ —
110
110
(1 i nuW RIM he ftlltd
n
14
IJ
BIWI

000)
n i»«ii
'k !.,«,>
DtMM
-------
                                                           fc.
  .,.tuJ
       ..  nt>l ' ,..'o  .*<* >tlC -
      i ~ n i <>*r-t •»'«•" .itui^t-i  Thai \\ (he c
      ; i he tina  points for
                          i.unitl  h£i*«n these
;h. '> for ihc Urtt eipar-
i  ,ii»,i UT ila>s Mr (he *x«»itd rtpcmncm. TTiis
cfkv -tw he c\pl*jncil hy ihc tltfTcrent compo*
  <»i  i hi.-  %4-ju4icr  vjcnplc1.  used  in  the iwn
'UK urs  _nii I ,,oiilJ  tie iCNicd  in  it loiuic  -.ludv
  >Hi.pl«:->  mlkxitU  I mm
ih ti
              JIIN4 I I

  r, nil* irum ihv%c %«TI§C rxpcrimcnu mdicaie
fk-c/ing «..m he -j (i-li.ihlc ;ind cffcvlivc iticans of
^ . ^v.inu  ,md  kiwljl sjinplcv  for  nuiriutll
«»•>   The  i-iintcnirjiian nJ" nnralc showed  no
, .mi  iri-nU *iih  "lurcjving  >Mr;i|tc nmc. I or
k pho\pti«n r  ,mjl\«n. ihcfrnien ^niptci must
     '«,»  -A ic hi n ^ppfi»i. •*
ihi-, Hmc the  phtiiphjic citnvcniniiHin will
kft..iKi;  "tii'iiJth  *iih  intfcjMtn*  i in ihinc>.iiirjiioi»  wnh siorapc lime.
ll *«iuniin|£ i til IK-.V nl*
'  "I nfl.JLV ll
                                   like hi ihink
  . (,'."•. "f  fhv*  julhi>is m
  iiklt.jiTiai »»l t M\' *ii«« ii*
                                                                         •mimes
                                                      A ndenon L. ( 1 1 t*J Similiiaeoiu ipiniophouwnrtnc daer-
           ol n*in(€ ind miraic tof He* mjcuian
         rAwi, ^CM 111.  1 23- 1 21.
              A,, liana G. P., Gtiffllhi F. i. and Ximmtr
   D  *  ||9J9t ScuonU  »nd iaKr-«miuI vimbiUiy M
   cHcmN.j| and biokipul  picimclcrt  M  Slorm  BJ»,
   Titmuiia. 1: ptiywa. chcmuity and  ih<  btomau uf
   component!  of the Food ckiin. .4«u< /. .Wor  f>ri*»«l
   ffri  40. JS'11.
Gilm»ru« M. {IWT1 Ch»nga m wmrpmc phcupliiie con-
   crnu»uon MJCUfTMt  Junnt ie»*»»t<:r umpk Moragt
        M,  and Key F, 1 1 914 > Slonp of Kitwaler  for
  n»uirnt >n>ly»i FHkM Ifanrf, 4 1-12.
Harvey M. W. (I Mil He «tiMnnion «rfpHoiph«lr ind «cu»l
  n*ntphoru> Hi vm vMdl. / M«r. AM, AIL if K  17.
  .117- Ml,
Joiimon K.  5. »nd  Petty R.. L I1W1 Dciermmaiio. d*
        nxt niinte » «a*»icr by low iajtauM *nity«»
          Ormmitr. II, l36O-U6fc.
Kanlnff  F.  (J976)  DetttmnawM  of piwffrfiwm,  In
          e/&*lMMr Aimiysu (Edited by Gtusho* K X,
      Ill- til. Owwte. Wctnhcttn,
          1C. anil Wwdl A, (I9MJ Oi te fMMife of
             qianH: photphitc.  nilnu *nd  neaciiwc ttU*
      m Atlinlic Ocnii *»itr nmpfai, Al4 etliuftnc  *»i«r»   *af.  ftrt,   16,
  91  IM.
MUkr A J. (19111 iMM— A iwbMWHW .for uncansiiaiiKii
  •on liocir leait tquain filling  C5IRO (AiMlr»ha| Oiv
           d bait.  Rep. VTI1/21.
      J. W.. Hum M . Zulht J,. Muco A. and Mender T.
  I19R2) A n>mp»miino« of lira uwayr mctbodi
  fur (he aiiah/Ms of nurepa and plmptkonu (nctiuiu M
          water , Chn^umkr Sri. H,  IM-J5I.
 C'l,
 ^pi
 ihc
 br
 Jfll
 thl
 eor
 wa(
  «a
and
                                                                                                                bat
                                                                                                                Oil
                                                                                                                hcc
                                                                                                                >nic
                                                                                                                it  i
                                                                                                                IV,,,
                                                                                                                  A!
                                                                                                                •1 O
                                                                                                               ceu.
                                                                                                               (MM
                                                                                                               fur t
-------
                       APPENDIX D
       An Equivalency Study on th« Pr»a«rvation
of Total organic carbon Samplas With uid Without meid
-------
                                                      Appendix D
                                                      Revision «J
                                                  Date: ll/lfi/95
                                                     Page 2 of 4
              99S  Florida Department of Environmental Protection
         SERP'iCo»p«LnsiVe  Quality  Assurance  Project  Plan
        )    The approval  did not  include  the analysis of  total
       carbon (TOC) by U>A Method 415.1 without pH preservation of
         £l.«  SERF demonstrated through an equivalency  ****.
         SS preserved samples  produced  equivalent results.    In
        to their commentf  SEEP has completed an equivalency study
        atinqTiw  significant difference  in the  results  of  TOG
        with and  without  pH preservation.   The results of  this
study are presented herein.
METHODS
nn 2  March  1995,   two 2-liter  bottles  of  surface water  warn
collected  fro« Florida Bay Station  16  (Murray KeyJ .   «»**««
Sil filled I according to the protocols described in SEW' • ConpQAF.
SSif iciUY   th« bottle* were rinsed three tines with sample vater
o?ior  to bing  filled.  The bottles *«re then stored  in  a dark
coiter JitSo^?i« and  transported to SEBP's laboratory on the same
day of  sample collection.
       laboratory one of the bottles was acidified with 0.5 ml of

                                                      "
                  TOC  and 15 labelled No Acid TOC).  Each of

           1^ '
analyzed.
                                                k method 415.1  as
                                                 and non-acidified
.«*. "«« anTlyzed""^;- thVcoarse^ 33  days from  sample
"Section, corresponding  with EPA's recommended holding tim. for
organic carbon analyses.

RESULTS




ustd  to tMt-5?eregultsy|ro]1 the  acidified  and non-acidified
                                                 population).   The
-------
                                                       Appendix 0
                                                       Revision Q
                                                   Date: 11/16/95
                                                      page 3 of 4
between the TOC concentrations of the acidified and non-acidified
samples*
-------
                                                        Appendix D
                                                        Revision 0
                                                    Data:  11/16/95
                                                        Page  4  of 4
BmltTof Acidified and »on-Jiciaifli«t TQC
s 	 i' 	 if.' "Hr-i^^mmaa
Days
0
1
7
8
13
21
22
23
24
25
26
27
32
33
BS^^BBBiiliBHBiMM^^^Wi^™^^
TOC (mg/lJ
Ho Acid
8.395
6.395
7.489
7.1S6
7.541
6.271
7.559
5,130
6.626
5,616
6.885
7.348
6.385
5.513
— ____ 	 i i ii
TOC lrag/1) 1
Acid 1
8,412 1
6.145 |
7.420 |
7.084 I
7.763
5.915
7.038
4.814
6.130
5.888
6.921 1
7.392
6.568
5,550
-------
        APPENDIX E





SERP Standard Operating Procedures
-------
      Standard Operating Procedures
       fof Total Phosphorus Analyse

Southeast Environmental Research Program
      Florida International University
                Version I

            September 1997
-------
  Table of Contents


  Section       Section

 ^
                                                                fife,

 1 0          TotaJ Phosphorus Methods
 '•'          Sample Preparation                                   2
       I.l-l   Sam-ptePreparation
       1.1.2   Wate- Saiqjte Preparation


 1.2    I0

      '•Z.!  AutoanafyKT Reagents

      1 -2,2  Total Phosphorus Standards
      J.2.3  AutoM^OTfaarun^paj

      1.2.4  AutoamlyaerCiftratkHi and
      1.2.5  AMoanaJj2» Statdown
      1.2.6

 -J          Caloilaticjns
                                                              g

=0         QMJC and Corraaiw Action


0          Total Pfiosphoms Forms
-------
                         Total Phosphorus in Soils and Sediments

Method ID:   R4 Phosphorus.Sed  MI
4,
       This method is used for the determination of total phosphorus in soils and sediments.
       The working range is from 0,5 to 10 mg/L of prepared sample (instrument cal. range).

2-      S^m|2.k,£,regi|rat[gn

       2,1    A portion of the sample is dried at 105° C.

       2,2    The dried sample is ground. Discard rocks.

1
       3.1    Sutfuric acid solution (H,SO4): Add 25 Ml of cone, H,SO4 to DI water and dilute
             to I liter.

       3.2    Potassium persulfate (K,S2OS): Dissolve 4 grams K:S4Og in DI water and dilute to
             1 liter,
       4.1    Do not use commercial detergents for glassware used in this determination.

       4.2    Weigh 0. 1 to 0.2 grams dried sample into an autoclavable phosphorus- free
             container and add 5 ml, D! water.

       4.3    Add 5 ml, of the sulfuric aeid solution (3.1 ) and 10 ml. of the potassium
             persulfate (3.2),

       4.4    Prepare a 100 ppm PO4 as P intermediate standard. A set of standards (suggested
             range: 0.5 to 1 0 mg/L PO4 as P) are digested in the same manner as the samples.

       4.5    Cover the container loosely with a cap or foil and autoclave for 30 minutes at
             250°F(120° C)and ISpsi.
5.      Analysis
       5.1    After digestion, phosphorus is determined by the automated single reagent method
             (Methods for the Chemical Analysis of Water and Wastes, EPA, Method 365,1 ).

       5.2    The wash water is 6.2 mL H2SO4 per liter,
-------
6.

      Dry weight basis;

      Phos rng/kg - ug/g =       .ag/mL phos  \  5 nil
                            gram s sa x ^ is o I ul s {d cc n 11 a 11
                                                                 Sed_TP.wpd
-------
   1.0 Total Phosphorus Methods

  For Hie ddermuation of total phosphorus in water, soii sediment, and tissue samples, SERF does not
  use the typical ammonium persuMate digestion because of the explosive hazards and special handling
  requirements associated with the use of this chemical. Instead, SERF uses a irodiicanQn of the sample
  preparation  methods described by Solorzano and Sharp (1910, Determination of tote/  dfcxrfwa/
  phasphorits andpartiatlale phosphorus in natural waters. LimnoL Qceanogr., 25(4), pp. 754-758 {see
  attached). Total phosphorus is determined in water, soil, sediment, and tissue samples by oxidizing and
  hydroJyzing  all of the phosphorus-containing compounds in a sample to soluble reactive  phosphate.
  Soluble reactive phosphate then is determined by reacting phosphate with molybdenum  (VI) and
  antimony (III) in an acid medium to form a phc^hoantimonylmdybdenuin complex; this complex is
  reduced with ascorbic acid to form a colored dye.

  Anafrj/sis for soluble reactive phosphorus  is performed by wet chemical analysis using a  angle-channel
  Alpkan RFA-5IO Nutrient Analyzer following EPA Method 365,1 and the procedure suggested by the
  Alpten Corporation, modified for optimum conditions in  our  laboratory.   SERF analyzes  total
  phosphorus on a separate autoanaiyzcr from that used for soluble inorganic nutrient analysis.
 LI    Sample Preparation

 Sample preparation for total phosphorus determination is done as soon as possible.  Water samples
 should be prepared within 24 hours of sample collection, and are often prepared imniediatdy upon
 return to the laboratory.
 1.1.1  Sample Preparation Reagents

       Magnesium suUjate	jMgSOjXJLLZ-N'  10.475 g magnesium suMate is dissolved in 250 ml
       DIW.  0.5 ml concentrated sulfurie acid is then added


              0.06 N - 5 ml cone, hydrochloric acid in I L total volume DIW.
              0,12 N - 10 ml cone, hydrochloric acid in I L total volume DIW
              0 18 N - 15 ml cone hydrochloric acid in I L total volume DIW,
              0.24 N - 20 ml cone, hydrochloric acid in I L total volume DIW.
       (Use caution when making add solutions.  Always add acid to water.  The raking of acid in
       water may generate heat.)
1,1,2  Water Sample Preparation

      1.     Prepare a tray with two or three 8 ml scintillation vials (without the aluminum-lined
             caps) per sample bottle plus two vials for DIW method reagent Wanks, two vials for
             SPEX stendards, and two vials for each matrix spike. Add 100 uJofOJTNMigSO*to
             each vial using the 5.0 ml dispenser tip (I = 100 jj) and an Eppendorf pipet setting of
-------
                I. Fin out a tort phosphorus preparation Jog sheet with the pJicement and contents of
               the vwls on the tray.  Record the date the MgSOi used was made,
         2.     AddS ml of sample water into each of the vials.
         3.     Pto ^ » M 8QGC oven and ewoaram to drynes^                 Record the
               log sheet
               Ash thej samples at SSGQC in a muffle furnace for 3 horn and allow to cod overnight
               Transfer the vials from the plastic trays to the metal trays, kc^ the vials in the exact
               same order as outlined on the sample preparation tag sheet A melt pellet (metee
               pout of S5TOC) should be placed in an empty vial in an empty space on one of the
               trays to confirm that the furnace readied 550DC,  Record the dale and time the
               samples were placed in the furnace and removed fit«i tl^ &n«ce and whether or not
               fe pellet melted.  Qnoe coot, return the vials from the metel trays to die plastic trays,
               keeping tl» vials in the exact same  order as outlined on the sample preparation tog
              sheet.                                          ,
                        each sample wth the aM^                          The normaJitv
              of the acid »s dependent on the salinity of the sample according to the Mowing tabfe:



              O.0-I5ppt   0.06 N
              l6-3Ippt           0.12 N
              39-S5ppt           OJSN
              56 - 80 ppt           0.24 N

              Record the date and time the acid was added, the acid con«iitraiioii(s) used, and the
              date
-------
                same order as outlined on the sample preparation log sheet  A mdt  pdlet {melting
                point of 550GQ should be placed in an empty viai in an empty space on one of the
                trays to confirm thai the  furnace reached  SSOQC.   Record the  date and tone the
                samples were placed in the furnace and removed from the furnace and whether or not
                the pete meted. Once cool, return the vials from the metal trays to the plastic trays,
               keeping the vials in the exact same order as outlined on the simple preparation log
               sheet
               Hydrolyze each sample with the addition of 10 ml of 0.24 N hydrochloric acid. Record
               the date and time the acid  was added and the date the acid was made  on the sample
               preparation log sheet.
               Cap each sample tightly with potyiined caps, shake using a vortexer, and put into an
               80DC oven overnight After removing from the oven, aflow to cod and shake again.
               Record the dates and times the vials were taken out of the oven and shaken on the
               sample preparation log sheet.
               Analyze at a I  10 dilution (200 (J of sample with 1 800 pi DIW),
 1.2    Analysis


 1.2.1  Autoanaiyzer Reagents

 Afl reagents are made with the high reagent-grade chemicals dissolved in douWe-^aornzed water.

 Blank and wash water:  The salinity of the blank water and the samples effect the shape of the peaks
 from the autoanalyzer, therefore we match the salinity of the blank and wash 'water to the salinity of the
 samples. Samples with salinities of 1 5 ppt or kss are run with nutrient-free DIW acidified with sulfuric
 acid (Z.OrmYlSL),   Samples with  saftroties greater than 15  ppt are .run with  nutrient-fiiee seawater
 aadified with sulfinic acid (3.0mVI5L), The nutrient-free seawater is obtained from the Sargasso Sea
 and stored in carboys fitted with ammonia traps.  Blank and wash  water are  pumped directly from
these carboys to the autoanalyzer,

Total phosphorus analysis requires ive reagents which are mixed Just prior to the analysis to make a
working reagent.

       Antimony potassium tartrate: 0 J5 g antimony potassium tartrate is dissolved in 250 ml DIW.

       Ammonium., molybdate:  20 g ammonium motybdate is dissolved in 500  ml  DIW.   Do not
       refrigerate.

       SuEjiic add solution:  140 ml cone, sulfuric acid is added to 900 ml DIW.
       (Use caution when making add solutions,  Always add acid to water.  The mixing of acid in
       water may generate heat)

      Ascorbic acid:   6.0 g asoorbK acid  is dissolved in 200 ml acetone and 200 ml  DIW
      Refrigerate
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        Sodium dbdecyl .suMate fSDSX 1 5% w/w:  15 g sodium dodeeyl sulfke is added to 85 ml
        DJW.
            gfg,. qxed reagent:  Combine 50 mJ sulfijric acid  solution, 5 ml antimony potassium
       tartraie solution, 15 ml ammonium molybdate, 30 ml ascorbic acid, and 2 ml SDS,
 1.2.2  Total Phosphorus Standards

 The primary standard for total phosphorus is the same as chat used for soluble reactive phosphate.

                        simdaidJLQOQ |iM:  Dissolve O.I 360 g potassium dihydrogen phosphate in
       i  L DIW, Add 2 ml chloroform  Final concentration is the equivalent of 1,0 ^motes/ml.

       SPEX aandaM. 0,SO,|iM:  1 5.5 pj of SPEX eoncsenttate (1000 ppm) in 1 L total volume DIW.

Working  standards  for water samples are prepared from the primary standard in DIW or Sargasso
Seawater  depending upon 'the salinity of the samples,  For water samples with salinities of IS ppt or
less, standards are prepared in DIW.  Sargasso Seawater is used for water samples with salinities
greater than 1 5 ppt. The working standards are made to bracket the expected concentration of the
samples as shown in Table 3.  A  log book is kept by the total phosphorus autoanalyzer.  In the log
book record the slope and correlation coefficient of the calibration curve, the 'water murk (freshwater
or seavaler), the instrument range setting, the technician's initials, and the preparation dates of the
primary phosphorus standard and five reagents.
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Table 1. Working standards for total phosphorus determination.
Working Standard
Low Standard Curve
SI
S2
S3
54
S5
High Standard Curve
SI
S2
S3
S4
S5
Standartl Curve for
Solid Samples
..
S2
S3
S4
JS5
Volume of Primary
Standard in 100 ml of
DIW or Seawater

10 pi
SO pi
100 ml
1 50 pi
200 pi

125 pi
250 nl
500 pi
750 pi
1000 pi

125 pi
250 pi
500 pi
750 pi
1000 pi
Phosphorus Standard
Concentration (pM)

0.10
0,50
LOO
l.SO
2.00

1.25
2.50
5.00
7,50
10.00

3-8? pg/g
7-?4 pg/g
»S,48pg%
23.22 pg/g
30.97 pg/g
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  1.2.3   Autoanalyzer Instrument Parameters

 Alpkam Rapid Flow Analyzer (RFA, AJpkem Corp., Clackamas, OR}) Model 510 with
        Sampler Model 301
 Ffowcdl: 5,5 mm
 Filter: 660 nm
 Heat bath: Omega Model CN90QGA, 45 CC
 Rise time: 3 sec,
 Absorbance range: 0.02 (for low standard curve) or 0.1 (for high or solid sample  standard
 curves) AUFS
 Sample time; 35 sec.
 Wash time; 65 sec.
 1.2.4  Autoanalyzer Calibration and Operation

 After power is turned on to all units and the tubes are reconnected to the rollers, start wash water
 (DlWor sea water, depending on the samples to be analyzed) and mixed reagent flowing through
 the autoanaJyzer Then flush the instrument for at least 10 minutes or until the baseline is stable,
 then press autozero   Load a few vials of high standard (S5) to be analyzed until 60% fl scale is
 achieved  The computer table is then created with the samples to be loaded.  When the samples
 are loaded, press
 Alt-1, wait 20 seconds, then press start on the sampler.

 Each run of the autoanalyzer begins  with the  running of a SYNC cup (SS) then a wash water
 blank,  A complete set of blanks and the 5 working standards described in Table I are then run.
 Following the standard curve is a carryover (which is the tow standard SI), a low standard (Si),
 and a check cal (S3)   Additionally, a blank sample  and an S4 are placed after every 10 sample
 viais in an autoanalyzer run to monitor baseline and  tntra-run calibration drift.  At the end of the
 run, at SS cup is run again,
 Samples that are out-of-range of the standard curve are diluted and reanalyzed.
L15 Autoanalyzer Shutdown

The following reagents are needed:

      Sodjyum jiydroxide (NaQHX I N: 40 g of sodium hydroxide is added to I L of DIW.

      Hydrochloric jBadXHCJL10% vhr.  100 ml of cone, hydrochloric acid in 1 L      total
volume.

Mar the last samples are analyzed, the instrument should be flushed with fresh wash water for 5
rain, 1N NaOH for 5 min, 10% HCI for 5 min, DIW for 5 min, and air for 5 min.  Turn off the
power at the power strip (heat bath remains on all the time). Remove the tubes from the rollers.
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  1.2.6 Autoanalyzer Preventahve Maintenance

  All spills are immediately cleaned up.  Following solid  sample anafyses, NaOH and  HQ ire
  flushed through the tubing longer (10 min each) or are pushed through with a syringe for greater
  pressure.  Any worn tubing is replaced immediately,


  1.3   Autoanalyzer Calculations

 Mpketn SoftPae  Plus  version 1.07 release 1.0 software is  used.   Absoitance  is  directly
 proportional to phosphorus concentration and is measured as peak height units. The peak heights
 on the output have  been corrected by the software  for carry  over and baseline.   The slope,
 intercept, and correlation coefficient are calculated by the software by first order regression.  The
 value for any  given  sample  is then calculated by (peak  height units  - interceptysiope.   The
 intercq* will impart i false concentration to all the values (ie. on the low scale, the  calaMon
 will mull in Wanks with 0 peak height units having around a 0,0? ^M concentration)  As the
 software is not aHe to automatically correct for this, the false Wank value must then be subtracted
from d results.  The earrectioii will be done in the data entry of the values.
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 tO   QA/QC and Connective Action

 The standard curve should have a correlation coefficient 0 0.995 and the slope of the line should
 fell within ± 2 S.D, of tlw historic mean (the allowable range is listed on the inside cover of the
 logbook),  A Ming  slope or correlation coefficient indicate  the need for either preventive
 maintenance on the autoanalyzer or re-maMng of the standards.

 To carry over (CO) shouJd be D 3%. The S4 continuing calibration checks should be ± 5% of the
 S4 value,  Equipment blanks and method reagent blanks should be D MDL (0.02 uM), QC check
 standards (SPEX or citrus leaf standards) should be ± 5% of the expected value.  Matrix spikes;
 should be i  S% of the expected value.  The precision of the 2 - 4 values produced for every
 sample should be Q 3%.  Outliers (> 1 S.D. of the mean) ean be disemded. Any samples and runs
which do not meet  these criteria may need to be reanalyzed. If a problem continues, preventative
maintenance on the autoanalyzer may be necessary.
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3.0    Tolil Phosphorus Forms

The ample preparation log sheets for water samples and solid (soil, sediment, and tissue) samples
ire shown in Figures I and 2. Figure 3 is a copy of a page from the instrument logbook.
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Fijpre 1.  Sample preparation log sheet for wattr simples.
                                                 ^r-     scwrrsw*.* r*w*,j
                                                  *      «"-• — rcn»n»i
fl..;a  .
                                                         Pnp.
                                                         S «i
                                                         puc LH OWMI (Bfl-Cl;
                                                         (OiCB K<}Sa, IMH BUM        t
                                                                             Init.
                                                              out at
                                                                     timm
                                                        Ate IA «M
                                                           Ck4t«
                                                                            I •!.(.
                                                                  a( «•
                                                        Old Ch* p«Ll«C -Bil? _____

                                                        Mi  MM  (S  *l  *CH,  MMJM,
                                                        w( pic La
                                                             VMTLWI.  put  ea*  i«ttor
                                                           15K5      THi    Init,

                                                         TBtaM owe oC «MMI

                                                           Die* ~~"   :flmm    [011.
                                                            a*c«      ¥!••    lilt.
                                                           	D«CB      tl»»    Invc.

                                                                  or  proalwn:
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Figure 2. Sample preparation log sheet for solid samples.
                                                        SOP 77 ZS» v.l  fan ~,

                                                        Tray
                                                             1200 jil 0.17N KqSO. - 1 at
                                                       Dili * -If mf •U^l« p«r •» V411 4IM
                                                       put  US OWiHI 180'Cl:
                                                            M^SO, LUB
                                                             one of  ov«n:
                                                       Puc LO anlft*  owmi (5SOT|:
                                                                            (nxt.
                                                       TlltMl out
                                                                    fT«

                                                       Old th»
                                                       MM *crd  (10 .X  0.2*11
                                                              i«d  put  in  av«n |«O*C1;
                                                             ciue  at
                                                          Bitii
                                                             'Cm or
-------
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      Standard Operating Procedures
 for Laboratory and Field Nutrient Analysis

Southeast Environmental Research Program
      Florida International University
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I
 Table of Contents

 Section Section                                         Page
 No.          MiH§                                                 No.

 1.0          Introduction                                           2

 2.0          F«W Procedures                                        3
 2)           Equipment Preparation                                  3
 2,2          Water Sample Containers and Cleaning                     4
 23           Water Sample Collection                                 4
 2.4           Soil/Sediment/Ttssue Sample Collection                    6
 2.5           Held Measurements                                     7
       2.5.1   Field Measurement Corrective Actions                     I
       2.5,2   SaliratyCowfcicdvity/Temperatuiie                         8
       2.53   Dissolved Oxygen                                       8
       2.5.4   Light Measurements                                     9
       2,5.5   pH                                                    10
       2.5.6   SEA-BIRD CTO                                        II
 3.0           Laboratory Procedures                                  IS
 3,1           DIW and Glassware Cleaning                             15
 3.2           Inorganic Filtered Nutrients                               15
 3,3           Total Phosphorus                                        21
 3.4           Total Nitrogen                                          24
 3.5           Total Organic Caibon                                    25
 3.6           ChlorophyU-a                                           26
 3.7           Alkaline Phosphatase Activity                             27
 3,8           TuiMdity                                              2S

40           QA/QC Samples                                        30
4. ]           Equipment Blanks                                       30
42           Matrix Spike Samples                                    30
4.3           Continuing Calibration Check Samples                     30
4,4           Quality Control Check Samples                           30
4.5           Sample Shipping and Cham of Custody                     30
4,6           Standard Receipt                                        31

5.0           Forms                                                 32

6.0           References                                             31
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 1.0    Introduction

 This document describes SERFs standard operating procedures for the collection and analysts of
 nutrient  samples.  The purpose of the document  is to  provide a cookbook of procedures and
 instrument operation used on a daily baas by SHIP employees, SEEP typically collects and analyzes
 bath fresh and saline surface waters for nutrient analyses. Soi/sedhnent and tissue (plant, fish) samples
 are processed and analyzed on a United basis, and  are also deserted in this document. Standard
 operating procedures used in SERFs mercury laboratory are presented in another document.
3) QAQC samples. A detaied description of SEUPs QA/QC pfocedures for the nutrient laboratory is
presented in SEMFs CompQAP.  to general, most QA/QC procedures are overseen by SERFs QA
•Officer.  Section three of this document describes only QA/QC simples thai need to be processed by
the laboratory tediwciaiB on a day-to-day basis,
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  10    Fidd Procedures

  2.1    Equipment Preparation

  Preceding a tnp to the field, the personnel responsible for collection of the samples are required to
  ensure  that  everything is prepared for the expedition.  This entails  making sure  that all sample
  containers are clean and properly labelled, and that ail sampling and field measurement equipment are
  properly deaned, charged and functioning within acceptable inks. Table I is an equipment checklist
  prepared for the sampling team.

 TABLE I
  Fidd Equipment Checklist

 Surface Water Sampling Equipment
  1.     Labeled and cleaned sample bottles (narrow-mouth plastic)
              60 mL (2 per site)
              125 mL (2 per site)
 2,     140 mL clean plastic syringes
 3,     Microceritnfuge tubes
 4.     2.5 cm in-line filter holders
 5.     2.5cm Whatman GF/F glass fiber filters
 6.     Filter forceps
 7.     2-5 gallon plastic bucket
 8,     Niskin sampler

 Field Measurement Equipment
 1,     S/C/T nwter and probe
 2.     Dissolved oxygen meter and probe
 3.     Spare meters and probes
 4,     Salinity/Conductivity Check Standard,
 5,     Light Sensor
6.    CTD
 7.     pH meter and buffers
 8     Instrument manuals

 Sample Preservation
 I.     Acetone {90%)
2.    Disposable polyethylene bottle
3,     Ice
4.    Coolers
5.    DI water (IL) for Equipment Blanks,

Boat Equipment                         Miscdtineous Equipment
 1.    GPS                              1.     Fidd data sheets
2.    Radio                            2,     Pencils
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 3     Portable Photic                           3,     Labd tape and waterproof pens
 4     Life Vests                                4.     DIW squeeze bottle (filled)
 5.     Depth Finder
 6.     Boat hook
 7,     Emergency Flares
 8.     Charts
 9     Tool Box
 10    Fire Extinguisher
 2.2    Water Sample Containers and Cleaning

 SERF typically collects three types of water samples:  1) filtered soluble nutrient samples; 2) unaltered
 total nutrient samples; and 3J cWorophyll-a samples.  Clean 60 mL HDPE bottles are used for filtered
 nutrient samples.  These bottles are cleaned by first rinsing three times with distilled water, then rinsing
 once with acetone to aid in drying and to remove organics. The bottles are shaken dry then capped.
 Clean 125 mL HDPE bottles are used for total nutrient samples.  These bottles are cleaned by rinsing
 three antes with distilled water.  Acetone is not used to dean the 125 mL bottles for totals analysis,
 l.S mL nnicrocentnfuge tubes are used to store the chlorophyll  samples.  These are used once then
 discarded Filter holders and syringes used to collected the filtered and chlorophyll samples are rinsed
 wdl with distilled water.  Syringes are allowed to air-dry in die dish drainer. Filter holders are placed
 right side up on a plastic tray and placed in an 80°F oven overnight to dry. Once dry, Whatman GF/F
 25 mm filters are placed in each holder. At the end of each field  day, all field instruments and coolers
 need to be wiped down with fresh water and dried before storing,

 23    Water Sample Collection

 Specie sampling locations are project specific.  In general, surface water, sediment, and plant tissue
 samples are collected from a boat, helicopter, airboat, or by a SCUBA diver.  To enure collection of
 undismrbed samples, the boat is advanced toward a sampling station from the downstream direction,
 Surface water samples are collected as grab  samples away from the outboard engine.  Sediment or
 tissue samples are collected by SCUBA diver or by wading toward the  sampling location  from  the
 downstream location. If surface water samples and sediment and/or tissue samples are collected at one
 location, then the  surface water samples are collected prior to  the collection of sediment  or tissue
 samples,  in areas of suspected high, concentrations such as  downgradient of a landfill, samples  are
collected ie order of suspected low concentration to higher concentration.

2J. 1          Filtered Water Samples (for soluble nutrient determinations)
       a.      Use dean 140 mL polypropylene syringes to collect filtered surface water samples.
       b.      Place the syringes to draw water 10 on  below the surface of the water into  the
              direction of water flow {if applicable).
       c.      Partially 61 the syringe and rinse with sample water three tunes,
       d      FiM the syringe with 120 or 140 mL of water.
       e.      Attach a filter holder (containing a new filter) to the end of the syringe and force about
              10 mL of sample through the filter to rinse.
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       f.      Use the remaning ffltraie from the syringe to rinse a 60 mi HDPE sample beetle three
              rimes.
       g.     Fill syringe with sample water again (if necessary^ and re-attach Star hokJer with filter.
       h      FIJI sample bottle to bottom of neck.  Multiple syringe volumes may contribute to a
              single sample bottle,
       i.      Repeat steps 
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 sampling location, pnor to collection of the sample.  Sample bottles, syringe, and filters are then rinsed
 and fiJIed from the water collected in the bucket followuig the procedures described above
 For water samples collected from a specific depth in the water column, a Niskin Sampler is used.  A
 metered line  is attuned  to the  Niskin sampler and, while open, the sampler is lowered to the
 appropriate depth. The sampler is considered to be rinsed as it is lowered through the water column.
 Once at the desired depth, a weighted messenger is sent down the fine to activate the dosing of the
 simpler, Water in the sampler is  extracted from a sample port at the bottom of the sampler.  Water
 collected from one cast of the sampler must be used to rinse and 5U all sample bottles and syringes.

 2.4     Soil/SedimentTissue Sample Collection

 The collection of soil/sediment/tissue samples are not commonly done, but are project specific.  For
 collection of these samples, they are stored in a cooler with ice while in the field, and upon return to the
 laboratory they are stored in a freezer.

 2.41  Surface Soil Samples

 Surface soil samples are collected from the upper 10 cm of an undisturbed location.  Surface  detritus is
 removed prior to sample collecnon  The surface soil samples are collected with at stainless sted trowel,
 spade, PVC core, polycarbonate core or by hand and placed into plastic, wide-mouth specimen cups.
 The  physical parameters of the soil, including color, moisture content,  presence of biota, and texture
 are described in the field notebook, if required to satisfy the project objectives. The sample depth, date
 and time of sample collection, and the amount of sample (or subsamples) collected are also recorded  in
 the field  notebook.  Roots may or may not be removed  from the soil samples depending upon the
 project objectives.

 Soil  samples are homogenized either in  the field or in the laboratory,, depending upon the project
objectives.  If homogenized in the field, the soil sample is placed into a  polypropylene mixing tray and
homogenized by slicing, mixing, and remixing of the sample.  The homogenized soil sample is then
placed  into a  wide-mouth specimen cup and stored in a cooler in the dark  for transport to the
laboratory.  In  the laboratory, soil sample are homogenized by mixing the entire sample in a blender.

2.4.2  Subsurface Soil Samples

Subsurface soil samples are collected using father polycarbonate or PVC core tubes, pushed into the
sod or sediment by hand by twisting the tube in a circular dock-wise and then in a counterdock-wise
movement  The depth of the soil surface on the outside and on the inskte of the ccwtoibeb measured
and recorded to determine compaction.

Once the core  is extracted, plastic caps or neoprene rubber stoppers are inserted and taped to the end
of the tube to prevent slippage and spillage. The top direction of the core tube is marked on the tube
along with the sample number and the tube ii  stored in an upright position during transport to the
laboratory.  In  the laboratory, the soil or sediment is extracted from the core tube and using  a stainless
sted knife, a sample for analysis is collected from the center of the  tube, away from the skies.  The
physical characteristics  of the soil are described in the field notebook,  along  with the approximate
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 amount of sample (or subsample coUected),

 In general, soil  sample composting or  splitting k the field is  not preferred  due to potential
 contamination concerns; the collection of duplicate samples in the field by collecting soil from the same
 sample source and homogerMzatoon of the samples in the laboratory with a Mender, is preferred.  If
 samples are to be homogenized in the field, then the samples wil] be extracted from the cote tube onto
 a polypropylene tray and mixed with a stainless sted or Teflon spatula,  The homogenized samples are
 then placed  into plastic, wide-mouth specimen cups and stored in a cooler in the dark for transport to
 the laboratory

 14J   Sediment Sample CoOectioii

 Sediment is  collected using either polycartioiate or PVC core tubes  or with an Ekman Dredge. The
 sediment sample is removed from the tubes or dredge and placed in a polypropylene tray. A stainless
 sted knife is used to  collect a section of soil from near the center  of the sample container.  These
 samples may be homogenized in the field by mixing with a spatula or homogenized in the  laboratory
 using a blender. Samples are stored in plastic wide-mouth specimen cups and stored in a cooler in the
 dark for transport to the  laboratory.   The amount of sediment collected,  ail eqppment used, the
 method of homogenkation, and the amount of sample stored are documented in the field notebook.

 2,4,4   Tissue Sample Collection

 Plant tissue  samples are coUected by gathering the plants  by hand and placed into plastic bags. The
 plant samples are kept in a cooler on ice until transported to the laboratory

 15    Fidd Measurements

 SERF typically measures temperature,, salinrty/conductivity, and dissolved oxygen at die surface and
 bottom of the water column at each station  For some projects, pH and  light measurements ire
 measured.  All field  measurements are taken contemporaneously with the sample collection to ensure'
 direct correlation of laboratory results with field measurements.  The water depth is determined from
 either a depth finder on the boat or from a weighted,  non-stretch line that  is marked,  in 10 cm
 increments.   The calibration of aD field instruments needs to be checked it the beginning of each day.
 after every four hours of operation, and at die end of each day.  Instrument performance  at each
 calibration check needs to  be recorded on the field instrument calibration sheet (see attached). AH
 instruments need to be fuUy charged overnight prior to their use in the  fidd

 A new ReM  Dati Sheet has been prepared (see attached).  This sheet  rnust be copied onto bond-water
 resistent paper and put onto t clipboard to take to die field   The sheets may be filled out in pencil;
however, errors are not allowed to be erased.  If an error is made, corrections must  be made by
drawng a single line through the error and entering the corrected information next to the error, then
initialling-

L5.I   Field Instrument Corrective Actions
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  A primary and backup meter and probe for each field instrument are brought on every sampling event
  If both the primary and backup field mstnjments fail during the trip, then the sampling event should be
  discontinued  until  proper functioning equipment can be obtained   SaJWty measurements are an
  exception to this ruJe If the S/GT meter is not functioning properly, the D.O, meter can suit be used
  in the following manner. Adjust the D.O. meter to a saUnity of zero  Record the temperature and 0,0.
  for each station on the Fidd Data Sheet, noting which stations the D.O. was measured using a salinity
  of zero.  Note the maJJunetiofi of the S/C/T meter on the instrument calibration sheet.  Back at die
  laboratory, use a functioning salinity meter and probe and record the salinity of sample remaining in the
  totaJ nutrient bottle on the field instalment sheet  The D.O, of each sample will then be corrected for
  the appropriate salinity,

  25.2   Sftiinity/Conductiviry/TempeiTiturT

  Salinity and/or conductance is checked daily with a solution of known salinity or conductance, while
  temperature is checked  daly against an MIST  thermometer. The S/OT meter probe and the NIST
  thermometer is inserted into 50 - 100 mL of the salinity or conductance standard. A salinity reading
 within 5% of the standard value, and a temperature within 0.1  degrees are considered acceptable.  If
 Sargasso  Seawater is used as the salinity standard, a value of 36,1  should be obtained, but values
 between 34,3  and 37.9  ppt are considered acceptable.   Values outside these acceptance criteria will
 requires the unit to be factory calibrated and the QA Officer or Dr. Ron Jones needs to be notified

 Surface temperature and salinity/conductivity is measured   by  submersing  die probe of  the
 saUn^/amducMvity/tcsnperature  (SCT) meter 10 cm under water. After the digital readout stanfees
 {less than 5 minutes), temperature is recorded in "C and salinity is recorded in parts per thousand (ppt).
  Conductivity is recorded in units of pnthos/cm.  The probe is then lowered to  10 cm from the bottom
 of the water column  After the  digital readout stabilizes, the bottom parameters  are recorded in the
 field notebook. Rinse the probe with DIW between stations, and shut the insmiment off

 2JL3  Dissolved Oxygen

 The  probe of the Orion model 840 Dissolved Oxygen meter is continuously polarized when attached to
 the meter,  if it has been  disconnected for over 1 hr, it requires  50 rain to repolarize.  No readings or
 calibration should be attempted within 50 min of connecting the probe. The calibration procedure is as
 follows:

       1.      Saturate the sponge in the calibration sleeve with detanked water and wait 50 rrun for
              ecjuilibratiort
       2.      Switch the meter on.
       3.      Depress and hold  the Mode Key  Pad until the display cursor is at Cal.
       4.      Depress quickly and rdea.se the Mode Key Pad  The display  will show three dashes j>
              -) and tine slope of the dectrode/membrane system A slope reading  between 0,7 and
              1.2 is considered acceptable.

 If calibration can not be property obtained, take the probe out of the sleeve and look  at the membrane
on the bottom  Check that there are no air bubbles and that the silver ring is silver color and the gold
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 cathode is gold in color  If air bubbles are present, remove the cap at the bottom of the probe, fill the
 cap wh new dectfoJyte solution and replace maJcing sure ttwc are cio air littles. If the membrane is
 damaged or loose, replace the entire membrane cap. If me aJver ring aixi/or gold cathode is tarnished,
 scape them carefully with a small glass fiber brush,  Soak for rwo hours in cleaning solution, then for
 [wo more hours in distilled water. Any time that the membrane cap is removed font the electrode, a
 minimum of 50 min is required for the instrument to repolarize prior to use,

 To take D.O readings in the field:
       I.     Remove the sleeve from the probe  Be  sure not to drop the sleeve in the water.
       2.     Submerse the probe 10 on beneath the water surface,
       3.     Use the Mode Key Pad to select the Cal mode,
       4,      Adjust the salinity display with the up and down arrow keys to match the previously-
              measured station salinity.
       5.      Use the Mode Key Pad to select readings in mg/1.
       6,      Gentry stir the probe until a constant reading is obtained
       7.      The probe should be rinsed with DIW between each station, and the instrument can be
              turned off between stations,

L5.4   Light Measurements

Light measurements are made utilizing two-4O sensors  mounted  on a PVC pipe and attached by cables
to a meter The distance between the sensors can be adjusted to 0.5 m or  1.0 m. The 1.0 m distance is
prderedif the depth allows CalibraOon of the instrument shoutld be as follows:

       I.      Plug the cables from the sensors into the meter (LI-1000).  Check that 'the numbered
              tags on the cables match  the channels of the meter, and that the Sensor probe tf
              matches the # on the meter.
       2,      Turn the meter on, and wait foe the display Hit the Chararf button. It should read MA
              for math, if not, continue  pressing  the Channel button until MA is displayed,   The
              number following MA, ending in the letters PC, is the  ratio of light at the bottom
              sensor to the top sensor.  Tr^ is the number thit you will be recording
       3.      Check the c^libniton of the instmn^
              vertical position over a non-reflective surface such as still water,  pavement or grass
              (not a white boat bottom or concrete dock).  Record the instrument calibration reading
              on 'the instrument calibration check sheet
       4,      The calibration reading  should be between 098 to  1 02 in air over a non-reflective
              surface,

If the calibration is within this range, check thai the multiplier for each sensor is correct
       1       Hit the CFG key once
       2.      Using the ENTER key scroll through the options for light-1 unti MULT- is obtained.
              Enter the negative multiplier number for sensor I in water.  The multiplier number
              should be on the tag attached to each sensor.
       3.      Hit enter and scroll through the options for Ught=2 until MULT- is obtained,  Enter
              the multiplier number for sensor 2 in water.
-------
        4      Hit  the  CHAN key until MA  is displayed  Cheek thai the catibranoit readira ts
               between 0.98 and 1,02.

  If ihe calibration is suM outside this range, instrument readings need to be made according to the
  following procedures:
        1.      Ai each station, determine the depth with the sounding line,  tf the depth is greater than
               1 m, adjust the sensors lobe 1m apart Recoid this distance as lew the dati sheet,
        2,      Stand on the amny side of the  boa.   Be careful when advancing to a station, that
               sediment is not srirred-up  into the water column. If necessaiy, move the boat  to a
               sunny, undisturbed location,
        3       Turn the instrument on.  Hold the PVC pipe with the sensors in a vertical position te
               ensure that the distance between the sensois  is indeed Im (or &5n\ if neees&yy).
               Submerge the sensors so that the top sensor is completely submerged.  Be careful not
              to hit the sediment bottom and stir-up mud, as this will invalidate the reading.  Also
              check that the bottom sensor is not covered with seagrass or algae.
       4.      If the instrument calibration was within  the occepted range, then the ratio IA can be
              read directly from the meter on the MA (math channel).
       5.      If the instrument b out of calibration, psadinp can not be made using the MA (math)
              channel.  Instead,  the incidence of light needs to be recorded  for each sensor
              individually
       6.      Depress the channd button until  IA appear*  Record leading for the first channel on
              the data sheet. Press the Channel  button again until 2A appears, and record the reading
              for the second channd. Minimize the time between recording the readings between the
              channels,
       7.      Turn the instrument off between tradings,

L5J   pH

An automatic temperature compensation (ATC)  probe  on the pH meter adjusts the pH reading for
temperature differences between stmduds and samples. The pH meter/probe is caibraied using a two-
point calibration as follows:

       I,      Choose pH G 01 mode
       1      Rinse probes (pH combination and ATC) in DIW. Blot dry. Rinse with 2 mL of pH
              7,00 bufe,  temerse probes in pH 7.00 buffir,
       1      Press CaJ button.  The meter will display*!, "and the pH value of the buffer, the meter
              automatically recognizes the pH  of the buffer solution. When pH stabilizes, press
              Enter,  The display will freeze for 3 seconds, and then display "2,".
      4      Rinse probes in DIW.  Btot dry.. Rinse with 2 mL of pH 10.00 buffer. Immerse prates
              in pH 10.00 buffer
       5.      Wait for pH display to stabilize, and press Biter.  Display now wiU say "PH" and be
              ready for sampk measurement
      6.      Rinse probe in DIW, placeprobe in pH 7.00 buffer, and cl«k that pH meter reading is
              within 0.05 pH units.
-------
 The response of the pH meter is checked with the pH 7 00 buffer after 4 hours of use and at the end of
 each use.  If the response is outside 0.05 pH units, the two^nt aiibraikKi is r^je^ed.  If instrument
 calibration can still not be achieved, then the instrument needs to be factory calibrated.  pH is
 detemuned at each station by collecting a sample of surface water in I dean, 400 mL polyethylene
 beaker alia" it is rinsed three tunes with sample water. The pH probe and ATC probe are submersed in
 the beaker, and the pH is recorded in the field note book.  Successive aliquots of surface water are
 collected until the pH of three successive aliquot agrees within 9,02 pH units.

 15.6  SEA-BIRD CTD (Modd: SEACAT SBC IW)3)

 Fidd measurements  detemuned  with the  CTD  include temperature, salinity,  dissolved  oxygen,
 photosynthettc  active radiation, turbidity, and depth.  These measurements  will be made using the
 SEA-BIRD CTD in profile mode.  At the beginning of every day prior to going out in the boat, set up
 the CTD according to die following procedures:

       I       Plug the computer cable into the CTD by removing the niber waterproof cap fest (do
              not lose this) and lining up the fat prong with the fitt hole.
       2.      Plug the other end of the computer cable into the back of the computer
       3      The CTD should be turned off! Check thas.
       4.      Turn on the computer.  After the C:\ prompt type cdteasoft. Once in the seasoft
              directory type TERM 19  Any tone that you ever want the SEA-BIRD to talk to the
              computer, you lave to be in the TERM 19 program.
       5.      Once in TERM 19, type DtS.  This cA^clcs the sams of the instrument  Check that the
              instrument is in die PROFILE mode. K" not, then type MP. Check that the pump delay
              is on 45 seconds.  If not, type SP and set minimum conductivity to 2500 and pump
              delay at 45 seconds. Check that the time and date are correct If not, type ST and set
              the current date and time,
       6.      Check that the battery charge is 7.0 volts or greater.  If less  than 7.0 votes then the
              batteries need to be changed  Six D cdl  batteries ate needed.  Read the instrument
              manual on how to change the batteries,
       7.      Once you are comfortable with the irismjment «tingSi and ttefe is no data in the CTD
              that you want to save, press IL to initialize logging. The instrument will ask if you are
              sum Initialize logging will erase aO of the stored data ia the instrument's memory, so
              do not initiilzeloHpng if there is data you siffl want to retrieve. If you are sure you
              want to initialize logging, type Y, then control Y.
       §,      Type QS for quiescence mode. This is an important step.  Without this step the CTD
              will not record data. If you do not want to erase the data in die €10 memory,, but just
              continue saving casts,  then do not do the initialize logging step, just go  into the
              quiescence mode.
       9.      Once mQS mode, quit TERM 19.

To take measurements in the field you have two options,  You can allow the CTD to record  data
internally, and/or you can see the real  time data by taking  the computer out on the boat with you. If
you don't have the computer, then be sure that the computer cable cap Is secured in place  prior to
lowering the instrument in the water.   Simply tuning the magnetic switch on and off will make the
-------
 instrument record each cast separately. The data can then be downloaded at the end of the day. If you
 have the computer on board, then cornea the long computer able to the CTD and computer and
 proceed as follows:

       10.    At the C:\scasoft prompt type Seasave.
       II,    Hit Acquire Real Time Data
       i 2,    Check that the data is saved to the appropriate directory
       13,    Hit FtO to acquire real time data.
       14.    Fill in header information, then hit escape to quit.
       ] 5.    The computer screen should read "Ready to turn CTD on".

To mike a cast be sure to do the following;

       [      Confirm the instrument  is property secured with a fine  For deep stations, you may
             want to have the end of the line tied to the boat Do not use the computer cable as the
             support line for the CTD.
       2.     Remove the protective tubing from the conductivity cell, and don't lose this. Mug Ac
             tubing connecting the DO probe to the conductivity ceil.
       3      Turn the instrument ON  by flipping the magietic switch on the skte of the uistnunent.
       4      Lower the instrument to just below the surface of the water (appro*. 0.5m).  Keep the
             instrument there until all of tl« bubbles have  escaped the instrument, This allows the
             instrument to equilibrate with the water temperature as well as compensates for the 45
             sec pump deity.
       5.      After  45 sec, lower the instrument to the bottom of the station, then retrieve.  The
             optimum speed of lowering is Im per second, however, the pump on the  instrument
             helps to compensate for differences in lowering speed.
       6.     Once the instrument is on the boat, turn it OFF.
       7,      Follow steps 10 through 15 above to set up the computer for the ne^

At the end of each day, the data must be downloaded from the instrument to the computer.

       I.     Rinse the  entire instrument with fiesh water.  Rinse the  conductivity  cell  weU with
             deioruzcd water Put fresh D1W in the conductivity eefl tubing and replace.
       2.     Phig the computer cable into the SEA-BIRD CTD and irtooie bade of the computer.
       3,     Type CPSEASQfT, then TERM19.
       3.     Type  OS  again to cheek the status of the instrument This in  an  important step to
             establish the connection between the coinpiitaraalth«iiKiiument
       4.     Type DHL The SEA-BIRD wtU then begin to ro^ through each C3^ stanmg with m
       5.     Press  the  F9 Key to upload the data.   Each cast will be saved separately under a
             common name.  Only six characters are allowed  for a fie name and the program
             automatically attaches two characters to the end of the name, therefore, you must limit
             you file names to four characters.  Each east wul be saved in sequential order such as
             XXXXQO; XXXXD1,  XXXXQ2, etc.   For each cast,  header information will be
             requested  such as cast number, lat, tang, notes, etc.  Fill out this infiMTnation for each
             cast.
-------
6.     Once all of the data is uploaded, backup up tile data on i disk.
-------
 3.0     Laboratory Procedures

 11     Dl W and Glassware Cleaning

 Two types of anaiyte-free water are produced in the laboratory: daorazed-
-------
 above. The nitme  concentranon before reduction is subtracted  front the nitrite concentration after
 reduction to give  nitrate concentration.   Soluble  reactive phosphate is determined  by reacting
 phosphate with molybdenum (IV) and antimony (HI) in an acid medium to form a phosphoantmioTOl-
 mdybdenum complex; this complex is reduced with ascorbic acid to form a colored dye.

 32.2 Autoanalyzer Reagents

 Ail reagents are made with the high reagent-grade chemicals dissolved in double-deiomzed water.

 Blank and wash water:  The salinity of the blank water and the samples effect the shape of the peaks
 from the autoanalyzer, therefore we match the salinity of the blank and wash water to the salinity of the
 samples.  Samples  with salinities of IS ppt or less are fun  with nutrient-free DIW,  Samples with
 saiimites  prater than  15  ppt  are  run  with nutrient-free seawater acidified  with sulfuric acid
 (25%L/IOOOmL). The nutrient-free seawater is obtained torn the Sargasso Sea and stored in carboys
 fitted with ammonia traps.  Blank and wash water are pumped directly from these carboys  to the
 autoaraiyzer.

 Ammonhiin reagents:  Four separate reagents are required by the autoai^yaer for ammoifflurn analysk
 compJexing reagent, alkaline phenol, hypochlorite and, nitroferricyanide.

       Ccmptecing reagent   25g sodium citrate is dissolved in 500 mL of DIW  05 mL of 10 N
       sodium hydroxide is then added.

       Alkaline phenol: 5 mL of 10 N sodium hydroxide and 10 mL 20% phenol in ethanot are added
       to 100 mL of DIW.   Store  this  reagent in an amber bottle  where it is stable at room
       temperature for a month.

       Hypochlorite.  10 mL fresh hypochlonte is added to 100 mL DIW This reagent is not stable
       aril must be made daily

       Nitroferricyarude:  0 25g sodium ratrofemcyanide is dissolved in 500 mL DIW.  Store in an
       ante" bottle where it is stable at room temperature for a month.

 Nitrite  reagents:  Two  reagents are  required  for  nitnte  analysis:  sulfanilamide  and N-l-
 naphthylethylenediamine.

       Siifanilamide:  Cautiously add EOO mL cone  hydrochloric acid to 700 mL of DIW.  Dissolve
       10 g suifanilamide. Dilute to 1 L total volume. Store the solution at room temperature or the
       refrigerator.
                                 (NED):  Dissolve  I g of NED in 1000  mL DIW.  Store the
       solution in a dark bonk in the refrigerator.

Nitrate reagents: Nitrate determination requires the reagents bed above for nitnte, plus an inidazole
buffer and cupncsulfate.
-------
•              Imidazole buffer  681 g irmdazole is dissolved in I L DfW.  The pH of this solution is
                adjusted to 7 5 by the addjtion of hydrochloric acid,  Store in a tightly sealed bottle at room
                temperature

                Cypric sulfate:  0.3125 g of euprie sufrate is dissolved in 125  mL DIW.  This solution can be
                stored indefinitely at room temperature.

         Solute reactjyejhpjnjhatc.n?aienjg: This requires four reagents* three of which are mixed just prior to
         the analysts to make a working reagent. The components of the mixed reagent are antimony potassium
         tartraie, ammonium molybdate, and sulfuric acid. The fourth reagent is ascorbic aad

               Antimony potassium tartrate: 0 75g antimony potassium tartraie is dissolved in 250 mL DIW

               Ammonium molybdate: 6,667g ammonium molybdate is dissolved in 500 mL DIW.  Do not
               refrigerate.

               SuJfunc acid solution:  140 mL cone, suJfuric acid is added to 900 mL DIW

               Ascorbic acid:  6 Og ascorbic acid is dissolved in 200 mL acetone and 200 mL DIW

^             Working mixed reagent: Combine 50 mL sulfunc acid solution, 5  mL antimony potassium
P             tartraie solution, and 45 mL ammonium molybdate,

         3.L3 Au toanalyzer Standards

         Pnmary standards are made by dissolving anhydrous  salts of the anaryte of interest in D[W, and
         preserving the standard solutions with chloroform.  All primary standards iraist be made using grade A
         flasks and stored in the glass bottles marked for these standards, Al primary standards must be made
         up cm at least a quarterly bask  Once made, the standard bottles need to be dated and initialed  Prior
         to discarding the old standards, both the new and old standards should be run on the RFA. The new
         standards should be within 5% of the old values. Once this is confirmed, then the old standards can be
         discarded.

         A combined mixed standard is made by combining the primary standards of' nitrate, ammonium, and
         phosphate in one solution.  We are having a hard time maintaining the concentration  of nitrite in the
         mixed standard, therefore, the tittite primary standard b
         a ratio of 4 mL of the mixed standard with  I mL of the nitrite primary standard-  This new mixed
         standard is then diluted to give working standards that bracket the range of most of the samples,
         Samples that are more concentrated than the highest standards are diluted.

               Ammonium Primary Standard:  Dissolve 0 33035 g ammonium sulfate in 1000  mL DPW  Add
•t             2 mL chloroform  Final  concentration: S.O ujnoles/mL-

               Nitrite Primary Stmdaaj- Dissolve 0,0690 g sodium nitrite in 1000 mL DIW.  Add 2 mL
-------
        chJorofom.  final concentration: LO jirnoJes/mL

        Nitrgte, .Primary Standard: Dissolve 1,020 g potassium nitrate in 1 000 mL D1W. Add 2 mL
        chloroform.  Final concentration: 10.0
                                Dissolve 0, 1360 gpotassmmdihydrogen phosphate En IQCWmL
        DIW, Add 2 mL chloroform. Ftnal concentration; 1.0 nmoJ«a/mL,

        Mixed Standard:  Combine 25 rnL ammonium primaiy  standarf,  10 mL nitrate primary
        standard, 25 mL phosphate primaiy standard and 20 mL DfW.

       Working Standards:  Mm 4 mL of the mixed standard with  I  mL of the nitrite primary
       standard.  Then dilute this new mixed standard according to Table 2 to prodjce the wwkina
       standards                                                                     s


       .Efficiency Standard: Mix' SO |iL of the nitrate primary standard in 100 mL of DIW,
Tafatt L   Working standards for fnorganic  nutrient detenmnation  on the Alptern  RFA 300
ajtomaJyzo-.  Mixed standard volume refers to the amount of mixed standard tdded to 100 mL
num«t-ftee srawata (seawater sample) or DIW (ftrahwater samples).  SRF is soluble reactive
phosphate  N+N is nitrate (NO.O + nitrite (NQt>
             Volume
Woiting      Mixed
Working Standard Concentration (pmoles/L)
Standard
BLANK
SI
S2
S3
S4
S5
Standard
0
100
200
400
600
goo
SRP
0
0.25
0.50
LOO
1.50
2,00
NH*'
0
1.25
2.50
5,00
7.50
10.00
NQi"
0
0.20
0.40
OJO
1.20
L60
N(V
	 o ~~
1,00
2.00
4.00
6.00
8.00
N+N
•"**•' • 	 ._
0
UQ
2.40
4,80
720
9.60
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 3-2.4   Autoanaryzcr Calibration

 Prior to starting a run on the autoanaiyzer, the injection needle is placed into the SS standard and allowed to
 run through the instrument.  The percent fldl scab of the high standard cm each channel is recorded and
 compared to the previous day's run.  The percent full scale should not change greater than 5% on a daily basis,
 Changes greater than 5% may indicate that either the  standards were not prepared correctly, or that  the
 instrument is in need of an overhaul.

 Each run of the autoanalyzer begins with the auming of a SYNC cup then a wash water blank, A complete set
 of blinks and the 5 working standards described in Table 5,2 are then run. Following the standard curve is a
 carryover (which is the low standard SI), then an SI cup  is  run again.  A check cal (S3) and an efficiency cup
 follow.  Additionally, a blank sample and an S4 are run every 10 analyses in an autoanalyzer run to monitor
 basdne and intra-run calibration drift.  At the end of the run, an S5 cup is run again. Any drift in the sensitivity
 of the autoanalyzer during the run is detected by this drift check, and corrections are made to account for any
 drift.  A log book is  kept  to monitor the calibration curve parameters.   Substantial changes in the curves
 indicate the need for either preventative maintenance on the autoanaiyzer or re-making of the standards.

1.2*5  AutoansJyrer Prevrntalive Maintenance

 After every run of the autoanalyzer, the inside of the tubing  is washed with a ID min flow of detergent (Kem-
 Wash), followed by a  10 min Row of 10% (v/v) hydrochloric add,  followed by a 10 man flow of DIW  The
system is then pumped dry, The peristaltic pump rollers are cleaned using ethanol-dipped cotton swabs.   All
spills are immediately cleaned up.  Any worn tubing is replaced immediately  An hour meter attached to the
instrument keeps track of the use time, after every 200 hr of use, the instrument receives a thorough overhaul.
For each overhaul, ail tubing is changed, the pump rollers are reconditioned, and the filters  are inspected and
changed if necessary.
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33 Total Phosphorus

For the determination of total phosphorus in water, soil, sediment, and tissue samples, SERF does not use the
typical ammonium persuJfete digestion because of the explosive hazards and special handling requirements
associated with the use of this chemical Instead, SERF uses a modilealOT
described by SoJorzano and Sharp (1980. DelennitiatioH of total dissolved phosphorus and paniculate
pboyhonts in natural waters. Umnd. Oceanogr , 25(4), pp. 754-758 (see attached).  Total phosphorus is
determined in water, soil, sediment, and  tissue samples by oxidizing and hydralyang all of the phosphorus-'
containing compounds  in  a sample to  soluble  reactive  phosphite, and determining the soluble reactive
phosphorus concentration  by the same autoanah/zer  method  described above.   SERF has a separate
autoanalyzer used for the analysts of total  phosphorus,

13. 1  Total Phosphorus Sample Preparation

Sample preparation for total phosphorus determination is done as soon as possible. Water samples should be
prepared  within 24 hours  of sample collection, and are often prepared immediately upon return  to  the
laboratory.

3J.I.1 Water Samples

       I .      Prepare a tray with two or three E nil scintillation vials (without the aluminum-lined caps) per
              sample bottle Add 100 uj of 0 1 7 N  MgSQ« to each vial using the Eppendotf ptpet setting of
              I. Fill out a Total Phosphorus Preparation Log Sheet wkh the placement and contents of the
             vials on the tray.
      2.     Add 5 mL of water sample from each total bottle into each of the vials.
      3,     Place tray in an 80°C oven and evaporate to dryness (usually overnight)
      4.     Ash the samples at 5SO°C  in  a muffle furnace fir 3 hours and allow to cool overnight,
      5.     Hydrolyze each sample with the addition of 5 rnL of hydrocWorie  add.  The normality of the
             add is dependent on die salinity of the sample according to the following table:

                                  HQ..cqiieeiitratic»ii
             0.0- 15 ppt   0.06 N
              I6-35ppt           OJ2N
             36- 55 ppt           0.18N
             56 - 80 ppt           0.24 N

      6.     Cap eadiswnpietif^iUy with pofytined caps, shake using t vorto«r, and put into an 8CfC oven
             overnight.  After renioving fhxn the oven, altow to cool and shake again.

J J. 1.2 Soils, Sediment ami Tissue Samples

       I.     Dry sample in an 80°C oven for 2 days, then grind.
      2.     Add 25  mg  of sample into 10 mL glass scintillation vial (remove aluminum lined caps).
             Prepare two  vials per sample,  Fffl out a Total Phosphorus Preparation Log Sheet with the
-------
              placement and contents of the vials on the tray
       3.      Add 200 pi ofO. I7N MgSOi and I mL OiW to etch sample vial. Then dry and ash the sample
              as described for water samples.
       4.      Place tray in an SQ*C oven and evaporate to dryncss (uaaJJy overraght).
       5      Ash the samples at S50°C in a muffle fiirnace fbr 3 hows and allow to cool overnight.
       6      Hydrolyzeeaeh  sample with the addition of 1 0 mL of 0.24 N hydrochloric add
       7,      Cap each vial tightly with polylined caps and put tn 8G*C oven overnight
       8.      Cool and shake, allow to stand overnight.
       9.      Analyze at a 1 : 10 dilution (200 pi of sample with 1 800 |J DIW).
                                                              »
3.3.2   Total Phosphorus Reagents

The reagents used for total phosphorus are the same as those used for soluble reactive phosphorus presented in
Section 3.2.2.

333   Total Phosphorus Standards

The primary standard for total phosphorus is the same as that used for soluble reactive phosphate.

       Pjmgjgte Pnmarv Standard:  Dissolve 0. 1350 g potassium dUiydrogen phosphate in 1 000 mL DIW,
       Add 2 rnL chloroform  Final concentration: I 0
      Tntal t> Secondary Standard for water samples:  Put 20 jjjL of phosphate pommy standard into 10 mL
      ofDfW

Working standards for water samples are prepared from the primary standard in DIW or Sargasso Seawiter
depending upon the salinity of the samples.  For water samples with salinities of 15 ppt or less, standards are
prepared in  DIW.  Sargasso Seawater is used for water samples with salinities greater than 15 ppt  The
workng standards are made to bracket the expected concenttitioiiofthesiriifilesasshow«niTable3.  A log
books kept by the total phosphorus aitoanaryar, In the log book rword the slope and eonrfairon coefficient
of th* caliiration curve, the concentration of the high standard, the number of samples run, the water matrix
(fresitwmter or seawater) and the technician's name.
-------
 Tifote J.      Working standards for Total Phosphorus detairunatioii.
Woriung Sundard
Low Standard Curve
SI
S2
S3
54
SS
High Slandard Curve
SI
S2
S3
S*
S5
Standard Curve for Solid
Samples
SI
S2
S3
S4
53
Volume of Primary
Sundard in 100 nil of
DlWorScawaicr

10 t*i
»)J
100 pj
150 jd
200^

125^1
250^1
500^1
750 1*|
IQOOuJ

125 (J
250 ,J
500 ^
750 pJ
lOOO^J
PJwsphoros Standard
Conccniration (|iM)

010
OSO
LOO
t.50
106

1.25
2,50
5.00
750
10.00

3-i7^&
7.74 ps/g
15M p^/g
23,22 pgfg
30.97 )Hte
3.3.4  Total Phosphorus Automnmlyrer Preventive Msutenanct
The dewing and preventive maintenance schedule for the total phosphorus autoanalyzer is tht same as
for ite filtered nutrient aytoinalyzer.
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 3,4   Total Nitrogen

 An ANTEK Instruments, Inc. Model 7000N Nitrogen Analyzer is used to determine total nitrogen of 5 uJ
 of a preserved water sample.   The instalment is run according to the  Instalfation/Operauon/Service
 Manual provided by ANTEK Instruments, Inc., except that oxygen gas is used as a carrier gas instead oi
 argon to promote complete recovery of the nitrogen in the water samples.

 3.4.1  Total Nitrogen Sample Preparation

 Water samples for total nitrogen should be processed within 24 hours of sample collection and is often
 performed immediately upon return of the samples to the laboratory.  Water sample preparation for total
 nitrogen  includes transferring t ,5 mL of water sample from the unaltered sample bottle to a small glass
 vial. The sample is acidified with 10 uJ of 3 N HCt, using an Eppendorf pipet on a setting of 1. The glass
 viais are sealed with a teflon-lined crimp cap, labelled, and stored in a refrigerator at 2"C until analyzed.

 3.4.2  ToiaJ Nitrogen Reagents

 ACS reagent-grade 3 N HQ is made by adding 125 mL of concentrated 12 N HO into a 500 mL flask
 and diluting to the mark with DlW

3.4.3  Total Nitrogen Standard

A primary standard is made by dissolving 0 3612  g anhydrous potassium nitrate in 100 mL Dl W. This
standard has a concentration of 0.5 mgN/mJL.  A working standard of 2.0 mgffl is nude by adding 400 \j.l
primary standard in 100 mL D1W.  Vials of the 2.0 mg/1 standard are prepared identical to samples.
Specifically,  1.5 mL of this standard is placed into a glass autoanalyzer sample vial  and acidified with 10
ul of 3 N HQ,  Duplicate vials of this standard are run in triplicate prior to each run, after every 20
samples, and at 'the end of the run to check instrument calibration.

A one-point calibration curve is obtained for each instrument run by beginning the run with duplicate 2.0
mgN/1 standards.  Zero  total nitrogen has a signal of zero.  Irrtra-run drift in  the calibration curve is
monitored by insertion of a blank and a 2.0 mgN/1 standard after every 20 samples and at the end of each
run.

3,4.4  Total Nitrogen Preventive Maintenance

The maintenance schedule for the ANTEK instrument includes replacing the septa on the autosaxnpler
every SO samples, and replacing the column, septa every  40 samples.  On a daily basis,  the vacuum
pressure needs to be monitored and should be at 25 inches of mercury.  The combustion column should
be changed as needed.
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 3.5   Total Organic Carbon

 Total organic carbon samples are analyzed by hot-platinum catalyst combustion of the non-purgeable
 organic carbon in the sample to COt on a Shimadzu TOC-5000 Total Organic Carbon Analyzer,

 3.5,1  Total Organic Carbon Sample Preparation

 Sample preparation includes pipetting 4 mL from each unfiltered sample bottle into glass sample vials.
 Glass sample vials are cleaned  by soaking in DIW  with RBS  35 Concentrate cleaning solution and
 autodaving for IS  minutes. The vials are rinsed three times with DIW then pyt upside-down in a test
 tube rack in the drying oven until dry (usually overnight).  In order to remove inorganic carbon while in
 the automatic sampler, the samples are acidified and then purged for i minutes with COi-free air prior to
 analysis.

 3.5.2  Total Organic Carbon Reagent!

 25%FhojphoricAcid.  Add 500  mL of 85% phosphoric add to 1,500 mL of DIW.  This reagent is put in
 the reagent bottle in the instrument

 3 N HydrogMpnc Acid.  ACS reagent-grade 3 N HCI  is made by adding 125 mL of concentrated 12 N
 HO into  a 500 mL  flask and diluting to the mark with DIW.   This reagent is used to acidify the samples
 while in the autosampler

 3.5 J  Total Organic Carbon Standards

 A primary standard is made by dissolving 2.125  g reagent-grade potassium hydrogen phthakte in 100 mL
 zero-grade DIW. The concentration  of this primary standard is 10,000 tngC/L. Working standards are
 prepared  of concentrations 0, 5, 10,20 and 50 mgC/L by adding 0, 20,40, SO and 200 uL of the primary
standard to 40 mL aliquots of zero-grade DIW.  A standard curve, is run at the beginning of every sample
run.  To monitor for infra-run drift, a blank and a Ugh 10 mg/1 standard is run in the middle and end of
each tun.  Each run and the instrument's performance needs to be recorded in the instrument log book.

3.5.4  Total Orgaoic Carbon Prtventative Maintenance

The TOC instrument maintenance schedule  includes checking the reagent level, the DIW level, and the
gas level  on a daily basis. Replace the tubing and the needles on a daily basis and change the column
every 2000 samples.  A detailed schedule of replacement parts and. regeneration of catalyst is contained in
the operator's manual for the instrument-  This schedule should be followed.
-------
 3.6   Slica
 3,7   Chlorophytl-a

 An extractive fluorometric technique is used to determine chlorophyll-a concentration.  Acetone extracts
 of suspended material collected on filters are excited with 435 run light, and the fluorescent emission of
 light at 667 run is measyied using a Fluoro IV Spectrofluoroineter (Gilford Instruments, QberliiL, Ohio).
 The amount of fluorescence is directly proportional to chlorophyll concentration as determined by a.
 standard curve of chlorophyll prepared in 90% acetone solution.

 3.7.1   Chlorophyll Sample Preparation

 Samples are brought to the laboratory on the same clay of collection and stored in the dark in a freezer at
 a temperature of * 15"C   Samples should be kept in the freezer for a minimum of 48 hours to allow for
 complete extraction of the suspended, material from the filters to the acetone.  Analysis should be
 performed within 7 days of sample collection.

 3.7.2  Chlorophyll Reagents

 WiAoetone.	In a large 1000 mL cylinder add 900 mL of acetone and 100 mL of DIW. Store in a glass
 1000 mL bottle and seal with a teflon lined cap,

 3.7J  Chlorophyll Standards

 Put the contents of I vial of I ing/L chlorophyH-a standard from  Sigma Chemical Co, (St.  Louis, Mo)
 into 200 mL of 90%  acetone.   Determine the exact  concentration of this high  standard on  the
 spectrophotofneter at a wavelength of 664 run and using the equation given in Section 1.6.5,  Make 5 to
 7 standards from the high standard in a range from 0 - 250 ug/L,  All of these standards need to be in
90% acetone.  Analyze these standards on the spectrofluorometer according to the following procedures:

      a.     Turn on spectrofluorometer and allow to warm up for at least one hour.
      b.     Set excitation to 435 nm and emission to 667 nm (Hit  2 ENTER, 435  ENTER, 667
             RETURN*.
      c.     Place an empty, glass cuvette in slot 2 and hit calibration key.
      d.     After calibration, set high voltage to 700 (Hk 3,2 ENTER, 700 RETURN),
      e.     Set the response to 4 seconds (Fit 3.5 ENTER, 4 RETURN).
      f.      Place 90% acetone in a clean, glass cuvette in slot 2, check to see that it reads 00.  If it
             doesn't, hit the AUTO ZERO button.  If it is still not zero, dean the glass cuvette to be
             sure it is free of fingerprints.
      g.     Place another dean, glass cuvette in,  slot  1  and check to see that it' reads zero.  If It
             doesn't, hit AUTO ZERO again or dean the cuvette.
      h.     Suction off the 90% acetone from slot  I, Rinse the cuvette with acetone and suction off.
      i.      Run each  of calibration standards as you vtoiAd a  sample.  Specifically, mix  750  uJL of
-------
              each standard with 2250 jjjL of 90% acetone in the cuvette in Slot i,  Rinse the cuvetti
              with acetone between each standard
       j.      Determine the slope of the calibration curve of relative fluorescence  to  chlorophyl
              concentration. Check that the linear correlation coefficient is 10. 95.

 3.7.1  Chlorophyll Sample Analysis

       a.      Remove samples from the freezer.
       b.      Push the filters down to the bottom of the centrifuge vials with a spatula,
       c.      Place the vials in the centrifuge and spin for I - 3 minutes.
       d      Place 750 pj- of the acetone extract from the first vial into the fluorometer glass cuvette in
              slot  1,
       e.      Add 2250 |iL of 90% acetone to the cuvette and mix twice with a disposable pipet
       £      Close the hood of the instrument and allow the reading to equilibrate.  Hit READ PRINT
              to record relative fluorescence
       g.      Suction off the sample from the cuvette, rinse with acetone, suction again and repeal
              procedures d-gfor each sample.

 3,7.5   Chlorophyll Calculations

       a      Determine the chlorophyll concentration in the high standard spectrophotometricaUy using
              the extinction coefficient of 8767  (L*gm-E*cm-l) folio wing equation by Jeffrey and
              Humphrey (1975):
             Chl-a(pg/L) = (absorbance/E7.67)*

      b.     Determine the chlorophyll concentration using the following equation:

             Chl-a (pg/L) - R.F. * slope * (15 mL/0.75 niL) / L filtered

      where,  ELF, is the sample relative fluorescence; slope is the dope of the standard curve;
      15 mL is the amount of acetone in the microcentrifuge used for extraction, 0 75 mL is the'
      amount of the acetone extract removed from the vial and placed in the cuvette; and the L
      Altered is the amount of water filtered in the field (e.g. 120 or 140 ml = 0 12 or 0. 14 L).

      c.     Calculate the mean chlorophyll concentration at each station from duplicate samples.

3.8   Alkaline Phosph»t«e Activity

The alkaline phosphatase activity (APA) assay measures the activity of alkaline phosphalase, an enzyme
used by bacteria to  mineralize phosphate from organic compounds.  The assay is performed by adding a
known concentration of an organic phosphate compound (methylfluorescein phosphate, or MFP) to  an
unfiltered water sample. Alkaline phosphatase in the water sample cleaves 'the phosphate from the MFP,
leaving methylfluorescein (MF), a highly fluorescent compound. The concentration of MF at  the end of
the assay is proportional to the APA of the sample,
-------
 3.3.1   APA Simple Preparation

 APA measurements are made within 12 to 24 h of sample collection. Duplicate 3 mL subsampies from
 each sample bottle are pipetted into disposable plastic cuvettes, and 30 |iL of a MFP solution are added
 to each

 The  fluorescence  of these subsamples  are immediately  measured  using  a  Gilford Fhioro  IV
 Spectrafluorameter (excitation » 430 nm, emission - 50? nm) and recorded. Samples are placed in an
 incubator at 25 CC for 2 hr   Fluorescence of all the samples is then measured again using the same
 excitation and emission wavelengths.  The amount of MF produced in 2 h is quantified by comparison to
 a standard curve.

 3.S.2  APA Reagents

       MethylfluonacBin	Phosphate jjojutjgn:  52.55 mg of anhydrous 3-o-melhyjfkorescetn phosphate
       is dissolved in 100 mL of 100 mM Tris buffer, pH = 8.7,  Concentration of this stock solution is 1
       mM.

       Trizma Buffer  Dissolve 12.8 g of Trizma crystals, pH=SJ in  I L ofDfW.

3.8.3 APA Standards and Calibration

A stock standard solution of methylfluorescetn is diluted to make working standards that bracket the
concentration of MF in the APA assays after 2 hr. Working standards are made up from standard stock
solution and the fluorescence of the working standards is measured each day that analyses are performed,

       Methvlfluorcscein Standard Stock Solution:   Dissolve 0.0346 g methylftuorcscein in 100 mL
       methanol. Concentration of this standard stock solution is 1 mM  This solution is kept  in 1,8 mL
       centrifuge vials in the freezer  One vial is thawed each day prior to use..

       yVgikiiig_Standards:  0, 3, 7.5, 15 and 30 pL of standard stock solution are diluted into 3.0 mL of
      Trizma buffer, to give standards of 0, 1,2,5,5 and 10 uM methylfluorescein

1.8.4  APA Sample Analysis

      a.    Turn the machine on to warm up, preferably an hour.
      b.    Set the excitation and emission wavelengths (Hit 2 ENTER, 430 ENTER, 507 RETURN),
      c.    Set the response time to 4 seconds (Hit 3.5 ENTER, 4  RETURN).
      d.    Calibrate the machine wtth an existing cuvette in slot 2. Hit calibrate
      e.    After calibration, set high voltage to 425 (Hit 3.2 ENTER, 425 RETURN).
      f.     Put in blank (Trizma buffer) and see if it reads zero. If not, zero the instrument by hitting
            AUTO BLANK,
      g.    Analyze each  standard,  'pressing  READ  PRINT after  each  to record the  relative
            fluorescence.
-------
                h.     Prepare the samples by placing  3  mL of sample into each  of two disposable plastic
                      cuvettes.  Put 30 \&» of stock MFP into etch sample cuvette and mk with a disposable
                      pipet.
                L     tnsert each sample cuvette into slot I, dose the hood, and hit READ PRINT to record th*
                      relative fluroescence when the number stabilizes.
                j.     Place the sample cuvettes into an incubator at 25 CC for 2 hr, then repeat step i,

         3.9    Turbidity

         Turbidity is often determined for unaltered (total) samples immediately upon return to the laboratory. An
         HF Scientific Inc. model ORT-tS C turbidimeter is used. This instrument is portable and can be taken
         into the field for field  determinations of turbidity. Turbidity needs to be done on the samples within 24
         noun of samples collection. Therefore, if the samples can not be brought back to the lab within one day
         of sample collection, then the turbidimeter needs to be taken out into the field.

         3.9. i  Turbidity Standards and Calibration

         The instrument reads directly in Nephdornetric Turbidity Units (NTUs).   Calibration is done quarterly
         with a  3-point calibration by diluting a 4000 NTU  stock Formazm solution.  The  following table
         summarizes the preparation of the calibration solutions.
         Tible 2.     Turbidity Standards


         Value       Pipet into a 200 mL volumetric flask

         198 NTU    9,9 mL of 4000 NTU stock. Add DIW to mark,

         19 8 NTU    20 mL of the 19S NTU dilution made above. Add DIW to mark.

         2.0 NTU     2.0 mL of the 198 NTU dilution made abom  Add DIW to mark.
||
For proper calibration of the unit, access to the trimoots on the right side of the instrument needs to be
made.  See Figure 2 in the instrument manual for location of the tnmoots.  Proceed with the instrument
calibration as dictated in the instrument manual.

3,9.2   Turbidity Sample Analysis

Sampie readings are made according to the following procedures:

       a.     Turn the instrument range knob to a scale of 20,
-------
 b.    Pfaee the 0.02 NTU
      an the instrument.

HC     Ir£^?.•** "•!* -«• «*« rfftn mu is M«L

                  ,                          fer ttts ««Pte « both rte ^0 rt 200
      scales. Record this reading on turbidity datt sheet
f     Turbidity m done on sample water ejected In die unffltered (total) bottle,
8     Rinse
      hottte well,
     Record tlte sample rieading on the 200 scute

                                                                     for
-------
     40   QA/QC Sample,




     •*-'    Equipment Blanks




     These arc labdfed as Cl,
                                                                            •-
    *2   Mitrii Spike Samples CLabelted M§)



















  «
4
         (hat
-------
»
         of all stmpJcs sent
        4-6

-------
40
Forms
      Sheet



     Fom,
                    31
-------
a) Field Instrument CaJi brat ion Form
Sampling Event
Date
Names
                                                        Comments
          Instrument
          Number
 Probe   J Time  CaJibratioa Check
 Number
                                    32
-------
ata She,  »9lul light
                                        Fl«ld D*t* Sh««t
                               D«pth
                                                                             H«th«r  Condi tiTnT"
D.O.
                                                                                 Vol
                                                   33
-------
iia
-------
       Data

       Project
       Sample nos,
       Technician
    f
ndard
Reading 1
Reading 2
                                             33
-------
       Reference
 Jeflrej, S,W, and G.F. Humphry. 1975. New Spectrophotmnetric       Equations for
      Determining Chlorophylls a, b, ci and ca in Higher Plants, Algae and natural
      Phytoplankton.  Bioehem Physiol. Pfianzen (BPP)t 84 167, S. 191-194,
Sofonmo L. and 1H, Sharp.  1980. Determination of Tola! dissolved Phosphorus and
Paniculate    Phosphorus in Natural Waters.  25(4). pp. 754-758.

Hashimoto, S., K. Fujiwara, and Keiichlro F.  1985.  Relationship Between Alkaline Phosphatase
Activity and Orthopfiosphmte in the Present Tokyo Bay.  EnviroiL Sci. Health, A20(7)t 711-809.
-------
                                                                          Section 1
                                                                      Date: 4/20/99
                                                                        Page 1 of 1
                 COMPREHENSIVE QUALITY ASSURANCE PLAN
                                Mercury Laboratory
                                 Prepared by and for:
                       Southeast Environmental Research Program
                            Florida International University
                                      OE148
                                   University Park
                                Miami, Florida 33199
                                   (305) 348-3095
                                FAX: (305) 348-4096
Ronald D. Jones, Ph.D.                                            Date
SERF Director and Professor
Ruth B. Justiniano                                          Date
SERF Quality Assurance Officer
Sylvia S. Labie                                            Date
FDEP QA Officer
                                       1 -1
-------
                                                                                            Section 2
                                                                                        Date: 4/20/99
                                                                                          Page 1 of 4
                                      TABLE OF CONTENTS
                                                                          No. of        Revision
Section       Title                                                        Pages         Date

1.0           Title Page                                                    1             12/24/97

2.0           Table of Contents                                             4             4/20/99

3.0           Statement of Policy                                           1             03/06/95

4.0           Organization and Responsibility                                2             4/20/99
              4.1    Capabilities
              4.2    Key Personnel

5.0           Quality Assurance Objectives (Precision, Accuracy,               3             4/20/99
              and Method Detection Limits)

6.0           Sampling Procedures                                          12             4/20/99
              6.1    Sampling Capabilities
              6.2    Sampling Equipment and Cleaning Procedures
                    6.2.1   Sampling Equipment
                    6.2.2  Sampling Equipment Cleaning Procedures
              6.3    Sample Containers and Cleaning Procedures
              6.4    Sampling Protocols
                    6.4.1   Surface Water Sampling
                    6.4.2  Surface Soil Sample Collection
                    6.4.3   Subsurface Soil  Sample Collection
                    6.4.4  Sediment Sample Collection
                    6.4.5   Pore Water Sample Collection
                    6.4.6 Fish Sample Collection
              6.5    Sample Documentation and Identification
              6.6    Sample Preservation, Holding Times and Sample Volume
              6.7    Sample Dispatch
              6.8    Reagent Storage and Waste Disposal

7.0           Sample Custody                                              7             4/20/99
              7.1    Field Custody
              7.2    Laboratory Custody
              7.3    Electronic Data Records
                                                2-1
-------
                                                                                             Section 2
                                                                                         Date: 4/20/99
                                                                                           Page 2 of 4
                                                                                         Revision
Section       Title                                                         Pages         Date

8.0           Analytical Procedures                                          4             4/20/99
              8.1    Laboratory Operations
              8.2    Laboratory Glassware Cleaning
              8.3    Reagent and Chemical Storage
              8.4    Waste Disposal

9.0           Calibration Procedures and Frequency                           10            4/20/99
              9.1    Instrument
              9.2    Standard Receipt and Traceability
              9.3    Standard Sources and Preparation
              9.4    Instrument Calibration

10.0          Preventive Maintenance                                        2             4/20/99
              10.1   Routine Maintenance
              10.2   Maintenance Documentation
              10.3   Contingency Plans

11.0          Quality Control Checks and Routines to Assess
              Precision Accuracy and Calculation of MDLs                     5             4/20/99
              11.1   Field QC Checks
              11.2   Laboratory QC Checks
              11.3   Routine Method Used to Assess Precision
                    and Accuracy
              11.4   Method Detection Limits

12.0          Data Reduction, Validation, and Reporting                       3             4/20/99
              12.1   Data Reduction
              12.2   Data Validation
              12.3   Data Reporting
              12.4   Data Storage

13.0          Corrective Action                                              3             4/20/99

14.0          Performance and System Audits                                 6             4/20/99
              14.1   Field Audits
              14.2   Laboratory Audits

15.0          Quality Assurance Reports                                     1             03/06/95
                                                 2-2
-------
Section
APPENDIX A
APPENDIX B
       Title

       Method Validation for Part per Trillion (ppt)
       Concentrations of Total Mercury
       in Water, Solid, and Tissue Samples

       Related Scientific Articles
13
50
    Section 2
Date: 4/20/99
  Page 3 of 4
Revision
Date

04/18/96
4/20/99
APPENDIX C
       SERF Mercury Lab Standard Operating
       Procedures
             4/20/99
APPENDIX D
APPENDIX E
       Examples of Instrument Printouts for Total
       and Organic Mercury Determinations

       Method Validation for Organomercury Compounds
       in Water, Sediment, and Tissue Samples

                           LIST OF FIGURES
Figure       Figure
No.          Title
16
                                                           Page
                                                           No.
             4/20/99
11/21/97
             Revision
             Date
4.1           SERF Mercury Laboratory
             Organization Chart
6.1           Vacuum System for the Collection of Surface
             Water Samples
7.1           Sample Chain of Custody
7.2           Mercury Sample Log Checklist
       11/24/97
7.3           Instrument Log Book
7.4           Standard Prep Log
8.1           Hg Lab Decontamination Log Book
12.1         Final Data Report
14.1         Mercury Laboratory Field Audit Checklist
14.2         Mercury Lab oratory Audit Checkli st
                                                           4-2

                                                           6-5
                                                           7-2
                                                           7-6
                                                           7-7
                                                           8-3
                                                           12-3
                                                           14-2
                                                           14-4
                                                                  7-5
             4/20/99

             06/26/97
             11/24/97
             11/24/97
             11/24/97
             11/24/97
             4/20/99
             03/06/95
             03/06/95
Table
No.
                                         LIST OF TABLES
Table
Title
Page
No.
Revision
Date
5.1
Quality Assurance Objectives
Field Measurements
                                               2-3
5-1
4/20/99
-------
5.2           Quality Assurance Obj ectives
                    Laboratory Measurements
5.3           Sample Preparation Methods
6.1           SERF Sampling Capabilities
6.2           Field Sampling Equipment
6.3           Miscellaneous Sampling Equipment
6.4           Sample Containers, Sizes, Preservations and
              Holding Times
8.1           Reagent and Chemical Storage
       07/10/95
9.1           Field Instrument List
9.2           Laboratory Instrument List
9.3           Standard, Source, Preparation, and Storage
9.4           Instrument Calibration
10.1          Field Equipment Preventive Maintenance
10.2          Laboratory Equipment Preventive Maintenance
11.1          Quality Control Checks
13.1          Corrective Actions for the Laboratory
13.2          Correction Actions for the Field
5-2

5-3
6-2
6-3
6-4
6-7
9-2
9-2
9-3
9-7
10-1
13-2
13-3
       8-4
       10-2
       11-2
    Section 2
Date: 4/20/99
  Page 4 of 4
4/20/99

4/20/99
4/20/99
4/20/99
06/26/97
4/20/99
06/26/97
4/20/99
4/20/99
4/20/99
03/06/95
       4/20/99
       4/20/99
4/20/99
03/06/95
                                                 2-4
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                                                                                Section 3
                                                                           Date: 03/06/95
                                                                              Page 1 of 1
3.0    Statement of Policy
The  Southeast Environmental Research Program (SERF) is made up  of university research
professors and their staff from Florida International University (FIU). FIU is one of the nine State
University System (SUS) universities and all SERF personnel are employees of the State of Florida.
 The goals of SERF  are  to advance scientific research,  the  understanding of biogeochemical
processes, and to publish results in high quality refereed scientific publications.  Pertinent to these
goals, is the  need to  collect accurate,  high quality,  and reproducible data, which can only be
obtained through strict internal and external quality assurance practices.   SERF is committed to
follow sound quality assurance/quality control (QA/QC) practices for the purposes of producing
verifiable quality data.

The professors associated  with SERF have been involved  in monitoring  surface water quality in
Florida Bay, Biscayne Bay, the Everglades, other areas of South Florida, and the world's oceans for
over 15 years.  The SERF mercury  laboratory  is currently the EPA contract laboratory for the
Ecological Risk Assessment of Mercury Contamination in the Everglades Ecosystem (R-EMAP
Project).

This Comprehensive Quality Assurance  Plan (CompQAP) describes the  sampling and analytical
methods used by SERF personnel for mercury.  These procedures are used to ensure the integrity
and accuracy  of field and laboratory data collection and analysis.  The CompQAP has been
prepared in  accordance with the Florida  Department  of Environmental Protection  (FDEP)
guidelines.  Project-specific objectives and sampling protocols will be described  in more detail in
Quality Assurance Project Plans (QAPPs).
                                           3-1
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                                                                                 Section 4
                                                                             Date: 4/20/99
                                                                               Page 1 of 2

4.0    Organization and Responsibility

4.1    Capabilities

The mercury research  group at SERF conducts both field  sampling and laboratory analysis of
mercury.   SERF  performs field  sampling of surface water, pore water  (water in  soils and
sediments), soils, sediments, and animal (fish) tissue.  Low level mercury concentrations (parts per
trillion) in water samples (surface water,  pore water,  and groundwater), solid  samples (soils,
sediments), and tissue samples (fish) are determined in the laboratory.

4.2    Key Personnel

Dr. Ronald D. Jones is the director of the Southeast Environmental Research Program (SERF) at
Florida International  University (Figure 4-1).  As director,  Dr. Jones supervises all laboratory and
field operations and personnel. He provides a final review of all data and documents produced.

Mr. Pete Lorenzo is  the SERF  laboratory manager.  In this role, he is responsible for the proper
execution of the daily field and laboratory  operations.  He provides  scheduling of field and
laboratory personnel, and is responsible for the collection, custody,  storage, and analysis  of all
samples.

Ms. Pura Rodriguez de la Vega is the SERF Data manager. She is responsible for checking all the
data produced in the lab according with QC criteria and for the preparation of the final data reports.

Ms.  Ruth Justiniano is the SERF QA officer.  She is  responsible for preparing all QAPs, and
overseeing that the field and laboratory operations  are performed  according to the QAPs.  She is
also responsible for a final check of all data produced with respect to QC criteria, initiating and
conducting audits, and preparing QA reports.

Mr. Julio Lopez is the chief mercury chemist. In this role, he is responsible for the proper execution
of laboratory operations.  He is responsible for the custody, storage, and analysis of all samples.
Additional mercury laboratory technicians include Ms. Martha Bascoy and Frances de Jesus.
                                           4-1
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                                                              Section 4
                                                           Date: 4/20/99
                                                            Page 2 of 2
Figure 4.1- SERF Mercury Laboratory Organization Chart
                       Dr.  Ronald D. Jones
                       SERF Director
                         Pete Lorenzo
                         SERF Lab Manager
   Chief  Chemist
                                              Pura Rodriguez  de  la Vega
                                              Data Manager
  Technicians:
  Martha  Bascoy
  Frances de Jesus
                                              Ruth Justiniano
                                              QA/QC Officer
                                 4-2
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                                                                               Section 5
                                                                           Date: 4/20/99
                                                                            Page 1 of 3
5.0    Quality Assurance Objectives (Precision, Accuracy, and
       Method Detection Limits)

Field  determined  parameters include temperature, conductivity,  and pH of surface water  and
porewater (Table 5.1). Mercury is determined in surface waters, pore waters, ground waters, soils,
sediments, and tissue (fish) samples. Dry weight is determined on soil/sediment samples, while wet
weight is determined on fish samples. Laboratory precision, accuracy, and method detection limits
(MDLs) for these parameters (Table 5.2) are determined using in-house, historically generated data.

Sample preparation methods for analysis of total mercury and organomercury compounds are listed
in Table 5.3. Details of the sample preparation methods are given in Appendices A, B, C, and E.
TABLE 5.1
Quality Assurance Objectives
Field Measurements
Method No.
EPA 170.1
EPA 120.1
EPA 150.1
SM 2520 (B)
Matrix
Surface Water, Pore Water
Surface Water, Pore Water
Surface Water, Pore Water
Surface Water,Pore Water
Parameter
Temperature
Conductivity
PH
Salinity
EPA = U.S. Environmental Protection Agency.  Methods for Chemical Analysis of Water and
       Wastes, Revised March 1983.
SM=  Standard Methods for  Examination of Water and Wastewater,  1989, 18th
       Edition.
                                          5-1
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                                                                                      Section 5
                                                                                  Date: 4/20/99
                                                                                    Page 2 of 3
TABLE 5.2
Quality Assurance Objectives
Laboratory Measurements
Analyte
Inorganic
Mercury
Methyl & Ethyl
Mercury
Total Mercury
Methyl & Ethyl
Mercury
Total Mercury
Dry Weight
Wet Weight
Matrix
Water
Water
Water
Soils,
Sediments
Tissue
Soils,
Sediments
Tissue
Soil,
Sediments
Tissue
Analytical
Method
(d)
(e)
(d)
(f)
(d)
(d)
ASTM
D22 16-80
ASTM
D4638
Precision
(a)
< 20 %*
< 30 %**
< 20 %*
< 30 %**
< 30 %**
< 20 %**
< 20 %**
< 20 %**
< 20 %**
Cone.
Range (b)
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
L,M,H
Accuracy
(%R) (a)
90-110
75 - 125
80 - 120
N.A.
70-130
80 - 120
70-130
N.A.
N.A.
Cone.
Range (b)
L
H
L
N.A.
M
L
L
N.A.
N.A.
MDL (c)
(PPt)
0.3
0.02
0.3
0.02 ppb
0.02 ppb
4.3 ppb
3. 2 ppb
N.A.
N.A.
  *:    Relative Standard Deviation.
 * *:    Relative Percent Difference of Duplicates.
 (a)    Temporary QA targets for precision and accuracy (valid until enough in-house, historical data is
    available).
 (b)    Concentration Range of the linear calibration used to determine precision and accuracy values.
       Calibration range to 1000 ppt.
       L = lower 20% of linear calibration range
       M = from 20% to 80% of the linear calibration range
       H = the upper 80% of the linear calibration range
(c)    Method Detection Limits (MDLs) determined by EPA procedure described in 40 CFR Part  136,
       Appendix B, revision 1.11.
(d)    Inorganic and total mercury determined using a PSA Merlin Plus Fluorescence Detector. Method
       validation package included in Appendix A.
                                                5-2
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                                                                                    Section 5
                                                                                Date: 4/20/99
                                                                                  Page 3 of 3

(e)     Organic mercury determined by capillary gas chromatography coupled with atomic fluorescence
       detection as described by Cai et al. (1996).
       Y. Cai., R. Jaffe, A. Alii, and R. Jones. 1996.  Determination of organomercury compounds in aqueous
       samples by capillary  GC - atomic fluorescence spectrometry following solid-phase extraction.. Analytica
       ChimicaActa 334(251-259)
(f)     Organic mercury determined by capillary gas chromatography coupled with atomic fluorescence
       detection as described by Cai et al (1997).
       Y. Cai, G. Tang, R.  Jaffe,  and  R. Jones.  1997.  Evaluation  of some isolation methods for
       organomercury determination  in soil and fish samples by capillary gas chromatography-atomic
       spectrometry.
       TABLE 5.3
       Sample Preparation Methods
Description
Bromination
Preconcentrated with sulfhydryl
cotton fiber, eluted with KBr and
CuSO4, extracted with
dichloromethane
Sodium thiosulfate clean-up,
isolation with cupric chloride,
extraction with dichloromethane
Slurried, Acidification, Autoclave
Digestion
Slurried, Autoclave Digestion
Matrix
Water
Water
Sediment/Tissue
Sediment
Tissue
Sample Prep, for these Methods
Total Mercury
Methyl & Ethyl Mercury
Methyl & Ethyl Mercury
Total Mercury
Total Mercury
       Jones, R.D., M.E. Jacob son, R. Jaffe, J. West-Thomas, C. Arfstrom, and A. Alii.  1995. Method
       Development and Sample Processing  of Water, Soil, and Tissue for the Analysis of Total and
       Organic Mercury by Cold Vapor Atomic Fluorescence Spectrometry.  Water, Air and Soil
       Pollution. 80:1285-1294. (See Appendix B.)
                                                5-3
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                                                                                Section 6
                                                                            Date: 4/20/99
                                                                             Page 1  of  12

6.0    Sampling Procedures

6.1    Sampling Capabilities

SERF performs sampling of surface water, pore water, soil and sediments and animal tissue (fish)
for determination of total, inorganic, and organic mercury (Table 6.1)

6.2    Sampling Equipment and Cleaning Procedures

6.2.1   Sampling Equipment

Preceding a trip to the field, the personnel responsible for collection of the samples are required to
ensure that everything is prepared  for the expedition.  This entails making sure that all sample
containers are clean, properly labeled, and stored in plastic bags for transport to the field. Table 6.2
lists the field sampling  equipment used for each  matrix,  while Table 6.3  list the miscellaneous
sampling equipment.

Surface water samples are collected using a vacuum system.  Surface water typically has extremely
low levels of total mercury (less than  10 ppt), and the incorporation of sediment within the sample
bottle may lead  to misleadingly elevated  levels of mercury.   The vacuum system illustrated in
Figure 6.1 is designed to reduce the collection of sediment and other large particles in the  water
samples.   A 2L Teflon sample bottle is housed within a plastic vacuum chamber. A screen holder
is  attached to the end of either a 1.5 or 3 ft-long Teflon sampling pole.  The screen holder is
constructed of polyethylene and polysulfone and houses 105 |om Nytex netting. A vacuum pump is
used to create a vacuum  within the chamber. All tubing and fittings associated with the system are
constructed of Teflon.

Pore water samples are  collected using  plastic syringes equipped with Teflon tubing.  Soil and
sediment samples are collected using either polyethylene specimen cups, polycarbonate core tubes,
a Wildco Eggshell Core or and Eckman Dredge. Fish are collected using a dip net. All samples are
collected with the sampler wearing at least one pair of gloves.

6.2.2   Sampling Equipment Cleaning Procedures

The vacuum system is rinsed with sample water three times prior to sample collection by placing a
2L polyethylene bottle in the system and filling. The Nytex netting is replaced prior to each sample
collection.  Additional cleaning measures attempted in the field, such  as detergent washes or acid
rinsing is not conducted due to potential  mercury contamination from these solutions.  Surface
waters contain such  low levels  of mercury that the potential  of mercury contamination of the
samples in the field is
                                           6-1
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                                                                    Section 6
                                                                 Date: 4/20/99
                                                                  Page 2 of 12
TABLE 6.1
SERF Sampling Capabilities
Parameter Group
Inorganic Mercury
Methyl & Ethyl Mercury
Total Mercury
Sample Source
Surface Water, Pore Water
Surface Water, Pore Water,
Tissue
Surface Water, Pore Water,
Tissue


Soils, Sediments,
Soils, Sediments,
                                    6-2
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                                                                   Section 6
                                                                Date: 4/20/99
                                                                 Page 3 of 12
TABLE 6.2
Field Sampling Equipment
Equipment


Water Samples
Vacuum
Apparatus







Syringe



Soils, Sediments
Specimen Cups

Core Tubes

Wildco Eggshell
Core
Eckman Dredge

Fish Tissue
Dip Net

Construction



Housing: Plastic

Tubing: Teflon

Screen Holder:
Polyethylene with
polysulfone
Screen: 105 |JVI
Nytex netting
120 ml plastic
(HDPP) with
Teflon tubing


Polyethylene

Polycarbonate

Stainless Steel

Stainless Steel


Nylon

Use



Collection








Purging,
Collection



Sample
Collection
Sample
Collection
Corer

Sample
Collection

Sample
Collection
Parameter
Groups


Total, inorganic,
and methyl &
ethyl mercury in
Surface Water





Total, inorganic,
and methyl &
ethyl mercury in
Pore Water

Total and methyl
& ethyl mercury
Total and methyl
& ethyl mercury
Total and methyl
& ethyl mercury
Total and methyl
& ethyl mercury

Total and methyl
& ethyl mercury
Restriction,
Precautions,
Notes

Wear 2 pairs of
gloves







Use new tubing
prior to each
sampling event


Wear single pair
of gloves
Wear single pair
of gloves
Wear single pair
of gloves
Wear single pair
of gloves

Wear single pair
of gloves
                                    6-3
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                                                                                          Section 6
                                                                                     Date: 4/20/99
                                                                                      Page 4 of 12
TABLE 6.3
Miscellaneous Sampling Equipment

Surface Water Sampling Equipment

1.       Labeled sample bottles
2.       ZiplockBags
3.       Sounding Line

Pore Water Sampling Equipment

1.       Water Level Indicator
2.       Ph meter
3.       S/C/T meter
4.       pH Buffers (7.00 and 10.00)
5.       Conductivity check Standard
6.       Plastic Beaker
7.       Labeled Sample Bottles

Soil, Sediment & Sampling Equipment

1.       Labeled Sample Containers
2.       Measuring Rule

Tissue Sample Collection

1.       Ziplockbags

Sample Preservation and Transportation Supplies
1.       Ice
2.       Coolers
3.       Shipping labels and forms
        Sample container labels
        Sealing tape
Protective Clothing

1.       Vinyl Gloves (inner gloves)
2.       Shoulder length polyethylene gloves (outer gloves)

Documentation Supplies

1.       Notebooks/logs/field sheets
2.       Pens, Markers
3.       Sample container labels
4.       Custody transmittal forms

Reference Materials

1.       COMPQAP/SOP
2.       Site map
                                               6-4
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                                                                          Section 6
                                                                       Date: 4/20/99
                                                                       Page 5 of 12
       Figure 6.1
       Vacuum System for the Collection of Surface Water Samples
Vacuum
Pump
                                                                      Teflon
                                                                      .Sampling
                                                                      Pole
                   Plastic
                   Vacuum
                   Container
                      2L Teflon
                      Sample
                      Bottle
Screen
Holder
                                          6-5
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                                                                                Section 6
                                                                            Date: 4/20/99
                                                                            Page 6 of 12

high.  The simple rinsing of the vacuum system with sample water three times prior to  sample
collection has proved acceptable in measuring parts per trillion levels of mercury in surface water
samples collected as part of the USEPA Ecological Risk Assessment of Mercury Contamination in
the Everglades Ecosystem: R-EMAP Study (USEPA 1993).

The Eckman dredge and the  core tubes used in soil and sediment sample collection are subject to
precleaning in the laboratory prior to  transportation to  a field site.  All surfaces are washed
thoroughly with hot, tap water, using a brush to remove large or stubborn particles.  Liquid lab
detergents are not used due to possible contamination with mercury.  The equipment is then rinsed
with acid (0.5N HC1 and 0.05N HNCb), then with "mercury-free" water.  The equipment is allowed
to air dry completely, then it  is wrapped in plastic bags for storage and transportation to the field.
The Eckman dredge is cleaned in the field between samples by rinsing with the water overlying the
sediment  to be  collected.  This  is appropriate since  surface  water has  significantly lower
concentrations of mercury then the sediment.  Core tubes are not reused  between samples,  and
therefore,  do not require additional cleaning in the field.  The plastic syringes and Teflon tubing
used to collect pore water samples are  rinsed three times with the pore  water prior  to  sample
collection.  Following sample collection, the plastic syringes and Teflon tubing is rinsed with  acid
(0.5N HC1 and 0.05N HNCb), then with "mercury-free" water.   The dip  net is rinsed with the
surface water at each fish sampling station.

All field cleaning procedures  are documented in the field note book.  Any sampling equipment used
once in the field and not cleaned in the field are tagged with the sample location and cleaned under
controlled conditions in the laboratory. All field equipment is cleaned upon return to the laboratory
by rinsing with acid (0.5N HC1  and 0.05N HNOs), then with "mercury-free" water.  The equipment
is allowed to air dry completely, then it is wrapped in plastic bags for storage and transportation to
the field.   Any  field equipment  suspected  of being  contaminated and  can not be cleaned  is
discarded.

6.3    Sample Containers and Cleaning Procedures

Sample containers, preservation methods, and appropriate holding times for each matrix are listed
in Table 6.4. New Teflon sample bottles are etched with a unique number and decontaminated with
the method outlined below.  Once cleaned, one bottle  from the batch is filled with mercury-free
water (DIW) and analyzed as a quality control check for batch contamination.

Teflon sample bottles are cleaned and reused indefinitely.  After old samples are discarded, the
bottles are rinsed three times  with mercury-free DIW and filled with 1% HC1. After filling,  1 ml of
brominating agent is added for every 50 ml and the bottle
                                          6-6
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                                                                        Section 6
                                                                    Date: 4/20/99
                                                                     Page 7 of 12
TABLE 6.4
Sampling Containers, Sizes, Preservations and Holding Times
Sample Type/
Parameter
Water/ Total, Inorganic and
Methyl & Ethyl Mercury
Soils, Sediments/ Total and
Methyl & Ethyl Mercury
Tissue/ Total and Methyl &
Ethyl Mercury
Container/
Size
Teflon, 2-liter
Polyethylene
Specimen cups
Plastic Bags
Preservative
10 ml HClper 2
liters of sample
Frozen
Frozen
Holding Time
28 days in a Hg-free
room
Indefinitely, but
preferably within 28
days
Indefinitely, but
preferably within 28
days
                                      6-7
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                                                                                 Section 6
                                                                             Date: 4/20/99
                                                                             Page 8 of 12

is shaken and stored in a mercury-free clean room until used.  When ready to be used, 500 |ol of
hydroxylamine hydrochloride is added to each bottle to remove all of the free bromine.  The bottle
is then shaken, emptied, and the bottle and cap are rinsed three times with mercury-free water. All
sample containers are placed in new plastic bags for transport to the field.

Mercury-free water is produced by filtering  tap water through a Culligan system consisting of
activated charcoal  and two mixed bed ion exchange cartridges.  The filtered water is piped to a
mercury-free clean room, where it is passed through a Barnstead Mega-ohm B Pure system.   This
system is fitted with two filters (Thermolyne:  colloid/organic-D0835, and ultrapure-D0809) in line
with a 0.22 micron pleated particle filter.  Mercury levels are not detectable in this water in both our
laboratory and in an independent laboratory analysis (<0.1 ppt).  The only water used in the mercury
laboratory is this mercury-free water and it is used for blank preparation and final decontamination
rinse. Documentation is maintained within the laboratory demonstrating the reliability and "purity"
of the analyte free water from analysis of method reagent blanks. Mercury-free water containers are
cleaned by rinsing with 0.5N HC1 and 0.05N HNOs, then three times with the mercury-free water
prior to filling.

6.4    Sampling Protocols

For the determination of ultra-low levels of mercury (parts per trillion) clean sampling protocols
must be employed throughout the field sampling effort. The field methods described herein were
developed  for  the USEPA Ecological  Risk  Assessment of Mercury Contamination in the
Everglades Ecosystem: R-EMAP study (USEPA,  1993). These  sampling protocols are described in
SERP's internal standard operation procedures (Appendix D). A copy of the SERF S.O.P. is carried
to the field during each sampling event.

For each sampling event, one of the field crew members is designated as the "clean person".  This
person is responsible for all sample handling, including sample collection, securing  the sample
container in a plastic bag, and placing the sample in the cooler.  All samples are collected with the
sampler wearing vinyl  gloves.  For collecting water samples,  the sampler  dons shoulder length
polyethylene gloves over the vinyl gloves.  All samples are secured in a plastic bag prior to placing
in the cooler.  Water samples are most susceptible to mercury contamination, therefore, they are
enclosed in two plastic bags.  All  samples are  stored in  coolers for transport to the laboratory.
These coolers are used exclusively for low level mercury samples.

Specific sampling locations  are chosen based  on criteria described in the appropriate Quality
Assurance Project Plans.  In general, surface water, sediment, and tissue samples are collected from
a boat, helicopter, or airboat.  Airboat,  van, and helicopter  exhaust are a potential source of
mercury. To ensure collection of undisturbed and uncontaminated samples, the boat or airboat is
advanced  toward  a  sampling station from  the downstream  direction, while the helicopter is
advanced toward a station from the downwind direction. Samples are collected from the bow of the
boat away from the engine.   If wading  or  walking is  possible, samples should  be collected
approximately 10 meters upgradient from the boat, airboat, or helicopter. If surface water samples
and  sediment and/or tissue samples  are to be  collected  at one  location, then the sequence for
sampling is surface water, sediment, then tissue samples. In areas of suspected high concentrations,
                                           6-8
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                                                                                Section 6
                                                                            Date: 4/20/99
                                                                            Page 9 of 12

samples are collected in order of suspected low concentration to higher concentration.

6.4.1   Surface Water Sampling

All surface water samples, whether from an ocean, bay, canal, or marsh are collected according to
the following protocols.

       1.      Advance to the sampling station from the downgradient direction.
       2.      The "clean person" will put on a pair of vinyl gloves, then a pair of
              shoulder length polyethylene gloves and handle the vacuum system
              sampling pole and sampling container.   Other members of  the
              sampling team, wearing a pair of vinyl gloves, can provide assistance
              with creating and releasing the vacuum in the vacuum chamber. The
              "clean person" will  also don a pair of waders if necessary.
       3.      Place  a 2-liter plastic, rinse, bottle  in  the  vacuum  chamber.
              Submerge the sampling pole and screen holder beneath the surface
              of the water.  Create a vacuum in the chamber and fill the bottle to
              rinse the screen and tubing with the sample water.    Release  the
              vacuum and discard the rinse water in the  bottle  downstream of the
              sampling location.
       4.      Remove a  24iter  Teflon bottle from  its  protective  plastic bag,
              remove the cap and place the bottle within the vacuum system.
       5.      Submerge the sampling pole and screen holder to a depth applicable
              to the project objectives,  create a vacuum within the chamber,  and
              fill the bottle.
       6.      Release the vacuum in the chamber and remove the bottle.
       7.      Tightly cap the bottle, and place in a ziplock bag and seal it. Place
              the  sample  in a second bag and seal it.   Place  the double-bagged
              sample in a cooler.

Duplicate water  samples are collected  by placing another 24iter Teflon bottle within the vacuum
chamber immediately following collection of the first sample.  Split samples for inter4aboratory
comparison are made in the "clean-room" in the laboratory, where the first sample is preserved with
acid, then split into two equal sample volumes.

6.4.2   Surface Soil Sample Collection

       1.      Advance to the sampling station from the downwind direction.
       2.      The "clean person" will put on a pair of vinyl gloves and a pair of
              shoulder  length  polyethylene  gloves  and  handle the  sample
              container.
       3.      Remove a 4-ounce specimen cup from its protective plastic bag.
       4.      Remove surface detritus prior to sample collection.
       5.      Using a stainless steel  trowel, spade or spatula collect a grab sample  of
              surface soil (upper 10 cm) and place into the 4-ounce specimen cup.
                                          6-9
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                                                                                Section 6
                                                                            Date: 4/20/99
                                                                           Page 10 of 12

       6.      Place the lid on the cup, label the cup, secure in a ziplock bag and
              place in a cooler.

Duplicate  surface  soil samples are collected following the above  procedures  using  the  same
sampling equipment used to collect the first sample.  Soil samples are homogenized either in the
field or in the laboratory, depending upon the project objectives.  If homogenized in the field, the
soil sample is placed into a polypropylene mixing tray and homogenized by slicing, mixing, and
remixing of the sample.  The homogenized soil sample is then placed into a wide-mouth specimen
cup and stored in a cooler in the dark for transport to the laboratory. In the laboratory, soil samples
are homogenized by mixing the entire sample in a blender.

6.4.3   Subsurface Soil Sample Collection

       1.      Advance to the sampling station from the downwind direction.
       2.      The "clean person" will put on a pair of vinyl gloves and a pair of
              shoulder  length polyethylene  gloves  and  handle the  sample
              container.
       3.      Remove a plastic core tube from its protective plastic bag.
       4.      Push the core tube  into the soil by hand while rotating the tube in a
              circular motion.
       5.      Cap the top of the  core tube with either a plastic or rubber  stopper,
              then extract the core tube.
       6.      Cap the bottom end of the core tube, label the core indicating the top
              direction.
       7.      Seal the core in a plastic bag and place in a cooler.

A duplicate subsurface  soil  sample is  collected according to  the  procedure described  above
immediately following the collection of the first sample.  Soil samples are homogenized either in
the field or in the laboratory, depending upon the project objectives.  If homogenized in the field,
the soil sample is placed into a polypropylene mixing tray and homogenized by slicing, mixing, and
remixing of the sample.  The homogenized soil sample is then placed into a wide-mouth specimen
cup and stored in a cooler in the dark for transport to the laboratory. In the laboratory, soil samples
are homogenized by mixing the entire sample in a blender.

6.4.4   Sediment Sample Collection

Sediment samples are collected either with polycarbonate core tubes or with an Ekman Dredge.
The Ekman Dredge is used  during sample of quiescent waters such as impoundments or lakes,
while the core tubes are used in moving waters such as rivers or streams to minimize the loss of
fine particles. Samples collected with core tubes are collected following the procedures outlined in
Section 6.4.3.  Sediment samples  collected with an Ekman Dredge are collected according to the
following protocols.

       1.      Advance to the sampling station from the downgradient direction.
       2.      The "clean person" will put on a pair of vinyl gloves and a pair of
                                         6-10
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                                                                                Section 6
                                                                            Date: 4/20/99
                                                                           Page 11 of 12

              shoulder  length  polyethylene  gloves  and  handle  the  sample
              container.
       3.      Other members of the sampling team can assist in securing the line
              of the dredge to the boat or helicopter.
       4.      Slowly lower the dredge through the water column to the bottom.
       5.      Close the dredge to collect the sediment, then pull up the dredge.
       6.      The  "clean person"  will use a stainless steel  knife or spatula  to
              collect a section of the sediment from  the center of the dredge and
              place into a clean specimen cup.
       7.      Cap and label the specimen cup. Place the cup in a ziplock bag and
              into a cooler.

A duplicate sediment sample is collected immediately following the collection of the first sample
using the same sampling equipment used to collect the first sample.  Soil samples are homogenized
either in the field or in the laboratory, depending upon the project objectives. If homogenized in the
field, the soil  sample is placed into a  polypropylene mixing tray and homogenized by slicing,
mixing, and remixing of the sample. The homogenized soil sample is then placed into a wide-
mouth  specimen cup and  stored in a cooler in the dark for transport to the laboratory. In the
laboratory, soil samples are homogenized by mixing the entire sample in a blender.

6.4.5  Pore Water Sample Collection

SERF  collects  pore water from either temporary or  permanently  placed  lysimeters.  Prior  to
sampling, the water level  and bottom of the lysimeter are measured to determine the standing
volume of water. Using either a peristaltic pump or  a  syringe equipped  with Teflon tubing, the
lysimeter is  purged of three volumes of standing water or pumped  dry.  The  volume  of water
removed is  recorded in the field  note book.  Temperature,  specific conductance and pH are
monitored while purging.  If the lysimeter does not produce enough water, then it is pumped dry
and sampled immediately following recovery.  Since SERF does not sample hazardous water, the
purge water is allowed to drain on the ground away from the lysimeter. Pore water is collected in 2-
liter  sample bottles (Table  6.4), after the bottle is rinsed three times with sample  water.  Duplicate
samples are collected immediately following the collection of the first  sample using the same
sampling equipment and tubing.  Split samples for interlaboratory comparison are prepared in the
laboratory "clean-room" where the  first sample is preserved with acid, then split  into two equal
volumes.

6.4.6  Fish Sample Collection

Fish are collected from a helicopter, boat, or airboat using  a dip net.  The fish are identified and
placed  in ziplock bags. The bags containing the fish are labeled and stored in a cooler with ice.

6.5     Sample Documentation and Identification

All sample bottles or containers are  pre-labeled in  the laboratory prior to transport to the field site.
Labels  consisting of colored tape are attached to the side of the bottle.  Water-proof ink pens are
                                          6-11
-------
                                                                               Section 6
                                                                           Date: 4/20/99
                                                                           Page 12 of 12

used to mark the labels. The collection of all samples is recorded in the field notebook.

Documentation brought into the field include:

1.      Equipment checklist
2.      Field Notebook
3.      SERF Internal S.O.P.
4.      Field equipment manuals (if appropriate)
5.      Chain of custody form

6.6    Sample Preservation, Holding Times, and Sample Volume

Sample containers, sizes,  preservatives, and maximum holding times, by matrix are included in
Table 6.4.  Samples are preserved in the field by putting in a cooler with ice for transport to the
laboratory.  These coolers  are used exclusively for low level mercury samples.

In the laboratory, the 24iter bottles with water sample are preserved with 10 ml of trace metal grade
HC1 to  a pH less than 2.  The HC1 is added to  the water bottles in a "mercury-free" room.
Hydrochloric acid is preferred over nitric acid as it results in higher recoveries of mercury (Ahmed
et al. 1987). The pH of the water sample is checked by shaking the bottle and then pouring a small
amount of the sample onto a pH test strip. The water samples are stored in the "mercury-free" room
and analyzed within 28 days.

Acid addition is completed within the mercury-free room following  collection of the  samples,
because addition of acid to sample bottles has resulted in a measurable uptake of mercury from the
atmosphere.  This uptake is measurable if the acid is added to the sample bottle either in the
laboratory prior to sample collection or in  the  field following sample collection.  The addition of
HC1 to the sample bottles  in a mercury-free "clean room" within the  same day of sample collection
results in no measurable loss or addition of mercury.  This method of preservation is considered
standard protocol by EPA Region IV in Athens,  GA, EPA ORD-EMSL in Cincinnati and Battell
Marine Science Laboratory in Sequim, Washington (USEPA, 1993).

The fish and sediment samples are stored in a freezer in the mercury laboratory.  These samples can
remain in the freezer for an indefinite time; however, SERF prefers to process the sediment and the
fish samples within 28 days of receipt.

6.7    Sample Dispatch

Samples are stored in coolers (on wet ice for sediment and tissue  samples) and delivered to the
SERF laboratory by the field personnel on the same day of sample collection. Samples to be sent to
an out-side laboratory  are shipped no  later then one  day following  sample  collection using a
common carrier and overnight delivery. These samples are placed in individual plastic, sealable
bags and packaged with bubble wrap or styrofoam. Non-insulated cardboard boxes are used for
shipment of water samples, while insulated coolers with ice are used for sediment and fish samples.

                                         6-12
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                                                                              Section 6
                                                                          Date: 4/20/99
                                                                          Page 13 of 12
6.8    Reagent Storage and Waste Disposal
Field reagents are not required for mercury sampling.  Acid preservative is added to the water
samples in a "mercury-free"  room within the laboratory.   SERF does not perform  sampling  of
hazardous waste sites, and there is no generation of field wastes.
                                         6-13
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                                                                                 Section 7
                                                                             Date: 4/20/99
                                                                               Page 1 of 7
7.0    Sample Custody
Sample custody is controlled by SERF, mainly  since the employees responsible  for  sample
collection are also the same employees responsible for sample analysis.  Should the need arise to
send samples via courier to another laboratory, then the sample chain-of-custody (Figure 7.1) and/or
one supplied by the contract laboratory will be used. This form will be included within the sample
cooler and protected within a plastic, sealable bag.  A copy of the form will be retained by SERF in
project specific files.  Upon receipt of the samples, the receiving laboratory will be requested to sign
the sample chain-of-custody form and send a copy of the  signed form via  mail or facsimile to
SERF.  The QA officer will be in charge of ensuring that a copy of the signed chain-of-custody
form is obtained from the receiving laboratory.

Sample bottles sent by SERF to another laboratory are sent  differently according to their matrix.
Water samples are sent sealed in individual plastic bags and then in a  larger plastic bags.  The
samples  are packaged in  cardboard  boxes filled with packing material  (peanuts) to prevent
breakage. Fish and sediment samples are shipped in coolers with ice.  The lids and drain ports of
the coolers are secured with  shipping tape  to avoid opening.  These samples are sent  overnight
delivery, and all  shipping receipts are kept and maintained in a central file location.  Sample
personnel responsible for sample  delivery are identified in  the chain of custody form as well as
common carriers that might have been used in the process.

SERF also  often receives  samples  (surface water, ground water, soils, sediments,  and tissue)
collected by other researchers for analysis.  A completed  SERF chain-of-custody form will  be
required to accompany the samples and will be signed by the QA  officer  or SERF technician
receiving the samples.   These samples  will be inspected  by the SERF QA officer  or SERF
technician  for  integrity and completeness  according to the chain-of-custody  form.   Any
discrepancies between the samples received  and the chain-of-custody form will  be reported
immediately to the researcher that  collected the samples. A copy of the chain-of-custody  form will
be kept in the project specific files.

All sample bottles are pre-labeled in  the laboratory prior to transport to the field site.  Labels
consisting of colored tape are attached to the side of the bottle.   Water-proof ink pens are used to
mark the labels.  Since sample containers used for the suspended matter samples, sediment samples
and tissue samples are used only once,  they are marked with water-proof ink pens directly on the
outside of the sample container.

Each  sample container is labeled with a unique sample identification number as indicated below:

       A AA### YYMMDDB.
                                           7-1
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                                                                                                                                                 Section 7
                                                                                                                                            Date: 4/20/99
                                                                                                                                              Page 2 of 7
FIGURE 7.1 Sample Chain-of Custody
                                           SOUTHEAST ENVIRONMENTAL RESEARCH PROGRAM

                                     OE 148 (office)A/H 321 (lab), University Park, Miami, FL 33199, 305-348-3095
                                                   Chain of Custody Record/Sample Log - Mercury
Page of
CLIENT/PROJECT NAME: (ACCOUNT NO.: AUTHORIZATION:
DELIVERED BY:
RECEIPT
BOTTLE
ID

















RECEIVED BY:

SAMPLE
ID

















MATRIX *

















COLLECTION
DATE TIME


































#OF
REPLICATES

















PRESERVATIVE

















DATE AND TIME:
ICE IN COOLERS?:
ANALYSES
THG

















OHG

















AFDW

















BULKD

















TP

















TN

















TOC

















SAMPLE COMMENTS

















' Matrix: FW = fresh wate, SI/I/ = seawater, S = soil/sediment, P = particulates, T = tissue (fish)
'*: Analyses and methodsTHG (Total mercury, see CompQAP); OHG (Organic Mercury, see CompQAP); AFDW (Ash-Free Dry Weight, ASTM D2974-87); BULKD (Bulk Density, ASTM D4531-

  TP (Total Phosphorus, EPA 365.1), TOC (Total Organic Carbon, EPA 415.1); TN (Total Nitrogen, Antek);
                                                                           7-2
-------
                                                                               Section 7
                                                                           Date: 4/20/99
                                                                             Page 3 of 7

The  first letters in the sample identification number (AAA) refer to the program name.   For
example, the three letters ECS would be used to designate the EPA Canal .Sampling program.  The
first  set of numbers (###) can vary from 1 to 999 and refers to the sample location number.  The
date  of collection follows in a year, month, day format. The second letter designation (B) refers to
the type of media collected and will be a W, S, or T to represent water,  soil/sediment, or tissue,
respectively. The reusable water  sample containers are  etched with permanent  numbers. These
numbers will be identifying the sample as an additional character after the W. An example of the
sample label is included below:

       ECS101950115W34

Sample numbers are recorded on sample containers, in field notebook, and sample log list.

SERF often receives samples collected by other researchers.  When this is the case, SERF uses the
unique sample  numbers supplied by the other researcher.

7.1    Field Custody

Loose4eaf field notebooks are used for all field documentation. Once QA checked, the sheets are
removed from the notebooks and kept in project-specific files.  All field notebook  entries are made
in waterproof ink. If an error is made, corrections are made by drawing a single  line through  the
mistake and initialed by the person making the correction, entering the corrected information next
to the error.

General field notebook entries include the following: name and number of sampling trip; date of
sampling trip;  general weather and water conditions (waves  and tides);  name of individuals in
sampling team; sample identification number; time of sample  collection; a  description of  the
sampling location; and latitude  and longitude as  determined  with a  GPS  unit, and  sample
preservation method.  Additional information includes sampling equipment used,  decontamination
procedures used, types of QC samples collected, the use of fuel powered units if any, and the depth
that the samples were collected. For the collection of pore water samples, additional information
recorded in the field notebook includes the date and time of purging, the equipment used, the water
level in the lysimeter, the bottom depth of the lysimeter,  the volume of water  removed during
purging, and the specific conductance, temperature, and pH during purging.  For soil and sediment
samples, additional  information  recorded in  the field  notebook include the depth  of sample
collection, physical characteristics of the soil, and method of homogenization.  For tissue samples,
identifying characteristics of the fish are included.

In addition  to the field notebook,  the field sampling team keeps a field instrument sheet.  On this
sheet is recorded the number of each field instrument and probe,  as well as instrument calibration
check information.

7.2    Laboratory Custody

Upon transport of the samples to the  SERF laboratory at FIU, the Chief Chemist checks that the
                                          7-3
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                                                                                Section 7
                                                                            Date: 4/20/99
                                                                              Page 4 of 7

number and identity of the samples matches those on the field notebook (if sampled by FIU) and on
the chain-of-custody form. The samples and coolers are checked for presence of ice, odors and/or
contamination. In addition, the integrity of the samples is checked and any bottles found broken or
leaking are noted in the field notebook and chain-of-custody form.  Samples are logged-in by the
Chief Chemist on the Mercury Sample Log List (Figure 7.2). The temperature of the samples are
checked.  Sample bottles found broken, leaking,  or not properly preserved are rejected from
analysis, and noted on the chain-of-custody form.  The Mercury Sample Log List is kept into the
corresponding sample set folder and serves to track the samples collected from a sampling event
through sample storage, analysis, data validation, and sample disposition with dates and authorized
initials.

Samples will not be rejected based  on incomplete documentation. Analysis will continue,  but
efforts will be made to get the missing information.  If there is still missing information by the time
the results are complete, it will be noted in the data report.

Samples are stored in the appropriate conditions, "mercury-free" room or freezer, in a locked room,
with access to the room limited to SERF employees.  Standards are  stored separately from all
samples. Sample preparation methods are described in the Standard Operating Procedures for the
laboratory (Appendix  C).   Primary and secondary standards for analysis  of  water samples  are
prepared on a daily basis. The standard concentration  and resulting peak height are recorded in the
instrument log book (Figure 7.3). Preparation of all standards (primary and secondary) are recorded
on a separate log (Figure 7.4).

Sample analysis is tracked through sample preparation sheets, instrument printouts, and analytical
calculation sheets.  Examples of each of these sheets for each matrix (water, sediment, tissue) are
included in Appendix D.  Sample analysis is also recorded on the instrument log book (Figure 7.3).
All laboratory  documentation,  Sample  Log Lists, chain-of-custody forms, standard  prep logs,
sample prep logs, instrument printouts, and calculation sheets are kept indefinitely by the  Chief
Chemist in a locked cabinet. All internal memos, phone logs, and sample receipt/log-in forms are
saved as well.

7.3 Electronic Data Records

Data from field measurements and  laboratory analyses are compiled and summarized in  computer
spreadsheet format (Microsoft Excel).  Separate spreadsheets for each sampling day are kept, and a
compilation of all data to date  is  made.  Spreadsheets are stored both on the hard drive of the
computer, as well as onto write-protected floppy disks.  In the event of computer equipment failure,
the data files on the floppy disks are used as backup.  All spreadsheet calculations are checked by
the Chief Chemist or by the QA Officer on a calculator.

The access to these electronic records is  password protected.  A hard copy of the spreadsheets are
stored in the project files indefinitely.

All deletions or corrections will be documented on  a hard copy of the spreadsheet and the person
making the corrections will initial any changes.
                                           7-4
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                                                                                    Section 7
                                                                                Date: 4/20/99
                                                                                  Page 5 of 7
Records of all aspects relating to changes, updates, problems and maintenance of the instrument
and database software will be maintained in the instrument logbooks.

 FIGURE 7.2. Mercury Sample Log Checklist
Sample Checklist
                  Date Received:

                  Date Collected: _

            Collected From (Area):

                Lab Receipt Date:

                   Sample Type:


  Description of Sample Containers
            Analyses
            Required

             THg

            OrgHg

              TP

          Bulk Density

        Ash Free Dry Wt

            NPOC

            Turbidity
    Freshwater

    Seawater
             Technician:

            Received From:

Soil         	Particulates

Sediments
   Number of Containers:

      Type of Containers:

  Containers Labelled as :
Tissue (Fish)
Date Required:  Date Performed:    Data Discarded:
                                Date / Data
                                  Entry:
                                            7-5
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                               Section 7
                            Date: 4/20/99
                              Page 6 of 7
7-6
-------
                                                                     Section 7
                                                                 Date: 4/20/99
                                                                   Page 7 of 7
FIGURE 7.3. Instrument Log Book
                                    7-7
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                                                                     Section 7
                                                                 Date: 4/20/99
                                                                   Page 8 of 7
FIGURE 7.4. Reagent and Standard Prep Log
                                    7-
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                                                                                Section 8
                                                                            Date: 4/20/99
                                                                              Page 1 of 4
8.0    Analytical Procedures
SERF determines total and inorganic mercury concentrations by Cold Vapor Atomic Fluorescent
Spectrometry (CVAFS). A PS Analytical (PSA) 10.025 Millennium Merlin is used to detect total
and inorganic mercury in water samples while a PS Analytical (PSA) Merlin Plus CVAFS mercury
analysis system  equipped with a  PSA autosampler,  a PSA vapor generator,  and a  mercury
fluorescence detector Model PSA 10.023 is used for determination of total and inorganic mercury
in soil and sediment  samples.

The method validation for part per trillion (ppt) concentrations of inorganic and total mercury in
water, solid, and tissue samples (April, 1996) is included in Appendix A. A detection limit of 0.3
parts per trillion (ppt) Hg in water samples is  obtained at a precision of better than 5% relative
standard deviation and an accuracy between 90 and 110%.  Higher levels  of precision and  accuracy
are obtained for sediment and tissue samples due to their inherent higher mercury concentrations.

Organomercury concentrations are determined by capillary gas chromatography coupled with
atomic fluorescence detection (GC-AFS) as described by Cai et  al.  (1996) and Cai et al (1997).
Chromatography is performed with a Hewlett-Packard  (Model 5890 Series n) gas chromatograph
coupled with an HP (Model 7673)  automatic sampler.  A Merlin Mercury Fluorescence  Detector
System (AFS), Model 10.023, (P.S.  Analytical) is used. Initial extracts of sediment and tissue
samples are subjected to sodium thiosulfate clean-up and the organomercury species are isolated as
their chloride  derivatives by cupric chloride and subsequent extraction into  a small volume of
dichloromehtane.  For water samples, the organomercury compounds are pre-concentrated using a
sulfhydryl cotton fiber adsorbent,  followed by elution with Kbr and CuSCn and  extraction in
dichloromethane.   Detection limits  of 0.02  ppt  and 0.02  ppb  are  obtained  for water  and
sediment/tissue samples, respectively. The  method validation for organomercury compounds in
water, sediment, and tissue samples  (November, 1997) is also included in Appendix A.

See Appendix C  for a detailed description  of the  currently used methods in the  corresponding
Standard Operating Procedures.

8.1     Laboratory Operations

Mercury contamination at levels near the method detection limit is a consistent problem  as water
samples easily absorb  mercury from the air and improperly cleaned glassware.  To minimize
contamination, all technicians are required to wear vinyl gloves.  In addition, all glassware, acids,
reagents, pipettes etc. are kept dedicated to mercury analysis and stored in a  mercury-free clean
room.  The clean room contains a  bank of laminar flow hoods equipped with gold and  charcoal
filters.  The floor is  covered with flypaper to trap  particulates.  The clean room also contains a
separate water supply, a refrigeration unit, a drying oven, and an analytical balance used exclusively
for  mercury determinations.  Potential contamination  in  the clean room is checked weekly by
monitoring acidified  (1% HC1) water samples,  which are stored open inside the clean room.  If
significant levels of mercury are detected in these samples (>20 ppt), then  the source of the mercury
contamination is located and eliminated. If necessary, the gold and charcoal filters within the flow
hoods are reconditioned.
                                          8-1
-------
                                                                                 Section 8
                                                                             Date: 4/20/99
                                                                               Page 2 of 4
8.2    Laboratory Glassware Cleaning

Laboratory glassware is kept to a minimum, with Teflon bottles and beakers used when possible.
All reusable laboratory glass bottles, volumetric flasks, and graduated cylinders, and teflon beakers
are dedicated to the preparation and storage of a specific reagent, and are rinsed between usage with
acid (0.5N HC1 and 0.05N HNCb), three times with DIW, and stored  in the mercury-free room.
The volumetric flask used for making the primary standard is dedicated  for that standard and rinsed
only with the standard.  Glassware or plastic containers that have come  in contact with  samples,
such as ampoules and scintillation vials are used once then discarded.

New containers are decontaminated. A log book kept in the Hg-clean  lab (Figure 8.1) is used to
document new containers, dates of decontamination with initials of involved personnel. Results of
quality control tests are also documented in this log book.

8.3    Reagent and Chemical Storage

Reagents and chemicals used in the mercury laboratory include acids, dry chemicals, solvents, and
compressed gases  (Table 8.2).  All acids and dry chemicals are stored in the mercury-free  clean
room.  As each reagent or chemical is received  it is  dated and initialed by the person unpacking it.
When the container is opened for the first time it is dated again and initialed by the opener.  While
being used in the laboratory, compressed gas cylinders are secured upright with straps or chains.

8.4    Waste Disposal

Wastes produced in the laboratory include liquid acids, solvents and salt mixtures.  Many of these
reagents are spent during sample prep and analysis.  Any remaining waste  acids or salt mixtures are
neutralized or diluted, respectively, then washed down the sink to the sanitary sewer. According to
Bade County Code of Regulations Chapter 24-1 l(d), effluents containing 0.01 mg/1 or less of
mercury may be discharged to a sanitary sewer.  The source standard with a concentration of 1 mg/1
Hg, is never emptied  down the sink.  This standard is used  completely to make the primary
standard.  The primary standard has a mercury concentration of 0.1 mg/1, and is diluted 1:10 before
discharged to the sink.  Secondary standards  have a high concentration of 0.0005 mg/1 and do  not
need to be diluted before discharged to the sink. Empty reagent bottles are rinsed with hot tap water
and disposed in trash receptacles. Waste solvents, such as dichloromethane, are stored in a clearly
marked, capped, glass container within a fume hood.  When the container is full  it is picked up
from the laboratory by FIU's Environmental Health  and Safety Department who in turn ensure that
the solvent waste is disposed of by an licensed and approved hazardous waste disposal facility.
                                           8-2
-------
                                                                   Section 8
                                                                Date: 4/20/99
                                                                 Page 3 of 4
FIGURE 8.1 Hg Lab Decontamination Log Book
                                    8-3
-------
                                                                    Section 8
                                                                Date: 4/20/99
                                                                  Page 4 of 4
TABLE 8.1
Reagent and Chemical Storage
Chemical
Laboratory Chemicals
Mineral Acids
Dry Chemicals
Solvents
Compressed Gases
Method of storage

Stored in original glass containers in the mercury-free room.
Stored in original containers in
Stored in original containers in
flammable.
the mercury-free room.
a locked cabinet marked
Secured upright in laboratory.
                                    8-4
-------
                                                                                 Section 9
                                                                             Date: 4/20/99
                                                                              Page 1 of 10

9.0    Calibration Procedures and Frequency

9.1    Instrument

SERF determines total and inorganic mercury concentrations by Cold Vapor Atomic Fluorescent
Spectrometry  (CVAFS)  and  organomercury  concentrations by capillary gas  chromatography
coupled  with atomic  fluorescence detection (GC-AFS).  Instrument lists  for both  field  and
laboratory are included in Tables 9.1 and 9.2, respectively.

9.2    Standard and Reagent Receipt and Traceability

Primary  standards traceable to NIST  reference standards are  purchased from reliable scientific
supply firms. The manufacturer's certificates for each standard received are kept on file in a central
location. The  standards and reagents  are  received by the Chief Chemist, inspected, dated,  and
initialed  directly on all chemical bottles.  Once opened, the standard/reagent bottles are  dated and
initialed again.

Primary and secondary standards are prepared daily by diluting the source  and primary  standards,
respectively, with mercury-free water.  Records of the standard and reagent preparation ( including
calibration, QC, and MDL standards)  are kept in the reagent and standard prep log book (Figure
7.4).   Once prepared, the standard/reagent  solutions  are dated,  initialed,  marked  with the
concentration, and referenced  to the stock solutions  with the date the stocks  were opened.  The
expiration date and storage instructions are recorded as well on the standard/reagent bottles. As no
new standard  or reagent is prepared until the previous  one has been either completely  used or
expired and discarded, the logbook records link the preparation with every specific analysis.

9.3    Standard Sources and Preparation

The source, preparation, and storage of standards for each sample matrix are included on  Table 9.3.
 Standard preparation methods are available in the laboratory SOPs (Appendix C).  The calibration
secondary  standard  for total  and inorganic mercury is prepared on a daily basis from  a  primary
NBS certified mercury source standard of 1000 |ig Hg/ml (Fisher Scientific) and the second source
secondary standard is prepared from a primary SPEX 1000 |ig Hg/ml solution. Due to  their high
mercury  concentrations, the primary and secondary  standards are stored outside the mercury-free
room.  The  working calibration  and  second source standards are prepared  daily   from the
corresponding secondary standard solution.

The methyl and ethylmercury chloride standards are purchased from Ultra Scientific. The primary
standards are  prepared from  the  source by dissolving  appropriate amounts of the standards in
Optima grade methanol ( Fisher Scientific ). A mixed methyl & ethylmercury chloride  secondary
standard is prepared in methanol from the primary solutions and stored in dark.  The working,
spiking , and calibration standards are prepared consecutively by dilutions in DIW.

A detailed description of the standard  preparation procedure for every matrix/analyte combination
is included in the specific SOPs in Appendix C.
                                           9-1
-------
                                                                      Section 9
                                                                  Date: 4/20/99
                                                                   Page 2 of 10
TABLE 9.1
Field Instrument List
Manufacturer
Field Equipment
Orion
Orion
Model

140 Conductivity/
Salinity/
Temperature Meter
SA 250 Meter and
Ross Combination
Electrode
Parameters

Conductivity,
Temperature
PH
Matrix

PW
PW
TABLE 9.2
Laboratory Instrument List
Manufacturer
P. S. Analytical Ltd.
P.S. Analytical Ltd.
Hewlett-Packard
Wilmont Castle Co.
Fisher Scientific
Allied
Osterizer
Model
Merlin Plus
Fluorescence
Detector (detector
PSA 10.023)
10.025 Millennium
Merlin System
Model 5890 Series H
Gas Chromatograph
Thermatic 60
Autoclave
73 8F Isotemp Oven
Model 7303DA
Balance
10 Speed Blender
Parameter
Inorganic and Total
Mercury
Inorganic and Total
Mercury
Methyl & Ethyl Mercury
Methyl & Ethyl Mercury
and Total Mercury
Dry Weight
Wet and Dry Weight
Methyl & Ethyl Mercury
and Total Mercury
Matrix
S, SED, T
SW, PW, GW
SW, PW, GS, S,
SED, T
S, SED, T
S, SED
S, SED, T
S, SED, T
                                     9-2
-------
                                                                                                               Section 9
                                                                                                            Date: 4/20/99
                                                                                                            Page 3 of 10
TABLE 9.3
Standard, Source, Preparation, and Storage
Instrument/
Parameter
Merlin Plus
Fluorescence
Detector


















Standard
Sources
FISHER
SMI 14-100






SPEXPLHG4-
2Y





NIST Sediment
8407 and 8406
NBS Oyster
Tissue 566a

NRCC
DORM-2

How Received
lOOOppm Solution
(100ml)






lOOOppm Solution
(100ml)




	 SRMs 	
Dry Soil Standards

Dry Tissue Standard


Dry Tissue Standard

Source
Storage
Room
Temperature
outside the
Hg-free room




Room
Temperature
outside the
Hg-free room




Desiccator in
the Hg-free
room
Desiccator in
the Hg-free
room
Desiccator in
the Hg-free
room
Preparation from Source
. Secondary from source:
100 ppb

. Working from secondary:
See SOPs 002-99 and 003-
99 in Appendix C

O J?
. secondary trom source:
100 ppb
. Working (QC-check)from
secondary: See SOPs 002-
99 and 003-99 in Appendix
C.

Digested as if a solid
sample
Digested as if a tissue
sample

Digested as if a tissue
sample

Lab Stock Storage
Room Temp, outside
the Hg-free room





Room Temp inside
the Hg-free room





Not Applicable

Not Applicable


Not Applicable

Preparation
Frequency
Daily







Daily





Daily

Daily


Daily

                                                          9-3
-------
                                                                                                               Section 9
                                                                                                            Date: 4/20/99
                                                                                                            Page 4 of 10
TABLE 9.3
Standard, Source, Preparation, and Storage
Instrument/
Parameter
10.025
Millennium
Merlin
System




HP Gas
Chromato-
graph





Standard
Sources
FISHER
SMI 14-100



SPEXPLHG4-
2Y

Ultra Scientific





How Received
1 000 ppm Solution
(100ml)



1000 ppm Solution
(100ml)

Dry methyl- and
ethylmercury
chloride crystals





Source
Storage
Room
Temperature
outside the
Hg-free room


Room
Temperature
outside the
Hg-free room
Desiccator
outside the
Hg-free room





Preparation from Source
. Secondary from source:
100 ppb
. Working from secondary:
See SOP 001-99 in
Appendix C

. Secondary from source:
100 ppb
. Working (QC-check)from
secondary: See SOP 001-99
in Appendix C
. Primary from source in
methanol

. Secondary from primary
in methanol


.Working from secondary
inDIW
Lab Stock Storage
Room Temp, outside
the Hg-free room
Room Temp, inside
the Hg-free room


Room Temp, outside
the Hg-free room
Room Temp, inside
the Hg-free room
Stored in a dark
bottle in desiccator
outside the Hg-free
room.
Stored in a dark
bottle in desiccator
outside the Hg-free
room.
Not Applicable
Preparation
Frequency
Daily



Daily

Yearly

Monthly


Weekly
                                                          9-4
-------
                                                                                                               Section 9
                                                                                                            Date: 4/20/99
                                                                                                            Page 5 of 10
TABLE 9.3
Standard, Source, Preparation, and Storage
Instrument/
Parameter
HP Gas
Chromato-
Graph (cont.)






Orion
S/C/T Meter






Orion pH
Meter
Analytical
balances
Standard
Sources
Ultra Scientific






Canada
National
Research
Council
Orion







Fisher
Scientific, Inc.
Troemner

How Received

Dry methyl- and
ethylmercury
chloride crystals




SRM
Dry Tissue Standard

1000ml
Conductivity
Solutions (98.6,
993, and 102822
|omhos/cm) and
Salinity standard
(Gulf Stream Water,
36 ppt)
pH 4.0, 7.0 and 10.0
solutions
Stainless Steel
(class S weights)
Source
Storage
Desiccator
outside the
Hg-free room




Desiccator in
Hg-free room

Room
Temperature






Room
Temperature
Room
Temperature
Preparation from Source

. Spiking from Working in
DIW

. Calibration from Spiking
in DIW
See SOPs 004-99, 005-99,
and 006-99 in Appendix C
Digested as if tissue sample

Used Directly







Not Applicable

Not Applicable

Lab Stock
Storage
Not Applicable


Not Applicable



Not applicable

Room
Temperature






Not Applicable

Not Applicable

Preparation
Frequency
Daily


Daily



Daily

Replace on
expiration






Replace on
expiration
Daily, Semiannual
Service Calibration
                                                          9-5
-------
                                                                                Section 9
                                                                           Date: 4/20/99
                                                                            Page 6 of 10

An NIST certified Tennessee River sediment (8406, 60 ppb Hg or 8407, 50 ppm Hg) is used as a
Standard Reference Material (SRM) for total mercury determination in soils and sediments .
Either an NBS certified oyster tissue (566a , 60 ppb Hg) or a NRCC (National Research Council
of Canada)  certified dogfish muscle (DORM-2,  4600 ppb Hg) is  used as the SRM for total
mercury analysis in fish  tissue  samples. Both the sediment and tissue SRMs are digested  and
analyzed in the same manner as the unknown samples.

The NRCC certified dogfish muscle (DORM-2, 4600 ppb Hg) is also used as standard reference
material for organic mercury determination in fish tissue samples.

9.4 Instrument Calibration

All field and laboratory instruments are calibrated, and checked for proper function in the field prior
to analysis.   Table 9.4  summarizes the calibration  procedures for both  field and  laboratory
instruments.  Calibration procedures for all instruments are described below.

9.4.1  Field Instruments

Field  instrument calibration checks are recorded on the Field Instrument Calibration Sheet, which
are kept in individual project files.

9.4.1.1.  Salinity/Conductivity/Temperature

The Orion model 140  Salinity/Conductivity/Temperature meter, with a 014010 4-electrode probe,
is factory calibrated and compensated for temperature. Salinity and/or conductance is checked daily
with a solution of  known salinity or conductance, while temperature is checked daily against an
NIST thermometer. The S/C/T meter probe and the NIST thermometer is inserted into 25 ml of the
salinity and/or conductance standard (See Table 9.3). A conductivity and/or salinity reading within
5% of the standard value, and a temperature within 0.1 degrees are considered acceptable.  Values
outside these acceptance criteria will require the unit to be factory calibrated.

9.4.1.2. pH

The pH meter/probe  is  calibrated before each field day.  We use an automatic temperature
compensation (ATC) probe to adjust for  differences in temperature between standards and samples.
 Standard  pH  buffers ( pH  7.00, cat. no.  SB108-500; and  10.00, cat. no. SB  116-500)are
purchased from Fisher Scientific.  The two-point calibration procedure is as follows:

       1.      Choose pH 0.01 mode.
       2.      Rinse probes (pH combination and ATC) in DIW.  Blot dry. Rinse with ca. 2 ml of
              pH 7.00 buffer. Immerse probes in pH 7.00 buffer.
                                          9-6
-------
TABLE 9.4
Instrument Calibration
Instrument
Orion S/C/T Meter
Conductivity-
Temperature
Orion pH Meter

PSA Merlin Plus
Mercury System


GC-AFS



Calibration
Type

Continuing
Check
Continuing
Check
Initial
Continuing
Initial
Continuing

Initial

Continuing

No. of
Standards

3
1
2
1
4
1 Blank
1 Interned.

5

1 Blank
1 Interned.

Type of
Curve

Linear
Linear
Linear
Linear
Linear


Linear



Acceptance/ Rejection
Criteria

Conductivity within 5%
of Standard Value
Temperature within 0.1
degrees of NIST
thermometer value
Reading must be with
0.05 pH units.
Reading must be within
0.05 pH units.
R2>0.995
Value of Zero
85-1 15% of initial
calibration
R2>0.995

Value of Zero
85-1 15% of initial
calibration
Frequency

Daily, prior to use,
every 4 hours, and
end of each use.
Daily
Daily, prior to use.
Every 4 hours, and
end of each use.
Daily, prior to each
run
Every 10 samples

Daily, prior to each
run
Every 10 samples

                                                                                                                Section 9
                                                                                                             Date: 4/20/99
                                                                                                             Page 7 of 10
                                                          9-7
-------
                                                                                                                  Section 9
                                                                                                              Date: 4/20/99
                                                                                                               Page 8 of 10
TABLE 9.4 (cont.)
Instrument Calibration
Instrument
10.025 Millennium Merlin
System


Calibration
Type
Initial
Continuing

No. of
Standards
4
1 Blank
1 Interned.

Type of
Curve
Linear


Acceptance/ Rejection
Criteria
R2>0.995
Value of Zero
85-1 15% of initial
calibration
Frequency
Daily, prior to each
run
Every 10 samples

                                                           9-8
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                                                                                 Section 9
                                                                             Date: 4/20/99
                                                                              Page 9 of 10

       3.     Press Cal button. The meter will display ".1." and the pH value of the buffer; the
              meter automatically recognizes the pH of the buffer solution.  When pH stabilizes,
              press Enter. The display will freeze for 3 seconds, and then display ".2.".
       4.     Rinse probes in DIW.  Blot dry.  Rinse with ca. 2 ml of pH 10.01 buffer. Immerse
              probes in pH 10.00 buffer.
       5.     Wait for pH display to stabilize, and press Enter.  Display now will say "PH" and be
              ready for sample measurement.
       6.     Rinse probe  in DIW,  place probe in pH 7.00 buffer,  and  check that pH  meter
              reading is within 0.05 pH units.
 In case of low pH level samples, the pH 4.00 and pH 7.00 standards will be used in the calibration
procedure.

The response of the pH meter is checked with the pH 7.00 buffer after 4 hours of use and at the end
of each use. If the response is outside 0.05 pH units, the two-point calibration is repeated.

9.4.2   Laboratory Instruments

The  PS  Analytical  Merlin Plus  and Millennium Merlin mercury instruments  are  calibrated
according to the following procedures:

       1.     Initial  calibration is a four-point standard  curve.   The  range of
              standards reflect the expected range of sample concentrations.  For
              low  level water samples,  standards include  0, 2.5,  5 and 10 ppt.
              Standards run for tissue and sediment samples usually include 0, 25,
              50, and 100 ppt.
       2.     All standards are run in duplicate and plotted on a linear calibration
              graph using the software inherent to the instrument or a specific
              Microsoft Excel calculation template.
       3.     The  linear correlation coefficient is checked by the analyst to ensure
              that  it is  0.995 or better. Standard curves  outside the acceptable
              limits are run again, and new standards are prepared if necessary.
       4.     A second source standard  (calibration check) is analyzed at the end
              of the standard curve with a concentration of 1-2 times the PQL to
              monitor instrument sensitivity and accuracy.
       5.     A method  blank  and a  middle  level standard are  analyzed in
              duplicate following the standard  curve and  at a frequency of 5%,
              thereafter. The blanks  should be less than the corresponding MDL
              and the middle level standard should fall within the 85-115 % of the
              initial calibration range. If outside the acceptable levels, the  run is
              stopped, and initial calibration is begun again.
       6.     For  solid and tissue  samples analyze one QC check standard, in
              duplicate, per sample set.

Multiple dilutions of the primary standard, as required to make the low calibration standard of 10
ppt, often results in error, thereby producing a standard curve that does not intercept the origin. The
                                           9-9
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                                                                                  Section 9
                                                                              Date: 4/20/99
                                                                             Page 10 of 10
sensitivity of the Merlin Plus System is such that a zero mercury concentration results in a zero
result.  Therefore, once the standard curve is checked for linearity within the acceptable limits, the
curve is dropped parallel through the origin by subtracting the intercept value from all the points.
Mercury concentrations in samples are then determined by comparing sample peak heights to the
new standard curve.

The results of the standard curve generated, the resultant correlation coefficient, and results of QC
check samples for each run are kept with the analytical results in project specific files. Examples of
standard curves generated for each matrix (water, sediment, tissue) are included in Appendix D.

The GC-AFS system is calibrated for organic mercury analysis according to the following:

       1.     A standard curve is created at the beginning of each  run by running the
              following  concentrations: 0.0, 0.833, 1.667,  2.500, and 3.333 pg/joL for
              water samples; 0.0, 1.25, 2.50, 3.75, and 5.00  pg/joL for solid samples.
       2.      All standards are run in duplicate and plotted on a linear calibration graph
              using the software inherent to the instrument or a specific Microsoft Excel
              calculation template.
       3.     The linear correlation coefficient is checked by the analyst to ensure that it is
               0.995 or better.  Standard curves outside the acceptable limits are run again,
              and new standards are prepared if necessary.
       4.     A blank and a middle level standard are analyzed in duplicate following the
              standard curve and at a frequency of 5%, thereafter. The blanks should be
              less than the corresponding MDL and the middle level standard should fall
              within the 85-115 % of the initial calibration range. If outside the acceptable
              levels, the run is stopped, and initial calibration is begun again.
       5.     All samples are run in duplicate.
       6.    For sediment and tissue samples two duplicate samples and one matrix spike
              sample are run for every sample.
                                           9-10
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                                                                              Section 10
                                                                           Date: 4/20/99
                                                                             Page 1 of 2
10.0   Preventive Maintenance
10.1   Routine Maintenance

Preventive maintenance is an essential part of a properly functioning laboratory.  Maintenance of
field and laboratory instruments are summarized on Tables 10.1  and 10.2.  For the Merlin Plus
System, maintenance includes running DIW through the instrument for 15 minutes at the beginning
and end of each day. The gas separator is cleaned as needed.

10.2    Maintenance Documentation

A use log book is kept on each mercury instrument.  Instrument response to calibration standards,
the  number of samples run, and the hours of instrument use are recorded in each log book.  In
addition, all maintenance activities for each instrument are recorded in the  log book. A record of
service performed by the manufacturer or other service contractor is kept in the instrument files.

10.3    Contingency Plans

SERF maintains a stock of spare parts for its analytical instruments.  Instruments which can not be
fixed by SERF personnel are sent to the manufacturer or other service contractor.

TABLE 10.1 Field Equipment Preventive Maintenance
Instrument
pH meter
Dissolved oxygen meter
and S/C/T meter
Activity
Check batteries - recharge
Check liquid in probe
Replace probes
Rinse with analyte-free water
Check batteries - recharge
Check probes
Frequency
Daily
Daily
Every 6 to 9 months
Before and after each use
Daily
Daily
                                         10-1
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TABLE 10.2 Laboratory Equipment Preventive Maintenance
                                                                            Section 10
                                                                         Date: 4/20/99
                                                                           Page 2 of 2
 Instrument
Activity
Frequency
 PSA Merlin Plus
Rinse with DIW for 15 minutes
Replace tubing
Replace wash water
Clean gas separator
Beginning and end of day
As needed
As needed
As needed
 PSA Millennium Merlin
 System
Rinse with DIW for 15 minutes
Replace tubing
Replace wash water
Clean gas separator
Beginning and end of day
As needed
As needed
As needed
 GC-AFS
Replace Septum
Replace Column
Replace Pyrolyzer
Replace silanized glass wool in glass
linear
Every 100 injections
As needed
As needed
As needed
 Analytical Balances
Clean weighing compartment
Clean interior/exterior
Check calibration
Factory service calibration
Daily
Monthly
Daily
Semi annually
 Ovens and Refrigerators
Check temperature
Calibrate with NIST thermometer
Daily
Annually
                                        10-2
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                                                                             Section 11
                                                                           Date:4/20/99
                                                                             Page 1 of 5
11.0   Quality Control  Checks and  Routines to Assess  Precision, Accuracy  and
       Calculation of MDLs

SERF uses both field and laboratory QC check samples.  Each of these QC check samples are
included on Table 11.1.

11.1   Field QC Checks

SERP's  field quality  control includes the collection of one duplicate sample for every 10 field
samples collected. In addition, according to FDEP-QA-001/90, one pre-cleaned equipment blank is
prepared for every 10 samples.  For sampling events involving 1 to 10 samples, one equipment
blank is prepared. This blank is prepared in the field prior to sampling by pouring or rinsing using
analyte-free water on each piece of precleaned field sampling equipment.  Equipment blanks for
surface water samples are  collected by running analyte-free, water through the vacuum system then
into the sample bottle. For pore water samples, the equipment blank is prepared by running DIW
through the peristaltic pump then into sample bottles.   For  soil  and sediment samples, the
equipment blank is prepared by pouring DIW over the sampling equipment and into the appropriate
sample  bottles.  All duplicate and  blank  samples are placed in  appropriate bottles with the
corresponding preservatives for each analysis. The collection of blank samples are recorded in the
field note book. For field equipment cleaned in the field, an additional equipment blank is prepared
following the field cleaning procedures at a frequency of one per sampling event or one every 10
samples, whichever is greater.  The time and number of all equipment blanks are recorded in the
field note book.

Field instrument checks are completed  prior to each sampling event, once every four hours of
operation and  at the  end  of the field sampling event.   The results of  the  field QC  checks are
recorded on the Field Instrument Calibration Sheet.  Field equipment not functioning properly are
not used to collect  data  until they are brought back to the  laboratory  for maintenance and
recalibration. Duplicate field equipment and probes are kept on hand in the laboratory if needed.

11.2   Laboratory QC Checks

SERP's  standard laboratory QC checks includes blanks, replicates, matrix spikes and QC
standards and QC check samples. Method reagent blanks consisting of analyte-free water are
prepared exactly like a sample and run prior to each instrument calibration.  As standard practice
SERF usually analyzes all samples in replicate. In the laboratory, water samples are split into
two bottles, and each bottle is analyzed three times for a total of six data points for one sample
location. One of every ten water samples has two additional bottles prepared so that two bottles
are analyzed asreplicates and two bottles are spiked to serve as matrix spikes. For total mercury
determinations, two ampoules are prepared for each sediment and fish sample, and each ampoule
is analyzed two times. For organic mercury determinations, four replicate samples are prepared
for each fish and sediment sample, with  two run as replicate samples and the remaining two are
spiked to serve as matrix spikes.
                                          11-1
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                                Section 10
                              Date: 4/20/99
                               Page 2 of 2
11-3
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                                                                                                                                      Section 11
                                                                                                                                   Date:4/20/99
                                                                                                                                     Page 2 of 5
Table 11.1
Quality Control Checks
 Type
Description
No. of samples
per event
Frequency (all parameter groups unless
specified)
 Field
 Equipment Blank
 (non-field cleaned
 equipment)
Fill or rinse all pre-cleaned sampling
equipment (tubing, syringes, filter holders,
etc.) with analyte-free water, fill
appropriate sample containers and preserve
according to each analysis.
                  1 prepared on-site at the beginning of the sampling
                  event

                  1 prepared on-site at the beginning of the sampling
                  event, and after every 20 samples
 Equipment Blank
 (field cleaned
 equipment)
If equipment is cleaned on-site, then
prepare additional equipment blank sample
by filling or rinsing the field-cleaned
equipment with analyte-free water, filling
the appropriate sample containers and
preserve according to each analysis.
                  1 at the beginning and end of the sampling event
                                                                                    1 after every 20 samples or 5 % (whatever is
                                                                                    greater)
 Field Duplicate
A duplicate sample collected and analyzed
for the same parameters as the original
sample.
1-10
1 sample is collected in duplicate

1 after every 10 samples or 5 % (whatever is
greater)
 Field Measurements
 QC Check Standards

 pH meter
Record the results of calibration check
standards for all field measurement
equipment.
Record two or more pH readings in field
note book until sequential values are within
0.02 pH units.
1 or more
                                                                  1 or more
Beginning of each sampling event, once every four
hours, and again at end of the sampling day
Every sample.
                                                                      11-2
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                                                                                                                                    Section 11
                                                                                                                                  Date:4/20/99
                                                                                                                                   Page 3 of 5
TABLE 11.1 Continued.
Quality Control Checks
 Type
Description
No. of Samples
per Event	
Frequency (All parameters unless specified)
 Laboratory
 Method Reagent Blank
Analyte-free water
1 or more
samples
1 at beginning of a run, after every 10 samples, and at
the end.
 Replicate Samples
Re-analysis of a sample
1 or more
samples
Every sample is analyzed 2 to 4 times
 Continuing Calibration
 Standards
One standard at a level of 1 to 2X the PQL
(included in the standard curve) and one
intermediate standard
1 or more
samples
Analyzed at the beginning of each run, and at a
frequency of 5%, thereafter.
 Matrix Spikes
One sample from a set (not blanks) is split
in two, and one of the duplicates is spiked
with a known concentration (3 to 5 times
higher than the original expected
concentration) prior to sample preparation.
1 or more
samples
1 sample in a set or at a frequency of 5%, whichever is
greater.  Except for organic mercury in sediment and
tissue samples, 1 matrix spike is performed on every
sample.
 Quality Control Check
 Standards
Standards from an independent source that
are certified and traceable (i.e. NIST). Can
be interchanged as one of the continuing
calibration check standards.
1 or more
samples
Analyzed at the beginning of each run to check the
initial calibration of the standard curve.
 Quality Control Check
 Samples
Samples of known analytical concentration
that are submitted blind to the analyst.
These samples are either prepared in house
or obtained from an independent source.
1 or more
samples
Analyzed in duplicate quarterly.
                                                                     11-3
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                                                                              Section 11
                                                                            Date: 4/20/99
                                                                              Page 4  of 5
Matrix spikes samples are prepared by adding a known concentration approximately 2 to 5 times
the original  expected concentration (e.g. 1 ppt for total mercury water samples) to the duplicate
bottles or ampoules. The concentrations from the unspiked duplicate is subtracted from the spiked
result and the percent recovery is determined by comparing the remainder to the known spike
concentration.

Continuing calibration standards (intermediate level) are run at the beginning of each run and at a
frequency of 5% thereafter.  A QC check standard (a certified standard from an independent source)
is run at the beginning of a run to check the calibration curve. A quality control check standard is
typically an intermediate or high end standard.

A Standard Reference Material sample (if available) is included in every run to check the accuracy
of the analytical procedure. Quality control check samples are prepared in-house or from an NIST
or other certifying source and are submitted  blind to the analyst on a quarterly basis to check
instrument and user performance. If the blind QC check sample results is not acceptable, the results
will be reported in the QA report to FDEP.

11.3   Routine Method Used to Assess Precision and Accuracy

Precision and accuracy of each analytical parameter determined in the laboratory is determined on a
daily basis.  Precision is defined as the agreement or closeness of two or more results.  As stated
above, SERF performs 2 to 8 replicate analyses on the same sample.  For samples analyzed 3  or
more times, SERF usually determines the mean (X) and standard deviation (SD)  of the replicate
analyses and estimates precision in terms of percent relative standard deviation (% RSD) using the
following equation:
                    %RSD=   SD * 100
                                X

The acceptance criteria for % RSD depends on the analyte/matrix combination (See Table 5.2).

The Relative Percent Difference (RPD) is another parameter used to  monitor the precision of our
analytical results and it  is calculated for Matrix Spike  duplicates and/or sample  duplicates.  The
acceptance criteria is usually RPD <= 20 - 30 % (See Table 5.2 for specific analyte/matrix targets).

Replicate  results that  are outside the +/-2SD range are automatically eliminated from the
calculations by the corresponding Microsoft Excel template to ensure precision and reliability  of
the final results.

Accuracy is defined as the agreement between the analytical results and the known concentration.
Accuracy is determined by running matrix spikes  (MS) and/or standard reference materials (SRM)
and is determined as percent recovery (% R) according to the following equations:

                    %R=  Cs-Cu  * 100
                    MS     S
                                           11-4
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                                                                               Section 11
                                                                            Date: 4/20/99
                                                                              Page 5 of 5
Where:
        Cs = concentration of spiked sample
        Cu = concentration in unspiked sample
         S = expected concentration of spike in sample
        %R = percent recovery
                     % R = Sample Concentration * 100
                     SRM    True Value

The control limits for accuracy are +/- three standard deviations of the historical percent recovery
average , with warning limits set at +/-  two standard deviation.  When no historical  limits  are
available SERF usually uses an acceptance limit of 75-125% of the expected value (See Table 5.2).

The results obtained for each quality control check are compared to their acceptable  limits  for
precision and accuracy on a daily basis. New limits (both control and warning) based on historical
data are calculated on a quarterly basis .

11.4   Method Detection Limits

Method detection limits (MDLs) have been determined according to the EPA procedure described
in 40 CFR  Part 136, Appendix B, revision 1.11, except that a multiplier of 3 is used instead of the
Student's t  value.  Specifically, seven or more replicate samples containing an analyte at a known
low concentration are analyzed according to the appropriate analytical procedure for that analyte. A
standard deviation for the replicates is determined and the MDL  is computed as 3  times  the
standard deviation.   The practical  quantitation  limit (PQL) is defined as 12 times the standard
deviation. MDLs and PQLs are routinely verified/updated on a yearly basis.
                                           11-5
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                                                                                Section 11
                                                                             Date: 4/20/99
                                                                               Page 1 of 5
12.0   Data Reduction, Validation and Reporting

12.1   Data Reduction

Data reduction is not necessary for field data, as field measurements are read directly from the field
instruments in their appropriate reportable units. The pH meter and SCT meter are automatically
compensated for temperature.

All data reduction (both field and laboratory) is performed according to the protocols specified by
the analytical methods listed in Section 5. Each technician is responsible for data entry of field data
from the field notebook into Microsoft Excel spreadsheets.  Instrument produced  peak heights are
converted to concentrations by comparison to the standard curve by the  analytical  instrument.
Sediment and tissue samples are  corrected for dilutions and for the weight of the sample by the
analyst.

Replicate sample results are further reduced to provide one data point  per sampling location. The
mean  and  standard  deviation  of each  sample  result  is  calculated using  Microsoft  Excel
spreadsheets.  Any replicate result that is two  standard deviation away from the  mean (+ or -)  is
removed from the replicate data set.

12.2   Data Validation

The Chief Chemist and analytical technicians  are responsible for the collection, custody, storage,
and analysis of all of the samples.  It is their responsibility to check for sample integrity and that the
samples are analyzed within the appropriate holding times. They are also responsible for the proper
maintenance of all equipment and cleaning of laboratory glassware. They provide the first check on
instrument calibration, method blanks, and equipment blank results,  and  ensure  that all method
specifications have been met.  If problems arise  during  an analysis, such as failure of proper
equipment calibration, or unusual sample results,  it is their responsibility to verbally notify the
laboratory director as soon as possible.

The QA Officer is responsible for a second  check  of instrument calibration by comparing the
present instrument responses  to historical values.   The QA Officer checks all sample preparation
and instrument logs. In addition, the QA  officer checks the results of method blanks, equipment
blanks, sample  replicates,  matrix spikes  and field  calibration  checks  and determines that the
instrument precision and accuracy is within  the  QA objectives listed in Section  5.  Obvious
anomalous results are subject to re-analysis.

Dr. Jones, the director, is responsible for the final  review of all data and  documents that are
submitted to the client (EPA, DOI, NFS,  FDEP,  SFWMD).  Due to  his extensive experience in
analytical chemistry, Dr. Jones can apply both  objective and subjective techniques to data review.
From his  knowledge of analytical chemistry, Dr. Jones can interpret the data in its environmental
context.   In addition, through his collection of historical data in South  Florida, Dr. Jones can
identify potential outliers in a data set.
                                           12-1
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                                                                              Section 11
                                                                           Date: 4/20/99
                                                                             Page 2 of 5
12.3   Data Reporting
Once the instrument calibration and sample results have been validated, they are entered into input
data files. The laboratory technicians are responsible for entering the raw data into the spreadsheet
and providing a first check of data entry.  The QA officer provides a second check of the input data,
spreadsheet calculations and output file formats.  Once all of the data has been validated, the QA
officer will provide a written statement of validation along with the data report.

For  data reports issued to  the client for DEP related work, or for reports issued  to DEP, the
following information will be included:
       a.      Laboratory name, address, and phone number
       b.      Client name and/or site name
       c.      CompQAP number
       d.      Client or field identification number
       e.      S ampl e i dentifi cati on numb er
       f      Method  name and number/reference of each analysis
       g.      Analytical result with applicable data qualifiers
       h.      Date of sample preparation
       i.      Time of sample preparation if holding time is less than 48 hours
       j.      Date of sample analysis
       k.      Date and time of sample collection
       1.      Identification   of all  laboratories  providing  analytical  results,
              including their CompQAP number

A copy of the final data report is included as Figure 12.1.

12.4   Data Storage

Data input  files and final report files are stored on hard drive and floppy disk using names that
readily identify a sampling event.  Files labeled by sampling event are stored in a locked file cabinet
with limited access by SERF employees only.  These files contain hard copies of the file input and
output as well as all raw laboratory data sheets and field note book sheets.  Raw laboratory output
data sheets  are identified with a date, analysis, analyst  initials, and sampling  event  number.
Pursuant to Chapter 62-160 F.A.C., all records will be maintained for a minimum of 3 years.
                                          12-2
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                                                                           Section 11
                                                                        Date: 4/20/99
                                                                          Page 3 of 5
   FIGURE 12.1
   Final Data Report
   Southeast Environmental Research Program
   Mercury laboratory
   CompQAP No.:	
   Client Name:
   Site Name:
                     Florida International University
                     OE 148      Miami, FL 33199
                     (305) 348-3095
   Matrix (water, sediment, fish):
Sample
ID

























Bottle
#

























Sampling
Date

























Sampling
Time

























Sampling
Depth (m)

























Sample
Prep
Date/Time

























Sample
Anal.
Date/Time

























Parameter
Name/SOP#

























Result
/units

























QA
Code

























Other Laboratories providing analytical results:
Lab :	  CompQAP # :_
Lab:
CompQAP # :
Analyses:

Analyses:
                                         12-3
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                                                                     Section 11
                                                                   Date: 4/20/99
                                                                     Page 4 of 5
SERF Lab Manager:
                                      12-4
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                                                                                Section 13
                                                                             Date: 4/20/99
                                                                               Page 1 of 3
13.0   Corrective Action
Corrective action  is taken whenever the quality  assurance  objectives have  not  been met.  A
summary  of the corrective actions for the laboratory and for the field are included in Tables 13.1
and 13.2, respectively.

The analyst, either the Chief Chemist or the technicians, are responsible for providing a first check
for compliance, and initiating corrective action procedures as described in Table 13.1.  The QA
Officer is responsible for  a second  check for compliance, and  initiating corrective action as
appropriate.  If problems continue, then the analyst and/or QA officer will notify the laboratory
director immediately, who may initiate further steps in solving the problem.

Any corrective action taken will  be  documented  in one of the following:   analyst log books,
instrument log  books, or project-specific files. Samples requiring reanalysis will be noted on the
analysis sheet.

FDEP recommended corrective action will be initiated as a result of systems or performance audits,
split samples or data validation review.
                                           13-1
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                                                                             Section 13
                                                                          Date: 4/20/99
                                                                            Page 2 of 3
TABLE 13.1
Corrective Actions for the Laboratory
 QC Activity
Acceptance Criteria
Recommended Corrective
Action
 Initial Instrument Blank
Instrument response 0.995
Reanalyze standards, if same
response, reoptimize
instrument, if same response,
prepare new standards, notify
Dr. Jones and QA Officer
 Matrix Spikes
See Table 5.2 and specific
SOPs in Appendix C
Reanalyze matrix spike, if
same response, prepare and
run a new matrix spike, if
same response, notify Dr.
Jones and QA Officer.
 QC Check and Continuing
 Calibration Standards
See Table 5.2 and specific
SOPs in Appendix C
Reanalyze check standard, if
same response, prepare new
check standard, if same
response, prepare new
primary and calibration
standards, notify Dr. Jones
and QA Officer.
 Replicate Sample
See Table 5.2 and specific
SOPs in Appendix C
Determine cause: baseline
drift, carryover, etc.
Reanalyze all samples
between duplicates, notify
Dr. Jones and QA Officer.
 Duplicate Sample
See Table 5.2 and specific
SOPs in Appendix C
Reanalyze duplicates,
reanalyze all samples
between duplicates; notify
Dr. Jones and QA Officer
                                         13-2
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TABLE 13.2
Corrective Actions for the Field
                                                                              Section 13
                                                                           Date: 4/20/99
                                                                             Page 3 of 3
 QC Activity
Acceptance Criteria
Recommended Corrective
Action
 Initial Calibration Standards
Value within +/- 5% of
expected value
Reanalyze standards, if same
response, optimize
instrument, if same response,
use new standards; notify
Dr. Jones and QA Officer.
 QC Check Standards
Value within +/- 2 standard
deviations of the historical
value
Reanalyze QC check
standard, if same response,
prepare new QC check
standard, if same response,
recalibrate; notify
Dr. Jones and QA Officer.
 Equipment/Trip Blank
Value 
-------
                                                                               Section 14
                                                                            Date: 4/20/99
                                                                              Page 1 of 6
14.0   Performance and System Audits

Dr. Jones supervises all aspects of field and laboratory activities. He requires the laboratory and all
instrumentation to be clean and working at optimum conditions.  He is knowledgeable on the inner-
workings of each instrument and checks on their performance as well as on the performance of the
laboratory personnel continually.

14.1    System Audits

14.1.1  Field Audit

A field audit is conducted at least on an annual basis by the QA Officer.  During these audits, the
QA Officer will  review and evaluate  the  various components  of the measurement system  to
determine their proper selection and use according the specific Project Quality Assurance Plan.
Specifically, the auditor will provide a detail  review  of sampling technique,  field instrument
calibration, field decontamination procedures, sample  custody, sample preservation, and field note
book documentation. The checklist included as Figure 14.1 will be used during the field audit, any
discrepancies or deviations will be noted in the checklist and corrected immediately.  At the end of
the audit, the QA officer will date and sign the checklist stating that the audit was completed, and a
copy of the checklist will be put in the project-specific files.

14.1.2  Laboratory Audit

A laboratory system  audit is conducted  on a weekly basis by  the Chief Chemist.  These audits
consist of an evaluation of all laboratory activities.  The Chief Chemist inspects that the procedures
and documentation for sample log-in, sample preparation, and sample preservation are appropriate
for the methodology and Project QA plan.  In addition, the  Chief Chemist checks that the samples
are analyzed within  their appropriate holding  times, and that the instrumentation is  properly
calibrated and that the  appropriate type and number of QA  samples are run.  The  checklists
included as Figure 14.2 is used  during the audit.   Deficiencies found during the audit are
documented on the checklist as well as in one of the  following as considered appropriate for the
deficiency: sample log, instrument log, sample preparation  log.  A copy of the checklist is kept in
the project specific files as well as in the QA Officer's notebook.

14.2   Performance Audits

Laboratory performance audits take place continually  or at least on a weekly basis.  A portion of
these audits are conducted by all people in the laboratory including the analyst, Chief Chemist, and
QA Officer. Instrument performance is checked continually by the analyst with analysis of standard
curves,  sample replicates, method blanks,  and  equipment blanks.    Many  of the analyses are
performed and checked within 24  hours to seven days of sample  collection, allowing  for any
deficiencies to be corrected and samples re-analyzed if needed. The results of these  performance
 audits conducted by
                                          14-1
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                                                                        Section 14
                                                                     Date: 4/20/99
                                                                       Page 2 of 6
Figure 14.1 Field Audit Checklist
       Auditor:
Field Audit Checklist
                Date of Audit:
Y






Y





Y






N






N





N






Water Sample Collection
* Sampling station advanced from downgradient
direction.
* A clean person is designated and dons two pair of
sloves.
* Other crew members don one pair of gloves.
* Vacuum system tubing is rinsed three times with
samole water orior to samole collection.
* Sample is properly labeled, double-bagged, and stored in
a cooler.
* Microcentrifuge tubes are stored in the dark in a cooler
with ice.
Soil/Sediment Sample Collection
* Sampling station advanced from downwind direction.
* A clean person is designated and dons two pair of
sloves.
* Sampling equipment clean prior to each sample
collected.
* Sample are homogenized in the field appropriately.
* Sample containers are labeled correctly, bagged, and
olaced in a cooler.
Porewater Sample Collection
* Volume of standing water in the lysimeter is determined
correctlv.
* Three volumes of standard water are purged.
* Field parameters are monitored during purging until
stable.
* Sampling equipment tubing and sample bottles are
rinsed three times orior to samole collection.
*Clean person dons two pairs of gloves.
* Sample containers are labeled correctly, bagged, and
olaced in a cooler.
Comments






Comments





Comments






                                      14-2
-------
Figure 14.1 Field Audit Checklist (Continued)
       Auditor:
Field Audit Checklist (cont.)
                   Date of Audit:
                                                                          Section 14
                                                                       Date: 4/20/99
                                                                         Page 3 of 6
Y



Y












Y



N



N












N



Tissue Sample Collection
* Sample station advanced from downstream direction.
*Clean person dons two pairs of gloves.
* Fish samples are labeled correctly, bagged, and placed
in a cooler.
Field Notebook
The following are recorded in the field notebook:
* Names of the field crew
*Weather conditions
* Time of sample collection
* Time of QC sample collection
* Temperature, Salinity, conductivity, pH of purge water
* Volume of water purged.
* Sample numbers and station names.
* Field equipment cleaning procedures.
* Soil/Sediment sample homogenization procedure.
* The use of fuel powered units.
* Number of QC samples collected.
General
* Samples are collected away from engine exhaust.
* Appropriate number of QC samples are collected.
* Samples are brought to the laboratory on the same day
of samole collection.
Comments



Comments












Comments



                                       14-3
-------
                               Section 14
                            Date: 4/20/99
                              Page 4 of 6
14-4
-------
                                                                       Section 14
                                                                    Date: 4/20/99
                                                                      Page 5 of 6
Figure 14.1 Laboratory Audit Checklist
                            Laboratory Audit Checklist
      Auditor:                                Date of Audit:
Y










Y




Y






N










N




N






Instrument Response
* Instrument notebook is up to date.
* High standard within 10 % of expected value.
* Calibration curve correlation coefficient better than
OQQ
-------
                                                                         Section 14
                                                                       Date: 4/20/99
                                                                         Page 6 of 6
Figure 14.2 Laboratory Audit Checklist (Continued)
       Auditor:
Laboratory Audit Checklist (cont.)
                      Date of Audit:
Y






N






Data Management
* Project Files up to date.
* Data input up to date and correct.
* Calculations performed correctly.
* Output files in correct format.
* Data values within 2 standard deviations of historical
mean.
* Data reports up to date.
Comments






                                       14-6
-------
                                                                              Section 14
                                                                           Date: 4/20/99
                                                                             Page 7 of 6
the analyst are on instrument log books and instrument printouts on a daily basis.

The Chief Chemist checks the instrument log books on a weekly basis to check that instruments are
running within their appropriate QA objectives.  The Chief Chemist may also prepare samples and
submit them blind to the analyst to check instrument and user performance.  The results of these
samples are documented in the Chief Chemist notebook.

The QA Officer will review the results of equipment blanks, matrix spike samples, blind samples,
sample replicates, and split samples from another laboratory on at least a semi-annual basis.  The
QA Officer will determine if instrument accuracy and precision values are within the project QA
objectives.   The results of the QA Officer's review will be documented  in the QA Officer's
notebook. Any discrepancies determined between instrument performance and the QA objectives'
will be included in the QA report to FDEP.

Currently, SERF  is not involved in a regular external audit program; however, we are available to
receive on-site audits by FDEP at any time.
                                         14-7
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                                                                               Section 15
                                                                           Date: 03/06/95
                                                                              Page 1 of 1
15.0   Quality Assurance Reports
SERF will submit quality assurance reports for all Quality Assurance Project Plans at a frequency
according to Table V of Appendix D  of the FDEP QA Manual. The QA Officer is responsible for
the preparation of these reports.  In general, if no audits were performed and no significant QA/QC
problems have been identified, then SERF will prepare a brief letter stating these facts in lieu of a
detailed quality assurance report.

A detailed QA report will be prepared when:

       1.      Activities were conducted in a manner other than those described by the CompQap
              or QAPP.
       2.      Preservation or holding requirements were not met.
       3.      Quality control checks were unacceptable.
       4.      Precision, accuracy, or MDL objectives were not met.
       5.      Corrective action was taken.
       6.      Internal or external audits were conducted and discrepancies were noted.

According to FDEP guidelines, these QA reports will include the following:

       1.      Title Page including the time period of the report,  the QA Project Plan Title and
              Plan number, the laboratory name, address  and phone number, and the preparer's
              name and signature.
       2.      Table of contents if the report is over 10 pages long.
       3.      The results of performance or system audits to include, date of audit, system tested,
              name of auditor,  parameters analyzed, results of tests, deficiencies or failures, and
              an explanation of the problem  and the corrective action taken.
       4.      Significant QA/QC problems.
       5.      Corrective actions taken.
                                          15-1
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                                    APPENDIX A

   Method Validation for Part per Trillion (ppt) Concentrations of Inorganic and Total
                     Mercury in Water, Solid, and Tissue Samples

                             Limited Use Method Validation

                                 Prepared by and for:

                       Southeast Environmental Research Program
                             Florida International University
                                       OE148
                                   University Park
                                 Miami, Florida 33199
                                    (305) 348-3095
                                FAX:  (305)348-4096
Ronald D. Jones, Ph.D.                                             Date
SERF Director and Professor
Nancy A. Black                                            Date
SERF Quality Assurance Officer
Sylvia S. Labie                                             Date
FDEP QA Officer
-------
                                                                             Appendix A
                                                                          Date: 04/18/96
                                                                            Page 2 of 13
1.0    Scope and Application
This method covers the  determination of parts per trillion  (ppt) levels of total and inorganic
mercury in water, soils, sediment, and tissue (fish) samples.  A method detection limit of 0.3 ppt is
obtainable for water samples at a precision of less than 5% relative standard deviation (%RSD) and
an accuracy between 90 and 110%. The concentrations of mercury in sediment and tissue samples
are significantly higher than in water samples and can be determined at better precision (<5 %RSD)
and accuracy (90 to 110 %R).  Linear calibrations up to 1 part per million (ppm) can be obtained
and higher concentrations can be measured with dilution.

2.0    Summary of Method

Total and inorganic mercury  concentrations are determined by Cold  Vapor Atomic Fluorescent
Spectrometry (CVAFS). In this method, mercury in a liquid sample is vaporized and stripped from
the remaining liquid by a carrier gas (Argon).  A sheath  gas (also Argon) constrains the mercury
vapor to a small stream  as it  passes by a light source and photomultiplier tube.  The mercury
concentration is determined by atomic fluorescence.

An PS Analytical (PSA) Merlin Plus mercury analysis system equipped with  an autosampler, vapor
generator, fluorescence detector and  a PC-based integrator package is  used to  detect total and
inorganic mercury.  The  system is run according to the manual provided  by the manufacturer,
except lower flow rates are used for the carrier and sheath gases.  Low detection levels of 0.3 ppt
Hg in water samples are obtained with flow rates of 0.14 L/min and 0.125 L/min for the carrier and
sheath gases, respectively.  For the higher concentrations of mercury detected in sediment and tissue
samples, flow rates of 0.35 L/min for the carrier gas and 0.2 L/min for the sheath gas are used. To
accurately regulate the gas flow for optimum conditions,  SERF installed an  Omega model FMA-
78P2 electronic mass flow controller in front of the PSA Merlin Plus instrument.

Water sample preparation includes digestion by a brominating procedure to breakdown all mercury
complexes.  Sediment samples and tissue samples are digested with concentrated nitric  acid  in
sealed ampoules, and subsequently autoclaved.

An NBS standard of  1000 |ig Hg/1 is used and diluted to  obtain the  appropriate linear standard
curve.  High standards of 10 ppt and 400 ppt are used for  water/tissue and  sediment samples,
respectively. NBS oyster tissue 60 ng/g (566a), NRCC dogfish muscle 4.64 jig/g (DORM-2), NIST
sediment nominal  50  jjg/g (8407), and  NIST sediment 60 ng/g (8406) are used to check the
accuracy of the tissue and sediment results.
                                           A-2
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                                                                              Appendix A
                                                                           Date: 04/18/96
                                                                             Page 3 of 13

3.0    Interferences

3.1    Matrix Interferences

There are no matrix interferences with this method.  By digesting the water samples with bromine,
all mercury complexes including organomercury compounds, sulphide complexes and complexes
with organic material  (e.g.  fulvic acids) are broken down.   Additionally,  acid digesting and
autoclaving results in a complete breakdown of mercury in the sediment and tissue samples.

3.2    Environmental Interferences

Mercury contamination at levels near the method detection limit is a consistent problem as samples
easily absorb mercury from the air and improperly cleaned glassware.  To minimize contamination,
all technicians are required to wear surgical vinyl gloves. In addition, all glassware, acids, reagents,
etc. are stored in a mercury-free clean room.  The clean room contains a bank of laminar flow hoods
equipped with gold and charcoal filters. The floor is covered with flypaper to trap particulates.
Potential contamination in the clean room is checked weekly by monitoring acidified (1% HC1)
water samples, which  are stored open inside the clean room.   If significant levels of mercury is
detected in these samples (<20 ppt), then the source of the mercury contamination is identified and
eliminated.  The  gold and charcoal  filters  within  the laminar flow hoods are reconditioned if
necessary.

Mercury-free DIW  is  produced by filtering tap water through  a Culligan system  consisting  of
activated charcoal and two mixed bed ion exchange cartridges.  This water is piped to the clean
room where is then passed through a Barnstead Mega-ohm B  Pure system.  This system is fitted
with two filters (Thermolyne: colloid/organic-D0835, and ultrapure-D0809)  in line with a 0.22
micron pleated particle filter.  Mercury levels are not detectable (<0.1 ppt) in this water by both our
laboratory and by and independent laboratory analysis. This is the only water used for all analyses.
3.3    Laboratory Glassware and Sample Bottle Cleaning

Laboratory glassware is kept to a minimum, with Teflon bottles and beakers used when possible.
All reusable glass bottles, volumetric flasks, graduated cylinders, and teflon beakers are dedicated
to the preparation and storage of a specific reagent, and are rinsed between usage with acid (0.5N
HC1 and 0.05N HNOs) and rinsed three times with DIW. One volumetric flask is kept dedicated to
making the primary standard and is rinsed only with this standard. Glassware or plastic containers
that have come in contact with samples, such as ampoules and scintillation vials are used once then
discarded.

Teflon sample bottles that have been used previously are  rinsed three times with DIW and filled
with 1% HC1. After filling, 1 ml of mixed brominating agent is added for every 50 ml, and the
bottle is shaken.  This mixture remains in the bottles until used.  Prior to their use,  500 |ol of
hydroxylamine hydrochloride is added to remove the free bromine.  The bottle and cap are then
rinsed three times with DIW.  Sediment cups and 20 ml  scintillation vials are non-reusable and
                                           A-3
-------
                                                                              Appendix A
                                                                           Date: 04/18/96
                                                                             Page 4 of 13

discarded.

4.0    Safety Precautions

Bromine vapors are toxic; therefore, prepare the brominating agent beneath a  hood.   Keep all
containers with the brominating agent securely capped when moved or stored.  Neutralize sample
bottles with hydroxylamine hydrochloride prior to their use.

Hydroxylamine hydrochloride is a skin and eye irritant and can cause dermatitis. A face shield and
gloves must be worn when handling this material.

The exhaust fumes from the atomic fluorescence spectrophotometer are toxic and must be  ducted
away. The low pressure mercury discharge lamp used for fluorescence determination emits intense
U. V. radiation.  This lamp must not be viewed directly.

5.0    Apparatus and Materials

Analytical instrumentation includes an PSA Merlin Plus mercury analysis system equipped with the
following:

       Autosampler         Vapor Generator
       Fluorescence Monitor IBM compatible computer system

In addition, an Omega model FMA-78P2 electronic mass flow controller is installed in front of the
PSA Merlin Plus instrument.  All of the above equipment is stored beneath a protective hood.  All
other standard laboratory equipment (Teflon beakers, glassware, pipettes, etc.) is kept within the
clean room  and dedicated to mercury analysis.   A mercury-dedicated refrigerator,  oven, and
analytical balance are kept within the clean room.  Polyethylene scintillation vials (20 ml) with
polypropylene caps are used with the  autosampler.  Water  samples suspected  of low mercury
concentration are injected into the instrument manually from 125 ml teflon bottles.
                                           A-4
-------
                                                                             Appendix A
                                                                         Date: 04/18/96
                                                                           Page 5 of 13

Additional equipment needed for sediment and tissue sample preparation include:

       glass bottled blender  autoclave
       syringe              oven
       plastic specimen cups balance
       10 ml ampoules

6.0    Reagents

6.1    Bromination Reagents

0.1 M Potassium Bromate
Heat 8.385 g KBrO3 overnight in a glass scintillation vial (Kimble 74511) at 250° C +/- 20° C in a
furnace to remove mercury. After cooling dissolve the potassium bromate in 500 ml of DIW and
store in a borosilicate glass bottle with a Teflon cap. Prepare Weekly.

0.2 M Potassium Bromide
Heat 11.9 g KBr overnight in a glass scintillation vial at 250° C +/- 20° C to remove mercury. After
cooling dissolve the potassium bromide in 500 ml of DIW and store in a borosilicate glass bottle
with a Teflon cap. Prepare weekly.

0.05 M Potassium Bromide (KBr) - 0.1 M Potassium Bromate (KBrCh)
Mix equal volumes (100 ml) of bromate and bromide  in a borosilicate glass (150 ml) bottle with a
Teflon cap.  Prepare daily.

6.2    Hydroxylamine Hydrochloride

Dissolve  6 g of NH2OH-HC1 in 50 ml of DIW in a 60 ml  Teflon bottle. Prepare weekly.

6.3    Stannous Chloride

Add 50 ml  of 12 N HC1 to 40 g of Stannous Chloride (SnCb). Bring to 1000 ml  with DIW in a
borosilicate glass bottle with a Teflon cap.  Stannous chloride is purged of any traces of mercury
with argon gas continuously throughout the analysis. Prepare fresh daily.

6.4    12 N Hydrochloric Acid

Concentrated HC1 (12 N HC1) is dispensed via a pipette or poured into a graduate cylinder, either of
which has been previously acid washed and rinsed three times with DIW.
                                          A-5
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                                                                              Appendix A
                                                                           Date: 04/18/96
                                                                             Page 6 of 13
6.5    16 N Nitric Acid
Concentrated Nitric acid (16 N) is dispensed through a pipette, which has been previously washed
and rinsed three times with DIW.

6.6    Standards

Due to its high concentration, primary stock standard is prepared and stored outside of the mercury-
free clean room.  The primary stock standard is made by addition of 100 |ol of SEPEX (PLHG4-2X)
(1000 |ig/ml) to 1000 ml of DIW with 10 ml of trace metal grade HC1 in a glass, volumetric flask
with a ground glass stopper.  This standard is prepared daily.  Secondary standards are prepared
daily in 500 ml Teflon bottles by adding concentrated HC1 (5 ml) to 495 ml of DIW. The primary
stock is brought into the clean room and 50 jj] - 250 |ol (depending on final concentration of
10 ppt - 50 ppt) is added to the bottles containing the water-acid mixture with a pipette.

6.7    Standard Reference Material

The following standard reference  materials are used to check the accuracy and precision of the
tissue and sediment digestion methods and analyses:

       DORM-2 Dogfish muscle (NRCC)
       556a Oyster tissue (NBS)
       8406 Sediment (MIST)
       8407 Sediment (MIST)

These standard reference materials are stored and dried according to the Certificate of Analysis
accompanying each standard. The standards are digested following the  same procedures used for
tissue and sediment samples. They are prepared and analyzed on a daily basis.

7.0    Calibration

A linear calibration curve is  run prior to each sample run.  For low level water samples, standards
include 0, 2.5, 5 and 10 ppt.  Standards run for tissue and sediment samples  include 0, 100, 250,
and 400 ppt.  All standards are run in replicate and plotted using the software inherent to the
instrument.  Linear regression analysis is used to determine the  best-fit calibration line with a
regression coefficient (r ) of 0.998 or better.  Standard curves outside the acceptable limits are run
again, and new standards are prepared if necessary.

The sensitivity of the Merlin Plus System is such that a zero mercury concentration results in a zero
result.  However, multiple dilutions of the source  standard as required to produce the low standard
of 10 ppt, often results in error, thereby  producing a  standard curve that does  not intercept the
origin. Therefore, once the standard curve is checked for linearity, a new linear calibration curve is
recalculated using the high standard and forcing the intercept through zero.  Mercury concentrations
in samples are then determined by comparing sample peak heights to the new standard curve.

                                           A-6
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                                                                            Appendix A
                                                                         Date: 04/18/96
                                                                           Page 7 of 13

8.0    Quality Control

8.1    Method Detection Limit

The method detection limit (MDL) of 0.3 ppt is determined for this method according to the EPA
procedure described in 40 CFR Part 136, Appendix B, revision 1.11, except that a value of 3 is used
in place of the Student's T value.  Specifically, seven or more replicate samples containing a known,
low concentration of mercury are analyzed.  The standard deviation of the  replicate analyses is
determined  and the MDL is computed as 3 times the standard deviation.

Table A.I
Method Detection Limit
Matrix


Spiked DIW
(DIW plus Ippt
Hg)




Sediment






Hg
Concentration
(PPt)
2.315
2.093
2.216
2.167
2.290
2.093
2.118
84.30 ppb
85.42ppb
82.44 ppb
8 1.32 ppb
84.30 ppb
82.44 ppb
82.81 ppb
Mean


2.185






83. 29 ppb






Standard
Deviation (S)

0.085






1.42 ppb






MDL = 3 x S


0.255






4.27 ppb






8.2    Precision

Precision is defined as the agreement or closeness of two or more results of the same sample, and
is determined in terms of percent relative standard deviation (% RSD) using the following
equation:

                    %RSD=_s_* 100,
                             X

where, s and X represent the standard deviation and mean, respectively, of two or more results of

                                          A-7
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                                                                            Appendix A
                                                                         Date: 04/18/96
                                                                          Page 8 of 13
the same sample. The analytical precision of this method is variable with more precise
measurements obtained at higher mercury concentrations.

Table A.2
Precision
Matrix
Water
Water
Water
Soil/Sediment Slurry
Tissue Slurry
Hg Concentration
0.3 - 30 ppt
5 - 500 ppt
1-1000 ppt
1 ppt - 400 ppt
1 ppt - 400 ppt
Precision
%RSD
<5%
<5%
<5%
<5%
<5%
8.3    Accuracy

Accuracy is defined as the agreement between the analytical results and the known concentration.
 Accuracy is determined by running continuing calibration standards or by check standards and is
determined as percent recovery (%R) according to the following equation:

                    % R = Observed Standard Concentration * 100.
                            Known Standard Concentration

Instrument accuracy is determined on a daily basis by performing multiple analysis (5 or more
replicates) of the high standard.  Percent recoveries between 90 and 110% are obtained for water
samples with a high standard of 10 ppt. For solid and tissue samples with a high standard of 400
ppt, percent recoveries between 95 and 105% are obtained.
                                          A-8
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                                                                           Appendix A
                                                                        Date: 04/18/96
                                                                          Page 9 of 13
Table A.3
Accuracy
Matrix
Water
Water
Water
Soil/Sediment Slurry
Tissue Slurry
Hg Concentration
0.3 - 30 ppt
5 - 500 ppt
1 - 1000 ppt
5 - 400 ppt
5 - 400 ppt
Accuracy (% Recovery)
90-110
90-110
90-110
90-110
90-110
8.4    QC Checks

Calibration check samples are run in duplicate following at the beginning and after every 10
samples.  For solid and tissue samples, NIST or NBS standards are run after every 20 samples.
Accuracy for each of these calibration check samples and standards must be within 90 to 110%
or the samples must be run again.

9.0    Sample Collection, Preservation, and Handling

9.1    Water Samples

Water samples are collected in Teflon bottles.  Collection is done while wearing shoulder length
polyethylene gloves over a pair of vinyl gloves. Surface water samples are collected through a
105 |im nylon screen via a vacuum system to reduce the amount of sediment collected. Samples
are double bagged in zip-lock polyethylene bags and placed in a plastic ice chest/cooler used
exclusively for low level mercury  samples.  Samples are returned to the laboratory upon the same
day of sample collection and preserved in the mercury-free clean room with 0.5 ml of trace metal
grade HC1 per 100 ml of sample.  Sample analysis within 28 days is recommended.

9.2    Sediment Samples

Sediment samples are collected in polyethylene specimen cups (Elkay non-sterile wide mouth
specimen cups with screw caps - 128  ml volume) and placed in polyethylene zip-lock bags.  All
field samples are kept in a cooler used exclusively for low level mercury samples until they are
returned to the laboratory, where they are stored in a freezer. Samples can be stored indefinitely
within the freezer; however, analysis within 28 days is recommended.
9.3    Tissue Samples
                                         A-9
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                                                                             Appendix A
                                                                          Date: 04/18/96
                                                                          Page 10 of 13
Fish are collected with a dip net and stored in plastic bags for transport to the laboratory. In the
laboratory fish are stored within the freezer indefinitely; however, analysis within 28 days is
recommended.

10.0   Sample Extraction/Preparation

10.1   Water Samples

Water samples analyzed for inorganic mercury do not require additional sample preparation prior
to analysis. For analysis of total mercury, the samples are placed in an ultraviolet cabinet for 12
hours, allowed to cool, then 2.5 ml of KBrOs/KBr solution is added to 125 ml of each water
sample. The sample is left to brominate for one hour in the Hg-free room; after which 500 |il of
hydroxylamine hydrochloride is added to the solution to inhibit further reaction. Samples are
permitted to settle for at least 10 minutes before analysis.

10.2   Soils and Sediment Samples

Preparation of soil/sediment samples is done outside the mercury-free room, due to their high
mercury concentrations. Soil/sediment samples are homogenized and slurried in a glass bottle
blender.  A mixture of 120 cc of soil/sediment and 50 ml of DIW is blended for three minutes.
With a syringe, 10 ml of the slurry is collected for dry weight determination. Another  10 ml is
pipeted into a polyethylene specimen cup and diluted to 50 ml with DIW containing 5% HC1 to
neutralize any carbonate contained in the sediments. The slurry is mixed well, then 1 ml of the
slurry is transferred to a 10 ml ampoule with 2 ml of concentrated nitric acid (total volume in the
ampoule is 3 ml) and left to sit for 20 minutes. The ampoule is sealed and autoclaved for 1 hour
at 105 C.  The ampoules are allowed to cool completely to room temperature, and then 0.5 ml of
the  ampoule solution is put into a 20 ml polyethylene scintillation vial containing 19.5  ml of
DIW and 1% HC1 for a dilution of 1:40.

The 10 ml of slurry collected for dry weight is weighed, dried in an oven overnight at 80°C, and
weighed again.  Duplicate or triplicate samples are dried and weighed until a constant weight is
obtained.  This constant weight is then divided by 10 to obtain the dry weight of sediment within
the  original 1  ml extracted for analysis.

10.3   Tissue Samples

Fish samples are prepared similar to soil/sediment samples, except that the initial addition of HC1
to neutralize carbonates is not performed.  For small fish (Gambusia sp.), the entire fish is
weighed, placed in ampoules and digested. For large fish (bass and catfish), a stainless steel core
tube, 4 mm in diameter, is used to collect three tissue plugs from the left fillet of each fish. Care
is taken to collect muscle tissue and not scales or bones. The three plugs are combined in a 10
ml ampoule, weighed, and digested according to the procedures described  above in Section 10.2.
 The weight of the tissue sample that is digested and used for analysis is usually between 0.3 g
and 0.4 g.
                                          A-10
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                                                                            Appendix A
                                                                         Date: 04/18/96
                                                                         Page 11 of 13
11.0   Sample Cleanup and Separation

Additional sample cleanup and separation are not necessary to separate the mercury from the
sample matrix. The bromination process used for the water samples results in a complete
conversion of all organic forms of mercury to mercury (II).  In addition, the acidification
followed by autoclaving the sediment and tissue samples results in a complete digestion of the
sample.

12.0   Sample Analysis

The PSA Merlin Plus Fluorescence detector is operated according to the manufacturer
specifications with the following modifications:

•      An Omega model FMA-7882 mass flow controller with a channel selector is
       installed at the front of the instrument.  This flow controller is used to more
       accurately regulate the flow rates of the carrier and sheath gases (both argon)
       while the flow controllers supplied with the instrument on the hydride generator
       are open to full capacity.  For low level mercury in water samples, the optimum
       flow rates of the carrier and sheath gases are 140 cc/min and 125 cc/min,
       respectively. For high level mercury, such as in sediment and tissue samples,
       optimum flow rates of the carrier and sheath gases are 350 cc/min and 200 cc/min,
       respectively.

•      When analyzing water samples from 125 ml teflon bottles, the auto sampler is
       removed and the switch box is modified to sip only from the right sampling tube.

The procedure for sample analysis includes:

1.      Tighten the peristaltic pump (pumps wash water, waste water, sample and
       stannous chloride).
2.      Turn on the wash water to the system
3.      Turn on the computer
4.      Turn on the gas to the system. The argon (Zero grade) flows through two gas
       purifiers (charcoal and gold) and a moisture trap before reaching the instrument.
5.      Turn on the line stabilizer/conditioner.
6.      Check to make sure no tubes are crimped, and that flow is smooth in all tubes
       before proceeding.
7.      Check gas flow at the mass flow controller.
       Note: For low level Hg-concentrations the optimum level of the carrier gas has
       been determined to be 140 cc/min while the sheath gas level has been optimized at
       125 cc/min. At higher Hg-concentrations the carrier gas is 350 cc/min, and the
       sheath gas is 200 cc/min. The membrane dryer gas flow rate is 1 L/min.
8.      Allow the system to run on DIW for 15 minutes.
                                         A-11
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                                                                            Appendix A
                                                                         Date: 04/18/96
                                                                          Page 12 of 13
9.      After 15 minutes switch the instrument to SnCb.
10.    Note: the sensitivity dial on the instrument is run at highest sensitivity for water
       but may be lowered for running of sediment, soil and tissue samples. This method
       is adequate for samples of the range we have run to date.
11.    When the instrument is ready, zero the fluorescence detector and run acidified
       water (0 ppt) to check baseline response of the instrument and guard against
       unexplained contamination from reagent preparation. When peak height of D.I. is
       0.0-0.3 the standards may be run. Initially one high standard is run to test for
       consistency of standard preparation and machine function.  The range of standards
       will reflect the concentration of samples to analyze. Eight  standards (four
       concentrations, two replicates) are run for each standard curve. Standards run for
       low level samples are 2.5, 5, and 10 ppt.  Standards, blanks, and high level
       samples (generally fish, sediments and soil)  may be run in  plastic scintillation
       vials. Water samples for total-Hg are digested and analyzed in 125 ml teflon
       bottles. Digested acidified DIW water samples are analyzed along with the
       samples as reagent blanks. This number is subtracted from sample  values.
12.    After running the standards, two samples of the 0 ppt (acidified water) are
       analyzed before running the samples. Each  125 ml water sample is analyzed at
       least three times. Tissue and sediment samples are run in replicate. One run of
       fifty samples plus standards takes approximately 2 hours and uses approximately
       10 ml of SnCb per sample.  A new standard curve is run when the  SnCb is
       replaced. In addition to running a full set of standards at the beginning of the
       analysis for each bottle of stannous chloride, a replicate of the highest standard
       and zero ppt are run after every 10 samples.

       Note: When sampling  from 125 ml teflon bottles, the auto sampler tray is
       removed and the connections are modified to sample only from the right sampling
       tube. This is done by disconnecting the right (internal) sampling tube as well as
       the corresponding tube to the hydride generator and replaced with a longer teflon
       tube that directly connects the sampling tube to the hydride generator.

Instrument Shutdown:

1.      If you are using the results directly from the  company supplied computer program,
       make sure you have printed and/or saved results. This program does not reliably
       transfer files to ASCII  or Excel although it has functions for these tasks.
2.      Replace the SnCb solution  with DIW and flush the instrument for  5 minutes.
3.      Turn off the wash water and disconnect tubing from DIW bottle.
4.      Run the pump until no more liquid is present in the pump tubing.
5.      Turn off the gas.
6.      Turn off the line stabilizer and the computer.
7.      Release tubing in the Hydride generator and peristaltic pump.
8.      Check the waste water container and empty  if necessary.
                                         A-12
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                                                                             Appendix A
                                                                         Date: 04/18/96
                                                                          Page 13 of 13
13.0   Calculations
The calculations program supplied with the AFS does not have an adequate curve fitting function
for low level mercury concentrations. Therefore, the instrument data is transferred as an ASCII
file into an Excel spreadsheet. Sample concentration is determined using the linear calibration
curve equation:

       Y = M*X + B,

where Y is the sample concentration, M is the slope of the best-fit line through the calibration
points, X is the sample peak height, and b is the intercept of the line with the Y axis. Sample
concentration is further corrected for background noise or drift, if any, by subtraction. In
addition, if the sample was diluted prior to analysis, the sample concentration is multiplied by the
dilution factor. An additional correction for dry and wet  sample weight is performed for
soil/sediment and tissue samples, respectively.

The concentration of mercury per gram of soil/sediment or of tissue (Cng) is obtained from the
following  equation:

       CHg = (SC * D.F. * 0.003)/(W)

where SC  is the sample concentration in ng/1 (ppt), D.F. represents the final dilution factor, 0.003
represents the volume  of sample in each ampoule in liters, W is either the dry weight of
soil/sediment in 1 ml of solution extracted for analysis, or the wet weight of the fish digested in
the ampoule (whole fish or plug samples).

14.0   Confirmation

As yet, no other analytical method has been developed to measure sub-part per trillion
concentrations of mercury. Confirmation can only be obtained by analysis of duplicate samples
by other laboratories with similar capabilities. Laboratories currently used by SERF for
confirmation include the EPA laboratory in Athens, GA and Batelle Marine Sciences Laboratory
in Sequim, WA.

15.0   Method Performance

This method measures inorganic and total mercury in water samples at concentrations between
0.3 ppt and 1000 ppt with a precision of better than 5% RSD and an accuracy between 90 and
110%. Mercury concentrations between 5 and 500 ppt in sediment and tissue samples are easily
measured, with higher concentrations determined following dilution. Accuracy and precision of
the higher mercury concentrations in the sediment and tissue samples can be obtained at
precision and accuracy levels of better than 5% RSD and between 90 and 110%, respectively.
                                          A-13
-------
     APPENDIX B
Related Scientific Articles
-------
 Contents

 Jones, Jacobson, Jaffe, West-Thomas, Arfstrom, and Alii.  1995.  Method Development and
 Sample Processing of Water, Soil, and Tissue for the Analysis of Total and Organic Mercury
 by Cold Vapor Atomic Fluorescence Spectrometry. Water, Air and Soil Pollution.  80:  1285-
 1294.

 Alii, Jaffe, and Jones. 1994. Analysis of organomercury compounds in sediments by capillary
 GC  with atomic fluorescence detection. Journal of High Resolution Chromatography. Vol
 17, pp. 745-748.

Lee and Mowrer. 1988. Determination of methylmercury in natural waters at the sub-nanograms
 per liter level by capillary gas chromatography after adsorbent preconcentration.

 Cai, Jaffe, Alii, and Jones. 1996. Determination of organomercury compounds in aqueous
 samples by capillary gas chromatography-atomic fluorescence spectrometry following  solid-
 phase extraction. Analytica ChimicaActa 334 (1996) 251-259.

Evaluation of some isolation methods for organomercury determination in soil and fish samples
 by capillary gas chromatography-atomic fluorescence spectrometry. Intern. J. Environ. Anal.
 Chem. Vol. 68 (3), pp. 331-345.
-------
                APPENDIX C




SERP Mercury Lab Standard Operating Procedures
-------
SERF Mercury Lab Standard Operating Procedures (SOP)
SOP
Number
001-99
002-99
003-99
004-99
005-99
006-99
SOP Title
Determination of Total Mercury in Water Samples
Determination of Total Mercury in Soils and Sediments
Determination of Total Mercury in Fish Samples
Determination of Organic Mercury in Water Samples
Determination of Organic Mercury in Soil/Sediment Samples
Determination of Organic Mercury in Fish Tissue Samples
Issue Date
04/15/99
04/15/99
04/15/99
04/15/99
04/15/99
04/15/99
-------
                             APPENDIX D
Examples of Instrument Printouts for Total and Organic Mercury Determinations
-------
                                                                       Appendix E
                                                                    Date:  11/21/97
                                                                      Page 1  of 16
                                   APPENDIX E
   Method Validation for Organomercury Compounds in Water, Sediment, and Tissue
                                     Samples

                            Limited Use Method Validation

                                 Prepared by and for:

                       Southeast Environmental Research Program
                            Florida International University
                                      OE148
                                  University Park
                                Miami, Florida 33199
                                  (305) 348-3095
                                FAX: (305)348-4096
Ronald D. Jones, Ph.D.                                      Date
SERF Director and Professor
Doraida Diaz                                            Date
SERF Quality Assurance Officer
Sylvia S. Labie                                      Date
FDEP QA Officer
                                       E-l
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                                                                            Appendix E
                                                                        Date:  11/21/97
                                                                           Page 2 of 16
1.0    Scope and Application
This method covers the determination of parts per trillion (ppt) levels of organomercury compounds
in water, soils, sediment,  and tissue (fish) samples.   Organomercury compounds that  can  be
detected by the methods described herein include methylmercury (MeHg) and ethylmercury (EtHg).
Method detection limits (MDL) of 0.02 ng/L (ppt) and 0.02 ng/g (ppb) are obtainable for both
methyl- and ethylmercury in water and sediment/tissue samples, respectively.

2.0    Summary of Method

Organomercury concentrations are determined by capillary gas chromatography  coupled with
atomic fluorescence spectrometry (GC-AFS) as described by Alii et al. (1994). Initial extracts of
sediment and tissue samples are subjected to sodium thiosulfate clean-up and the organomercury
species are  isolated  as  their  bromide derivatives by  acidic KBr and CuSQt  and subsequent
extraction into  a small  volume  of dichloromehtane.   For water samples, the organomercury
compounds are pre-concentrated using a sulfhydryl cotton fiber adsorbent, followed by elution with
acidic KBr and CuSO4 and extraction in dichloromethane.

Chromatography is performed with a Hewlett-Packard (Model 5890 Series n) gas chromatograph
coupled with an FIP (Model 7673) automatic sampler.  A Merlin Mercury Fluorescence Detector
System, Model 10.023, (P.S. Analytical) is used.

All mercury standards are purchased from Ultra Scientific. Stock standard solutions of methyl- and
ethylmercury chloride are prepared by dissolving appropriate amounts of the standards in  optima
grade methanol (Fisher Scientific). These solutions are stored in dark brown bottles at <20°C and
diluted with dichloromethane.

3.0    Interferences

3.1    Matrix Interferences

For analysis of organic mercury in water samples, pH, chloride ion concentration and salinity must
be within the domain of 2-5, <0.37 M and <20 °/o, respectively.   The normally occurring
concentrations of ions such  as sulfate,  calcium, and  magnesium, as well as the presence  of
dissolved organic carbon have no effect on the analysis.
Low levels of recovery  are obtained  for fish tissue (70%-80%) and soil  and  sediment samples
(70%-85%). The exact cause for the low recovery of organic mercury is unknown yet assumed to
be related to the sample matrix. Due to the low levels of recovery for these matrices, matrix spike
recoveries must be determined on every sediment and tissue sample.

3.2    Environmental Interference's

                                          E-2
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                                                                              Appendix E
                                                                          Date:  11/21/97
                                                                             Page 3 of 16
Mercury contamination at levels near the method detection limit is a consistent problem as samples
easily absorb mercury from the air and improperly cleaned glassware. To minimize contamination
all technicians are required to wear surgical vinyl gloves. In addition, all glassware, acids, reagents,
etc. are stored in a mercury-free clean room. The clean room contains a bank of laminar flow hoods
equipped with gold and charcoal filters.  The floor is covered with flypaper to trap paniculate.

Mercury-free DIW is produced by  filtering tap  water through  a Culligan system consisting of
activated charcoal and two mixed bed ion exchange cartridges.  This water is piped to the clean
room where it is then passed through a Barnstead Mega-ohm B Pure system. This system is fitted
with two filters (Thermolyne:  colloid/organic-D0835,  and ultrapure-D0809)  in line with  a  0.22
micron pleated particle filter. Organic mercury levels are not detectable (<0.02 ppt) in this water.
This is the only water used for all analyses.

3.3    Laboratory Glassware and  Sample Bottle Cleaning

Laboratory glassware is kept to a minimum, with Teflon bottles and beakers used when possible.
All reusable glass bottles, volumetric flasks, graduated cylinders, and teflon beakers are dedicated
to the preparation and storage of a specific reagent, and are rinsed between usage with acid (0.5N
HC1 and 0.05N HNOs) and rinsed three times with DIW.  Glassware or plastic containers that have
come in contact with  samples, such as ampules and scintillation vials are used once then discarded.

Teflon sample bottles that have been used previously for the collection of water samples are rinsed
three times with DIW and filled with 1% HC1. After filling, 1 ml of mixed brominating agent is
added for every 50 ml, and the bottle is shaken.  This mixture remains in the bottles until used.
Prior to their use, 500 jjj of hydroxylamine hydrochloride is added to remove the free bromine.  The
bottle and cap are then rinsed three times with DIW.  Sediment cups and 20 ml scintillation vials
are non-reusable and  discarded.
                                           E-3
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                                                                             Appendix E
                                                                         Date:  11/21/97
                                                                            Page 4 of 16
4.0    Safety Precautions
Bromine vapors are toxic; therefore, prepare the brominating agent beneath a hood.  Keep  all
containers with the brominating agent securely capped when moved or stored. Neutralize sample
bottles with hydroxylamine hydrochloride prior to their use.

Dichloromethane is a  skin, eye, and respiratory irritant. A face shield  and gloves must be worn
when handling this material. This material should only be handled under  a fume hood.

The exhaust fumes from the atomic fluorescence spectrophotometer are toxic and must be ducted
away. The low pressure mercury discharge lamp used for fluorescence determination emits intense
U. V. radiation.  This lamp must not be viewed directly.

5.0    Apparatus and Materials

A schematic diagram  of the  GC-AFS  system used in this work  is  shown  in Figure I and the
optimum operating conditions are summarized in Table I. A Hewlett-Packard (Model  5890 Series
n) gas chromatograph  coupled with an HP (Model 7673) automatic sampler is used. A fused-silica,
bonded  phase megabore column (15 m x 0.53 mm i.d., 1 |am non-polar  DB-1 coating, J &  W
Scientific) and the splitless injection mode is employed. The effluent from the column is led
through a pyrolyzer (P.S. Analytical Ltd., UK), positioned inside the GC  oven via a piece of 65 cm
length of deactivated  fused-silica (0.53 mm  i.d., J &  W  Scientific), which is connected to the
column with a glass "press fit" union (J & W Scientific). The Hg atoms formed in the pyrolysis unit
are transferred from the outlet end of the deactivated fused-silica tubing to the fluorescence detector
(teflon transfer line, 0.5 mm i.d., Alltech Associates). The transfer  line  is passed through a small
hole on the top of the GC oven to a Merlin Mercury Fluorescence Detector, and the connections are
made via teflon unions.

A real time chromatographic  control and data acquisition system  (E-Lab, Version 4.1 OR, OMS
TECH, INC.) is interfaced with the GC and AFS detector system.   Additional equipment needed
for sediment and tissue sample preparation include:

       glass bottled blender  oven
       syringe              balance
       plastic specimen cups
       10 ml ampules
       autoclave
                                          E-4
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                                                                            Appendix E
                                                                        Date:  11/21/97
                                                                           Page 5 of 16
Figure I.  Gas Chromatographic-Atomic Fluorescence  Spectrometric System.  1A: Helium, IB:
Argon, 2:  Oxygen trap, 3: Mercury trap, 4: Moisture trap, 5: Automatic sampler, 6: Injector,  7:
Column, 8: Press-fit union, 9: Pyrolyzer, 10:  Deactivated fused-silica 0.53mm i.d.,  11:  Teflon
unions,  12:  Teflon  transfer line  0.5mm i.d., 13:  Atomic  Fluorescence  detector,  14:  E-Lab
chromatographic control and data acquisition system,  15: Mass flow controller-Channel A make-
up, Channel B sheath gas.
                                          E-5
-------
                                                                         Appendix E
                                                                     Date: 11/21/97
                                                                        Page 6 of 16
Table I. Optimized operating conditions of GC-AFS.	
Gas chromatograph.
Injector temperature         250°C
Temperature program        1 min at 40 C, 60 C/min to 140 C,
                          3 min at 140°C, 50°C/min to 200°C,
                          10minat200°C.
Pyrolyzer temperature               800°C
Column flow               4.0 ml/min
Make-up flow              60 ml/min

Atomic fluorescence system
Sheath gas flow             300 ml/min
Integrate time               0.25s
Calibration range           1000 (most sensitive)
Fine gain                  10 (maximum)
Recorder output voltage             IV
Damping switch                   On
(for signal smoothing)
                                        E-6
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                                                                             Appendix E
                                                                         Date:  11/21/97
                                                                            Page/ of 16

6.0    Reagents

6.1    Bromination Reagents

0.1 M Potassium Bromate
Heat 8.385 g KBrCb overnight in a glass scintillation vial (Kimble 74511) at 250° C +/- 20° C in a
furnace to remove mercury. After cooling dissolve the potassium bromate in 500 ml of DIW and
store in a borosilicate glass bottle with a Teflon cap. Prepare Weekly.

0.2 M Potassium Bromide
Heat 11.9 g KBr overnight in a glass scintillation vial at 250° C +/- 20° C to remove mercury. After
cooling dissolve the potassium bromide in 500 ml of DIW and store in a borosilicate glass bottle
with a Teflon cap. Prepare weekly.

0.05 M Potassium Bromide (KBr) - 0.1 M Potassium Bromate (KBrCh)
Mix equal volumes (100 ml) of bromate and bromide in a borosilicate glass (150 ml) bottle with a
Teflon cap. Prepare daily.

6.2    Acidic Potassium Bromide

Dissolve 180 g of potassium bromide in 200 mL of DIW.  Add 50 ml of trace metal grade sulfuric
acid to 100 ml of DIW. Combine the two solutions in a 1  liter flask.  After the solution has cooled
to  room temperature bring the flask up to 1 L with DIW.  Store the solution in the mercury-free
room in a 1 liter glass bottle with a Teflon lined cap. Prepare as needed.

6.3    1.0 M Copper Sulfate, 0.5 M Copper Chloride, 0.01 M Sodium Thiosulfate

Dissolve the appropriate amounts of each  of these salts in DIW.  Store in separate glass 0.5 L
bottles with Teflon line caps in the mercury-free  room.   Prepare  as needed.  All solutions  are
extracted with dichloromethane prior to use.

6.4    Dichloromethane

Dichloromethane is stored in its original glass container and dispensed through a pipette.
                                          E-7
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                                                                              Appendix E
                                                                          Date:  11/21/97
                                                                             Page 8 of 16
6.4    Standards
All Hg standards are purchased from Ultra  Scientific.  Stock standard solutions of methyl- and
ethylmercury chloride are prepared by dissolving appropriate amounts of the standards in optima
grade methanol (Fisher Scientific).  These solutions are stored in dark brown bottles, under a hood
outside the mercury-free room at <20°C.

A secondary standard is prepared on a weekly basis by diluting the primary standard by 100 in
methanol. Working standards are prepared on a daily basis by diluting the appropriate amount of
the secondary standard in a solution of 0.8 |oL DI water and 0.3  ml acidic KBr/CuSO4 (3:1), then
extracting with  100 |oL dichloromethane. A five point standard curve is produced within the linear
range of 0 to 6.67 pg Hg/|oL for water samples and of 0.0 to 6.0 pg Hg/|oL for solid samples. (Note,
that every standard and sample is injected into the GC-AFS in 5 |oL volumes.)

6.5    Gases

All gases are supplied by Liquid Carbonic  Specialty Gases and are of zero grade quality.  Helium
(99.995%) is used  as the carrier gas (GC),  passed first through an oxygen trap, then through a Hg
trap (gold-activated carbon) and a moisture trap prior to the GC.  Argon (99.998%) is employed as
the make-up gas and the sheath gas for the GC-AFS system and is also passed through moisture and
Hg traps before use.  Its flow is regulated  by a mass flow controller (Omega) equipped with two
channels, channel A (make-up flow) and channel B (sheath gas flow, see Figure I).

6.5    Synthesis of Sulfydryl-cotton (SHC) fiber adsorbent.

This synthesis follows the procedure used by Lee and Mowrer (1989). A mixture is first prepared
by adding the following reagents in sequence to round bottom flask: 100 ml thioglycolic acid, 60 ml
acetic anhydride, 40 ml acetic acid (36%)  and 0.30 ml concentrated sulfuric acid. The mixture is
allowed to cool to 45°C, then 30 g of cotton wool are added and  allowed to soak thoroughly in the
mixture. The reaction bottle is placed in an oven for 3 to 4 days at 40°C, then the product is placed
in a filter-funnel with  suction filtration and  washed  thoroughly with deionized water to remove
traces of thioglycolic acid. The  SHC fiber obtained is dried at 40°C for 24 h and stored at room
temperature  (20°C).

7.0    Calibration

A linear calibration curve is run prior to  each  sample  run (See section 6.4).  Linear regression
                                                                                o
analysis is used to determine the best-fit calibration line with a regression coefficient (R ) of 0.995
or better.  Standard  curves  outside the  acceptable limits  are run again,  and new  standards are
prepared if necessary.

8.0    Quality Control

                                           E-8
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                                                                            Appendix E
                                                                        Date:  11/21/97
                                                                           Page 9 of 16
8.1    Method Detection Limit
The method detection limit (MDL) is determined for this method according to the EPA procedure
described in 40 CFRPart 136, Appendix B, revision 1.11, except that a value of 3 is used in place
of the Student's T value.   Specifically,  seven or more reagent  blanks  are analyzed and  the
instrument  baseline noise is determined.  The standard  deviation of the replicate analyses is
determined and the MDL is computed as 3 times the standard deviation.
Table A.I
Method Detection Limit
Matrix


Water









Sediment
/
Tissue






MeHg Cone. EtHg
Cone.

0.0092 ng/L 0.0090 ng/L
0.0092 ng/L 0.0090 ng/L
0.0135 ng/L 0.0132 ng/L
0.0221 ng/L 0.0216 ng/L
0.0221 ng/L 0.0216 ng/L
0.0105 ng/L 0.0102 ng/L
0.01 17 ng/L 0.01 14 ng/L
0.0141 ng/L 0.0138 ng/L
0.0234 ng/L 0.0228 ng/L
0.0092 ng/L 0.0090 ng/L
0.028 ng/g 0.005 ng/g
0.005 ng/g 0.010 ng/g
0.011 ng/g 0.008 ng/g
0.003 ng/g 0.014 ng/g
0.015 ng/g 0.005 ng/g
0.014 ng/g 0.020 ng/g
0.014 ng/g 0.015 ng/g
0.010 ng/g 0.004 ng/g
0.014 ng/g 0.010 ng/g
Mean


MeHg
0.0145 ng/L


EtHg
0.0142 ng/L




MeHg
0.013 ng/g


EtHg
0.010 ng/g



Standard
Deviation
(S)
MeHg
0.0055 ng/L


EtHg
0.0057 ng/L




MeHg
0.007 ng/g


EtHg
0.005 ng/g



MDL = 3 x
S

MeHg
0.017 ng/L


EtHg
0.017 ng/L




MeHg
0.021 ng/g


EtHg
0.015 ng/g



                                          E-9
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                                                                           Appendix E
                                                                       Date:  11/21/97
                                                                         Page 10 of 16
8.2    Precision

Precision is defined as the agreement or closeness of two or more results of the same sample, and
is determined in terms of percent relative standard deviation (% RSD) using the following
equation:

                    %RSD=_s_* 100,
                             X

where, s and X represent the standard deviation and mean, respectively, of two or more results of
the same sample. The analytical precision of this method is variable with more precise
measurements obtained at higher mercury concentrations.
Table A.2
Precision
Matrix
Water
Sediment/Tissue
MeHg and EtHg
Precision
%RSD
<10
<10
8.3    Accuracy

Accuracy is defined as the agreement between the analytical results and the known concentration.
 Accuracy is determined by running continuing calibration standards, check standards, and matrix
spike samples and is determined as percent recovery (%R) according to the following equation:

                    % R = Observed Standard Concentration * 100.
                            Known Standard Concentration

Instrument accuracy is determined on a daily basis by performing matrix spike samples.  Percent
recoveries between 95  -  105%  and between 80  -  120%  for  methyl-  and ethylmercury,
respectively, in water. For solid and tissue samples recoveries of 70 - 85% and 70 - 80% are
obtained, respectively. Due to these low recoveries, matrix spike samples must be done on every
tissue and sediment sample in order to compensate for matrix effects.
                                        E-10
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                                                                            Appendix E
                                                                        Date:  11/21/97
                                                                         Page 11 of 16
Table A.3
Accuracy
Matrix
Water
Soil/Sediment
Tissue
Accuracy (%
MeHg
95 - 105
70-85
70-80
Recovery)
EtHg
80 - 120
70-85
70-80
8.4    QC Checks

Calibration check samples are run in duplicate following the standard curve at the beginning and
after every 10 samples.  Three replicate samples are prepared for each solid and tissue sample.
Two of the replicates are run as replicate samples, while one of the samples is spiked to serve as
a matrix spike. The percent recovery is determined for all solid and tissue samples, and this
recover factor is applied to each sample. A standard reference material for methylmercury in
tissue is available from the Canadian National Research Council (DORM-2 Dogfish muscle and
liver).  Standard reference material for ethylmercury  is not yet available.

9.0    Sample Collection, Preservation, and Handling

9.1    Water Samples

Water samples are collected in Teflon bottles. Collection is done while wearing shoulder length
polyethylene gloves over a pair of vinyl gloves.  Surface water samples are collected through a
105 |im nylon screen via a vacuum system to reduce  the amount of sediment collected.  Samples
are double bagged in  zip-lock polyethylene bags and placed in a plastic ice chest/cooler used
exclusively for mercury samples.  Samples are returned to the laboratory upon the same day of
sample collection, acidified with HC1 to a pH<2, then stored in the mercury-free clean room and
                                         E-ll
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                                                                            Appendix E
                                                                        Date:  11/21/97
                                                                          Page 12 of 16

analyzed within 28 days. Immediately prior to processing for analysis the sample pH is increased
to above 3 with NaOH.
9.2    Sediment Samples

Sediment samples  are collected in polyethylene specimen cups (Elkay non-sterile wide mouth
specimen cups with screw caps - 128 ml volume) and placed in polyethylene zip-lock bags.  All
field samples are kept in a cooler used exclusively for low level mercury samples until they are
returned to the laboratory, where they are stored in a freezer.  Samples can be stored indefinitely
within the freezer; however, analysis within 28 days is recommended.

9.3    Tissue Samples

Fish are collected with a dip net and stored in plastic bags for transport to the laboratory. In the
laboratory fish are stored within the freezer indefinitely and analyzed within 28 days.

10.0   Sample Extraction/Preparation

10.1   Water Samples

The determination  of organic mercury in water samples involves an adsorbent pre-concentration
of the organomercurials onto sulfydryl-cotton fibers.  The sulfydryl-cotton (SFC) fiber columns
are made of a 5 ml  screening column (Fisher Scientific) containing 0.16 g of SFC fiber, packed 1
cm high.  The water sample is passed through the column by vacuum.  Five-mi of an acidic
potassium bromide and 1.0 M copper sulfate mixture (2:1) are then pipetted on the surface of the
adsorbent and the  eluate is collected in  a 6 ml  glass vial.  This is extracted with 0.25 ml
dichloromethane on a shaker and centrifuged as described above.  The dichloromethane layer is
then transferred to a 2 ml glass sampling vial and subjected to GC analysis.

10.2   Soils, Sediment and Tissue Samples

Preparation of soil/sediment samples is done outside the mercury-free room, due to  their  high
mercury concentrations.  Soil/sediment samples are homogenized and slurred  in  a glass bottle
blender.  A mixture of 120 cc of soil/sediment and 50 ml of DIW is blended for three minutes.
With a syringe, 10 ml of the slurry is collected for dry weight determination.

The extraction procedure for soil/sediment and tissue samples consists of three steps.   Step 1. A
1.0-5.0 g portion of the homogenized sample is placed in a 20 ml  borosilicate glass scintillation
vial (Kimble, #74511). To the vial 5 ml distilled water, 3.0 ml of 1.0 M copper sulfate and 3.0
ml  of acidic potassium bromide solution are added.  The mixture  is shaken  for 1 hr at 330 rpm
(Gyrotory Shaker Model G2). Dichloromethane (5 ml) is added and the mixture is shaken for 24

                                         E-12
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                                                                             Appendix E
                                                                         Date: 11/21/97
                                                                          Page 13 of 16

h at 330 rpm and then centrifuged for 10 min at 5000 g in a Sorvall Model RC-5 refrigerated
centrifuge (Dupont). Step 2. An exactly known volume of the dichloromethane layer (3.0-4.0
ml) is transferred to a 7.0 ml borosilicate glass scintillation vial (Kimble, #0333726) and 1.0 ml
of 0.01 M sodium  thiosulfate is  added.  The mixture is  shaken for 20 min at 330 rpm and
centrifuged at high speed in a IEC clinical centrifuge. Step 3. The aqueous layer (0.8 - 0.9 ml) is
placed in a 1.5 ml microcentrifuge tube (Fisherbrand, Fisher Scientific), and 0.3 ml of acidic KBr
and CuSO4 mixture (3:1) and 0.1 ml dichloromethane  are added. The contents are mixed for 1
min on a Vortex Genie mixer and centrifuged for 2 min at high  speed (16,749 x g) in a Hermle
centrifuge. The dichloromethane is transferred to a 2.0 ml glass sampling vial containing a few
crystals of anhydrous sodium sulphate and subjected  to GC analysis. Injections of 5.0 |oL  are
used.  Samples  spiked  with known concentrations of methyl-  and ethylmercury chloride  are
extracted to evaluate the recovery factor used for quantification.

The 10 ml of slurry collected for dry weight is weighed, dried in an oven overnight at 80°C, and
weighed again.  Duplicate or triplicate samples are dried and weighed until a constant weight is
obtained.  This constant weight is then divided by 10 to obtain the dry weight of sediment within
the original 1 ml extracted for analysis.

10.3   Tissue Samples

Fish samples are prepared similar to soil/sediment samples. For small  fish (Gambusia sp.)  the
entire fish is weighted and placed in the 20 ml borosilicate glass  scintillation vial.  For large fish
(bass and catfish), a stainless steel core tube, 4 mm in diameter, is used to collect three tissue
plugs from the left fillet of each fish.  The three plugs are weighed then placed in the borosilicate
glass scintillation vial and digested as for the soil and sediment samples.

11.0   Sample Cleanup and Separation

The sample cleanup and separation procedures are described in detail above under Section 10.0
Sample Extraction/Preparation.
                                         E-13
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                                                                              Appendix E
                                                                          Date:  11/21/97
                                                                            Page 14 of 16

12.0   Sample Analysis

The procedure for sample analysis is as follows:

1.      Turn on main switch (controls computer plus AF detector).
2.      Turn on conditioner (controls gas meter).
3.      Screw teflon tubing that carries helium from the GC column to AF detector.
4.      Turn on pyrolyzer.
5.      Fill up solvent containers with CFhCh.
6.      Place samples in the autosampler and write sequence of samples.
7.      Press "zero" in the AF detector several times until it stabilize (it takes about an hour
       or more).
8.      Type "elab" at the prompt sign.
9.      Select "method".
10.    Select "retrieve". Hit "enter" twice.
11.    Hit "escape", select "go".
12.    Enter total # of samples to be run and press "enter".
13.    Enter file name and press "enter".
14.    Press "start" in the autosampler.
15.    A curve  is created at the beginning  of each  run by  running the following
       concentrations: 0.0, 0.83, 1.67,  3.33, and 6.67 pg/|oL for water samples; 0.0, 2.0, 4.0,
       and 6.0  pg/joL for solid samples.
16.    A blank is run following the calibration curve.
17.    A low and a high standard are run to check the calibration curve.
18.    A blank sample is run prior to running the actual samples.
17.    High  standards are run after each  set of ten samples.  The run ends with a high
       standard followed by a blank.
18.    All samples are run in duplicate.
19.    For sediment and tissue samples two duplicate samples and one matrix spike sample
       are run for every sample.
20.   QC check standard made from a different source  is used to confirm calibration.

A  consistent system  for determining peak responses  has been established by properly selecting
threshold level of the data acquisition program ( see attached chromatograms).

13.0   Calculations

Sample concentration is determined using the linear calibration curve equation:

       H = M * X + B,

where H is the sample concentration in pg/Dl, M  is  the slope of the best-fit line through the

                                          E-14
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                                                                             Appendix E
                                                                         Date:  11/21/97
                                                                           Page 15 of 16

calibration points, X is the sample peak height, and b is the intercept of the line with the Y axis.
Sample concentration is further corrected for background noise or drift, if any, by subtraction.

The formulas used to calculate the final organomercury results are as follows (see attached sheet):

Column       A: sample No. (a, b, c, d)
              B (gram): wet sample weight
              C (gram): dry sample weight
                           C=B*R
                           R: sample dry/wet ratio
              D (ng/g):  standard concentration spiked into sample based on dry weight
                           D=1000/(C*1000)
              E (ml): volume of CFbCh transferred at the first extraction step initially, 5 ml
              of CFhCh is added to sample for extraction).
              F (ml): volume of Na2S2O3 transferred at the back extraction procedure
              (initially,  1.0 ml of Na2S2O3  is added to the CH2Cb  extract).
              G (*E+5): peak area
              H (pg/Dl): concentration of organomercury in sample
                           I=(H* V/C)*(5.0/E* 1.0/F)* 1/1000
                                  V(D1): volume of CH2C12 added at the final extraction
                                  step.
                                  5.0/E: correction factor for the first CFbCh extraction
                                  step.
                                  1.0/F: correction factor for the Na2S2O3 back extraction
                                  step.
              J (ng/g): average concentration of unspiked samples (a & b).
              K (ng/g):  standard deviation of concentration of unspiked samples.
              L (%): recovery of the spiked sample
                     L=(I-J)/D* 100
              M(%): averages of the recoveries (L).
              N (ng/g):  recovery corrected  sample concentration.
              O (ng/g):  recovery corrected  standard deviation.

14.0   Confirmation

As  yet,  no other analytical method  has been  developed to  measure  sub-part per  trillion
concentrations of organic mercury compounds.  Confirmation can only be obtained by analysis of
duplicate samples by other laboratories with  similar capabilities.   Laboratories currently used by
SERF for confirmation include the EPA laboratory in Athens, GA and Batelle Marine Sciences
Laboratory in Sequim, WA.
                                          E-15
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                                                                            Appendix E
                                                                        Date:  11/21/97
                                                                         Page 16 of 16
15.0   Method Performance
This method measures organic mercury compounds (methylmercury) in water and sediment/tissue
samples at method detection limits of 0.02 ppt and 0.02 ppb, respectively. Following the same
procedures described herein, similar detection limits can be obtained for ethylmercury.

16.0   References

Alii, A., R. Jaffe, and R. Jones.  1994.  Analysis  of organomercury compounds in sediments by
capillary GC with atomic fluorescence  detection.  Journal of Kgh Resolution Chromatography.
17:745-748.

Lee, Y.H.  and Mowrer, J.  1989.  Determination of methylmercury in natural waters at the sub-
nanograms per liter level by capillary gas chromatography after adsorbent preconcentration.  Anal.
Chim. Acta. 221:259-268.
                                         E-16
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                                                                Appendix A
                                                                 Revision 1
                                                            Date:  04/18/S6
                                                               Page 1 of 14
                                APPENDIX A
 Method Validation for Pirt per Trillion (ppt) Concentrations of Inorganic and Total
                 Mercury In Wafer, Solid, and Tissue Samples

                        Limited Usi Method Validation

                            Prepared by and for:

                  Southeast Environmental Research Program
                        Florida International University
                                  OE 143
                              University Park
                            Miami. Florida 33199
                              POSJ 341-3095
                           FAX;  1305) 348-4096
Ronald 0. Jones, Ph.DX/                       '     Date
SERF Director and
Nancy A£r BlackDate
SERF Quality Assurance Officer
Sylvia S. Labie                                       Date
FDEP OA Officer
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                                                                 Appendix A
                                                                  Revision 1
                                                             Date:  04/18/96
                                                                Page 2 of  14
1.0   Scope and Application
This method covers the determination of parts per trillion {ppt) levels of total and
inorganic mercury in water, soils, sediment, and tissue  (fish) samples. A method
detection limit of 0.3 ppt is obtainable for water samples at a precision of less than
5% relative standard deviation <%RSDt and in accuracy between 80 and 110%. The
concentrations of mercury in sediment and tissue samples are significantly higher than
in water samples and can be determined at bitter precision {< 5 %RSD| and accuracy
(90 to 110 %fl).  Linear calibrations up to 1 part per million (pprn) can be obtained
and higher concentrations can be measured with dilution.

2.0   Summary of Method

Total and inorganic mercury concentrations are determined by Cold Vapor Atomic
Fluorescent Spectromttry (CVAFS).  In this method, mercury in  a liquid sample is
vaporized and  stripped from the remaining liquid by a  carrier gas (Argon!. A sheath
gas (also Argon) constrains the mercury vapor to a small stream as it passes by a light
source and photomultiplier tube. The mercury concentration is determined by atomic
fluorescence.

An  PS Analytical  (PSA)  Merlin Plus mercury analysis  system equipped  with an
autosamplir,  vapor generator, fluorescence  detector and a PC-based integrator
package is used to detect total and inorganic mercury. The system is run according
to the manual provided by the manufacturer, except lower flow rates are used for the
carrier and sheath gases. Low detection levels of 0.3 ppt Hg in water samples are
obtained with  flow ratts of 0.14 Umin and 0.125  Umin for the carrier and sheath
gases, respectively. For the higher concentrations of mercury detected in sediment
and tissue samples, flow rates of 0,35 Umin for the carrier gas and 0,2 L/min for the
sheath gas are used, To accurately regulate the gas flow for optimum conditions,
SERF installed an Omega model FMA-78P2 electronic mass flow controller in front of
the PSA Merlin Plus instrument.

Water sample preparation includes digestion by a brominatlng procedure to breakdown
at! mercury complexes.   Sediment samples and tissue  samples  are digested with
concentrated nitric acid in sealed  ampules, and subsequently autoclaved.

An NBS standard  of 1000 f/g Hg/l is used and diluted to obtain the appropriate linear
standard curve. High standards of 10 ppt and 400 ppt are used for water/tissue and
sediment samples, respectively.  NBS oyster tissue 60 ng/g (566a), NRCC dogfish
muscle 4,64 j/g/g IOQRM-2),  MIST sediment nominal 50 #g/g  (8407), and NIST
sediment 60 ng/g {8406) are used to check the accuracy of the tissue and  sediment
results.
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                                                                   Appendix A
                                                                    Revision T
                                                              Date: 04/18/96
                                                                 Page 3 of 14
3.0   Interferences

3,1   Matrix Interferences

To overcome matrix interferences due to organic substances in the water samples  the
samples ara left in an ultraviolet cabinet for 12 hours. By digesting the water samples
with bromine afterward, any remaining mercury complexes including organomercury
compounds,  sulphide complexes and  complexes with organic  material  (e.g. fulvic
acids} are broken down.  Additionally, acid digesting and autocfaving results in a
complete breakdown of mercury in the sediment and tissue samples.

3.2   Environmental Interferences

Mercury contamination at levels near the method detection  limit is a consistent
problem as  samples easily absorb mercury from  the air and improperly cleaned
glassware. To minimize contamination, all technicians are required to wear surgical
vinyl gloves.  In addition, all glassware, acids, reagents, etc. are stored in a mercury-
free clean room. The clean room contains a bank of laminar flow hoods equipped with
gold  and charcoal  filters.  The  floor is covered with flypaper to trap particulars.
Potential contamination in the clean room is checked weekly by monitoring acidified
U %  HCU water samples, which  are stored open inside the clean room. If significant
levels of mercury is detected in these samples (< 20 ppth  then the source of  the
mercury contamination is identified and eliminated.  The gold  and charcoal filters
within the laminar flow hoods are reconditioned if necessary.

Mercury-free DIW  is  produced  by filtering tap water through a  twiligan system
consisting of activated charcoal and two mixed bed ion exchange cartridges. This
water is piped to the clean room where  is then passed through a Barnstead Mega-ohm
B Pure system. This system is  fitted  with two filters  (Thermolyne: colloid/organic-
DG831, and  ultrapure-DQSQiJ  in line with a 0.22 micron pleated particle filter.
Mercury levels are not detectable (<0,1 pptJ in this water by  both our laboratory and
by and independent laboratory analysis. This is the  only water used for all analyses.
3.3   Laboratory Glassware and Sample Bottle Cleaning

Laboratory glassware is kept  to a minimum, with Teflon bottles and beakers used
when passible. All reusable glass bottles, volumetric flasks, graduated cylinders, and
teflon beakers are dedicated to the preparation and storage of a specific reagent, and
are rinsed between usage with acid (0.5N HCl and 0.05N HNO3) and rinsed three
times with DIW.  One  volumetric flask is kept dedicated to  making the primary
standard and is rinsed only with this standard. Glassware or plastic containers that
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                                                                  Appendix A
                                                                   Revision 1
                                                              Data:  04/18/96
                                                                 Page 4 of 14

have comt in contact with samples, such as ampules and scintillation vials are used
once then discarded.

Teflon sample bottles that have been used previously are rinsed three times with DIW
and  filled with 1 % HCL  After filling, t ml of mixed brominating agent is added for
every iO ml and the bottle is shaken, This mixture remains in the bottles until used
Prior to their use, 500 #1 of hydrexylamine hydrochloride is added to remove the free
bromine. The bottle and cap are then rinsed three times with DIW.  Sediment cups
and 20 ml scintillation vials are non-reusable and discarded,

4.0   Safety Precautions

iromine vapors are tojcic; therefore, prepare the brorniniting agent beneath a hood.
Keep all containers with the brominating agent securely capped  when  moved or
stored. Neutralize sample bottles with hydroxylamina hydrochloride prior to their use.

Hydroxylamina hydrochloride is a skin and eye irritant and can cause dermatitis.  A
face shield and gloves must  bt worn when handling thii material.

The  exhaust fumes from the atomic fluorescence spectrophotometer are toxic and
must be ducted  away.  The low pressure  mercury discharge lamp used  for
fluorescence determination emits intense U.V, radiation.  This  lamp  must not be
viewed directly.

5.0   Apparatus and Materials

Analytical instrumentation includes an PSA Merlin Plus mercury  analysis system
equipped with the following:

      Autosampler           Vapor Generator
      Fluorescence Monitor    IBM compatible computer system

In addition, an Omega model FMA-78P2 electronic mass flow controller is installed in
front of the PSA Merlin Plus instrument.  All of the above equipment is stored beneath
a  protective hood.   All other  standard  laboratory equipment (Teflon  beakers,
glassware, pi pets, etc.)  is  kept  within the clean room and  dedicated to mercury
analysis.  A mercury-dedicated refrigerator, oven,  and analytical balance are kept
within the clean room, Polyethylene scintillation vials (20 ml} with polypropylene caps
are  used with the autosarnpler.  Water  samples  suspected of low mercury
concentration are injected into the instrument manually from 125 ml teflon bottles.
                                     A-4
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                                                                  Appendix A
                                                                   Revision i
                                                              Date:  04/18/96
                                                                 Page 5 of  14

Additional equipment needed for sediment and tissue sample preparation include:

      glass bottled blender     autoclave
      syringt                  oven
      plastic specimen cups    balance
      10 ml ampules

6.0   Reagents

6.1   Bro mi nation Reagents

Q..1 . M .te|assii4m=lg:rjDjma|i
Heat 8,38i g KBr03 overnight in a glass scintillation vial IKimble 74511) at 250° C
+ /- 20° C in a furnace to remove mercury.  After cooling dissolve the potassium
bromate in iOO ml of QIW and store in a borosilicate glass bottle with a Teflon cap,
Prepare Weekly.

Q.2 M Potassium Bromide
Heat 1 1 .9 g  KBr overnight in a glass  scintillation vial at 250* C  + /- 20* C to remove
mercury. After cooling dissolve the  potassium bromide in 100 mi of DIW and store
in a borosilicate glass bottle with a Teflon cap.  Prepare weekly,
0.05 M PQWs^umMfOS^^^^^ - 0. 1 M PpjajSSium Bromate (KBrO3l
Mix equal volumes 1100 ml) of bromate and bromide in a borosilicate glass II 50 ml!
bottle with i Teflon cap. Prepare daily,

6.2   Hydroxylimine Hydrochloride

Dissolve 6 fl of NHjQH • HC1 in SO ml of OIW in a 60 ml Teflon bottle. Prepare weekly,

6.3   Stannous Chloride

Add 50 ml  of 12 N HO to 40 g of Stannous Chloride (SnCI2S.  Bring to  1000 ml with
DIW in a borostlicate glass bottle with a Teflon cap. Stannous chloride is purged of
any trices  of mercury with argon gas continuously throughout the analysis. Prepare
fresh daily.

6,4   1 2 N Hydrochloric Acid

Concentrated HCI (12 N HGIJ is dispensed via a pipette or poured into a graduate
cylinder, either of which has been previously acid washed and rinsed three times with
DIW.
                                     A-R
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                                                                  Appendix A
                                                                   Revision t
                                                              Date:  04/13/96
                                                                 Page 6 of 14
 6.1    16 N Nitric Acid

 Concentrated  Nitric  acid (16  N> is  dispensed  through a pipet, which  has betn
 previously washed and rinsed three times with OIW,

 6,6   Standards

 Dus to its high concentration, primary stock standard is prepared and stored outside
 of the mercury-free clean room.  The primary stock standard is made by addition of
 100 * of SEPEX (PLHG4-2X) (1000 ng/mil to 1000 ml of DiW with  10 ml of trace
 metal grade HCI in a glass, volumetric flask with a ground glass stopper,  This
 standard is prepared daily. Secondary standards are prepared daily in 500 ml Teflon
 bottles by adding concentrated HCI (5 mil  to 495 ml of DiW. The primary stock is
 brought into the clean room and 50 jil - 250 n\ (depending on final concentration of
 10 ppt - iO ppt! is added to the bottles containing the water-acid mixture with a
 pipit.

 6.7   Standard Reference Material

 Thi following  standard reference materials are used to check  the accuracy and
 precision of the tissue and sediment digestion methods and analyses:

      DORM-2 Dogfish muscle (NRCC)
      556a Oyster tissue (NBS)
      8406 Sediment (NIST)
      1407 Sediment (MIST)

Thate standard reference materials are stored  ind dried according to the Certificate
of Analysis accompanying each standard. The standards are digested following the
same  procedures used for tissue ind sediment samples.  They are prepared and
analyzed on a daily basis,

7,0   Calibration

A linear calibration curve Is run prior to each sample run.  For low level water samples,
standards include 0,  2.5, 5 and 10  ppt.  Standards run for tissue and  sediment
samples include 0, 100, 250, and 400 ppt.  All standards are run in replicate and
plotted using the software inherent to the instrument.  Unear regression analysis Is
used to determine the bast-fit calibration  line with a regression coefficient (r2} of
0,998 or better. Standard curves outside the acceptable limits are run again, and new
standards are prepared if necessary.
                                    A-fi
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                                                                   Appendix A
                                                                    Revision 1
                                                              Date:  04/18/96
                                                                 Page 7 of 14

 The sensitivity of the Merlin Plus System is such that a zero mercury concentration
 results in a zero result. However, multiple dilutions of the source standard as required
 to product the low standard of 2,5 ppt, often results  in error, thereby  producing a
 standard curve that does not intercept the origin. Therefore, once the standard curie
 is checked for linearity, a new linear calibration curve is recalculated using the hiah
 standard and forcing the intercept through zero. Mercury concentrations in samples
 art then determined by comparing sample peak heights to  the new standard curve,

 8.0   Quality Control

 8.1   Method Detection Limit

 The method detection limit (IVIDU of 0.3 ppt is determined for this method according
 to the EPA  procedure described in  40 CFR  Part 136,  Appendix Bf revision 1.11,
 except that a value of 3 is used in place of the Student's T value. Specifically, seven
 or more  replicate samples containing a known, low concentration of mercury are
 analyzed. The standard deviation of the replicate analysis is determined and the MDL
 is computed as 3 times the standard deviation.

 Tabla A.I
 Method Detection Urnft
MatrU

Spited DIW
(DIW plus IP pi
Hg)




Sediment






Hi Concantrnion
Ipptt
2,315
2,093
2.216
2.167
2.290
2.QS3
2.118
84.30 ppto
8S.42 opb
82.44 ppb
81 ,32 ppb
84.30 ppb
82.44 ppb
§2,81 ppb
Mean

2.115






83,29 ppb






Standard
Deviation (S)
0.085






1,42 ppb






MDL » 3 x S

0.2,55






4.27 ppb






8.2   Precision

Precision is defined as the agreement or closeness of two or more results of the
same sample, and  is determined in terms of percent relative standard deviation i%
RSD) using"the following equation:
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                                                                  Appendix A
                                                                   Revision 1
                                                              Date:  04/18/96
                                                                 PageS of 14
                     RSD  =_£, * 100,
                            X
 where, s and X represent the standard deviation and mean, respectively of two or
 more remits of the same sample.  The analytical precision of this method is
 variable with more precise measurements obtained at higher mercury
 concentrations,
Tabl. A.2
PrvdiJon
           Matrix
Hf Concentration
                                                             %RSO
           Watar
  0.3 • 30 ppt
                                                             < 5%
           Water
  5 - 500
                                                             < i%
           Water
  1 • 1000 ppt
                                                             < i%
                Slurry
 1 ppt« 400 ppt
                                                             < 5%
        Tissue Slurrv
 1 ppt - 400 ppt
                                                             < 5%
8.3   Accuracy

Accuracy is defined as the agreement bitween the analytical results and the
known concentration. Accuracy is determined by running continuing calibration
itandards or by check standards and is determined as percent recovery (%RJ
according to the following equation:
                        -Observed Standard Cgjnjp.entration
                         Known Standard Concentration
                          1OO.
Instrument accuracy is determined on a daily basis by performing multiple analysis
(5 or mors repiicatesl of the high standard.  Percent recoveries between 90 and
110% are obtained for water samples with a high standard of 10 ppt. For solid
and tissue samples with a high standard of 400 ppt, percent recoveries between
96 and 105% are obtained.
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                                                                 Appendix A
                                                                  Revision T
                                                             Date:  04H8/96
                                                                Page 9 of 14
 Tafafa A,3
8.4   QC Checks

Calibration check samples are run in duplicate following at the beginning and after
every 10 samples.  For solid and tissue samples, NIST or MBS standards are run
after every 20 samples,  Accuracy for each of these calibration check samples and
standards must  be within 90 to 110% or the samples must be run again,

8.0   Sample Collection, Preservation, and Handling

9,1   Water Samples

Water samples are collected In Teflon bottles. Collection is done while wearing
shoulder length  polyethylene gloves over a pair of vinyl gloves.  Surface water
samples are collected through a 105 j/m nylon screen via a vacuum system to
reduce the amount of sediment collected. Samples are double bagged in zip-lock
polyethylene bags and placed in a plastic ice chest/cooler used exclusively for low
level mercury samples.  Samples are returned to the laboratory upon the same day
of sample collection and preserved In the mercury-free clean room with 0,5 ml of
trace metal grade HCI per 100 ml of sample. Sample analysis within 28 days is
recommended.

9.2   Sediment Samples

Sediment samples are collected in polyethylene specimen cups (Elkay non-sterile
wide mouth specimen cups with screw caps - 128 ml volumel and placed in
polyethylene zip-lock bags. All field samples are kept in a cooler used exclusively
for low level mercury samples until they are returned to the laboratory, where they
are stored in a freezer. Samples can be stored indefinitely within the freezer;
however, analysis within 28 days is recommended.
                                    A-q
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                                                                   Appendix A
                                                                    Revision 1
                                                              Datt: 04/18/9i
                                                                Page 10 of 14
9.3   Tissue Samples
Fish are collected with a dip net and stored in plastic bags for transport to the
laboratory- In the laboratory fish are stored within the freezer indefinitely;
however, analysis within 28 days is recommended.

10.0  Sample Extraction/Preparation

10.1  Water Samples

Water samples analyzed for inorganic mercury do not require additional sample
preparation prior to analysis, For analysis of total mercury, the samples are placed
in an ultraviolet cabinet for 12  hours, allowed to cool, then 2.5 ml of KBrQ3/KBr
solution is added to 121 ml of  each water sample.  The sample is left to brominate
for one hour in the Hg-free room; after which 500 jri of hydroxylamine
hydrochloride is added to  the solution to inhibit further reaction. Samples are
permitted to settle for at least  10 minutes before analysis.

10.2  Soils and Sediment Samples

Preparation of soil/sediment samples is done outside the mercury-free room, due to
their high mercury concentrations.  Soil/sediment samples are homogenized and
slurried in a glass bottle blender,  A mixture of 120 cc of soil/sediment and SO mi
of DIW is blended for three minutes.  With a syringe, 10 ml of the slurry is
collected for dry weight determination.  Another 10 ml is pipetted into a
polyethylene specimen cup and diluted to §0 ml with DIW containing 5% HCI to
neutralize any carbonate contained  in the sediments.  The slurry is mixed well, then
1 ml of the slurry is transferred to a 10 ml ampule with 2 ml of concentrated nitric
acid (total volume in the ampule is  3 ml) and left to sit for 20 minutes.  The
ampule is sealed and autoclaved for 1 hour at 105®C,  The ampules are  allowed to
cool completely to room temperature, ind then 0.5 ml of the ampule solution is
put into a 20 mi polyethylene scintillation vial containing 19.5 ml of DIW and 1 %
HCI for a dilution of 1:40.

The 10 ml of slurry collected for dry weight is weighed, dried in an oven overnight
at 80*6, and weighed again. Duplicate or triplicate samples are dried and weighed
until a constant weight is obtained. This constant weight is then divided by 10 to
obtain the dry weight of sediment within the original 1 ml extracted for analysis.

10.3  tissue Samples

Fish samples are prepared similar to soil/sediment samples, except that the initial
addition of HO to neutralize carbonates is not performed. For small fish (Gambusia
                                     A.in
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                                                                  Appendix A
                                                                   Revision 1
                                                             Date: 04/18/96
                                                               Page 11 of 14

sp.J, the entire fish is weighed, placed in ampules and digested. For large fish
Ibass and catfish), a stainless steel core tube, 4 mrn in diameter, is used to collect
three tissue plugs from the left fillet of each fish.  Care is taken to collect muscle
tissut and not scales or bones. The three plugs are combined in a 10 ml ampule,
weighed, and digested according  to the procedures described above In Section
10.2. The weight of the tissue sample that is digested and used for analysis is
usually between 0.3 g and 0.4 g.

11.0  Sample Cleanup and Separation

Additional sample cleanup and separation are not necessary to separate the
mercury from the sample matrix.  The bromination process used for the water
samples results in a complete conversion of all organic forms of mercury to
mercury (II), In addition, the acidification followed by  autoelaving the sediment
and tissue samples results in a complete digestion of the sample.

12,0  Sample Analysis

The PSA Merlin Plus Fluorescence detector is operated according to the
manufacturer specifications with the following modifications:

*     An Omega model FMA-7882 mass flow controller with a channel
      selector is installed at the front  of the Instrument. This flow controller
      is used to more accurately regulate the flow rates of the  carrier and
      sheath gases {both argon) while the flow controllers supplied with the
      instrument on the hydride generator are open to full capacity.  For low
      level mercury in water samples, the optimum flow rates of the carrier
      and sheath gases are 140 cc/min and 125 cc/min, respectively.  For
      high level mercury* such as in sediment and tissue samples, optimum
      flow rates of the  carrier and sheath gases are 350 cc/min and 200
      cc/min, respectively,

*     When analyzing water samples from  121 ml teflon bottles, the auto
      sampler is removed and the switch box is modified to sip only from
      the right sampling tube.

The procedure for sample analysis includes:

1.     Tighten the peristaltic pump (pumps wash water, waste water,
      sample and stannous chloride).
2.     Turn on the wash water to the system
3.     Turn on the computer
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                                                                  Appendix A
                                                                   Revision 1
                                                             Date: 04/18/96
                                                               Page 12 of 14
4,    Turn on the gas to the system.  The argon (Zero grade* flows through
      two gas purifiers (charcoal and gold! and a moisture trap before
      reaching the instrument.
5.    Tyrn on the line stabilizer/conditioner.
6,    Check to make sure no tubes are crimped, and that flow is smooth in
      all tubes before proceeding.
7,    Check gas flow at the mass flow controller.
      Note; For low level Hg-coneentrations the optimum level of the carrier
      gas has been determined to be  140 cc/rnin while the sheath gas level
      has been optimized at 125 ee/min. At higher Hg-eoneentraliens the
      carrier gas is 3SO cc/min, and the sheath gas is 200 cc/min.  The
      membrane dryer gas flow rate is 1  i/min.
8,    Allow the system to run on DIW for 1S minutes.
9.    After 1S minutes switch the instrument to SnCI*.
10.   Note: tht sensitivity  dial on the instrument is run at highest sensitivity
      for water but may be lowered for runnfng of sediment, soil and tissue
      samples. This method is adequate for samples of the range we have
      run to date.
11.   When the instrument is ready, zero the fluorescence detector and run
      acidified water (0 ppt» to check baseline response of the instrument
      and guard against unexplained contamination from reagent
      preparation. When peak height of D.I. is 0.0-0.3 the standards may
      be run.  Initially one high standard is run to test for consistency  of
      standard preparation and machine function. The range of standards
      will reflect the concentration of samples to analyze.  Eight standards
      (four concentrations, two replicates! mm run for each standard curve.
      Standards run for low level samples are 2.5, i, and 10 ppt.
      Standards, blanks, and high level samples (generally fish, sediments
      and soil) may be tun in plastic scintillation vials. Water samples for
      total-Hg are digested and analyzed  in 125 ml teflon bottles. Digested
      acidified DIW water samples are analyzed along with the samples as
      reagent blanks. This  number is subtracted from sample values.
12,   After running the standards, two samples of the 0 ppt (acidified
      water) are analyzed before running the samples.  Each 125 ml water
      sample  is analyzed at least three times. Tissue and sediment samples
      are run  in replicate. One run of fifty samples plus standards takes
      approximately 2 hours and uses approximately 10 ml of SnCla per
      sample.  A new standard curve  is run when the SnCl2 is replaced.  In
      addition to running a full set of standards at the beginning of the
      analysis for each bottle of stannous chloride, a replicate of the highest
      standard and zero ppt are run after every 10 samples.
                                    A-12
-------
                                APPENDIX. B
Jonas Jacofason  Jaffi, Waat-ThoniiS, Arfewom, ind All. 1934. Method Davetopment
                    of Water, Soil, and Tissyfl hir fhfl Amifsis of Total and Organm
                                      Soictorn^ Watir, Air and Sol.
-------
  Method Development and Sample Processing of

  Water,  Soil, and Tissue for the Analysis of Total
     and Organic Mercury by Cold Vapor Atomic
               Fluorescence  Spectrometry
 R 0  Jones1"", M.E, Jacobson1, R. Jaffa*3, J. West-Thomas', C. Arfstram'
                           and A. ^IIJ1-3
 1 Southeast Environmental Research Program, 3 Department of Chemistry,
  3 Drinking Water Research Center, * Department of Biological Sciences.
Florida International University, University Park, Miami, Florida 33199, USA.
                        (*««, »» m* Watoflic.1 flirt ti«Ml ««m*»I«.

                        '*'' «
                       fl.h ih.
                . A W* ««., PS JiMlyited irtomic fhM».c.r*.
            with .11 •u»i«npl.r. wpc.r ^MrMor, nuonw
               u«d in th. d«wnln«i»n cf «m Hg. Th.
                                ,                             of  th.
                           «b.rt. Th. araa^c Hg compound, .r. duttd **th . «n.ll
       to fhdW*  .          oigin.rn.murv W«« ** !^ *-d
                                         .Kifectiori
            Mupl»al with Mamie fluo«ic«fK* d««ut»rt,

                           1. Introduction
Mercury is a widely distributed pollutant in the aiwiranment and ha* gained
consldeiable toxicological concern in recent years. In some cases, the desired
quamtatior,  levels  of this metal  challenge the  detection l.mrts of *a
instrumentation md  methods In  current use (Swift and Campbell, 139J,
Kamroin and Kno*. 19921. This has certainly encouraeed t^udev^ophnie"lthQ*
sensitive reliable and precise methods for the analysis of HQ. Funher, the
oroanie forms of Hg,  particularly methyl mercury 
-------
ECDJ  iRubi « at., 1S92; Q'Reillv, 1982J with or without pre-denVatiiation of
the organic mercury compounds T!w instrumentation and sample preparation
of the existing methods strongly limit the ultimate sensitivity and efforts to
lower the deletion  limits  have not b«tn  entirety successful (Swift and
Campbell, 1933J. In  addition, the ECO is an wseleoive detector ana the
column has to be tediously conditioned with large injections of HO (HI ehlondi
to alleviate poor ehromatographie response to organomercurials (Might and
Capar, 1984; Rwbi era*. 1932; Uthi etat.t 1972; Bryan and Ungston, 1992;
Bulska et at,,  1992L   These disadvantages demonstrate ths  need for the
development of new methods in this field.
       TTiis papir describes atomic fhiorasoinee-basetf methods for analyzinfl
total  Hfl  and  organic Hg  compounds  at  tow  part-per-trilian  levels  in
environmental and biological samples. Tha atomic fluorescence f AFSI method
SBtoom,  1989;  AID era/., 19941 has become increasingly important compared
to CVAAS, since tht instnimentil detection  limit of this  mrthod is about 1
pieogram o*r less and at least one order of magnitude better than for CVAAS
(Undqvist, 1993J. Total H§ analysis involves thrwt srages: samplt  digestion,
coid vapor generation arwJ  atomic fluorescence detection.
       in wattr  samples,  the  difficulty in measuring  MtHg  and  other
orsanonweurJals lies  in concentrating these  compounds from solution. This
work employs a sulfydryl cotton fibre medium (Lee and Mowrar, 19891 which
effectively adsorbs and prtconcentrates trace levels of organomercurials. The
orfanic Hg compounds are elutad with acMfc potassium bromidi ind ixtracted
into dichtorarnethana and subjecttid to GC analysis with APS detection, Sotl,
sedimtnt and tissue samples are treated with acidic potassium bromide and
copper sulfati, and extracted with dichloromethane. The initial extracts an
mybiicted to  sodium  thiosulfati*  clean-up  subsuqent  to  capillary gas
chromatography with  atomic fluortscenca detection (AID et at.t  1994S.

                       2. Materials and Methods
2 1 SAMPLE COLLECTION AND PREPARATION   *
Surfaci  water  samples  art coltactid in 2 L Teflon {Nalgunei bottles using a
¥acuum system- Samplis are sertuned (IDS pn Nytex rutting! to prevent the
colltetion of large particles with tin watir samples. All tubhigs and fittings
used in the sampling  system art constructed of tifton CSffiP.  mtirnal SOP,
1994J  The aamplts are collicwd by a 'dean person' using do«bl« gloves
(short vinyl gloves undur shouldar length polyethylene gloves, QaltTechl and
a double bagging technique,  All  samples  am placed in rip-lock polyethylinB
bags fRsher Sdentificl.  then in an additional plastic sampte bag and placed in
an icschest/coolir. In the  eltan room, concentrated Hydrochloric aod»  (wae«
metal grade. Fisher Sci»ntific> is added to tha wattr samples for preservation.
       Surface, soil and sediment samples art collected using either a stainless
steel soadi, trowei or Eekman dredge. These samples are placed into wide
mouth polyethylene specimen c«ps C1 25 ml, fisher Scientific!. Subsurface soil
or sediment samples are collected in polycarbonate core tubes. Upon arrival to
the laboratory tha samples are immediately frozen to preserve their etiemical
           samples are collected using a dip net, with the sampler wearing
two pairs of gloves. The fish are placed in tip-lock sample bags, labelled, and
stored in a cooler with ice for transport to the laboratory. Rsh samples remain
frozen until ready for analysis.

2 2 SAMPLE DIGESTION FOR TOTAL MERCURY DETERMINATION
Wat& Samples. Water samples are digested in a 125 mL teflon bottle w»th  1
-------
mL HQ and 2.5 mL potassium brnmati (ICBrQ^/potassium bramWa (KBrO)
niaum overnight tS»kles. a* *. 1380! Boom and fittgerald, 19881. These
caLta am pwpared and «m*hi «" capped bottle*! in the Hg-cltan room.
Prior to analysis, BOO jA. hydnneylaraine hydraehteride is added to destroy
excess bfomint awl the samplsi thoroughly shaken.
Sof mdS^anmt Ssmpfe. Soils (such as p*at, marts and marly peati are first
homoiinizBd by adding 30 to 10 mL of deionizid water and blended for 3
minutss to a uniform  eonslstsncy with  a  blendur (QsuriierJ. From the
homogenized slurry I mL to diluted into 45 mL of Q.6N  HO to neutralize' any
eartaonatas. In a diwn spiemwi cup. Of this mixture t rnL is placed in a 10 mL
anmuto with 2 mL of eon^ntrattd nroie acid WNO,L {trace mitaJ grade, Rshtr
SciintiflcJ. Vdesmic sisto are first siavid through a *8§ mesh stainless  steal
sieve. In a' 10 mL ampuln, 0.5 g of the awwd sample '& dJgestBd with 1 mL of
0 6N HO wid 2 mL HMO* Olg«st»d soil and stdimant samples sir* taft to stand
under a fum» hood for 20 mtoutiw. The amputes are subseqyf ntiy sealed and
lutodavtd for 1 h at 1i1*C. Before amlysis the digestates are  dilutad witft
0.12N Ha solution in a 20 rnL polyethylent vial.
ffsft SmipMs* To quantify total Hi in small fish « 0.4 9, < 30 mm in length!
tha entire flsh i« weighid and placed in 10 mL imputes and digested using 1
mL dtionilid water tnd 2 mL eonctntrated HNQ,* After sending 20 minutes
under a furfii hood, *e ampules are sealed and autoclav«d as described above.
For thi analysis of law fish (ipprosdmately 30 em or JongerS, 3 tissue plugs
(stainless steel core tube, 4 mm m diameter] are taken from the left side (using
only  muscto tissue!, and  combined  to  obtain a repws^itative  sampla
{approximately 0.4 0). TH» samples ire fhftn processid as indicated above for
aoil and sadlment,                                      ,     . * «,,
      Thes« digerton procedyras result in the conversion of organic forms
of HO to inorganic m«ury |Hg"*l. The digested sampte are introduced to the
cold  vapor generator, at which point tin Ctl} chloride is used TO effectively
reduce Inorganic mercury (Ha**! to its elemental gaseous form (Hg»J. pr
-------
    Vapor Gmwatim. in th* continuous flow vapor pm" •V""*' JJJJJ
    duced to HgCOI following *• addition °* «"» <**"••
^ped AMI the solution fin th* 1» hMd si^ratorl by
Then* 01 argon flow depends on whethir the analysts is
levels of Hg determination CP-S. Analytical,  1 §S2J.
£«nfc A.W«c» I*"*** A snoath gas (also argon* « used m
th* HS vapor through a chimney past a Hint source and a I**0™**'"'*
tetart itritfit anilas to ««h «l»r. VWth a sptdfic Woh «tf Hfl tamp
£4  iCaZd«»n Ltd, IMridgri  and . M «4 ^
isolation of tf)i raqyired txdtation and tmission wavalnngths is
              fl          towl Hi analvsli ar« erf caitifiad ACS g«da «d
        eomrmrdaUv from Rihv Sdintifle. urtaai «l«'w«|1^; *
         Biwn systim OOCMM! in thi HgndMn mom! produce* afl cte.on.zad
wu«d ta mattiO UP »Q«w. ^^Pl- diflemm, calibration scions
^ solution and autlity control standards. This waur isfimfitoiid jtawoh
rSlidan  wttim consisting of activated charcoal and twc > mmd INd .on
««hanga cMridgw btfart bring pfptd to ita Hfl-d»an mom. 0.1 N «rt^ 0^
N KfrO and  1-7 M hydroxyiamjnt hydroehlonds solutions are made up by
dissolving th« apppropriatB amount of tha sate to dttanind v«wr. The KBrOa
^dKbVO  -2 ?Whi«d ovemignt In a  gla*i vial at  25Q®C  to «mov«
            Tin diiistino solution is made up daily by mJ*hti equal votoas
           OtN ICBrO, Id 0.2N KBrO aolutton.. AB iolution. are praparad
                                            Itad cas.
o                ,      .                .
    and stored in borosilfcate botdi* with ttflon Itad caps.
   rZworidng standard. are prepared daiyfmm. Hi ^ck aoUta , «100
    md dllutsd to thi dtsirtd concentration. Th« stock solution is also
    SkvSS a commardany avaitabte mercury standart  1 1000 ugWL
   Mu-iriN. idlson, NJI. Caltoration solutions ^r^^j" *»*
         and stibiHttd by adding S mL concentrawd Hd.  No i^
        * for quality control of Hfl In wattr near yUratrace tovds.
                       60n8/fl  8406!
mittrial* for quality contro o   fl n w
SSjfiilUJilu. 60n8/fl  8406! ^«~ « '"J'.
Tissyi!64 ng/gj quality control standards am obaM  from tf»
Institute of Standards and Tachnotoev (Gaitntnsburo, MDJ.
    ORGANIC MERCURY
            f *S msw Ss^pte*. A 1.0-S.O g portion of the
                d^Ttl is^ed in . 20 nil ***•*+*
           *745t 1 ). To th* vial I mL distillsd water, 3.0 mL of 1 .0 M copper
           S TmL  of acidic potassium  Imridi «*£  « jriM. Tta
           shaken for t  hr  «  330  rpin  (Gwotory »*"  "J*Lg;
 Dichloromtthant IS mU is added and *•!•**« "• A*-"** ILSef RC S
 rpm and than centrifiiflid for  10 min at SOOO x fl in a S"""*""* "^


            rSL «333726» and 1.0 WL of 0.01 H«^«"""£
            mixture is shaken for 20 min  at 330 rpm and centrtfuged at high
        aSai cemrifu^ Tne a,uMus lay^O.S mU 1. J— « «
      icrocantrifyoB tubt (Rsherbrand, Rsher SclsntiflcJ, a«J 0.3 rnL d =0.5 iM
        dhMli and  0,3 mL dichloromathane ^f^^^S^tSSi
       to 1 rnin on a Vortex Ganie mi*« and cwtnfugid for 2 mm at higrt
       MB 74i" a) to a Herrnle centrifuge.  The dichloramOTnan* Is ttansf^ad
       0 i Si^mSii via. contaWng a law crys^ of ***"•-»"
 Slohate^nd subjaetfld to GC analysis. Injections of 5.0 *L are us«l Sampte
 sp fed with knZn concemrations  of m«h¥. - and tthlyimrairy chlonde are
-------
                  the recovery factor ""^ *»
              TM .ulfrdryKofteii (SFC) fibre columns »• made ** 1
                   containing 0.1 g of SFC fibre padwd loosely and as
                     SFC columns at. connect in stries ami the water
                through tf»M bv vacuum.  Q«* mL of acidic pota^unt
           0 J wL of 1.0 U cow* sutftti are then pipetted on tfw surface
          rbaiit and «• eluatt to eo!li«nd in a 2 mL micro-Centr,fu0» tubt
      SdMHId.  71* H extracted with 0.2 mL «fehtemmi*ani on a VOTOM
            for   1.S  min and  cantrtfuged  as dsscfibed  above,  The
                      thin  translerrtd to a 2 mL glass lamptafl  viiJ
                      of anhydrous sodium suifate and subjected to GC
analysis.

2 i INSTRUMENTATION AND ANALYSIS
A Ichmtte diagraiti of «• GC-AFS systtn, used in *is work . shown »
Rgure I and the optimum oparatlno conditions art summarized m Tabla ILA
        Gas
                  atosraphtc-Atomic Huorescenct Spectrametric Systim,
                     "i oLvwn mp. 3: Mercury «p, 4; Moteluri trap 5,
                  : lr*cw, 7: Colymn, 8: Priss^fit union, 3: Pyrolyset, 10.
                     O-SSmm Ld. It." Ttflon unions, 12; Teflon wansftr
                 Atomic Ruonscence ditactor. 1 4: E^b ehnnmonphic
                       systim, IS: yellow controJter-ChanniJ A mate-
 up, Chamtal B sheath pas.
HewJett-Pakard
                    58SO Series 111 gas chramatograph coupled wi* an HP
                       sampler is  UNO. A fy.ed-sito,  bonded phase
                n 5 m K 0.53 mm i,d., 1 ^n non-poiar DB-1  conno. J * W
          andi spiitl«« inieetio. mode i. empbwd. The effiuem from the
-------
column is led thrown a pyroivstr (PA Analytical Ltd.,
tha GC ovwi Jdi « pea* a* 65 cm length ef diaettvattd
id  J & W Scientific!, which is conrwemtt to tha column with a glast  prts*
fff" union P &  W SewfWffieJ. Tht Hfl items fornmd in the pyratysis ynrt we
transferred from Ha outint end of tha deactivated fused-siEca tubing to the
ftuomsrainen dettctor (teflon transfer lint, 0.5 mm i.d.. AHtteh AsncMtas).
Thi trwsfsr linn is passed through a small hate on the top of th*i GC own to
a Mirfin Mtfcurv Ryorsscance Detector, and the connietions we made VM
teflon unions,


Gas chmmatograpfa*
Injector temperature         250^0
Temperaaire program        1 mm at 40«C 60eC/min to 1 40°C,
   P                     3 min at 1 40°C» 50°Dmin to 200°a
                          lOminatlOCPC,
P^olysw tempiraturt        800°C
Column flow                4-° mL/min
Make-up flow               ®5 mUmin
Atomic fluorescence system
Shiath gas flow            300 mL/min
                                          .
Calibration rang*            1 000 (most stnsmval
Rni §ain                  10 (maximuml
Raeorder ouffut voltago      IV
Damping switch            0°
If or signaJ smoothing)

       A r«al tfanw chromatographle conrtrol and data acquisition system (E-Labr
Vtatan 4.10R, QMS TECH. INC.! Is «tirfae*J with the CSC md AFS deticw
avst«m  in thb wortc tht dwtction  Bmit is definid  ai the amount of Hg
mmsarv to giva a peak arta equal to thres times tni standard deviition of

te«rSroia^sS'aTLppned by Liquid Carbonic Speciality Gases and anof
zero orade quality,  Halium (i3,995%! is yst d as ttt» carmr gas CGQ. passed
           an o^an wap, then trough a Hg trap **********
                   rior to die GC. Argon (3S.iS8%J to employtd ai tt»
                    heath gai for tht GC-AFS tyttw i«J to also payed
        mu.    HB traps before urn to flow is regul^d by » rwltow
cooler (Omegal enyipptd with two ehanntls, diannul A (rnaka^ ftowl and
channel B (sheath gas flow, aw Bgyre 1),                      ««™ j.
    iwfs. Double dHonHed watir produetd bv a Barwwad B^™^^5^1
     in aH so lutbna. Certifierf ACS grade potassium bromU^ «pp«r«I» sulfm
    *<»}  chloridt  and  sodium  ttiimuHatt  (fisher Sciwtitei  «ua«d
throyghout this work,  The acidic potissium bromide •***"***"'**'
dtoaoMng  1TO g in 200 mL water. Trace m0uU gr.de  ememmmd sulptanc
SsO mL fisher Scientific! is added to 100 mL of watw. After eootog to
room  timperttura the solutions am mixed and made  yp to 1  L
Copper su^att (1.0 ML copper chloride (0.5 Ml and ssdium *
Ml solutions art prepared by dissolving  appropriate amoyfitt
water. All solutions are eirtracted with dichtoromethana iprior to «""•
^nM Ai Hi standards am purchased from Ultra Sdentrfte. Stock stwdard
         rf mXl. and ethylnwcwy cMorid. are ^
appropriatt amount*  of  the standards  In optima grade
-------
   ttcl. Thus! solution* am stored in dark brown bottles aid diluted with
dichlorometnane to give woridno standards of the desired concentrations whan
     e                    (SHQ fiber sdsorf«»f. This synthesis follows the
procedure us«d by L»* and  Mowrer (l9Sa|. A mixture is first preparid by
addino the foJtewiriB reagents in sequence to  round bottom  flaslc 100 » rat
thioojyeoie add, 60 mL acetic anhydride, 40 mL acetic acid (36%t and 0.30
mL eoncemratid suJfurie add, Tha mixture is allowed to cool to 45 C» then 30
a erf cotton wool art addid and alowneJ to soak thorouohly '« tile mixture. The
reaction bottle m placed in an own for 3 to 4 days at 4CJ°C then the product
it placed 
-------
Tabla Hi. Precision, rtcnvwy and method detection Unite for
                          and organic Hg.
                                                            . total
    Analyta

   ^mmiir****^^****^

  Inorganic Hg
   •ri^	

   Total Hg
   •111-    '"™


   Total Hg
   Total Hg
  Organic Hg
   (MeHg*.
	 — 	 ...mrnii.ni-
Matrix
Water
Water
Tissue INBS
oyster tissue
1i66a 84
ng/gj
Soils,
sediments
WIST
sediment
840660
no/fll
Water
_.
Soils,
sediments,
tissue
PfBGBlOn
[%RSD)
^s
^.5
-------
                                                                .t
 netM SHC fiber ba« a WQh td«tiviW tar organic mercury compounds, it
avoids th* txtreetion of mxmmms compound which causes sawra
                  *™ obtained using the calibration curves generated
daily Ttw (dttoridfa of n»ithv»- and frthvlmercwv ara ustd « craate the
standard deration curves txpressid in terms of p«ak aisa v*
               tarid, coi««trati«i (pg HgM |i injectionl.  Thi . i^tanv
                of «• «3naJ to a 2 PO Hg/5 ^L standard was 1 .5%
                      JH-3K The linear range usid for the sineratton of
eaibration e«ve» ta 0 and
                            Rttantlon tfm«
                         of pure organic
                                               standards on new
       , EM: 1238.6 pi HB/ll
4 Da Ho/nL and the toiar correlation coefficients am typically 0.9S8 and
0                                                         ve
                                             chtonde
                    this «Iue is influenced by differences
              aftect the pwtUonino °* wganic Hg compoynds. Further
                 wninition |%R) to ividen«d by tht lack of offoal
                 (for organic Hg analysis) and the «rr«nt n.ed for .
 standardis).
-------
                         4. Conclusion
     ampule digestion of inwranmumal and biological samples tor
            described In ttiH ink* b I relatively « J""**1
               of 9S - 105% recovery of Ho8, Oiissiton of «
               « s«Hed tO mL ampule is a dim arid «
      far Ha dottrmiMtion. Whan thate samples an aotodawd
       tek wry taty » <•« sample. aollibl. for AFS ds
vassal dioestion foltowwd by cold vapor generation and atomic
dMKrion hw yliWtd dtwctioo limits that allow tf» quantifl^iioii of
levels of Ha hi wawr sarnplas. Th« preparatton tadiniquas and use of an
dean room  Navi mad* It possibls to fidyc* signifirantfy conamHiat.oii of
          ^ ^       of orflanic H§ by GC, sample
bacoma adsor bad or bound to the stationary phase of thi colymn aftar vanous
Wertions, exerting i negative aftaet on thi tfficieriey of *• analysb. With a
         Sck^a«ion  MP.  dim torftr«iCBS can  be  e
ramoMd, alowing efficient analysis of the oroaromerairials. In water
the omanic Hg compounds can to tffleientiy pr«eorKirittat»d OIMO
fltar  which also providt a sample  ctoaimp. Th*  column  Bfe
oSuSSt to^«r «** ** d«frUP •"•» OTd CT" bl USid FOUtinfll¥ fW
analysis of orianomercurials with no apparent to,ss »i rfficiency.

                      Acknowledgements
Thk study was supported by tiw National Park Strviee (Everglades National
Park* and th» United  Status  Eftvilronrnartal  Prowction Agency throuflh
cooptfative agretment (AI 280-1 -SO 181.
                          Rafftrencos
F%*MIi mmf «»™«i-~* »™
n~^_ A * - l»B9 Cffi. J, Artu Aqu*t. Sa ••!.
•SZ: H £ atTilSL.U W. F.: Itti^t CM* M 501. Itl-IK.
SyaKi^Rtsrsss^-M.
      c
      ?•

                              a. ^ a. •.
                                    U7-1S6.
-------
                                                          Appendix C
                                                           Rwision 1
                                                        Date: 11/1997
                                                         Page 1 of 10
                           APPENDIX C

Standard Operating Procedures for Total and Inorganic Mercury Analysis in
                    Water, Sediment and Tissue
-------
                                                           Appendix C
                                                            Revision 1
                                                         Date: 11/19S7
                                                          Page 2 of 10
STANDARD OPERATING PROCEDURES FOR TOTAL AND INORGANIC MERCURY
              ANALYSIS  IN WATER,  SEDIMENT AND flSSCE
             Southeast Environmental Research Program,

                  Florida International University
                          University Park
                        Mi ami,  Florida 33199
                  Version 10,   November 19, 1997
C Previous  versions written  July  27,  1993;  September  13,  1993;
S€f»t«mfo@r  21,  1993;  November 4,  1993;  April  1,  1994;  April  18,
1994; May 20, 1994; April 18, 1996;  and September 15,1997.)
                                 C-2
-------
                                                                     Appends C
                                                                      Revision 1
                                                                  Dale: 11/19/97
                                                                    Page 3 erf 10
MERCURY
COLLECTION AND STORAGE

      Water samples are collected in Teflon (FEP) bottles. Collection of samples is done
using vinyl double gloves (Polyethylene shoulder length PPE glove, QakTeeh) bagging
technique.  Samples are  then placed in zip-Jock polyethylene bags,  then placed  in an
additional plastic sample bag in a plastic ice chest/cooler. In the laboratory 10 ml of trace
metal grade HCI is added to preserve samples.  These additions are done in an Hg-ciean
room {described below). Soil samples are collected in polyethylene specimen cups (Elkay
non-sterile wide mouth specimen cups with screw caps - 128 ml volume) and placed in
pQlyetihylerte zip-lock bags, All field samples are kept in a cooler until they are returned to
the laboratory.  These coolers are used eseeJusively tor low level Hg samples-
      Acidified water samples may be stored in Teflon (Nalgene FEP) bottles in the Hg-
free room or refrigerator, Refrigeration at 2°C and freezing at -2Q°C are used for storage of
low tevel Hg samples. Teflon (FEP) bottles and storage of water samptes in an Hg-elean
room or refrigerator is recommended.
      Water samples in Polyetiiyiene (Nalgene LDPE) bottles stored in the Bg-dean room
show high accumulation of Hg (refrigerator stored sample® show minor accumulation of Hg)
and cannot be  used for storage of low level Hg samptes, The plastic leaches mercury into
the samples. This effect is facilitated by acid washing, Mercury accumulated in acid washed
bottles to approximately 70-80 ppt with accumulation in non-swashed bottJes at 15 ppt in 30
days. Samples  having higher levels of mercury (sediment and tissue), storage vessel type
is not as critical,
ANALYTICAL METHODS

CLEAN ROOM

      All glassware, acids, reagents, etc, are stored in the Hg-clean room. It is equipped
with a bank of laminar flow hoods, a  separate water supply and gold-charcoal filter
apparatus, refrigeration unit drying oven, analytical balance, and a "flypaper" covered floor
which is changed when needed,
   Contamination is checked weekly by monitoring  acidified (t%  HCI) replicate water
samples which  are stored open in tie Hg-dean  room. Date  on ttiis quality contonol
monitoring is stored both as an Excel file on computer and as had ropy in a data notebook.
 If significant levels of Hg are found (>20 ppt) fhe source of contamination will be located
and if necessary, gold and charcoal filters will be reconditioned.
                                      C-3
-------
                                                                      Appendix C
                                                                       Revision 1
                                                                   Date: 11/19/97
                                                                     Page 4 of 10
CLEANING PROCEDURES

      Teflon bottles which have been previously used for samples are rinsed three times
with DIW and filled witti 125 ml of 1 % HCI, To this, 1 ml of mixed brominating agent (see
reagent section for preparation) for every 50 ml erf acid water is added and the bottle is
shaken, This miindtyre remains in the bottles until it is used. Prior to using these bottles 500
jjl of hydrt»cylamine nydrochloride is added to remove all free bromine. The bottle, bottle
fnouiii and cap are then  rinsed three times in DIW. Reusable teflon bottles (used  for
standards) are not rinsed.
      Reusable laboratory glassware (graduating cylinders) are rinsed three times with
DIW, The volumetric flask used for making up the  primary standard, and  reagent storage
bottles are not rinsed.
      Sediment cups, 20 ml scintillation vials (both plastic and  glass) are non-reusabJe
and discarded.
WATER SAMPLE PREPARATION FOR Hg ANALYSIS

      Water samples may be analyzed for inorganic Hg and for total Hg. For inorganic Hg
analysis samples are acidified as mentioned above and  are  then  ready  for analysis,
Samples to be analyzed for total mercury are prepared using the following reagents:

REAGENTS

1) Mercury-free Water

      Tap water is first filtered through a Culligan system consisting of activated charcoal
and two mixed bed ion exchange cartridges and then piped to the mercury-clean room.  It is
then passed through a Bamstead Mega-ohm B Pure system. This system is fitted with two
fitters (Ttiermolvne; colloid/organic-D0835, and ultrapure-DQ8Q9)  in line with A 0,22 micron
pleated  particle filter.   Mercury  levels  are  not detectable by both  our methods  and
independent laboratory analysis {<0.1 ppt). The only water available for use in the Hg
laboratory is (his Hg-free water.  All reference to DIW in Biis SOP should be assumed to be
Hg-free water as described above.

2) Bromination reagents;

0,1 M Potassium Brornate:
Heat 8.385 g KBrOa overnight in a glass scintillation vial (IQmble 74511) at 250°C ± 20°C in
a furnace to remove mercury.  After cooling dissolve the potassium bromate in 500 ml of
deionized water and store in a borosilicate bottle.  Prepare weekly.

0,2 M Potassium Bromide:
Heat 11.9 g KBr overnight in a glass scintillation  vial at 250°C ± 20°C to remove mercury.
After cooling dissolve the potassium bromide in  500 ml of deionized water and store  in a
                                       C-4
-------
                                                                    Appendix C
                                                                     Revision 1
                                                                  Date: 11/19^7
                                                                   Page 5 of 10
borostlicate bottle. Prepare weekly.

0,05 M Potassium Bromide (KBr): 0.1 M Potassium Bromate (KBrOa)
Mix equal volumes (100 mi) of bromate and bromide  in a 150  ml screw cap teflon
borosilieate bottle. Prepare daily,

3) Hydroxyfamine Hydrochloric!©
Dissolve 6.0 g of NH20H.HCI in 50 ml of deiooized water in a 60 ml teflon bottle.  Prepare
weekly,

4} Slannous Chloride: To 40 g of Stannous Chloride (SnCb) add 50 ml of 12 N HCI.  Bring
to 2000 ml using Hg-free deionized water in a borosilieate glass bottle. Prepare daily. The
stannous chloride is made Hg-free by purging it with argon for 20 minutes before running
samples. Thereafter, the purging continues throughout fm entire analysis.

5) 12 N HCI: Concentrated HCI (12 N HCI) is poured into a  graduate cylinder which has
been previously add washed and rinsed three times wifri DIW.

6) Wash water 150 ml of concentrated HCI (12N HO) is added to 15 L of DIW in a 15 L
teflon bottle (Nalgene lowboy) and shaken.
DIGESTION OF WATER SAMPLES

   Samples are placed in an ultraviolet cabinet for 12 hours, allowed to cool, and tften
brominated for one tour in the Hg-ctean room,  125 ml of acidified sample (0.625 ml 12 N
HCI is added to each 125 ml sample) is brominated by adding 2.5 nil KBrOafKBr mixed
reagent {as described above, Reagents section #2} to each sample bottle. Then, 500 pi of
hydroxylamine hydroch bride is added to the solution to inhibit further reaction. Samples
are permitted to      for at least 10 min before analysis.
SOILS AND SEDIMENTS (CARBONATE AND CLASTIC)

      Preparation of soil and  sediment samples  is done outside tie  Hg-dean  room.
Sediment samples are homogenized and slurried using a glass bottled btender {which is
cleaned in between samples by rinsing three times with tap water),  120 mi of sediment is
slurried with 50 ml of distilled water.  This mixture is then blended for 3 minutes.  Using a
syringe,  10 ml of slurry are removed, placed in a polyethylene specimen cup and diluted by
adding 40 ml of 5% HCI (The HCI acts to neutralize carbonate sediments prior to digestion.
It is necessary to prevent a violent reaction when the ampule is subsequently sealed and
autoclaved).  After mixing, 1 ml of this solution is transferred to a 10 ml ampule using a
1000 cc syringe (with the tip cut off).  Nitric acid {2 ml cone, HNOs) is added to the ampule
which is left to stand for 20 minutes. The ampule is then sealed and autodaved for 1 hr at
105°C. Ampules must be cooled completely before further processing.
                                      c-5
-------
                                                                    Appendix C
                                                                     Revision 1
                                                                 Date: 11/19/97
                                                                   Page 6 of 10
   To process ampule contents, pipette 0,5 ml erf the digested  solution into a  20 ml
polyethylene scintillation vial (Klmbie # 58504) containing 20 0 ml of 0.12 N HCI solution.
PLANT AND ANIMAL TISSUES

      Animal and plant       are treated the same as sediments.  Initial dilutions of
tromogenate vary with the type of tissue.  In addition tie HCI step used to neutralize
carbonates is not used for tissue analysis. For small fish {such as Gambusia), the entire
fish is weighed, placed in ampules and digested as for sediments. For targe fish (bass and
catfish), using a stainless steel core tube, three 4 mm cores (without      or bones) from
the left fillet are combined and weighed.  The cores are weighed in 10 ml  ampules and
digested as above for sediments.  The weight of tissue sample that is used for analysis is
usually between 0.3 g and 0.4 g. Tissue samples weighing more than 0.4 g tend to explode
the ampules in the autoclave.
DIGESTION OF STANDARD REFERENCE MATERIAL AND SPIKED MATERIAL

      A series of method      have been run both with spiked tissue, spiked sediment,
and NBS or  NIST certified  samples to test for digestion efficiency.  NBS oyster tissue
(566a), NRCG dogfish muscle (DORM-2), NIST sediment nominal 50 ^g (8407) and 60
jjg/g (8406) were used in these tests. In addition, a sample of certified material is digested
and run with each analysis of tissue or sediment Digestion efficiency is between 98-102%
in all cases.

SAMPLE STORAGE AFTER PREPARATION

      Sediment, and tissue samples may be stored in Ihe sealed ampules for an indefinite
period after they have been autoclaved.
STANDARD PREPARATION

   All preparation and storage of working standards  is done in  a Hg-etean  room.
Secondary standard is prepared and stored outside tie Hg-cJean room (because of its high
Hg concentration).  The primary stock standard is made by addition of 100 pi of NBS
certified secondary Hg standard (SEPEX PLHG4-2X) (1000 \jglm\) to deionked water plus
10 ml of trace metal grade HCI, and made up to 1 L in a 1000 ml flask, This standard is
prepared daily.  Working standards are made in 500 ml teflon (FEP) bottles.  For each
working standard, concentrated HCI (5 ml} is added to 495 ml  of deionized water When
acids and brominating agents are added, the external laboratory hood is turned on creating
a negative pressure in the area where acid addition is being done.  The primary stock is
then  brought into the Hg-dean room and depending on final concentration,  the required
amount of primary stock is added to the bottles containing the water-acid mixture. Working
                                     C-6
-------
                                                                     Appendix C
                                                                      Revision 1
                                                                   Date; 11/19/97
                                                                    Page? of 10
standards mm made up daily.
      The working standard used for low level Bo-concentration (e.g. water samples) are
0, 2.5. 5 and 10 ppt. In the 500 mi acid-water mixture, 0, 12.5, 25 and 50 ^1 of the stock are
used respectively. The 5 ppt standard is used as the  continuing calibration standard and
the 1  ppt is run as a low level check, All pipettes,  micropipettes and pipette  tips are
calibration checked before use, using an analytical balance,  The temperature of the clean
room is approximate 21 °C.
Secondary standards  used for tissue and sediment analysis are 0, 100, 250 and 400 ppt.
These required standards are made up in the 500 ml acid-water mixture, using 0, 0.5. 1.25
and 2.0 ml of the secondary standard respectively.  The 250 ppt standard is used as the
continuing calibration standard while the 100 ppt is run as a low level check .
ANALYTICAL INSTRUMENTAL TECHNIQUE

  Cold Vapor Atomic Fluorescence Spectrometry (CVAFS)  is the method  used for Hg
determination.  The system used is a PSA Merlin Plus supplied by Qoestron corporation,
Princeton,  New Jersey 08543.  This system contains an autesanrtpler, vapor generator,
fluorescence monitor, and an IBM-compatible computer system  as tie electronic data
interface.  In the CVAFS method, SnCh is mixed with the liquid sample fed by the auto
sampler, which then enters a gas liquid fritted  separator.   The  sample flows ttirough
peristaltic pump tubing. As mercury enters the vapor phase it is stripped and carried along
a gas stream (Argon- Zero grade) to the detector.  Tha method detection limit (MDL) is
approximately 0,255 ppt  (S.D X 3},  Baseline noise translates into variation of between
0 087-0,185 ppt.
Modifications to the apparatus are:

1} The pump in the hydride generator has been changed to a peristaltic pump.

2) Modification of the computer output using Excel to permit more accurate representation
of tire peak height data,

3} An Omega model FMA-7882 mass flow controller wJth a channel selector  is installed at
the front of the instrument. This flow  controller is used to more accurately  regulate flow
     of the carrier and sheath gas, while the flow controllers on the hydride generator are
open to full capacity.


Procedure for operating the instrument

1) Tighten  the peristaltic pump (pumps wash water, waste water, sample, and stannous
chloride),

                                       C-7
-------
                                                                      Appendix C
                                                                       Revision 1
                                                                   Date: 11/19/9?
                                                                     Page 8 erf 10
2) Turn on the wash water to the system,

3) Tun on the computer,

4) Turn on the gas to the system.  The argon (Zero grade) flow© through two gas purifiers
(charcoal and gold) before reaching the instrument,

5) Turn on the line stabilizer/conditioner,

6) Check to make sure no tubes are crimpeci, and that flow is smooth in all tubes before
proceeding,

7) Check gas flow at the mass flow controller,
Note: For low level Hg-coneentrations tie optimum  level of the carrier gas  has  been
determined to be 0,14 L/min, while the sheath gas level has been optimized at 0,125 Umin.
At higher Hg<»ncentrations the carrier gas is 0.35 Umin, and the sheath gas is 0.2 L/min,

8) Allow the system to run on DlW for 15 minutes.

9) After 15 minutes switch the instrument to SnCb.

10) Note: the sensitivity dial on the instrument is run at highest sensitivity for water but may
be lowered for running of sediment, soil and tissue samples.  This method is adequate for
samptes of the range we have run to date,

11} When the instrument is ready, zero the fluorescence detector and run acidified water (0
ppt)  to  check baseline response of the  instrument and guard  against  unexplained
contamination from reagent preparation.  When peak height of DIW is 
-------
                                                                     Appendix C
                                                                      Revision 1
                                                                   Date: 11H9S7
                                                                    Page 9 of 10
and b represents the contamination by water. The mercury concentration is then obtained
from the standard curve.

Ail reagent blanks are made up to a final volume of 125 ml, The slope obtained from this
curve  give the concentration of mercury  in the reagents.  This number is subtracted from
sample values,

12) Standards, blanks, and high level samples (generally fish, sediments and soil) may  be
run in plastic scintillation vials. Water samples for total-Hg are digested and analyzed in
125 ml teflon bottles. Each 125 ml water sample is analyzed at least three times. Tissue
and sediment samples are run in replicate.  When using the autosampfer, fifty samples
including standards takes approximately 2-1/2 hours. Each sample uses 10 mf of SnCb per
sample. A new standard curve is run when the SnClaX In addition to running a full set of
standards at the beginning of tie analysis for each bottle of stannous chloride, a replicate
of the highest standard and zero ppt are run after every 10 samples,

Note: When sampling from 125 ml teflon bottles, the auto sampler tray is removed and the
connections are modified  to sample only from the right sampling tube. This is done  by
disconnecting the right (internal)  sampling tube as well as the corresponding tube to the
hydride generator and replaced with a longer teflon tube tiat directly connects the sampling
tube to the hydride generator. After every 12 analyses and at the end of the run, the mid-
level and 0 ppt standards are analyzed in duplicate.
Instrument Shutdown:

1) If you are using the results directly from the company supplied computer program, make
sure you have printed and/or saved results, This program does not reliably transfer files to
ascii or Excel although it has functions for these tasks,
2) Replace the SnCb solution with DIW and flush the insttumerrt for 5 minutes.
3) Turn off the wash water,
4) Run ttie pump until no more liquid is present in the pump     tubing,
5) Turn off the gas.
6} Turn off the line stabilizer and the computer.
7) Release tubing in the Hydride generator and peristaltic pump.
8} Check ttre waste water container and empty if necessary.

Computer Procedure:

1) Choose LIBRARY, press select to choose methods and to see methods stored.
2) For ANALYSIS choose "analyze", "batch". Specify batch (sample) size. The computer
will ask  you whether ttre sample tray is in position and if you wish to change the sample
fray.  If you respond "NO" twice, the instrument will then align the sample tray to the run you
have specified.  It will then be necessary to return to the analyze  menu and check batch
etc. you may then respond "YES" to the questions about tray position. This response will
                                       C-9
-------
                                                                     Appendix C
                                                                      Revision 1
                                                                  Date: 11/19/97
                                                                   Page 10 of 10
initiate the run. The instalment will analyze 50 samples. If you have more than 50 samples
you must re-select analyze and you can choose a reference number which reflects the
actual number of sampfes you are running.
3) To run standards,       "CALIBRATION" then select new curve.
DATA TRANSFER

      We do not find the program supplied with the CVAFS          for our needs.
Specifically, the curve fitting function is not adequate for low level samples {< 1 ppi). We
therefore after printing results from the machine, save the     as an asd file and transfer it
into an     spreadsheet

DATA HANDLING

For wafer samples, during each run a sample is spiked with  1 ppt mercury concentration,
The mercury concentration of the sample is then subtracted from the mercury concentration
of the spiked sample. Fish and soil samples are not spiked for total mercury analysis and
the recovery is determined by using NIST reference materials,

THE STANDARD CURVE
Currently the  NIST standard available for Hg is 1000 (ig/ml. With appropriate dilutions,
standards can be made reproducible  to 10  ppt using  standard dilution and pipetting
procedures.  The intercept location in the standard curve calculation becomes critical to
proper  calculation of concentrations.    We  have found  that  the  most  reliable and
reproducible results are generated by running a set of standard pind then checking if the
standard regression is acceptable {linear coefficient >0,S8).  f tie'regression coefficient is
acceptable and the mid-level continuing standards are ± 10% of the expected value, the
curve is dropped parallel through the origin. The peak height units for each sample are
then compared to this new curve  to determine Hg concentration.  This method is used for
water  samples  and  has also  been found to  be comparable  to traditional estimating
procedures used in sediment, soil and tissue analysis.

All data is printed as hard copy and stored on computer disks.  We maintain a back-up
copy for each disk.
                                       C-10
-------
                           APPENDIX D
Laboratory Documentation (Sample Prep Logs, Analytical Analysis, Standard
  Curves, Sample Calculations) for Water, Sediment, and Tissue Samples
-------
     1 PREPARATION Of SIDIMiNT SAMPLES FOR ORGANIC MBlCUW ANALYSIS
NBTM of project
TedYUQift:
Sample
No.



























CupW!
ft)




























WogWof
we*»ed.f^


























Weight o* dry
9Cd. *eup


























We^Mof
(toy sad,.



























Rabooi


























                                                                    No, erf sample*
                                                                    Date of Xknatysis
                                                                        SOP m Date:
                                                                            Bend I25ce of sal with DJ water.


                                                                            Date    Tme    Wl

                                                                            Wagh 5fnL of aiurry and % m dynng
                                                                            oven a( 60' C owinigrit


                                                                            Date    Time     Irm

                                                                            Take out mm and itowte coot
                                                                            Date     TRM    In*
                                                                            Weigri dry teofawrt
                                                                            Date     Tim*    In*
-------
Table  2.  PRE-TREATMENT FOH SEDIMENT ORGAHQMERCTOlf ANALYSIS
Samples:
Technican
           Number of samples:
           Data:
           f
                        2nd.
Ref
Samp. No
                                              W.S
1st
v
2nd
                               Ref
Please do not forget reference stardand.
-------
         SC-RESULTS  FOR
GC rile nane:
CC analysis date:
         ANALYSIS

Pr*treata»nt Dtta:
-------
SOUTHEAST ENVIRONMENTAL RESEARCH PROGRAM
        ORGANIC MERCURY ANALYSIS
            DATA INTEGRATION
Name of pro tec
Technician:

SAMPLE ID


























t:


FILE NAME








!

















No, of samples:
Dale of analysis

METHYL Hq
Aulo int. Manual tfil,




























ETHYL Hg
uto int. Manual iru.

























-------
Sample source:
Technican:
                                                 Sample numbers:
                                                 Prep. Oate:
Reference Stardands:

           amount of 5Pi/uI m^td stardand added-
           amount of CH2CI2 added:
-------

                  SOUTHEAST ENVmQNMiNTAL RiSEARCH PHQGBAM
                           TOTAL MEBCUHY ANALYSIS
NAME OF PROJECT:

DATE OF ANALYSIS:

TECHNICIAN:
                                         MATRIX:
REF. *
SAMPLE ID
DILUTION
                                                 COMMENTS
-------
                SOUTHEAST BJVIHONMOITAL RESEARCH PRQGfiAM
                          TOTAL MERCURY IN WATS
    9 AND REVISION DATE.
NAME OF PROJECT:,
DATE OF PREPARATION:
DATE OF ANALYSIS,
TECHNICIAN:
REF *












A
^F




















^^
^^





SAMPLE 101









































BOTTLE #









































DESCRIPTION









































DIGESTION PROCEDURE

Split water samples into I25ml_ teflon battles
and acidify with QJ25mL 12N HCI, Then place
the samples in ihe ultraviolet caOinet for 12 h.
allow 10 cool. Ihen brominate for 1 h

REAGENTS:

Weigh out 8,3&5g at KBrQ3 and 1 V9q of KBr
Heat overnight «n a muWc furnace at 2SD'C,

Date Time Inrt.

Take out of muffle furnace and allow to cool

Date Time init.

Dissolve each reagent in 001 water and make
yp to a final volume of SOOmL. Store reagents in
borosilicaie Dottles and they last for 1 week,

Dale Time Init.

Mix equit vol. C100mi) of KBrOa and KBr reagents are
and store in a boroalicate totUe. Mate (his daiiy

Date Time Init.

Dissolve I2g Of hydroxytammme hydroctilonde
in irjQmL 001 water, ftAake this weekly
and stare in a borosilicate bottle.

Oate Time Init.

Add Z5mt of mixed reagent io each
sample and digest for t h.

Date Time Init,

After digesting for 1h add 0.5 mL hydraxylamme
hydrochlonde to each sample.
-------
                     SOUTHEAST EIWIRONMENTAL RE^ARCH PROGRAM
                                 TOTAL MERCURY \H FfSH
          RB/IS1QN DATE
          NAME OF PROJECT:
   OF PREPARATION:
:CHNIC1AN:
*MPLEID'	JWT OFFiSHlSEX~
                              LENGTH
COMMENTS
DIGESTION PROCEDURE

Determine ite length and sex of
fisft and weigti in a 10mL glass
ampule.
                                                               Date
                          Time     (nit.
                                                               Add 1ml_ of DDI water in 2mL
                                                               eonc, HNO3, Leave for 20 mm.
                                                               undef the fiood. Then seal.
                                                               Dale
                          'Time
                 Init,
                                                               Place in autoclave in a water-
                                                               laih for 1 Nourai 10S'C.

                                                               Datt     Time    Init,

                                                               Date of analysis:

                                                               Date     Time    Intt.
-------
                       SOUTHEAST ENVIRONMENTAL RESEARCH PRQGfiAM
                                   TOTAL MERCURY IN SOIL
SOP No, AND REVISION DATE.

DATE GF PREPARATION:	,

TECHNICIAN:
SAMPLE
DESCRIPTION
CUP WT |WET WT. 1 DRY
                                                   NAME OF PROJECT
                                                                  DIGESTION PROCEDURE.

                                                                  Blend "125 cc of soil win 01
                                                                  water Add 4SmL of O.SN HC1
                                                                  to SnriL of slurry and leave for th.
                                                                  Date
                                                           Time
                                                                                   Inrt.
                                                                  Take tint of acidified sluny and
                                                                  pipetle into a 10mL glass ampute
                                                                  Add 2mL cone. HNQa, Leave
                                                                  for 20 mirt under ihe hood.
                                                                 Dale
                                                           Time
                                                   Inn
                                                                       SmL of slurry antj dry m
                                                                 drytng oven (80* C) overnight
                                                                 Date
                                                           Time
                                                                 Take out at oven
                                                                 Date
                                                           Time
                                                   M,
                                                   I mi
                                                                 Place in auioclave in a waterdaih
                                                                 for 1  hour at 105" C.
                                                                 Date
                                                           Time
                                                   I nit
-------
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Ref
00 1
002
003
004
005
0O6
007
008
009
010
HQ
Hq
HQ
HQ
Hq
Hq
Hq
Hq
Oil
oo i
002
003
004
005
006
007
OOB
009
010
Oil
O12
'013
014
ots
016
• 017
oia
019
020
021
022
023
024
025
026
027
029
029
030
O31
032
033
034
035
senr to LPTi on n NOV 94
Out-put
0,0
I. 1
0 . 0
IBB. 1
0.0
2.6
0. 1
0.4
144.6
2.S
2,4
2. a
44,5
44.4
91, 8
91.3
141 .6
141.7
1.5
Concentration
0 . Oui.ipp t
0 . OuOpp t
0 , OOOpp t
>30.ppt
0 . OOOpp t
0 . 0«Xipp t
0 . OOOpp t
O.OOOppt
S5.6Sppt
O . OOOpp t
O.OOppt
O.OOppt
1 O.OOppt
1 O.OOppt
20. OOpp t
20 .TOpp t
30. OOpp t
30, OOpp t
^ 0.234ppt
5-4'lf/-i.Ai-l>7lpPt
5.3 -*• 11.054ppt
5,4"
5.3
4.1
5.6 -
4.9*
4.0
1 t.OBOppt
VL'. * . 1 . 053pp t
•- 0.793ppt
- . lM17ppt
' ' 0.97lppt
, 0.76aPpt
6. CM 1.207ppt
0,7-
0.6
0.6-J
Jr^cT^
143. 5J
" 274
2.6
1.2-1
o.oJ
0.2J
0.5-t
1.4
1.3-1
0.3-1
0.2
0,7^
1.3*
2.5
0.3-
• i"4sTr^
i ^^
f. '..v.0.052ppt
* '" 0.034ppt
0.034ppt
31 .Olppt
3O.8lppt
0.415ppt
j(yO.4T7ppt
- 'Y 'o . 16Qpp t
-C|J O.OOOppt
i O.OOOppt
t- :-"''O.014ppt
; t . O,2Olppt
.0.187ppt
": " '''O.QOOppt
: 0 . OOOpp t
O.067ppt
^ y\ O.192ppt
{**' 0.43Bppt
O.OOOppt
v 30.72ppt
,l4iw.B_.,' 30,46ppt
"~2f . a
3,4
O.5O4ppt
0.&31ppt
1 . 4-lt,t _ O.ZOlppt
0 . 9 1 > ; 0 . 094pp t
0,4-1 0 . OOOpp t
Runs
1
I
1
I
I
1
1
i
1
1
I
1
l
I
1
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0 . OOpp t
O.OOppt
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O.OOppt
O.Ouppt
0.00 Q/P
O.OO Q/P
O.OO Q/P
O.Oo Q/P
0.00 Q/P
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0.00 O/P
0,00 0/P
O.OOppt
O.OOppt
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0 . OOpp t
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O.OOppt
O.OOppt
O . OOp p t
0 . oop p t
O.OOppt
O.OOppt
0 . OOpp t
O.OOppt
O.OOppt
Tiine Date
21:45 10 NQV
21:49 10 Nov
21:54 10 MOV- '
22:01 10 NOV •
22;u6 lu Nov '
22: 10 tO Nov •
22:14 10 Nav '
22:18 IO Nov '
22:24 10 Nov <
22:28 10 Nav •
22:32 10 Nov s
22:26 tu Nov !
22:40 IO Nav <
22:44 ID Nov <
'22:49 10 NQV c
22:53 10 Nav £
22:58 10 NQV '
22:03 lO Nov «
23:U9 to NQV (
23: 13 ID NQV <
23: 1Q tO Nov <
23:22 10 Nov '
23:26 10 NQV (
23:30 iu Nov <
23:34 tO Nav (
23:3B ID Nov <
23:42 10 Nov <
23s 46 1O Nav -
23:51 IO Nov *
22:S5 tO NQV '
22:59 10 Nov (
00:05 11 Nov '
00 : It 11 Nov <
00:15 11 Nav
00:19 11 Nav '
OOs 23 11 Nov
00:27 11 Nov
O0;31 11 Nav
00:35 It NQV
00:39 11 Nov
00:42 11 Nov
00:48 It Nav
00:52 li Nov
00:56 11 Nov
01:01 11 Nav
0 1 : 05 11 Nov
01:09 11 Not'
01:15 It Nov
01:20 11 Nov
0 1 : 25 1 i Nov
01:29 11 Nov
01:33 11 Nov
01:37 11 Nav
01:41 11 Nov
-------
::
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75
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02:50
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03:16
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-------
             i  Run
        1     HCJ
leaaj no  Sta  2  Run
        -     HQ
        Std  Z  Run
   -cd 2-     Hg
Heading Std  4  Run
   Std 4     .HQ
                  I Psait Height^     2.4
                    Z, 4-     Q. Ot'po t
                  t Peak' Height=     2.0
                    ~ - a      o.ooppt
                  1 Peal; Heidht=   44 «j
                   *4.5     IO.OOppt
                  i  Peak Height^   44,4
                   **-*     tO,OOppt
         (,,.-                -—••-'-J'PIJI,
     "9  atd 5 Run    1  Peak  Heights   91.8
     iff *^L     H i( _       **•*».      	         *
Std 5     Hg
rfinq Std 6 Run
Sfcd 6     wn
                     91.8      20.00ppt
                    1 Peak  Height-    9;
                     91.S      20.OOppt
        Std 7 Ryn   1 Peak Height=
   Std 7     Hg
     ng std a Run
   Std 8     Hg
                 141.6      30.OOpp t
                 1 Peak Heig.ht=   141.7
                 141,7      30.QOpp t
S
c
e
n
c
        In Mater tlferlln)  Fit  : Least
      1
      2
      3
l.aiB 2.435  B.431
i.aai 2.767  1.5B3
li.BB 44.54  -i.49
ID.UD 44*39  ~9.52
2B.BB 91,76  -8.32
                                 Peak ^rea=   61.0
                                 i    0.00 0/P    22^~2
                                 Pesi  Area=  143,5

                                 Peak Area- 2549.5
                                 i    0.00 U/P   22:4u
                                 Peak Area= J54Z.S
                                 I    0.00 0/P    22:44
                                 Peak  Area= 5265.5
                                 I     0,00 0/P    22:49
                                 Peak  Area= 5236,0
                                 i     0.00 Q/P    22:52
                                 Peak  Areas S1B5.S
                                 I     O.Ou Q/P    22:5d
                                 Peak  Area= 8O87.0
                                 i     O.OO  0/P    22:0'
                                                       •  i.* r •
                                                              ne
                                                                     a
                                             Cane Output  Fit
                                         6. 2i.8i 91.3B -B.42
                                         ?  3B.il 141.5 8.4B1
                                         0  se.ae 141.7 8.441
                                        Linear Curr Coeff=B.999Z
                                        ¥ tntereept=   B,4
                      Concentration ppt         '

                       Printed fr^ji ToucAStone  10  Now 94
                                                 . Oupp t
                                                        iS.d
                                                        23:09
-------
  -11-94
   UTH FLORIDA WATES MANAGEMENT 01 VISION
STRUCTURE SAMPLING
TOTAL M6HCLWY ANALYSIS
WATER SAMPLES COLLECTED NOVEMBER 3 1934
y
30
30
30
30
30
30


SAMPLE
ID
REAGENT
SLANK
A #24


SSA #24


SSA #24

S7#43
FIELD
BLANK
S7#43
FIELD
SLANK
*
WK
X
143,5
143.1
141J
143,1
141.2
141,2

•
P.H.


0
5.4
SJ
5.4
5.3
5.6
*
4.0
4.9
0.0
0.2

1.4
1.3

0.3
0,2
0,7









Hg-CONC
{PPTJ


.14
.12
.14
.12
.18

0.84
1.03
0.00
0.04

0.30
0,27

0.06
0,04
0,1 S

Consist
StdErrc
R Squari
Mo. of 0
Degrees

X Coefflc
StdErt-e
MEAN





1,13

1.15


0.94

0.02


0.28


0,06
                                    Regression Output
                                                             0
                                                       0218B2S
                                                           ERR
                                                             €
                                                             S
                                      S.D.
                                       0.01
                                       0.03
                                       0.09
                                       0.02
                                      0.01
                                             0.2f078B
                                             0.00062S
                                                         JO
                                                      SB
SIS1 #66
                                                     3151
             P.M.   Hg-CONC  MEAN
                     (PPT)
                                                                    0.9
                                                                    0,4
               1.0
               1.4
                                                                    1.0
                                                                    1,6
                       0.19
                       aoe
 0.21
 0,30
                       0.21
                       0.34
                                                                                     0,14
                                                                                     0.25
          0.27
                                                                                             S.D.
                                                                                              O.OS
                                         Q.CJ4
                                                                                              006
                                                                   2.0     0.42
                                                                   1.5     0,32      0,37     O.OS
                                                                   0,1
                                                                   0.4
              1.9
              1.3
0.02
0.08
0.40
0,27
                                                                                    o.as
                                                                                    0.34
                                        0.03
                                                                                             s.oe
                                      0.05
-------
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                                       197,6

                                     Oppfr
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             =i . 37341 Teoi^g:.

             Cone* Output FiC

         i  i.eea 1,442 i.ei

         2  e.floa B.;i8g B.afi

         31 IBB.i 36.7B -2.21

         41 iiB.B 35.31 -5lfe

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                                                      Straiirht Line  ^

                                                      No
                                                                             —''VCfitS
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                                                                            . •ii.---'<-.*^^,
                                                                             *IA-~- i.sjiT;;
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          •:->.••:-.. ,"-^.-'   --"^P
                            IF .
                            .IP-,'
                                               Std  Cone  Output  Fit

                                                6  ^B.B  32.53  -Z.68

                                                7  508,§  iBfi.4 -1.16

                                                  -J5BB-..9  1H7.5 i,H?2

                                               Linear Crr Coeff=1,8003
                               A
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-------
EWRGMiOfS SEDIMENT 3MWl£
      :CTHJ «** AND s&r&um i MI
    V         X
  SOD OX)    17*3
  509,000
  500 ODD    Ht 100
                              Ma trf CO
                              O*gr«w al fHMHam
                                                0009
                                                10,307
                                                 EflH
                                                4.OJO
                                                3000
                                                     ill 0
                                                     ama
3E&MENT SM«KeS
ouiAtauRvtv
3AMP1.ES COLLECTED WAY 1EMM
SAMPLE
        cam.    eoc:   DHJJHOH   COM,   IAMPUE
         I*.H      tppt)   FACTOIl    MMC.   ftT
                                                                                 HORUMJZEGI
                                                                                                          ao
  fl-BL
              08TS
              a.io
                       3,230
                                 u
                                           »00
                                                                            O.O3
                                                                                       31*7
              8,30
                       5,3»     1*8"
3.DO
3.O3

3,«J
                         133
                                 11 SB
                                 11,00
                                           moo
                                               0.807
                                               OJ07

                                               1.317
                                               UI7
                                                                            Q.O2
                                                                            0-02
                                                                                       4B.4B
                                 10.3J
                             MOO    ITU-TIM     0.744
                             3LD3    304 UB     0.744
              33.30
                                 03.30      SOW   1»B19
                                 B3,oi      mm   ia
                                                              0,8
O.O3

0,03
O.C3

0,01
oat

o.oa
0.02
                                                                          i3.it
                                                                          ia at
                                                                                              000
                                                                                                            0,00
                                                                                             o.oo
                                                                                                            3-B3
1400     i3-»»     aeju     »J»
13.5O     14B23     41.10
                                                              O.M7

                                                              OJW
f30

?,ao
7,10
   3TD
              5330
              4T.10     «223
              4fl.OO     45.1M
                                 IMS
         O.B23     1«.*1      SU»
         e.223
                   150-07
                   147.32
                                                              1.334
                                                              1.3J4
                                                  3170.34B     O,121
aura
a.ot
tut
0,03
0.03
                                                                        IW.37
                                                                        IB. TO     110.13

                                                                        t2B.11
                                                                        143.H     !»*•

                                                                        17B.OI
                                                                                        43.7B
                             21.00   1777,7M
                             J1.0D
                                               0,115
                                               Q.113
                                                                          7B.DO
                                                                          TBM
                                                                          71.41
                                                                          OB.fi
                                                                                              2.31
                                3.413
-------
¥ X
SQO.OOQ 166.000
500.000 157.700
500,000 164,500
Regression Output:
Constant
Sid Err of Y Est
fl Squared
No. of Observations
Degrees of Freedom
X Cooffia8ni(s)
Sid En- af Coot.
SAMPLE P.H.
I.D,
69 SJO
5.70
96 19,10
I fl. 70
1 130 11.40
" 11,30
144 „ 34. tO
33.30
111 3460
39.OO
133 71.00
70.70
103 10,70
11.10
STD 36.200
35.700
CQRH.
P.H
4,625
4,625
16.225
17.825
10.525
1Q.4SS
33225
32.425
33,925
38J2S
70.125
69.625
9.825
10.25
35.325
34.825
CONG
(ppt)
1482
14,82
S5.§?
S4.74
32.32
32.02
102.03
995fl
104.18
117.08
21S.3S
214.43
30,17
31.40
108.48
106.95
DILUTION
FACTOR
20.00
2000
20.00
20.00
20.00
20.00
20.00
20,00
20.00
20.00
20.00
20.00
20.00
2000
21.000
21.000
3.071
Q.CWfl
conn.
CQNC.
296.3S1
298.351
1119.379.
1094011
643.445
640303
2G40.i79
1991.543
2083.673
234 1. §37
43Q7.076
4296,650
603.451
€28.01 §
227B.144
2245.898
0.000
13.587
ERR
3.000
2JXJO

SAMPLE
WT. GRM
3.681
3.681
0.551
0.551
1 096
1.096
2.0B2
2.0B2
.5.837
f.837
S.942
5.942
1.690
1.690
0.113
0.113


ragHg/g sed
(ppb)
0,07
0,07
0.01
0.01
0.02
0.02
0.04
0.04
0,12
Q.t2
0.12
0.12
0,03
0.03



NORMALIZED
WT, (PPB)
12.01
12.08
304,73
298.04
S8.47
87.63
147.02
143.48
S3 55
60. IB
108.73
108.26
3.56
55.74
60.268
59.415


MEAN
i2.ee
301 .39
38.05
145.25
56.86
108.50
54.65
59.84
-------
 TOTAL MERCURY ANALYSIS
 EPA SEDIMENT SAMPLES

 CANAL SURVEY - MAY 1994            CANAL SURVEY - SEPTEMBER 1 i94

 SAMPLE   MEAN     S.D            SAMPLE   MEAN     SO
    ID                                  ID

      iS    49.49      0.00               103    54.65      1.09
      62   136.48      7.34               118    lijfi      3.31
      67    28.21      3.66             "  130    aa.OS      0.42
      68    S8.i4      2.83               133   100,50      0,23
      69    12.GB      0.00               144   145,25      1.77
      83   196.13      0.44
      i§    28.32      0.00
      93   176.65      1,36
      96   301.39      3,34             STD      69,1 fl      7.17
      97    41.55      Z21
      99    13.61      0.00
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-------
                                PeaJe Report
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-------
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-------
                                PeaJc Report
Time     16:4is33                                      ®ate    1/28/1997
  ta Pile; 2IJAH1S
 ethod File;

                               Gh 1 Detactor:


NUMBER    RET. TIME      MffiA        HEISHT     IDENTIFIER   CONCEHTR&T1ON

  1       00:00:56     4-755E+05    2.228E+04
  2       OOs02:13     4.067E*Qi    2.22SE+05
  3       00:03:20     1.665E+06    9.162E-I-04
  4       00:05:11     1.27824-05    1.227EHH14
  S       00:05:38     4.S31E+04    1.600E+O4
  6       00:OfS24     1.637E+05    S.975E+03
-------
Tina        : 16 Ml; 33
Data File   : 28JSS16
Method File :
                       Data i/aa/lii?
                 at: i
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                                                         €3;  0.25
-------
         16:41:33
  ta File: 2SJAH16
       file:
                                Peat Report
                                                       Date
                                                     1/2S/1§§7
                              Ch  l Detector:
NOMBEB

  1
  2
  3
  4
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  6
  7
  8
  §
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 11
RET. TIME
AREA
HEIGHT
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00:00:56
00:02:13
00:03:20
00:03: 59
00:05:11
00:05:38
00:06:10
00:06:35
00:08:17
00:08:43
00:09:24
4.778E+OS
4.067E-HOG
1.833E+06
3.034E-I-OS
1.142E405
3.317E-HJS
1.241E+05
2.323E+05
8.190E+Q4
1.994E+05
1.612E+OS
2.237E4-04
2.228E+OS
9.514E+04
1.384E+04
1.227E+04
2.026E+04
1.69SE+04
1.505E+04
9.030E+03
1.244E+04
1.013E404
-------
              Original  Research  Papers
                                  L^*»'_ t..~a,	.,„
Analysis  of Organomercury Compounds  in Sediments  by
Capillary GC  with Atomic  Fluorescence  Detection
Azatm Alii1-21, Rirfotf Jaffa2'31, and Ronald Jones''4K
Florida Inlemalional University, University Par*;. Miami. Florida 33199. USA


Key Wordsi

Qrganamercury compounds
Capillary GC
Atomic fluorescence detection
Summary

Analysis of methyl- and ethylmereury {MM and EM) haltdes in bio
logical and environmental samples is generally performed by gas
ehrenwlography with electron capture detection. Tedious sample
work-up protocols and poor chromatograptibc response (using
packed columns) tisve, however, shown the need tor the develop-
ment of new methods in this field.

This paper reports a sensitive method, free from these deficiencies.
lot the determination of methyl- and ethylmercury. The organomer-
cury compounds {MM and EM) are first released from me sample
matrix,  by the combined action of acidic potassium bromide and
cupric ions, and then extracted Into dlcMoromethane. The initial
extracts are subjected to ihiosullaie cleen-up and the organomer-
cury species ire isolated as thetr chloride derivatives by addition of
cupric chloride, and subsequent extraction into a small volume at
organic solvent. Capillary GC coupled with atomic fluorescence
detection provided excellent separation efficiencies for methyl- and
elhylmeregry and proved to be a very selective and sensitive tech-
nique The absolute detection limit lor both MM and EM was found
10 toe 0,2 pg.
1 Introduction

Mercury is a widely distributed environmental pollutant. Its oigantc
compounds, particularly methylmercury. are lar more toae than
elemental mercury or its inorganic salts |l,2|. Such widespread
hazaid and toxioological concern have stimulated a great, demand
for reliable, precise, and sensitive methods for the determination of
organomercury (MM and EM) compounds in water, sediments, fish,
and other biological samples.

The analytical technique most commonly used for determination of
organomercury compounds is gas chromatography using electron
capture detection (GC-ECD} |l-11[. with or without prior deiwau-
zatmn of the mercury compounds. Other techniques involve den-
vatizacjon by butyration |12,13], aqueous phase ethylation [I4-16|,
or hydridizatjon [17.181, coupled with microwave-induced plasma
{MTPJ [10,12,13,19-22[. atomic absorption [14,16,23-2?'], or atomic
fluorescence 115,28,29] detection Most of the chromatographic
methods reported have  ysed packed columns 15,7.8,10,11.16]  A
wide variety of stationary phases have been recommended for use


J Southeast Environmental Research Program
"' Determent a( Chemistry
* tanking Water Research Center
11 Deparunenr. ol Biological Sciences
[is organic mercury analysis, but many o! these have shown one or
more deficiencies 1 17, 1 1 -13[
(a) moderate to severe peak tailing;

(b) poor column efficiency which often leads to problems  with
interferences,

(e'S pooi and often variable response to MM ana EM, and

(d) leducerf peak areas (or heights) of MM and EM from sediment
or fish extracts, despite good responses from standards prior to
       ol sample extracts
       [ll| investigated this undesirable behavior in detail and
proposed 'passivation' o( the packed column, pnor to analytical
measurements, by use of a concentrated solution of metemy(H)
chlonde in benzene (later replaced by toluene) [12| The passivation
procedure must, unfortunately, be repealed frequently as the bene-
fits or the conditioning gradually dimmish, and the onset of ion-nx-
chanqe and adsorption processes prevents satisfactory eluiion of
the mercury species [1,11,13] The injection of largo amounts of
mercury(ll) chloride has several other drawbacks 1 1 ]

{a) gradual and irreversible contamination ot election capture de-
tectors;

{b) rapid deterioration ol the performance of the column; and

(c) long penods during which no analysis can he performed

This report descnbes a procedure loi the analysis of organic mer-
cury which successfully addresses the above ehrornalographic
drawbacks. The method, a modification of the procedure developed
by Cappon and Smith 15], employs a non- polar capillary column lor
hjghei separation efficiency.  The initial extracts are subjected to
sodium Lhiosulfate clean-up  pnor to  GC analysis with a highly
sensitive atomic fluorescence detector system.

2 Experimental

2,1 Simple Preparation

Sediment samples (from a freshwater marsh, Everglades National
Park, Flonda, USA) were collected in non-sterile, wide- mouth speci-
men cups (125 mL, Fishdr Scientific) and those not analyzed imme-
diately were frozen at -20 °C to preserve the samples' chemical
integnty. Each sample was homogenized with distilled water (30-
50 mL) fci 3 mui  at high speed,  using a blender (Qstenzer), to s
uniform consistency.
Journal ol High Resolution Chroma!CHjraphy
                          VOL. 17, NOViM86R 1994   745
-------
 Analysis of Qn^nomercury Compounds in Sediments by Capillary GC with AFD
 2,2 Procadtm

 A portion (1.0-5.0 g) of the homogenized sample was placed in a
 20 mL boroalicate glass sontiUanon vial (KinibJe #74511). Distilled
 water (S mL)» Mowed by copper sulfate {1.0 M: 3,0 mL) and acidic
 potassium bromide solution {10 mL) were added and the mixture
 was shaken for 1 h at 330 rpm (Gyratory Shaioer Model G2), Dichfo-
 fomethane (5 mL) was added and the mixture shaken for 12 h ai
 330 rpm and then centrifuged for 10 rnin at 5000 g uj a Sorvall Model
 EC-S refrigerated centrifuge (Dupont), An exactly known volume of
 the didtJorornelhine layer (3.5-4.0 mL) was transferred to a 7.0 mL
 borostiicaie glass scintillation vial {Fisher Scientific #0333725) and
 sodium ihiosuiJate solution (0.01 M; 1,0 mL) was added.. The mixture
 was shaken for 20 inin at 330 rpm and centrifuged at high speed in
 a EC  clinical centrifuge The aqueous layer (0.9 mL) was placed in
 a 2.0 mL microcentrifuge tube (Fisherbrand, Fisher Scientific), and
••> copper chionde (0.5 M; 0.3 mL) and dichJoTometfaarie (0.3 mL) were
 added. The contents were mixed for 1 min on a Vortex Geme mixer
 and oentnfuged for 2 min at high speed in a Hermte centrifuge. The
 dichtoromethane was  transferred to a 2,0 mL glass sampling vial
 containing a few crystals of anhydrous sodium sulfate and submit-
 ted for GC analysis using 5,0 uL injections,  Samples spiked with
 known concentrations of methyl- and ettrylmercury were extracted
 to evaluate the recovery facior used for quantification

 2.3 Analysis and Instrumentation

 A schematic diagram of the GC-AFS system used in this work ts
 presented in Figure 1. Chiomarography was performed with a
 Hewlett • Packard (Model 5890 Senes I) gas chromatograph coupled
 with an  HP (Model 7673) automatic sampler and fitted  with a
 15 m x 0.53 mm i.d (Megabore) fused silica column coated with a
 1 jim film of the non-polai  bonded phase DB-l {J&W Scientific).
 Splitless  injection was employed: the injector  temperature was
 250 "C, The column oven temperature was held at 40 *C for 1 nan
 after injection, programmed at 60 a/min to 140 °C, which was held
 for 3 min. then programmed at 50 "tain to 200 SC which was held
 for 10 mm, The column and make-up flows were 40 and 60 mL/min.
 respectively,
 The column eluate was led through a pyrolyzer (P S, Analytical Ltd,,
 UK) posaoned inside the GC oven, via a 65 cm long deactivated
 fused alica tubing (0.53 mm i,d. J&W Saenofic).  which was con-
 nected to the column with a glass 'press-fit" union 0&W Scientific) :
 the pyrdyaer temperature was 800 *C. The mercury atoms foimed
 in the pyrolysis uwt were transfened, via 0.5 mm i.d. tubing {PER
 Alltech Associates), from the outlet of the deactivated fused silica
 tubing to the iuoreseence detector. The transfer line was passed
 through a small hole in the top of the GC oven to the detector and
 the connections were made with FTFE unions.

 A MerKn Mercury Fluorescence Detector System (AFS). Model
 10,023, (P. 5. AnaiyacalS was used. In operation the sample was fed
 to the detector as a gas which was channelled through a chimney
 past a light source and a photomultiplief tube at nghi angles to each
 other.  The optical assembly was sheathed in a flow of argon
 (300 mL/min).  Efficient isolation of the required exaiaaon and
 emission wavelengths was achieved by means of a specific high
 intensicy mercury lamp source (Cathodeon, Cambridge. UK} and a
 fixed. 254 nm filter,

 The integrate  time was 0.25 s, the  calibration  range  1000 (most
 sensitive), the fine gam 10 ftnajomurn), the recorder output voltage
 1 V, and the damping switch was on (for signal smoothing), A
 real-time chromatographic control and data acquisition  system
 (E-Lab. Version 4. 1 0 R, QMS Tech) was interlaced with the GC and
 AFS detector system, to this work, the detection limit was defined
 as the amount  of mercury giving a peak arei eoual to three Urnes
 the standard deviation of the background signal.
 GBB chramBtographK - atomic Uuoracanca Hpeclrorrwtrlc lyirtmni 1 A, fxr
 Ihim-1B, argon; 2, azygmi **K *, mercury trap; *, maiitur* lr*p; 5, automatic
 sampler;6, injudor;7.column.fl.pfMi'fll:union;9.pyrnryien 10, cl*«ctr»Hted
 1X83 mm Ld, htowi s*iic«; 11, PTFE unions; 12, 0,5 mm Ml. FTFE transfer llna;
 13, alamlc fluorescence detector; 14, E-Lah chromalogrvplik: control Hid data
 acquisition system; 15, mass flow controller Channel A miM*-up, Channel &
 sheath gin.
AM gases were supplied by Lio^iid Carbonic Speciality Gases and
were of zeio grade quality. The camer gas was helium (9&.S95 %),
purified by passage through, first, an oxygen trap, then a mercury
trap (gold-activated carbon} and a moisture trap. Argon (99.9S8 %),
employed as mate-up gas and sheath gas for the AFS, was also
passed through both a moisture trap and a mercury trap before use ,
Its flow was regulated by a mass flow controUet (Omega) equipped
with two channels, channel A (make-up flow) and channel 8 (sheath
gas  flow,  Figure 1),  The mercury trap  was used as a means of
avoiding  deterioration of the detector's signal-to-noise ratio as a
result of possible contamination of the camer and sheath gases.

2.5 Reagents

Distilled, deionized water produced by a Bamstead B-Pure system
was used in all solutions. Certiied ACS grade potassium bromide,
copperd) sutfate, copper© chtonde, aid sodium ttoosulfate (Fisher
Scientific) were used throughout this work. The addle potassium
bromide solution was prepared by dissohring iSOgrn 200 mL water,
Trace metal grade concentrated sulfunc acid (50 mL, Fish« Scien-
tific) was added to 100 mL of water. After cooling to room tempera-
ture  the solutions were mixied and  made up to 1 L with water.
Copper sulfate {1,0 M), copper chloride (0.5 M), and sodium thiosul-
fate  (0,01  M) solutions were pepared by dissolving appropriate
amounts  of the salts in water. All solutions were extracted with
dJchloromethane prior to use.

2J Standards

All mercury standards were purchased from Ultra Scientific. Stock
standard solutions of dumethylmercury, methyl-, and ethylmercury
chionde (DMM, MMC, and EMC) were prepared by dissolving
appropriate amounts of the standards in optima grade methane-!
(Fisher Scientific). These solutions were  stored in dark brown bot-
tles at -10 °C and diluted with dJcftloromethane to  give  working
 746
        VOL. 17, NOVEMBER
                                                                                       Journal of Hiuh Rfisolulion
-------
                                                                                        m Sadim«nts By Capiltaiy GC wrth AFD
  stanciaids of the desired concentrations when required. Under such
  condition, these stock solutions were stable lor several months.


  3 Results and Discussion

  3.1 Chromaiography of Organomnreury Compounds

  In the analysis of organomercury compounds, the denvatizanon
  techniques mvolred can he ome-consumuig and the denvatized
  products may not necessarily reflect the actual concentration of the
  vanous organic mercury speaes native to the simple, fa the aque-
  ous phase ethylation technique, both inorganic mercury {Hg2*} and
  EM are derivatiaed to diMhylmercury and thus the quantification of
  inorganic  mercury and EM  inherent in the  sample can become
  difficult. Another disadvantage is the use of the BCD far detection.
  Evidence for the partial on-column decomposition of MMC has
  been reported (1,11[. This would result in the loss of the electron-
  capturing  moiety which would render the ECD an unsuitable de-
  tEctoi. In addition, mercuric chloride conditioning of the GG column
  is associated with severe drawbacks f 1] and this 'passivation' tech-
  nique is a major limitation of the analytical method. As evidenced
  by these disadvantages,  there is need  for more straightforward
  methods in the analysis of organomercuiy compounds.

 The objectives of this work were to develop a method for the direct
 solvent extraction of oiganornercury compounds  from sediments
 {with diehloromethane} foOowed by GC analysts, This, Iwwever,
 resulted in irreversible GC column problems if no further sample
 clean - up steps were pert armed, A typical chramatogram of tile pure
 mixed mercury standards (DMM, MMC. and EtAQ is shown in
 Figure 2A. Ctearly. the chromatogram  is indicative of excellent
 chromaiogiaphic behavior.

 The flisc injection of a sediment extract (I, e, from sediment acidified
 with acidic potassium bromide and  extracted with  dichlo-
 romethane after addition of copper sutfate}, also resulted in excel-
 lent chromajjographie  behavior for MM and EM present in the
 sample, A  consecutive injection of the same sampte extract re-
 sulted, however, in no detector signal for these compounds and
 ehroinatograms obtained from the sediment samples showed, fur-
 thermore, broad bands eluttng at elevated column temperatures
 (2QQ-25G *G), indicative of the eluQon of high molecular waghl polar
 compounds,
           tMti
                MM
                                                    B
                                               EN
   fl                   la     a	^

                     Retention timm
Figure?
(*) Chromalogram of pure organic ffutfcury standards on new column: OMM,
2.CH pg Hf; MMC, 3.79 ps Wf; BlIC. 2,50 pg Hg. (B) Chroma togram of s*
Mfflpte alter irilosullate clean up (MM, 194S.7 pg Hg/g; EM, 1236.6 pg I
  Interesnngiy, after such column detenoration, injection of the three
  standard compounds PMM, MMC. and EMC) showed  that the
  non-polar compound, DMM, chromatographed without noQeeaCte
  interferences, whereas MMC and EMC were not detected. Column
  bate-out and removal of a short length of as inlet end did not
  improve its efficiency. Once a new column (same stationary phase,
  DB-1} had been installed, however, with the glass liner, deactivated
  fused  silica, and transfer fine unchanged, excellent separation effi-
  ciency was agam obtained for the organic mercury standards, This
  clearly indicates that  the poor chromatogiaphjc response pre-
  viously observed was associated with column detenoratwn and not
 with the injection or detectoi ends of the GC-AFB system. It seems
 likely that there is strong interaction of the polar organomerciuy
 compounds with high molecular weight compounds {possibly con-
 taining sulfur) which have interacted with the stationary phase As
 will be shown below, these interferences could be removed from
 the sample matrix by use of a thiosuKate ctean-up step.

 Sodium thiosuOfaie has a high complexmg affinity for organic mer-
 cury !5rS,33] and can provide rapd dean-up of the initial extracts.
 Figure 21 shows a typical chromatogiafn from a sediment extract
 subjected to sodium thiosulJate dean-up, Note that both MM and
 EM were efficieniiy separated. DMM cannot be adequately ana-
 lyzed by methods relying on low pH eMiaction/preseivation. since
 strongly acidic conditions convert DMM to MM. This explains the
 absence of DMM to Figure 2B; it is unrelated to the thiosulfate
 ctean-up proceduie, With this sampte pretreatment, the  column
 was used routinely for several months with no  apparent loss m
 efficiency. The cdumn.efflciency and detection lirrute for dimethyl-
 mercury, methyl-, and ethylmerciny species under the optimized
 GC-AFS conditions are shown in Table I

 Table 1
 Comparison at column emciencics and detection limits for DMM,
 MMC, and EMC determined by GC-AFS.
Analyte

DMM
MMC
EMC
^]±SD
[min|
3.38 ±0,0
6J2±O.Q4
7.32 ±0.03
W^
[min|
0.13
0.25
0.23
nfti*
InT'l
271
200
391
D.I*
[pal
0.3
0.2
0.2
" Retention turn
M Piak width at hall msHmum height.
a NumtK* ol Oieoretiral platts pet unit length, a = 5.S4EH W *W,^
111 Datecttnn torot


Using the ttriosulate ctean-up pro«dure. no roercunc chlonde
conditioning is necessary and thus the limitations imposed by this
process are avoided. In addition, the employment of mercury fluo-
rescence detection overcomes the inefficient detection of meicury.
characteristic of the ECD, which results from partial on-column
decomposition of methylmencury chtonde. With this analytical
method the organic meicury species {commonly MM and EM)
present in a sample can be acoaately determined and quantiried
This is a major advantage ovw the ethylation technique where the
quanttfcattan of EM becomes difficult.

3.2 Quantification and Analysis

Quantitative data were obtained using calibration curves (peak area
against concentration of organomeratry chloride  in piccgrams of
mercury (pg Hg) per 5 jii injection} generated daily using standard
solutions of methyl- and ethylmeicury chlorides. The relative stand-
      D) High
                                                                                          VOL. 17. NOVEMBER 1994   747
-------
 Analysis of Orqanomercury Compounds in Sediments by Capillary GC wiih AFD
 aid dananon erf the signal for a 3.16 pg Hg/5 pL standard was 1.5 %
 lor peak area measurements (fi = 3), The calibraDtsi curves gener-
 ated were linear between at least 0 and 4 pg Hg/5 uL. AB sediment
 samples analyzed in this.study fell within this linear range. Linear
 conetoeffl eoeffiaente (/l] for the calbratian curves were 0.938 and
 O.S99 for MMC and EMC lespecavely.

 Quality control was established by determination of percentage
 recoveries for each sample using surrogates as described below. A
 recovery factor ffl} which vaned between 45 and 65 % for methyl-
 mercujy and SO and 80 % for ethylmercuiy was used in the calcu-
 lations to  compensate for  losses erf the analvtes during sample
 preparation. R was determined for each sample by analyzing  an
 eqmvalent imount of the same sample spUffid with a known amount
 of methyl- and erhylmercury and determining the fraction of each
 compound recovered. It is necessary to determine an I? value  for
 each sample since  this is influenced by differences in sample ma-
 trices which affect  the partitioning of organornercuiy compounds
 [18,32.34|.

 4 Conclusion

 This ehrorriatographtc tecnmgue for the analysis of oiganomercuiy
 compounds involves no prederivatizanon of the analytes. aid or-
 ganic mercury species present in the. samples  can be accurately
 determined,  In addition, the absolute detection tats ware 0,3 pg
 foi dimeihyimercury and 0.2 pg for methyl* and ethylmereury; these
 figures are ca four times belter than those obtained with existing
 methods, Direct analysis, /.a without sample clean-up,  of dJchb-
 romethane extracts of sediment samples from Everglades National
 Park confirmed previous reports  11.7,11] of severe deterioration of
 the  GC column; this  resulted in complete loss of efficiency for
 organic mercury chJondes after only a few injections, Use of the
 thiosuHate back-extraction step  described above,  however, suc-
 cessfully removed matrix interferences, enabling routine analysis of
 organomercury compounds with no detectable loss of column effi-
 ciency.

 Acknowledgement

 This wortt was supported by trie United Slats Enwironmintal Protection
 Agency and Everglades National Park through coopeiativeagreement CA-
 5280-1-9016,
 References
 II]  E. Ruhr. HA. Loretao, C. Casaui. AM. Cam. and R. Qua, J Cteomaiogi. 605
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 121  G. W flrysn and IV J, Lanpston. EIWIW ftjJUit 7B11992) 89
|3|  J.F Uilie, J. S&eexm, and B Cnli J. ASSK. Oil. Anal Can SS < 19733 583.
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iSl  C.JCw*»n and J Carom. Anal Chem.4»ri9(771 365

IS]  S.C. Wgfliand SG Capar. J ASSPC. Ott. Anal Ctan. « "^j 715

PI  P. Lmsens. C Casus. C. MeuSermn, and W flae^m, J CJircaitogi
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[81  L W Jtajfcs an(t 0 fl Keener. J. Enmon. Ouatty 3 f 1 57* 121

[91  Y.H. Lou and J Mawux, Anal. Cbiim. Acta HI f 1989J Z»

[IQt SC Might 3MM.T.  Cbrcaan. J. Assoc. Oil. Anal, Chem TO 1 1997) 24.

|l II J O'teJfc J. Clkiotnatogr. 239 \\9B2} 433.

1121 E. flutete. D C Bawer. and tV ftecft. Ami Chun. ACM  249 n«l) 545

[131 S. Bulsla, H. Saaetiarg. O.C Baxw, W ftecu D. Elk/wen, and 1*.
|14|  5, fiatJiSOflwute. O.FX. ainsre*, and JH. Wrter, Aftal Chem 58 (1986) 35.

|15|  W. fflocm. Can. J Rsh. .Aquat So. « (I9B91 1 131.

1 16|  S. aspstWHrntasaKi P J. Crag. Ana! Own. Acta 24B rtQSU 563

1 171  M MfcpiMi. F AM F£. flnnetonan. and  0 J, Oton. Ewwor, So, Technai. 2B
   (1992) 1*7
| ti| PI Grasg, D, Mawue, W Osiaft, 0.1.x. fldnaraf. and F. M^mn, Analvst tl? (19921
   323.

|t9| S.C.K. Shorn, H. King, and &.$. Hault. Anal. Chem. 64 (1992J 2«4,

|2D| O.M C7jeeniv9|r and W.1V flan»«, J. Anak. At Sp«K»i 4 (1989) W3

|2l| P. Lansens, M lecmafera. aafl IV. Saiyefts, Waui. Ail. and ScU KilluL 56 (1991)
   IDS.

                                                  Chiin. Acta 234

                    , WStoun-song, nod H. Heflgr^fifA Fiaenius' z Anal. Chcm
|22]  ft iansBjii C. MeuSeinan, M. Leemalseis, mid W
    (1990)417
|23|  J. Guj-d/n, AT.
|24|  Cft ^fanna. J.f. Tyson and S Mciniosta, Anal. Chem, S»fl993t 653

|2o|  H. SaKiiTxita T. Taaaynsu. and N Yaaehava. AtuiJ SLI. a (IKJZi 35

|2S|  E. Muoai, M, Htraguent D. Mm. T. Talcmictu. and M. Goto. Anal Ctam. Acts 23B
|27|  C Saizsonti. C. Sacrtero, M, Aetna. O. AtvBwo. and S. Afentastf. J Oiromatagt.
|Z8|  ff.P SWiftand J.F GampOeiL SsxxOmaam 8 (1993) 10

1291  W. Stan and W RGgefaW, Anal. Chim Acta 10« (1988) 151

|301  D, Grpsen and M Maatop. Water Au, and Soil Pollui 98 U9S II 507.

|31|  M. Mmk W.jtei. Au. and gat FtjlKil SE (1991 
-------
  Anafyoca CMnnre jieto. 22i {1989 > 253-268
       T Bern** Pubtkhtn B.V., AmOteaiMm — Print**
                                                  238
  DETERMINATION OF METHYLMEHCURY IN NATURAL
  WATEKS AT THE SUB-NANQGRAMS PER LITRE LEVEL BY
  CAPILLARY GAS CHROMATOGRAPHY AFTER ADSORBENT
  PRECONCINTRATION                        *"a vrujriw
 Y.H. LEE* and J. MQWRER
 i R*«ivedl 23rd November 1988 )
 SUMMARY
w*.
                           torn Witer „,

                                 ^^-t
                                 it fto. iiuwpfflie Bleiearr,|j.4^J mJ
         with d«*wn-«pta«« dw^tfcn, Tta d.tatiott limit for
 nf I  IB . 44 w«ter urnpk. Four .uriaw
      ^.mtntnltm tetmii th, tw
                                              mid to twl th.
                                           •
        m di&mii nnftn mtw unpla tanged fen 0.68 to §.« ng L-
  In m»nt y*wa, elevated mercury levels, meraiiy being present wainly as
inethylnwniiiy (MeHg), have been observed in &th in remote oligotropiiic
Jakea Inenaaed acidification of the lake water combined with high faiunie con-
tent have been shown to inmasa the MeHg content tether in fiah, woplank-
ton and algae (1-8J.
  Thentore, there bm been a rekindling of Interest in mercury, to ntabluh
why these fiah hmvt elevated Hf concentrationa and to understand how Hg
species are tranBported/transformed in the biogeochenikml eyclt. To be able
to study th« dyninik behivioiur of MeHg in the biogeochemical cycle, the abil-
«y to measure it in natural wtter at the nf 1" l and sub-nf |- " level ia crociaL
I he difficulty in metsurtof MeHf in natural waten in remote anas Uea in
concentrating it from golutton. Most previous aaalytical methods involvt many
M^IS, suffer from poor extraction efficiencies and require targe sample volumes,
  Most of the previous procedures  hive generally used a seltetiv* pweoncen-
ratton treatment followed by m adequately sensitive analytical techniipw (9-
»» J . Extraction with an organic solvent ^benzene or toluene) is the moat pop-
                  0
-------
 260

 ular preconcentration method. However, because the partition coefficient
 MeHg between benzene and water is low,  (ca, 5-10 [9 f), this method ia
 adequate for concentrations <0,S ng I"*1, Several kinds of ion
 lating resins for concentrating MeHg from nat'iral water have also
 ported. Their main functional group is the sulphur donor atom, which._
 the bonding of heavy raetal ions. Owing to their low capacities, relatively
 amounts of resin are required, and because of their strong bonding to Mu
 large volumes of strong eluents such as a strong acid or a chelating agent {
 ourea) are commonly used, often followed by a further concentration using
 extraction method. In addition, pretreatment of the resin before use is gei
 ally required [9,16,18], thereby prolonging the time for sample analysis.
  The aulphydryl cotton fibre  {SCF) adsorbent, produced by introducing
 aulphydryl functional group into natural cotton fibres, is very effective for
 centrating trace amounts of MeHg  [14,20,21 J. Previous work [li.,22]
 onatrated that the use of a small amount of SCF adsorbent for concentra
 MeHg followed by gas chromatography with electron-capture detection  (_
 ECD) permits the measurement of sub-ng 1*"l levels of MeHg in natural watei
 Recently, by the application of capillary GC together with a modified col
 concentration treatment with SCF adsorbent, significant improvements <
 made in the sensitivity of the  method. For mimic-rich water samples a
 stage preconeentrmtion procedure consisting of batch concentration as the fi
 and column concentration as the second stage baa also been developed
 evaluated. These two concentration procedures are compared with respect
 the detection limit and interferences in this paper,

 EXPERIMENTAL

  Methylmereury is preconcentrated from water on to a SCF adsorbent, tb
 the adsorbed MeHg is eluted using a small volume of 2 M HCl and thus aepa-J
 rated from inorganic mercury. Benzene is used to extract methyImercury chic
 ride (MeHgCl) from the eluate and the MeHgCl in the benzene extract ii
 determined  by GC-ECD.

 Handling of the water swnpfe
  Sample collection and handling were done carefully to avoid contaminate
AH glassware used was manufactured of borosilicate or Pyrex glass. New glasa-l
ware was treated with aqua regia. Sample bottles, glass separating funnels and!
 PTFE and siSicone-rubber tolling were leached in 2-4% HCl for at least 24 b-f
Screw-capped sample vials with PTFE-coated septa (2 and 3.5 ml), used fo
benzene extraction, were treated with 10% HCl and thoroughly rinsed and!
leached for  several days in deiomzed water, and before use were rinsed with]
ethanol and acetone and dried at 1§0°C, The fresh water sample (1-4 U
stored in a cold (6e C), dark room after sampling, and analysis was carried oat]
-------
         •$ soon as possible (within 1
         I*? 3*%
        mU. dum,
        Reagents and satuiions
          Stock solutions of MeHeCl
                                                 (2 If) HC!
                                                          wa.
       Synthesis of SCP adsorbent
        The SCP adsorbent was ayntiiesi^j    _j

P
                 D-                          "
    *«-                             .          •• — P^-n^t™
-------
 262
 Pif, 1. Sefamtie diagram tit the column concentration apparatus.
*?
                                        <— SAMPLE
                                          tritnvoiR
                                          i l
                                SCF G«J8E —>
                                10xl« en
                     H*SmTie fflllHR
                     COATCH HITH PTFE
                                                      <— StF
                                                                                  CM
 Fig. 2. Schematic dapmm of tiw batch concentration apoamtu*,
umn. The eluate w^ collected In a 3.5-ml aci«w-capped sample vial with a
PWE-coated septum and shaken vigorously with 0,6 ml of benzine for
The benzene extinct was then analysed % GC-ECD.

Two-stage concentration (butch-column procedure)
  About 2-4 1 of the sample (MeHg concentration >0,OS ng l~l) were tram-
hired Into & Pjrox-glas* vunL After pH adjustment, two pieces of SCF gaui*
weie fi3ted on a cylindrical glass frame and then placed in the middle of the
glass vessel. Thi water was steed for 1.5 h uainf a magnetic stirrer coatwi
withFITE (Pig, 2).
  Fot desorptian of MeHgf the two pieces of SCF gauze were removed from
the glass frame, rinswd with defonized water to wash off my adsorbed humk
substances and packed into a small funnel. After squeezing water fe»m the
adsorbent with a glass rod, 9 ml of 2 M HC1 were used to elute MeHgr then the
adsorbent was rinsed with  ca. 30 ml of deioniased water. The eiuate and the
-------
     solution obtain«f aft* •
                          Pk^ppedwiih-aiw,'
         -» usea to de**..*:  •«:-*—»jr coiunjn *mj _ 0  ua *V*efoctm»i

   ««"i?iS^f'^eS^?*i^i23S3j"'«w
   ^"•fifiS l&Tfi'PUl An d£* II      ^'CJ&ft i*I fTj« T^-*   ^^Jr *^J E^jjft ^fJTtl'l F^tt   •
     ™=«asSaS^ar

  ^^*^1
-------
                 284
                 times of benzene and eiuate, respectively. The extraction efficiency |£)
                 tained from this eiperiiaent when l/Hjo/Vb=3 was a65±0.02 U=25).
                 setting £=0,65 in the equation
                 the partition coefficient (K=MeHgCyMeHiClKj® ) was 5.6, which is
                 close to the value of 6 obtained by Fujlta and Iwashima [9 } for a solution
                 containing L7 M HCI and 30% NaCl.
for
GC analysis                                                   ,  ,   -•
  GC analyses were performed at the highest available detector sensitivity!
detector (attenuation X1). Temperature programming was impossible owing!
to disturbances to the baseline at this low attenuation. Because the highest j
sensitivity of the detector is used, impurities in the solvents and reagents used]
Mid/or those  introduced during sample preparation can easily mask the]
MeHgCl peak. Previously* a packed column had been used (11 ], However, thsj
separation from the solvent pe«k and nearby mterferinf peaks was very poor;]
Baseline separation from the solvent peak and improved separation fern in- •
terferinf petki w«s obtained by using a wide-bore capUtoy column (see li-J
perimental and fig. 3a^b>, The sensitivity was also improved             1
  MeHgCl la eatily decomposed when exposed to active sites on glass and metah
surfaces at etevmted temperature*. Therefore, the injection Uner was ^anued
twice using 10% diehtorodimetbylsilnne in toluene Dewmposition of MeHfCI i
                              Tim*
 Fit 3
 of bmwne atnrt ift*r
 r'M*Hg,
                                     : ( A) 3 4 of staiid«fdb«ii*MM «ihrtiwi. LSnf ml-*MeH|C1
                                                       Ins* GM ««&« «»ter wiitainuig 0-lS
-------
                                                                                            265
.02 (n«25). In-
6, which is very
PI  for a solution
ector sensitivity
mpoasible owing
luse the highest
id reagents used
sastly mask  the
L]. However, the
3 waa veiy poor.
aration from in-
;o]unm (tee Ei-
         metal
itioii of MeHgCl
    even observed on the capillary column. The column could be regenerated
 by successive rinses with hexane, toluene and methanoi.
   The chromatographic separation is shown in fig. 3. The interfering peaks
 on either side of MeHgCl wett suspected to be derived from the HC1 used as
 elueni 5n the preconcentration steps. Attempts were mtde to remove these
 interfering compounds from the HCl, and the best results were obtained by
 extracting freshly prepared 2 M HO several times with benzene.
   Each sample analysis respited about 30 tnin to elute ail the peaks that could
 interfere with a subsequent injection. The ECD response to MeHfCl was linear
 over the range required for these analyses ( 1.5-20 pg) and the correlation coef-
 ficient of the linear regression for the calibration graph waa generally better
 than 0.990. The detection limit waa ca. 0.5-LO pg.
ARafym of artificial and field umter
  In order to measure and contra! the quality of the analytical results with the
methods developed in this study, MeHg waa determined in artificial water sam-
ples, blanks and field water samples spiked with known concentrations of
MeHg.
  To evaluate the two-stage preconcentration method and to compare it with
the column method, several experiments were done to assess the recovery of
methylmercury in artificial waters using both methods. The  concentration
ranges chosen corresponded to those found in fresh water samples. The results
in Table 1 show that MeHg wan quantitatively adsorbed on the absorbent using
the column concentration method. The recovery of the spiked MeHg varied
from 31 to 108% with a standard deviation of 9.3% and a mean value of 95.8%.
The interval estimate of the mean, value was ±8,3% (95% confidence level).
The recovery of spiked MeHg from the two-stage method varied from 4S to
75% and increased with increasing MeHg concentration. Figure 4 shows that

TABLE 1

Recovery of «pjiad mtthylmMrurr in artificial water
                          BMthod
                                       Volum* (1)
                       Mtthylmaneury
                       concratrmtion
               R«covtry(%l
               ( Mean ± 3-D.)
                          Column
             0,1-4

             4
r containing 0.15 Of
0.1-30

0,05
0.1
0.2
OJ
0.4
01
                                                                       (tt-21
                                                                      ,(rt«2)
                                                                71.0±5v6 (n=2)
-------
 266
Fig. 4 Linear reftwmion between rtcovrry of gpilced M*Hg sod M*Hf concentration in j
mur swnptet, HM error bra correspond to standard devwtxma o/mt**u«d Me Hj concent
shcwa in I^bb 1.
the correlation coefficient, ra=sOJ35t is high. The lower recovery eoi
with that of the column method was mainly due to losses of MeHg in the bat
concentration atep.
  The blank was also checked for contributions of MeHg from the reagei
and the method uaed No MeHg was detected in the blank for either method,1!
  For field samples, 2-41 of water were usually used for the determination <
MeHg (> 0.05 Bg l~l). The column method was generally applied for;
with a low content of bumtc substances (dissolved organic carbon < 5 mg T^
or colour <20 tug Pt I~l). The column method was not used for hmnic-
sample waters, aa humic substances may interact on the surface of mineral^
particiea occurring in the colloidal state, resulting in partial or complete block-
age of the column, and tiiey may also produce emulsions during the extraction!
step, making it difficult to separate the small volume (0,6 ml) of benzene ex-1
tract from the aqueous phase. These two problems could be avoided by using]
the two-stage method,
  Table 2 shows that the MeHg concentrations in two surface waters deter-1
mined by use of the two preconcentration methods were within 15% of the]
mean.
  As a cheek on the difference among MeHg determinations ia filtered and]
linfiltered surface waters, two lake waters were examinedTabie 3 shows that]
the MeHg concentrations in the filtered and unfiltered waters were within 15%;
of the mean and the recoveries of spiked MeHg were very close to those ob-
tamed with the artificial waters {see Fig. 4).
  Compared with the column  concentration method, the two-stage concentra-
tion treatment had the disadvantages of a larger number of chemical steps and j
lower yields. However, the two-stage method had less problem with the for-
-------
                                                                                                  267
                                 T.4BLE2
"Hg concentration in wtTidU}
>w*r
          the
 surface
ere within
              dttur- '
              of the
       in filtemd and
ed.Table 3 show* that
itera wen within 15*
    close to those ofa-
 of chemical steps and
        with tbe for-
                            r   TABLES
-------
  268
  Klor AB and EKA and the Battery AssodationK Thanks an* due to E  Km
  JT ™? E-Jf™ for a9«iflta*« with the manuscript and to Mr. Simm* Li *
  Mr. Zifan Xiao for technical asssutanos with the analytical work
  REFERENCES

  2
                       Swedat State ftiwr Bawd, ViDia^. s^tdeo. 1S81 o, M^
  7
  i
                ttdTA H.JBM. BdL Envitat. Cottua. TteioJ^ 27 (IHD20!
                   «W»«ttoH.Bu**«»«irtli§,L«iiton,l9S4,p«iffl
 „  ^•^™*^^Ilm^il^^'^»SctTidiiititMi9(isaiJSB.
 10

 11	—-,«,,

 12  Y.'fttoti.AotiaiSm.Aa*, 74 (1979 MOT?
 13  P.B. Goulden and H J. Anthony, Anal CUn. Arta, 120 (1980) 129,

 m »  ••>«»»!*      ....   ™™*  •••'•W* %*§^>^Mli*( 'Wff % -I-WVV/ V0U |H
 40
 17  J,Y,
 18

                               Chua, A*ti, US (1980)
              o, Y, K«ttd« tnd Y, fflkatt, fat. J,
          *'
                          R«riB|», TtiicaL Environ.
                                                    13 ( 1987} 1S3.
21
                                           180,
22 Y^-^»^H-ilultbeif,Eii¥ho^Ttoi^Cbe^ildiial^
23 A, I vuftldt amd 0- LiDdqviat, Atiwn, Enviroiu IS (1982 > i§!7,
24  G.C,UaM.Q,Yu«BdQ,aWing,AmSdL
                                           , § ( 1904) 47
-------
APPENDIX C:  Data Reviews
-------
EVERGLADES ECOSYSTEM ASSESSMENT
         (PHASE II REMAP)
            Data Review
         May 1999 Sampling
-------
                            Data Review, May 1999 Sampling

                                        Foreward

The data review documents developed by the US Environmental Protection Agency (EPA) as
part of the Investigation of Mercury Contamination in the Florida Everglades Ecosystem and
Everglades Ecosystem Assessment (Phase II REMAP) Project are presented in the Data Review
May 1999 (M4) and September 1999 Sampling (M5) documents.

The Phase II data review determines whether the Data Quality Objectives (DQO) have been
satisfied as outlined in the Quality Assurance Project Plan (QAPP). The M4 and M5 Sampling
results were analyzed to determine whether they met the criteria developed during the planning
phase and whether the total error within the tolerable decision error ranges as specified in the
QAPP to support decisions.

The Data Review, May 1999 Sampling document summarizes the assessments of the critical and
non-critical parameters. Ten percent of the samples were randomly  selected during the validation
process  to characterize the  quality of the data set. Five of the eleven critical parameters are
qualified with a "J". Parameters associated with this qualifier should be considered an estimate
for a number of quality control variances. The results for total phosphorus, total nitrogen, total
organic  carbon in surface water and methylmercury and bulk density in soil should be considered
an estimate based on findings. A table summarizing the critical and non-critical parameters is
enclosed in the Data Review document along with the detailed calculations and criteria for each
selected sample and parameter.
-------
                              TABLE OF CONTENTS
1.     Critical QA/QC Summaries
      la.    SERC
      Ib.   Battelle

2.     Non-Critical QA/QC Summaries
      2a.    SERC
      2b.   Battelle

3.     Critical QA/QC Review
      3 a.   Water-SERC
      3b.   Water - Battelle
      3c.    Soil - SERC
      3d.   Fish - SERC

4.     Interlaboratory Comparisons
-------
CRITICAL QA/QC SUMMARIES
-------







O"s
Os
Os
£>
S
• • 2
a> j§
Ji «
O £H
03 o3
00 PH
§ T3
?£ O
cd +j
CL> '£
00 Q
P*"1 fli
a £
H 13
CL> vo
1 °
QH ' '
" !-H
03 ,O
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•g 2
-2 ^
PH «
^ 1
§ a
M ^3
Q S
oo .S
W fe
M S
•,
"H
o
•9
1
r/i







LengthAVeight |
Total Mercury

c
"B

AFDW
Total Phosphorus
Methyl Mercury
Methyl Mercury
Total Mercury

O





!-S

.





1 1
0-fc
*
s

I
u
o
•     .a  E
                   S    jj

                   I   S
                   c .SP -&


                   "En "En £
                   I  E tt

                   |2 l
                   E? JH o
                   3-5
                   'B >$ '•

                   P  rrt

K                      OJ
                      w '
-------
SERC
-------
EPA SESD South Florida Phase II Dry Season Sampling:  May 1999
Summarized Findings for 10% of the Critical Parameters Reviewed
Total Mercury in Surface Water Analyzed By SERC













Sample ID by QC
Batch
M4-508-SWF
M4-809-SWF
M4-533-SWF
M4-538-SWF
M4-548-SWF
M4-556-SWF
M4-872-SWF
M4-501-SWF
M4-566-SWF
M4-568-SWF
M4-586-SWF
M4-576-SWF
M4-594-SWF
M4-599-SWF


a
«

% ^ ° 1
So -a S S M
*2;_ 1 ^ § -o M
| 2 5 j | £ - g .S
Ctf (U'OB §J  | t I'SQM
SoSuSuu£^^









X
X



S~

2;
_
S
n

•Q
H

^

•o
S
S




X








X
Comments:
1. Samples from 61 stations were analyzed.
2. Results are an average of 3 separate runs.
3. No matrix spikes were reviewed for batches that included samples 568 and 586.
4. Potential matrix effects are indicated for samples 548 and 599 based on matrix spike recoveries.
Footnotes:
" X " Indicates this situation did occur.
-------
EPA SESD South Florida Phase II Dry Season Sampling: May 1999
Summarized Findings for 10% of the Critical Parameters Reviewed
Total Mercury in Fish Analyzed By SERC

Sample ID by QC
Batch
M4-501-FIF
M4-508-FIF
M4-533-FIF
M4-538-FIF
M4-548-FIF
M4-556-FIF
M4-566-FIF
M4-568-FIF
M4-576-FIF
M4-586-FIF
M4-594-FIF
M4-599-FIF
M4-809-FIF
M4-872-FIF
u
S.
Matrix Spike Not Reviewed for I
Data Entry Check Not Noted

"3 _
u -S
1 J 1 J 1 1 5
|||{l|||
E I s « ^ £ 1 (2
M = " 0 (3 B H .3
NO SAMPLE
*
*


*
*
*
* V**
Si! V**

X**
NO SAMPLE



X**
X**
X**
X**
1
5
a
1
i














Comments:
1. Documentation of data entry checked was not reviewed, with the exceptions of 576, 594,
  599, 809, and 872 where documentation of data entry checked was found.
2. QAPP holding times were exceeded for samples 566, 568, 576, 594, 599, 809, and 872.

Footnotes:
" * "  Refer to the Standard Operating Procedures.
" ** " The fish samples were frozen prior to analysis. SERC references a study demonstrating
      no significant loss of analyte for frozen samples exceeding holding times.The study can be provided by FIU upon request.
" X " Indicates this situation did occur.
-------
EPA SESD South Florida Phase II Dry Season Sampling:  May 1999
Summarized Findings for 10% of the Critical Parameters Reviewed
Total Phosphorus in Surface Water Analyzed By SERC









Sample ID by QC
Batch
M4-501-SWF
M4-508-SWF
M4-533-SWF
M4-538-SWF
M4-548-SWF
M4-556-SWF
M4-566-SWF
M4-568-SWF
M4-576-SWF
M4-586-SWF
M4-594-SWF
M4-599-SWF
M4-809-SWF
M4-872-SWF

f
M
£
1 *
I z ,
"5 ** °* .j
5 - 1 1 1
5 » w S «
3 5 i 1 £
i fr 1 5 1
* CM | (2
.B W a Z ™
•B s is >• s
J 3 ^ U 2
g o a u B


j
3 -s
-o S Q 'S
g "3 g -e ^
I ! i 1 i
Ci w « S F
* -i 'S a 1
£ 1 s 1 !
c — = "; -^
"S ™ 3 «
^f § ~ O B
o 3 £ o o
U U PH Z Z
* ** x***
x***
* ** x***
* x***
NO SAMPLE
# x***
# ## x***
# x***
# x***
# x***
# x***
# x***
# x***
# x***











"o
z
1
C5
1

s
H
X
•c
is
'-C
aj
1

X

X

X
X
X
X
X
X
X
X
X
Comments:
1. Blank results included with this batch were >3 times the MDL.
2. The blank results were significantly different (0.021 ppm vs. 0.0081 ppm) in this batch.
3. Holding times were exceeded for samples 501, 533, and 566.
4. Documentation of data entry check was not reviewed, with the exception of 501 where
  documentation of data entry check was verified.

Footnotes:
" * "  Refer to the Standard Operating Procedures.
" ** " Holding time goal only.
" *** " Blanks were reported above the MDL. Lab water was used as the blank water but not in the sample digestion process.
       Procedures have been modified to correct this.
" X " Indicates this situation did occur.
-------
EPA SESD South Florida Phase II Dry Season Sampling: May 1999
Summarized Findings for 10% of the Critical Parameters Reviewed
Total Nitrogen in Surface Water Analyzed By SERC


Sample ID by QC
Batch
M4-501-SWF
M4-508-SWF
M4-533-SWF
M4-538-SWF
M4-548-SWF
M4-556-SWF
M4-568-SWF
M4-576-SWF
M4-586-SWF
M4-594-SWF
M4-599-SWF
M4-566-SWF
M4-809-SWF
M4-872-SWF
^
M
Matrix Spike Not Reviewed for
Data Entry Check Not Noted
Holding Time Exceeded
X * **
X * **
* **
* **
NO SAMPLE
* **
* **
* **
* **
* **
* **
* **
* **
* **

A
« _
u -S
j« +- "£
•o a ! ! 1 | 1
1 s K = -s $ S
1 A | ? 1 1 I
^ ! i ! s f «
^ 2 ° = 'I = 1
h S t i 'i o M
U ^ O C3 £ O O
O P5 O O PH 2 2
X NA X
X X*** NA X
X*** NA
X*** NA

X*** NA
X*** NA X
X*** NA X
X*** NA X
X*** NA X
X*** NA X
X*** NA
X*** NA
X*** NA
1
^
Potential Matrix Effect (Data I











X
X
X
Comments:
1. No matrix spikes, dups/reps, or CCVs were reviewed for batches containing samples 501 and 508.
2. Documentation of data entry check was not reviewed for any samples.
3. QAPP holding time goals were exceeded for all samples analyzed.
4. Blank results for all sample batches, except the batch containing sample 501, were > 3 times the MDL a
  follows: 1/1 blanks included in sample 508 batch; 1/3 blanks included in the sample 533 batch;
  3/3 blanks included in the sample 568 batch and 1/3 blanks included in the sample 566 batch.
5. Correlation coefficients is not applicable is this analysis (blank and one other point curve).
6. A blank correction was used for sample 501.  Sample was diluted with the lab water.
7. Potential matrix effects are indicated for samples 566, 809, and 872 based on matrix spike recoveries.

Footnotes:
" * "  Refer to the Standard Operating Procedures.
" ** " Holding time goal only.
" *** "  Blanks were reported above the MDL. Lab water was used as the blank water but not in the sample digestion process.
       Procedures have been modified to correct this.
" X " Indicates this situation did occur.
-------
EPA SESD South Florida Phase II Dry Season Sampling:  May 1999
Summarized Findings for 10% of the Critical Parameters Reviewed
Total Organic Carbon in Surface Water Analyzed By SERC













Sample ID by QC
Batch
M4-501-SWF
M4-508-SWF
M4-533-SWF
M4-538-SWF
M4-548-SWF
M4-556-SWF
M4-566-SWF
M4-568-SWF
M4-576-SWF
M4-586-SWF
M4-594-SWF
M4-599-SWF
M4-809-SWF
M4-872-SWF

u
"8
M
1
"9
Oi
.1
1
hH
"o
Z
Oi
«
03
X
"E
1




NO













.3
1
^
"o
_r
u
J-
u
£>

•8
n
*
*
*
X



i
u

w ^ *
1 , a 1 ^
S 1 ^ (2 1
Q 'S A ^ 1

•— Ci ^ «*- v
^ *- « - ^
U! 0 g ° *
a Z ™ W -S
S > = li §
o U 5 o «
a u M u u
X
X
X
X




.=
•B 'S
S -, M
« 5 -
I 1 •=
« E 1
'C a .2

*S °" ^
u ^
1 "s. I
'SOB
£ o o
PH Z Z




SAMPLE
*
*
*
*
*
*
*
*
*
X
X
X
X
X
X
X
X
X









?
Z
£.
"
3
"S
S

u
S
td
X
•c
"S
g

c
1














Comments:
1. Holding times were exceeded for all samples.
2. Based on the Sept. 99 technical review of the SERC laboratory, the QA/QC check standards that were being
  used were made in 1998.  Standards should be prepared at least every 2 months.
3. Based on the Sept. 99 technical review of the SERC laboratory, it was noted that sample injection volumes
  were slightly less than was indicated by the setting of the pipette system (~4%).
4. The laboratory comparisons that were performed did show a bias between the two laboratories. It is unknown why the
  laboratory results don't compare, but each laboratory is using a different method and instrument.

Footnotes:
" * "  Refer to the Standard Operating Procedures.
" X "  Indicates this situation did occur.
-------
EPA SESD South Florida Phase II Dry Season Sampling: May 1999
Summarized Findings for 10% of the Critical Parameters Reviewed
Total Phosphorus in Soil Analyzed By SERC











Sample ID by QC
Batch
M4-508-SFF
M4-533-SFF
M4-538-SFF
M4-594-SFF
M4-501-SFF
M4-548-SFF
M4-556-SFF
M4-566-SFF
M4-568-SFF
M4-576-SFF
M4-586-SFF
M4-599-SFF
M4-809-SFF
M4-872-SFF

0
«
« J
•o ,o s —
1 £ » ^ 1

C £ X _ "S "= ^ •« W
If-' j * 1 - 1 a
S | 1 « o f £ 1 * ?
* i i H ? 1 1 I ! 1
cSu g SsZ fe c S" (2
! !• £ p 55 1 1 a a e< 5
S= M = (2r^* o a a
L.^td S^i ®™ 3^
»;.fc_«2>- c |i §™QP3
^L2«oU^o«^oo
pHgnauMuupHZZ
* X
* X
* X
*
*
*
*
*
*
*
*
*
*
*
?
Z
£.
J
^
s
C5
trix Effect (D
C3
§
"3

c
1














Comments:
1. No blank results were reviewed for sample 508 batch.
2. QAPP holding time goals were exceeded for all samples analyzed.
3.1/4 dups analyzed in the sample 594 batch exceeded RPD DQOs.
4.1/9 stds analyzed in the sample 594 batch exceeded %R DQOs.

Footnotes:
" * " Holding time goal only.
" X " Indicates this situation did occur.
-------
EPA SESD South Florida Phase II Dry Season Sampling: May 1999
Summarized Findings for 10% of the Critical Parameters Reviewed
Soil Ash-Free Dry Weight Analyzed By SERC


Sample ID by QC
Batch
M4-501-SFF
M4-508-SFF
M4-533-SFF
M4-538-SFF
M4-548-SFF
M4-556-SFF
M4-566-SFF
M4-568-SFF
M4-576-SFF
M4-586-SFF
M4-594-SFF
M4-599-SFF
M4-809-SFF
M4-872-SFF
1
M A
•s ,o "s
1 £ •s °
§ 1 3 , s
| | 2 | j i J
ii!|J*l!
i t " i i i « i
1-1-3155
s •- H ~ ^ 2 . °




Precision Criteria Not Met
No Dups/Reps Reviewed
No Blanks Reviewed in Batch
X
X





X



I
-------
EPA SESD South Florida Phase II Dry Season Sampling:  May 1999
Summarized Findings for 10% of the Critical Parameters Reviewed
Soil Bulk Density Analyzed By SERC




Sample ID by QC
Batch
M4-508-SFF
M4-533-SFF
M4-538-SFF
M4-594-SFF
M4-501-SFF
M4-548-SFF
M4-556-SFF
M4-566-SFF
M4-568-SFF
M4-576-SFF
M4-586-SFF
M4-599-SFF
M4-809-SFF
M4-872-SFF
1
S f •§ <3
111, | 1
liilsill
^ *- ^ y ^2^ «
^Sow M ^ ^*H ^
I 1 ! I 1 1 5 I
l^-s^i^sS
s -c w -s z 3 . 1
i "1 -S — f* a ^ s
fiSoauSou
















i
"o
03
:cision Criteri
Z
PH
















•g
1
Dups/Reps Ri
o
X
X
X
X
X
X
X
X
X
X
X
X
X
X

•5
3
•d
u
£
a
i
1
1
«
o














X
«
5
&
a
ential Matrix
£














Comments:
1. All project samples for this parameter were analyzed in the same analytical batch.
2. No dups/reps were reviewed for this analytical batch.
Footnotes:
" X " Indicates this situation did occur.
-------
Battelle
-------
EPA SESD South Florida Phase II Dry Season Sampling: May 1999
Summarized Findings for 10% of the Critical Parameters Reviewed
Methylmercury in Surface Water Analyzed By Battelle Laboratory



Sample ID by QC
Batch
M4-500-SWB
M4-538-SWB
M4-556-SWB
M4-566-SWB
M4-576-SWB
M4-809-SWB
M4-901-SWB

^
B
L.
trix Spike Not Reviewed fo
i








ta Entry Check Not Noted
ding Time Exceeded
V Not Reviewed
a a b
*
*
*
*
*


3
nk Result >3 MDL
rr. Coef. Not Reviewed
nnot Reproduce Results Ca
S o a
« O O








cision Criteria Not Met
£








Dups/Reps Reviewed
o








Blanks Reviewed in Batch
o
**
**
**
**
**
* **
* **
"o
Z
S
ential Matrix Effect (Data
(S







Comments:
1. Instrument blanks were not reviewed for any samples.
2. Documentation of data entry check was not reviewed for any samples.

Footnotes:
" * " Refer to the Standard Operating Procedures.
" ** " Method blanks were reported only.
" X " Indicates this situation did occur.
-------
NON-CRITICAL QA/QC SUMMARIES
-------
SERC
-------
Non-Critical Parameters Analyzed by SERC
Review of the May, 1999 (M4) Data Set










Analysis
NH4
NO2
NO3
PO4
CH4
C02
APA
Mineral Content
Diatoms
Pigments
Chlorophyll a
Ethyl Mercury
Supporting Documentation


a
S

a
0
's1
PH
1
X
X
X
X
X
X
X
X
X
**
**
**

•g
(J,
C3
PH

a
5
X
X
X
X
X
X
X
X
X
**
**
**
Laboratory Records


a
0
8

!>
o
Calibrati
X
X
X
X
X
X
NR
NA
X
**
**
**
g
H

Q
a
,0
w
bo

'w
t
X
X
X
X
X
X
X
X
X
**
**
**



T3
N

<
S£
Paramete
X
X
X
X
X
X
X
X
X
**
**
**






13
rg
'a
CO
X
X
X
X
NR
NR
NR
NA
NR
**
**
**




T3
s
3
«
1
f
Q
X
X
X
X
X
X
X
X
NR
**
**
**
So
0
0
c
a
S
C3
s
Instrume
X
X
X
X
X
X
X
X
NR
**
**
**






bo
o

^o

S
CO
1
m
X
X
X
X
X
X
X
X
NR
**
**
**








bo
S
X
X
X
X
X
X
X
X
NR
**
**
**



$
"§
S
S
o
o
y
1
CO
X
X
X
X
NR
NR
NR
X
NR
**
**
**



•.§
§
C3
t5
1
Performc
X
X
X
NR
NR
NR
NR
NR
NR
**
**
**
Footnotes:
" * " Analyses are in the process of being analyzed.
" ** " No analyses required.
"NR" Not Reviewed
" NA " Not Applicable
" X " Indicates this situation did occur.
-------
Battelle
-------
Non-Critical Parameters Analyzed by Battelle Laboratories
Review of the May, 1999 (M4) Data Set











Analysis
Total Mercury (water)
Methylmercury (soil)
Methylmercury (floe)
Methylmercury (periphyton)
Supporting Documentation


a
PH
-^
a
o
Q'
PH
O

X
X
X
X

•§

3
PH

"§
s
a
o
o
a
1
CO
NR
NR
NR
NR

01
0

§
>
W
o
g
1
NR
NR
NR
NR
Footnotes:
"NR" Not Reviewed
" X " Indicates this situation did occur.
-------
CRITICAL QA/QC REVIEW
-------
Water - SERC
-------
Recalculated Results for 10% of the Total Phosphorus in Surface Water Sample Set
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 11/30/99, njs 12/3/99
 J \       /
Checked by jtm 1/6/00
Sample
M4-508-SWF
M4-538-SWF
M4-548-SWF
M4-556-SWF
M4-566-SWF
M4-568-SWF
M4-576-SWF
M4-586-SWF
M4-594-SWF
M4-599-SWF
M4-809-SWF
M4-872-SWF
Sample
UMS
UMS
MS
MS
CCV
CCV
CCV
CCV
CCV
CCV
CCV
M537
M537D
M561
M561D
M574
M574D
M599
M599D
Digestion Blk
Digestion Blk
QC Batch
08-06-99 Channel 2
"
"
"
"
"
"
"
"
"
"
"

"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
Qualifier
Note


NO SAMPLE









Qualifier
Note


"M"
"M"















"**"
"**"
Dilution
1
1

1
1
1
1
1
1
1
1
1
Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Rep
um
1.20
1.08

0.26
0.19
0.31
0.17
0.53
0.49
0.47
0.31
0.30
Rep
um
0.138422
0.133859
1.02088
1.092386
1.493456
1.48841
1.520315
1.520315
1.497409
1.513901
1.483366
0.764442
0.693524
1.877519
1.649798
0.269442
0.267805
0.466677
0.475123
0.586559
0.169684
Base Line
Factor
um
-0.09
-0.09

-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
Base Line
Factor
um
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
-0.09
Peak-
Base Line
um
1.29
1.17

0.35
0.28
0.4
0.26
0.624
0.577
0.556
0.402
0.39
Peak-
Base Line
um
0.228
0.224
1.111
1.182
1.583
1.578
1.610
1.610
1.587
1.604
1.573
0.854
0.784
1.968
1.740
0.359
0.358
0.557
0.565
0.677
0.260
MW
g
31
31

31
31
31
31
31
31
31
31
31
MW
g
31
31
31
31
31
31
31
31
31
31
31
31
31
31
31
31
31
31
31
31
31
Corrected
Peak
*MW
39.99
36.27

10.85
8.68
12.4
8.06
19.344
17.887
17.236
12.462
12.09
Corrected
Peak
*MW
7.08
6.94
34.44
36.65
49.09
48.93
49.92
49.92
49.21
49.72
48.77
26.49
24.29
60.99
53.93
11.14
11.09
17.26
17.52
20.97
8.05
Sample
Results
ppm
0.040
0.036

0.011
0.009
0.012
0.008
0.019
0.018
0.017
0.012
0.012
Sample
Results
ppm
0.00708
0.00694
0.03444
0.03665
0.04909
0.04893
0.04992
0.04992
0.04921
0.04972
0.04877
0.02649
0.02429
0.06099
0.05393
0.01114
0.01109
0.01726
0.01752
0.02097
0.00805
Detection
Limit
ppm
0.0006
0.0006

0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
Detection
Limit*3
ppm
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
No sample was collected
SPK
CONC
(ppm)


0.0401
0.0401
0.05
0.05
0.05
0.05
0.05
0.05
0.05










R%


68.6
74.1
98.17
97.86
99.84
99.84
98.42
99.44
97.55










RPD

2.018

-6.236








8.659

12.285

0.456

-1.506


"**" Blanks were reported above the MDL.  Lab water was used as the blank water but not in the sample digestion process. Procedures have been modified to correct this.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
-------
Recalculated Results for 10% of the Total Phosphorus in Surface Water Sample Set
Analyzed by Florida International University (SERC) for the May 1999 Dry Season  (M4)
Entered by njs 03-06-00
Checked by
Sample
M4-501-SWF
Sample
UMS
UMS
MS
MS
CCV
CCV
CCV
CCV
CCV
Digestion Blk
Digestion Blk Dup

11 -09-99 Channel 1

11 -09-99 Channel 1
"
"
"
"
"
"
"
"
"
"
Qualifier
Note
"H"
Qualifier
Note









"**"
"**"
Dilution
1
Dilution
1
1
1
1
1
1
1
1
1
1
1
Rep
um
2.8344317
Rep
um
0.642113
0.611171
1.885198
1.922837
7.547741
7.94943
7.713398
7.920441
7.810336
0.467208
0.324104
Base Line
Factor
um
-0.45
Base Line
Factor
um
-0.45
-0.45
-0.45
-0.45
-0.45
-0.45
-0.45
-0.45
-0.45
-0.45
-0.45
Peak-
Base Line
um
3.284
Peak-
Base Line
um
1.092
1.061
2.335
2.373
7.998
8.399
8.163
8.370
8.260
0.917
0.774
MW
g
31
MW
g
31
31
31
31
31
31
31
31
31
31
31
Corrected
Peak
*MW
101.817383
Corrected
Peak
*MW
33.86
32.90
72.39
73.56
247.93
260.38
253.07
259.48
256.07
28.43
24.00
Sample
Results
ppm
0.102
Sample
Results
ppm
0.03386
0.03290
0.07239
0.07356
0.24793
0.26038
0.25307
0.25948
0.25607
0.02843
0.02400
Detection
Limit
ppm
0.0006
Detection
Limit*3
ppm
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
Sample was reanalyzed on 11-09-99.
SPK
CONC
(ppm)


0.0401
0.0401
0.25
0.25
0.25
0.25
0.25


R%


98.5
101.4
99.17
104.15
101.23
103.79
102.43


RPD

2.874

-1.599







Sample
M4-533-SWF
Sample
UMS
UMS
MS
MS
CCV
CCV
CCV
CCV
CCV
002b
002b-Duplicate
Digestion Blk
Digestion Blk

11 -08-99 Channel 2

11 -08-99 Channel 2
"
"
"
"
"
"
"
"
"
"
"
"
Qualifier
Note
"H"
Qualifier
Note


"M" (NR)
"M" (NR)







"**"
"**"
Dilution
1
Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
Rep
um
4.15
Rep
um
0.282074
0.309724
0.473718
0.581571
1.458868
1.50171
1.533685
1.541847
1.55805
1.208445
1.21742
0.586559
0.169684
Base Line
Factor
um
0
Base Line
Factor
um
0
0
0
0
0
0
0
0
0
0
0
0
0
Peak-
Base Line
um
4.150
Peak-
Base Line
um
0.282
0.310
0.474
0.582
1.459
1.502
1.534
1.542
1.558
1.208
1.217
0.587
0.170
MW
g
31
MW
g
31
31
31
31
31
31
31
31
31
31
31
31
31
Corrected
Peak
*MW
128.638282
Corrected
Peak
*MW
8.74
9.60
14.69
18.03
45.22
46.55
47.54
47.80
48.30
37.46
37.74
18.18
5.26
Sample
Results
ppm
0.129
Sample
Results
ppm
0.00874
0.00960
0.01469
0.01803
0.04522
0.04655
0.04754
0.04780
0.04830
0.03746
0.03774
0.01818
0.00526
Detection
Limit
ppm
0.0006
Detection
Limit*3
ppm
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
Sample was reanalyzed on 11-09-99.
SPK
CONC
(ppm)


R%


No spike added
No spike added
0.05
0.05
0.05
0.05
0.05




90.45
93.11
95.09
95.59
96.60




RPD

-9.344

-20.440






-0.740


"**" Blanks were reported above the MDL. Lab water was used as the blank water but not in the sample digestion process. Procedures have been modified to correct this.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 15 to 125% range.
"NR" Data was unavaliable for review.
"H"  Analysis digestion performed after holding times have expired.
-------
Recalculated Results for  10% of the Total Nitrogen Sample  Set
Analyzed by Florida International University (SERC) for the May  1999 Dry  Season (M4)
Entered by gtc ll/30/99,njs 12/3/99     Checked byjtm 1/6/00
Sample
M4-501-SWF
Method Blk
CCV
QC CHECK

M4-508-SWF
Method Blk
CCV
QC CHECK

M4-533-SWF
M4-538-SWF
M4-548-SWF
M4-556-SWF
Method Blk
Method Blk
Method Blk
QC CHECK
CCV
CCV
UMS
MS
MSD

M4-568-SWF
M4-576-SWF
M4-586-SWF
M4-594-SWF
M4-599-SWF
QC-599
QC-599-DUP
Method Blk
Method Blk
Method Blk
QC CHECK
QC CHECK
CCV
UMS
MS
MSD

M4-566-SWF
M4-809-SWF
M4-872-SWF
Method Blk
Method Blk
Method Blk
QC CHECK
QC CHECK
CCV
UMS
MS
MSD
Qualifier
Note


"NR"



»**»

"NR"



No Sample


,**,













"DQO"
"DQO"
,**,
,,»»„
uttii











uttii





"M"
"M"
Dilution
1:10




1




1
1

1










1
1
1
1
1
1
1










1
1
1









Repl
uM
172485
48612
Rep 2
uM
171475
38487
Rep 3
uM
151729
28525
Information was not Provided
684703

535115
46700
714826
695739

545591
37807
692031
704954

473656
37454
704188
Information was not Provided

532258
707980

640134
25908
79060
25672
655188
667998
694053
163178
531790
517371

562075
492921
796009
781529
712788
712788
727782
32428
38913
49809
499954
690152
709855
335909
618182
590507

337987
379303
406587
31327
35654
27287
522155
643389
631208
437051
590787
646740

571333
740035

650338
29682
50585
21609
679795
662450
680057
168819
535324
515613

544621
471658
823680
821147
700149
700149
689657
35506
28302
35709
580180
631733
633784
400566
643383
615465

369404
355621
392109
21013
33785
22116
532227
578379
603723
404652
591598
625091

577420
712903

635815
24182
43646
15354
712524
630057
681458
152700
565577
525167

540689
509015
798954
789371
706622
706622
73358
27407
41033
34505
556717
647739
625810
357801
596345
616454

336643
331947
411261
28646
24202
15431
497563
638163
590386
415914
622457
619866
Rep 4
uM







721796










635203









727782







650619












610675



Rep 5
uM







702294










639381









689657







621389












588524



Rep 6
uM







707545










674006









733358







651475












587068



Average
Replicates
uM
165230
38541

695132

518121
40654
707113


560337
720306

642096
26591
57764
20878
682502
653502
685189
161566
544230
519384

549128
491198
806214
797349
711726
706520
496932
31780
36083
40008
545617
656541
648822
364759
619303
607475

348011
355624
403319
26995
31214
21611
517315
619977
601931
419206
601614
630566
Blank
Correction
uM
46842
46842

46842

















































Corrected
Peak
uM
118388
-8301

648290

















































Slope
0.0000029
0.0000029

0.0000029

0.0000029
0.0000029
0.0000029


0.000002958
0.000002958

0.000002958
0.000002958
0.000002958
0.000002958
0.000002958
0.000002958
0.000002958
0.000002958
0.000002958
0.000002958

0.00000335
0.00000335
0.00000335
0.00000335
0.00000335
0.00000335
0.00000335
0.00000335
0.00000335
0.00000335
0.00000335
0.00000335
0.00000335
0.00000335
0.00000335
0.00000335

0.00000344
0.00000344
0.00000344
0.00000344
0.00000344
0.00000344
0.00000344
0.00000344
0.00000344
0.00000344
0.00000344
0.00000344
Average
Replicate
x Slope
0.34
-0.02

1.88

1.50
0.12
2.05


1.66
2.13

1.90
0.08
0.17
0.06
2.02
1.93
2.03
0.48
1.61
1.54

1.84
1.65
2.70
2.67
2.39
2.37
1.67
0.11
0.12
0.13
1.83
2.20
2.18
1.22
2.08
2.04

1.20
1.22
1.39
0.09
0.11
0.07
1.78
2.13
2.07
1.44
2.07
2.17
Dilution
Correction
10
1

1

1
1
1


1
1

1
1
1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1
1
1
1
1
Sample
Results
ppm
3.43
-0.02

1.88

1.50
0.12
2.05


1.66
2.13

1.90
0.08
0.17
0.06
2.02
1.93
2.03
0.48
1.61
1.54

1.84
1.65
2.70
2.67
2.39
2.37
1.67
0.11
0.12
0.13
1.83
2.20
2.18
1.22
2.08
2.04

1.20
1.22
1.39
0.09
0.11
0.07
1.78
2.13
2.07
1.44
2.07
2.17
Detection
Limit
/3 times (ppm)
0.03/0.09
0.03/0.09

0.03/0.09

0.03/0.09
0.03/0.09
0.03/0.09


0.03/0.09
0.03/0.09

0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09

0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09

0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
SPK
CONC
(ppm)



2



2









2
2
2
0
1
1











2
2
2
0
1
1







2
2
2
0
1
1
R%



94.00



102.63









100.9
96.65
101.3

113.2
105.8











91.5
110.1
108.8

85.4
81.4







88.9
106.6
103.5

62.7
72.7
RPD






















4.672







34.831








1.928












-4.699
atrix effect based on matrix spike recovery outside of 75 to l25°-» r^
results are out of the Data Quality Objective/QAPP control limits.
"M"  Analyte exhibits potential
"DQO" Precision and/or Accuracy
"NR" Data was unavailable for review.
"**" Blanks were reported above the MDL. Lab water was used as the blank water but not in the sample digestion process. Procedures have been modified to correct this.
-------
Recalculated Results for 10% of the Total Organic Carbon in Surface Water Sample Set
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 11/30/99, njs 12/3/99
Checked by jtm 1/6/00
Sample
M4-501-SWF
M4-508-SWF
M4-533-SWF
M4-538-SWF
M4-548-SWF
M4-556-SWF
M4-566-SWF
M4-568-SWF
M4-576-SWF
M4-586-SWF
M4-594-SWF
M4-599-SWF
M4-809-SWF
M4-872-SWF
Qualifier
Note
"H"
"H"
"H"
"H"
NO SAMPLE
"H"
"H"
"H"
"H"
"H"
"H"
"H"
"H"
"H"
Dilution
1
1
1
1

1
1
1
1
1
1
1
1
1
Instrument
Result
ppm
40.02
22.54
33.56
40.72

30.59
21.29
22.21
22.73
30.78
26.91
35.08
22.47
22.56
Blank Factor
ppm
0
0
0
0

0
0
0
0
0
0
0
0
0
Sample
Results
ppm
40.02
22.54
33.56
40.72
NA
30.59
21.29
22.21
22.73
30.78
26.91
35.08
22.47
22.56
Detection
Limit
ppm
0.12
0.12
0.12
0.12

0.12
0.12
0.12
0.12
0.12
0.12
0.12
0.12
0.12
Sample
Method Blank
Method Blank
Method Blank
Method Blank
Method Blank
Method Blank
CCV10
CCV5
CCV10
CCV5
CCV10
UMS
UMS
MS
MS
537
537D
561
561D
574
574D
599
599D
894
894D
Qualifier
Note















*
*
*
*
*
*




Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Instrument
Result
ppm
1.05
1.116
1.231
0.993
1.083
0.893
10.82
6.077
10.67
6.149
10.74
7.865
7.789
13.95
13.96






34.63
35.52
27.81
28.83
Blank Factor
ppm
1.061
1.061
1.061
1.061
1.061
1.061
1.061
1.061
1.061
1.061
1.061
1.061
1.061
1.061
1.061






0
0
0
0
Sample
Results
ppm
-0.01
0.06
0.17
-0.07
0.02
-0.17
9.76
5.02
9.61
5.09
9.68
6.80
6.73
12.89
12.90






34.63
35.52
27.81
28.83
Detection
Limit *3
ppm
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
Spike
Cone
(ppm)
0
0
0
0
0
0
10
5
10
5
10


8
8
0
0
0
0
0
0
0
0
0
0
R%






97.59
100.32
96.09
101.76
96.79


76.06
77.14










RPD












1.123

-0.078







-2.537

-3.602
" * " Unable to verify
"H" Analysis digestion performed after holding times have expired.
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 12/1/99, njs 12/3/99          Checked by jtm 1/6/00

Sample
M4-508-SWF-1


M4-508-SWF-2


M4-508-SWF-3


M4-809-SWF-1


M4-809-SWF-2


M4-809-SWF-3


QA-511-SWF-1


QA-511-SWF-2


QA-511-SWF-3


QA-511-SWF-Matrix Spike


Instrament Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-11
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
QC
Batch
BK13EF1
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
Qualifier
Note















































Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Instrument
Reading
Peak Height
Rep 1,2,3
120.10
120.70
115.90
116.90
117.60
119.20
121.20
118.00
122.90
61.10
61.80
60.40
59.60
60.90
60.20
55.10
55.70
57.30
66.10
68.5
67.5
65.90
67.3
66.7
64.70
63.8
65
81.40
81
79.5
2.59
89.10
90.60
88.60
89.60
86.50
91.00
88.60
85.80
90.80
89.70
84.70
89.00
84.60
88.90
96.70
87.60
Method
Reagant Blank
Peak Hieght
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5

4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
4.5
Corrected
Reading
Peak Height
Rep 1,2,3
115.60
116.20
111.40
112.40
113.10
114.70
116.70
113.50
118.40
56.60
57.30
55.90
55.10
56.40
55.70
50.60
51.20
52.80
61.60
64.00
63.00
61.40
62.80
62.20
60.20
59.30
60.50
76.90
76.50
75.00
2.59
84.60
86.10
84.10
85.10
82.00
86.50
84.10
81.30
86.30
85.20
80.20
84.50
80.10
84.40
92.20
83.10

Y ratio
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
18.6
Hg
Concentration
ppt
6.39
6.43
6.16
6.22
6.26
6.34
6.45
6.28
6.55
3.13
3.17
3.09
3.05
3.12
3.08
2.80
2.83
2.92
3.41
3.54
3.48
3.40
3.47
3.44
3.33
3.28
3.35
4.25
4.23
4.15
0.14
4.68
4.76
4.65
4.71
4.54
4.78
4.65
4.50
4.77
4.71
4.44
4.67
4.43
4.67
5.10
4.60
Averaged
Result
ppt


6.33


6.27


6.34


3.13


3.08


3.02


3.40


3.20


3.41


4.21
















4.67
DETECTION
LIMIT/*3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONC
(ppm)



























1
1
1

5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
R%





























80.02

93.59
95.25
93.03
94.14
90.71
95.69
93.03
89.94
95.47
94.25
88.72
93.48
88.61
93.37
102.00
91.93
Standard
Deviation


0.14


0.07


0.13


0.04


0.04


0.14


0.07


0.04


0.08


0.06
















0.20
Relative
Standard
Deviation


2.3


1.0


2.0


1.2


1.2


4.5


2.0


1.2


2.4


1.3
















4.2
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 12/1/99, njs 12/3/99                   Checked by jtm 1/6/00

Sample
M4-533-SWF-1


M4-533-SWF-2


M4-533-SWF-3


M4-538-SWF-1


M4-538-SWF-2


M4-538-SWF-3


QA-532-SWF-1


QA-532-SWF-2


QA-532-SWF-3


QA-532-SWF-Matrix Spike


Instrament Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-11
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
QC
Batch
HG12EF1
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
Qualifier
Note















































Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Instrument
Reading
Peak Height
Rep 1,2,3
39.10
41.90
40.30
42.70
40.20
41.30
37.20
39.20
38.20
57.30
58.10
59.80
55.80
54.30
55.10
59.30
55.70
59.80
58.20
60.4
59
60.10
58.8
62.9
60.20
59.8
60.1
77.00
76.5
78.3
3.07
72.80
73.00
72.90
74.20
68.30
70.60
78.20
72.20
72.80
69.60
77.30
75.50
80.00
76.50
76.10
74.90
Method
Reagant Blank
Peak Hieght
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39

9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
9.39
Corrected
Reading
Peak Height
Rep 1,2,3
29.71
32.51
30.91
33.31
30.81
31.91
27.81
29.81
28.81
47.91
48.71
50.41
46.41
44.91
45.71
49.91
46.31
50.41
48.81
51.01
49.61
50.71
49.41
53.51
50.81
50.41
50.71
67.61
67.11
68.91
3.07
63.41
63.61
63.51
64.81
58.91
61.21
68.81
62.81
63.41
60.21
67.91
66.11
70.61
67.11
66.71
65.51

Y ratio
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
15.7
Hg
Concentration
ppt
1.95
2.13
2.03
2.18
2.02
2.09
1.82
1.95
1.89
3.14
3.19
3.30
3.04
2.94
3.00
3.27
3.03
3.30
3.20
3.34
3.25
3.32
3.24
3.51
3.33
3.30
3.32
4.43
4.40
4.52
0.20
4.16
4.17
4.16
4.25
3.86
4.01
4.51
4.12
4.16
3.95
4.45
4.33
4.63
4.40
4.37
4.29
Averaged
Result
ppt


2.03


2.10


2.01


3.21


2.99


3.14


3.07


3.21


3.31


4.45
















4.24
DETECTION
LIMIT/*3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONC
(ppm)



























1
1
1

5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
R%





























113.51

83.10
83.37
83.23
84.94
77.21
80.22
90.18
82.32
83.10
78.91
89.00
86.64
92.54
87.95
87.43
85.86
Standard
Deviation


0.09


0.08


0.12


0.08


0.05


0.14


0.07


0.14


0.09


0.06
















0.20
Relative
Standard
Deviation


4.5


3.9


5.8


2.6


1.6


4.4


2.4


4.3


2.6


1.4
















4.8
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 12/1/99, njs 12/3/99                         Checked by jtm 1/6/00

Sample
M4-548-SWF-1


M4-548-SWF-2


M4-548-SWF-3


QA-858-SWF-1


QA-858-SWF-2


QA-858-SWF-3


QA-858-SWF-Matrix Spike


Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
QC
Batch
BK25EF1
"
"
"
"
"
"
"
"
HG24EFI
"
"
"
"
"
"
"
"
"
"
"
BK25EF1
"
"
"
"
"
Qualifier
Note









*
*
*
*
*
*
*
*
*
* "M"
* "M"
* "M"






Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Instrument
Reading
Peak Height
Rep 1,2,3
173.70
177.50
181.00
171.70
171.60
164.90
165.80
162.80
162.40
31.40
31.00
31.00
32.60
33.00
34.40
32.30
33.00
34.30
107.90
106.7
108.6
1.37
73.40
74.15
73.35
70.60
72.60
Method
Reagant Blank
Peak Hieght
3.57
3.57
3.57
3.57
3.57
3.57
3.57
3.57
3.57
3.57
3.57
3.57
3.57
3.57
3.57
3.57
3.57
3.57
3.57
3.57
3.57

3.57
3.57
3.57
3.57
3.57
Corrected
Reading
Peak Height
Rep 1,2,3
170.13
173.93
177.43
168.13
168.03
161.33
162.23
159.23
158.83
27.83
27.43
27.43
29.03
29.43
30.83
28.73
29.43
30.73
104.33
103.13
105.03
1.37
69.83
70.58
69.78
67.03
69.03

Y ratio
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
11.4
11.4
11.4
11.4
11.4
11.4
11.4
11.4
11.4
11.4
11.4
11.4
15.2
15.2
15.2
15.2
15.2
15.2
Hg
Concentration
ppt
11.52
11.77
12.01
11.38
11.37
10.92
10.98
10.78
10.75
2.51
2.48
2.48
2.62
2.66
2.78
2.59
2.66
2.77
9.42
9.31
9.48
0.09
4.73
4.78
4.72
4.54
4.67
Averaged
Result
ppt


11.77


11.22


11.28


2.49


2.69


2.62


9.40





4.69
DETECTION
LIMIT/*3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONC
(ppm)


















5
5
5

5
5
5
5
5
R%




















135.69

94.53
95.54
94.46
90.74
93.44
Standard
Deviation


0.25


0.26


0.45


0.02


0.09


0.12


0.09





0.09
Relative
Standard
Deviation


2.1


2.4


4.0


0.8


3.2


4.4


0.9





2.0
"*" A single digestion batch prepared on 5-34-99 was split into two runs. The matrix spike is reported in File HG24EFI and the sample under review is reported in File BK25EFI. The digestion batch demonstrates the digestion process was performed under certain criteria

"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 70 to 130% range.
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 12/1/99, njs 12/3/99                   Checked by jtm 1/6/00

Sample
M4-556-SWF-1


M4-556-SWF-2


M4-556-SWF-3


M4-556-SWF-Matrix Spike


M4-872-SWF-1


M4-872-SWF-2


M4-872-SWF-3


M4-501-SWF-1


M4-501-SWF-2


M4-501-SWF-3


Instrament Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-11
CCV-12
CCV-13
CCV-14
QC
Batch
HG21EF2
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
Qualifier
Note













































Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Instrument
Reading
Peak Height
Rep 1,2,3
51.70
53.60
55.70
53.60
55.80
54.00
53.50
52.40
50.30
143.90
150.90
145.40
39.00
41.70
38.80
35.60
36.00
34.40
36.40
38.50
37.60
300.70
292.50
290.40
293.40
290.00
297.40
296.60
296.30
296.10
2.46
106.50
106.60
109.80
111.10
105.30
105.70
108.10
103.20
110.30
106.60
103.00
106.80
107.60
102.90
Method
Reagant Blank
Peak Hieght
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76

7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
7.76
Corrected
Reading
Peak Height
Rep 1,2,3
43.94
45.84
47.94
45.84
48.04
46.24
45.74
44.64
42.54
136.14
143.14
137.64
31.24
33.94
31.04
27.84
28.24
26.64
28.64
30.74
29.84
292.94
284.74
282.64
285.64
282.24
289.64
288.84
288.54
288.34
2.46
98.74
98.84
102.04
103.34
97.54
97.94
100.34
95.44
102.54
98.84
95.24
99.04
99.84
95.14

Y ratio
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
19.8
Hg
Concentration
ppt
2.28
2.38
2.49
2.38
2.50
2.40
2.38
2.32
2.21
7.07
7.44
7.15
1.62
1.76
1.61
1.45
1.47
1.38
1.49
1.60
1.55
15.22
14.79
14.69
14.84
14.67
15.05
15.01
14.99
14.98
0.13
5.13
5.14
5.30
5.37
5.07
5.09
5.21
4.96
5.33
5.14
4.95
5.15
5.19
4.94
Averaged
Result
ppt


2.39


2.43


2.37


7.22


1.67


1.43


1.55


14.90


14.85


14.92














5.14
DETECTION
LIMIT/*3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONC
(ppm)









5
5
5



















5
5
5
5
5
5
5
5
5
5
5
5
5
5
R%











96.99



















102.61
102.71
106.04
107.39
101.36
101.78
104.27
99.18
106.56
102.71
98.97
102.92
103.75
98.87
Standard
Deviation


0.10


0.06


0.09


0.19


0.08


0.04


0.12


0.28


0.19


0.18














0.14
Relative
Standard
Deviation


4.4


2.5


3.9


2.7


5.0


3.0


7.4


1.9


1.3


1.2














2.6
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 12/1/99, njs 12/3/99                   Checked by jtm 1/6/00

Sample
M4-566-SWF-1


M4-566-SWF-2


M4-566-SWF-3


M4-566-SFW-Matrix Spike


Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
QC
Batch
HG20EF1
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
Qualifier
Note























Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Instrument
Reading
Peak Height
Rep 1,2,3
22.60
24.90
24.40
23.00
22.80
22.50
23.80
23.20
23.70
90.90
97.40
97.80
3.35
68.60
69.40
63.60
65.00
63.60
65.00
65.80
63.20
64.80
64.40
Method
Reagant Blank
Peak Hieght
2.28
2.28
2.28
2.28
2.28
2.28
2.28
2.28
2.28
2.28
2.28
2.28

2.28
2.28
2.28
2.28
2.28
2.28
2.28
2.28
2.28
2.28
Corrected
Reading
Peak Height
Rep 1,2,3
20.32
22.62
22.12
20.72
20.52
20.22
21.52
20.92
21.42
88.62
95.12
95.52
3.35
66.32
67.12
61.32
62.72
61.32
62.72
63.52
60.92
62.52
62.12

Y ratio
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
11.7
Hg
Concentration
ppt
1.79
1.99
1.95
1.82
1.80
1.78
1.89
1.84
1.88
7.79
8.36
8.40
0.29
5.83
5.90
5.39
5.52
5.39
5.52
5.59
5.36
5.50
5.46
Averaged
Result
ppt


1.91


1.80


1.86


8.19










5.54
DETECTION
LIMIT/*3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONC
(ppm)









5
5
5

5
5
5
5
5
5
5
5
5
5
R%











126.50

116.63
118.04
107.84
110.30
107.84
110.30
111.71
107.14
109.95
110.90
Standard
Deviation


0.11


0.02


0.07


0.34










0.18
Relative
Standard
Deviation


5.6


1.2


3.9


4.2










3.3
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 12/1/99, njs 12/3/99           Checked by jtm 1/6/00

Sample
M4-568-SWF-1


M4-568-SWF-2


M4-568-SWF-3


M4-586-SWF-1


M4-586-SWF-2


M4-586-SWF-3


No Matrix Spike with Batch
Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-11
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
QC
Batch
HG11EF2
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
Qualifier
Note


















"M" (NR), "*"

















Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Instrument
Reading
Peak Height
Rep 1,2,3
36.4
35.9
35.7
32.7
33.2
29.9
33.2
33
33.5
182.30
182.90
183.40
186.00
185.70
185.90
184.70
180.80
184.10

3.35
79.4
79.5
81.7
78.7
76.7
79
77.3
76.7
74.4
77.1
80.3
81.6
78.7
77.2
73.6
74.7
Method
Reagant Blank
Peak Hieght
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51


4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
4.51
Corrected
Reading
Peak Height
Rep 1,2,3
31.89
31.39
31.19
28.19
28.69
25.39
28.69
28.49
28.99
177.79
178.39
178.89
181.49
181.19
181.39
180.19
176.29
179.59

3.35
74.89
74.99
77.19
74.19
72.19
74.49
72.79
72.19
69.89
72.59
75.79
77.09
74.19
72.69
69.09
70.19

Y ratio
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6

15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
15.6
Hg
Concentration
ppt
2.10
2.07
2.06
1.86
1.89
1.67
1.89
1.88
1.91
11.73
11.76
11.80
11.97
11.95
11.96
11.88
11.63
11.84

0.22
4.94
4.95
5.09
4.89
4.76
4.91
4.80
4.76
4.61
4.79
5.00
5.08
4.89
4.79
4.56
4.63
Averaged
Result
ppt


2.08


1.81


1.93


11.76


11.96


11.84

















4.85
DETECTION
LIMIT/*3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9

0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONC
(ppm)




















5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
R%




















98.78
98.91
101.81
97.85
95.22
98.25
96.01
95.22
92.18
95.74
99.97
101.68
97.85
95.88
91.13
92.58
Standard
Deviation


0.02


0.12


0.13


0.04


0.01


0.12

















0.16
Relative
Standard
Deviation


1.1


6.5


6.9


0.3


0.1


1.0

















3.3
" * " Analyst Error, Sample was not spiked by mistake.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 70 to 130% range.
"NR" Data we--, ruiuvnlmble for review.
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 12/1/99, njs 12/3/99                   Checked by jtm 1/6/00

Sample
M4-576-SWF-1


M4-576-SWF-2


M4-576-SWF-3


M4-576-SWF-Matrix Spike


M4-594-SWF-1


M4-594-SWF-2


M4-594-SWF-3


Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
QC
Batch
HG07EFI
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
Qualifier
Note
































Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Instrument
Reading
Peak Height
Rep 1,2,3
54.40
52.1
54.8
46.10
45.5
46.7
65.60
64.3
63.9
75.80
75
74.2
58.30
60.5
61.6
58.10
57.2
57.1
55.90
55.2
58
0.60
85.60
83.40
92.10
90.40
84.90
85.90
89.40
87.60
84.90
86.20
Method
Reagant Blank
Peak Hieght
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78

6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
6.78
Corrected
Reading
Peak Height
Rep 1,2,3
47.62
45.32
48.02
39.32
38.72
39.92
58.82
57.52
57.12
69.02
68.22
67.42
51.52
53.72
54.82
51.32
50.42
50.32
49.12
48.42
51.22
0.60
78.82
76.62
85.32
83.62
78.12
79.12
82.62
80.82
78.12
79.42

Y ratio
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
17.4
Hg
Concentration
ppt
2.82
2.68
2.84
2.32
2.29
2.36
3.48
3.40
3.38
4.08
4.03
3.99
3.05
3.18
3.24
3.03
2.98
2.98
2.90
2.86
3.03
0.04
4.66
4.53
5.04
4.94
4.62
4.68
4.89
4.78
4.62
4.70
Averaged
Result
ppt


4.14


3.25


2.84


4.03


3.54


3.40


3.03










4.75
DETECTION
LIMIT/*3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONC
(ppm)









1
1
1










5
5
5
5
5
5
5
5
5
5
R%











119.30










93.21
90.61
100.89
98.88
92.38
93.56
97.70
95.57
92.38
93.92
Standard
Deviation


0.09


0.04


0.48


0.05


0.10


0.03


0.12










0.16
Relative
Standard
Deviation


2.1


1.1


16.9


1.2


2.8


1.0


4.0










3.5
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 12/1/99, njs 12/3/99           Checked by jtm 1/6/00

Sample
M4-599-SWF-1


M4-599-SWF-2


M4-599-SWF-3


M4-599-SWF-Matrix Spike


Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-11
CCV-12
CCV-13
CCV-14
QC
Batch
HG10EF1
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
Qualifier
Note









"M"
"M"
"M"















Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Instrument
Reading
Peak Height
Rep 1,2,3
44.00
43.50
42.80
43.80
40.00
44.40
45.20
42.80
43.60
61.20
63.6
64.1
4.44
81.50
80.90
83.50
83.70
82.80
80.10
75.10
72.50
81.60
78.10
79.50
79.50
80.90
79.90
Method
Reagant Blank
Peak Hieght
5.28
5.28
5.28
5.28
5.28
5.28
5.28
5.28
5.28
5.28
5.28
5.28

5.28
5.28
5.28
5.28
5.28
5.28
5.28
5.28
5.28
5.28
5.28
5.28
5.28
5.28
Corrected
Reading
Peak Height
Rep 1,2,3
38.72
38.22
37.52
38.52
34.72
39.12
39.92
37.52
38.32
55.92
58.32
58.82
4.44
76.22
75.62
78.22
78.42
77.52
74.82
69.82
67.22
76.32
72.82
74.22
74.22
75.62
74.62

Y ratio
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
15.0
Hg
Concentration
ppt
2.66
2.62
2.57
2.64
2.38
2.68
2.74
2.57
2.63
3.84
4.00
4.03
0.30
5.23
5.19
5.36
5.38
5.32
5.13
4.79
4.61
5.23
4.99
5.09
5.09
5.19
5.12
Averaged
Result
ppt


4.01


3.29


2.61


3.96














5.12
DETECTION
LIMIT/*3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONC
(ppm)









1
1
1

5
5
5
5
5
5
5
5
5
5
5
5
5
5
R%











134.58

104.55
103.73
107.30
107.57
106.34
102.63
95.77
92.21
104.69
99.89
101.81
101.81
103.73
102.36
Standard
Deviation


0.04


0.16


0.08


0.11














0.21
Relative
Standard
Deviation


1.0


5.0


3.2


2.7














4.1
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 70 to 130% range.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                  Station ID  M4-501-SWF     Surface Water
Laboratory Records
Data Report (Attached)
Total P
Total N
TOC
Total Hg
MeHg
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Data Entry Checked by Another
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Blank Spike/CCV Recoveries
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Data Entry Checked by Another
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
5-1 1-99/No Time
5-26-99/1130
11/09/99
X
FW=SW
5-1 1-99/No Time
8-30-99/1646
9-2-99/1623
X
FW=SW
5-1 1-99/No Time
No Digestion
06/13/99

X
FW=SW
5-1 1-99/No Time
05/20/99
05/21/99

X
FW=SW
5-1 1-99/No Time


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.102
ppm
EPA 365.1
Raw Data Initialed
O.OOOSppm (O.Olmnol/L 97)
Injection Vial
Injection Vial
sample aliquot
1:10
3.43
ppm
Antek
Raw Data Initialed
0.03 ppm
NA
4ml
sample aliquot
1
40.02
ppm
EPA415.1
Raw Data Initialed
0.12 ppm
1000ml
1000ml
sample aliquot
1
14.95
ppt
EPA 1631
JL
0.3 ppt
Battelle Lab
is Main Lab



ppt
EPA 1630
JL
0.02 ppt

X
X
Yes
No
X
Past Holding Time Goal
No
X
Past HT
Yes (FLD)
X
Yes
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
By Run Date/ID
**
NR
0.718
100%
95%
0.0006-0.2 ppm
0.997
By Run Date/ID
-0.02 ppm
NR
1 RPD (NR)
95% R (NR)
94%
0.03 and>
NA
By Run Date/ID
No Digestion
Good After Correction
-0.634,-0.9RPD
77% R
96-102%R
0.12 ppm and>
0.999

File ID
X
0.128 ppt 
0.9988

File ID








NA
I!
**
No
Yes

No
Yes
"H"
Yes
Yes



SESD is main lab
                        Notes
                             For TOC analysis, only 2 of 5 duplicate samples run were recorded, due to inability to read the instrument printout.
                             Total Nitrogen analysis: Reported RPD data and Matrix Spike Recoveries could not be reviewed (NR).
                             SESD Laboratory was switched to be the main laboratory for MeHg. FIU is responsible for 10% of the MeHg.
                             ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                             been corrected to demonstrate samples uncontaminated.
-------
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
           Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative (Acid, Temp..)
             Collection Data/Time
               Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
M4-501-SWF Surface Water
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time

In Hg lab Area
None
X
X
Not Noted
Date/No Time

InHg Lab Area

Validation Criteria
NA
"
I!
"
I!
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
X
X
X
Notes on Printouts
X



Notes on Printouts

X
NA
uM
X
X
uM
X
X
ppm
SFW=SWF
X
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) | Fall 98 (68.2%R) Fail | Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
                Applied Qualifiers^
"H"
Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR  " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
" ** " The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process.  Procedure has
been corrected to demonstrate samples uncontaminated.
-------
May 1999 Samples for Critical Parameters Analyzed by  SERC
With the  10% Full QA/QC Review
                  Station ID   M4-508-SWF
Surface Water
Laboratory Records
Data Report (Attached)
Total P
Total N
TOC
Total Hg
MeHg
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Data Entry Checked by Another
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Blank Spike/CCV Recoveries
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Data Entry Checked by Another
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
5-1 1-99/No Time
5-26-99/1130
08/06/99
X
FW=SW
5-1 1-99/No Time
5-26, 8-27-99/1220
8-30-99/0957
X
FW=SW
5-1 1-99/No Time
No Digestion
06/13/99

X
FW=SW
5-1 1-99/No Time
5-12-99/1800
05/13/99

X
FW=SW
5-1 1-99/No Time


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.04
ppm
EPA 365.1
Raw Data Initialed
0.0006ppm
Injection Vial
Injection Vial
sample aliquot
1
1.504
ppm
Antek
Raw Data Initialed
0.03 ppm
NA
4ml
sample aliquot
1
22.53
ppm
EPA415.1
Raw Data Initialed
0.12 ppm
1000ml
1000ml
sample aliquot
1
6.35
ppt
EPA 1631
JL
0.3 ppt
Battelle Lab
is Main Lab



ppt
EPA 1630
JL
0.02 ppt

No
X
Yes
No
X
Past Holding Time Goal
No
X
Past HT
Yes (FLD)
X
Yes
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
By Run Date/ID
**
RecalibrationBlks Good
Sample Dups-Good
74%
CCV %R Good
0.0006-0.2 ppm
0.9958
By Run Date/ID
0.12>MDL
NR
2 RPD (NR)
65% (NR)
102.1 %R
0.03 and>
NA
By Run Date/ID
No Digestion
Good After Correction
-0.634,-0.9RPD
77% R
96-102%R
0.12 ppm and>
0.999

File ID
X
0.14 ppt 
0.9998

File ID








No
Yes
"**", "M"
No
Not All Info Given
"**", "M"
No
Yes
"H"
Yes
Yes




                        Notes
                              For TOC analysis, only 2 of 5 duplicate samples run were recorded, due to inability to read the instrument printout.
                              Total Nitrogen analysis: Reported RPD data and Matrix Spike Recoveries could not be reviewed (NR).
                              SESD Laboratory was switched to be the main laboratory for MeHg. FIU is responsible for 10% of the MeFlg.
                              ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                              been corrected to demonstrate samples uncontaminated.
-------
                      Station ID    M4-508-SWF
Surface Water
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
           Integrity of Data Quality
             Deviations From SOP
                      Observations
Sample Management Records
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































Sampling Location ID
Matrix
Preservative (Acid, Temp..)
Collection Data/Time
Laboratory ID Code
Sample Handling/Storage
Log-in Procedures
Raw Data (Attached)
Sample Work Sheets
Sample Run Logs
Instrument Raw Data
Bench Sheets
Sample Preparation Logs
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory u
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
ses the same ID as the
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
In Hg lab Area
None
X
X
Not Noted
Date/No Time
In Hg Lab Area


NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
X
X
X
Notes on Printouts
X



Notes on Printouts

                                           I!**!!  IIA/TII
                                                 M"
                                                                   I!**!! IIA/TII
           M"
"H"
X
X
uM
X
X
uM
X
X
ppm
SFW=SWF
X
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) | Fall 98 (68.2%R) Fail | Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                      Organization
          Performance (Pass/Fail)

Validation Criteria
                Applied Qualifiers [

Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "  Analysis  digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X " =  Attached or Verified
" ** " The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
been corrected to demonstrate samples uncontaminated.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                  Station ID  M4-533-SWF     Surface Water
Laboratory Records
Data Report (Attached)
Total P
Total N
TOC
Total Hg
MeHg
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Data Entry Checked by Another
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Blank Spike/CCV Recoveries
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Data Entry Checked by Another
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
5-10-99/No Time
5-26-99/1130
11/09/99
X
FW=SW
5-10-99/No Time
5-26,8-27-99/1220
8-30-99/1338
X
FW=SW
5-10-99/No Time
No Digestion
06/13/99

X
FW=SW
5-10-99/No Time
05/12/99
05/13/99

X
FW=SW
5-10-99/No Time


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.129
ppm
EPA 365.1
Raw Data Initialed
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
1.657
ppm
Antek
Raw Data Initialed
0.03 ppm
NA
4ml
sample aliquot
1
33.56
ppm
EPA415.1
Raw Data Initialed
0.12 ppm
1000ml
1000ml
sample aliquot
1
2.01
ppt
EPA 1631
JL
0.3 ppt
Battelle Lab
is Main Lab



ppt
EPA 1630
JL
0.02 ppt

No
X
Yes
No
X
Past Holding Time Goal
No
X
Past HT
Yes (FLD)
X
Yes
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
By Run Date/ID
**
RecalibrationBlks Good
Sample Dups-Good
NR
CCV %R Good
0.0006-0.2 ppm
0.998
By Run Date/ID
lof3>MDL
NR
1.7 RPD
109. 5% Average
100.9 %R
0.03 and>
NA
By Run Date/ID
No Digestion
Good After Correction
-0.634,-0.9RPD
77% R
96-102%R
0.12 ppm and>
0.999

File ID
X
0.2ppt
0.9998

File ID








No
Yes
"**", "M"
No
Yes
I!**!!
No
Yes
"H"
Yes
Yes




                        Notes
                             For TOC analysis, only 2 of 5 duplicate samples run were recorded, due to inability to read the instrument printout.
                             Total Nitrogen analysis: Reported RPD data and Matrix Spike Recoveries could not be reviewed (NR).
                             SESD Laboratory was switched to be the main laboratory for MeHg. FIU is responsible for 10% of the MeFlg.
                             ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                             been corrected to demonstrate samples uncontaminated.
-------
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
           Integrity of Data Quality
             Deviations From SOP
                      Observations
Sample Management Records
M4-533-SWF Surface Water
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































Sampling Location ID
Matrix
Preservative (Acid, Temp..)
Collection Data/Time
Laboratory ID Code
Sample Handling/Storage
Log-in Procedures
Raw Data (Attached)
Sample Work Sheets
Sample Run Logs
Instrument Raw Data
Bench Sheets
Sample Preparation Logs
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
uses the same ID as th
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
e Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
In Hg lab Area
None
X
X
Not Noted
Date/No Time
In Hg Lab Area


NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
X
X
X
Notes on Printouts
X



Notes on Printouts

                                          I!**!!  IIA/TII
                                               , "M"
"H"
X
X
uM
X
X
uM
X
X
ppm
SFW=SWF
X
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) | Fall 98 (68.2%R) Fail | Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                    Measuring Unit
PE Results (Attached)
                      Organization
           Performance  (Pass/Fail)

Validation Criteria
                Applied Qualifiers [

Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"   Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "  Analysis  digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X " = Attached or Verified
" ** " The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process.  Procedure has
been corrected to demonstrate samples uncontaminated.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                  Station ID  M4-538-SWF     Surface Water
Laboratory Records
Data Report (Attached)
Total P
Total N
TOC
Total Hg
MeHg
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Data Entry Checked by Another
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Blank Spike/CCV Recoveries
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Data Entry Checked by Another
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
5-10-99/No Time
5-26-99/1130
08/06/99
X
FW=SW
5-10-99/No Time
5-26, 8-27-99/1220
8-30-99/1338
X
FW=SW
5-10-99/No Time
No Digestion
06/13/99

X
FW=SW
5-10-99/No Time
05/12/99
05/13/99

X
FW=SW
5-10-99/No Time


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
aliquot
1
0.036
ppm
EPA 365.1
Raw Data Initialed
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
2.131
ppm
Antek
Raw Data Initialed
0.03 ppm
NA
4ml
sample aliquot
1
40.72
ppm
EPA415.1
Raw Data Initialed
0.12 ppm
1000ml
1000ml
sample aliquot
1
3.14
ppt
EPA 1631
JL
0.3 ppt
Battelle Lab
is Main Lab



ppt
EPA 1630
JL
0.02 ppt

No
X
Yes
No
X
Past Holding Time Goal
No
X
Past HT
Yes (FLD)
X
Yes
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
By Run Date/ID
**
RecalibrationBlks Good
Sample Dups-Good
Reported 74% (NR)
CCV %R Good
0.0006-0.2 ppm
0.9958
By Run Date/ID
lof3>MDL
NR
1.7 RPD
109. 5% Average
100.9 %R
0.03 and>
NA
By Run Date/ID
No Digestion
Good After Correction
-0.634,-0.9RPD
77% R
96-102%R
0.12 ppm and>
0.999

File ID
X
0.2ppt
0.9998

File ID








No
Yes
"**", "M"
No
Yes
I!**!!
No
Yes
"H"
Yes
Yes




                        Notes
                             For TOC analysis, only 2 of 5 duplicate samples run were recorded, due to inability to read the instrument printout.
                             Total Nitrogen analysis: Reported RPD data and Matrix Spike Recoveries could not be reviewed (NR).
                             SESD Laboratory was switched to be the main laboratory for MeHg. FIU is responsible for 10% of the MeFlg.
                             ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                             been corrected to demonstrate samples uncontaminated.
-------
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
           Integrity of Data Quality
             Deviations From SOP
                      Observations
Sample Management Records
M4-538-SWF Surface Water
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































Sampling Location ID
Matrix
Preservative (Acid, Temp..)
Collection Data/Time
Laboratory ID Code
Sample Handling/Storage
Log-in Procedures
Raw Data (Attached)
Sample Work Sheets
Sample Run Logs
Instrument Raw Data
Bench Sheets
Sample Preparation Logs
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
uses the same ID as th
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
e Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
In Hg lab Area
None
X
X
Not Noted
Date/No Time
In Hg Lab Area


NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
X
X
X
Notes on Printouts
X



Notes on Printouts

                                          I!**!!  IIA/TII
                                               , "M"
"H"
X
X
uM
X
X
uM
X
X
ppm
SFW=SWF
X
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) | Fall 98 (68.2%R) Fail | Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                    Measuring Unit
PE Results (Attached)
                      Organization
           Performance  (Pass/Fail)

Validation Criteria
                Applied Qualifiers [

Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"   Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "  Analysis  digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X " = Attached or Verified
" ** " The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process.  Procedure has
been corrected to demonstrate samples uncontaminated.
-------
May 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID   M4-548-SWF     Surface Water
Laboratory Records
Data Report (Attached)
Total P
Total N
TOC
Total Hg
MeHg
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Data Entry Checked by Another
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Blank Spike/CCV Recoveries
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Data Entry Checked by Another
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
5-9-99/No Time
Sample Lost
Sample Lost
X
FW=SW
5-9-99/No Time
Sample Lost
Sample Lost
X
FW=SW
5-9-99/No Time
Sample Lost
Sample Lost

X
FW=SW
5-9-99/No Time
5-23-99/1800
05/25/99

X
FW=SW
5-9-99/No Time


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppm
EPA 365.1
Raw Data Initialed
0.0003ppm (O.Olumol/L 97)





ppm
Antek
Raw Data Initialed
0.03 ppm





ppm
EPA415.1
Raw Data Initialed
0.12 ppm
1000ml
1000ml
sample aliquot
1
11.27
ppt
EPA 1631
JL
0.3 ppt
Battelle Lab
is Main Lab



ppt
EPA 1630
JL
0.02 ppt










Yes (FLD)
X
Yes
Yes

28 days

FIU/SERC Laboratory uses the same ID as the Sampling Station ID
By Run Date/ID







By Run Date/ID







By Run Date/ID








File ID
X
0.093 ppt 
0.9998

File ID

















Yes
Yes
"M"



                       Notes
                            Sample container or containers for total phosphorus, total nitrogen and TOC were misplaced and therefore analysis could
                            not be performed.
                            Total Hg analysis: No method blanks and no blank spike recoveries were reported.
                            SESD Laboratory was switched to be the main laboratory for MeHg. FIU is responsible for 10% of the MeHg.
                            MeHg results from FIU are pending.
-------
             Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                      Observations
Sample Management Records
M4-548-SWF Surface Water
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































Sampling Location ID
Matrix
Preservative (Acid, Temp..)
Collection Data/Time
Laboratory ID Code
Sample Handling/Storage
Log-in Procedures
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
uses the same ID as th
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
e Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
In Hg lab Area
None
X
X
Not Noted
Date/No Time
In Hg Lab Area

                                                                                                                "M"
NA




NA




NA




X
X
X
Notes on Printouts
X



Notes on Printouts




uM


uM


ppm
SFW=SWF
X
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) | Fall 98 (68.2%R) Fail | Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                      Organization
          Performance  (Pass/Fail)

Validation Criteria
                Applied Qualifiers [

Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "  Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X " =  Attached or Verified
" ** " The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process.  Procedure has
been corrected to demonstrate samples uncontaminated.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                  Station ID  M4-556-SWF     Surface Water
Laboratory Records
Data Report (Attached)
Total P
Total N
TOC
Total Hg
MeHg
                        Notes
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Data Entry Checked by Another
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Blank Spike/CCV Recoveries
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Data Entry Checked by Another
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
5-8-99/No Time
5-26-99/1130
08/06/99
X
FW=SW
5-8-99/No Time
5-26, 8-27-99/1220
8-30-99/1338
X
FW=SW
5-8-99/No Time
No Digestion
06/13/99

X
FW=SW
5-8-99/No Time
05/20/99
05/21/99

X
FW=SW
5-8-99/No Time


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
aliquot
1
0.011
ppm
EPA 365.1
Raw Data Initialed
O.OOOSppm (O.Olmnol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
1.90
ppm
Antek
Raw Data Initialed
0.03 ppm
NA
4ml
sample aliquot
1
30.59
ppm
EPA415.1
Raw Data Initialed
0.12 ppm
1000ml
1000ml
sample aliquot
1
2.38
ppt
EPA 1631
JL
0.3 ppt
Battelle Lab
is Main Lab



ppt
EPA 1630
JL
0.02 ppt

No
X
Yes
No
X
Past Holding Time Goal
No
X
Past HT
Yes (FLD)
X
Yes
Yes

28 days

FIU/SERC Laboratory uses the same ID as the Sampling Station ID
By Run Date/ID
**
RecalibrationBlks Good
Sample Dups-Good
74%
CCV %R Good
0.0006-0.2 ppm
0.9958
By Run Date/ID
1 of3>MDL
NR
1.7 RPD
109. 5% Average
100.9 %R
0.03 and>
NA
By Run Date/ID
No Digestion
Good After Correction
-0.634,-0.9RPD
77% R
96-102%R
0.12 ppm and>
0.999

File ID
X
.128ppt
0.9988

File ID








No
Yes
"**", "M"
No
Yes
I!**!!
No
Yes
"H"
Yes
Yes




                             For TOC analysis, only 2 of 5 duplicate samples run were recorded, due to inability to read the instrument printout.
                             Total Nitrogen analysis: Reported RPD data and Matrix Spike Recoveries could not be reviewed (NR).
                             SESD Laboratory was switched to be the main laboratory for MeHg. FIU is responsible for 10% of the MeHg.
                             ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                             been corrected to demonstrate samples uncontaminated.
-------
                      Station ID
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
           Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
             Collection Data/Time
               Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation Criteria
M4-556-SWF Surface Water
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time

In Hg lab Area
None
X
X
Not Noted
Date/No Time

InHg Lab Area

NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
X
X
X
Notes on Printouts
X



Notes on Printouts

X
X
uM
X
X
uM
X
X
ppm
SFW=SWF
X
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) | Fall 98 (68.2%R) Fail | Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
                Applied Qualifiers^

Data Qualifiers/Footnotes:
                                         I!**!!  IIA/TII
M"
"H"
" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR  " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
" ** " The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process.  Procedure has
been corrected to demonstrate samples uncontaminated.
-------
May 1999  Samples for Critical Parameters Analyzed by SERC
With the  10% Full QA/QC Review
                   Station ID   M4-566-SWF
Surface Water
Laboratory Records
Data Report (Attached)
Total P
Total N
TOC
Total Hg
MeHg
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Data Entry Checked by Another
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Blank Spike/CCV Recoveries
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Data Entry Checked by Another
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
5-7-99/No Time
5-26-99/1130
08/06/99
X
FW=SW
5-7-99/No Time
5-26-99/1030,Date Not Noted
8-4-99/1507
X
FW=SW
5-7-99/No Time
No Digestion
06/13/99

X
FW=SW
5-7-99/No Time
05/19/99
05/20/99

X
FW=SW
5-7-99/No Time


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.009
ppm
EPA 365.1
Raw Data Initialed
O.OOOSppm (O.Olmnol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
1.197
ppm
Antek
Raw Data Initialed
0.03 ppm
NA
4ml
sample aliquot
1
21.29
ppm
EPA415.1
Raw Data Initialed
0.12 ppm
1000ml
1000ml
sample aliquot
1
1.86
ppt
EPA 1631
JL
0.3 ppt
Battelle Lab
is Main Lab



ppt
EPA 1630
JL
0.02 ppt

No
X
Yes
No
X
Past Holding Time Goal
No
X
Past HT
Yes (FLD)
X
Yes
Yes

28 days

FIU/SERC Laboratory uses the same ID as the Sampling Station ID
By Run Date/ID
**
RecalibrationBlks Good
Sample Dups-Good
74%
CCV %R Good
0.0006-0.2 ppm
0.9958
By Run Date/ID
lof3>MDL
NR
-3. 68 RPD
62.7, 72.7% R
88.9%, 106.6%R
0.03 and>
NA
By Run Date/ID
No Digestion
Good After Correction
-0.634,-0.9RPD
77% R
96-102%R
0.12 ppm and>
0.999

File ID
X
0.295 ppt 
0.996

File ID








No
Yes
"**", "M"
No
Yes
"**", "M"
No
Yes
"H"
Yes
Yes




                         Notes
                              For TOC analysis, only 2 of 5 duplicate samples run were recorded, due to inability to read the instrument printout.
                              For Total Nitrogen Analysis, 1 of 3 instrument blanks were above the 3 times MDL limit.
                              Total Nitrogen analysis: Reported RPD data and Matrix Spike Recoveries could not be reviewed (NR).
                              SESD Laboratory was switched to be the main laboratory for MeHg.  FIU is responsible for 10% of the MeHg.
                              ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                              been corrected to demonstrate samples uncontaminated.
-------
                      Station ID   M4-566-SWF
             Surface Water
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
           Integrity of Data Quality
             Deviations From SOP
                      Observations
Sample Management Records
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































Sampling Location ID
Matrix
Preservative (Acid, Temp..)
Collection Data/Time
Laboratory ID Code
Sample Handling/Storage
Log-in Procedures
Raw Data (Attached)
Sample Work Sheets
Sample Run Logs
Instrument Raw Data
Bench Sheets
Sample Preparation Logs
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
uses the same ID as the
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time

In Hg lab Area
None
X
X
Not Noted
Date/No Time
InHg Lab Area


NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
X
X
X
Notes on Printouts
X



Notes on Printouts

Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                      Organization
          Performance (Pass/Fail)

Validation Criteria
X
X
uM
X
X
uM
X
X
ppm
SFW=SWF
X
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) | Fall 98 (68.2%R) Fail | Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
                Applied Qualifiers^

Data Qualifiers/Footnotes:
                                          I!**!!  IIA/TII
M"
                                                                 I!**!! IIA/TII
M"
"H"
" J "   Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
" ** " The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
been corrected to demonstrate samples uncontaminated.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                  Station ID  M4-568-SWF     Surface Water
Laboratory Records
Data Report (Attached)
Total P
Total N
TOC
Total Hg
MeHg
                        Notes
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Data Entry Checked by Another
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Blank Spike/CCV Recoveries
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Data Entry Checked by Another
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
5-7-99/No Time
5-26-99/1130
08/06/99
X
FW=SW
5-7-99/No Time
5-26-99/1030
8-4-99/1155
X
FW=SW
5-7-99/No Time
No Digestion
06/13/99

X
FW=SW
5-7-99/No Time
5-10-99/1800
05/11/99

X
FW=SW
5-7-99/No Time


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.012
ppm
EPA 365.1
Raw Data Initialed
O.OOOSppm (O.Olmnol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
1.842
ppm
Antek
Raw Data Initialed
0.03 ppm
NA
4ml
sample aliquot
1
22.21
ppm
EPA415.1
Raw Data Initialed
0.12 ppm
1000ml
1000ml
sample aliquot
1
1.93
ppt
EPA 1631
JL
0.3 ppt
Battelle Lab
is Main Lab



ppt
EPA 1630
JL
0.02 ppt

No
X
Yes
No
X
Past Holding Time Goal
No
X
Past HT
Yes (FLD)
X
Yes
Yes

28 days

FIU/SERC Laboratory uses the same ID as the Sampling Station ID
By Run Date/ID
**
RecalibrationBlks Good
Sample Dups-Good
74%
CCV %R Good
0.0006-0.2 ppm
0.9958
By Run Date/ID
3of3>MDL
NR
1.2 RPD
83.4%R
100.8 - 108 %R
0.03 and>
NA
By Run Date/ID
No Digestion
Good After Correction
-0.634,-0.9RPD
77% R
96-102%R
0.12 ppm and>
0.999

File ID
X
0.221 ppt 
0.9995

File ID








No
Yes
"**", "M"
No
Yes
I!**!!
No
Yes
"H"
Yes
Yes
"M (NR)"



                             For TOC analysis, only 2 of 5 duplicate samples run were recorded, due to inability to read the instrument printout.
                             Total Nitrogen analysis: Reported RPD data and Matrix Spike Recoveries could not be reviewed (NR).
                             SESD Laboratory was switched to be the main laboratory for MeHg. FIU is responsible for 10% of the MeHg.
                             ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                             been corrected to demonstrate samples uncontaminated.
-------
             Total Samples/Matrix
               Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
               Analytical Problems
        QA/QC Acceptance Limits
           Integrity of Data Quality
             Deviations From SOP
                      Observations
Sample Management Records
M4-568-SWF Surface Water
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































Sampling Location ID
Matrix
Preservative (Acid, Temp..)
Collection Data/Time
Laboratory ID Code
Sample Handling/Storage
Log-in Procedures
Raw Data (Attached)
Sample Work Sheets
Sample Run Logs
Instrument Raw Data
Bench Sheets
Sample Preparation Logs
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
uses the same ID as th
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
e Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time

In Hg lab Area
None
X
X
Not Noted
Date/No Time
InHg Lab Area


NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
X
X
X
Notes on Printouts
X



Notes on Printouts

Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                    Measuring Unit
PE Results (Attached)
                      Organization
           Performance  (Pass/Fail)

Validation Criteria
X
X
uM
X
X
uM
X
X
ppm
SFW=SWF
X
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) | Fall 98 (68.2%R) Fail | Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
                Applied Qualifiers^

Data Qualifiers/Footnotes:
                                          I!**!!  IIA/TII
M"
"H"
"M (NR)"
" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"   Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
" ** " The blanks are reported above MDL,  Lab water was used as a blank but, not in the sample digestion process.  Procedure has
been corrected to demonstrate samples uncontaminated.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                  Station ID  M4-576-SWF     Surface Water
Laboratory Records
Data Report (Attached)
Total P
Total N
TOC
Total Hg
MeHg
                        Notes
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Data Entry Checked by Another
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Blank Spike/CCV Recoveries
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Data Entry Checked by Another
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
5-4-99/No Time
5-26-99/1130
08/06/99
X
FW=SW
5-4-99/No Time
5-26-99/1030
8-4-99/1155
X
FW=SW
5-4-99/No Time
No Digestion
06/13/99

X
FW=SW
5-4-99/No Time
5-6-99/1800
05/07/99

X
FW=SW
5-4-99/No Time


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.008
ppm
EPA 365.1
Raw Data Initialed
O.OOOSppm (O.Olmnol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
1.648
ppm
Antek
Raw Data Initialed
0.03 ppm
NA
4ml
sample aliquot
1
22.73
ppm
EPA415.1
Raw Data Initialed
0.12 ppm
1000ml
1000ml
sample aliquot
1
2.84
ppt
EPA 1631
JL
0.3 ppt
Battelle Lab
is Main Lab



ppt
EPA 1630
JL
0.02 ppt

No
X
Yes
No
X
Past Holding Time Goal
No
X
Past HT
Yes (FLD)
X
Yes
Yes

28 days

FIU/SERC Laboratory uses the same ID as the Sampling Station ID
By Run Date/ID
**
RecalibrationBlks Good
Sample Dups-Good
74%
CCV %R Good
0.0006-0.2 ppm
0.9958
By Run Date/ID
3of3>MDL
NR
1.2 RPD
83.4%R
100.8 - 108 %R
0.03 and>
NA
By Run Date/ID
No Digestion
Good After Correction
-0.634,-0.9RPD
77% R
96-102%R
0.12 ppm and>
0.999

File ID
X
0.03 ppt 
0.9994

File ID








No
Yes
"**", "M"
No
Yes
I!**!!
No
Yes
"H"
Yes
Yes




                             For TOC analysis, only 2 of 5 duplicate samples run were recorded, due to inability to read the instrument printout.
                             Total Nitrogen analysis: Reported RPD data and Matrix Spike Recoveries could not be reviewed (NR).
                             SESD Laboratory was switched to be the main laboratory for MeHg. FIU is responsible for 10% of the MeHg.
                             ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                             been corrected to demonstrate samples uncontaminated.
-------
                      Station ID
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
           Integrity of Data Quality
             Deviations From SOP
                      Observations
Sample Management Records
M4-576-SWF Surface Water
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































Sampling Location ID
Matrix
Preservative (Acid, Temp..)
Collection Data/Time
Laboratory ID Code
Sample Handling/Storage
Log-in Procedures
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
uses the same ID as th
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
e Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time

In Hg lab Area
None
X
X
Not Noted
Date/No Time
InHg Lab Area

Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                      Organization
          Performance  (Pass/Fail)

Validation Criteria
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
X
X
X
Notes on Printouts
X



Notes on Printouts

X
X
uM
X
X
uM
X
X
ppm
SFW=SWF
X
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) | Fall 98 (68.2%R) Fail | Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
                Applied Qualifiers^

Data Qualifiers/Footnotes:
                                         I!**!!  IIA/TII
M"
"H"
" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
" ** " The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process.  Procedure has
been corrected to demonstrate samples uncontaminated.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                  Station ID  M4-586-SWF     Surface Water
Laboratory Records
Data Report (Attached)
Total P
Total N
TOC
Total Hg
MeHg
                        Notes
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Data Entry Checked by Another
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Blank Spike/CCV Recoveries
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Data Entry Checked by Another
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
5-6-99/No Time
5-26-99/1130
08/06/99
X
FW=SW
5-6-99/No Time
5-26-99/1030
8-4-99/1155
X
FW=SW
5-6-99/No Time
No Digestion
06/13/99

X
FW=SW
5-6-99/No Time
5-10-99/1800
05/11/99

X
FW=SW
5-6-99/No Time


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.019
ppm
EPA 365.1
Raw Data Initialed
O.OOOSppm (O.Olmnol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
2.705
ppm
Antek
Raw Data Initialed
0.03 ppm
NA
4ml
sample aliquot
1
30.78
ppm
EPA415.1
Raw Data Initialed
0.12 ppm
1000ml
1000ml
sample aliquot
1
11.85
ppt
EPA 1631
JL
0.3 ppt
Battelle Lab
is Main Lab



ppt
EPA 1630
JL
0.02 ppt

No
X
Yes
No
X
Past Holding Time Goal
No
X
Past HT
Yes (FLD)
X
Yes
Yes

28 days

FIU/SERC Laboratory uses the same ID as the Sampling Station ID
By Run Date/ID
**
RecalibrationBlks Good
Sample Dups-Good
74%
CCV %R Good
0.0006-0.2 ppm
0.9958
By Run Date/ID
3of3>MDL
NR
1.2 RPD
83.4%R
100.8 - 108 %R
0.03 and>
NA
By Run Date/ID
No Digestion
Good After Correction
-0.634,-0.9RPD
77% R
96-102%R
0.12 ppm and>
0.999

File ID
X
0.221 ppt 
0.9995

File ID








No
Yes
"**", "M"
No
Yes
I!**!!
No
Yes
"H"
Yes
Yes
"M (NR)"



                             For TOC analysis, only 2 of 5 duplicate samples run were recorded, due to inability to read the instrument printout.
                             Total Nitrogen analysis: Reported RPD data and Matrix Spike Recoveries could not be reviewed (NR).
                             SESD Laboratory was switched to be the main laboratory for MeHg. FIU is responsible for 10% of the MeHg.
                             ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                             been corrected to demonstrate samples uncontaminated.
-------
             Total Samples/Matrix
               Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
               Analytical Problems
        QA/QC Acceptance Limits
           Integrity of Data Quality
             Deviations From SOP
                      Observations
Sample Management Records
M4-586-SWF Surface Water
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































Sampling Location ID
Matrix
Preservative (Acid, Temp..)
Collection Data/Time
Laboratory ID Code
Sample Handling/Storage
Log-in Procedures
Raw Data (Attached)
Sample Work Sheets
Sample Run Logs
Instrument Raw Data
Bench Sheets
Sample Preparation Logs
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
uses the same ID as th
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
e Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time

In Hg lab Area
None
X
X
Not Noted
Date/No Time
InHg Lab Area


NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
X
X
X
Notes on Printouts
X



Notes on Printouts

Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                    Measuring Unit
PE Results (Attached)
                      Organization
           Performance  (Pass/Fail)

Validation Criteria
X
X
uM
X
X
uM
X
X
ppm
SFW=SWF
X
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) | Fall 98 (68.2%R) Fail | Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
                Applied Qualifiers^

Data Qualifiers/Footnotes:
                                          I!**!!  IIA/TII
M"
"H"
"M (NR)"
" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"   Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
" ** " The blanks are reported above MDL,  Lab water was used as a blank but, not in the sample digestion process.  Procedure has
been corrected to demonstrate samples uncontaminated.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                  Station ID  M4-594-SWF     Surface Water
Laboratory Records
Data Report (Attached)
Total P
Total N
TOC
Total Hg
MeHg
                        Notes
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Data Entry Checked by Another
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Blank Spike/CCV Recoveries
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Data Entry Checked by Another
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
5-5-99/No Time
5-26-99/1130
08/06/99
X
FW=SW
5-5-99/No Time
5-26-99/1030
8-4-99/1155
X
FW=SW
5-5-99/No Time
No Digestion
06/13/99

X
FW=SW
5-5-99/No Time
5-6-99/1800
05/07/99

X
FW=SW
5-5-99/No Time


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.018
ppm
EPA 365.1
Raw Data Initialed
O.OOOSppm (O.Olmnol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
2.675
ppm
Antek
Raw Data Initialed
0.03 ppm
NA
4ml
sample aliquot
1
26.91
ppm
EPA415.1
Raw Data Initialed
0.12 ppm
1000ml
1000ml
sample aliquot
1
3.02
ppt
EPA 1631
JL
0.3 ppt
Battelle Lab
is Main Lab



ppt
EPA 1630
JL
0.02 ppt

No
X
Yes
No
X
Past Holding Time Goal
No
X
Past HT
Yes (FLD)
X
Yes
Yes

28 days

FIU/SERC Laboratory uses the same ID as the Sampling Station ID
By Run Date/ID
**
RecalibrationBlks Good
Sample Dups-Good
74%
CCV %R Good
0.0006-0.2 ppm
0.9958
By Run Date/ID
3of3>MDL
NR
1.2 RPD
83.4%R
100.8 - 108 %R
0.03 and>
NA
By Run Date/ID
No Digestion
Good After Correction
-0.634,-0.9RPD
77% R
96-102%R
0.12 ppm and>
0.999

File ID
X
0.03 ppt 
0.9994

File ID








No
Yes
"**", "M"
No
Yes
I!**!!
No
Yes
"H"
Yes
Yes




                             For TOC analysis, only 2 of 5 duplicate samples run were recorded, due to inability to read the instrument printout.
                             Total Nitrogen analysis: Reported RPD data and Matrix Spike Recoveries could not be reviewed (NR).
                             SESD Laboratory was switched to be the main laboratory for MeHg. FIU is responsible for 10% of the MeHg.
                             ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                             been corrected to demonstrate samples uncontaminated.
-------
                      Station ID
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
           Integrity of Data Quality
             Deviations From SOP
                      Observations
Sample Management Records
M4-594-SWF Surface Water
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































Sampling Location ID
Matrix
Preservative (Acid, Temp..)
Collection Data/Time
Laboratory ID Code
Sample Handling/Storage
Log-in Procedures
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
uses the same ID as th
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
e Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time

In Hg lab Area
None
X
X
Not Noted
Date/No Time
InHg Lab Area

Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                      Organization
          Performance  (Pass/Fail)

Validation Criteria
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
X
X
X
Notes on Printouts
X



Notes on Printouts

X
X
uM
X
X
uM
X
X
ppm
SFW=SWF
X
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) | Fall 98 (68.2%R) Fail | Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
                Applied Qualifiers^

Data Qualifiers/Footnotes:
                                         I!**!!  IIA/TII
M"
"H"
" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
" ** " The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process.  Procedure has
been corrected to demonstrate samples uncontaminated.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                  Station ID  M4-599-SWF     Surface Water
Laboratory Records
Data Report (Attached)
Total P
Total N
TOC
Total Hg
MeHg
                        Notes
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Data Entry Checked by Another
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Blank Spike/CCV Recoveries
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Data Entry Checked by Another
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
5-6-99/No Time
5-26-99/1130
08/06/99
X
FW=SW
5-6-99/No Time
5-26-99/1030
8-4-99/1155
X
FW=SW
5-6-99/No Time
No Digestion
06/13/99

X
FW=SW
5-6-99/No Time
5-9-99/1800
05/10/99

X
FW=SW
5-6-99/No Time


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.017
ppm
EPA 365.1
Raw Data Initialed
O.OOOSppm (O.Olmnol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
2.388
ppm
Antek
Raw Data Initialed
0.03 ppm
NA
4ml
sample aliquot
1
35.08
ppm
EPA415.1
Raw Data Initialed
0.12 ppm
1000ml
1000ml
sample aliquot
1
2.64
ppt
EPA 1631
JL
0.3 ppt
Battelle Lab
is Main Lab



ppt
EPA 1630
JL
0.02 ppt

No
X
Yes
No
X
Past Holding Time Goal
No
X
Past HT
Yes (FLD)
X
Yes
Yes

28 days

FIU/SERC Laboratory uses the same ID as the Sampling Station ID
By Run Date/ID
**
RecalibrationBlks Good
Sample Dups-Good
74%
CCV %R Good
0.0006-0.2 ppm
0.9958
By Run Date/ID
3of3>MDL
NR
1.2 RPD
83.4%R
100.8 - 108 %R
0.03 and>
NA
By Run Date/ID
No Digestion
Good After Correction
-0.634,-0.9RPD
77% R
96-102%R
0.12 ppm and>
0.999

File ID
X
0.3ppt
0.9998

File ID








No
Yes
"**", "M"
No
Yes
I!**!!
No
Yes
"H"
Yes
Yes
"M"



                             For TOC analysis, only 2 of 5 duplicate samples run were recorded, due to inability to read the instrument printout.
                             Total Nitrogen analysis: Reported RPD data and Matrix Spike Recoveries could not be reviewed (NR).
                             SESD Laboratory was switched to be the main laboratory for MeHg. FIU is responsible for 10% of the MeHg.
                             ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                             been corrected to demonstrate samples uncontaminated.
-------
             Total Samples/Matrix
               Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
               Analytical Problems
        QA/QC Acceptance Limits
           Integrity of Data Quality
             Deviations From SOP
                      Observations
Sample Management Records
M4-599-SWF Surface Water
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































Sampling Location ID
Matrix
Preservative (Acid, Temp..)
Collection Data/Time
Laboratory ID Code
Sample Handling/Storage
Log-in Procedures
Raw Data (Attached)
Sample Work Sheets
Sample Run Logs
Instrument Raw Data
Bench Sheets
Sample Preparation Logs
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
uses the same ID as th
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
e Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time

In Hg lab Area
None
X
X
Not Noted
Date/No Time
InHg Lab Area


NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
X
X
X
Notes on Printouts
X



Notes on Printouts

Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                    Measuring Unit
PE Results (Attached)
                      Organization
           Performance  (Pass/Fail)

Validation Criteria
X
X
uM
X
X
uM
X
X
ppm
SFW=SWF
X
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) | Fall 98 (68.2%R) Fail | Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
                Applied Qualifiers^

Data Qualifiers/Footnotes:
                                          I!**!!  IIA/TII
M"
"H"
"M"
" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"   Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
" ** " The blanks are reported above MDL,  Lab water was used as a blank but, not in the sample digestion process.  Procedure has
been corrected to demonstrate samples uncontaminated.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                  Station ID  M4-809-SWF     Surface Water
Laboratory Records
Data Report (Attached)
Total P
Total N
TOC
Total Hg
MeHg
                        Notes
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Data Entry Checked by Another
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Blank Spike/CCV Recoveries
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Data Entry Checked by Another
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
5-1 1-99/No Time
5-26-99/1130
08/06/99
X
FW=SW
5-1 1-99/No Time
5-26-99/1030,Date Not Noted
8-4-99/1507
X
FW=SW
5-1 1-99/No Time
No Digestion
06/13/99

X
FW=SW
5-1 1-99/No Time
05/20/99
05/21/99

X
FW=SW
5-1 1-99/No Time


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.012
ppm
EPA 365.1
Raw Data Initialed
O.OOOSppm (O.Olmnol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
1.223
ppm
Antek
Raw Data Initialed
0.03 ppm
NA
4ml
sample aliquot
1
22.47
ppm
EPA415.1
Raw Data Initialed
0.12 ppm
1000ml
1000ml
sample aliquot
1
3.02
ppt
EPA 1631
JL
0.3 ppt
Battelle Lab
is Main Lab



ppt
EPA 1630
JL
0.02 ppt

No
X
Yes
No
X
Past Holding Time Goal
No
X
Past HT
Yes (FLD)
X
Yes
Yes

28 days

FIU/SERC Laboratory uses the same ID as the Sampling Station ID
By Run Date/ID
**
RecalibrationBlks Good
Sample Dups-Good
74%
CCV %R Good
0.0006-0.2 ppm
0.9958
By Run Date/ID
1 of3>MDL
NR
-3. 68 RPD
62.7, 72.7% R
88.9%- 106.6%R
0.03 and>
NA
By Run Date/ID
No Digestion
Good After Correction
-0.634,-0.9RPD
77% R
96-102%R
0.12 ppm and>
0.999

File ID
X
0.14 ppt 
0.9998

File ID








No
Yes
"**", "M"
No
Yes
"**", "M"
No
Yes
"H"
Yes
Yes




                             For TOC analysis, only 2 of 5 duplicate samples run were recorded, due to inability to read the instrument printout.
                             Total Nitrogen analysis: Reported RPD data and Matrix Spike Recoveries could not be reviewed (NR).
                             SESD Laboratory was switched to be the main laboratory for MeHg. FIU is responsible for 10% of the MeHg.
                             ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                             been corrected to demonstrate samples uncontaminated.
-------
             Total Samples/Matrix
               Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
               Analytical Problems
        QA/QC Acceptance Limits
           Integrity of Data Quality
             Deviations From SOP
                      Observations
Sample Management Records
M4-809-SWF Surface Water
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































Sampling Location ID
Matrix
Preservative (Acid, Temp..)
Collection Data/Time
Laboratory ID Code
Sample Handling/Storage
Log-in Procedures
Raw Data (Attached)
Sample Work Sheets
Sample Run Logs
Instrument Raw Data
Bench Sheets
Sample Preparation Logs
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
uses the same ID as th
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
e Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time
In Hg lab Area
None
X
X
Not Noted
Date/No Time
InHg Lab Area


NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
X
X
X
Notes on Printouts
X



Notes on Printouts

Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                    Measuring Unit
PE Results (Attached)
                      Organization
           Performance  (Pass/Fail)

Validation Criteria
X
X
uM
X
X
uM
X
X
ppm
SFW=SWF
X
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) | Fall 98 (68.2%R) Fail | Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
                Applied Qualifiers^

Data Qualifiers/Footnotes:
                                          I!**!! IIA/TII
M"
                                                                  I!**!! IIA/TII
, "M"
"H"
" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"   Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
" ** " The blanks are reported above MDL,  Lab water was used as a blank but, not in the sample digestion process.  Procedure has
been corrected to demonstrate samples uncontaminated.
-------
May 1999  Samples for Critical Parameters Analyzed by SERC
With the  10% Full QA/QC Review
                   Station ID    M4-872-SWF
Surface Water
Laboratory Records
Data Report (Attached)
Total P
Total N
TOC
Total Hg
MeHg
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Data Entry Checked by Another
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Blank Spike/CCV Recoveries
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Data Entry Checked by Another
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
5-8-99/No Time
5-26-99/1130
08/06/99
X
FW=SW
5-8-99/No Time
5-26-99/1030,Date Not Noted
8-4-99/1507
X
FW=SW
5-8-99/No Time
No Digestion
06/13/99

X
FW=SW
5-8-99/No Time
05/20/99
05/21/99

X
FW=SW
5-8-99/No Time


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.012
ppm
EPA 365.1
Raw Data Initialed
O.OOOSppm (O.Olmnol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
1.387
ppm
Antek
Raw Data Initialed
0.03 ppm
NA
4ml
sample aliquot
1
22.56
ppm
EPA415.1
Raw Data Initialed
0.12 ppm
1000ml
1000ml
sample aliquot
1
1.55
ppt
EPA 1631
JL
0.3 ppt
Battelle Lab
is Main Lab



ppt
EPA 1630
JL
0.02 ppt

No
X
Yes
No
X
Past Holding Time Goal
No
X
Past HT
Yes (FLD)
X
Yes
Yes

28 days

FIU/SERC Laboratory uses the same ID as the Sampling Station ID
By Run Date/ID
**
RecalibrationBlks Good
Sample Dups-Good
Reported 74%
CCV %R Good
0.0006-0.2 ppm
0.9958
By Run Date/ID
lof3>MDL
NR
-3. 68 RPD
62.7, 72.7% R
88.9% - 106.6%R
0.03 and>
NA
By Run Date/ID
No Digestion
Good After Correction
-0.634,-0.9RPD
77% R
96-102%R
0.12 ppm and>
0.999

File ID
X
.128ppt
0.9988

File ID








No
Yes
"**", "M"
No
Yes
"**", "M"
No
Yes
"H"
Yes
Yes




                         Notes
                              For TOC analysis, only 2 of 5 duplicate samples run were recorded, due to inability to read the instrument printout.
                              For Total Nitrogen Analysis, 1 of 3 instrument blanks were above the 3 times MDL limit.
                              Total Nitrogen analysis: Reported RPD data and Matrix Spike Recoveries could not be reviewed (NR).
                              SESD Laboratory was switched to be the main laboratory for MeHg.  FIU is responsible for 10% of the MeHg.
                              ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                              been corrected to demonstrate samples uncontaminated.
-------
Station ID    M4-872-SWF
Surface Water
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X
Not Noted
Date/No Time

In Hg lab Area
None
X
X
Not Noted
Date/No Time

In Hg Lab Area

                    I!**!! IIA/TII
                          M"
                                           I!**!!  IIA/TII
          M"
"H"
             Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
             Collection Data/Time
               Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation Criteria
                Applied Qualifiers [

Data Qualifiers/Footnotes:

" J "   Concentration reported should be  considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "  Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X " = Attached or Verified
" ** " The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
been corrected to demonstrate samples uncontaminated.
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
NA
X
X
With Raw Printout
X
X
X
X
Notes on Printouts
X



Notes on Printouts

X
X
uM
X
X
uM
X
X
ppm
SFW=SWF
X
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) | Fall 98 (68.2%R) Fail | Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
-------
Water - Battelle
-------
10 % Recalculated Results for Methylmercury in Surface Water
Analyzed by Battelle Marine Sciences Laboratory for the May 1999 Dry Season (M4)
Entered by mwb 01/07/00, njs 01/10/00
Sampling Station
ID
M4-500-SWB
M4-538-SWB
Method Blank
Instrument Blank
M4-506-SWB (QA)
M4-506-SWB (QA-DUP)
M4-508-SWB (QA)
M4-508-SWB(QAMS)
Stdl34 (QACCV)

M4-556-SWB
Method Blank
Instrument Blank
M4-553-SWB (QA)
M4-553-SWB (QA-DUP)
M4-555-SWB (QA)
M4-555-SWB (QA-MS)
Std 134 (QA-CCV)

M4-566-SWB
M4-576-SWB
Method Blank
Instrument Blank
M4-569-SWB (QA)
M4-569-SWB (QA-DUP)
M4-566-SWB (QA)
M4-566-SWB (QA-MS)
Std 135 (QA-CCV)

M4-809-SWB
Method Blank
Instrument Blank
M4-577-SWB (QA)
M4-577-SWB (QA-DUP)
M4-559-SWB (QA)
M4-559-SWB (QA-MS)
Std 135 (QA-CCV)

M4-901-SWB
Method Blank
Instrument Blank
M4-870-SWB (QA)
M4-870-SWB (QA-DUP)
M4-877-SWB (QA)
M4-877-SWB (QA-MS)
Std 135 (QA-CCV)
Battelle
MSL Code
1329-90
1329-100
BLK05 18991

1329-93
1329-93
1329-94
1329-94MS
13290519

1329-110
BLK05 18991

1329-107
1329-107
1329-109
1329-109MS
13290520

1329-120
1329-130
BLK052499

1329-123
1329-123
1329-120
1329-120MS


1329-140
BLK060499

1329-131
1329-131
1329-113
1329-1 13MS


1329-149
BLK052699

1329-145
1329-145
1329-147
1329-147MS

Data Qualifier
Note



NR








NR









NR








NR








NR





QC
Batch
13290519
11
11
"
11
"
11
"
11

13290520
11
"
11
"
11
"
11

13290525
"
"
11
"
11
"
11
"

13290604
"
11
"
11
"
11
"

13290527
"
11
"
11
"
11
"
Instrument
Peak
Height
12812
2455
221

1042
1117
1081
8490


1960
0

1085
1103
856
9617
381

1026
410
247

1174
1189
1026
9186


4475
336

2006
1881
7458
19818


3691
123

359
361
1103
8483

Distilled
Sample
Vomme(ml)
49.727
50.463
51.378

50.982
51.932
49.494
49.419


50.948
50.503

50.056
50.228
50.670
50.277


50.407
50.089
50.134

50.181
50.254
50.407
50.325


49.133
49.951

50.855
50.646
48.831
49.294


50.225
50.761

50.344
50.589
50.596
50.016

Volume
Analyzed
(ml)
49.727
50.463
51.378

50.982
51.932
49.294
49.419


50.948
50.503

50.056
50.228
50.670
50.277


50.407
50.089
50.134

50.181
50.254
50.407
50.325


49.133
49.951

50.855
50.646
48.831
49.294


50.225
50.761

50.344
50.589
50.596
50.016

Distillation
Correction
Factor
0.857
0.857
0.857

0.857
0.857
0.857
0.857


0.946
0.946

0.946
0.946
0.946
0.946


0.904
0.904
0.904

0.904
0.904
0.904
0.904


0.936
0.936

0.936
0.936
0.936
0.936


1
1

1
1
1
1

Y intercept
187
187
187

187
187
187
187


93
93

93
93
93
93


98
98
98

98
98
98
98


339
339

339
339
339
339


104
104

104
104
104
104

Slope
(factor)
54.3
54.3
54.3

54.3
54.3
54.3
54.3


56.1
56.1

56.1
56.1
56.1
56.1


52.4
52.4
52.4

52.4
52.4
52.4
52.4


83.4
83.4

83.4
83.4
83.4
83.4


46.2
46.2

46.2
46.2
46.2
46.2

Blank
Correction
Factor
0
0
0

0
0
0
0


0
0

0
0
0
0


0.0626
0.0626
0.0626

0.0626
0.0626
0.0626
0.0626


0
0

0
0
0
0


0
0

0
0
0
0

Hg
Concentration
PPt
5.46
0.966
0.0142

0.360
0.385
0.390
3.610


0.690
-0.035

0.373
0.379
0.284
3.569


0.326
0.069
0.000

0.390
0.396
0.326
3.750


1.078
-0.001

0.420
0.390
1.868
5.062


1.55
0.008

0.11
0.11
0.43
3.63

DETECTION
LIMIT
PPt
0.0233
0.0229
0.0225

0.0227
0.0223
0.0235
0.0234


0.0206
0.0208

0.0209
0.0209
0.0207
0.0209


0.0218
0.0219
0.0219

0.0219
0.0218
0.0218
0.0218


0.0216
0.0212

0.0208
0.0209
0.0197
0.0195


0.0198
0.0195

0.0197
0.0196
0.0196
0.0198

ICV/CCV
CONC








38.40








40.37









167








70.9








83.1
TRUE
CONC








38.95








38.95









161








81








82.7
%R








98.6








103.6









103.7








87.5








100.5
Amount
Spiked
(ppm)







3.35








3.29









3.29








3.35








3.31

Amount
Recovered
(ppm)







3.221








3.286









3.424








3.195








3.199

%R







96








100









104








95








97

Relative
Percent
Difference





6.56








1.46









1.44








7.38








0.296



"NR" Not Reviewed
-------
May 1999 Samples for Critical Parameters Analyzed by Battelle
With the  10% Full QA/QC Review
Total Methylmercury in Surface Water
                                             Sampling Station ID
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
   Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates  (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
   Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                      Notes
M4-500-SWB
M4-538-SWB
M4-556-SWB
M4-566-SWB
1329-90
M4-500-SWB
surface water = SW
05/1 1/99
05/18/99
05/19/99
13290519
49.727
49.727
aliquot
1
5.46
ng/L (ppt)
1631/1630
Deuth
0.0233
1329-100
M4-538-SWB
surface water = SW
05/10/99
05/18/99
05/19/99
13290519
50.463
50.463
aliquot
1
0.966
ng/L (ppt)
1631/1630
Deuth
0.0229
1329-110
M4-556-SWB
surface water = SW
05/08/99
05/19/99
05/20/99
13290520
50.948
50.948
aliquot
1
0.690
ng/L (ppt)
1631/1630
Deuth
0.0206
1329-120
M4-566-SWB
surface water = SW
05/07/99
05/24/99
05/25/99
13290525
50.407
50.407
aliquot
1
0.326
ng/L (ppt)
1631/1630
Deuth
0.0218
NR
LIMS
Yes (28 days HT)
NR
LIMS
Yes (28 days HT)
NR
LIMS
Yes (28 days HT)
NR
LIMS
Yes (28 days HT)
1329-90
13290519
0.0142
NR
6.56
96
98.6
0.0233 and >
0.99964
1329-100
13290519
0.0142
NR
6.56
96
98.6
0.0229 and >
0.99964
1329-110
13290520
-0.035
NR
1.46
100
104
0.0206 and >
0.99958
1329-120
13290525
0.0626 *
NR
1.44
104
104
0. 02 18 and >
0.99953
NR
LIMS
Yes
NR
LIMS
Yes
NR
LIMS
Yes
NR
LIMS
Yes
                           "*" Method blank is above the true MDL, but less than 3 times the MDL.
-------
                                                        Sampling Station ID
                                      M4-500-SWB
M4-538-SWB
M4-556-SWB
M4-566-SWB
Narrative Description (Attached)
             Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results  (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation Criteria
                Applied Qualifiers [
76/Waters
X
X
X
X
X
X
X
X
76/Waters
X
X
X
X
X
X
X
X
76/Waters
X
X
X
X
X
X
X
X
76/Waters
X
X
X
X
X
X
X
X
X
X
NR
X
X
X
NR
X
X
NR
X
X
X
NR
X
X
NR
X
X
X
NR
X
X
NR
X
X
X
NR
X
X
X
NA
X
X
X
X
NA
X
X
X
X
NA
X
X
X
X
NA
X

X
X
ng/L
X
X
ng/L
X
X
ng/L
X
X
ng/L

NR
NR
NR
NR
NR
NR
NR
NR





X= Attached or Verified
Data Qualifiers

"J"  Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B" Analyte concentration in the associated blank was >3 times the MDL.
"H" Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May  1999 Samples for Critical Parameters Analyzed by Battelle
With the  10% Full QA/QC Review
Total Methylmercury in Surface Water
                                                Sampling Station ID
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
   Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
   Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                      Notes
M4-576-SWB
M4-809-SWB
M4-901-SWB
1329-130
M4-576-SWB
surface water = SW
05/04/99
05/24/99
05/25/99
13290525
50.089
50.089
aliquot
1
0.0688
ng/L (ppt)
1631/1630
Deuth
0.0219
1329-140
M4-809-SWB
surface water = SW
05/11/99
06/03/99
06/04/99
13290604
49.133
49.133
aliquot
1
1.08
ng/L (ppt)
1631/1630
Deuth
0.0216
1329-149
M4-901-SWB
surface water = SW
05/06/99
05/26/99
05/27/99
13290527
50.225
50.225
aliquot
1
1.55
ng/L (ppt)
1631/1630
Deuth
0.0198
NR
LIMS
Yes (28 days HT)
NR
LIMS
Yes (28 days HT)
NR
LIMS
Yes (28 days HT)
1329-130
13290525
0.0626 *
NR
1.44
104
104
0.0219 and >
0.99953
1329-140
13290604
-0.0008
NR
7.38
95
87.5
0.0216 and >
0.9993
1329-149
13290527
0.00799
NR
0.296
97
100.5
0.0198 and >
0.9991
NR
LIMS
Yes

NR
LIMS
Yes

NR
LIMS
Yes

"*" Method blank is above the true MDL, but less than 3 times the MDL.
-------
                                                            Sampling Station ID
                                       M4-576-SWB
M4-809-SWB
M4-901-SWB
Narrative Description (Attached)
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance (Pass/Fail)

Validation Criteria
                Applied Qualifiers [
76/Waters
X
X
X
X
X
X
X
X
76/Waters
X
X
X
X
X
X
X
X
76/Waters
X
X
X
X
X
X
X
X
X
X
NR
X
X
X
NR
X
X
NR
X
X
X
NR
X
X
NR
X
X
X
NR

X
X
X
NA
X
X
X
X
NA
X
X
X
X
NA
X

X
X
ng/L
X
X
ng/L
X
X
ng/L

NR
NR
NR
NR
NR
NR




X =  Attached or Verified


Data Qualifiers

"J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"   Analyte concentration in the associated blank was >3 times the MDL.
"H"   Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
Soil - SERC
-------
10 % Recalculated Results for Total Phosphorus in Soil/Sediment
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by njs 12/13/99
Checked by jtm 1/6/00
Sample
M4-548-SFF
M4-556-SFF
M4-566-SFF
M4-568-SFF
M4-576-SFF
M4-586-SFF
Sample
Citrus Leaves
Citrus Leaves
CCV
CCV
CCV
CCV
CCV
CCV
M4-551-SFF
M4-551-SFF-D
M4-560-SFF
M4-560-SFF-D
M4-570-SFF
M4-570-SFF-D
M4-581-SFF
M4-581-SFF-D
Blanks
Blanks
QA/QC
Batch
09-09-99 C-2
II
II
II
II
II
QA/QC
Batch
09-09-99 C-2
it
ii
ii
ii
ii
ii
ii
ii
ii
ii
ii
ii
ii
ii
ii
ii
ii
Qualifier
Note






Qualifier
Note


















Dilution
Factor






Dilution
Factor


















Weight
grams
0.0252
0.0245
0.0249
0.0254
0.0250
0.0255
Weight
grams
0.0254
0.0253






0.0251
0.0250
0.0254
0.0250
0.0250
0.0252
0.0250
0.0253


Peak Height
um
26247
6488
16474
12716
19354
4965
Peak Height
um
94650
90102
64169
67661
69660
69487
69191
69102
21188
20312
12005
10963
19409
19955
21100
18511
-681
-417
Slope
um
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
Slope
um
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
3089.1016
Sample
Results
ug/g (ppm)
337.2
85.7
214.2
162.1
250.6
63.0
Sample
Results
ug/g (ppm)
1206.3
1152.9
20.8
21.9
22.6
22.5
22.4
22.4
273.3
263.0
153.0
142.0
251.3
256.3
273.2
236.9
-0.2
-0.1
Detection
Limit
ug/g (ppm)
0.06
0.06
0.06
0.06
0.06
0.06
Detection
Limit*3
ug/g (ppm)
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18







SPK
CONC
ug/g (ppm)
1300
1300
23.23
23.23
23.23
23.23
23.23
23.23

















R%
92.79
88.68
89.42
94.29
97.07
96.83
96.42
96.30

















RPD

4.529







3.823

7.489

-1.977

14.259


-------
10 % Recalculated Results for Total Phosphorus in Soil/Sediment
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by njs 12/13/99
Checked by jtm 1/6/00
Sample
M4-501-SFF
Sample
Citrus Leaves
Citrus Leaves
CCV
CCV
M4-507-SFF
M4-507-SFF-D
Blanks
Blanks
QA/QC
Batch
09-09-99 C-l
QA/QC
Batch
09-09-99 C-l
it
ii
ii
ii
ii
ii
ii
Qualifier
Note

Qualifier
Note








Dilution
Factor
1
Dilution
Factor








Weight
grams
0.0252
Weight
grams
0.0254
0.0253


0.0249
0.0250


Peak Height
um
11374
Peak Height
um
93700
93689
60533
62707
55239
54625
-787
-503
Slope
um
2945.1703
Slope
um
2945.1703
2945.1703
2945.1703
2945.1703
2945.1703
2945.1703
2945.1703
2945.1703
Sample
Results
ug/g (ppm)
153.3
Sample
Results
ug/g (ppm)
1252.6
1257.4
20.6
21.3
753.2
741.9
-0.3
-0.2
Detection
Limit
ug/g (ppm)
0.06
Detection
Limit*3
ug/g (Ppm)
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18


SPK
CONC
ug/g (Ppm)
1300
1300
23.23
23.23






R%
96.35
96.72
88.48
91.66






RPD

-0.383

-3.528

1.519


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-------
 10 % Recalculated Results for Total Phosphorus in Soil/Sediment
Analyzed by Florida International University (SERC) for the May  1999 Dry Season (M4)
Entered by njs 12/13/99
Checked by jtm 1/6/00
Sample
M4-599-SFF
M4-809-SFF
M4-872-SFF
Sample
Citrus Leaves
Citrus Leaves
CCV
CCV
CCV
CCV
CCV
CCV
M4-607-SFF
M4-607-SFF-D
M4-619-SFF
M4-619-SFF-D
M4-868-SFF
M4-868-SFF-D
Blanks
Blanks
QA/QC
Batch
10-29-99 Cl
II
II
QA/QC
Batch
10-29-99 Cl
II
II
II
II
II
II
II
II
II
II
II
II
II
II
II
Qualifier
Note



Qualifier
Note
















Dilution
Factor
1
1
1
Dilution
Factor
















Weight
grams
0.0256
0.0249
0.0245
Weight
grams
0.0252
0.0254






0.0254
0.0253
0.0251
0.0251
0.0248
0.0250


Peak Height
um
12575
12430
10557
Peak Height
um
78667
83527
60224
64529
63127
64203
65533
64460
4084
3798
7527
8136
27687
27915
3
-268
Slope
um
2781.3245
2781.3245
2781.3245
Slope
um
2781.3245
2781.3245
2781.3245
2781.3245
2781.3245
2781.3245
2781.3245
2781.3245
2781.3245
2781.3245
2781.3245
2781.3245
2781.3245
2781.3245
2781.3245
2781.3245
Sample
Results
ug/g (ppm)
176.6
179.5
154.9
Sample
Results
ug/g (ppm)
1122.4
1182.3
21.7
23.2
22.7
23.1
23.6
23.2
57.8
54.0
107.8
116.5
401.4
401.5
0.0
-0.1
Detection
Limit
ug/g (ppm)
0.06
0.06
0.06
Detection
Limit*3
ug/g (ppm)
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18




SPK
CONC
ug/g (ppm)
1300
1300
23.23
23.23
23.23
23.23
23.23
23.23












R%
86.34
90.95
93.21
99.87
97.70
99.37
101.43
99.77












RPD

-5.203







6.863

-7.776

-0.017


"J"  Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject" Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
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M4-533-SFF

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| M4-556-SFF

o>
(N
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a\
(N
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OO
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(N
0
0
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4
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4
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PH
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0
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(N
0
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m
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Q
PH
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GO
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F~
F~
t~
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0
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00
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O
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0

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0
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M4-576-SFF

8
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(N
0
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0
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GO
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t>
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4
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0
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oo
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m
0

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0
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t^

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OO
o
W~)

(N
S
O
a\
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m
^0
t>
^sO
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(N
0
0
5
s
b
P
PH
PH
GO
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a\
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4
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<:
a
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o

g
o
m
o
(N
O
0
^sO
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^D
S
o
•n
(N
0
0
m
?
s
b
P
CM
Q
PH
PH
GO
O
c\
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4
S
<;
a

S
OO
^sO
^t
(N
OO
^sO
0
^sO
t^
m
oo
m
o
oo
o
o
0
0
t^

t^

PH
PH
GO
4
c\

•^t
(N
O>
0
^sO
oo
oo
oo
o
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(N
(N
O
o
0
t^
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0

o
o
o
0
a\
(N
0
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m
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(N
0
0
(N
O
t>

| M4-809-SFF

5
^t
c\
a\
0
NO
"O
^D
W~)
O
O
^t
o
o
0
o
oo
s
(N
•n
(N
0
0
m
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oo
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PH
PH
GO
OO
4
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<:
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•^t
OO
NO
c\
0
NO
rn
(N
m
o
o
oo
o
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0
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t^
m

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(N
0
0
fs
00
s

fe
fe
C/3
i
4
S;
<:
a
o
rn
0
-------
10 % Recalculated Results for Bulk Density in Soil/Sediment
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by njs 12/16/99
Checked by jtm 01/06/00
Sample
M4-501-SFF
M4-508-SFF
M4-533-SFF
M4-538-SFF
M4-548-SFF
M4-556-SFF
M4-566-SFF
M4-568-SFF
M4-576-SFF
M4-586-SFF
M4-594-SFF
M4-599-SFF
M4-809-SFF
M4-872-SFF
QA/QC
Batch
09-09-99 C-2
11
11
11
11
11
11
11
11
11
11
11
11
"
Qualifier
Note
*
*
*
*
*
*
*
*
*
*
*
*
*
*
CupWt
(g)
10.52172
10.52172
10.52172
10.52172
10.52172
10.52172
10.52172
10.52172
10.52172
10.52172
10.52172
10.52172
10.52172
10.52172
Sample Volume
(mL)
80
60
80
80
70
70
60
60
90
80
60
40
60
70
Cup +
Wet Sediment (g)
90.6780
85.1097
92.6565
93.0177
77.1153
91.0047
81.8973
77.0048
110.6919
100.647
98.4345
88.1801
78.9859
92.1029
Sample Wet
Weight (g)
80.1563
74.5880
82.1348
82.4960
66.5936
80.4830
71.3756
66.4831
100.1702
90.1253
87.9128
77.6584
68.4642
81.5812
Vol/Weight
Ratio
0.9981
0.8044
0.9740
0.9697
1.0512
0.8697
0.8406
0.9025
0.8985
0.8877
0.6825
0.5151
0.8764
0.8580
Dried Cup +
Dried Sed (g)
14.8775
14.2825
18.6297
26.2454
15.4151
24.4034
19.7691
16.7999
22.6543
47.0813
22.1843
17.9186
14.7799
21.6815
Bulk Density
g/mL
0.0544
0.0627
0.1013
0.1965
0.0699
0.1983
0.1541
0.1046
0.1348
0.4570
0.1944
0.1849
0.0710
0.1594
EPA Prep
Dilution
0.40
0.25
0.50
0.40
0.67
1.00
0.50
0.33
1.00
1.00
0.67
0.40
0.33
1.00
Corrected Bulk
Density g/mL
0.14
0.25
0.20
0.49
0.10
0.20
0.31
0.32
0.13
0.46
0.29
0.46
0.22
0.16
  There are no duplicates/replicates reported with this parameter set.
-------
 10 % Recalculated Results for Methylmercury in Soil Samples Analyzed by
Florida International University Laboratory for the May 1999 Dry Season (M4)
Entered by mwb 02/02/00 Checked By: njs 04-12-00
Sampling Station
ID
M4-501-SDF-A
M4-501-SDF-B
M4-501-SDF-C
M4-501-SDF-D
Correlation Coefficient
Blank- 1
Blank-2
ccv

M4-533-SDF-A
M4-533-SDF-B
M4-533-SDF-C
M4-533-SDF-D
Correlation Coefficient
Blank- 1
Blank-2
ccv
ccv

M4-548-SDF-A
M4-548-SDF-B
M4-548-SDF-C
M4-548-SDF-D
M4-556-SDF-A
M4-556-SDF-B
M4-556-SDF-C
M4-556-SDF-D
Correlation Coefficient
Blank- 1
Blank-2
ccv
ccv
ccv

Data Qualifier
Note
"H"
"H"
"H"
"H"
"NR"




"H"
"H"
"H"
"H", "M"
"NR"





"H"
"H"
"H"
"H"
"H"
"H"
"H"
"H", "M"
"NR"






QC
Batch
32000a
32000a
32000a
32000a
32000a
32000a
32000a
32000a

032400b
032400b
032400b
032400b
032400b
032400b
032400b
32000a
32000a

80699
80699
80699
80699
80699
80699
80699
80699
80699
80699
80699
80699
80699
80699

Wet
Sample
Weight (g)
4.650
4.046
5.910
6.463





4.602
4.753
4.697
4.246






4.475
4.095
4.073
4.088
4.190
4.153
4.467
4.718







Dry/Wet
Weight
Ratio
0.028
0.028
0.028
0.028





0.129
0.129
0.129
0.129






0.0745
0.0745
0.0745
0.0745
0.171
0.171
0.171
0.171







First
Extraction
Volume(ml)
4
4
3.8
4

4.8
3.2


4
4
3.8
4

4
4



3.6
3.6
2.2
3.0
3.4
3.0
2.9
5.0

5.0
3.3




Back
Extraction
Volume(ml)
0.6
0.6
0.6
0.6

0.6
0.6
0.6

0.6
0.6
0.6
0.6

0.6
0.6
0.6
0.6

0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.8

0.8
0.8




Final
Extraction
Volume(ul)
200
200
200
200

200
200
200

200
200
200
200

200
200
200
200

200
200
200
200
200
200
200
200

200
200




Spiked
Concentration
(ng/g)


4.530
4.140



3.75



1.800
1.990



2.5
2.5



3.30
3.28


1.31
1.24



3.75
3.75
3.75

MeHg
Peak
Area
4.63
1.54
6.99
8.76

0.00
0.00
4.670

0.00
0.00
2.86
2.86

0.00
0.00
5.270
4.960

1.52
0.86
4.65
4.56
1.27
0.60
3.06
4.23

0.00
0.00
7.10
2 42
9.65

Y intercept
0.12
0.12
0.12
0.12



0.228

-0.049
-0.049
-0.049
-0.049



-0.049
-0.049

-0.072
-0.072
-0.072
-0.072
-0.072
-0.072
-0.072
-0.072

-0.072
-0.072
-0.072
-0.072
-0.072

Slope
1.730
1.730
1.730
1.730



1.296

2.360
2.360
2.360
2.360



2.360
2.360

1.821
1.821
1.821
1.821
1.821
1.821
1.821
1.821

1.821
1.821
1.821
1.821
1.821

MeHg
Concentration
(ng/g)
8.56
3.27
10.71
11.66



3.60

0.00
0.00
0.88
0.92



2.23
2.10

0.87
0.54
4.78
3.43
0.36
0.19
0.95
0.72



3.90
1.33
5.30

RPD

89.38

-8.49






0.00

-4.96







47.17

33.03

59.71

27.39







Average
MeHg Cone.
(ng/g)

5.92

11.18






0.00

0.90







0.70

4.10

0.28

0.83







Standard
Deviation


































%R



121.44



96.09




47.47



89.32
84.07




103.35



43.80



103.97
35.44
141.31

Final
Result
ng/g



4.87

0
0





0.00

0
0






0.68



0.63







Data Qualifiers
"H" Analysis digestion performed after holding times have expired.
"M" Analyte exhibits potential matrix effect based on matrix spike recovery outside of 70 to 130% range.
"NR"  Not Reviewed.
-------
 10 % Recalculated Results for Methylmercury in Soil Samples Analyzed by
Florida International University Laboratory for the May  1999 Dry Season (M4)
Entered by mwb 02/02/00
Sampling Station
ID
M4-566-SDF-A
M4-566-SDF-B
M4-566-SDF-C
M4-566-SDF-D
Correlation Coefficient
Blank- 1
Blank-2
ccv
ccv

M4-568-SDF-A
M4-568-SDF-B
M4-568-SDF-C
M4-568-SDF-D
Correlation Coefficient
Blank- 1
Blank-2
ccv

M4-576-SDF-A
M4-576-SDF-B
M4-576-SDF-C
M4-576-SDF-D
Correlation Coefficient
Blank- 1
Blank-2
ccv
ccv

M4-586-SFF-A
M4-586-SFF-B
M4-586-SFF-C
M4-586-SFF-D
Correlation Coefficient
Blank- 1
Blank-2
ccv
Data Qualifier
Note
"H"
"H"
"H"
"H"
"NR"


"DQO"
"DQO"

"H"
"H"
"H"
"H"
"NR"


"NR"

"H"
"H"
"H"
"H"
"NR"





"H"
"H"
"H"
"H", "M"
"NR"



QC
Batch
81299
81299
81299
81299
81299
81299
81299
81299
81299

121499
121499
121499
121499
121499
121499
121499
121499

32600
32600
32600
32600
32600
32600
32600
32600
32600

82099
82099
82099
82099
82099
82099
82099
82099
Wet
Sample
Weight (g)
5.557
5.435
5.400
5.156






4.181
3.423
5.350
4.482





4.624
4.560
4.240
6.438






4.302
4.217
4.263
5.321




Dry/Wet
Weight
Ratio
0.13
0.13
0.13
0.13






0.0727
0.0727
0.0727
0.0727





0.111
0.111
0.111
0.111






0.327
0.327
0.327
0.327




First
Extraction
Volume(ml)
3.2
3.4
3.2
3.2

4
3.8



3.6
3.0
3.0
3.0

4.0
4.0


4.0
3.6
4.0
3.2

4.0
4.0



1.6
2.4
2 2
2.0

4.0
4.0

Back
Extraction
Volume(ml)
0.8
0.8
0.8
0.8

0.8
0.8



0.8
0.8
0.8
0.8

0.8
0.8


0.6
0.6
0.6
0.6

0.6
0.6



0.8
0.8
0.8
0.8

0.8
0.8

Final
Extraction
Volume(ul)
200
200
200
200

200
200
200
200

200
200
200
200

200
200


200
200
200
200

200
200



200
200
200
200

200
200

Spiked
Concentration
(ng/g)


1.07
1.12



2.5
2.5



1.93
2.30







1.59
1.05



2.5
2.5



0.54
0.43



2.5
MeHg
Peak
Area
4.58
2.00
7.74
6.53

0.00
0.00
7.750
7.640

0.00
0.00
5.11
4.48

0.00
0.00


4.92
3.91
8.30
7.71

0.00
0.00
4.95
4.03

0.00
0.00
0.50
0.52

0
0
2.91
Y intercept
1.011
1.011
1.011
1.011



1.011
1.011

0.42
0.42
0.42
0.42

0.42
0.42


0.18
0.18
0.18
0.18

0.18
0.18
0.18
0.18

-0.436
-0.436
-0.436
-0.436

-0.436
-0.436
-0.436
Slope
1.94
1.94
1.94
1.94



1.94
1.94

2.13
2.13
2.13
2.13

2.13
2.13


1.85
1.85
1.85
1.85

1.85
1.85
1.85
1.85

1.430
1.430
1.430
1.430

1.430
1.430
1.430
MeHg
Concentration
(ng/g)
1.28
0.54
2 22
1.96



3.99
3.94

0.00
0.00
2.57
2.69





2.16
1.93
3.97
3.04



2.68
2.18

0.00
0.00
0.14
0.13



2.03
RPD

81.65

12.36







0.00

-4.54






11.04

26.67







0.00

8.71




Average
MeHg Cone.
(ng/g)

0.91

2.09







0.00

2.63






2.05

3.50







0.00

0.14




Standard
Deviation





































%R



108.16



159.79
157.53




124.34








110.50



107.03
87.14




28.16



81.40
Final
Result
ng/g



0.84

0
0






0.00

0
0





1.85

0
0






0.00

0
0

Data Qualifiers
"H" Analysis digestion performed after holding times have expired.
"M" Analyte exhibits potential matrix effect based on matrix spike recovery outside of 70 to 130% range.
"NR" Not Reviewed.
-------
 10 % Recalculated Results for Methylmercury in Soil Samples Analyzed by
Florida International University Laboratory for the May 1999 Dry Season (M4)
Entered by mwb 02/02/00
Sampling Station
ID
M4-594-SFF-A
M4-594-SFF-B
M4-594-SFF-C
M4-594-SFF-D
Correlation Coefficient
Blank- 1
Blank-2
ccv

M4-599-SFF-A
M4-599-SFF-B
M4-599-SFF-C
M4-599-SFF-D
Correlation Coefficient
Blank- 1
Blank-2
ccv
ccv

M4-809-SFF-A
M4-809-SFF-B
M4-809-SFF-C
M4-809-SFF-D
Correlation Coefficient
Blank- 1
Blank-2
ccv
ccv
ccv
ccv

M4-872-SDF-A
M4-872-SDF-B
M4-872-SDF-C
M4-872-SDF-D
Correlation Coefficient
Blank- 1
Blank-2
ccv

Data Qualifier
Note
"H"
"H"
"H"
"H"
"NR"




"H"
"H"
"H"
"H"
"NR"





"H"
"H"
"H"
"H", "M"
"NR"







"H"
"H"
"H"
"H"
"NR"


"NR"

QC
Batch
121599
121599
121599
121599
121599
121599
121599
121599

32500
32500
32500
32500
32500
32500
32500
32500
32500

91099
91099
91099
91099
91099
91099
91099
91099
91099
91099
91099

032800b
032800b
032800b
032800b
032800b
032800b
032800b
032800b

Wet
Sample
Weight (g)
4.296
4.078
4.985
4.492





4.440
5.363
6.011
5.235






5.473
5.544
5.194
5.326








4.517
4.562
4.351
4.722





Dry/Wet
Weight
Ratio
0.105
0.105
0.105
0.105





0.102
0.102
0.102
0.102






0.0416
0.0416
0.0416
0.0416








0.119
0.119
0.119
0.119





First
Extraction
Volume(ml)
3.2
3.6
3.4
3.2

4.0
4.0


3.8
4
4
4

4.0
4.0



3.8
3.6
3.8
3.6

4.0
4.0





4.0
4.0
4.0
4.0

4.0
4.0


Back
Extraction
Volume(ml)
0.8
0.8
0.8
0.6

0.8
0.8


0.6
0.6
0.6
0.6

0.6
0.6



0.8
0.8
0.8
0.8

0.8
0.8





0.6
0.6
0.6
0.6

0.8
0.8


Final
Extraction
Volume(ul)
200
200
200
200

200
200


200
200
200
200

200
200



200
200
200
200

200
200





200
200
200
200

200
200


Spiked
Concentration
(ng/g)


1.430
1.590



3.75



1.220
1.400



2.5
2.5



3.47
3.39



3.75
3.75
3.75
3.75



1.45
1.33





MeHg
Peak
Area
2.49
3.94
7.09
4.96

0.00
0.00
5.940


2.57
7.68
9.09

0.00
0.00
5.270
7.660

0.00
0.00
1.77
1.75



6.80
6.22
7.35
5.71

0.83
1.39
7.44
7.97

0.00
0.00


Y intercept
0.39
0.39
0.39
0.39

0.39
0.39
0.39

-0.09
-0.09
-0.09
-0.09

-0.09
-0.09
-0.09
-0.09

0.289
0.289
0.289
0.289

0.289
0.289
0.289
0.289
0.289
0.289

0.08
0.08
0.08
0.08

0.42
0.42


Slope
2.09
2.09
2.09
2.09

2.09
2.09
2.09

2.47
2.47
2.47
2.47

2.47
2.47
2.47
2.47

2.168
2.168
2.168
2.168

2.168
2.168
2.168
2.168
2.168
2.168

3.82
3.82
3.82
3.82

2.13
2.13


MeHg
Concentration
(ng/g)
1.03
1.53
2.38
2.62



2.84


0.79
2.11
2.87



2.13
3.10

0.00
0.00
1.24
1.27



3.14
2.87
3.39
2.63

0.17
0.28
1.57
1.55





RPD

-38.82

-9.51








-30.44







0.00

-1.76









-49.52

1.30





Average
MeHg Cone.
(ng/g)

1.28

2.50






0.79

2.49







0.00

1.25









0.22

1.56





Standard
Deviation








































%R



80.89



75.79




129.76



85.34
124.05




36.56



83.64
76.51
90.41
70.23




95.92





Final
Result
ng/g



1.58

0
0





0.61

0
0






0.00

0
0








0.23

0
0


Data Qualifiers
"H" Analysis digestion performed after holding times have expired.
"M" Analyte exhibits potential matrix effect based on matrix spike recovery outside of 70 to 130% range.
"NR" Not Reviewed.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID    M4-501-SFF
Soil/Sediment
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
            Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
            Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Calibration % R (high and low range^
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
               QC Limits Met

                      Notes
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
5-1 1-99/No Time
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
5-11-99/NoTime
03/20/00
03/20/00
X
SD = SF = S = Soil
5-1 1-99/No Time
09/03/99
09/09/99
The Batch Numbers are referenced by the Sample ID range. They are s





ppm
CVAF


4.65, 4.046 g
200ul
aliquot
See Worksheets
4.87
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
153.3
ug/g
EPA 365.1
Angel
0.06

X
SD = SF = S = Soil
5-1 1-99/No Time
06/25/99
06/25/99
lecific to this project.
0.025 g
0.025 g
0.025 g
NA
0.9608
%
ASTM D2974-87
SG/JL


X
SD = SF = S = Soil
5-1 1-99/No Time
NA
Not Provided

80
80
80
NA
0.0544
g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL


28 days
SOP
Yes
No (Goal Only)
Yes
X
No (Goal Only)
Yes
X
NA
Yes
X
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID








32000a
NA
yes
89.38
121.44
96.09
0.2 ng/g and>
NR
9-9-99 C-l
NA in Soils
-0.3, -0.2
<20 RPD
96%R
88 - 92%R
60 ppm and >
0.996

06/25/99
NA
NA
None Reported
NA
NA
NA
NA

Not Provided
NA
NA
None Reported
NA
NA
NA
NA


Battelle Lab
SOP
Yes
"DQO"

Yes Y
X ]
"DQO

es Yes
< X
(NR)11 "DQO (NR)"

No descriptive narratives were provided by FIU.
Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
Total Phosphorus and MEHG were digested past the holding time. Holding time is a goal only.
Some analysis for AFDW were Re-Run based on negative numbers reported, but no QA/QC batches were re-run.
No duplicate/replicate measurements were taken with the Bulk Density analysis.
-------
                     Station ID     M4-501-SFF
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID  Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
The Narrative Section will be written after all of the analyses are completed













































X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC





Yes
Yes
Yes
Yes
Yes
X
X
X
X
X
X
X
NA
X
X
X
X
NA
X
X




Yes
Yes
ng/g
X
X
Ug/g
X
X
%
X
X
g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
               Applied Qualifiers |_
"DQO"
"DQO (NR)11
"DQO (NR)11
Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
11 R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
            Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
            Duplicates  (RPD)
Matrix Spike Recoveries (75-125)
    Calibration % R (high and low range^
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analys!
        All Calculation Checked
               QC Limits Met

                      Notes
M4-508-SFF Soil/Sediment
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
5-11-99/NoTime
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
5-1 1-99/No Time
No Analysis Performed

X
SD = SF = S = Soil
5-11-99/NoTime
09/03/99
10/01/99
The Batch Numbers are referenced by the Sample ID range. They are s





ppm
CVAF






No Analysis Performed




0.025 g
0.025 g
Aliquot
1
291.7
ug/g
EPA 365.1
Angel
0.06

X
SD = SF = S = Soil
5-1 1-99/No Time
06/25/99
06/25/99
lecific to this project.
0.025 g
0.025 g
0.025 g
NA
0.9713
%
ASTM D2974-87
SG/JL


X
SD = SF = S = Soil
5-1 1-99/No Time
NA
Not Provided

80
80
80
NA
0.0627
g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL


28 days



Yes
X
No (Goal Only)
Yes
X
NA
Yes
X
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
















10-1-99C-1
NA in Soils
None Reported
<20RPD
98 - 102%R
96-102 %R
60 ppm and >
0.998

06/25/99
NA
NA
None Reported
NA
NA
NA
NA

Not Provided
NA
NA
None Reported
NA
NA
NA
NA


Battelle Lab



Yes Y
X ]
"B (NR)" "DQO

es Yes
< X
(NR)" "DQO (NR)"

No descriptive narratives were provided by FIU.
Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
Total Phosphorus and MEHG were digested past the holding time. Holding time is a goal only.
Some analysis for AFDW were Re-Run based on negative numbers reported, but no QA/QC batches were re-run.
No duplicate/replicate measurements were taken with the Bulk Density analysis.
There is no analysis for MeHg.
-------
                     Station ID     M4-508-SFF
             Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID  Transferred
          All Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance (Pass/Fail)

Validation Criteria
               Applied Qualifiers I
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
The Narrative Section will be written after all of the analyses are completed













































X
X
Not Noted
Date/No Time




X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC


Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC










X
X
X
X
X
X
X
NA
X
X
X
X
NA
X
X







X
X
Ug/g
X
X
%
X
X
g/mL

NA
NA


NA
NA
NA
NA
NA
NA
"B (NR)"
"DQO (MR)"
"DQO (NR)"
Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 "  Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X " = Attached or Verified
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID    M4-533-SFF
Soil/Sediment
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
            Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
            Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Calibration % R (high and low range^
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
               QC Limits Met

                      Notes
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
5-10-99/NoTime
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
5-10-99/NoTime
03/24/00
03/24/00
X
SD = SF = S = Soil
5-10-99/NoTime
09/03/99
10/01/99
The Batch Numbers are referenced by the Sample ID range. They are s





ppm
CVAF


4.602, 4.753
200ul
aliquot
See Worksheets
0
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
231.2
Ug/g
EPA 365.1
Angel
0.06

X
SD = SF = S = Soil
5-10-99/NoTime
06/25/99
06/25/99
lecific to this project.
0.025 g
0.025 g
0.025 g
NA
0.9261
%
ASTM D2974-87
SG/JL


X
SD = SF = S = Soil
5-10-99/NoTime
NA
Not Provided

80
80
80
NA
0.1013
g/mL
ASTM D453 1-86
SG/JL
0.001 g/cc


28 days
SOP
Yes
No (Goal Only)
Yes
X
No (Goal Only)
Yes
X
NA
Yes
X
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID








032400b
NA
yes
0
47.47
89.32, 84.07
0.2 ng/g and>
0.9913
10-1-99C-1
NA in Soils
None Reported
<20 RPD
98 - 102%R
96-102 %R
60 ppm and >
0.998

06/25/99
NA
NA
<20RPD
NA
NA
NA
NA

Not Provided
NA
NA
None Reported
NA
NA
NA
NA


Battelle Lab
SOP
Yes
"M"

Yes Y
X ]
"B (NR)"

es Yes
< X
"DQO (NR)11

No descriptive narratives were provided by FIU.
Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
Total Phosphorus and MEHG were digested past the holding time. Holding time is a goal only.
Some analysis for AFDW were Re-Run based on negative numbers reported, but no QA/QC batches were re-run.
No duplicate/replicate measurements were taken with the Bulk Density analysis.
-------
                     Station ID     M4-533-SFF
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
The Narrative Section will be written after all of the analyses are completed













































X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC





Yes
Yes
Yes
Yes
Yes
X
X
X
X
X
X
X
NA
X
X
X
X
NA
X
X




Yes
Yes
ng/g
X
X
Ug/g
X
X
%
X
X
g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
               Applied Qualifiers |_
"B (NR)"
"DQO (MR)"
Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID    M4-538-SFF
Soil/Sediment
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analysl
       All Calculation Checked
            Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
            Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Calibration % R (high and low range^
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analysl
       All Calculation Checked
               QC Limits Met

                      Notes
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
5-10-99/NoTime
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
5-10-99/NoTime
No Analysis Performed

X
SD = SF = S = Soil
5-10-99/NoTime
09/03/99
10/01/99
The Batch Numbers are referenced by the Sample ID range. They are s





ppm
CVAF






No Analysis Performec




0.025 g
0.025 g
Aliquot
1
105.6
ug/g
EPA 365.1
Angel
0.06

X
SD = SF = S = Soil
5-10-99/NoTime
06/25/99
06/25/99
>ecific to this project.
0.025 g
0.025 g
0.025 g
NA
0.48
%
ASTM D2974-87
SG/JL


X
SD = SF = S = Soil
5-10-99/NoTime
NA
Not Provided

80
80
80
NA
0.1965
g/mL
ASTM D453 1-86
SG/JL
0.001 g/cc


28 days



Yes
X
No (Goal Only)
Yes
X
NA
Yes
X
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
















10-1-99C-1
NA in Soils
None Reported
<20 RPD
98 - 102%R
96-102 %R
60 ppm and >
0.998

06/25/99
NA
NA
<20RPD
NA
NA
NA
NA

Not Provided
NA
NA
None Reported
NA
NA
NA
NA


Battelle Lab



Yes Y
X 3
"B (NR)"

es Yes
< X
"DQO (NR)"

No descriptive narratives were provided by FIU.
Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
Total Phosphorus and MEHG were digested past the holding time. Holding time is a goal only.
Some analysis for AFDW were Re-Run based on negative numbers reported, but no QA/QC batches were re-run.
No duplicate/replicate measurements were taken with the Bulk Density analysis.
-------
                     Station ID    M4-538-SFF
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
The Narrative Section will be written after all of the analyses are completed













































X
X
Not Noted
Date/No Time




X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC


Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC










X
X
X
X
X
X
X
NA
X
X
X
X
NA
X
X







X
X
ug/g
X
X
%
X
X
g/mL

NA
NA


NA
NA
NA
NA
NA
NA
Validation Criteria
               Applied Qualifiers |_
"B (NR)"
"DQO (NR)"
Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID    M4-548-SFF
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analysl
       All Calculation Checked
            Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
            Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Calibration % R (high and low range^
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analysl
       All Calculation Checked
               QC Limits Met

                      Notes
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
5-9-99/No Time
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
5-9-99/No Time
08/06/99
08/06/99
X
SD = SF = S = Soil
5-9-99/No Time
09/03/99
09/09/99
The Batch Numbers are referenced by the Sample ID range. They are s





ppm
CVAF


4.475g,4.095g
200ul
aliquot
See Worksheet
0.68
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
337.2
Ug/g
EPA 365.1
Angel
0.06

X
SD = SF = S = Soil
5-9-99/No Time
06/25/99
06/25/99
>ecific to this project.
0.025 g
0.025 g
0.025 g
NA
0.91
%
ASTM D2974-87
SG/JL


X
SD = SF = S = Soil
5-9-99/No Time
NA
Not Provided

80
80
80
NA
0.0699
g/mL
ASTM D453 1-86
SG/JL
0.001 g/cc


28 days
SOP
Yes
No (Goal Only)
Yes
X
No (Goal Only)
Yes
X
NA
Yes
X
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID








80699
NA
yes
47.17
103.35
103.97,35.44, 141.31
0.2 ng/g and>
0.9963
9-9-99 C-2
NA in Soils
-0.1, -0.2
<20 RPD
89 - 93%R
89 - 97%R
60 ppm and >
0.9969

06/25/99
NA
NA
<20RPD
NA
NA
NA
NA

Not Provided
NA
NA
None Reported
NA
NA
NA
NA


Battelle Lab
SOP
Yes
11 DQO "
Yes Y
X 3


es Yes
< X
"DQO (NR)"

No descriptive narratives were provided by FIU.
Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
Total Phosphorus and MEHG were digested past the holding time. Holding time is a goal only.
Some analysis for AFDW were Re-Run based on negative numbers reported, but no QA/QC batches were re-run.
No duplicate/replicate measurements were taken with the Bulk Density analysis.
-------
                    Station ID    M4-548-SFF
  M4-548-SDF
Soil/Sediment
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                    Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                    Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
           Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                    Organization
          Performance  (Pass/Fail)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
The Narrative Section will be written after all of the analyses are completed













































X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC





Yes
Yes
Yes
Yes
Yes
X
X
X
X
X
X
X
NA
X
X
X
X
NA
X
X




Yes
Yes
ng/g
X
X
Ug/g
X
X
%
X
X
g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
               Applied Qualifiers |_
     "DQO"
"DQO (NR)"
Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID    M4-556-SFF
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
            Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
            Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Calibration % R (high and low range^
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
               QC Limits Met

                      Notes
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
5-1 1-99/No Time
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil

08/06/99
08/06/99
X
SD = SF = S = Soil
5-8-99/No Time
09/03/99
09/09/99
The Batch Numbers are referenced by the Sample ID range. They are s





ppm
CVAF


4.190g,4.153g
200ul
aliquot
Blending Dilution
0.63
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
85.7
ug/g
EPA 365.1
Angel
0.06

X
SD = SF = S = Soil
5-11-99/NoTime
06/25/99
06/25/99
lecific to this project.
0.025 g
0.025 g
0.025 g
NA
0.4567
%
ASTM D2974-87
SG/JL


X
SD = SF = S = Soil
5-1 1-99/No Time
NA
Not Provided

80
80
80
NA
0.1983
g/mL
ASTM D453 1-86
SG/JL
0.001 g/cc


28 days
SOP
Yes
No (Goal Only)
Yes
X
No (Goal Only)
Yes
X
NA
Yes
X
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID








80699
yes
NA
59.71
43.8
103.97,35.44, 141.31
0.2 ng/g and>
0.9963
9-9-99 C-2
NA in Soils
-0.1, -0.2
<20 RPD
89 - 93%R
89 - 97%R
60 ppm and >
0.9969

06/25/99
NA
NA
<20RPD
NA
NA
NA
NA

Not Provided
NA
NA
None Reported
NA
NA
NA
NA


Battelle Lab
SOP
Yes
"M", "DQO"
Yes Y
X ]


es Yes
< X
"DQO (NR)"

No descriptive narratives were provided by FIU.
Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
Total Phosphorus and MEHG were digested past the holding time. Holding time is a goal only.
Some analysis for AFDW were Re-Run based on negative numbers reported, but no QA/QC batches were re-run.
No duplicate/replicate measurements were taken with the Bulk Density analysis.
For MeHg samples, a matrix spike is performed with every sample and is used to correct the results for loss of analyte.
-------
                     Station ID     M4-556-SFF
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
The Narrative Section will be written after all of the analyses are completed













































X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC





Yes
Yes
Yes
Yes
Yes
X
X
X
X
X
X
X
NA
X
X
X
X
NA
X
X




Yes
Yes
ng/g
X
X
Ug/g
X
X
%
X
X
g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
               Applied Qualifiers |_
"M", "DQO"
"DQO (NR)"
Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID    M4-566-SFF
Soil/Sediment
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analysl
       All Calculation Checked
            Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
            Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Calibration % R (high and low range^
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analysl
       All Calculation Checked
               QC Limits Met

                      Notes
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
5-7-99/No Time
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
5-7-99/No Time
08/12/99
08/13/99
X
SD = SF = S = Soil
5-7-99/No Time
09/03/99
09/09/99
The Batch Numbers are referenced by the Sample ID range. They are s





ppm
CVAF


5.557, 5.435
200 ul
aliquot
See Worksheets
0.84
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
214.2
Ug/g
EPA 365.1
Angel
0.06

X
SD = SF = S = Soil
5-7-99/No Time
06/25/99
06/25/99
>ecific to this project.
0.025 g
0.025 g
0.025 g
NA
0.8627
%
ASTM D2974-87
SG/JL


X
SD = SF = S = Soil
5-7-99/No Time
NA
Not Provided

80
80
80
NA
0.1541
g/mL
ASTM D453 1-86
SG/JL
0.001 g/cc


28 days
SOP
Yes
No (Goal Only)
Yes
X
No (Goal Only)
Yes
X
NA
Yes
X
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID








81299
NA
yes
81.65
108.16
159
0.2 ng/g and>
0.9566
9-9-99 C-2
NA in Soils
-0.1, -0.2
<20 RPD
89 - 93%R
89 - 97%R
60 ppm and >
0.9969

06/25/99
NA
NA
<20RPD
NA
NA
NA
NA

Not Provided
NA
NA
None Reported
NA
NA
NA
NA


Battelle Lab
SOP
Yes
"M", "DQO"
Yes
X


Yes
X


Yes
X
"DQO (NR)"

No descriptive narratives were provided by FIU.
Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
Total Phosphorus and MEHG were digested past the holding time. Holding time is a goal only.
Some analysis for AFDW were Re-Run based on negative numbers reported, but no QA/QC batches were re-run.
No duplicate/replicate measurements were taken with the Bulk Density analysis.
For MeHg samples, a matrix spike is performed with every sample and is used to correct the results for loss of analyte.
-------
                     Station ID     M4-566-SFF
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
The Narrative Section will be written after all of the analyses are completed













































X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC





Yes
Yes
Yes
Yes
Yes
X
X
X
X
X
X
X
NA
X
X
X
X
NA
X
X




Yes
Yes
ng/g
X
X
Ug/g
X
X
%
X
X
g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
               Applied Qualifiers |_
"M", "DQO"
"DQO (NR)"
Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the  10% Full QA/QC Review
                 Station ID    M4-568-SFF
Soil/Sediment
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analysl
        All Calculation Checked
            Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
            Duplicates  (RPD)
Matrix Spike Recoveries (75-125)
    Calibration % R (high and low range^
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analysl
        All Calculation Checked
               QC Limits Met

                      Notes
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
5-7-99/No Time
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
5-7-99/No Time
12/14/99
12/14/99
X
SD = SF = S = Soil
5-7-99/No Time
09/03/99
09/09/99
The Batch Numbers are referenced by the Sample ID range. They are s





ppm
CVAF


4.181g,3.423g
200ul
aliquot
Blending Dilution
0
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
162.1
ug/g
EPA 365.1
Angel
0.06

X
SD = SF = S = Soil
5-7-99/No Time
06/25/99
06/25/99
lecific to this project.
0.025 g
0.025 g
0.025 g
NA
0.87
%
ASTM D2974-87
SG/JL


X
SD = SF = S = Soil
5-7-99/No Time
NA
Not Provided

80
80
80
NA
0.1046
g/mL
ASTM D453 1-86
SG/JL
0.001 g/cc


28 days
SOP
Yes
No (Goal Only)
Yes
X
No (Goal Only)
Yes
X
NA
Yes
X
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID








121499
NA
yes
0.00
124.34
NR
0.2 ng/g and >
NR
9-9-99 C-2
NA in Soils
-0.1, -0.2
<20RPD
89 - 93%R
89 - 97%R
60 ppm and >
0.9969

06/25/99
NA
NA
<20 RPD
NA
NA
NA
NA

Not Provided
NA
NA
None Reported
NA
NA
NA
NA


Battelle Lab
SOP
Yes
"DQO"
Yes
X


Yes
X


Yes
X
"DQO (NR)"

No descriptive narratives were provided by FIU.
Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
Total Phosphorus and MEHG were digested past the holding time. Holding time is a goal only.
Some analysis for AFDW were Re-Run based on negative numbers reported, but no QA/QC batches were re-run.
No duplicate/replicate measurements were taken with the Bulk Density analysis.
For MeHg samples, a matrix spike is performed with every sample and is used to correct the results for loss of analyte.
-------
                     Station ID     M4-568-SFF
             Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID  Transferred
          All Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance (Pass/Fail)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
The Narrative Section will be written after all of the analyses are completed









Narrative summaries will be written following the completion on the data analysis
































X
X
Not Noted
Date/No Time
FIU/SERC Laboratory

Internal COC
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
Is the same as station ID
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC





Yes
Yes
Yes
Yes
Yes
X
X
X
X
X
X
X
NA
X
X
X
X
NA
X
X




Yes
Yes
ng/g
X
X
Ug/g
X
X
%
X
X
g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
               Applied Qualifiers |_
"DQO"
"DQO (NR)"
Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 "  Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X " = Attached or Verified
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID    M4-576-SFF
Soil/Sediment
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
            Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
            Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Calibration % R (high and low range^
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
               QC Limits Met

                      Notes
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
5-4-99/No Time
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
5-4-99/No Time
03/26/00
03/26/00
X
SD = SF = S = Soil
5-4-99/No Time
09/03/99
09/09/99
The Batch Numbers are referenced by the Sample ID range. They are s





ppm
CVAF


4.624
4.56
aliquot
See Worksheet
1.85
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
250.61
ug/g
EPA 365.1
Angel
0.06

X
SD = SF = S = Soil
5-4-99/No Time
06/25/99
06/25/99
lecific to this project.
0.025 g
0.025 g
0.025 g
NA
0.7171
%
ASTM D2974-87
SG/JL


X
SD = SF = S = Soil
5-4-99/No Time
NA
Not Provided

80
80
80
NA
0.1348
g/mL
ASTM D453 1-86
SG/JL
0.001 g/cc


28 days
SOP
Yes
No (Goal Only)
Yes
X
No (Goal Only)
Yes
X
NA
Yes
X
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID








32600
NA
yes
11.04
110.5
107.03,87.14
0.2 ng/g and>
NR
9-9-99 C-2
NA in Soils
-0.1, -0.2
<20 RPD
89 - 93%R
89 - 97%R
60 ppm and >
0.9969

06/25/99
NA
NA
<20RPD
NA
NA
NA
NA

Not Provided
NA
NA
None Reported
NA
NA
NA
NA


Battelle Lab
SOP
Yes

Yes Y
X ]


es Yes
< X
"DQO (NR)"

No descriptive narratives were provided by FIU.
Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
Total Phosphorus and MEHG were digested past the holding time. Holding time is a goal only.
Some analysis for AFDW were Re-Run based on negative numbers reported, but no QA/QC batches were re-run.
No duplicate/replicate measurements were taken with the Bulk Density analysis.
For MeHg samples, a matrix spike is performed with every sample and is used to correct the results for loss of analyte.
-------
                     Station ID     M4-576-SFF
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
The Narrative Section will be written after all of the analyses are completed









Narrative summaries will be written following the completion on the data analysis
































X
X
Not Noted
Date/No Time
FIU/SERC Laboratory i

Internal COC
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
Is the same as station ID
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC





Yes
Yes
Yes
Yes
Yes
X
X
X
X
X
X
X
NA
X
X
X
X
NA
X
X




Yes
Yes
ng/g
X
X
Ug/g
X
X
%
X
X
g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
               Applied Qualifiers |_
"DQO (NR)"
Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID    M4-586-SFF
Soil/Sediment
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
            Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
            Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Calibration % R (high and low range^
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
               QC Limits Met

                      Notes
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
5-6-99/No Time
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
5-6-99/No Time
08/20/99
08/20/99
X
SD = SF = S = Soil
5-6-99/No Time
09/03/99
09/09/99
The Batch Numbers are referenced by the Sample ID range. They are s





ppm
CVAF


4.302g,4.217g
200ul
aliquot
Blending Dilution
0
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
63
ug/g
EPA 365.1
Angel
0.06

X
SD = SF = S = Soil
5-6-99/No Time
06/25/99
06/25/99
lecific to this project.
0.025 g
0.025 g
0.025 g
NA
0.2126
%
ASTM D2974-87
SG/JL


X
SD = SF = S = Soil
5-6-99/No Time
NA
Not Provided

80
80
80
NA
0.457
g/mL
ASTM D453 1-86
SG/JL
0.001 g/cc


28 days
SOP
Yes
No (Goal Only)
Yes
X
No (Goal Only)
Yes
X
NA
Yes
X
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID








82099
NA
yes
0
28.16
81.4
0.2 ng/g and>
0.9713
9-9-99 C-2
NA in Soils
-0.1, -0.2
<20 RPD
89 - 93%R
89 - 97%R
60 ppm and >
0.9969

06/25/99
NA
NA
>20RPD
NA
NA
NA
NA

Not Provided
NA
NA
None Reported
NA
NA
NA
NA


Battelle Lab
SOP
Yes
"M"
Yes
X


Yes
X
"DQO"

Yes
X
"DQO (NR)"

No descriptive narratives were provided by FIU.
Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
Total Phosphorus and MEHG were digested past the holding time. Holding time is a goal only.
Some analysis for AFDW were Re-Run based on negative numbers reported, but no QA/QC batches were re-run.
No duplicate/replicate measurements were taken with the Bulk Density analysis.
For MeHg samples, a matrix spike is performed with every sample and is used to correct the results for loss of analyte.
-------
                     Station ID    M4-586-SFF
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
The Narrative Section will be written after all of the analyses are completed













































X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC





Yes
Yes
Yes
Yes
Yes
X
X
X
X
X
X
X
NA
X
X
X
X
NA
X
X




Yes
Yes
ng/g
X
X
Ug/g
X
X
%
X
X
g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
               Applied Qualifiers |_
"DQO"
"DQO (NR)"
Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
            Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
            Duplicates  (RPD)
Matrix Spike Recoveries (75-125)
    Calibration % R (high and low range^
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analys!
        All Calculation Checked
               QC Limits Met

                      Notes
M4-594-SFF Soil/Sediment
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
5-5-99/No Time
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
5-5-99/No Time
12/15/99
12/15/99
X
SD = SF = S = Soil
5-5-99/No Time
09/03/99
09/09/99
The Batch Numbers are referenced by the Sample ID range. They are s





ppm
CVAF


4.296g,4.078g
200ul
aliquot
See Worksheet
1.58
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
330.6
ug/g
EPA 365.1
Angel
0.06

X
SD = SF = S = Soil
5-5-99/No Time
06/25/99
06/25/99
lecific to this project.
0.025 g
0.025 g
0.025 g
NA
0.6824
%
ASTM D2974-87
SG/JL


X
SD = SF = S = Soil
5-5-99/No Time
NA
Not Provided

80
80
80
NA
0.1944
g/mL
ASTM D453 1-86
SG/JL
0.001 g/cc


28 days
SOP
Yes
No (Goal Only)
Yes
X
No (Goal Only)
Yes
X
NA
Yes
X
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID








121599
NA
yes
-38.82
80.89
75.79
0.2 ng/g and >
0.9881
9-9-99 C-la
NA in Soils
-0.3, -0.4
<20RPD
95 - 96%R
62 - 100%R
60 ppm and >
0.9952

06/25/99
NA
NA
<20 RPD
NA
NA
NA
NA

Not Provided
NA
NA
None Reported
NA
NA
NA
NA


Battelle Lab
SOP
Yes
"DQO"
Yes Y
X ]
"DQO"

es Yes
< X
"DQO (NR)"

No descriptive narratives were provided by FIU.
Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
Total Phosphorus and MEHG were digested past the holding time. Holding time is a goal only.
Some analysis for AFDW were Re-Run based on negative numbers reported, but no QA/QC batches were re-run.
No duplicate/replicate measurements were taken with the Bulk Density analysis.
For MeHg samples, a matrix spike is performed with every sample and is used to correct the results for loss of analyte.
-------
                     Station ID     M4-594-SFF
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID  Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance (Pass/Fail)

Validation Criteria
               Applied Qualifiers I
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
The Narrative Section will be written after all of the analyses are completed













































X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC





Yes
Yes
Yes
Yes
Yes
X
X
X
X
X
X
X
NA
X
X
X
X
NA
X
X




Yes
Yes
ng/g
X
X
Ug/g
X
X
%
X
X
g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
"DQO"
"DQO"
"DQO (NR)"
Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 "  Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X " = Attached or Verified
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID    M4-599-SFF
Soil/Sediment
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
            Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
            Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Calibration % R (high and low range^
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
               QC Limits Met

                      Notes
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
5-6-99/No Time
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
5-6-99/No Time
03/25/00
03/25/00
X
SD = SF = S = Soil
5-6-99/No Time
10/13/99
10/29/99
The Batch Numbers are referenced by the Sample ID range. They are s





ppm
CVAF


4.44, 5.363
200ul
aliquot
See Worksheet
0.61
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
176.6
ug/g
EPA 365.1
Angel
0.06

X
SD = SF = S = Soil
5-6-99/No Time
06/25/99
06/25/99
lecific to this project.
0.025 g
0.025 g
0.025 g
NA
0.9124
%
ASTM D2974-87
SG/JL


X
SD = SF = S = Soil
5-6-99/No Time
NA
Not Provided

80
80
80
NA
0.1849
g/mL
ASTM D453 1-86
SG/JL
0.001 g/cc


28 days
SOP
Yes
No (Goal Only)
Yes
X
No (Goal Only)
Yes
X
NA
Yes
X
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID








32500
NA
yes
-30.44
129.76
85.34, 124.05
0.2 ng/g and>
0.9985
10-29-99 C-l
NA in Soils
0.0, -0.1
<20 RPD
86-91%R
93- 101%R
60 ppm and >
0.9962

06/25/99
NA
NA
<20RPD
NA
NA
NA
NA

Not Provided
NA
NA
None Reported
NA
NA
NA
NA


Battelle Lab
SOP
Yes
"DQO"
Yes Y
X ]


es Yes
< X
"DQO (NR)"

No descriptive narratives were provided by FIU.
Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
Total Phosphorus and MEHG were digested past the holding time. Holding time is a goal only.
Some analysis for AFDW were Re-Run based on negative numbers reported, but no QA/QC batches were re-run.
No duplicate/replicate measurements were taken with the Bulk Density analysis.
For MeHg samples, a matrix spike is performed with every sample and is used to correct the results for loss of analyte.
-------
                     Station ID     M4-599-SFF
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
The Narrative Section will be written after all of the analyses are completed













































X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC





Yes
Yes
Yes
Yes
Yes
X
X
X
X
X
X
X
NA
X
X
X
X
NA
X
X




Yes
Yes
ng/g
X
X
Ug/g
X
X
%
X
X
g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
               Applied Qualifiers |_
"DQO"
"DQO (NR)"
Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID    M4-809-SFF
Soil/Sediment
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
            Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
            Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Calibration % R (high and low range^
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
               QC Limits Met

                      Notes
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
5-1 1-99/No Time
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
5-11-99/NoTime
09/10/99
09/10/99
X
SD = SF = S = Soil
5-1 1-99/No Time
10/13/99
10/29/99
The Batch Numbers are referenced by the Sample ID range. They are s





ppm
CVAF


5.473g,5.544g
200ul
aliquot
Blending Dilution
ND
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
179.5
ug/g
EPA 365.1
Angel
0.06

X
SD = SF = S = Soil
5-1 1-99/No Time
06/25/99
06/25/99
lecific to this project.
0.025 g
0.025 g
0.025 g
NA
0.9644
%
ASTM D2974-87
SG/JL


X
SD = SF = S = Soil
5-1 1-99/No Time
NA
Not Provided

80
80
80
NA
0.071
g/mL
ASTM D453 1-86
SG/JL
0.001 g/cc


28 days
SOP
Yes
No (Goal Only
Yes
X
No (Goal Only)
Yes
X
NA
Yes
X
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID








91099
NA
yes
0
36.57
good
0.2 ng/g and>
0.9957
10-29-99 C-l
NA in Soils
0.0, -0.1
<20 RPD
86-91%R
93- 101%R
60 ppm and >
0.9962

06/25/99
NA
NA
<20RPD
NA
NA
NA
NA

Not Provided
NA
NA
None Reported
NA
NA
NA
NA


Battelle Lab
SOP
Yes
"M"
Yes Y
X ]


es Yes
< X
"DQO (NR)"

No descriptive narratives were provided by FIU.
Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
Total Phosphorus and MEHG were digested past the holding time. Holding time is a goal only.
Some analysis for AFDW were Re-Run based on negative numbers reported, but no QA/QC batches were re-run.
No duplicate/replicate measurements were taken with the Bulk Density analysis.
For MeHg samples, a matrix spike is performed with every sample and is used to correct the results for loss of analyte.
-------
                     Station ID     M4-809-SFF
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
The Narrative Section will be written after all of the analyses are completed













































X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC





Yes
Yes
Yes
Yes
Yes
X
X
X
X
X
X
X
NA
X
X
X
X
NA
X
X




Yes
Yes
ng/g
X
X
Ug/g
X
X
%
X
X
g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
               Applied Qualifiers |_
"DQO (NR)"
Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID    M4-872-SFF
Soil/Sediment
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
            Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
            Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Calibration % R (high and low range^
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analys!
       All Calculation Checked
               QC Limits Met

                      Notes
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
5-8-99/No Time
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
5-8-99/No Time
03/28/00
03/28/00
X
SD = SF = S = Soil
5-8-99/No Time
10/13/99
10/29/99
The Batch Numbers are referenced by the Sample ID range. They are s





ppm
CVAF


4.517,4.562
200ul
aliquot
See Worksheet
0.23
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
154.9
ug/g
EPA 365.1
Angel
0.06

X
SD = SF = S = Soil
5-8-99/No Time
06/25/99
06/25/99
lecific to this project.
0.025 g
0.025 g
0.025 g
NA
0.628
%
ASTM D2974-87
SG/JL


X
SD = SF = S = Soil
5-8-99/No Time
NA
Not Provided

80
80
80
NA
0.1594
g/mL
ASTM D453 1-86
SG/JL
O.OOlg/cc


28 days
SOP
Yes
No (Goal Only)
Yes
X
No (Goal Only)
Yes
X
NA
Yes
X
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID








32800b
NA
yes
-49.52
95.92
NR
0.2 ng/g and>
NR
10-29-99 C-l
NA in Soils
0.0, -0.1
<20 RPD
86-91%R
93-101%R
60 ppm and >
0.9962

06/25/99
NA
NA
<20RPD
NA
NA
NA
NA

Not Provided
NA
NA
None Reported
NA
NA
NA
NA


Battelle Lab
SOP
Yes
"DQO (NR)11
Yes Y
X ]


es Yes
< X
"NR"

No descriptive narratives were provided by FIU.
Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
Total Phosphorus and MEHG were digested past the holding time. Holding time is a goal only.
Some analysis for AFDW were Re-Run based on negative numbers reported, but no QA/QC batches were re-run.
No duplicate/replicate measurements were taken with the Bulk Density analysis.
For MeHg samples, a matrix spike is performed with every sample and is used to correct the results for loss of analyte.
-------
                     Station ID     M4-872-SFF
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
The Narrative Section will be written after all of the analyses are completed













































X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC
X
X
Not Noted
Date/No Time

Not Noted
Internal COC





Yes
Yes
Yes
Yes
Yes
X
X
X
X
X
X
X
NA
X
X
X
X
NA
X
X




Yes
Yes
ng/g
X
X
Ug/g
X
X
%
X
X
g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
               Applied Qualifiers |_
"DQO"
                                                                     "NR"
Data Qualifiers/Footnotes:

" J "   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
" Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
" R2 " Correlation Coefficient is out of QAPP limits.
" M "   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
" B "   Analyte concentration in the associated blank was >3 times the MDL.
" H "   Analysis digestion performed after holding times have expired.
" NR " Data was unavailable for review.
" DQO " Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
" X "  =  Attached or Verified
-------
Fish - SERC
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 12/01/99       Checked by njs
Sample
M4-508-FIF-1

M4-508-FIF-2

M4-508-FIF-3

M4-508-FIF-4

M4-508-FIF-5

M4-508-FIF-6

M4-508-FIF-7

M4-533-FIF-1

M4-533-FIF-2

M4-533-FIF-3

M4-533-FIF-4

M4-533-FIF-5

M4-533-FIF-6

M4-533-FIF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM2#12
DORM2#12
DORM2#14
DORM2#14
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV10-
CCV-11
CCV-1 2
QC
Batch
HO01OF1
















































Qualifier
Note

















































Instrument
Reading
Peak Height
107.9
109.4
36.5
36
39.3
39.1
83.3
83.6
47.3
46.9
45.4
45.7
32.6
32.3
93.8
93.8
85.7
84
97.6
97.1
186
185.5
116.7
116.7
127.1
127.4
173.1
174.5
2.457
1.503
1.98
1.264
0.3
36.1
36.3
33.4
33.6
81.4
82.2
80.1
80.4
80.6
80.4
78.9
80.1
81.5
81.4
79.9
79
Y Intercept
Slope
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
0.4200
Hg
Concentration
(PPt)
256.9
260.5
86.9
85.7
93.6
93.1
198.3
199.0
112.6
111.7
108.1
108.8
77.6
76.9
223.3
223.3
204.0
200.0
232.4
231.2
442.9
441.7
277.9
277.9
302.6
303.3
412.1
415.5
5.9
3.6
4.7
3.0
0.7
86.0
86.4
79.5
80.0
193.8
195.7
190.7
191.4
191.9
191.4
187.9
190.7
194.0
193.8
190.2
188.1
Vol.
added
(mL)
0.5
0.5
0.5
0.5
1
1
1
1
1
1
1
1
1
1
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
1
1
1
1
1
1
0.5
0.5

0.1
0.1
0.1
0.1












Average
Reagent
Blank (ng)
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386
0.386





0.386
0.386
0.386
0.386












Corrected Hg
Concentration
(ng)
31.21
31.65
10.30
10.16
5.51
5.48
12.11
12.15
6.71
6.65
6.42
6.47
4.50
4.46
67.28
67.28
61.44
60.21
70.03
69.66
54.09
53.94
83.80
83.80
18.68
18.72
25.58
25.79
0.37
0.23
0.58
0.37

51.44
51.73
47.57
47.85












Weight
offish
(g)
0.2244
0.2244
0.1461
0.1461
0.0989
0.0989
0.0918
0.0918
0.1362
0.1362
0.0972
0.0972
0.1196
0.1196
0.3507
0.3507
0.428
0.428
0.3388
0.3388
0.2082
0.2082
0.3355
0.3355
0.1482
0.1482
0.0942
0.0942





0.0098
0.0098
0.01
0.01












Hg
Concentration
ppb
139.10
141.05
70.52
69.52
55.70
55.40
131.91
132.40
49.26
48.82
66.09
66.55
37.66
37.28
191.86
191.86
143.55
140.69
206.69
205.62
259.78
259.07
249.79
249.79
126.04
126.34
271.54
273.77




0.0007
5249.31
5278.62
4756.69
4785.40
0.1938
0.1957
0.1907
0.1914
0.1919
0.1914
0.1879
0.1907
0.1940
0.1938
0.1902
0.1881
Averaged
Result
ppb

140.08

70.02

55.55

132.15

49.04

66.32

37.47

191.86

142.12

206.15

259.42

249.79

126.19

272.65

0.30

0.48
0.0007

5263.97

4771.04












Averaged
Reported
Result (ppb)













78.66













206.88



0.386
0.0007



5017.50











0.192
Detection
Limit/*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)

































4600
4600
4600
4600
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
R%

































#####
#####
#####
#####
96.90
97.86
95.36
95.71
95.95
95.71
93.93
95.36
97.02
96.90
95.12
94.05
Standard
Deviation




































285.08











0.0024
Relative
Standard
Deviation




































5.7











1.24
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 12/01/99       Checked by njs
Sample
M4-538-FIF-1

M4-538-FIF-2

M4-538-FIF-3

M4-538-FIF-4

M4-538-FIF-5

M4-538-FIF-6

M4-538-FIF-7

M4-548-FIF-1

M4-548-FIF-2

M4-548-FIF-3

M4-548-FIF-4

M4-548-FIF-5

M4-548-FIF-6

M4-548-FIF-7

Method Blank- 1

Method Blank-0.5

Instrument Blank
DORM2#3
DORM2#3
DORM2#4
DORM2#4
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-11
CCV-1 2
CCV-1 3
CCV-1 4
QC
Batch
HO02OF1


















































Qualifier
Note



















































Instrument
Reading
Peak Height
22.4
22.2
13.5
13.7
29.7
29.5
16.5
16.8
24.4
24.3
15
14.6
15
14.7
50.5
50.9
79.6
80
30.9
30.2
19.2
19.1
41.1
40.1


25.8
24.4
1
0.4
0.2
0.1
1
31.7
31.3
36.6
36.9
88
87.4
84.2
85.5
86.6
86.8
86.2
87
87.8
88.1
84.6
86.1
88.4
88.9
Y Intercept
Slope
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213


0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
0.4213
Hg
Concentration
(PPt)
53.2
52.7
32.0
32.5
70.5
70.0
39.2
39.9
57.9
57.7
35.6
34.7
35.6
34.9
119.9
120.8
188.9
189.9
73.3
71.7
45.6
45.3
97.6
95.2


61.2
57.9
2.4
0.9
0.5
0.2
2.4
75.2
74.3
86.9
87.6
208.9
207.5
199.9
202.9
205.6
206.0
204.6
206.5
208.4
209.1
200.8
204.4
209.8
211.0
Vol.
added
(mL)
1
1
0.5
0.5
0.5
0.5
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1


1
1
1
1
0.5
0.5

0.1
0.1
0.1
0.1














Average
Reagent
Blank (ng)
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074
0.074


0.074
0.074





0.074
0.074
0.074
0.074














Corrected Hg
Concentration
(ng)
3.28
3.25
3.87
3.93
8.60
8.54
.39
.44
.57
.56
.17
.11
.17
.12
7.48
7.54
11.83
11.89
4.55
4.44
2.80
2.78
6.07
5.92


3.78
3.57
0.15
0.06
0.06
0.03

45.30
44.73
52.31
52.74














Weight
offish
(g)
0.1210
0.1210
0.1413
0.1413
0.2727
0.2727
0.098
0.098
0.1133
0.1133
0.0966
0.0966
0.1019
0.1019
0.0557
0.0557
0.0688
0.0688
0.0389
0.0389
0.0696
0.0696
0.0609
0.0609


0.0306
0.0306





0.0101
0.0101
0.0145
0.0145














Hg
Concentration
ppb
27.1
26.8
27.4
27.8
31.5
31.3
24.4
24.9
31.6
31.4
22.5
21.8
21.3
20.8
134.2
135.3
171.9
172.8
116.9
114.2
40.2
40.0
99.7
97.2


123.7
116.8




0.0024
4484.9
4428.2
3607.7
3637.3
0.2089
0.2075
0.1999
0.2029
0.2056
0.2060
0.2046
0.2065
0.2084
0.2091
0.2008
0.2044
0.2098
0.2110
Averaged
Result
ppb

26.95

27.58

31.42

24.65

31.48

22.14

21.07

134.79

172.37

115.54

40.08

98.48



120.24

0.10

0.04
0.0024

4456.58

3622.46














Averaged
Reported
Result (ppb)













26.47













113.58



0.074
0.0024



4039.520













0.206
Detection
Limit/*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6


3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)

































4600
4600
4600
4600
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
R%

































97.50
96.27
78.43
79.07
#####
#####
99.93
#####
#####
#####
#####
#####
#####
#####
#####
#####
#####
#####
Standard
Deviation




































589.81













0.0033
Relative
Standard
Deviation




































14.6













1.62
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 12/01/99       Checked by njs
Sample
M4-556-FIF-1

M4-556-FIF-2

M4-556-FIF-3

M4-566-FIF-1

M4-566-FIF-2

M4-566-FIF-3

M4-566-FIF-4

M4-566-FIF-5

M4-566-FIF-6

M4-566-FIF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
SRM
DORM2#5
SRM
DORM2#6+A308
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV10-
CCV-11
CCV-1 2
CCV-1 3
CCV-1 4
CCV-1 5
CCV-1 6
CCV-1 7
CCV-1 8
QC
Batch
HO07OF1














































Qualifier
Note















































Instrument
Reading
Peak Height
39.2
38.4
31.9
31.5
7.1
6.6
86.3
87.3
60.8
61.2
35
34.7
64.3
64.6
91.6
90.9
47.9
47.7
58.6
59
1.9
1.3
0.8
0.7
1.2
29.2
28.8
28
27.9
77.1
77.1
74.2
74.7
78
70.2
69.7
70.4
78.2
78.5
78.4
78.1
75
74.3
79.4
78.7
77.6
78.2
Y Intercept
Slope
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
0.3958
Hg
Concentration
(PPt)
99.0
97.0
80.6
79.6
17.9
16.7
218.0
220.6
153.6
154.6
88.4
87.7
162.5
163.2
231.4
229.7
121.0
120.5
148.1
149.1
4.8
3.3
2.0
1.8
3.0
73.8
72.8
70.7
70.5
194.8
194.8
187.5
188.7
197.1
177.4
176.1
177.9
197.6
198.3
198.1
197.3
189.5
187.7
200.6
198.8
196.1
197.6
Vol.
added
(mL)
1
1
1
1
1
1
1
1
0.5
0.5
0.5
0.5
0.2
0.2
1
1
1
1
1
1
1
1
0.5
0.5

0.1
0.1
0.1
0.1


















Average
Reagent
Blank (ng)
0.244
0.244
0.244
0.244
0.244
0.244
0.244
0.244
0.244
0.244
0.244
0.244
0.244
0.244
0.244
0.244
0.244
0.244
0.244
0.244





0.244
0.244
0.244
0.244


















Corrected Hg
Concentration
(ng)
6.00
5.87
4.83
4.77
0.89
0.81
13.49
13.65
18.65
18.77
10.63
10.54
48.98
49.21
14.34
14.22
7.38
7.35
9.08
9.15
0.30
0.21
0.25
0.22

44.24
43.63
42.41
42.26


















Weight
offish
(g)
0.102
0.102
0.1084
0.1084
0.0293
0.0293
0.0952
0.0952
0.2015
0.2015
0.1619
0.1619
0.3513
0.3513
0.1386
0.1386
0.0744
0.0744
0.1407
0.1407





0.0098
0.0098
0.01
0.01


















Hg
Concentration
ppb
58.78
57.53
44.59
44.00
30.24
27.53
141.73
143.40
92.56
93.17
65.67
65.10
139.43
140.08
103.43
102.63
99.20
98.77
64.56
65.01




0.00303
4514.50
4452.32
4241.39
4226.16
0.1948
0.1948
0.1875
0.1887
0.1971
0.1774
0.1761
0.1779
0.1976
0.1983
0.1981
0.1973
0.1895
0.1877
0.2006
0.1988
0.1961
0.1976
Averaged
Result
ppb

58.16

44.30

28.88

142.56

92.87

65.39

139.75

103.03

98.98

64.79

0.25

0.23
0.0030

4483.41

4233.77


















Averaged
Reported
Result (ppb)





43.78













101.05



0.244
0.0030



4358.59

















0.192
Detection
Limit/*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)

























4600
4600
4600
4600
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
R%

























98.14
96.79
92.20
91.87
97.40
97.40
93.73
94.37
98.53
88.68
88.05
88.93
98.79
99.17
99.04
98.66
94.74
93.86
#####
99.42
98.03
98.79
Standard
Deviation




























146.48

















0.0079
Relative
Standard
Deviation




























3.4

















4.13
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 12/01/99       Checked by njs
Sample
M4-568-FIF-1

M4-568-FIF-2

M4-568-FIF-3

M4-568-FIF-4

M4-568-FIF-5

M4-568-FIF-6

M4-568-FIF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM2#12
DORM2#12
DORM2#14
DORM2#14
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CC VI CI-
GGY- 11
CCV-1 2
CCV-1 3
CCV-1 4
QC
Batch
HO08OF1




































Qualifier
Note





































Instrument
Reading
Peak Height
104.83
100.55
76.78
76.78
90.09
89.86
70.13
70.6
65.85
65.37
50.87
50.87
66.56
66.32
8.2
7.9
2.5
2.9
1.2
42.3
42.9
38.3
39
87.6
88.2
84.1
83.8
84.5
85.7
85.8
85.2
77
77.2
90
90.7
83.4
82.5
Y Intercept
Slope
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
0.4207
Hg
Concentration
(PPt)
249.2
239.0
182.5
182.5
214.1
213.6
166.7
167.8
156.5
155.4
120.9
120.9
158.2
157.6
19.5
18.8
5.9
6.9
2.9
100.5
102.0
91.0
92.7
208.2
209.7
199.9
199.2
200.9
203.7
203.9
202.5
183.0
183.5
213.9
215.6
198.2
196.1
Vol.
added
(mL)
















0.5
0.5

0.1
0.1
0.1
0.1














Average
Reagent
Blank (ng)
0.997
0.997
0.997
0.997
0.997
0.997
0.997
0.997
0.997
0.997
0.997
0.997
0.997
0.997





0.997
0.997
0.997
0.997














Corrected Hg
Concentration
(ng)
14.70
14.06
10.50
10.50
12.49
12.46
9.50
9.58
8.86
8.79
6.62
6.62
8.97
8.93
1.23
1.18
0.73
0.85

59.63
60.49
53.90
54.90














Weight
offish
(g)
0.141
0.141
0.0919
0.0919
0.069
0.069
0.0942
0.0942
0.0917
0.0917
0.0701
0.0701
0.0538
0.0538





0.0118
0.0118
0.0116
0.0116














Hg
Concentration
ppb
104.26
99.72
114.26
114.26
181.07
180.57
100.90
101.65
96.66
95.88
94.45
94.45
166.74
166.07




0.0029
5053.62
5126.50
4646.50
4732.99
0.2082
0.2097
0.1999
0.1992
0.2009
0.2037
0.2039
0.2025
0.1830
0.1835
0.2139
0.2156
0.1982
0.1961
Averaged
Result
ppb

101.99

114.26

180.82

101.28

96.27

94.45

166.40

1.21

0.79
0.0029

5090.06

4689.74














Averaged
Reported
Result (ppb)













122.21



0.997
0.0029



4889.90













0.201
Detection
Limit/*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)



















4600
4600
4600
4600
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
R%



















#####
#####
#####
#####
#####
#####
99.95
99.60
#####
#####
#####
#####
91.51
91.75
#####
#####
99.12
98.05
Standard
Deviation






















235.69













0.0096
Relative
Standard
Deviation






















4.8













4.75
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by Rtc 12/01/99
                     Checked by njs
Sample
M4-576-FIF-1

M4-576-FIF-2

M4-576-FIF-3

M4-576-FIF-4

M4-576-FIF-5

M4-576-FIF-6

M4-576-FIF-7

M4-594-FIF-2

M4-594-FIF-3

M4-594-FIF-4

M4-594-FIF-5

M4-594-FIF-6

M4-594-FIF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM2#12
DORM2#12
DORM2#14
DORM2#14
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV10-
CCV-11
CCV-1 2
CCV-1 3
CCV-1 4
CCV-1 5
CCV-1 6
CCV-1 7
CCV-1 8
CCV-1 9
CCV-20
QC
Batch
HO12OF1
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
»
"
Qualifier
Note























































Instrument
Reading
Peak Height
63.9
65.5
147.2
147.8
94.8
89.6
145.7
148.6
71.7
70.1
133.7
136.4
115.5
111.1
151.1
150.7
114.7
108.5
127.2
128.3
89.2
87.7
81.3
81.6
144.2
144.5
0.8
0.2
0.2
0.3
1.5
38.7
38.8
40
39.6
77.6
77.6
77.2
78.8
78.3
79.7
77.2
76.4
74.7
74.2
85.9
85.6
82.5
81.6
82
81.2
83.7
83.5
79.5
79.5
Y Intercept
Slope
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
0.4396
Hg
Concentration
(PPt)
145.4
149.0
334.8
336.2
215.7
203.8
331.4
338.0
163.1
159.5
304.1
310.3
262.7
252.7
343.7
342.8
260.9
246.8
289.4
291.9
202.9
199.5
184.9
185.6
328.0
328.7
1.8
0.5
0.5
0.7
3.4
88.0
88.3
91.0
90.1
176.5
176.5
175.6
179.3
178.1
181.3
175.6
173.8
169.9
168.8
195.4
194.7
187.7
185.6
186.5
184.7
190.4
189.9
180.8
180.8
Vol.
added
(mL)
0.2
0.2
0.2
0.2
0.5
0.5
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.5
0.5
0.5
0.5










0.5
0.5

0.1
0.1
0.1
0.1




















Average
Reagent
Blank (ng)
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07





0.071
0.071
0.071
0.071




















Corrected Hg
Concentration
(ng)
43.97
45.08
101.39
101.80
26.45
25.00
100.35
102.35
49.35
48.25
92.08
93.94
79.54
76.51
42.21
42.09
32.02
30.29
18.16
18.32
12.71
12.50
11.58
11.62
20.59
20.64
0.11
0.03
0.06
0.08

53.01
53.15
54.80
54.25




















Weight
offish
(g)
0.3209
0.3209
0.3221
0.3221
0.1871
0.1871
0.3248
0.3248
0.2094
0.2094
0.2676
0.2676
0.3355
0.3355
0.218
0.218
0.1744
0.1744
0.0729
0.0729
0.0945
0.0945
0.0787
0.0787
0.1148
0.1148





0.0116
0.0116
0.0119
0.0119




















Hg
Concentration
ppb
137.03
140.47
314.77
316.06
141.39
133.61
308.97
315.13
235.67
230.40
344.11
351.06
237.08
228.04
193.61
193.10
183.61
173.67
249.09
251.25
134.52
132.25
147.14
147.69
179.40
179.77




0.0034
4570.2
4582.0
4604.8
4558.7
0.1765
0.1765
0.1756
0.1793
0.1781
0.1813
0.1756
0.1738
0.1699
0.1688
0.1954
0.1947
0.1877
0.1856
0.1865
0.1847
0.1904
0.1899
0.1808
0.1808
Averaged
Result
ppb

138.75

315.42

137.50

312.05

233.04

347.59

232.56

193.35

178.64

250.17

133.39

147.42

179.58

0.07

0.07
0.0034

4576.07

4581.74




















Averaged
Reported
Result (ppb)













245.27











180.42



0.071
0.0034



4578.91



















0.182
Detection
Limit/*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)































4600
4600
4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%































99.35
99.61
#####
99.10
88.26
88.26
87.81
89.63
89.06
90.65
87.81
86.90
84.96
84.39
97.70
97.36
93.84
92.81
93.27
92.36
95.20
94.97
90.42
90.42
Standard
Deviation


































4.01



















0.0076
Relative
Standard
Deviation


































0.1



















4.19
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 12/01/99       Checked by njs
Sample
M4-599-FIF-1

M4-599-FIF-2

M4-599-FIF-3

M4-599-FIF-4

M4-599-FIF-5

M4-599-FIF-6

M4-599-FIF-7

M4-809-FIF-1

M4-809-FIF-2

M4-809-FIF-3

M4-809-FIF-4

M4-809-FIF-5

M4-809-FIF-6

M4-809-FIF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM2#16
DORM2#16
DORM2#17
DORM2#17
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-11
CCV-1 2
CCV-1 3
CCV-1 4
QC
Batch
HO13OF1


















































Qualifier
Note



















































Instrument
Reading
Peak Height
97.7
97.6
143.3
142.6
143.4
150.9
122.2
124.3
140.6
141.7
104.2
104.9
123.7
123.5
47.6
46.7
38.9
39.8
79.4
80.3
46.5
45.8
44.4
44.9
43.2
43.9
116.6
116.6
13.2
12.7
6.4
6.6
0.9
37
37
40
40.3
88.1
88.6
87.7
87.2
82.2
81.7
85.9
85.5
79.3
79.9
81
81.8
81.5
81.1
Y Intercept
Slope
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
0.4347
Hg
Concentration
(PPt)
224.8
224.5
329.7
328.0
329.9
347.1
281.1
285.9
323.4
326.0
239.7
241.3
284.6
284.1
109.5
107.4
89.5
91.6
182.7
184.7
107.0
105.4
102.1
103.3
99.4
101.0
268.2
268.2
30.4
29.2
14.7
15.2
2.1
85.1
85.1
92.0
92.7
202.7
203.8
201.7
200.6
189.1
187.9
197.6
196.7
182.4
183.8
186.3
188.2
187.5
186.6
Vol.
added
(mL)
0.2
0.2
1
1
0.5
0.5
0.2
0.2
0.2
0.2
0.2
0.2
0.5
0.5
0.2
0.2
0.2
0.2
0.5
0.5
0.5
0.5
0.2
0.2
0.2
0.2
0.5
0.5
1
1
0.5
0.5

0.1
0.1
0.1
0.1














Average
Reagent
Blank (ng)
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858
1.858





1.858
1.858
1.858
1.858














Corrected Hg
Concentration
(ng)
66.24
66.17
18.91
18.81
38.72
40.84
83.32
84.78
96.14
96.91
70.77
71.26
33.14
33.09
31.32
30.69
25.26
25.88
20.61
20.86
11.30
11.10
29.09
29.44
28.25
28.74
31.13
31.13
1.91
1.84
1.81
1.87

49.47
49.47
53.63
54.04














Weight
offish
(g)
0.2005
0.2005
0.1279
0.1279
0.116
0.116
0.2133
0.2133
0.3574
0.3574
0.2894
0.2894
0.119
0.119
0.2891
0.2891
0.2561
0.2561
0.1951
0.1951
0.1553
0.1553
0.2348
0.2348
0.321
0.321
0.1989
0.1989





0.0119
0.0119
0.0121
0.0121














Hg
Concentration
ppb
330.38
330.04
147.85
147.06
333.77
352.07
390.62
397.48
269.01
271.16
244.55
246.24
278.52
278.04
108.34
106.17
98.62
101.07
105.63
106.94
72.76
71.48
123.89
125.38
88.02
89.54
156.53
156.53




0.0021
4156.9
4156.9
4432.1
4466.5
0.2027
0.2038
0.2017
0.2006
0.1891
0.1879
0.1976
0.1967
0.1824
0.1838
0.1863
0.1882
0.1875
0.1866
Averaged
Result
ppb

330.21

147.45

342.92

394.05

270.08

245.39

278.28

107.25

99.84

106.28

72.12

124.64

88.78

156.53

1.88

1.84
0.0021

4156.90

4449.31














Averaged
Reported
Result (ppb)













286.91













107.92



1.858
0.0021



4303.101













0.192
Detection
Limit/*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)

































4600
4600
4600
4600
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
R%

































90.37
90.37
96.35
97.10
#####
#####
#####
#####
94.55
93.97
98.80
98.34
91.21
91.90
93.17
94.09
93.74
93.28
Standard
Deviation




































206.77













0.0076
Relative
Standard
Deviation




































4.8













3.95
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the May 1999 Dry Season (M4)
Entered by gtc 12/01/99       Checked by njs
Sample
M4-872-FIF-1

M4-872-FIF-2

M4-872-FIF-3

M4-872-FIF-4

M4-872-FIF-5

M4-872-FIF-6

M4-872-FIF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM2#18
DORM2#18
DORM2#19
DORM2#19
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-11
CCV-1 2
CCV-1 3
CCV-1 4
QC
Batch
HO22OF1




































Qualifier
Note





































Instrument
Reading
Peak Height
98.8
99.6
141.2
139.8
87.9
87.9
120.2
120
46.9
46.5
73.3
72.6
98
98.8
5
4.8
2.3
2.5
1.3
32.9
32.6
39.8
39.8
91.2
91.8
90.6
90.6
89.1
89.5
89.2
90.9
88.9
89.7
89.1
89
88.7
89
Y Intercept
Slope
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
0.4589
Hg
Concentration
(PPt)
215.3
217.0
307.7
304.6
191.5
191.5
261.9
261.5
102.2
101.3
159.7
158.2
213.6
215.3
10.9
10.5
5.0
5.4
2.8
71.7
71.0
86.7
86.7
198.7
200.0
197.4
197.4
194.2
195.0
194.4
198.1
193.7
195.5
194.2
193.9
193.3
193.9
Vol.
added
(mL)
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5








0.5
0.5

0.1
0.1
0.1
0.1














Average
Reagent
Blank (ng)
0.658
0.658
0.658
0.658
0.658
0.658
0.658
0.658
0.658
0.658
0.658
0.658
0.658
0.658





0.658
0.658
0.658
0.658














Corrected Hg
Concentration
(ng)
25.82
26.04
37.19
36.81
22.90
22.90
31.56
31.51
5.78
5.73
9.40
9.31
12.80
12.91
0.69
0.66
0.62
0.67

42.57
42.18
51.64
51.64














Weight
offish
(g)
0.131
0.131
0.2128
0.2128
0.1423
0.1423
0.1774
0.1774
0.0742
0.0742
0.0517
0.0517
0.0704
0.0704





0.0101
0.0101
0.0145
0.0145














Hg
Concentration
ppb
197.13
198.76
174.76
172.99
160.94
160.94
177.90
177.60
77.91
77.17
181.91
180.06
181.76
183.32




0.0028
4215.1
4176.1
3561.4
3561.4
0.1987
0.2000
0.1974
0.1974
0.1942
0.1950
0.1944
0.1981
0.1937
0.1955
0.1942
0.1939
0.1933
0.1939
Averaged
Result
ppb

197.95

173.87

160.94

177.75

77.54

180.99

182.54

0.67

0.64
0.0028

4195.63

3561.36














Averaged
Reported
Result (ppb)













164.51



0.658
0.0028



3878.494













0.196
Detection
Limit/*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)



















4600
4600
4600
4600
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
R%



















91.63
90.79
77.42
77.42
99.37
#####
98.71
98.71
97.08
97.52
97.19
99.04
96.86
97.73
97.08
96.97
96.64
96.97
Standard
Deviation






















448.50













0.0022
Relative
Standard
Deviation






















11.6













1.12
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the  10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID C
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analysl
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analys
        All Calculation Checked
               QC Limits Met

                       Notes
M4-501-FIF
 Fish
  Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
No Samples were Collected
FS = FI = Fh = Fish
No Samples were Collected


No Samples were Collected
FS = FI = Fh = Fish
No Samples were Collected


No Samples were Collected
FS = FI = Fh = Fish
No Samples were Collected


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppb
CVAF
No Sample
3.2 ppb





mm
Measurement
No Sample
NA





g
Measurement
No Sample
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID








By: Date/Time







By: Date/Time







                            Samples were not collected and/or delivered to the SERC Laboratory.
-------
                     Station ID
M4-501-FIF
Fish
                                           Total Hg
                                 Length
                              Weight
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
            Total Samples/Matrix	
              Methods/Parameters	
       Range of Samples analyzed	
          Holding Time Summary	
              Analytical Problems	
        QA/QC Acceptance Limits	
          Integrity of Data Quality	
            Deviations From SOP
                     Observations
Sample Management Records    No Chain of Custody	Sample log summary only
            Sampling Location ID
                          Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
             Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                    Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
           Sample ID Transferred
          All Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)


Not Noted
Date/No Time


Not Noted
Date/No Time


Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC






Notes are the raw data and the instrument data.









ppb


mm


o
&
NA
NA
NA
NA
NA
NA
Validation Criteria
               Applied Qualifiers |  No Samples were Collected  |   No Samples were Collected  |    No Samples were Collected
X =  Attached or Verified
Data Qualifiers

"J"  Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B" Analyte concentration in the associated blank was >3 times the MDL.
"H" Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
               Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                       Notes
M4-508-FIF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
5-1 1-99/No Time
06/03/99
07/01/99
X
FS = FI = Fh = Fish
5-11-99/NoTime
06/03/99
06/03/99
X
FS = FI = Fh = Fish
5-1 1-99/No Time
06/03/99
06/03/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
89.7 (Average of 7)
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
22-30
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
0.0989 - 0.2244
g
Measurement
MB
NA
No
X
Yes (28 day Holding Time)
No
X
No (Goal Only)
No
X
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG01GF1
0.386
0.0007
<20RPD
DORM103-115%R
93 - 98%R
3. 2 ppb and >
0.9999
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
No
X

No
X


No
X


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only, not a hard deadline.
Measurements offish length and weight were measured after holding time goals.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M4-508-FIF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA
Validation Criteria
                Applied Qualifiers [_
X=  Attached or Verified
Data Qualifiers

"J"  Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B" Analyte concentration in the associated blank was >3 times the MDL.
"H" Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
               Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                       Notes
M4-533-FIF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
5-11-99/NoTime
06/03/99
07/01/99
X
FS = FI = Fh = Fish
5-1 1-99/No Time
06/03/99
06/03/99
X
FS = FI = Fh = Fish
5-11-99/NoTime
06/03/99
06/03/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
200-1000
206. 9 (Average of 7)
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
21-32
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
0.0942 - 0.428
g
Measurement
MB
NA
No
X
Yes (28 day Holding Time)
No
X
No (Goal Only)
No
X
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG01GF1
0.386
0.0007
<20RPD
DORM103-115%R
93 - 98%R
3. 2 ppb and >
0.9999
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
No
X

No
X


No
X


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only, not a hard deadline.
Measurements offish length and weight were measured after holding time goals.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M4-533-FIF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA
Validation Criteria
                Applied Qualifiers [_
X=  Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID
M4-538-FIF
Fish
Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
               Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                       Notes
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
5-10-99/No Time
06/03/99
07/02/99
X
FS = FI = Fh = Fish
5-10-99/No Time
06/03/99
06/03/99
X
FS = FI = Fh = Fish
5-10-99/No Time
06/03/99
06/03/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
26. 47 (Average of 7)
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
20-25
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
0.0966 - 0.2727
g
Measurement
MB
NA
No
X
Yes (28 day Holding Time)
No
X
No (Goal Only)
No
X
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG02GF1
0.074
0.0024
<20 RSD
78 - 98%R
100 - 106%R
3. 2 ppb and >
0.9991
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
No
X
No
X


No
X


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only, not a hard deadline.
Measurements offish length and weight were measured after holding time goals.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M4-538-FIF
Fish
                                            Total Hg
                                 Length
                             Weight
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance (Pass/Fail)
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA
Validation Criteria
                Applied Qualifiers \_
X =  Attached or Verified


Data Qualifiers

"J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"   Analyte concentration in the associated blank was >3 times the MDL.
"H"   Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID
M4-548-FIF
Fish
Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
               Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                       Notes
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
5-9-99/No Time
06/04/99
07/02/99
X
FS = FI = Fh = Fish
5-9-99/No Time
06/04/99
06/04/99
X
FS = FI = Fh = Fish
5-9-99/No Time
06/04/99
06/04/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
6 Fish
6 Fish
Aliquot
1000
113.6 (Average of 6)
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
15-23
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
0.0306 - 0.0696
g
Measurement
MB
NA
No
X
Yes (28 day Holding Time)
No
X
No (Goal Only)
No
X
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG02GF1
0.074
0.0024
<20 RSD
78 - 98%R
100 - 106%R
3. 2 ppb and >
0.9991
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
No
X
No
X


No
X


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only, not a hard deadline.
Measurements offish length and weight were measured after holding time goals.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M4-548-FIF
Fish
                                            Total Hg
                                 Length
                             Weight
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance (Pass/Fail)
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA
Validation Criteria
                Applied Qualifiers \_
X =  Attached or Verified


Data Qualifiers

"J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"   Analyte concentration in the associated blank was >3 times the MDL.
"H"   Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID
M4-556-FIF
Fish
Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
               Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                       Notes
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
5-8-99/No Time
06/04/99
07/07/99
X
FS = FI = Fh = Fish
5-8-99/No Time
06/04/99
06/04/99
X
FS = FI = Fh = Fish
5-8-99/No Time
06/04/99
06/04/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
3 Fish
3 Fish
Aliquot
1000
43. 78 (Average of 3)
ppb
CVAF
FDL/JL
3. 2 ppb
NA
3 Fish
3 Fish
NA
15-25
mm
Measurement
MB
NA
NA
3 Fish
3 Fish
NA
0.0293-0.1084
g
Measurement
MB
NA
No
X
Yes (28 day Holding Time)
No
X
No (Goal Only)
No
X
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG07GF1
0.244
0.003
<20 RSD
92 - 98%R
88 - 100%R
3. 2 ppb and >
0.9999
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
No
X
No
X


No
X


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only, not a hard deadline.
Measurements offish length and weight were measured after holding time goals.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M4-556-FIF
Fish
                                            Total Hg
                                 Length
                             Weight
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance (Pass/Fail)
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA
Validation Criteria
                Applied Qualifiers \_
X =  Attached or Verified


Data Qualifiers

"J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"   Analyte concentration in the associated blank was >3 times the MDL.
"H"   Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID
M4-566-FIF
Fish
Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
               Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                       Notes
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
5-7-99/No Time
06/09/99
07/07/99
X
FS = FI = Fh = Fish
5-7-99/No Time
06/09/99
06/09/99
X
FS = FI = Fh = Fish
5-7-99/No Time
06/09/99
06/09/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
200-1000
10 1.1 (Average of 7)
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
22-35
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
0.0744-0.3513
g
Measurement
MB
NA
No
X
No (Goal Only)
No
X
No (Goal Only)
No
X
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG07GF1
0.244
0.003
<20 RSD
92 - 98%R
88 - 100%R
3. 2 ppb and >
0.9999
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
No
X
"H"
No
X


No
X


No descriptive narratives were provided by FIU.
Sample for total mercury was digested past holding time.
Holding time goals set for the length and weight measurements are guidelines only, not a hard deadline.
Measurements offish length and weight were measured after holding time goals.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M4-566-FIF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA
Validation Criteria
                Applied Qualifiers \_
X =  Attached or Verified


Data Qualifiers

"J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"   Analyte concentration in the associated blank was >3 times the MDL.
"H"   Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
               Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                       Notes
M4-568-FIF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
5-7-99/No Time
06/16/99
07/08/99
X
FS = FI = Fh = Fish
5-7-99/No Time
06/16/99
06/16/99
X
FS = FI = Fh = Fish
5-7-99/No Time
06/16/99
06/16/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
1000
122. 2 (Average of 7)
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
20-25
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
0.0538-0.141
g
Measurement
MB
NA
No
X
No (Goal Only)
No
X
No (Goal Only)
No
X
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG08GF1
0.997
0.0027
<20 RSD
102- 111 %R
91 - 108 %R
3. 2 ppb and >
0.999
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
No
X
"H"
No
X


No
X


No descriptive narratives were provided by FIU.
Sample for total mercury was digested past holding time.
Holding time goals set for the length and weight measurements are guidelines only, not a hard deadline.
Measurements offish length and weight were measured after holding time goals.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M4-568-FIF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA
Validation Criteria
                Applied Qualifiers [_
X=  Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID
M4-576-FIF
Fish
Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
               Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                       Notes
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
5-4-99/No Time
06/18/99
07/12/99
X
FS = FI = Fh = Fish
5-4-99/No Time
06/18/99
06/18/99
X
FS = FI = Fh = Fish
5-4-99/No Time
06/18/99
06/18/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
200-500
245. 3 (Average of 7)
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
24-31
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
0.1871-0.3355
g
Measurement
MB
NA
Yes (MB)
X
No (Goal Only)
No
X
No (Goal Only)
No
X
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG12GF1
0.071
0.0034
<20 RSD
99 - 100 %R
84 - 97%R
3. 2 ppb and >
0.9998
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (MB)
X
"H"
No
X


No
X


No descriptive narratives were provided by FIU.
Sample for total mercury was digested past holding time.
Holding time goals set for the length and weight measurements are guidelines only, not a hard deadline.
Measurements offish length and weight were measured after holding time goals.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M4-576-FIF
Fish
                                            Total Hg
                                 Length
                             Weight
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance (Pass/Fail)
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA
Validation Criteria
                Applied Qualifiers \_
X =  Attached or Verified


Data Qualifiers

"J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"   Analyte concentration in the associated blank was >3 times the MDL.
"H"   Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                 Analysis Date
                 QC Batch ID
             Digestion Volume
                 Total Volume
       Sample Volume Analyzed
                     Dilution
                      Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                      Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
               Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                       Notes
M4-586-FIF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
No Samples were Collected
FS = FI = Fh = Fish
No Samples were Collected


No Samples were Collected
FS = FI = Fh = Fish
No Samples were Collected


No Samples were Collected
FS = FI = Fh = Fish
No Samples were Collected


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppb
CVAF
No Sample
3. 2 ppb





mm
Measurement
No Sample
NA





g
Measurement
No Sample
NA
FIU/SERC Laboratory uses the same ID as the Sampling Station ID







By: Date/Time






By: Date/Time






                            Samples were not collected and/or delivered to the SERC Laboratory.
-------
                     Station ID
M4-586-FIF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
          Performance  (Pass/Fail)
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed





























Not Noted
Date/No Time


Not Noted
Date/No Time


Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC






Notes are the raw data and the instrument data.










ppb


mm


g

NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
                Applied Qualifiers [_
X=  Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
               Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                       Notes
M4-594-FIF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
5-5-99/No Time
06/23/99
07/12/99
X
FS = FI = Fh = Fish
5-5-99/No Time
06/23/99
06/23/99
X
FS = FI = Fh = Fish
5-5-99/No Time
06/23/99
06/23/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
6 Fish
6 Fish
Aliquot
200 - 1000
180.4 (Average of 6)
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
22-30
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
0.0729-0.218
g
Measurement
MB
NA
Yes (MB)
X
No (Goal Only)
No
X
No (Goal Only)
No
X
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG12GF1
0.071
0.0034
<20 RSD
99-100 %R
84 - 97%R
3. 2 ppb and >
0.9998
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (MB)
X
"H"
No
X


No
X


No descriptive narratives were provided by FIU.
Sample for total mercury was digested past holding time.
Holding time goals set for the length and weight measurements are guidelines only, not a hard deadline.
Measurements offish length and weight were measured after holding time goals.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M4-594-FIF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA
Validation Criteria
                Applied Qualifiers [_
X=  Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID
M4-599-FIF
Fish
Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
               Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                       Notes
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
5-6-99/No Time
06/23/99
07/13/99
X
FS = FI = Fh = Fish
5-6-99/No Time
06/23/99
06/23/99
X
FS = FI = Fh = Fish
5-6-99/No Time
06/23/99
06/23/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
200 - 1000
286. 9 (Average of 7)
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
23-35
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
0.116-0.3574
g
Measurement
MB
NA
Yes (MB)
X
No (Goal Only)
No
X
No (Goal Only)
No
X
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG13GF1
1.858
0.0024
<20 RSD
90-97
93 - 102
3. 2 ppb and >
0.9988
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (MB)
X
"H"
No
X


No
X


No descriptive narratives were provided by FIU.
Sample for total mercury was digested past holding time.
Holding time goals set for the length and weight measurements are guidelines only, not a hard deadline.
Measurements offish length and weight were measured after holding time goals.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M4-599-FIF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA
Validation Criteria
                Applied Qualifiers \_
X =  Attached or Verified


Data Qualifiers

"J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"   Analyte concentration in the associated blank was >3 times the MDL.
"H"   Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
               Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                       Notes
M4-809-FIF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
5-11-99/NoTime
07/06/99
07/13/99
X
FS = FI = Fh = Fish
5-1 1-99/No Time
07/06/99
07/06/99
X
FS = FI = Fh = Fish
5-11-99/NoTime
07/06/99
07/06/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
200 - 500
107.9 (Average of 7)
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
Unable to read raw data
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
0.1553-0.321
g
Measurement
MB
NA
Yes (MB)
X
No (Goal Only)
No
X
No (Goal Only)
No
X
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG13GF1
1.858
0.0024
<20 RSD
90-97
93 - 102
3. 2 ppb and >
0.9988
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (MB)
X
"H"
No
X


No
X


No descriptive narratives were provided by FIU.
Sample for total mercury was digested past holding time.
Holding time goals set for the length and weight measurements are guidelines only, not a hard deadline.
Measurements offish length and weight were measured after holding time goals.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M4-809-FIF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA
Validation Criteria
                Applied Qualifiers [_
X=  Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID
M4-872-FIF
Fish
Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
               Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                       Notes
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
5-8-99/No Time
07/06/99
07/22/99
X
FS = FI = Fh = Fish
5-8-99/No Time
07/06/99
07/06/99
X
FS = FI = Fh = Fish
5-8-99/No Time
07/06/99
07/06/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
164.5 (Average of 7)
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
Unable to read raw data
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
0.0517-0.2128
g
Measurement
MB
NA
No
X
No (Goal Only)
No
X
No (Goal Only)
No
X
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG22GF1
0.658
0.0028
<20 RSD
77 - 92 %R
96-100 %R
3. 2 ppb and >
0.9998
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
No
X
"H"
No
X


No
X


No descriptive narratives were provided by FIU.
Sample for total mercury was digested past holding time.
Holding time goals set for the length and weight measurements are guidelines only, not a hard deadline.
Measurements offish length and weight were measured after holding time goals.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M4-872-FIF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
X
X
Not Noted
Date/No Time
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA
Validation Criteria
                Applied Qualifiers \_
X =  Attached or Verified


Data Qualifiers

"J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"   Analyte concentration in the associated blank was >3 times the MDL.
"H"   Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
INTERLABORATORY COMPARISONS
-------
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-------
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-------
May 1999 Samples

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-------
EVERGLADES ECOSYSTEM ASSESSMENT
         (PHASE II REMAP)
            Data Review
      September 1999 Sampling
-------
                         Data Review, September 1999 Sampling

                                       Fore ward

The data review documents developed by the US Environmental Protection Agency (EPA) as
part of the Investigation of Mercury Contamination in the Florida Everglades Ecosystem and
Everglades Ecosystem Assessment (Phase II REMAP) Project are presented in the Data Review
May 1999 (M4) and September 1999 Sampling (M5) documents.

The Phase II data review determines whether the Data Quality Objectives (DQO) have been
satisfied as outlined in the Quality Assurance Project Plan (QAPP). The M4 and M5 Sampling
results were analyzed to determine whether they met the criteria developed during the planning
phase and whether the total error within the tolerable decision error ranges as specified in the
QAPP to support decisions.

The Data Review, September 1999 Sampling document summarizes the assessments of the
critical and non-critical parameters. Ten percent of the samples were randomly selected during
the validation process to characterize the quality of the data set. Three of the eleven critical
parameters are qualified with a "J". Parameters associated with this qualifier should be
considered an estimate for a number of quality control variances. The results for methylmercury
in surface water, methylmercury and in soil and bulk density in soil should be considered an
estimate based on findings. A table summarizing the critical and non-critical parameters is
enclosed in the Data Review document along with the detailed calculations and criteria for each
selected sample and parameter.
-------
                              TABLE OF CONTENTS
1.     Critical QA/QC Summaries
      la.    SERC
      Ib.   Battelle

2.     Non-Critical QA/QC Summaries
      2a.    SERC
      2b.   Battelle

3.     Critical QA/QC Review
      3 a.   Water-SERC
      3b.   Water - Battelle
      3c.    Soil - SERC
      3d.   Fish - SERC

4.     Interlaboratory Comparisons
-------
CRITICAL QA/QC SUMMARIES
-------
EPA  SESD  South Florida Phase II Wet Season Sampling: September 1999
Summarized Qualifiers for  10%  of the Critical Parameters Reviewed
Station ID
M5-622
M5-633
M5-643
M5-653
M5-663
M5-673
M5-683
M5-693
M5-703
M5-714
M5-726
M5-738
M5-828
M5-944
M5-656
M5-661
M5-672
M5-684
M5-712
M5-823
M5-920
Qualifier
Notation
Surface Water
SERC Laboratory
Total Phosphorus
»**»
»**»
»**»
»**»
»**»
"B(NR)"
"B(NR)"
"B(NR)M
"B(NR)"
"B(NR)M
»**»
»**»
»**»
»**»








Total Nitrogen
»**»
»**»
»**»
»**»
»**»
»**»
»**»
»**»
»**»
»**»
»**»
»**»
»**»
»**»>»M"








TOG









"H"
"H"
"H"

"H"








Total Mercury



"M"


















Battelle Lab
Methyl Mercury

11 M"
11 M"







"M", "DQO"
"M", "DQO"


"M"
11 M"
11 M"
"M"


"M", "DQO"
"J"
Soil/ Sediment
SERC Laboratory
Methyl Mercury

11 M"
11 M"
"DQO CNR)"
"M"

"M", "DQO"
"M", "DQO"
"M", "DQO"
"M", "DQO"
"M"
"DQO"
"DQO CNR)", "M"
"M", "DQO"







"J"
Total Phosphorus
"B CNR)"
"B CNR)"
"B (NR)"
"B (NR)"
"B (NR)"
"B (NR)"
"B (NR)"
"B (NR)"
"B (NR)"
"B (NR)"
"B (NR)"
"B (NR)"
"B (NR)"
"B (NR)"








AFDW
"DQO (NR)"
"DQO (NR)"
"DQO (NR)"
"DQO (NR)"
"DQO (NR)"
"DQO (NR)"
"DQO (NR)"
"DQO (NR)"
"DQO (NR)"
"DQO (NR)"
"DQO (NR)"
"DQO (NR)"
"DQO (NR)"
"DQO (NR)"








Bulk Density
"DQO (NR)"
"DQO (NR)"
"DQO CNR)"
"DQO (NR)"
"DQO (NR)"
"DQO CNR)"
"DQO CNR)"
"DQO (NR)"
"DQO (NR)"
"DQO CNR)"
"DQO CNR)"
"DQO (NR)"
"DQO (NR)"
"DQO (NR)"







"J", "***"
Fish
SERC Laboratory
Total Mercury

11 M"




















Length/Weight






















"J"  Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met

"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Obj ective/QAPP control limits.

" *"  The matrix recoveries were below QAPP QA limits.  MeHg matrix spikes are run with every sample and the sample is adjusted based on matrix affects.
" **" Blanks were reported above the MDL. Lab water was used as the blank water but not in the sample digestion process.
" ***" Phase II soil/sediment samples were prepped with a high speed blender which may alter comparability with the phase I bulk density values.
Comments:
The coefficient of variance (R2) values for methyl mercury were not reviewed.
-------
SERC
-------
EPA SESD South Florida Phase II Wet Season Sampling: September 1999
Summarized Findings of the Full QA/QC Review
Total Mercury in Surface Water Analyzed By SERC








Sample ID by QC
Batch
M5-622-SWF
M5-633-SWF
M5-643-SWF
M5-653-SWF
M5-663-SWF
M5-673-SWF
M5-683-SWF
M5-693-SWF
M5-703-SWF
M5-714-SWF
M5-726-SWF
M5-738-SWF
M5-828-SWF
M5-944-SWF


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Footnotes:

" X " Indicates this situation did occur.
-------
EPA SESD South Florida Phase II Wet Season Sampling:  September 1999
Summarized Findings of the Full QA/QC Review
Total Mercury in Fish Analyzed By SERC











Sample ID by QC
Batch
M5-622-FIF
M5-633-FIF
M5-643-FIF
M5-653-FIF
M5-663-FIF
M5-673-FIF
M5-683-FIF
M5-693-FIF
M5-703-FIF
M5-714-FIF
M5-726-FIF
M5-738-FIF
M5-828-FIF
M5-944-FIF

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Footnotes:
" *** " Holding time goal only.
" X " Indicates this situation did occur.
-------
EPA SESD South Florida Phase II Wet Season Sampling:  September 1999
Summarized Findings of the Full QA/QC Review
Total Phosphorus in Surface Water Analyzed By SERC
^
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Sample ID by QC '5 a
Batch 1 |
M5-622-SWF
M5-633-SWF
M5-643-SWF
M5-653-SWF
M5-663-SWF
M5-673-SWF
M5-683-SWF
M5-693-SWF
M5-703-SWF
M5-714-SWF
M5-726-SWF
M5-738-SWF
M5-828-SWF
M5-944-SWF


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Footnotes:
" *** " Blanks were reported above the MDL. Lab water was used as the blank water but not in the sample digestion process.
      Procedures have been modified to correct this.
"NR" Data was not available for review.
" X " Indicates this situation did occur.
-------
EPA SESD South Florida Phase II Wet Season Sampling:  September 1999
Summarized Findings of the Full QA/QC Review
Total Nitrogen in Surface  Water Analyzed By SERC












Sample ID by QC
Batch
M5-622-SWF
M5-633-SWF
M5-643-SWF
M5-653-SWF
M5-663-SWF
M5-673-SWF
M5-683-SWF
M5-693-SWF
M5-703-SWF
M5-714-SWF
M5-726-SWF
M5-738-SWF
M5-828-SWF
M5-944-SWF
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Comments:
1. Blanks were not reviewed in this data set.

Footnotes:
" *** " Blanks were reported above the MDL. Lab water was used as the blank water but not in the sample digestion process
      Procedures have been modified to correct this.
" X " Indicates this situation did occur.
-------
EPA SESD South Florida Phase II Wet Season Sampling:  September 1999
Summarized Findings of the Full QA/QC Review
Total Organic Carbon in Surface Water Analyzed By SERC





Sample ID by QC
Batch
M5-622-SWF
M5-633-SWF
M5-643-SWF
M5-653-SWF
M5-663-SWF
M5-673-SWF
M5-683-SWF
M5-693-SWF
M5-703-SWF
M5-714-SWF
M5-726-SWF
M5-738-SWF
M5-828-SWF
M5-944-SWF

1 j
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X
X
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"o
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Potential














Comments:
1. The laboratory comparisons that were performed did show a bias between the two laboratories.
The two laboratories are using two separate but approved EPA methods and instruments for the
TOC analysis.  This comparative difference may be cause by the methodology difference.
Footnotes:
" X " Indicates this situation did occur.
-------
EPA SESD South Florida Phase II Wet Season Sampling: September 1999
Summarized Findings of the Full QA/QC Review
Total Phosphorus in Soil Analyzed By SERC


Sample ID by QC
Batch
M5-622-SDF
M5-643-SDF
M5-663-SDF
M5-633-SDF
M5-653-SDF
M5-738-SDF
M5-673-SDF
M5-683-SDF
M5-693-SDF
M5-703-SDF
M5-714-SDF
M5-726-SDF
M5-828-SDF
M5-944-SDF
x
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No Dups/Reps Reviewed
No Blanks Reviewed in Batch
X
X
X
X
X
X
X
X
X
X
X
X
X
X
1
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Potential Matrix Effect (Data I














Comments:
1. No blank results were reviewed.
Footnotes:
" * " Holding time goal only.
" X " Indicates this situation did occur.
-------
EPA SESD South Florida Phase II Wet Season Sampling: September 1999
Summarized Findings of the Full QA/QC Review
Soil Ash-Free Dry Weight Analyzed By SERC













Sample ID by QC
Batch
M5-622-SDF
M5-633-SDF
M5-643-SDF
M5-653-SDF
M5-663-SDF
M5-673-SDF
M5-683-SDF
M5-693-SDF
M5-703-SDF
M5-714-SDF
M5-726-SDF
M5-738-SDF
M5-828-SDF
M5-944-SDF

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Footnotes:
" X "  Indicates this situation did occur.
-------
EPA SESD South Florida Phase II Wet Season Sampling: September 1999
Summarized Findings of the Full QA/QC Review
Soil Bulk Density Analyzed By SERC











Sample ID by QC
Batch
M5-622-SDF
M5-633-SDF
M5-643-SDF
M5-653-SDF
M5-663-SDF
M5-673-SDF
M5-683-SDF
M5-693-SDF
M5-703-SDF
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Footnotes:
"NR" Not Reviewed
" X " Indicates this situation did occur.
-------
Battelle
-------
EPA SESD South Florida Phase II Wet Season Sampling: September 1999
Summarized Findings of the Full QA/QC Review
Methylmercury in Surface Water Analyzed By Battelle Laboratory



Sample ID by QC
Batch
M5-622-SWB
M5-633-SWB
M5-643-SWB
M5-656-SWB
M5-661-SWB
M5-672-SWB
M5-684-SWB
M5-693-SWB
M5-703-SWB
M5-712-SWB
M5-726-SWB
M5-738-SWB
M5-823-SWB
M5-920-SWB
1
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X
X
X
X
X



X
X
X
X
Footnotes:
" X " Indicates this situation did occur.
-------
NON-CRITICAL QA/QC SUMMARIES
-------
SERC
-------
Non-Critical Parameters Analyzed by SERC
Review of the September, 1999 (M5) Data Set










Analysis
NH4
NO2
NO3
PO4
CH4
C02
APA
Mineral Content
Diatoms
Pigments
Chlorophyll a
Ethyl Mercury
Supporting Documentation


a
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a
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X
X
X
X
X
X
X
X
**
**
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a
5
X
X
X
X
X
X
X
X
X
**
**
**
Laboratory Records


a
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8

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X
X
X
X
X
X
NR
NA
X
**
**
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g
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Q
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X
X
X
X
X
X
X
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X
X
X
X
X
X
X
X
X
**
**
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13
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X
X
X
X
NR
NR
NR
NA
NR
**
**
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T3
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X
X
X
X
X
X
X
X
NR
**
**
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So
0
0
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Instrume
X
X
X
X
X
X
X
X
NR
**
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X
X
X
X
X
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X
X
X
X
X
X
X
NR
**
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$
"§
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X
X
X
NR
NR
NR
X
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•.§
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X
X
X
NR
NR
NR
NR
NR
NR
**
**
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Footnotes:
" * " Analyses are in the process of being analyzed.
" ** " No analyses required.
"NR" Not Reviewed
" NA " Not Applicable
" X " Indicates this situation did occur.
-------
Battelle
-------
Non-Critical Parameters Analyzed by Battelle Laboratories
Review of the September, 1999 (M5) Data Set











Analysis
Total Mercury (water)
Methylmercury (soil)
Methylmercury (floe)
Methylmercury (periphyton)
Supporting Documentation


a
PH
-^
a
o
Q'
PH
O

X
X
X
X

•§

3
PH

"§
s
a
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1
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NR
NR
NR
NR

01
0

§
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W
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g
1
NR
NR
NR
NR
Footnotes:
"NR" Not Reviewed
" X " Indicates this situation did occur.
-------
CRITICAL QA/QC REVIEW
-------
Water - SERC
-------
10 % Recalculated Results for Total Phosphorus in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-4-00
Checked by   njs 4-13-00
Sample
M5-622-SWF
M5-633-SWF
M5-643-SWF
M5-653-SWF
M5-663-SWF
Sample
MS
MS
UMS
UMS
CCV
CCV
CCV
CCV
CCV
CCV
CCV
M632
M632D
M642
M642D
M652
M652D
M662
M662D
Digestion Blk
Digestion Blk
QC Batch
EPA 1027 A
EPA1027A
EPA1027A
EPA 1027 A
EPA 1027 A
QC Batch
EPA 1027 A
EPA1027A
EPA1027A
EPA 1027 A
EPA 1027 A
EPA1027A
EPA1027A
EPA 1027 A
EPA 1027 A
EPA1027A
EPA1027A
EPA 1027 A
EPA 1027 A
EPA1027A
EPA1027A
EPA 1027 A
EPA 1027 A
EPA1027A
EPA1027A
EPA 1027 A
EPA 1027 A
Qualifier
Note





Qualifier
Note



















"B"
"B"
Dilution
1
1
1
1
1
Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Rep
um
0.220441
0.922642
1.001121
2.309137
0.182714
Rep
um
1.732597
1.78027
0.535236
0.550322
1.444091
1.482448
1.502425
1.500608
1.528572
1.52873
1.469296
1.004262
1.016345
3.067382
2.946699
0.16731
0.191554
0.193647
0.178326
0.08028
0.073422
Base Line
Factor
um
-0.07
-0.07
-0.07
-0.07
-0.07
Base Line
Factor
um
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
Peak-
Base Line
um
0.290441
0.992642
1.071121
2.379137
0.252714
Peak-
Base Line
um
1.803
1.850
0.605
0.620
1.552
1.572
1.571
1.599
1.599
1.539
1.074
1.086
1.086
3.137
3.017
0.237
0.262
0.264
0.248
0.150
0.143
MW
g
31
31
31
31
31
MW
g
31
31
31
31
31
31
31
31
31
31
31
31
31
31
31
31
31
31
31
31
31
Corrected
Peak
'MW
9.003671
30.771902
33.204751
73.753247
7.834134
Corrected
Peak
'MW
55.88
57.36
18.76
19.23
48.13
48.75
48.69
49.56
49.56
47.72
33.30
33.68
33.68
97.26
93.52
7.36
8.11
8.17
7.70
4.66
4.45
Sample
Results
ppm
0.0090
0.031
0.033
0.074
0.0078
Sample
Results
ppm
0.05588
0.05736
0.01876
0.01923
0.04813
0.04875
0.04869
0.04956
0.04956
0.04772
0.03330
0.03368
0.03368
0.09726
0.09352
0.00736
0.00811
0.00817
0.00770
0.00466
0.00445
Detection
Limit
ppm
0.0006
0.0006
0.0006
0.0006
0.0006
Detection
Limit'3
ppm
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018

SPK
CONC
(ppm)
0.04092
0.04092


0.05
0.05
0.05
0.05
0.05
0.05
0.05










R%
90.7
93.2


96.25
97.49
97.38
99.11
99.12
95.44
66.60










RPD

-2.610

-2.462








0.000

3.922

-9.720

5.985


-------
10 % Recalculated Results for Total Phosphorus in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-4-00
Checked by   njs 4-13-00
Sample
M5-673-SWF
M5-683-SWF
M5-693-SWF
M5-703-SWF
M5-714-SWF
Sample
MS
MS
UMS
UMS
CCV
CCV
CCV
CCV
CCV
CCV
CCV
Digestion Blk
Digestion Blk
QC Batch
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
QC Batch
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
Qualifier
Note





Qualifier
Note











Not Reported
Not Reported
Dilution
1
1
1
1
1
Dilution
1
1
1
1
1
1
1
1
1
1
1


Rep
um
0.199175
0.115462
0.119933
0.111397
0.089338
Rep
um
1.787068
1.88099
0.591248
0.402878
1.432253
1.482066
1.43088
1.482898
1.430812
1.474779
1.441135


Base Line
Factor
um
-0.06
-0.06
-0.06
-0.06
-0.06
Base Line
Factor
um
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06


Peak-
Base Line
um
0.259175
0.175462
0.179933
0.171397
0.149338
Peak-
Base Line
um
1.847
1.941
0.651
0.463
1.492
1.542
1.491
1.543
1.491
1.535
1.501


MW
g
31
31
31
31
31
MW
g
31
31
31
31
31
31
31
31
31
31
31


Corrected
Peak
'MW
8.034425
5.439322
5.577923
5.313307
4.629478
Corrected
Peak
'MW
57.26
60.17
20.19
14.35
46.26
47.80
46.22
47.83
46.22
47.58
46.54


Sample
Results
ppm
0.0080
0.0054
0.0056
0.0053
0.0046
Sample
Results
ppm
0.05726
0.06017
0.02019
0.01435
0.04626
0.04780
0.04622
0.04783
0.04622
0.04758
0.04654


Detection
Limit
ppm
0.0006
0.0006
0.0006
0.0006
0.0006
Detection
Limit'3
ppm
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018



SPK
CONC
(ppm)
0.04092
0.04092


0.05
0.05
0.05
0.05
0.05
0.05
0.05


R%
90.6
112.0


92.52
95.61
92.43
95.66
92.43
95.16
93.07


RPD

-4.959

33.815









Sample
M5-726-SWF
M5-738-SWF
M5-828-SWF
M5-944-SWF
Sample
MS
MS
UMS
UMS
CCV
CCV
CCV
CCV
CCV
Digestion Blk
Digestion Blk
QC Batch
EPA1027C
EPA1027C
EPA1027C
EPA1027C
QC Batch
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
Qualifier
Note




Qualifier
Note









"B"
"B"
Dilution
1
1
1
1
Dilution
1
1
1
1
1
1
1
1
1
1
1
Rep
um
0.093085
0.092087
0.199503
0.108243
Rep
um
1.696953
1.848965
0.582121
0.504826
1.461504
1.387512
1.437132
1.462591
1.432883
0.06032
0.065028
Base Line
Factor
um
-0.07
-0.07
-0.07
-0.07
Base Line
Factor
um
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
Peak-
Base Line
um
0.163
0.162
0.270
0.178
Peak-
Base Line
um
1.767
1.919
0.652
0.575
1.532
1.458
1.507
1.533
1.503
0.130
0.135
MW
g
31
31
31
31
MW
g
31
31
31
31
31
31
31
31
31
31
31
Corrected
Peak
'MW
5.055635
5.024697
8.354593
5.525533
Corrected
Peak
*MW
54.78
59.49
20.22
17.82
47.48
45.18
46.72
47.51
46.59
4.04
4.19
Sample
Results
ppm
0.005
0.005
0.008
0.006
Sample
Results
ppm
0.05478
0.05949
0.02022
0.01782
0.04748
0.04518
0.04672
0.04751
0.04659
0.00404
0.00419
Detection
Limit
ppm
0.0006
0.0006
0.0006
0.0006
Detection
Limit'3
ppm
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018
0.0018

SPK
CONC
(ppm)
0.04092
0.04092


0.05
0.05
0.05
0.05
0.05


R%
84.5
101.8


94.95
90.37
93.44
95.02
93.18


RPD

-8.248

12.600







-------
SERC Lab / EPA REMAP results
Total Phosphorus (TP) in Water by EPA Method 365.1 (modified)
: Analysis not performed
: Analysis not required
: Average of Two
Data Entered by:   njs  03-22-00
                                                                                                                                                Data Entry Checked by:mwb  03-28-00
Sampling Station
ID
M5-622-SWF
M5-623-SWF
M5-624-SWF
M5-625-SWF
M5-626-SWF
M5-627-SWF
M5-628-SWF
M5-630-SWF
M5-631-SWF
M5-632-SWF
M5-633-SWF
M5-634-SWF
M5-635-SWF
M5-636-SWF
M5-637-SWF
M5-638-SWF
M5-639-SWF
M5-640-SWF
M5-641-SWF
M5-642-SWF
M5-643-SWF
M5-644-SWF
M5-645-SWF
M5-646-SWF
M5-647-SWF
M5-648-SWF
M5-649-SWF
M5-650-SWF
M5-651-SWF
M5-652-SWF
M5-653-SWF
M5-654-SWF
M5-655-SWF
M5-656-SWF
M5-657-SWF
M5-658-SWF
M5-659-SWF
M5-660-SWF
M5-661-SWF
M5-662-SWF
M5-663-SWF
Matrix
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
Collection
Date
09/30/99
09/30/99
09/30/99
09/30/99
09/30/99
09/30/99
09/29/99
09/28/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/28/99
09/29/99
09/28/99
09/29/99
09/29/99
09/30/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/27/99
09/28/99
09/27/99
09/27/99
09/29/99
09/27/99
09/27/99
Time
1125
915
1018
1257
908
1050
1716
1520
1414
1010
1115
1510
1216
1405
1210
1630
1715
1116
1615
1011
910
1145
1447
1515
1102
1300
1620
1158
1410
959
1300
1145
1028
900
1751
1722
1205
1450
857
1610
1330
Digestion
Date
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
Run
Date
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
Time Elapsed
From Dig
8
8
8
8
8
8
9
10
9
9
9
9
9
9
9
9
10
9
10
9
9
8
10
10
10
10
10
10
10
10
10
10
10
10
11
10
11
11
9
11
11
Holding
Time (Days)
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
uM Instrument
Reading
0.220441
0.324684
0.173010
0.196394
0.191195
0.417754
0.221019
0.228900
0.243414
1.010300
0.922642
0.241825
0.240206
0.207492
0.284648
0.227518
1.362922
0.410096
0.398678
3.007040
1.001121
0.236817
0.924768
0.440584
0.348737
0.265804
0.222554
0.126759
0.381606
0.179430
2.309137
0.296783
2.465914
0.254429
0.432250
0.242427
0.215606
0.842130
0.186499
0.185990
0.182714
Blank
Correction
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
Corrected
uM Reading
0.290441
0.394684
0.243010
0.266394
0.261195
0.487754
0.291019
0.298900
0.313414
1.080300
0.992642
0.311825
0.310206
0.277492
0.354648
0.297518
1.432922
0.480096
0.468678
3.077040
1.071121
0.306817
0.994768
0.510584
0.418737
0.335804
0.292554
0.196759
0.451606
0.249430
2.379137
0.366783
2.535914
0.324429
0.502250
0.312427
0.285606
0.912130
0.256499
0.255990
0.252714
Phosphorus
Units (ppm, ug/g)
0.0090
0.012
0.0075
0.0083
0.0081
0.015
0.0090
0.0093
0.0097
0.033
0.031
0.0097
0.0096
0.009
0.011
0.0092
0.044
0.015
0.015
0.095
0.0332
0.0095
0.031
0.016
0.013
0.010
0.0091
0.0061
0.014
0.0077
0.074
0.011
0.079
0.0101
0.0156
0.0097
0.0089
0.028
0.0080
0.0079
0.0078
Detection
Limit (ppm)
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
QA/QC
Batch ID
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
QA Data
%R
83
83
83
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
%RPD
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
Matrix %R
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
Sample RPD









-1.2









4.01









-13.5









-3.8


Notes









Averaged Result









Averaged Result









Averaged Result









Averaged Result

-------
Sampling Station
ID
M5-664-SWF
M5-665-SWF
M5-666-SWF
M5-667-SWF
M5-668-SWF
M5-669-SWF
M5-670-SWF
M5-671-SWF
M5-672-SWF
M5-673-SWF
M5-674-SWF
M5-675-SWF
M5-676-SWF
M5-677-SWF
M5-678-SWF
M5-679-SWF
M5-680-SWF
M5-681-SWF
M5-682-SWF
M5-683-SWF
M5-684-SWF
M5-685-SWF
M5-686-SWF
M5-687-SWF
M5-688-SWF
M5-689-SWF
M5-690-SWF
M5-691-SWF
M5-692-SWF
M5-693-SWF
M5-694-SWF
M5-695-SWF
M5-696-SWF
M5-697-SWF
M5-698-SWF
M5-699-SWF
M5-700-SWF
M5-701-SWF
M5-702-SWF
M5-703-SWF
M5-704-SWF
M5-705-SWF
M5-706-SWF
M5-707-SWF
M5-708-SWF
Matrix
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
Collection
Date
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/26/99
09/27/99
09/27/99
09/26/99
09/26/99
09/28/99
09/26/99
09/26/99
09/26/99
09/27/99
09/26/99
09/26/99
09/26/99
09/26/99
09/26/99
09/25/99
09/25/99
09/26/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/26/99
09/25/99
09/25/99
09/25/99
09/26/99
09/25/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
Time
1100
1710
1655
1545
1207
1000
850
850
1100
1400
1025
1130
925
1310
1213
1335
900
1410
1615
850
1530
1434
915
1035
1527
1205
1350
1554
1200
1139
1702
1400
1510
1637
1030
1635
1750
1740
918
1655
1615
1725
1555
1500
900
Digestion
Date
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
Run
Date
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
Time Elapsed
From Dig
11
11
11
11
11
11
11
12
11
11
12
12
10
12
12
12
11
12
12
12
12
12
13
13
12
13
13
13
13
13
13
13
13
12
13
13
13
12
13
14
14
14
14
14
14
Holding
Time (Days)
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
uM Instrument
Reading
0.220172
0.142434
0.187586
0.247630
0.195497
0.172297
0.127174
0.130301
0.155700
0.199175
0.140264
0.163569
0.225253
0.195496
0.187692
0.162378
0.137051
0.118766
0.099750
0.115462
0.107606
0.127229
0.177588
0.170491
0.114608
0.100074
0.094508
0.107701
0.149260
0.119933
0.105080
0.095180
0.099830
0.141901
0.101514
0.101414
0.093274
0.108139
0.083187
0.111397
0.113856
0.130517
0.089133
0.152922
0.108196
Blank
Correction
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
Corrected
uM Reading
0.290172
0.212434
0.257586
0.317630
0.265497
0.242297
0.197174
0.200301
0.215700
0.259175
0.200264
0.223569
0.285253
0.255496
0.247692
0.222378
0.197051
0.178766
0.159750
0.175462
0.167606
0.187229
0.237588
0.230491
0.174608
0.160074
0.154508
0.167701
0.209260
0.179933
0.165080
0.155180
0.159830
0.201901
0.161514
0.161414
0.153274
0.168139
0.143187
0.171397
0.173856
0.190517
0.149133
0.212922
0.168196
Phosphorus
Units (ppm, ug/g)
0.0090
0.0066
0.0080
0.0098
0.0082
0.0075
0.0061
0.0062
0.0067
0.0080
0.0062
0.0069
0.0088
0.0079
0.0077
0.0069
0.0061
0.0055
0.0050
0.0054
0.0052
0.0058
0.0074
0.0071
0.0054
0.0050
0.0048
0.0052
0.0065
0.0056
0.0051
0.0048
0.0050
0.0063
0.0050
0.0050
0.0048
0.0052
0.0044
0.0053
0.0054
0.0059
0.0046
0.0066
0.0052
Detection
Limit (ppm)
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
QA/QC
Batch ID
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027A
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
QA Data
%R
83
83
83
83
83
83
83
83
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
%RPD
2.7
2.7
2.7
2.7
2.7
2.7
2.7
2.7
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
Matrix %R
97.1
97.1
97.1
97.1
97.1
97.1
97.1
97.1
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
107
Sample RPD








-14.1









7.84









6.4

















Notes








Averaged Result









Averaged Result









Averaged Result
















-------
Sampling Station
ID
M5-709-SWF
M5-710-SWF
M5-711-SWF
M5-712-SWF
M5-714-SWF
M5-715-SWF
M5-716-SWF
M5-718-SWF
M5-719-SWF
M5-720-SWF
M5-722-SWF
M5-723-SWF
M5-724-SWF
M5-725-SWF
M5-726-SWF
M5-727-SWF
M5-728-SWF
M5-729-SWF
M5-730-SWF
M5-731-SWF
M5-732-SWF
M5-733-SWF
M5-734-SWF
M5-735-SWF
M5-738-SWF
M5-740-SWF
M5-741-SWF
M5-742-SWF
M5-743-SWF
M5-744-SWF
M5-745-SWF
M5-746-SWF
M5-747-SWF
M5-823-SWF
M5-828-SWF
M5-838-SWF
M5-848-SWF
M5-859-SWF
M5-868-SWF
M5-878-SWF
M5-890-SWF
M5-908-SWF
M5-920-SWF
M5-932-SWF
M5-944-SWF
Matrix
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
Collection
Date
09/24/99
09/24/99
09/24/99
09/24/99
09/23/99
09/24/99
09/24/99
09/24/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/22/99
09/23/99
09/23/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/30/99
09/29/99
09/29/99
09/28/99
09/27/99
09/27/99
09/26/99
09/25/99
09/24/99
09/23/99
09/23/99
09/22/99
Time
1330
1430
1115
905
1715
1145
1310
1030
1715
0
1600
1500
1442
1323
1230
1216
1350
1027
1120
1725
917
910
1540
1700
1410
1245
1534
1418
1130
1224
1120
948
942
0
0
0
0
0
0
0
0
0
0
0
1224
Digestion
Date
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
12/09/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
Run
Date
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
12/21/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
10/27/99
Time Elapsed
From Dig
14
14
14
14
15
14
14
14
15
15
15
15
15
15
15
15
15
15
15
16
77
15
16
16
16
16
16
16
16
16
16
16
16
8
9
9
10
11
11
12
13
14
15
15
16
Holding
Time (Days)
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
uM Instrument
Reading
0.125360
0.092072
0.122320
0.084478
0.089338
0.072499
0.087589
0.086011
0.103145
0.088199
0.084810
0.083362
0.098319
0.088023
0.093085
0.087421
0.117803
0.095400
0.119505
0.080596
-0.019733
0.125068
0.115092
0.116421
0.092087
0.107290
0.107995
0.085193
0.062130
0.061631
0.084750
0.103167
0.131585
0.257252
0.199503
0.230777
0.282932
0.207392
0.202190
0.161276
0.101030
0.105677
0.089756
0.098859
0.108243
Blank
Correction
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.06
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.02
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
-0.07
Corrected
uM Reading
0.185360
0.152072
0.182320
0.144478
0.149338
0.132499
0.147589
0.146011
0.163145
0.148199
0.144810
0.143362
0.168319
0.158023
0.163085
0.157421
0.187803
0.165400
0.189505
0.150596
0.000267
0.195068
0.185092
0.186421
0.162087
0.177290
0.177995
0.155193
0.132130
0.131631
0.154750
0.173167
0.201585
0.327252
0.269503
0.300777
0.352932
0.277392
0.272190
0.231276
0.171030
0.175677
0.159756
0.168859
0.178243
Phosphorus
Units (pprn, ug/g)
0.0057
0.0047
0.0057
0.0045
0.0046
0.0041
0.0046
0.0045
0.0051
0.0046
0.0045
0.0044
0.0052
0.0049
0.0051
0.0049
0.0058
0.0051
0.0059
0.0047
ND
0.0060
0.0057
0.0058
0.0050
0.0055
0.0055
0.0048
0.0041
0.0041
0.0048
0.0054
0.0062
0.010
0.0084
0.0093
0.011
0.0086
0.0084
0.0072
0.0053
0.0054
0.0050
0.0052
0.0055
Detection
Limit (ppm)
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
QA/QC
Batch ID
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027B
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
RR1221B
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
EPA1027C
QA Data
%R
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
86.6
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
99.3
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
83.5
%RPD
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
4.5
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
8.6
Matrix %R
107
107
107
107
107
107
107
107
107
107
107
107
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
103.5
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
98.4
Sample RPD
8.2









4



















1.5









8.3





Notes
Averaged Result









Averaged Result









Sample was RR at Later Date









Averaged Result









Averaged Result




-------
Sampling Station
ID
QA-042-PEF
QA-031-PEF
QA-009-CB1
QA-008-CB1
QA-004-CB1
QA-003-CB2
QA-002-CB1
QA-001-CB2
QA-006-CB2
QA-008-CB2
QA-003-CB1
QA-001-CB1
QA-004-CB1
QA-007-CB2
QA-006-CB1
QA-005-CB2
QA-009-CB1
QA-005-CB1
QA-007-CB1
QA-002-CB2
Matrix
QA
QA
QA
QA
QA
QA
QA
QA
QA
QA
QA
QA
QA
QA
QA
QA
QA
QA
QA
QA
Collection
Date




















Time




















Digestion
Date
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
Run
Date
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
11/04/99
Time Elapsed
From Dig
36441
36441
36441
36441
36441
36441
36441
36441
36441
36441
36441
36441
36441
36441
36441
36441
36441
36441
36441
36441
Holding
Time (Days)
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
uM Instrument
Reading
4.983843
0.092094
0.037971
0.006699
-0.019526
-0.032538
-0.045807
-0.041997
-0.052202
-0.051369
-0.051713
-0.049857
-0.044320
-0.022949
-0.039655
-0.050702
-0.075141
-0.064787
-0.086683
-0.098451
Blank
Correction
-0.05
-0.05
-0.05
-0.05
-0.05
-0.05
-0.05
-0.05
-0.05
-0.05
-0.05
-0.05
-0.05
-0.05
-0.05
-0.05
-0.05
-0.05
-0.05
-0.05
Corrected
uM Reading
5.033843
0.142094
0.087971
0.056699
0.030474
0.017462
0.004193
0.008003
-0.002202
-0.001369
-0.001713
0.000143
0.005680
0.027051
0.010345
-0.000702
-0.025141
-0.014787
-0.036683
-0.048451
Phosphorus
Units (ppm, ug/g)
0.16
0.0044
0.0027
0.0018
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
Detection
Limit (ppm)
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
0.0006
QA/QC
Batch ID
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QAPEF-B
QA Data
%R
119.0
119.0
119.0
119.0
119.0
119.0
119.0
119.0
119.0
119.0
119.0
119.0
119.0
119.0
119.0
119.0
119.0
119.0
119.0
119.0
%RPD
3.8
3.8
3.8
.8
.8
.8
.8
.8
.8
.8
.8
.8
.8
.8
.8
.8
.8
.8
.8
.8
Matrix %R
91.5
91.5
91.5
91.5
91.5
91.5
91.5
91.5
91.5
91.5
91.5
91.5
91.5
91.5
91.5
91.5
91.5
91.5
91.5
91.5
Sample RPD





0









0





Notes





Averaged Result









Averaged Result




-------
10 % Recalculated Results for Total Nitrogen in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-4-00
                                   Checked by
                                                njs 4-13-00
Sample
M5-622-SWF
M5-633-SWF
M5-643-SWF
M5-646-SWF
M5-646-SWF-DUP
QC CHECK
FINAL QC CHECK
CALIBRATION(CCV)
UMS
MS
MSD

M5-653-SWF
M5-663-SWF
M5-670-SWF
M5-670-SWF-DUP
QC CHECK
FINAL QC CHECK
CALIBRATION(CCV)
UMS
MS
MSD

M5-673-SWF
M5-683-SWF
M5-693-SWF
M5-694-SWF
M5-694-SWF-DUP
QC CHECK
FINAL QC CHECK
CALIBRATION(CCV)
UMS
MS
MSD
QC
Batch
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99

ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99
ANTEK1 1-22-99

ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
Qualifier
Note


































Dilution
1
1
1
1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1
1
1
1
Repl
uM
343227
511879
413455
467139
357426
560256
511349
599725
224783
427292
447712

441081
248754
132693
138862
493197
530841
488747
159247
360735
357436

124723
86567
175772
196447
211076
531665
537072
513634
154071
378548
381315
Rep 2
uM
318989
844769
343769
462189
384134
560542
689147
617711
235423
426493
441435

467484
125909
178325
184219
494798
479427
486099
157095
357060
357852

130483
111428
183734
178343
218146
499298
509934
516662
148739
373538
382807
Rep 3
uM
341182
318851
349515
411953
609733
545656
NO DATA
597817
201768
439335
445373

454801
130425
189752
190633
503545
500823
480706
153871
352655
375127

142041
157823
152063
188588
211602
501055
517494
504139
140462
385616
417639
Rep 4
uM






532575

190281








486774

129351









518542

155780


Rep 5
uM






505166

200777








481913

143166









506820

137622


Rep 6
uM






516596

195350








488754

169985









533937

140945


Average
Replicates
uM
334466
558500
368913
447094
450431
555485
550967
605084
208064
431040
444840

454455
168363
166923
171238
497180
494755
485184
152119
356817
363472

132416
118606
170523
187793
213608
510673
520633
511478
146270
379234
393920
Blank
Correction
uM


































Corrected
Peak
uM
334466
558500
368913
447094
450431
555485
550967
605084
208064
431040
444840

454455
168363
166923
171238
497180
494755
485184
152119
356817
363472

132416
118606
170523
187793
213608
510673
520633
511478
146270
379234
393920
Slope
3.46767E-06
3.46767E-06
3.46767E-06
3.46767E-06
3.46767E-06
3.46767E-06
3.46767E-06
3.46767E-06
3.46767E-06
3.46767E-06
3.46767E-06

4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06

3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
Average
Replicate
x Slope
1.16
1.94
1.28
1.55
1.56
1.93
1.91
2.10
0.72
1.49
1.54

1.86
0.69
0.68
0.70
2.03
2.02
1.98
0.62
1.46
1.48

0.51
0.46
0.66
0.72
0.82
1.97
2.01
1.97
0.56
1.46
1.52
Dilution
Correction


































Sample
Results
ppm
1.16
1.94
1.28
1.55
1.56
1.93
1.91
2.10
0.72
1.49
1.54

1.86
0.69
0.68
0.70
2.03
2.02
1.98
0.62
1.46
1.48

0.51
0.46
0.66
0.72
0.82
1.97
2.01
1.97
0.56
1.46
1.52
Detection
Limit
/3 times (ppm)
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09

0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09

0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
SPK
CONC
(ppm)





2
2
2

1
1





2
2
2

1
1






2
2
2

1
1
R%





96.31
95.53
104.91

77.32
82.11





101.48
100.98
99.03

83.56
86.28






98.53
100.45
98.69

89.90
95.56
RPD




-0.744





-3.151




-2.552





-1.848





-12.863





-3.799
-------
10 % Recalculated Results for Total Nitrogen in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-4-00
                                       Checked by
                                                     njs 4-13-00
Sample
M5-703-SWF
M5-714-SWF
M5-720-SWF
M5-720-SWF-DUP
QC CHECK
FINAL QC CHECK
CALIBRATION (CCV
UMS
MS
MSD

M5-726-SWF
M5-738-SWF
M5-828-SWF
M5-823-SWF
M5-823-SWF-DUP
QC CHECK
FINAL QC CHECK
CALIBRATION (CCV
UMS
MS
MSD

M5-944-SWF
QA-PEF-042
QC CHECK
FINAL QC CHECK
CALIBRATION (CCV
UMS
MS
MSD

QC
Batch
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99

ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99
ANTEK 11-23-99

ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00

Qualifier
Note























"H"





"M"
"M"

Dilution
1
1
1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1

Repl
uM
198265
146542
157942
204677
494705
538788
531113
192383
399174
470479

101698
55020
142608
479929
332540
499770
521009
500661
185143
454798
488734

75363
91241
557158
531646
466930
235981
418044
412190

Rep 2
uM
209979
149006
157993
175963
500641
515388
538721
NO DATA
NO DATA
473802

97999
53674
128039
254735
263435
501408
517753
497732
190928
476171
422468

71121
88966
541509
450310
473767
220498
422999
406787

Rep 3
uM
200283
154812
263983
192998
501261
546990
533640
166266
422194
437260

102123
58051
141499
221256
271018
508584
511477
499122
191269
460173
419473

80588
84138
516509
446252
449217
211487
403444
408984

Rep 4
uM





517572

162009









510048

190971






431370

214280



Rep 5
uM





522517

178392









506203

186138






432341

208237



Rep 6
uM





516741

NO DATA









502547

182724






420695

204126



Average
Replicates
uM
202842
150120
193306
191213
498869
526333
534491
174763
410684
460514

100607
55582
137382
318640
288998
503254
511506
499172
187862
463714
443558

75691
88115
538392
452102
463305
215768
414829
409320

Blank
Correction
uM
































Corrected
Peak
uM
202842
150120
193306
191213
498869
526333
534491
174763
410684
460514

100607
55582
137382
318640
288998
503254
511506
499172
187862
463714
443558

75691
88115
538392
452102
463305
215768
414829
409320

Slope
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06

3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06

3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06

Average
Replicate
x Slope
0.81
0.60
0.77
0.76
1.99
2.10
2.13
0.70
1.64
1.84

0.40
0.22
0.55
1.27
1.15
2.00
2.03
1.99
0.75
1.84
1.76

0.28
0.33
2.02
1.70
1.74
0.81
1.56
1.54

Dilution
Correction
































Sample
Results
ppm
0.81
0.60
0.77
0.76
1.99
2.10
2.13
0.70
1.64
1.84

0.40
0.22
0.55
1.27
1.15
2.00
2.03
1.99
0.75
1.84
1.76

0.28
0.33
2.02
1.70
1.74
0.81
1.56
1.54

Detection
Limit
/3 times (ppm)
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09

0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09

0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09

SPK
CONC
(ppm)




2
2
2

1
1






2
2
2

1
1



2
2
2

1
1

R%




99.47
104.95
106.58

94.09
113.96






100.10
101.74
99.29

109.73
101.72



101.07
84.87
86.98

74.74
72.67

RPD



1.089





-11.439





9.757





4.443








1.337

"M" Analyte ext
"B" Analyte com
"H" Analysis dig
le associated blai
led after holding
                            sxpired.
-------
Total Nitrogen in Surface Water by Antek 7000N Analyzer
Analyzed by Florida International University (SERC) for the M5 Sampling Event
Entered by P Meyer 3-16-00
                                                                                   Checked by MWB 3-17-99

Sample ID
C bration Std
M -859-SWF
M -868-SWF
M -878-SWF
M -890-SWF
M -908-SWF
M -920-SWF
M -932-SWF
M -944-SWF
QA-PEF-042
Method Elk
QC CHECK
FINAL QC CHECK
CALIBRATION (CCV)
UMS
MS
MSB
Collect! o
Date

09/27/99
09/27/99
09/26/99
09/25/99
09/24/99
09/23/99
09/23/99
09/22/99
09/30/99







n
Time



0
0
0
0
0
1224








Digestion
Date

10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99

10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
Analysis
Date

02/24/00
02/24/00
02/24/00
02/24/00
02/24/00
02/24/00
02/24/00
02/24/00
02/24/99

02/24/00
02/24/00
02/24/00
02/24/00
02/24/00
02/24/00
Holding
Time

28
28
28
28
28
28
28
28
28







Time since
Digestion

11
11
12
13
14
15
15
16








Batch
ID
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00
ANTEK 2-24-00

Dil tion

















Rep 1
uM
525701
215269
154271
134538
144939
186405
177019
90343
75363
91241

557158


235981
418044
412190
Rep 2
uM
526548
219742
150371
120681
121187
150770
153909
93132
71121
88966

541509


220498
422999
406787
Rep 3
uM
545812
262595
132374
135089
139085
147939
135265
92001
80588
84138

516509

449217
211487
403444
408984
Rep 4
uM














214280


Rep 5
uM














208237


Rep 6
uM














204126


Average
Replicates
uM
532687
232535
145672
130103
135070
161705
155398
91825
75691
88115
#DIV/0!
538392
452102
463305
215768
414829
409320
Blank
Correction
uM

















Corrected
Peak
uM

















Slope

3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
3.75455E-06
Sample
Results
ppm
2.0
0.87
0.55
0.49
0.51
0.61
0.58
0.34
0.28
0.33
#DIV/0!
2.0
1.70
1.74
0.81
1.56
1.54
Detection
Limit
/3 times (ppm)
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
SPK
CONC
(ppm)











2
2
2
0
1
1
R%












101.1
84.9
87.0

74.7
72.7
RPD

















0.702

Notes


















Sample ID
Calibration Std
M5-622-SWF
M5-623-SWF
M5-624-SWF
M5-625-SWF
M5-626-SWF
M5-627-SWF
M5-628-SWF
M5-630-SWF
M5 -631 -SWF
M5-632-SWF
M5 -63 3 -SWF
M5-634-SWF
M5 -63 5 -SWF
M5-636-SWF
M5-637-SWF
M5-638-SWF
M5-639-SWF
M5-640-SWF
M5 -641 -SWF
M5-642-SWF
M5 -643 -SWF
M5-644-SWF
M5 -645 -SWF
M5-646-SWF
M5-646-SWF-DUP
M5-647-SWF
QC CHECK
FINAL QC CHECK
CALIBRATION (CCV)
UMS
MS
MSB
Collect™
Date

09/30/99
09/30/99
09/30/99
09/30/99
09/30/99
09/30/99
09/29/99
09/28/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/28/99
09/29/99
09/28/99
09/29/99
09/29/99
09/30/99
09/28/99
09/28/99
09/28/99
09/28/99






n
Time

1125
915
018
257
908
050
716
520
414
010
115
510
216
405
210
630
715
116
615
Oil
910
145
447
515
515
102






Digestion
Date
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
Analysis
Date
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
Holding
Time

28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
Time since
Digestion

8
8
8
8
8
8
9
10
9
9
9
9
9
9
9
9
10
9
10
9
9
8
10
10
10
10






Batch
ID
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99
ANTEK 11-22-99

Dil tion

































Rep 1
uM
580137
343227
338124
378167
335255
621794
642521
265927
835842
357200
365165
511879
361473
905949
372070
253943
236881
327237
188703
310685
461827
413455
286634
707285
467139
357426
552856
560256
511349
599725
224783
427292
447712
Rep 2
uM
564196
318989
277642
279081
409948
581728
467336
206367
213832
237339
445994
844769
745377
481772
423498
259897
423609
365156
138353
302740
698305

262451
525432
462189
384134
319623
560542
689147
617711
235423
426493
441435
Rep 3
uM
606086
341182
277333
312097
364416
663964
476298
209182
223102
320197
912951
318851
442938
268626
461376
381327
400616
257248
144729
258700
525778
349515
419779
714747
411953
609733
303044
545656
NO DATA
597817
201768
439335
445373
Rep 4
uM
591585



























532575

190281


Rep 5
uM
549470



























505166

200777


Rep 6
uM
569066



























516596

195350


Average
Replicates
uM
576757
334466
297700
323115
369873
622495
528718
227159
424259
304912
574703
558500
516596
552116
418981
298389
353702
316547
157262
290708
561970
368913
322955
649155
447094
450431
391841
555485
550967
605084
208064
431040
444840
Blank
Correction
uM

































Corrected
Peak
uM

































Slope

3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
3. 6767E-06
Sample
Results
ppm
2.00
1.2
1.0
1.1
1.3
2.2
1.8
0.79
1.5
1.1
2.0
1.9
1.8
1.9
1.5
1.0
1.2
1.1
0.55
1.0
1.9
1.3
1.1
2.3
1.6
1.6
1.4
1.93
1.91
2.10
0.72
1.49
1.54
Detection
Limit
/3 times (ppm)
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
SPK
CONC
(ppm)



























2
2
2
0
1
1
R%




























96.3
95.5
104.9

77.3
82.1
RPD

























0







-1.501

Notes
























Averaged Result








-------

Sample ID
Calibration Std
M5-648-SWF
M5-649-SWF
M5-650-SWF
M5 -651 -SWF
M5-652-SWF
M5 -65 3 -SWF
M5-654-SWF
M5 -65 5 -SWF
M5-656-SWF
M5-657-SWF
M5-658-SWF
M5-659-SWF
M5-660-SWF
M5 -661 -SWF
M5-662-SWF
M5-663-SWF
M5-664-SWF
M5-665-SWF
M5-666-SWF
M5-667-SWF
M5-668-SWF
M5-669-SWF
M5-670-SWF
QC CHECK
FINAL QC CHECK
CALIBRATION (CCV)
UMS
MS
MSB


Sample ID
Calibration Std
M5-671-SWF
M5-672-SWF
M5 -6 73 -SWF
M5-674-SWF
M5 -6 75 -SWF
M5-676-SWF
M5-677-SWF
M5-678-SWF
M5-679-SWF
M5-680-SWF
M5 -681 -SWF
M5-682-SWF
M5-683-SWF
M5-684-SWF
M5-685-SWF
M5-686-SWF
M5-687-SWF
M5-688-SWF
M5-689-SWF
M5-690-SWF
M5 -691 -SWF
M5-692-SWF
M5-693-SWF
M5-694-SWF
M5-695-SWF
QC CHECK
FINAL QC CHECK
CALIBRATION (CCV)
UMS
MS
MSB
Collectio
Date

09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/27/99
09/28/99
09/27/99
09/27/99
09/29/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99







Collect™
Date

09/26/99
09/27/99
09/27/99
09/26/99
09/26/99
09/28/99
09/26/99
09/26/99
09/26/99
09/27/99
09/26/99
09/26/99
09/26/99
09/26/99
09/26/99
09/25/99
09/25/99
09/26/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99






n
Time

1300
1620
1158
1410
959
1300
1145
1028
900
1751
1722
1205
1450
857
1610
1330
1100
1710
1655
1545
1207
1000
850







n
Time

850
1100
1400
1025
1130
925
1310
1213
1335
900
1410
1615
850
1530
1434
915
1035
1527
1205
1350
1554
1200
1139
1702
1400






Digestion
Date
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99

Digestion
Date
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
Analysis
Date
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99
/22/99

Analysis
Date
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
Holding
Time

28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28

Holding
Time

28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28






Time since
Digestion

10
10
10
10
10
10
10
10
10
11
10
11
11
9
11
11
11
11
11
11
11
11
11







Time since
Digestion

2
1
1
2
2
0
2
2
2
1
2
2
2
2
2
3
3
2
3
3
3
3
3
3
3






Batch
ID
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1/22/99
ANTEK 1-22-99
ANTEK 1-22-99

Batch
ID
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99

Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1


Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Rep 1
uM
506725
195415
190073
202719
232284
164527
441081
232309
401981
158814
257813
197929
235091
256887
245546
161244
248754
192693
166592
120440
113845
119877
170769
132693
493197
530841
488747
159247
360735
357436

Rep 1
uM
500975
159878
104355
124723
125753
152390
231671
262468
174053
171738
129009
155596
125590
86567
108359
105053
151803
196358
129513
251223
141638
117331
94457
175772
196447
179958
531665
537072
513634
154071
378548
381315
Rep 2
uM
491602
170765
228829
226317
229024
136002
467484
212404
387514
118805
259558
226304
224708
250824
166289
168397
125909
231429
175533
133857
134726
109636
200535
178325
494798
479427
486099
157095
357060
357852

Rep 2
uM
497931
145674
101760
130483
124615
159548
120766
204605
90666
174425
209021
177528
149978
111428
135766
121757
169314
157124
92050
250206
122848
85892
100500
183734
178343
187320
499298
509934
516662
148739
373538
382807
Rep 3
uM
469167
661397
177650
210854
210486
145060
454801
253030
381470
125068
318288
309284
225942
209501
183237
168970
130425
227007
163906
161569
142422
125466
198617
189752
503545
500823
480706
153871
352655
375127

Rep 3
uM
509543
155948
95662
142041
122624
133916
105473
136064
99955
130581
139227
200755
155942
157823
230429
119290
211790
191307
96958
271243
116755
97653
115030
152063
188588
196348
501055
517494
504139
140462
385616
417639
Rep 4
uM
491126
























486774

129351



Rep 4
uM
607795


























518542

155780


Rep 5
uM
491089
























481913

143166



Rep 5
uM
492210


























506820

137622


Rep 6
uM
489906
























488754

169985



Rep 6
uM
501289


























533937

140945


Average
Replicates
uM
489936
342526
198851
213297
223931
148530
454455
232581
390322
134229
278553
244506
228580
239071
198357
166204
168363
217043
168677
138622
130331
118326
189974
166923
497180
494755
485184
152119
356817
363472

Average
Replicates
uM
518291
153833
100592
132416
124331
148618
152637
201046
121558
158915
159086
177960
143837
118606
158185
115367
177636
181596
106174
257557
127080
100292
103329
170523
187793
187875
510673
520633
511478
146270
379234
393920
Blank
Correction
uM































Blank
Correction
uM
































Corrected
Peak
uM































Corrected
Peak
uM
































Slope

4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06
4.08217E-06

Slope

3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
3.85884E-06
Sample
Results
ppm
2.00
1.40
0.81
0.87
0.91
0.61
1.86
0.95
1.59
0.55
1.14
1.00
0.93
0.98
0.81
0.68
0.69
0.89
0.69
0.57
0.53
0.48
0.78
0.69
2.03
2.02
1.98
0.62
1.46
1.48

Sample
Results
ppm
2.00
0.59
0.39
0.51
0.48
0.57
0.59
0.78
0.47
0.61
0.61
0.69
0.56
0.46
0.61
0.45
0.69
0.70
0.41
0.99
0.49
0.39
0.40
0.66
0.77
0.72
1.97
2.01
1.97
0.56
1.46
1.52
Detection
Limit
/3 times (ppm)
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09

Detection
Limit
/3 times (ppm)
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
SPK
CONC
(ppm)
























2
2
2
0
1
1

SPK
CONC
(ppm)


























2
2
2
0
1
1
R%

























101.5
101.0
99.0

83.6
86.3

R%



























98.5
100.5
98.7

89.9
95.6
RPD
























-2.9





-0.800

RPD

























-13






-1.528

Notes























Averaged Result








Notes
























Averaged Result







-------

Sample ID
Calibration Std
M5-696-SWF
M5-697-SWF
M5-698-SWF
M5-699-SWF
M5-700-SWF
M5 -701 -SWF
M5-702-SWF
M5 -703 -SWF
M5-704-SWF
M5 -705 -SWF
M5-706-SWF
M5-707-SWF
M5-708-SWF
M5-709-SWF
M5-710-SWF
M5 -711 -SWF
M5-712-SWF
M5-714-SWF
M5 -71 5 -SWF
M5-716-SWF
M5-718-SWF
M5-719-SWF
M5-720-SWF
M5-722-SWF
M5 -723 -SWF
QC CHECK
FINAL QC CHECK
CALIBRATION (CCV)
UMS
MS
MSB


Sample ID
Calibration Std
M5-724-SWF
M5 -725 -SWF
M5-726-SWF
M5-727-SWF
M5-728-SWF
M5-729-SWF
M5-730-SWF
M5 -731 -SWF
M5-732-SWF
M5 -73 3 -SWF
M5-734-SWF
M5 -73 5 -SWF
M5-738-SWF
M5-740-SWF
M5 -741 -SWF
M5-742-SWF
M5 -743 -SWF
M5-744-SWF
M5 -745 -SWF
M5-746-SWF
M5-747-SWF
M5-823-SWF
M5-828-SWF
M5-838-SWF
M5-848-SWF
QC CHECK
FINAL QC CHECK
CALIBRATION (CCV)
UMS
MS
MSB
Collectio
Date

09/25/99
09/26/99
09/25/99
09/25/99
09/25/99
09/26/99
09/25/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/23/99
09/24/99
09/24/99
09/24/99
09/23/99
09/23/99
09/23/99
09/23/99







Collect™
Date

09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/22/99
09/23/99
09/23/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/30/99
09/29/99
09/29/99
09/28/99






1
Time

1510
1637
1030
1635
1750
1740
918
1655
1615
1725
1555
1500
900
1330
1430
1115
905
1715
1145
1310
1030
1715
0
1600
1500







1
Time

1442
1323
1230
1216
1350
1027
1120
1725
917
910
1540
1700
1410
1245
1534
1418
1130
1224
1120
948
942










Digestion
Date
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99

Digestion
Date
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
10/08/99
Analysis
Date
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99

Analysis
Date
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
/23/99
Holding
Time

28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28







Holding
Time

28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28










Time since
Digestion

































Time since
Digestion
































Batch
ID
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99

Batch
ID
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99
ANTEK 11/23/99

Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1


Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1

Rep 1
uM
508879
162320
73439
84802
25672
39785
53418
04815
98265
58737
45238
59852
37108
85514
22877
99087
13147
83774
46542
90333
171736
148783
155773
157942
162255
122325
494705
538788
531113
192383
399174
470479

Rep 1
uM
499878
177693
132768
101698
91707
112597
99739
126876
129140
127159
91575
109118
84652
55020
41659
51466
84603
54352
74632
79714
84326
97048
479929
142608
165416
206276
499770
521009
500661
185143
454798

Rep 2
uM
495740
219467
219848
153753
353233
227784
295054
266464
209979
200058
174366
160606
195536
227273
92577
229275
188271
192142
149006
128849
173478
156455
194613
157993
115898
139835
500641
515388
538721
NO BATA
NO BATA
473802

Rep 2
uM
496837
204268
106827
97999
103829
125752
103736
129193
136469
88978
88923
104863
72088
53674
77333
58015
80795
57829
79046
81919
79863
108171
254735
128039
173157
221671
501408
517753
497732
190928
476171

Rep 3
uM
492412
178111
290654
167225
312623
260241
203785
235091
200283
163973
172897
146831
218820
142298
87658
232242
133577
152521
154812
147125
144394
145131
211607
263983
131858
99471
501261
46990
33640
66266
22194
37260

Rep 3
uM
495823
210066
117482
102123
141283
100674
103797
126703
108501
95881
82010
113483
82188
58051
37119
57144
74001
62004
85463
75869
76716
101574
221256
141499
173612
205263
508584
511477
499122
191269
460173
419473
Rep 4
uM
499249


























517572

162009



Rep 4
uM
500894


























510048

190971


Rep 5
uM
500166


























522517

178392



Rep 5
uM
513553


























506203

186138


Rep 6
uM
512567


























516741

NO BATA



Rep 6
uM
509586


























502547

182724


Average
Replicates
uM
501502
186633
227980
201927
330509
242603
317419
402123
202842
174256
164167
155763
183821
185028
101037
220201
144998
176146
150120
122102
163203
150123
187331
193306
136670
120544
498869
526333
534491
174763
410684
460514

Average
Replicates
uM
502762
197342
119026
100607
112273
113008
102424
127591
124703
104006
87503
109155
79643
55582
52037
55542
79800
58062
79714
79167
80302
102264
318640
137382
170728
211070
503254
511506
499172
187862
463714
443558
Blank
Correction
uM

































Blank
Correction
uM
































Corrected
Peak
uM

































Corrected
Peak
uM
































Slope

3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06
3.98802E-06

Slope

3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
3.97803E-06
Sample
Results
ppm
2.00
0.74
0.91
0.81
1.32
0.97
1.27
1.60
0.81
0.69
0.65
0.62
0.73
0.74
0.40
0.88
0.58
0.70
0.60
0.49
0.65
0.60
0.75
0.77
0.55
0.48
1.99
2.10
2.13
0.70
1.64
1.84

Sample
Results
ppm
2.00
0.79
0.47
0.40
0.45
0.45
0.41
0.51
0.50
0.41
0.35
0.43
0.32
0.22
0.21
0.22
0.32
0.23
0.32
0.31
0.32
0.41
1.21
0.55
0.68
0.84
2.00
2.03
1.99
0.75
1.84
1.76
Detection
Limit
/3 times (ppm)
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09

Detection
Limit
/3 times (ppm)
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
0.03/0.09
SPK
CONC
(ppm)


























2
2
2
0
1
1

SPK
CONC
(ppm)


























2
2
2
0
1
1
R%



























99.5
105.0
106.6

94.1
114.0

R%



























100.1
101.7
99.3

109.7
101.7
RPD
























1.3







-4.776

RPD























9.9








1.896

Notes























Averaged Result










Notes






















Averaged Result









-------
10 % Recalculated Results for Total Organic Carbon in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-5-00
Checked by   njs 4-13-00
Sample
M5-622-SWF
M5-633-SWF
M5-643-SWF
M5-653-SWF
M5-663-SWF
M5-673-SWF
Sample
Method Blank
Method Blank
Method Blank
Method Blank
Method Blank
Method Blank
CCV10
CCV5
CCV10
CCV5
CCV10
UMS
UMS
MS
MS
627
627D
638
638D
648
948D
658
658D
668
668D
QC
Batch
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
QC
Batch
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
Qualifier
Note






Qualifier
Note

























Dilution
1
1
1
1
1
1
Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Instrument
Result
ppm
36.77
21.02
24.94
34.31
19.94
18.90
Instrument
Result
ppm
2.331
2.273
2.933
2.565
2.668
2.698
13.04
8.51
13.80
8.405
13.63
10.73
10.91
19.72
19.41
40.63
41.15
22.5
22.55
26.89
26.84
26.24
26.51
17.19
17.11
Blank Factor
ppm
0
0
0
0
0
0
Blank Factor
ppm
2.578
2.578
2.578
2.578
2.578
2.578
2.578
2.578
2.578
2.578
2.578
2.578
2.578
2.578
2.578
0
0
0
0
0
0
0
0
0
0
Sample
Results
ppm
36.77
21.02
24.94
34.31
19.94
18.90
Sample
Results
ppm
-0.25
-0.31
0.36
-0.01
0.09
0.12
10.46
5.93
11.22
5.83
11.05
8.15
8.33
17.14
16.83
40.63
41.15
22.50
22.55
26.89
26.84
26.24
26.51
17.19
17.11
Detection
Limit
ppm
0.12
0.12
0.12
0.12
0.12
0.12
Detection
Limit'3
ppm
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36

Spike
Cone
(ppm)
0
0
0
0
0
0
10
5
10
5
10


8
8
0
0
0
0
0
0
0
0
0
0
R%






104.62
118.64
112.22
116.54
110.52


112.38
106.25










RPD












-2.184

1.825

-1.272

-0.222

0.186

-1.024

0.466
-------
10 % Recalculated Results for Total Organic Carbon in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-5-00
Checked by   njs 4-13-00
Sample
M5-683-SWF
M5-693-SWF
M5-703-SWF
M5-714-SWF
M5-726-SWF
Sample
Method Blank
Method Blank
Method Blank
Method Blank
Method Blank
Method Blank
CCV10
CCV5
CCV10
CCV5
CCV10
UMS
UMS
MS
MS
686
686D
696
696D
706
706D
718
718D
729
729D
QC
Batch
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
QC
Batch
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
Qualifier
Note





Qualifier
Note

























Dilution
1
1
1
1
1
Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Instrument
Result
ppm
11.55
10.22
14.16
13.99
11.50
Instrument
Result
ppm
1.139
1.158
1.307
1.161
1.302
1.371
11.13
6.364
11.22
6.343
11.18
8.789
9.143
16.7
17
18.58
18.78
17.09
17.01
10.64
10.25
12.1
11.32
9.356
9.092
Blank Factor
ppm
0
0
0
0
0
Blank Factor
ppm
1.24
1.24
1.24
1.24
1.24
1.24
1.24
1.24
1.24
1.24
1.24
1.24
1.24
1.24
1.24
0
0
0
0
0
0
0
0
0
0
Sample
Results
ppm
11.55
10.22
14.16
13.99
11.50
Sample
Results
ppm
-0.10
-0.08
0.07
-0.08
0.06
0.13
9.89
5.12
9.98
5.10
9.94
7.55
7.90
15.46
15.76
18.58
18.78
17.09
17.01
10.64
10.25
12.1
11.32
9.356
9.092
Detection
Limit
ppm
0.12
0.12
0.12
0.12
0.12
Detection
Limit'3
ppm
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36

Spike
Cone
(ppm)
0
0
0
0
0
0
10
5
10
5
10


8
8
0
0
0
0
0
0
0
0
0
0
R%






98.90
102.48
99.80
102.06
99.40


98.89
98.21










RPD












-4.582

-1.922

-1.071

0.469

3.734

6.661

2.862
-------
10 % Recalculated Results for Total Organic Carbon in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-5-00
Checked by   njs 4-13-00
Sample
M5-738-SWF
M5-828-SWF
M5-944-SWF
Sample
Method Blank
Method Blank
Method Blank
Method Blank
Method Blank
Method Blank
CCV10
CCV5
CCV10
CCV5
CCV10
UMS
UMS
MS
MS
740
740D
838
838D
QA-042-PEF
QA-042-PEF-DUP
QA-003-CB1
QA-003-CB1-DUP
QC
Batch
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
QC
Batch
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
Qualifier
Note



Qualifier
Note























Dilution
1
1
1
Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Instrument
Result
ppm
6.326
18.67
7.77
Instrument
Result
ppm
1.163
1.223
1.275
1.082
1.037
0.822
11.70
6.771
11.85
6.519
11.5
8.889
9.033
18
17.9
5.777
6.133
22.06
21.88
0.82
0.838
0.883
0.881
Blank Factor
ppm
0
0
0
Blank Factor
ppm
1.1
1.1
1.1
1.1
1.1
1.1
1.1
1.1
1.1
1.1
1.1
1.1
1.1
1.1
1.1
0
0
0
0
0
0
0
0
Sample
Results
ppm
6.33
18.67
7.77
Sample
Results
ppm
0.06
0.12
0.18
-0.02
-0.06
-0.28
10.60
5.67
10.75
5.42
10.40
7.79
7.93
16.90
16.80
5.78
6.13
22.06
21.88
0.82
0.84
0.883
0.881
Detection
Limit
ppm
0.12
0.12
0.12
Detection
Limit'3
ppm
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36
0.36

Spike
Cone
(ppm)
0
0
0
0
0
0
10
5
10
5
10


8
8
0
0
0
0
0
0
0
0
R%






106.00
113.42
107.50
108.38
104.00


113.89
110.84








RPD












-1.832

0.593

-5.978

0.819

-2.171

0.227
-------
SERC Lab / EPA REMAP results
Total Organic Carbon (TOC) Water Analysis by EPA Method 415.1 (modified)
Analysis not performed
Analysis not required
Average of two
     Data Entered by:
Data Entry Checked by:
                              PMEYER 3-16-00
                                                                                                                                                         njs 3-17-00
Sampling Station
ID
M5-622-SWF
M5-623-SWF
M5-624-SWF
M5-625-SWF
M5-626-SWF
M5-627-SWF
M5-628-SWF
M5-631-SWF
M5-632-SWF
M5-633-SWF
M5-635-SWF
M5-637-SWF
M5-638-SWF
M5-639-SWF
M5-640-SWF
M5-641-SWF
M5-642-SWF
M5-643-SWF
M5-644-SWF
M5-646-SWF
M5-647-SWF
M5-648-SWF
M5-649-SWF
M5-650-SWF
M5-653-SWF
M5-654-SWF
M5-655-SWF
M5-656-SWF
M5-657-SWF
M5-658-SWF
M5-659-SWF
M5-660-SWF
M5-661-SWF
M5-662-SWF
M5-663-SWF
M5-664-SWF
M5-665-SWF
M5-666-SWF
M5-667-SWF
Matrix
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
Collection
Date
09/30/99
09/30/99
09/30/99
09/30/99
09/30/99
09/30/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/28/99
09/29/99
09/28/99
09/29/99
09/29/99
09/30/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/27/99
09/28/99
09/27/99
09/27/99
09/29/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
Time
1125
915
1018
1257
908
1050
1716
1414
1010
1115
1216
1210
1630
1715
1116
1615
1011
910
1145
1515
1102
1300
1620
1158
1300
1145
1028
900
1751
1722
1205
1450
857
1610
1330
1100
1710
1655
1545
Digestion
Date
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
Run
Date
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
Holding
Time (Days)
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
Time Elapsed
From Dig
21
21
21
21
21
21
22
22
22
22
22
22
22
23
22
23
22
22
21
23
23
23
23
23
23
23
23
23
24
23
24
24
22
24
24
24
24
24
24
TOC
Units (ppm)
36.77
22.28
27.22
28.27
22.65
40.89
19.60
17.69
17.99
21.02
17.36
20.24
22.53
25.40
16.23
26.20
39.12
24.94
29.06
33.42
37.49
26.86
27.75
30.02
34.31
27.46
35.39
18.45
33.66
26.38
26.98
29.14
22.07
25.77
19.94
27.47
23.95
20.49
18.52
QA/QC
Batch ID
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
QAData
% R | %RPD | Matrix %R | Sample RPD
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
118
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109
109





-1.27






0.22








0.19







-1.02










Notes





Averaged Result






Averaged Result








Averaged Result







Averaged Result









-------
M5-668-SWF
M5-669-SWF
M5-670-SWF
M5-672-SWF
M5-673-SWF
M5-674-SWF
M5-675-SWF
M5-676-SWF
M5-677-SWF
M5-678-SWF
M5-679-SWF
M5-680-SWF
M5-681-SWF
M5-683-SWF
M5-684-SWF
M5-685-SWF
M5-686-SWF
M5-687-SWF
M5-688-SWF
M5-689-SWF
M5-690-SWF
M5-691-SWF
M5-692-SWF
M5-693-SWF
M5-694-SWF
M5-695-SWF
M5-697-SWF
M5-699-SWF
M5-700-SWF
M5-701-SWF
M5-702-SWF
M5-703-SWF
M5-704-SWF
M5-705-SWF
M5-706-SWF
M5-707-SWF
M5-708-SWF
M5-709-SWF
M5-711-SWF
M5-712-SWF
M5-714-SWF
M5-715-SWF
M5-716-SWF
M5-718-SWF
M5-720-SWF
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/26/99
09/26/99
09/28/99
09/26/99
09/26/99
09/26/99
09/27/99
09/26/99
09/26/99
09/26/99
09/26/99
09/25/99
09/25/99
09/26/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/26/99
09/25/99
09/25/99
09/26/99
09/25/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/23/99
09/24/99
09/24/99
09/24/99
09/23/99
1207
1000
850
1100
1400
1025
1130
925
1310
1213
1335
900
1410
850
1530
1434
915
1035
1527
1205
1350
1554
1200
1139
1702
1400
1637
1635
1750
1740
918
1655
1615
1725
1555
1500
900
1330
1115
905
1715
1145
1310
1030
0
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
24
24
24
24
24
25
25
23
26
26
26
25
26
26
26
26
27
27
26
27
27
27
27
27
27
27
26
27
27
26
27
28
28
28
28
28
28
28
28
28
29
28
28
28
29
17.15
26.09
20.14
15.43
18.9
17.46
22.51
18.05
18.51
13.81
16.7
15.68
18.45
11.55
18.08
12.59
18.68
18.74
11.32
17.71
13.11
11.67
12.17
10.22
12.39
16.21
18.89
16.88
12.27
12.46
16.9
14.16
9.518
10.09
10.45
11
14.46
6.433
10.66
11.34
13.99
8.607
14.86
11.71
15.61
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
118
118
118
118
118
118
118
118
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
102
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
109
109
109
109
109
109
109
109
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
99
0.47















-1.07

















3.73








6.66

Averaged Result















Averaged Result

















Averaged Result








Averaged Result

-------
M5-722-SWF
M5-723-SWF
M5-724-SWF
M5-725-SWF
M5-726-SWF
M5-727-SWF
M5-728-SWF
M5-729-SWF
M5-730-SWF
M5-731-SWF
M5-732-SWF
M5-733-SWF
M5-734-SWF
M5-735-SWF
M5-738-SWF
M5-740-SWF
M5-741-SWF
M5-742-SWF
M5-743-SWF
M5-745-SWF
M5-746-SWF
M5-747-SWF
M5-823-SWF
M5-828-SWF
M5-838-SWF
M5-848-SWF
M5-859-SWF
M5-868-SWF
M5-878-SWF
M5-890-SWF
M5-908-SWF
M5-920-SWF
M5-932-SWF
M5-944-SWF
QA-001-CB1
QA-001-CB2
QA-002-CB1
QA-002-CB2
QA-003-CB1
QA-003-CB2
QA-004-CB1
QA-004-CB2
QA-005-CB1
QA-005-CB2
QA-006-CB1
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
WATER
WATER
WATER
WATER
WATER
WATER
WATER
WATER
WATER
WATER
WATER
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/22/99
09/23/99
09/23/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/30/99
09/29/99
09/29/99
09/28/99
09/27/99
09/27/99
09/26/99
09/25/99
09/24/99
09/23/99
09/23/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
1600
1500
1442
1323
1230
1216
1350
1027
1120
1725
917
910
1540
1700
1410
1245
1534
1418
1130
1120
948
942











1224











10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/23/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/23/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
29
29
29
29
29
29
29
29
29
30
29
29
30
30
30
30
30
30
30
30
30
30
22
23
23
24
25
25
26
27
28
29
29
30
30
30
30
31
30
30
30
30
30
30
30
10.69
8.841
14.08
10.02
11.5
9.453
11
9.22
11.77
11.64
8.877
8.521
10.67
9.589
6.326
5.96
8.7
8.733
5.541
9.547
8.579
11.02
20.76
18.67
21.97
26.26
25.24
15.95
14.76
13.02
15.23
15.89
8.945
7.77
0.75
0.765
0.713
0.92
0.882
0.753
0.814
0.758
0.91
0.787
0.755
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-23-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
102
102
102
102
102
102
102
102
102
102
102
102
111
111
111
111
111
111
111
111
111
111
111
111
111
111
111
111
111
111
111
111
111
111
111
111
111
108
111
111
111
111
111
111
111
2
2
2
2
2
2
2
2
2
2
2
2
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
99
99
99
99
99
99
99
99
99
99
99
99
112
112
112
112
112
112
112
112
112
112
112
112
112
112
112
112
112
112
112
112
112
112
112
112
112
101
112
112
112
112
112
112
112







2.86







-5.97








0.82












24.60
0.23













Averaged Result







Averaged Result








Averaged Result












Averaged Result
Averaged Result






-------
QA-006-CB2
QA-007-CB1
QA-007-CB2
QA-008-CB1
QA-008-CB2
QA-009-CB1
QA-009-CB2
QA-027-PEF
QA-031-PEF
QA-032-PEF
QA-042-PEF
QA-043-PEF
QA-044-PEF
QA-630-SWF
QA-634-SWF
QA-636-SWF
QA-645-SWF
QA-651-SWF
QA-652-SWF
QA-671-SWF
QA-682-SWF
QA-696-SWF
QA-698-SWF
QA-710-SWF
QA-719-SWF
QA-744-SWF
WATER
WATER
WATER
WATER
WATER
WATER
WATER
PE
WATER
PE
WATER
PE
PE
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99


























10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/21/99
10/22/99
10/21/99
10/22/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/21/99
10/22/99
10/21/99
10/22/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/21/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
10/22/99
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
30
30
30
30
30
30
30
29
30
29
30
29
29
29
29
29
29
29
29
29
30
30
30
30
30
30
0.786
0.742
0.739
0.764
0.815
0.941
0.75
46.52
0.797
12.6
0.83
6.78
2.204
21.20
29.86
38.62
42.34
30.65
21.46
19.43
14.36
17.05
10.91
14.72
13.83
7.704
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-22-99/TOC-A
10-21-99/TOC-B
10-22-99/TOC-A
10-21-99/TOC-B
10-22-99/TOC-A
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-21-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-B
10-22-99/TOC-A
111
111
111
111
111
111
111
118
111
118
111
118
118
118
118
118
118
118
118
118
102
102
102
102
102
111
1
1
1
1
1
1
1
2
1
2
1
2
2
2
2
2
2
2
2
2
2
2
2
2
2
1
112
112
112
112
112
112
112
109
112
109
112
109
109
109
109
109
109
109
109
109
99
99
99
99
99
112










-2.17










0.41














Averaged Result










Averaged Result




R:\wp_iiles\2110-247\report\pdi\Final DraftWppendix C\September 1999 DR\[toc.xls]TOC results
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-6-00
Checked by  njs 4-13-00

Sample
M5-622-SWF-1


M5-622-SWF-2


M5-622-SWF-3


M5-622-SWF-1-S


Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
QC
Batch
HG19JF1
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
Qualifier
Note





















Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Instrument
Reading
Peak Height
Rep 1,2,3
106.3
109.9
111.7
114.6
112.7
112.3
108.4
107.9
107.9
130.4
133.0
129.8
0.65
78.3
77.9
81.5
80.4
72.2
76.9
81.1
77.9
Method
Reagant Blank
Peak Hieght
0
0
0
0
0
0
0
0
0
0
0
0

0
0
0
0
0
0
0
0
Corrected
Reading
Peak Height
Rep 1,2,3
106.30
109.90
111.70
114.60
112.70
112.30
108.40
107.90
107.90
130.40
133.00
129.80
0.65
78.30
77.90
81.50
80.40
72.20
76.90
81.10
77.90

Y ratio
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
15.2
Hg
Concentration
ppt
7.19
7.44
7.56
7.76
7.63
7.60
7.34
7.30
7.30
8.83
9.00
8.79
0.04
5.30
5.27
5.52
5.44
4.89
5.20
5.49
5.27
Averaged
Result
ppt








7.46


8.87








5.30
DETECTION
LIMIT/* 3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONG
(ppt)









2
2
2

5
5
5
5
5
5
5
5
R%











70.65

105.99
105.45
110.33
108.84
97.74
104.10
109.78
105.45
Standard
Deviation








0.19


0.12








0.20
Relative
Standard
Deviation








2.5


1.3








3.8
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-6-00 Checked by
Sample
M5-633-SWF-1


M5-633-SWF-2


M5-633-SWF-3


M5-633-SWF-1-S


Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8

M5-944-SWF-1


M5-944-SWF-2


M5-944-SWF-3


Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-1 0
CCV-1 1
CCV-1 2
QC
Batch
HG13IF1
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11

HG13IF1
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
Qualifier
Note












































Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1

1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
njs 4-1 3-00
Instrument
Reading
Peak Height
Rep 1,2,3
52.4
51.0
49.7
48.7
51.4
48.0
43.7
46.8
41.2
59.3
61.3
60.9
1.55
90.8
90.8
87.4
88.0
81.9
86.4
81.7
85.0

32.6
27.7
19.7
25.1
29.3
26.1
29.1
30.7
30.3
2.95
85.0
86.1
76.8
76.3
82.1
84.4
79.4
80.9
77.7
76.6
84.8
87.0
Method
Reagant Blank
Peak Hieght
4.01
4.01
4.01
4.01
4.01
4.01
4.01
4.01
4.01
4.01
4.01
4.01

4.01
4.01
4.01
4.01
4.01
4.01
4.01
4.01

4.01
4.01
4.01
4.01
4.01
4.01
4.01
4.01
4.01

4.01
4.01
4.01
4.01
4.01
4.01
4.01
4.01
4.01
4.01
4.01
4.01
Corrected
Reading
Peak Height
Rep 1,2,3
48.39
46.99
45.69
44.69
47.39
43.99
39.69
42.79
37.19
55.29
57.29
56.89
1.55
86.79
86.79
83.39
83.99
77.89
82.39
77.69
80.99

28.59
23.69
15.69
21.09
25.29
22.09
25.09
26.69
26.29
2.95
80.99
82.09
72.79
72.29
78.09
80.39
75.39
76.89
73.69
72.59
80.79
82.99

Y ratio
17.8
17.8
17.8
17.8
17.8
17.8
17.8
17.8
17.8
17.8
17.8
17.8
17.8
17.8
17.8
17.8
17.8
17.8
17.8
17.8
17.8

15.1
15.1
15.1
15.1
15.1
15.1
15.1
15.1
15.1
15.1
15.1
15.1
15.1
15.1
15.1
15.1
15.1
15.1
15.1
15.1
15.1
15.1
Hg
Concentration
ppt
2.80
2 72
2.64
2.58
2.74
2.54
2.29
2.47
2.15
3.20
3.31
3.29
0.09
5.02
5.02
4.82
4.85
4.50
4.76
4.49
4.68

1.95
1.61

1.44
1.72
1.51
1.71
1.82
1.79
0.20
5.52
5.59
4.96
4.93
5.32
5.48
5.14
5.24
5.02
4.95
5.50
5.65
Averaged
Result
ppt








2.55


3.26


















1.69












5.27
DETECTION
LIMIT/* 3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9

0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONG
(ppm)









1
1
1

5
5
5
5
5
5
5
5











5
5
5
5
5
5
5
5
5
5
5
5
R%











71.67

100.33
100.33
96.40
97.09
90.04
95.24
89.81
93.62











110.36
111.86
99.19
98.51
106.41
109.54
102.73
104.77
100.41
98.91
110.09
113.09
Standard
Deviation








0.21


0.06


















0.17












0.27
Relative
Standard
Deviation








8.4


1.9


















9.9












5.2
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-6-00 Checked by
Sample
M5-643-SWF-1


M5-643-SWF-2


M5-643-SWF-3


M5-677-SWF-1


M5-677-SWF-2


M5-677-SWF-3


QA-677-SWF-1-S


Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-1 0
CCV-1 1
CCV-1 2
QC
Batch
HG07JF1
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
»
11
11
11
11
»
11
11
Qualifier
Note


































Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
njs 4-1 3-00
Instrument
Reading
Peak Height
Rep 1,2,3
18.4
16.4
13.6
14.1
15.7
16.8
19.3
18.4
15.9
15.5
20.2
14.3
11.7
16.9
14.9
15.8
19.5
17.0
42.6
40.8
45.2
4.85
60.3
61.2
61.9
61.3
62.5
60.6
60.9
57.7
55.8
60.0
65.2
60.6
Method
Reagant Blank
Peak Hieght
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78

2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
2.78
Corrected
Reading
Peak Height
Rep 1,2,3
15.62
13.62
10.82
11.32
12.92
14.02
16.52
15.62
13.12
12.72
17.42
11.52
8.92
14.12
12.12
13.02
16.72
14.22
39.82
38.02
42.42
4.85
57.52
58.42
59.12
58.52
59.72
57.82
58.12
54.92
53.02
57.22
62.42
57.82

Y ratio
12.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
14.6
14.6
14.6
14.6
14.6
14.6
14.6
14.6
14.6
14.6
14.6
14.6
12.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
Hg
Concentration
ppt
1.34
1.17
0.93
0.97
1.11
1.20
1.42
1.34
1.12
0.90
1.23
0.81
0.63
0.99
0.85
0.92
1.18
1.00
2.81
2.68
2.99
0.42
4.93
5.01
5.07
5.02
5.12
4.96
4.98
4.71
4.55
4.91
5.35
4.96
Averaged
Result
ppt








1.18








0.95


2.82












4.96
DETECTION
LIMIT/* 3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONG
(ppm)


















2
2
2

5
5
5
5
5
5
5
5
5
5
5
5
R%




















93.95

98.63
100.17
101.37
100.34
102.40
99.14
99.66
94.17
90.91
98.11
107.03
99.14
Standard
Deviation








0.17








0.18


0.16












0.20
Relative
Standard
Deviation








14.2








19.4


5.5












4.0
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-6-00 Checked by
Sample
M5-653-SWF-1


M5-653-SWF-2


M5-653-SWF-3


M5-632-SWF-1


M5-632-SWF-2


M5-632-SWF-3


QA-632-SWF-1-S


Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-1 0
CCV-1 1
CCV-1 2
CCV-1 3
CCV-1 4
CCV-1 5
CCV-1 6
CCV-1 7
CCV-1 8
CCV-1 9
CCV-20
CCV-21
CCV-22
QC
Batch
HG15JF1
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
Qualifier
Note


















"M"
"M"
"M"























Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
njs 4-1 3-00
Instrument
Reading
Peak Height
Rep 1,2,3
9.5
11.9
10.6
10.2
11.4
14.1
9.6
9.5
11.9
15.2
13.7
14.5
10.2
15.4
6.5
11.7
12.2
12.7
53.7
54.4
55.6
0.55
81.1
83.6
80.5
81.3
84.6
81.8
87.1
85.8
87.6
84.1
81.4
84.8
81.7
80.7
84.1
74.4
80.5
80.4
83.3
78.5
77.5
79.3
Method
Reagant Blank
Peak Hieght
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08

0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
0.08
Corrected
Reading
Peak Height
Rep 1,2,3
9.42
11.82
10.52
10.12
11.32
14.02
9.52
9.42
11.82
15.12
13.62
14.42
10.12
15.32
6.42
11.62
12.12
12.62
53.62
54.32
55.52
0.55
81.02
83.52
80.42
81.22
84.52
81.72
87.02
85.72
87.52
84.02
81.32
84.72
81.62
80.62
84.02
74.32
80.42
80.32
83.22
78.42
77.42
79.22

Y ratio
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
16.1
Hg
Concentration
ppt
0.60
0.76
0.67
0.65
0.72

0.61
0.60
0.76
0.97
0.87
0.92
0.65
0.98

0.74
0.77
0.81
3.43
3.47
3.55
0.04
5.18
5.34
5.14
5.19
5.40
5.22
5.56
5.48
5.59
5.37
5.20
5.41
5.22
5.15
5.37
4.75
5.14
5.13
5.32
5.01
4.95
5.06
Averaged
Result
ppt








0.67








0.84


3.48






















5.24
DETECTION
LIMIT/* 3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONG
(ppm)


















2
2
2

5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
R%




















132.17

103.54
106.74
102.78
103.80
108.02
104.44
111.21
109.55
111.85
107.38
103.93
108.27
104.31
103.03
107.38
94.98
102.78
102.65
106.36
100.22
98.94
101.24
Standard
Deviation








0.07








0.12


0.06






















0.20
Relative
Standard
Deviation








9.9








13.9


1.8






















3.8
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-6-00 Checked by
Sample
M5-663-SWF-1


M5-663-SWF-2


M5-663-SWF-3


M5-663-SWF-1-S


Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-1 0
CCV-1 1
CCV-1 2
QC
Batch
HG30F1
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
Qualifier
Note

























Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
njs 4-1 3-00
Instrument
Reading
Peak Height
Rep 1,2,3
29.30
30.40
29.40
30.30
30.10
28.00
33.70
30.40
29.50
50.60
58.30
55.30
2.53
80.30
84.00
95.20
86.00
70.60
71.60
74.90
70.60
72.10
68.30
76.00
70.30
Method
Reagant Blank
Peak Hieght
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29

5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
Corrected
Reading
Peak Height
Rep 1,2,3
24.01
25.11
24.11
25.01
24.81
22.71
28.41
25.11
24.21
45.31
53.01
50.01
2.53
75.01
78.71
89.91
80.71
65.31
66.31
69.61
65.31
66.81
63.01
70.71
65.01

Y ratio
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
16.6
Hg
Concentration
ppt
1.49
1.56
1.49
1.55
1.54
1.41

1.56
1.50
2.81
3.29
3.10
0.16
4.65
4.88
5.57
5.00
4.05
4.11
4.31
4.05
4.14
3.91
4.38
4.03
Averaged
Result
ppt








1.51


3.06












4.36
DETECTION
LIMIT/* 3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONG
(ppm)









2
2
2

5
5
5
5
5
5
5
5
5
5
5
5
R%











77.65

92.98
97.56
111.45
100.04
80.95
82.19
86.28
80.95
82.81
0.00
87.65
87.10
Standard
Deviation








0.05


0.24












0.53
Relative
Standard
Deviation








3.4


7.85












12.1
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-6-00
Checked by
                                             njs 4-13-00

Sample
M5-673-SWF-1


M5-673-SWF-2


M5-673-SWF-3


M5-683-SWF-1


M5-683-SWF-2


M5-683-SWF-3


M5-678-SWF-1


M5-678-SWF-2


M5-678-SWF-3


QA-678-SWF-1-S


Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-1 0
CCV-1 1
CCV-1 2
CCV-1 3
CCV-1 4
CCV-1 5
CCV-1 6
CCV-1 7
CCV-1 8
CCV-1 9
CCV-20
QC
Batch
HG29IF1
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
Qualifier
Note
























































Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Instrument
Reading
Peak Height
Rep 1,2,3
26.5
28.6
28.5
26.1
30.6
30.8
23.6
31.6
27.4
21.60
15.80
19.00
22.80
21.00
24.40
23.60
16.90
22.80
21.4
20.9
18.7
20.7
20.0
19.9
20.4
26.1
21.7
50.7
45.4
46.0
1.36
81.9
80.1
75.8
74.2
3.75
81.9
80.1
63.1
68
62.6
61.2
66.4
64.3
71.7
69.1
71.7
71.9
70.8
70.6
70.5
73.5
66.4
65.8
72
70.4
Method
Reagant Blank
Peak Hieght
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25

8.25
8.25
8.25
8.25

8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
8.25
Corrected
Reading
Peak Height
Rep 1,2,3
18.25
20.35
20.25
17.85
22.35
22.55
15.35
23.35
19.15
13.35
7.55
10.75
14.55
12.75
16.15
15.35
8.65
14.55
13.15
12.65
10.45
12.45
11.75
11.65
12.15
17.85
13.45
42.45
37.15
37.75
1.36
73.65
71.85
67.55
65.95
3.75
73.65
71.85
54.85
59.75
54.35
52.95
58.15
56.05
63.45
60.85
63.45
63.65
62.55
62.35
62.25
65.25
58.15
57.55
63.75
62.15

Y ratio
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
17.1
17.1
17.1
17.1
17.1
17.1
17.1
17.1
17.1
17.1
17.1
17.1
17.1
17.1
17.1
17.1
17.1
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
12.8
Hg
Concentration
ppt
1.47
1.64
1.63
1.43
1.80
1.81
1.23
1.88
1.54
1.07
0.61
0.86
1.17
1.02
1.30
1.23
0.70
1.17
0.79
0.76
0.63
0.75
0.71
0.70
0.73

0.81
2.55
2.24
2.27
0.08
4.43
4.32
4.06
3.97
0.30
5.92
5.77
4.41
4.80
4.37
4.26
4.67
4.51
5.10
4.89
5.10
5.12
5.03
5.01
5.00
5.24
4.67
4.63
5.12
5.00
Averaged
Result
ppt








1.60








1.01








0.73


2.35




4.20




















4.93
DETECTION
LIMIT/* 3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONG
(ppm)



























2
2
2

5
5
5
5

5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
R%





























80.93

88.62
86.46
81.28
79.36

118.39
115.50
88.17
96.05
87.37
85.12
93.48
90.10
102.00
97.82
102.00
102.32
100.55
100.23
100.07
104.89
93.48
92.51
102.48
99.91
Standard
Deviation








0.21








0.24








0.06


0.17




0.22




















0.42
Relative
Standard
Deviation








13.0








23.9








7.8


7.4




5.2




















8.6
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-6-00 Checked by
Sample
M5-693-SWF-1


M5-693-SWF-2


M5-693-SWF-3


M5-703-SWF-1


M5-703-SWF-2


M5-703-SWF-3


M5-626-SWF-1


M5-626-SWF-2


M5-626-SWF-3


QA-626-SWF-1-S


Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-1 0
CCV-1 1
CCV-1 2
CCV-1 3
CCV-1 4
CCV-1 5
CCV-1 6
CCV-1 7
CCV-1 8
CCV-1 9
CCV-20
CCV-21
QC
Batch
HG18JF1
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
Qualifier
Note




















































Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
njs 4-1 3-00
Instrument
Reading
Peak Height
Rep 1,2,3
22.10
22.8
24.5
22.00
23
23.8
25.00
25.1
27.4
26.10
25.9
25.5
24.10
20.9
22.4
22.60
22.7
22.1
30.2
28.9
32.5
27.4
28.4
27.4
26.8
26.9
26.1
58.7
58.1
53.6
1.75
93.3
94.3
89.7
85.2
90.9
92
88.5
85.1
85.4
87.2
85.5
95.3
94.8
90
92.3
95.3
92.9
91.1
89.3
86.1
83.80
Method
Reagant Blank
Peak Hieght
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08

1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
1.08
Corrected
Reading
Peak Height
Rep 1,2,3
21.02
21.72
23.42
20.92
21.92
22.72
23.92
24.02
26.32
25.02
24.82
24.42
23.02
19.82
21.32
21.52
21.62
21.02
29.12
27.82
31.42
26.32
27.32
26.32
25.72
25.82
25.02
57.62
57.02
52.52
1.75
92.22
93.22
88.62
84.12
89.82
90.92
87.42
84.02
84.32
86.12
84.42
94.22
93.72
88.92
91.22
94.22
91.82
90.02
88.22
85.02
82.72

Y ratio
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
17.3
Hg
Concentration
ppt
1.25
1.29
1.39
1.24
1.30
1.35
1.42
1.43
1.57
1.49
1.48
1.45
1.37
1.18
1.27
1.28
1.29
1.25
1.73
1.65

1.57
1.62
1.57
1.53
1.54
1.49
3.43
3.39
3.12
0.10
5.48
5.54
5.27
5.00
5.34
5.41
5.20
5.00
5.01
5.12
5.02
5.60
5.57
5.29
5.42
5.60
5.46
5.35
5.25
5.06
4.92
Averaged
Result
ppt








1.36








1.34








1.59


3.31





















5.28
DETECTION
LIMIT/* 3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONG
(ppm)



























2
2
2

5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
R%





























86.34

109.68
110.87
105.40
100.05
106.83
108.14
103.97
99.93
100.29
102.43
100.41
112.06
111.47
105.76
108.49
112.06
109.21
107.07
104.93
101.12
98.38
Standard
Deviation








0.10








0.11








0.08


0.17





















0.22
Relative
Standard
Deviation








7.6








8.3








5.0


5.0





















4.2
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-6-00
Checked by
                                             njs 4-13-00

Sample
M5-714-SWF-1


M5-714-SWF-2


M5-714-SWF-3


M5-735-SWF-1


M5-735-SWF-2


M5-735-SWF-3


QA-735-SWF-1-S


Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-1 0
CCV-1 1
CCV-1 2
CCV-1 3
CCV-1 4
CCV-1 5
CCV-1 6
CCV-1 7
CCV-1 8

QC
Batch
HG27IF1
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11

Qualifier
Note









































Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Instrument
Reading
Peak Height
Rep 1,2,3
19.7
15.5
15.1
16.9
16.5
15.0
17.0
18.0
16.9
17.9
2.0
4.3
1.7
2.0
3.9
7.3
7.7
8.0
43.5
45.4
42.6
1.01
50.1
56.0
58.1
58.3
55.4
58.6
55.5
53.1
55.0
54.0
55.2
56.2
54.5
53.8
56.5
55.9
55.5
55.9
Method
Reagant Blank
Peak Hieght
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00

0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
Corrected
Reading
Peak Height
Rep 1,2,3
19.70
15.50
15.10
16.90
16.50
15.00
17.00
18.00
16.90
17.90
2.00
4.30
1.70
2.00
3.90
7.30
7.70
8.00
43.50
45.40
42.60
1.01
50.1
56
58.1
58.3
55.4
58.6
55.5
53.1
55
54
55.2
56.2
54.5
53.8
56.5
55.9
55.5
55.9

Y ratio
12.1
12.1
12.1
12.1
12.1
12.1
12.1
12.1
12.1
13.9
13.9
13.9
13.9
13.9
13.9
13.9
13.9
13.9
13.9
13.9
13.9
12.1
12.1
12.1
12.1
12.1
12.1
12.1
12.1
12.1
12.1
12.1
12.1
12.1
12.1
12.1
12.1
12.1
12.1
12.1

Hg
Concentration
ppt
1.67
1.32
1.28
1.44
1.40
1.28
1.45
1.53
1.44
1.32
1.63
1.80
1.61
1.63
1.77
2.02
2.05
2.07
3.22
3.36
3.15
0.09
4.26
4.76
4.94
4.96
4.71
4.98
4.72
4.51
4.68
4.59
4.69
4.78
4.63
4.57
4.80
4.75
4.72
4.75

Averaged
Result
ppt








1.42








1.77


3.24


















4.71

DETECTION
LIMIT/* 3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9

SPK
CONG
(ppm)


















2
2
2

5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5

R%




















73.89

85.19
95.23
98.80
99.14
94.21
99.65
94.38
90.30
93.53
91.83
93.87
95.57
92.68
91.49
96.08
95.06
94.38
95.06

Standard
Deviation








0.13








0.25


0.11


















0.17

Relative
Standard
Deviation








8.9








14.1


3.3


















3.6
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-6-00

Sample
M5-726-SWF-1


M5-726-SWF-2


M5-726-SWF-3


M5-726-SWF-1-S


Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-1 0
CCV-1 1
CCV-1 2
CCV-1 3
CCV-1 4
CCV-1 5
CCV-1 6
CCV-1 7
CCV-1 8


QC
Batch
HG08JF1
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11


Qualifier
Note































Checked by

Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1

Instrument
Reading
Peak Height
Rep 1,2,3
10.5
11.7
9.8
13.4
8.3
10.3
11.1
5.7
8.3
33.8
35.5
35.3
0.40
62.4
62.9
60.9
59.3
58.7
60.3
55.0
60.5
59.1
60.9
60.5
56.2
61.8
60.6
60.8
58.7
69.9
63.3
njs 4-1 3-00
Method
Reagant Blank
Peak Hieght
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0

2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0
2. 0

Corrected
Reading
Peak Height
Rep 1,2,3
8.30
9.50
7.60
11.20
6.10
8.10
8.90
3.50
6.10
31.60
33.30
33.10
0.40
60.2
60.7
58.7
57.1
56.5
58.1
52.8
58.3
56.9
58.7
58.3
54
59.6
58.4
58.6
56.5
67.7
61.1


Y ratio
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5
12.5


Hg
Concentration
ppt
0.68
0.78
0.63
0.92
0.50
0.67
0.73
0.29
0.50
2.60
2.74
2 72
0.03
4.95
5.00
4.83
4.70
4.65
4.78
4.35
4.80
4.68
4.83
4.80
4.44
4.91
4.81
4.82
4.65
5.57
5.03


Averaged
Result
ppt








0.63


2.69


















4.81


DETECTION
LIMIT/* 3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9


SPK
CONG
(ppm)









2
2
2

5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5


R%











102.74

99.09
99.92
96.62
93.99
93.00
95.64
86.91
95.97
93.66
96.62
95.97
88.89
98.11
96.13
96.46
93.00
111.44
100.58


Standard
Deviation








0.18


0.08


















0.26


Relative
Standard
Deviation








29.1


2.8


















5.3
-------
10 % Recalculated Results for Total Mercury in Surface Water
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-6-00 Checked by
Sample
M5-738-SWF-1


M5-738-SWF-2


M5-738-SWF-3


M5-828-SWF-1


M5-828-SWF-2


M5-828-SWF-3


M5-718-SWF-1


M5-718-SWF-2


M5-718-SWF-3


QA-718-SWF-1-S


Instrument Blank
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-1 0
CCV-1 1
CCV-1 2
QC
Batch
HG05JF1
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
Qualifier
Note











































Dilution
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
njs 4-1 3-00
Instrument
Reading
Peak Height
Rep 1,2,3
33.8
35.3
33.1
36.1
37.3
35.8
38.9
36.0
34.9
28.6
31.0
34.9
33.5
36.7
27.9
30.2
33.5
32.2
10.1
11.9
11.9
7.4
11.0
11.7
11.6
11.0
15.5
32.1
32.9
29.6
0.7
93.3
94.3
89.7
85.2
90.9
92.0
88.5
85.1
85.4
85.4
87.2
83.8
Method
Reagant Blank
Peak Hieght
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32

5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
5.32
Corrected
Reading
Peak Height
Rep 1,2,3
28.48
29.98
27.78
30.78
31.98
30.48
33.58
30.68
29.58
23.28
25.68
29.58
28.18
31.38
22.58
24.88
28.18
26.88
4.78
6.58
6.58
2.08
5.68
6.38
6.28
5.68
10.18
26.78
27.58
24.28
0.70
87.98
88.98
84.38
79.88
85.58
86.68
83.18
79.78
80.08
80.08
81.88
78.48

Y ratio
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
12.3
12.3
12.3
12.3
12.3
12.3
12.3
12.3
12.3
12.3
12.3
12.3
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
10.9
Hg
Concentration
ppt
2.69
2.83
2.62
2.91
3.02
2.88
3.17
2.90
2.79
2.20
2.42
2.79
2.66
2.96
2.13
2.35
2.66
2.54
0.40
0.55
0.55
0.17
0.48
0.53
0.53
0.48
0.85
2.24
2.31
2.03
0.07
8.30
8.40
7.96
7.54
8.08
8.18
7.85
7.53
7.56
7.56
7.73
7.41
Averaged
Result
ppt








2.87








2.52








0.50


2.19












7.84
DETECTION
LIMIT/* 3
ppt
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
0.3/0.9
SPK
CONG
(ppm)



























2
2
2

5
5
5
5
5
5
5
5
5
5
5
5
R%





























84.43

166.08
167.97
159.28
150.79
161.55
163.63
157.02
150.60
151.17
151.17
154.57
148.15
Standard
Deviation








0.16








0.27








0.18


0.14












0.34
Relative
Standard
Deviation








5.7








10.9








34.9


6.6












4.3
-------
SERC Mercury Lab / EPA REMAP results
Total Mercury Analysis
: Analysis not performed
: Analysis not required
: Averaged Results
      Data Entered by:  PMEYER : 3/14/00
Data Entry Checked by:  MWB : 3/15/00
Sampling Station
ID
M5-622SWF
M5-623SWF
M5-624SWF
M5-625SWF
M5-626SWF
M5-627SWF
M5-628SWF

M5-631SWF
M5-632SWF
M5-633SWF

M5-635SWF

M5-637SWF
M5-638SWF
M5-639SWF
M5-640SWF
M5-641SWF
M5-642SWF
M5-643SWF
M5-644SWF

M5-646SWF
M5-647SWF
M5-648SWF
M5-649SWF
M5-650SWF
M5-651SWF

M5-653SWF
M5-654SWF
M5-655SWF
M5-656SWF
M5-657SWF
M5-658SWF
M5-659SWF
M5-660SWF
M5-661SWF
M5-662SWF
M5-663SWF
M5-664SWF
M5-665SWF
M5-666SWF
M5-667SWF
M5-668SWF
M5-669SWF
M5-670SWF

M5-672SWF
M5-673SWF
M5-674SWF
M5-675SWF
M5-676SWF
M5-677SWF
M5-678SWF
M5-679SWF
M5-680SWF
M5-681SWF
Matrix
SW
SW
SW
SW
SW
SW
SW

SW
SW
SW

SW

SW
SW
SW
SW
SW
SW
SW
SW

SW
SW
SW
SW
SW
SW

SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW

SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
Analysis
Method



























































Collection
Date
09/30/99
09/30/99
09/30/99
09/30/99
09/30/99
09/30/99
09/29/99

09/29/99
09/29/99
09/29/99

09/29/99

09/29/99
09/29/99
09/28/99
09/29/99
09/28/99
09/29/99
09/29/99
09/30/99

09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99

09/28/99
09/28/99
09/28/99
09/28/99
09/27/99
09/28/99
09/27/99
09/27/99
09/29/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/26/99
09/27/99
09/27/99
09/27/99

09/27/99
09/27/99
09/26/99
09/26/99
09/28/99
09/26/99
09/26/99
09/26/99
09/27/99
09/26/99
Time
11:25
9:15
10:18
12:57
9:08
10:50
17:16

14:14
10:10
11:15

12:16

12:10
16:30
17:15
11:16
16:15
10:11
9:10
11:45

15:15
11:02
13:00
16:20
11:58
14:10

13:00
11:45
10:28
9:00
17:51
17:22
12:05
14:50
8:57
16:10
13:30
11:00
17:10
16:55
13:10
13:07
10:00
8:50

11:00
14:00
10:25
11:30
9:25
13:10
12:13
13:35
9:00
14:10
Digestion
Date
10/18/99
10/18/99
10/14/99
10/19/99
10/15/99
10/15/99
10/01/99

10/01/99
10/15/99
10/12/99

10/14/99

10/06/99
10/01/99
10/15/99
10/15/99
10/01/99
10/07/99
10/06/99
10/18/99

10/14/99
10/06/99
10/15/99
09/29/99
10/15/99
09/29/99

10/15/99
10/15/99
10/14/99
10/15/99
10/04/99
10/01/99
10/15/99
09/29/99
10/01/99
10/15/99
09/29/99
10/06/99
09/28/99
09/29/99
10/08/99
10/06/99
10/15/99
10/12/99

09/29/99
09/28/99
10/01/99
10/15/99
10/14/99
10/06/99
09/28/99
10/06/99
09/29/99
10/14/99
Run
Date
10/19/99
10/19/99
10/14/99
10/20/99
10/18/99
10/18/99
10/04/99

10/04/99
10/15/99
10/13/99

10/14/99

10/07/99
10/04/99
10/18/99
10/15/99
10/04/99
10/08/99
10/07/99
10/19/99

10/14/99
10/07/99
10/15/99
09/30/99
10/15/99
09/30/99

10/15/99
10/18/99
10/14/99
10/18/99
10/05/99
10/04/99
10/15/99
09/30/99
10/04/99
10/18/99
09/30/99
10/07/99
09/29/99
09/30/99
10/11/99
10/07/99
10/18/99
10/13/99

10/01/99
09/29/99
10/04/99
10/15/99
10/14/99
10/07/99
09/29/99
10/07/99
10/01/99
10/14/99
Holding
Time (Days)
8
8
8
8
8
8
8

8
8
8

8

8
8
8
8
8
8
8
8

8
8
8
8
8
8

8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8

8
8
8
8
8
8
8
8
8
8
Time Elapsed
From Dig
18
18
14
19
15
15
2

2
16
13

15

7
2
17
16
3
8
7
18

16
8
17
1
17
1

17
17
16
17
7
3
18
2
2
18
2
9
1
2
12
9
18
15

2
1
5
19
16
10
2
10
2
18
Total Hg
Units (ppt)
7.45
2.16
2.59
2.66
1.59
0.88
2.80

3.06
0.84
2.55

1.63

1.16
2.26
2.8
2.03
1.04
1.53
1.18
2.84

1.4
1.28
3.89
2.45
1.61
1.14

0.66
1.27
0.98
1.4
1.29
1.99
1.31
0.53
2.52
3.56
1.47
1.58
2.16
0.68
0.64
0.97
1.66
1.64

1.60
1.61
-------
Sampling Station
ID

M5-683SWF
M5-684SWF
M5-685SWF
M5-686SWF
M5-687SWF
M5-688SWF
M5-689SWF
M5-690SWF
M5-691SWF
M5-692SWF
M5-693SWF
M5-694SWF
M5-695SWF

M5-697SWF
M5-698SWF
M5-699SWF
M5-700SWF
M5-701SWF
M5-702SWF
M5-703SWF
M5-704SWF
M5-705SWF
M5-706SWF
M5-707SWF
M5-708SWF
M5-709SWF

M5-711SWF
M5-712SWF
M5-714SWF
M5-715SWF
M5-716SWF
M5-718SWF

M5-720SWF
M5-722SWF
M5-723SWF
M5-724SWF
M5-725SWF
M5-726SWF
M5-727SWF
M5-728SWF
M5-729SWF
M5-730SWF
M5-731SWF
M5-732SWF
M5-733SWF
M5-734SWF
M5-735SWF
M5-738SWF
M5-740SWF
M5-741SWF
M5-742SWF
M5-743SWF

M5-745SWF
M5-746SWF
M5-747SWF
Matrix

SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW

SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW

SW
SW
SW
SW
SW
SW

SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW

SW
SW
SW
Analysis
Method




























































Collection
Date

09/26/99
09/26/99
09/26/99
09/25/99
09/25/99
09/26/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99

09/26/99
09/25/99
09/25/99
09/25/99
09/26/99
09/25/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99

09/24/99
09/24/99
09/23/99
09/24/99
09/24/99
09/24/99

09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/22/99
09/23/99
09/23/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99

09/22/99
09/22/99
09/22/99
Time

8:50
15:30
14:34
9:15
10:35
15:27
12:05
13:50
15:54
12:00
11:39
17:02
14:02

16:37
10:30
16:35
17:50
17:40
9:18
16:55
16:15
17:25
15:55
15:00
9:00
13:30

11:15
9:05
17:15
11:45
13:10
10:30

16:00
16:00
15:00
14:42
13:23
12:30
12:16
13:50
10:27
11:20
17:25
9:17
9:10
15:40

14:10
12:45
15:34
14:18
11:30

11:20
9:48
9:42
Digestion
Date

09/28/99
10/07/99
10/15/99
09/27/99
09/28/99
10/06/99
10/04/99
10/07/99
10/07/99
09/28/99
10/15/99
09/27/99
09/28/99

09/27/99
09/29/99
09/28/99
09/27/99
09/28/99
09/28/99
10/15/99
10/14/99
10/08/99
10/01/99
10/04/99
10/08/99
09/27/99

10/08/99
09/27/99
09/26/99
09/27/99
09/27/99
10/04/99

09/26/99
09/26/99
10/07/99
09/26/99
10/12/99
10/07/99
10/07/99
10/04/99
10/14/99
09/26/99
10/08/99
09/26/99
10/08/99
10/07/99
09/26/99
10/04/99
10/12/99
10/08/99
09/26/99
09/26/99

10/08/99
10/08/99
09/26/99
Run
Date

09/29/99
10/08/99
10/18/99
09/28/99
09/29/99
10/07/99
10/05/99
10/08/99
10/08/99
09/29/99
10/18/99
09/28/99
09/29/99

09/28/99
10/01/99
09/29/99
09/28/99
09/29/99
09/29/99
10/18/99
10/14/99
10/11/99
10/04/99
10/05/99
10/11/99
09/28/99

10/11/99
09/28/99
09/27/99
09/28/99
09/28/99
10/05/99

09/27/99
09/27/99
10/08/99
09/27/99
10/13/99
10/08/99
10/08/99
10/05/99
10/14/99
09/27/99
10/11/99
09/27/99
10/11/99
10/08/99
09/27/99
10/05/99
10/13/99
10/11/99
09/27/99
09/27/99

10/11/99
10/11/99
09/27/99
Holding
Time (Days)

8
8
8
8
8
8
8
8
8
8
8
8
8

8
8
8
8
8
8
8
8
8
8
8
8
8

8
8
8
8
8
8

8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8

8
8
8
Time Elapsed
From Dig

2
11
19
2
3
10
9
12
12
3
20
2
3

1
4
3
2
2
3
21
20
14
7
10
14
3

14
3
3
3
3
10

3
3
14
3
19
14
14
11
21
3
16
3
15
15
4
12
20
16
4
4

16
16
4
Total Hg
Units (ppt)

1.02
1.11
1.03
1.16
1.66
0.76
0.55
1
0.89
0.91
1.36
1.62
1.59

2. .16
0.81
1.75
2.31
0.85
0.85
1.34
1.19
0.65
0.83
1.39
0.65
2.14

1
2.51
1.43
2.99
2.2
0.50

1.45
1.26
0.91
1.51
0.71
0.63
1.06
0.76
1.02
1.2
0.78
1.29
1.49
1.49
1.77
2.87
2.78
2.31
1.64
2.19

1.44
1.88
3.09
QA/QC
Batch ID

HG29IF1
HG08JF1
HG18JF1
HG28IF1
HG29IF1
HG07JF1
HG05JF1
HG08JF1
HG08JF1
HG29IF1
HG18JF1
HG28IF1
HG29IF1

HG28IF1
HG01JF1
HG29IF1
HG28IF1
HG29IF1
HG29IF1
HG18JF1
HG14JF1
BK11JF1
HG04JF1
HG05JF1
BK11JF1
HG28IF1

BK11JF1
HG28IF1
HG27IF1
HG28IF1
HG28IF1
HG05JF1

HG27IF1
HG27IF1
HG08JF1
HG27IF1
HG13JF1
HG08JF1
HG08JF1
HG05JF1
HG14JF1
HG27IF1
BK11JF1
HG27IF1
BK11JF1
HG08JF1
HG27IF1
HG05JF1
HG13JF1
BK11JF1
HG27IF1
HG27IF1

BK11JF1
BK11JF1
HG27IF1
QA Data
%R

129.83
109
104.46
98.01
129.83
0
119
109
109
129.83
104.46
98.01
129.83

98.01
101
129.83
98.01
129.83
129.83
104.46
102.58
96.31
95
119
96.31
98.01

96.31
98.01
96.31
98.01
98.01
105

96.31
96.31
109
96.31
98.65
109
109
119
102.58
96.31
96.31
96.31
96.31
109
96.31
119
98.65
96.31
96.31
96.31

96.31
96.31
96.31
%RSD

23.91
10.59
11.18
18.46
7.01
22.80
26.71
25.30
7.48
15.16
7.58
10.69
9.98

9.24
20.00
11.10
18.46
7.01
10.92
8.34
26.15
29.55
18.03
13.57
31.11
10.57

14.28
13.82
8.91
4.45
18.46
34.92

10.55
12.31
13.86
8.91
8.90
29.12
19.25
6.80
18.31
18.81
17.88
12.40
20.72
14.38
12.05
5.73
4.44
6.60
9.58
8.91

9.14
8.27
9.33
Matrix %R





























































Notes




























































-------
Sampling Station
ID
M5-823SWF
M5-828SWF
M5-838SWF
M5-848SWF
M5-859SWF
M5-868SWF
M5-878SWF
M5-890SWF
M5-908SWF
M5-920SWF
M5-932SWF
M5-944SWF
Matrix
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
Analysis
Method












Collection
Date
09/30/99
09/29/99
09/29/99
09/28/99
09/27/99
09/27/99
09/26/99
09/25/99
09/24/99
09/23/99
09/23/99
09/22/99
Time
9:15
17:16
16:30
13:00
12:05
13:07
12:13
13:50
9:00
16:00
9:17
12:24
Digestion
Date
10/19/99
10/04/99
10/15/99
09/29/99
10/15/99
09/29/99
09/27/99
10/15/99
09/27/99
10/12/99
10/12/99
10/12/99
Run
Date
10/20/99
10/05/99
10/15/99
10/01/99
10/15/99
10/01/99
09/28/99
10/15/99
09/28/99
10/13/99
10/13/99
10/13/99
Holding
Time (Days)
8
8
8
8
8
8
8
8
8
8
8
8
Time Elapsed
From Dig
19
5
16
1
18
2
1
20
3
19
19
20
Total Hg
Units (ppt)
3.06
2.53
1.86
3.81
1.43
0.79
1.96
1
1.72
1.14
0.65
1.69
QA/QC
Batch ID
HG20JF1
HG05JF1
HG15JF1
HG01JF1
HG15JF1
HG01JF1
HG28IF1
HG15JF1
HG28IF1
HG13JF1
HG13JF1
HG13JF1
QA Data
%R
0
119
100.35
101
100.35
101
98.01
100.35
98.01
98.65
98.65
98.65
%RSD
14.27
10.87
7.21
6.47
14.03
16.41
12.49
19.04
9.78
8.08
27.72
9.95
Matrix %R













Notes













QA-630-SWF
QA-634-SWF
QA-636-SWF
QA-645-SWF
QA-652-SWF
QA-671-SWF
QA-682-SWF
QA-696-SWF
QA-710-SWF
QA-719-SWF
QA-744-SWF
QA-001-CB1
QA-001-CB2
QA-002-CB1
QA-002-CB2
QA-003-CB1
QA-003-CB2
QA-004-CB1
QA-004-CB2
QA-005-CB1
QA-005-CB2
QA-006-CB1
QA-006-CB2
QA-007-CB1
QA-007-CB2
QA-008-CB1
QA-008-CB2
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW
SW

















































































10/18/99
10/18/99
10/18/99
10/19/99
10/18/99
10/19/99
10/19/99
10/19/99
10/18/99
10/18/99
10/19/99
10/05/99
10/05/99
10/05/99
10/05/99
10/05/99
10/05/99
10/05/99
10/11/99
10/11/99
10/11/99
10/11/99
10/11/99
10/11/99
10/11/99
10/11/99
10/11/99
10/19/99
10/19/99
10/19/99
10/20/99
10/19/99
10/20/99
10/20/99
10/20/99
10/19/99
10/19/99
10/20/99
10/06/99
10/06/99
10/06/99
10/06/99
10/06/99
10/06/99
10/06/99
10/12/99
10/12/99
10/12/99
10/12/99
10/12/99
10/12/99
10/12/99
10/12/99
10/12/99
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8
8



























2.09
2.08
2.32
3.42
0.8
1.54
1.32
1.5
0.7
1.16
1.58
ND
ND
ND
ND
ND
1.94
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
HG19JF1
HG19JF1
HG19JF1
HG20JF1
HG19JF1
HG20JF1
HG20JF1
HG20JF1
HG19JF1
HG19JF1
HG20JF1
HG06JF1
HG06JF1
HG06JF1
HG06JF1
HG06JF1
HG06JF1
HG06JF1
HG12JF1
HG12JF1
HG12JF1
HG12JF1
HG12JF1
HG12JF1
HG12JF1
HG12JF1
HG12JF1
97.14
97.14
97.14
90.85
97.14
90.85
90.85
90.85
97.14
97.14
90.85
105.74
105.74
105.74
105.74
105.74
105.74
105.74
97.19
97.19
97.19
97.19
97.19
97.19
97.19
97.19
97.19
1.30
1.30
1.30
4.15
1.30
4.15
4.15
4.15
1.30
1.30
4.15
7.05
7.05
7.05
7.05
7.05
7.05
7.05
3.21
3.21
3.21
3.21
3.21
3.21
3.21
3.21
3.21
70.55
70.55
70.55
94.21
70.55
94.21
94.21
94.21
70.55
70.55
94.21
119.09
119.09
119.09
119.09
119.09
119.09
119.09
111.1
111.1
111.1
111.1
111.1
111.1
111.1
111.1
111.1



























-------
September 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID   M5-622-SWF    Surface Water
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                      Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                       Notes
Total P
                  Total N
                                     TOC
                                                      Total Hg
MeHg
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
09/30/99
10/08/99
10/27/99
X
FW=SW
09/30/99
10/08/99
1 1/22/99
X
FW=SW
09/30/99
10/21/99
10/21/99

X
FW=SW
09/30/99
10/18/99
10/19/99

X
FW=SW
09/30/99


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.009
ppm
EPA 365.1
AS
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
1.16
ppm
Antek
CB
0.03 ppm
NA
4ml
sample aliquot
1
36.77
ppm
EPA415.1
SB
0.12 ppm
1000 ml
1000 ml
sample aliquot
1
7.45
ppt
EPA 1631
JL
0.3 ppt
Battelle is
the Main Lab



ppt
EPA 1630

0.02 ppt
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
EPA1027A
NA
**
All <20 RPD
All Good
6of7CCVGood
0.0006 and > ppm
0.9966
ANTEK 11 -22-99
NA
NR
< 20 RPD
All Good
All Good
0.03 and >
NA
10-21-99/TOC-B
NA
All < MDL
All <20 RPD
All Good
All Good
0.12 and >
0.998

HG19JF1
NA

0.9975

File ID







Yes (FTN Associates)
Yes (FTN Associates)
**
Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)11
Yes (FTN Associates)
Yes (FTN Associates)

Yes (FTN Associates)
Yes (FTN Associates)




                            ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                            been corrected to demonstrate samples uncontaminated.
                            The Battelle lab is the primary lab for MeHg in Surface water.
-------
                     Station ID   M4-622-SWF     Surface Water
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
X
X
X
X
Not Noted, Refer to Laboratory and SESD SOP
X
X
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X

X

In Hg lab Area
None







X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X






X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
ppm
X
Yes (FTN Associates)
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) |Fall 98 (68.2%R) Fail| Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Validation Criteria
               Applied Qualifiers |_
"B (NR)"
X= Attached or Verified

Data Qualifiers
" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID   M5-633-SWF    Surface Water
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                      Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                       Notes
Total P
Total N
TOC
Total Hg
MeHg
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
09/29/99
10/08/99
10/27/99
X
FW=SW
09/29/99
10/08/99
1 1/22/99
X
FW=SW
09/29/99
10/21/99
10/21/99

X
FW=SW
09/29/99
10/12/99
10/18/99

X
FW=SW
09/29/99


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5 ml
10ml
sample aliquot
1
0.031
ppm
EPA 365.1
AS
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
1.94
ppm
Antek
CB
0.03 ppm
NA
4ml
sample aliquot
1
21.02
ppm
EPA415.1
SB
0.12 ppm
1000 ml
1000 ml
sample aliquot
1
2.55
ppt
EPA 1631
JL
0.3 ppt
Battelle is
the Main Lab



ppt
EPA 1630

0.02 ppt
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
EPA1027A
NA
**
All <20 RPD
All Good
6of7CCVGood
0.0006 and > ppm
0.9966
ANTEK 11-22-99
NA
NR
< 20 RPD
All Good
All Good
0.03 and >
NA
10-21-99/TOC-B
NA
All < MDL
All <20 RPD
All Good
All Good
0.12 and >
0.998

HG13JF1
NA

0.9994

File ID







Yes (FTN Associates)
Yes (FTN Associates)
**
Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)11
Yes (FTN Associates)
Yes (FTN Associates)

Yes (FTN Associates)
Yes (FTN Associates)




                            ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                            been corrected to demonstrate samples uncontaminated.
                            The Battelle lab is the primary lab for MeHg in Surface water.
-------
                     Station ID   M5-633-SWF     Surface Water
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                    Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
X
X
X
X
Not Noted, Refer to Laboratory and SESD SOP
X
X
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X

X

In Hg lab Area
None







X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X





X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
ppm
X
Yes (FTN Associates)
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) |Fall 98 (68.2%R) Fail) Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Validation Criteria
               Applied Qualifiers^
"B (NR)"
X= Attached or Verified

Data Qualifiers
" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID   M5-643-SWF    Surface Water
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                      Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                       Notes
Total P
Total N
TOC
Total Hg
MeHg
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
09/29/99
10/08/99
10/27/99
X
FW=SW
09/29/99
10/08/99
1 1/22/99
X
FW=SW
09/29/99
10/21/99
10/21/99

X
FW=SW
09/29/99
10/06/99
10/07/99

X
FW=SW
09/29/99


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.033
ppm
EPA 365.1
AS
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
1.28
ppm
Antek
CB
0.03 ppm
NA
4ml
sample aliquot
1
24.94
ppm
EPA415.1
SB
0.12 ppm
1000 ml
1000 ml
sample aliquot
1
1.18
ppt
EPA 1631
JL
0.3 ppt
Battelle is
the Main Lab



ppt
EPA 1630

0.02 ppt
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
EPA1027A
NA
**
All <20 RPD
All Good
6of7CCVGood
0.0006 and > ppm
0.9966
ANTEK 11-22-99
NA
NR
< 20 RPD
All Good
All Good
0.03 and >
NA
10-21-99/TOC-B
NA
All < MDL
All <20 RPD
All Good
All Good
0.12 and >
0.998

HG07JF1
NA

0.9984

File ID







Yes (FTN Associates)
Yes (FTN Associates)
**
Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)

Yes (FTN Associates)
Yes (FTN Associates)




                            ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                            been corrected to demonstrate samples uncontaminated.
                            The Battelle lab is the primary lab for MeHg in Surface water.
-------
                     Station ID   M5-643-SWF    Surface Water
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
X
X
X
X
Not Noted, Refer to Laboratory and SESD SOP
X
X
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X

X

In Hg lab Area
None







X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X





X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
ppm
X
Yes (FTN Associates)
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) |Fall 98 (68.2%R) Fail| Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Validation Criteria
               Applied Qualifiers |_
"B (NR)"
X = Attached or Verified

Data Qualifiers
" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID   M5-653-SWF    Surface Water
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                      Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                       Notes
Total P
Total N
TOC
Total Hg
MeHg
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
09/28/99
10/08/99
10/27/99
X
FW=SW
09/30/99
10/08/99
1 1/22/99
X
FW=SW
09/30/99
10/21/99
10/21/99

X
FW=SW
09/30/99
10/15/99
10/15/99

X
FW=SW
09/30/99


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.074
ppm
EPA 365.1
AS
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
1.86
ppm
Antek
CB
0.03 ppm
NA
4ml
sample aliquot
1
34.31
ppm
EPA415.1
SB
0.12 ppm
1000 ml
1000 ml
sample aliquot
1
0.66
ppt
EPA 1631
JL
0.3 ppt
Battelle is
the Main Lab



ppt
EPA 1630

0.02 ppt
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
EPA1027A
NA
**
All <20 RPD
All Good
6of7CCVGood
0.0006 and > ppm
0.9966
ANTEK 11-22-99
NA
NR
< 20 RPD
All Good
All Good
0.03 and >
NA
10-21-99/TOC-B
NA
All < MDL
All <20 RPD
All Good
All Good
0.12 and >
0.998

HG15JF1
NA

0.9975

File ID







Yes (FTN Associates)
Yes (FTN Associates)
**
Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)

Yes (FTN Associates)
Yes (FTN Associates)
"M"



                            ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                            been corrected to demonstrate samples uncontaminated.
                            The Battelle lab is the primary lab for MeHg in Surface water.
-------
                     Station ID   M5-653-SWF     Surface Water
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
X
X
X
X
Not Noted, Refer to Laboratory and SESD SOP
X
X
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X

X

In Hg lab Area
None







X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X





X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
ppm
X
Yes (FTN Associates)
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) |Fall 98 (68.2%R) Fail| Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Validation Criteria
               Applied Qualifiers |_
"B (NR)"
                                              "M"
X = Attached or Verified

Data Qualifiers
" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID   M5-663-SWF    Surface Water
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                      Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                       Notes
Total P
Total N
TOC
Total Hg
MeHg
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
09/27/99
10/08/99
10/27/99
X
FW=SW
09/27/99
10/08/99
1 1/22/99
X
FW=SW
09/27/99
10/21/99
10/21/99

X
FW=SW
09/27/99
09/29/99
09/30/99

X
FW=SW
09/27/99


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.0078
ppm
EPA 365.1
AS
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
0.69
ppm
Antek
CB
0.03 ppm
NA
4ml
sample aliquot
1
19.94
ppm
EPA415.1
SB
0.12 ppm
1000 ml
1000 ml
sample aliquot
1
1.51
ppt
EPA 1631
JL
0.3 ppt
Battelle is
the Main Lab



ppt
EPA 1630

0.02 ppt
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
EPA1027A
NA
**
All <20 RPD
All Good
6of7CCVGood
0.0006 and > ppm
0.9966
ANTEK 11-20-99
NA
NR
< 20 RPD
All Good
All Good
0.03 and >
NA
10-21-99/TOC-B
NA
All < MDL
All <20 RPD
All Good
All Good
0.12 and >
0.998

HG30F1
NA

0.9986

File ID







Yes (FTN Associates)
Yes (FTN Associates)
**
Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)

Yes (FTN Associates)
Yes (FTN Associates)




                            ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                            been corrected to demonstrate samples uncontaminated.
                            The Battelle lab is the primary lab for MeHg in Surface water.
-------
                     Station ID   M5-663-SWF    Surface Water
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
X
X
X
X
Not Noted, Refer to Laboratory and SESD SOP
X
X
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X

X

In Hg lab Area
None







X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X





X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
ppm
X
Yes (FTN Associates)
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) |Fall 98 (68.2%R) Fail| Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Validation Criteria
               Applied Qualifiers |_
"B (NR)"
X = Attached or Verified

Data Qualifiers
" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID   M5-673-SWF    Surface Water
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                      Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                       Notes
Total P
Total N
TOC
Total Hg
MeHg
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
09/27/99
10/08/99
10/27/99
X
FW=SW
09/27/99
10/08/99
1 1/23/99
X
FW=SW
09/27/99
10/21/99
10/21/99

X
FW=SW
09/27/99
09/28/99
09/29/99

X
FW=SW
09/27/99


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.008
ppm
EPA 365.1
AS
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
0.51
ppm
Antek
CB
0.03 ppm
NA
4ml
sample aliquot
1
18.9
ppm
EPA415.1
SB
0.12 ppm
1000 ml
1000 ml
sample aliquot
1
1.6
ppt
EPA 1631
JL
0.3 ppt
Battelle is
the Main Lab



ppt
EPA 1630

0.02 ppt
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
EPA1027B
NA
NR
<20RPD
All Good
All Good
0.0006 and > ppm
0.9964
ANTEK 11-23-99
NA
NR
< 20 RPD
All Good
All Good
0.03 and >
NA
10-21-99/TOC-B
NA
All < MDL
All <20 RPD
All Good
All Good
0.12 and >
0.998

HG29IF1
NA

0.9992

File ID







Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)

Yes (FTN Associates)
Yes (FTN Associates)




                            ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                            been corrected to demonstrate samples uncontaminated.
                            The Battelle lab is the primary lab for MeHg in Surface water.
-------
                     Station ID   M5-673-SWF     Surface Water
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
X
X
X
X
Not Noted, Refer to Laboratory and SESD SOP
X
X
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X

X

In Hg lab Area
None







X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X





X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
ppm
X
Yes (FTN Associates)
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) |Fall 98 (68.2%R) Fail| Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Validation Criteria
               Applied Qualifiers^    "B (NR)~
"B (NR)"
X = Attached or Verified

Data Qualifiers
" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID   M5-683-SWF    Surface Water
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                      Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                       Notes
Total P
Total N
TOC
Total Hg
MeHg
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
09/26/99
10/08/99
10/27/99
X
FW=SW
09/26/99
10/08/99
1 1/22/99
X
FW=SW
09/26/99
10/22/99
10/22/99

X
FW=SW
09/26/99
09/28/99
09/29/99

X
FW=SW
09/26/99


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.0054
ppm
EPA 365.1
AS
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
1.16
ppm
Antek
CB
0.03 ppm
NA
4ml
sample aliquot
1
11.55
ppm
EPA415.1
SB
0.12 ppm
1000 ml
1000 ml
sample aliquot
1
1.01
ppt
EPA 1631
JL
0.3 ppt
Battelle is
the Main Lab



ppt
EPA 1630

0.02 ppt
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
EPA1027B
NA
NR
<20RPD
All Good
All Good
0.0006 and > ppm
0.9964
ANTEK 11-23-99
NA
NR
< 20 RPD
All Good
All Good
0.03 and >
NA
10-22-99/TOC-B
NA
All < MDL
All <20 RPD
All Good
All Good
0.12 and >
1.0000

HG29IF1
NA

0.9992

File ID







Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)

Yes (FTN Associates)
Yes (FTN Associates)




                            ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                            been corrected to demonstrate samples uncontaminated.
                            The Battelle lab is the primary lab for MeHg in Surface water.
-------
                     Station ID   M5-683-SWF     Surface Water
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
X
X
X
X
Not Noted, Refer to Laboratory and SESD SOP
X
X
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X

X

In Hg lab Area
None







X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X





X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
ppm
X
Yes (FTN Associates)
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) |Fall 98 (68.2%R) Fail| Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Validation Criteria
               Applied Qualifiers^    "B (NR)~
"B (NR)"
X = Attached or Verified

Data Qualifiers
" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID   M5-693-SWF    Surface Water
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                      Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                       Notes
Total P
Total N
TOC
Total Hg
MeHg
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
09/25/99
10/08/99
10/27/99
X
FW=SW
09/25/99
10/08/99
1 1/23/99
X
FW=SW
09/25/99
10/22/99
10/22/99

X
FW=SW
09/25/99
10/15/99
10/18/99

X
FW=SW
09/25/99


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.0056
ppm
EPA 365.1
AS
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
0.66
ppm
Antek
CB
0.03 ppm
NA
4ml
sample aliquot
1
10.22
ppm
EPA415.1
SB
0.12 ppm
1000 ml
1000 ml
sample aliquot
1
1.36
ppt
EPA 1631
JL
0.3 ppt
Battelle is
the Main Lab



ppt
EPA 1630

0.02 ppt
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
EPA1027B
NA
NR
<20RPD
All Good
All Good
0.0006 and > ppm
0.9964
ANTEK 11-23-99
NA
NR
< 20 RPD
All Good
All Good
0.03 and >
NA
10-22-99/TOC-B
NA
All < MDL
All <20 RPD
All Good
All Good
0.12 and >
1.0000

HG18JF1
NA

0.9993

File ID







Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)

Yes (FTN Associates)
Yes (FTN Associates)




                            ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                            been corrected to demonstrate samples uncontaminated.
                            The Battelle lab is the primary lab for MeHg in Surface water.
-------
                     Station ID   M5-693-SWF     Surface Water
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
X
X
X
X
Not Noted, Refer to Laboratory and SESD SOP
X
X
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X

X

In Hg lab Area
None







X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X





X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
ppm
X
Yes (FTN Associates)
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) |Fall 98 (68.2%R) Fail| Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Validation Criteria
               Applied Qualifiers^    "B (NR)~
"B (NR)"
X = Attached or Verified

Data Qualifiers
" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID   M5-703-SWF    Surface Water
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                      Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                       Notes
Total P
Total N
TOC
Total Hg
MeHg
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
09/24/99
10/08/99
10/27/99
X
FW=SW
09/24/99
10/08/99
1 1/23/99
X
FW=SW
09/24/99
10/22/99
10/22/99

X
FW=SW
09/24/99
10/15/99
10/18/99

X
FW=SW
09/24/99


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.0053
ppm
EPA 365.1
AS
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
0.81
ppm
Antek
CB
0.03 ppm
NA
4ml
sample aliquot
1
14.16
ppm
EPA415.1
SB
0.12 ppm
1000 ml
1000 ml
sample aliquot
1
1.34
ppt
EPA 1631
JL
0.3 ppt
Battelle is
the Main Lab



ppt
EPA 1630

0.02 ppt
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
EPA1027B
NA
NR
<20RPD
All Good
All Good
0.0006 and > ppm
0.9964
ANTEK 11-23-99
NA
NR
< 20 RPD
All Good
All Good
0.03 and >
NA
10-22-99/TOC-B
NA
All < MDL
All <20 RPD
All Good
All Good
0.12 and >
1.0000

HG18JF1
NA

0.9993

File ID







Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)

Yes (FTN Associates)
Yes (FTN Associates)




                            ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                            been corrected to demonstrate samples uncontaminated.
                            The Battelle lab is the primary lab for MeHg in Surface water.
-------
                     Station ID   M5-703-SWF     Surface Water
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
X
X
X
X
Not Noted, Refer to Laboratory and SESD SOP
X
X
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X

X

In Hg lab Area
None







X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X





X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
ppm
X
Yes (FTN Associates)
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) |Fall 98 (68.2%R) Fail| Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Validation Criteria
               Applied Qualifiers^    "B (NR)~
"B (NR)"
X = Attached or Verified

Data Qualifiers
" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID   M5-714-SWF    Surface Water
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                      Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                       Notes
Total P
Total N
TOC
Total Hg
MeHg
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
09/23/99
10/08/99
10/27/99
X
FW=SW
09/23/99
10/08/99
1 1/23/99
X
FW=SW
09/23/99
10/22/99
10/22/99

X
FW=SW
09/23/99
09/26/99
09/27/99

X
FW=SW
09/23/99


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.0046
ppm
EPA 365.1
AS
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
0.60
ppm
Antek
CB
0.03 ppm
NA
4ml
sample aliquot
1
13.99
ppm
EPA415.1
SB
0.12 ppm
1000 ml
1000 ml
sample aliquot
1
1.42
ppt
EPA 1631
JL
0.3 ppt
Battelle is
the Main Lab



ppt
EPA 1630

0.02 ppt
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
No
Yes (FTN Associates)
Yes (FTN Associates)
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
EPA1027B
NA
NR
<20RPD
All Good
All Good
0.0006 and > ppm
0.9964
ANTEK 11-23-99
NA
NR
< 20 RPD
All Good
All Good
0.03 and >
NA
10-22-99/TOC-B
NA
All < MDL
All <20 RPD
All Good
All Good
0.12 and >
1.0000

HG27JF1
NA

0.9983

File ID







Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)
"H"
Yes (FTN Associates)
Yes (FTN Associates)




                            ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                            been corrected to demonstrate samples uncontaminated.
                            The Battelle lab is the primary lab for MeHg in Surface water.
-------
                     Station ID   M5-714-SWF     Surface Water
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
X
X
X
X
Not Noted, Refer to Laboratory and SESD SOP
X
X
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X

X

In Hg lab Area
None







X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X





X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
ppm
X
Yes (FTN Associates)
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) |Fall 98 (68.2%R) Fail| Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Validation Criteria
               Applied Qualifiers^    "B (NR)~
"B (NR)"
                        "H"
X = Attached or Verified

Data Qualifiers
" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID   M5-726-SWF    Surface Water
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                      Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                       Notes
Total P
Total N
TOC
Total Hg
MeHg
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
09/23/99
10/08/99
10/27/99
X
FW=SW
09/23/99
10/08/99
1 1/23/99
X
FW=SW
09/23/99
10/22/99
10/22/99

X
FW=SW
09/23/99
10/07/99
10/08/99

X
FW=SW
09/23/99


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.0051
ppm
EPA 365.1
AS
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
0.40
ppm
Antek
CB
0.03 ppm
NA
4ml
sample aliquot
1
11.5
ppm
EPA415.1
SB
0.12 ppm
1000 ml
1000 ml
sample aliquot
1
0.63
ppt
EPA 1631
JL
0.3 ppt
Battelle is
the Main Lab



ppt
EPA 1630

0.02 ppt
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
No
Yes (FTN Associates)
Yes (FTN Associates)
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
EPA1027C
NA
**
All <20 RPD
All Good
All Good
0.0006 and > ppm
0.9957
ANTEK 11-23-99
NA
NR
< 20 RPD
All Good
All Good
0.03 and >
NA
10-22-99/TOC-B
NA
All < MDL
All <20 RPD
All Good
All Good
0.12 and >
1.0000

HG08JF1
NA

0.9996

File ID







Yes (FTN Associates)
Yes (FTN Associates)
**
Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)
"H"
Yes (FTN Associates)
Yes (FTN Associates)




                            ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                            been corrected to demonstrate samples uncontaminated.
                            The Battelle lab is the primary lab for MeHg in Surface water.
-------
                     Station ID   M5-726-SWF    Surface Water
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
X
X
X
X
Not Noted, Refer to Laboratory and SESD SOP
X
X
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X

X

In Hg lab Area
None







X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X





X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
ppm
X
Yes (FTN Associates)
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) |Fall 98 (68.2%R) Fail| Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Validation Criteria
               Applied Qualifiers |_
"B (NR)"
                        "H"
X = Attached or Verified

Data Qualifiers
" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID   M5-738-SWF    Surface Water
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                      Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                       Notes
Total P
Total N
TOC
Total Hg
MeHg
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
09/22/99
10/08/99
10/27/99
X
FW=SW
09/22/99
10/08/99
1 1/23/99
X
FW=SW
09/22/99
10/22/99
10/22/99

X
FW=SW
09/22/99
10/04/99
10/05/99

X
FW=SW
09/22/99


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.005
ppm
EPA 365.1
AS
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
0.22
ppm
Antek
CB
0.03 ppm
NA
4ml
sample aliquot
1
6.33
ppm
EPA415.1
SB
0.12 ppm
1000 ml
1000 ml
sample aliquot
1
2.87
ppt
EPA 1631
JL
0.3 ppt
Battelle is
the Main Lab



ppt
EPA 1630

0.02 ppt
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
No
Yes (FTN Associates)
Yes (FTN Associates)
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
EPA1027C
NA
**
All <20 RPD
All Good
All Good
0.0006 and > ppm
0.9957
ANTEK 11-23-99
NA
NR
< 20 RPD
All Good
All Good
0.03 and >
NA
10-22-99/TOC-B
NA
All < MDL
All <20 RPD
All Good
All Good
0.12 and >
0.999

HG05JF1
NA

0.999

File ID







Yes (FTN Associates)
Yes (FTN Associates)
**
Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)
"H"
Yes (FTN Associates)
Yes (FTN Associates)




                            ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                            been corrected to demonstrate samples uncontaminated.
                            The Battelle lab is the primary lab for MeHg in Surface water.
-------
                     Station ID   M5-738-SWF    Surface Water
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
X
X
X
X
Not Noted, Refer to Laboratory and SESD SOP
X
X
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X

X

In Hg lab Area
None







X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X





X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
ppm
X
Yes (FTN Associates)
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) |Fall 98 (68.2%R) Fail| Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Validation Criteria
               Applied Qualifiers |_
"B (NR)"
                        "H"
X = Attached or Verified

Data Qualifiers
" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID   M5-828-SWF    Surface Water
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                      Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                       Notes
Total P
Total N
TOC
Total Hg
MeHg
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
09/28/99
10/08/99
10/27/99
X
FW=SW
09/28/99
10/08/99
1 1/23/99
X
FW=SW
09/28/99
10/22/99
10/22/99

X
FW=SW
09/28/99
10/04/99
10/05/99

X
FW=SW
09/28/99


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.0084
ppm
EPA 365.1
AS
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
0.55
ppm
Antek
CB
0.03 ppm
NA
4ml
sample aliquot
1
18.67
ppm
EPA415.1
SB
0.12 ppm
1000 ml
1000 ml
sample aliquot
1
2.52
ppt
EPA 1631
JL
0.3 ppt
Battelle is
the Main Lab



ppt
EPA 1630

0.02 ppt
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
EPA1027C
NA
**
All <20 RPD
All Good
All Good
0.0006 and > ppm
0.9957
ANTEK 11-23-99
NA
NR
< 20 RPD
All Good
All Good
0.03 and >
NA
10-22-99/TOC-B
NA
All < MDL
All <20 RPD
All Good
All Good
0.12 and >
0.999

HG05JF1
NA

0.999

File ID







Yes (FTN Associates)
Yes (FTN Associates)
**
Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)"
Yes (FTN Associates)
Yes (FTN Associates)

Yes (FTN Associates)
Yes (FTN Associates)




                            ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                            been corrected to demonstrate samples uncontaminated.
                            The Battelle lab is the primary lab for MeHg in Surface water.
-------
                     Station ID   M5-828-SWF    Surface Water
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
X
X
X
X
Not Noted, Refer to Laboratory and SESD SOP
X
X
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X

X

In Hg lab Area
None







X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X





X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
ppm
X
Yes (FTN Associates)
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) |Fall 98 (68.2%R) Fail| Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Validation Criteria
               Applied Qualifiers |_
"B (NR)"
X = Attached or Verified

Data Qualifiers
" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September 1999  Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID   M5-944-SWF    Surface Water
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                      Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
  Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                       Notes
Total P
Total N
TOC
Total Hg
MeHg
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FW=SW
09/22/99
10/08/99
10/27/99
X
FW=SW
09/22/99
02/24/00
02/24/00
X
FW=SW
09/22/99
10/22/99
10/22/99

X
FW=SW
09/22/99
10/12/99
10/13/99

X
FW=SW
09/22/99


The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
5ml
10ml
sample aliquot
1
0.0055
ppm
EPA 365.1
AS
0.0003ppm (O.Olumol/L 97)
Injection Vial
Injection Vial
sample aliquot
1
0.28
ppm
Antek
CB
0.03 ppm
NA
4ml
sample aliquot
1
7.77
ppm
EPA415.1
SB
0.12 ppm
1000 ml
1000 ml
sample aliquot
1
1.69
ppt
EPA 1631
JL
0.3 ppt
Battelle is
the Main Lab



ppt
EPA 1630

0.02 ppt
Yes (FTN Associates)
Yes (FTN Associates)
Yes
Yes (FTN Associates)
Yes (FTN Associates)
No
Yes (FTN Associates)
Yes (FTN Associates)
No
Yes (FTN Associates)
Yes (FTN Associates)
Yes



FIU/SERC Laboratory uses the same ID as the Sampling Station ID
EPA1027C
NA
**
All <20 RPD
All Good
All Good
0.0006 and > ppm
0.9957
ANTEK 2-24-00
NA
NR
< 20 RPD
74%
All Good
0.03 and >
NA
10-22-99/TOC-B
NA
All < MDL
All <20 RPD
All Good
All Good
0.12 and >
0.999

HG13JF1
NA

0.9994

File ID







Yes (FTN Associates)
Yes (FTN Associates)
**
Yes (FTN Associates)
Yes (FTN Associates)
"B (NR)", "M", "H"
Yes (FTN Associates)
Yes (FTN Associates)
"H"
Yes (FTN Associates)
Yes (FTN Associates)




                            ** The blanks are reported above MDL, Lab water was used as a blank but, not in the sample digestion process. Procedure has
                            been corrected to demonstrate samples uncontaminated.
                            The Battelle lab is the primary lab for MeHg in Surface water.
-------
                     Station ID   M5-944-SWF     Surface Water
            Total Samples/Matrix
              Methods/Parameters
       Range of Samples analyzed
          Holding Time Summary
              Analytical Problems
       QA/QC Acceptance Limits
          Integrity of Data Quality
            Deviations From SOP
                     Observations
Sample Management Records
            Sampling Location ID
                           Matrix
      Preservative (Acid, Temp..)
            Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                Sample Run Logs
             Instrument Raw Data
                    Bench Sheets
         Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All  Calculation Checked
                  Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
Total P
Total N
TOC
Total Hg
MeHg
The Narrative Section will be written after all of the analyses are completed













































X
X
X
X
X
X
Not Noted, Refer to Laboratory and SESD SOP
X
X
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
Status Sheet/Run Tracking Log
Internal COC
X
X

X

In Hg lab Area
None







X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X





X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
uM
X
Yes (FTN Associates)
ppm
X
Yes (FTN Associates)
ppt



South Florida Water Management District (SFWMD)
Spring 99 (60%R) |Fall 98 (68.2%R) Fail| Fall 98 (95%R) Pass
FDEP (9-99)
Fail
Never compared
NA
Validation Criteria
               Applied Qualifiers |_
"B (NR)", "M", "H"
                             "H"
X = Attached or Verified

Data Qualifiers
" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
Water - Battelle
-------
 10% Recalculated Results for Methylmercury in Surface Water Analyzed by
Battelle Marine Sciences Laboratory for the September 1999 Wet Season (M5)
Entered by mwb /njs 02/04/00
                          Checked by: njs 4-13-
Sampling Station
ID
M5-622-SWB
M5-622-SWB (QA-DUP)
M5-635-SWB
Method Blank
Instrument Blank
M5-623-SWB (QA)
M5-623-SWB (QA MS)
M5-623-SWB (QA MSB)
M5-633-SWB (QA)
M5-633-SWB (QA MS)
M5-633-SWB (QA MSB)
Borm-2 (QA-SRM)
StdlSO(QAICV)
Stdl34(QASVS)
Stdl35 (QACCV)
Stdl35 (QACCV)
Std 150 (QACCV)

M5-647-SWB
Method Blank
Instrument Blank
M5-642-SWB (QA)
M5-642-SWB (QA-BUP)
M5-643-SWB (QA)
M5-643-SWB (QA MS)
M5-643-SWB (QA MSB)
M5-656-SWB (QA)
M5-656-SWB (QA MS)
M5-656-SWB (QA MSB)
BORM-2 (SRM)
StdlSO(ICV)
Stdl34(SVS)
StdlSO(CCV)
Stdl34(SVS)
Stdl35(CCV)
StdlSO(CCV)
Stdl34(SVS)
Stdl34(SVS)
BORM-2 (SRM)
Stdl35(CCV)
StdlSO(CCV)
StdlSO(CCV)
StdlSO(CCV)

Battelle
MSL Code
1405-115
1405-115
1405-125
BLK101299

1405-116
1 405-1 16-MS
1 405-1 16-MSB
1405-124
1 405-1 24-MS
1 405-1 24-MSB







1405-135
BLK101399

1405-131
1405-1 31 -BUP
1405-132
1 405-1 32-MS
1 405-1 32-MSB
1405-142
1 405-1 42-MS
1 405-1 42-MSB















Bata Qualifier
Note




QC
Batch
101399MEB
101399MEB
101399MEB
101399MEB
Instrument
Peak
Height
12772
13196
814
304
Distilled
Sample
Volume(ml)
49.402
49.767
50.816
50.721
The Instrument Blanks were performed but, not reported















101399MEB
101399MEB
101399MEB
101399MEB
101399MEB
101399MEB
101399MEB
101399MEB
101399MEB
101399MEB
101399MEB
101399MEB

101499MEB
101499MEB
3215
13100
13576
990
9571
9881







1111
550
49.838
50.830
50.125
50.657
50.015
50.733







49.826
50.428
The Instrument Blanks were performed but, not reported










"M"




"M"
"M"






101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB
101499MEB

2853
3198
1505
8275
8651
990
9063
8674















50.525
50.757
50.666
50.78
49.660
49.418
49.859
50.325















Volume
Analyzed
(ml)
49.402
49.767
50.816
50.721

49.838
50.830
50.125
50.657
50.015
50.733
0.025
0.025
0.040
0.2
0.100
0.025

49.826
50.428

50.525
50.757
50.666
50.78
49.660
49.418
49.859
50.325
0.025
0.025
0.04
0.025
0.04
0.1
0.025
0.04
0.04
0.025
0.1
0.025
0.025
0.025

Distillation
Correction
Factor
0.890
0.890
0.890
0.890

0.890
0.890
0.890
0.890
0.890
0.890







0.788
0.788

0.788
0.788
0.788
0.788
0.788
0.788
0.788
0.788















Y intercept
492
492
492
492

492
492
492
492
492
492







475
475

475
475
475
475
475
475
475
475















Slope
(factor)
60.6
60.6
60.6
60.6

60.6
60.6
60.6
60.6
60.6
60.6







54
54

54
54
54
54
54
54
54
54















Blank
Correction
Factor
0
0
0
0

o
o
0
o
o
o







0
o

o
o
o
o
o
o
o
o















Hg
Concentration
ng/L
4.61
4.73
0.12
-0.07

1.01
4.60
4.84
0.18
3.37
3.43
4.21
82.5
2.74
290.0
168.5
77.9

0.30
0.03

1.11
1.26
0.48
3.61
3.87
0.245
4.05
3.83
4.11
86.9
0.000
79.8
3.43
157
88.4
1.89
0.000
4.79
173.9
89.2
81.0
94.8

BETECTION
LIMIT
ng/L
0.0226
0.0224
0.0219
0.022

0.0224
0.0219
0.0222
0.022
0.0223
0.022







0.0253
0.0250

0.0249
0.0248
0.0248
0.0248
0.0254
0.0255
0.0252
0.025















TRUE
CONG






3.43
3.48

3.49
3.44
4.47
87.3
3.12
321
161
87.3







3.44
3.51

3.5
3.44
4.47
87.3
3.12
87.3
3.12
161.2
87.3
3.12
3.12
4.47
161.2
87.3
87.3
87.3

%R






104.5
110.0

91.2
94.5
94.2
94.5
87.8
90.3
104.7
89.2







91.0
96.6

108.7
104.2
91.9
99.5
0.0
91.4
109.9
97.4
101.3
60.6
0.0
107.2
107.9
102.2
92.8
108.6

Relative
Percent
Bifference

2.66





5.10


1.93











13.07


6.94


-5.56















"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
 10 % Recalculated Results for Methylmercury in Surface Water Analyzed by
Battelle Marine Sciences Laboratory for the September 1999 Wet Season (M5)
Entered by mwb /njs 02/04/00
                          Checked by: njs 4-13-
Sampling Station
ID
M5-659-SWB
M5-669-SWB
Method Blank
Instrument Blank
M5-657-SWB (QA)
M5-657-SWB (QA-DUP)
M5-661-SWB(QA)
M5-661-SWB(QAMS)
M5-661-SWB(QAMSD)
M5-668-SWB (QA)
M5-668-SWB (QA MS)
M5-668-SWB (QA MSB)
Dorm-2 (SRM)
StdlSO(ICV)
Stdl34(SVS)
Stdl34(SVS)
StdlSO(CCV)
StdlSO(CCV)
Stdl35(CCV)

M5-674-SWB
M5-687-SWB
Method Blank
Instrument Blank
M5-684-SWB (QA)
M5-684-SWB (QA-DUP)
M5-675-SWB (QA)
M5-675-SWB (QA MS)
M5-675-SWB (QA MSB)
M5-685-SWB (QA)
M5-685-SWB (QA MS)
M5-685-SWB (QA MSB)
Borm-2 (ICV)
StdlSO(ICV)
Stdl34(SVS)
Stdl34(SVS)
StdlSO(CCV)
Stdl34(SVS)
Stdl34(SVS)
StdlSO(CCV)
StdlSO(CCV)

Battelle
MSL Code
1405-145
1405-155
BLK101499

1405-143
1 405-1 43-BUP
1405-147
1 405-1 47-MS
1405-1 47 -MSB
1405-154
1 405-1 54-MS
1 405-1 54-MSB








1405-1
1405-11
BLK092999

1405-8
1405-8-BUP
1405-2
1405-2-MS
1405-2-MSB
1405-9
1405-9-MS
1405-9-MSB










Bata Qualifier
Note



QC
Batch
101599MEB
101599MEB
101599MEB
Instrument
Peak
Height
783
989
0
Distilled
Sample
Volume(ml)
50.281
50.405
50.462
The Instrument Blanks were performed but, not reported










"M"








101599MEB
101599MEB
101599MEB
101599MEB
101599MEB
101599MEB
101599MEB
101599MEB
101599MEB
101599MEB
101599MEB
101599MEB
101599MEB
101599MEB
101599MEB

093099MEB
093099MEB
093099MEB
474
435
993
8434
7993
939
8969
7107








1551
2838
360
50.556
49.713
50.489
50.745
50.401
50.871
50.332
50.577








50.333
50.878
49.904
The Instrument Blanks were performed but, not reported










"M"
"M"






093099MEB
093099MEB
093099MEB
093099MEB
093099MEB
093099MEB
093099MEB
093099MEB
093099MEB
093099MEB
093099MEB
093099MEB
093099MEB
093099MEB
093099MEB
093099MEB
093099MEB

1100
1150
871
12438
12031
607
12073
11462










50.042
49.334
50.331
49.97
49.853
50.496
49.97
49.853










Volume
Analyzed
(ml)
50.281
50.405
50.462

50.556
49.713
50.489
50.745
50.401
50.871
50.332
50.577
0.025
0.025
0.040
0.040
0.025
0.025
0.050

50.333
50.878
49.904

50.042
49.334
50.331
49.97
49.853
50.496
49.97
49.853
0.025
0.050
0.100
0.040
0.050
0.040
0.100
0.050
0.05

Distillation
Correction
Factor
0.838
0.838
0.838

0.838
0.838
0.838
0.838
0.838
0.838
0.838
0.838








0.928
0.928
0.928

0.928
0.928
0.928
0.928
0.928
0.928
0.928
0.928










Y intercept
280
280
280

280
280
280
280
280
280
280
280








455
455
455

455
455
455
455
455
455
455
455










Slope
(factor)
49
49
49

49
49
49
49
49
49
49
49








69.6
69.6
69.6

69.6
69.6
69.6
69.6
69.6
69.6
69.6
69.6










Blank
Correction
Factor
0
0
0

o
o
0
o
o
o
o
o








0
o
0

0
0
0
0
0
0
0
0










Hg
Concentration
ng/L
0.24
0.34
-0.14

0.09
0.08
0.34
3.91
3.73
0.32
4.20
3.29
4.32
90.6
1.37
3.22
90.1
95.4
83.8

0.34
0.73
-0.03

0.20
0.22
0.13
3.71
3.60
0.05
3.60
3.42
4.11
173.7
5.19
1.08
170
2.36
7.92
180.8
174

BETECTION
LIMIT
ng/L
0.0235
0.0235
0.0235

0.0234
0.0238
0.0234
0.0233
0.0235
0.0233
0.0235
0.0234








0.0212
0.021
0.0214

0.0214
0.0217
0.0212
0.0214
0.0214
0.0212
0.0214
0.0214










TRUE
CONG







3.44
3.46

3.47
3.45
4.47
87.3
3.12
3.12
87.3
87.3
80.6








3.51
3.48

3.49
3.5
4.47
174.5
7.79
3.12
174.5
3.12
7.79
174.5
174.5

%R







103.8
97.8

112.1
86.1
96.6
103.8
43.9
103.2
103.2
109.3
104.0








102.1
99.6

101.8
96.3
91.9
99.5
66.6
34.6
97.4
75.6
101.7
103.6
99.7

Relative
Percent
Bifference





-20.69


-4.88


-24.48













8.89


-3.22


-5.17










"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
 10 % Recalculated Results for Methylmercury in Surface Water Analyzed by
Battelle Marine Sciences Laboratory for the September 1999 Wet Season (M5)
Entered by mwb /njs 02/04/00
                          Checked by: njs 4-13-00
Sampling Station
ID
M5-699-SWB
M5-699-SWB (QA-DUP)
Method Blank
Instrument Blank
M5-693-SWB (QA)
M5-693-SWB (QA MS)
M5-693-SWB (QA MSB)
M5-703-SWB (QA)
M5-703-SWB(QAMS)
M5-703-SWB(QAMSD)
Dorm-2 (QA CCV)
Stdl34(QACCV)
StdlSO(QACCV)
StdlSO(QACCV)
StdlSO(QACCV)
Stdl35(QACCV)
Stdl35(QACCV)

M5-709-SWB
M5-724-SWB
Method Blank
Instrument Blank
M5-720-SWB (QA)
M5-720-SWB (QA-DUP)
M5-707-SWB (QA)
M5-707-SWB(QAMS)
M5-707-SWB(QAMSD)
M5-712-SWB(QA)
M5-712-SWB(QAMS)
M5-712-SWB(QAMSD)
Dorm-2 (SRM)
StdlSO(ICV)
Stdl34(SVS)
Stdl34(SVS)
StdlSO(CCV)
StdlSO(CCV)
StdlSO(CCV)
StdlSO(CCV)

Battelle
MSL Code
1405-21
1 405-21 -DUP
BLK093099

1405-17
1405-17-MS
1405-17-MSD
1405-25
1405-25-MS
1405-25-MSD








1405-31
1405-41
BLK1 00499

1405-38
1405-38-DUP
1405-29
1405-29-MS
1405-29-MSD
1405-33
1405-33-MS
1405-33-MSD









Data Qualifier
Note



QC
Batch
100199MEB
100199MEB
100199MEB
Instrument
Peak
Height
1313
1305
0
Distilled
Sample
Volume(ml)
50.686
49.514
50.745
The Instrument Blanks were performed but, not reported

















100199MEB
100199MEB
100199MEB
100199MEB
100199MEB
100199MEB
100199MEB
100199MEB
100199MEB
100199MEB
100199MEB
100199MEB
100199MEB

100599MEB
100599MEB
100599MEB
798
12026
11747
1333
12023
13908








650
646
0
50.083
49.923
50.018
49.631
50.19
50.062








49.733
49.353
50.825
The Instrument Blanks were performed but, not reported

















100599MEB
100599MEB
100599MEB
100599MEB
100599MEB
100599MEB
100599MEB
100599MEB
100599MEB
100599MEB
100599MEB
100599MEB
100599MEB
100599MEB
100599MEB
100599MEB

1177
1144
759
11609
12339
597
9925
8998









49.97
50.399
49.956
49.747
49.529
49.446
50.461
50.369









Volume
Analyzed
(ml)
50.686
49.514
50.745

50.083
49.923
50.018
49.631
50.19
50.062
0.025
0.040
0.05
0.025
0.025
0.050
0.05

49.733
49.353
50.825

49.97
50.399
49.956
49.747
49.529
49.446
50.461
50.369
0.025
0.100
0.040
0.040
0.025
0.025
0.025
0.025

Distillation
Correction
Factor
0.937
0.937
0.937

0.937
0.937
0.937
0.937
0.937
0.937








0.842
0.842
0.842

0.842
0.842
0.842
0.842
0.842
0.842
0.842
0.842









Y intercept
490
490
490

490
490
490
490
490
490








332
332
332

332
332
332
332
332
332
332
332









Slope
(factor)
69.3
69.3
69.3

69.3
69.3
69.3
69.3
69.3
69.3








68.3
68.3
68.3

68.3
68.3
68.3
68.3
68.3
68.3
68.3
68.3









Blank
Correction
Factor
0
0
0

0
0
0
0
0
0








0
0
0

0
0
0
0
0
0
0
0









Hg
Concentration
ng/L
0.25
0.25
-0.1487

0.09
3.56
3.47
0.26
3.54
4.13
4.20
2.71
165.2
88.9
102.4
85.5
85.2

0.11
0.11
-0.11

0.29
0.28
0.15
3.94
4.22
0.09
3.31
2.99
4.22
332
3.66
3.32
85.7
95.7
94.0
86.0

DETECTION
LIMIT
ng/L
0.0209
0.0214
0.0209

0.0211
0.0212
0.0212
0.0213
0.0211
0.0211








0.0237
0.0239
0.0232

0.0236
0.0234
0.0236
0.0237
0.0238
0.0238
0.0233
0.0234









TRUE
CONG





3.51
3.48

3.49
3.5
4.47
3.12
174.5
87.25
87.25
80.6
80.6








3.51
3.52

3.46
3.46
4.47
349
3.12
3.12
87.3
87.3
87.3
87.3

%R





98.7
96.9

93.9
110.5
94.0
87.0
94.7
101.9
117.4
106.1
105.7








108.1
115.5

92.8
83.8
94.4
95.1
117.3
106.4
98.2
109.6
107.7
98.5

Relative
Percent
Difference

1.36




-2.64


15.36













-4.84


6.71


-9.97









"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
 10 % Recalculated Results for Methylmercury in Surface Water Analyzed by
Battelle Marine Sciences Laboratory for the September 1999 Wet Season (M5)
Entered by mwb /njs 02/04/00
                          Checked by: njs 4-13-
Sampling Station
ID
M5-734-SWB
Method Blank
Instrument Blank
M5-726-SWB (QA)
M5-726-SWB (QA-DUP)
M5-727-SWB (QA)
M5-727-SWB(QAMS)
M5-727-SWB(QAMSD)
M5-738-SWB (QA)
M5-738-SWB(QAMS)
M5-738-SWB(QAMSD)
Dorm-2 (SRM)
StdlSO(ICV)
Stdl34(SVS)
Stdl34(SVS)
StdlSO(CCV)
StdlSO(CCV)
StdlSO(CCV)

M5-859-SWB
Method Blank
Method Blank
Instrument Blank
M5-823-SWB (QA)
M5-823-SWB (QA-DUP)
QA-636-SWB (QA)
QA-636-SWB (QA-DUP)
M5-672-SWB(QA)
M5-672-SWB (QA MS)
M5-672-SWB (QA MSD)
QA-630-SWB (QA)
QA-630-SWB (QA MS)
QA-630-SWB (QA MSD)
QA-651-SWB(QA)
QA-651-SWB(QAMS)
QA-651-SWB(QAMSD)
Dorm-2 (SRM)
StdlSO(ICV)
Stdl34(SVS)
Stdl34(SVS)
Stdl34(SVS)
StdlSO(CCV)
Stdl35(CCV)
StdlSO(CCV)
Stdl34(SVS)
StdlSO(CCV)
StdlSO(CCV)
StdlSO(CCV)
StdlSO(CCV)

Battelle
MSL Code
1405-51
BLK1 00599

1405-43
1405-43-DUP
1405-44
1405-44-MS
1405-44-MSD
1405-53
1405-53-MS
1405-53-MSD








1405-165
BLK101899-rl
BLK101899-r2

1405-161
1405-1 61 -DUP
1405-171
1405-1 71 -DUP
1405-157
1 405-1 57-MS
1405-1 57 -MSD
1405-169
1 405-1 69-MS
1 405-1 69-MSD
1405-174
1405-174-MS
1 405-1 74-MSD














Data Qualifier
Note


QC
Batch
100699MEB
100699MEB
Instrument
Peak
Height
646
130
Distilled
Sample
Volume(ml)
49.353
49.082
The Instrument Blanks were performed but, not reported
"DQO"
"DQO"








"M"








100699MEB
100699MEB
100699MEB
100699MEB
100699MEB
100699MEB
100699MEB
100699MEB
100699MEB
100699MEB
100699MEB
100699MEB
100699MEB
100699MEB
100699MEB

101999MEB
101999MEB
101999MEB
595
717
521
10222
10097
421
10582
10461








1002
0
211
49.411
49.481
50.22
50.291
50.205
50.223
49.251
49.200








50.384
50.211
49.889
The Instrument Blanks were performed but, not reported

















"M"



"M"





101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB
101999MEB

4296
4413
3031
3069
1587
12483
13752
522
12575
12880
1448
11139
12623














50.069
50.635
50.64
50.649
50.707
50.311
49.238
50.835
50.42
49.737
50.938
50.009
49.971














Volume
Analyzed
(ml)
49.353
49.082

49.411
49.481
50.22
50.291
50.205
50.223
49.251
49.200
0.025
0.025
0.04
0.04
0.025
0.025
0.03

50.384
50.211
49.889

50.069
50.635
50.64
50.649
50.707
50.311
49.238
50.835
50.42
49.737
50.938
50.009
49.971
0.025
0.025
0.040
0.040
0.040
0.025
0.200
0.025
0.040
0.025
0.025
0.025
0.025

Distillation
Correction
Factor
0.841
0.841

0.841
0.841
0.841
0.841
0.841
0.841
0.841
0.841








0.919
0.919
0.919

0.919
0.919
0.919
0.919
0.919
0.919
0.919
0.919
0.919
0.919
0.919
0.919
0.919














Y intercept
305
305

305
305
305
305
305
305
305
305








279
79
52

79
79
52
52
79
79
79
79
79
79
352
352
352














Slope
(factor)
67.3
67.3

67.3
67.3
67.3
67.3
67.3
67.3
67.3
67.3








71.1
71.1
75.6

71.
71.
75.6
75.6
71.
71.
71.
71.
71.
71.
75.6
75.6
75.6














Blank
Correction
Factor
0
0

0
o
o
0
o
o
o
o








0
o
o

o
o
o
o
o
o
o
o
o
o
o
o
o














Hg
Concentration
ng/L
0.12
-0.06

0.10
0.15
0.08
3.48
3.45
0.04
3.69
3.65
3.76
95.40
2.32
3.70
89.80
85.30
81.70
0.22
-0.09
-0.04

1.23
1.25
0.76
0.77
0.39
3.71
4.19
0.07
3.73
3.88
0.31
3.10
3.53
4.24
88.6
2.87
2.74
1.94
103
343
88.1
0.0000
90.2
96.3
87.6
93.0

DETECTION
LIMIT
ng/L
0.0235
0.024

0.0239
0.0238
0.0235
0.0235
0.0235
0.0235
0.0239
0.024








0.0214
0.0215
0.0216

0.0216
0.0213
0.0213
0.0213
0.0213
0.0215
0.0219
0.0212
0.0214
0.0217
0.0212
0.0216
0.0216














TRUE
CONG






3.47
3.48

3.54
3.55
4.47
87.3
3.12
3.12
87.3
87.3
87.3










3.47
3.54

3.46
3.51

3.49
3.49
4.47
87.3
3.12
3.12
3.12
87
322
87.3
3.12
87.3
87.3
87.3
87.3

%R






98.2
96.8

103.0
101.6
84.1
109.3
74.4
118.6
102.9
97.7
93.6










95.6
107.1

105.8
108.4

80.1
92.4
94.9
101.5
92.0
87.8
62.2
118.0
106.5
100.9
0.0
103.3
110.3
100.3
106.5

Relative
Percent
Difference




34.62


-1.10


-1.08













1.75

1.39


12.03


3.81


12.95














"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
 10 % Recalculated Results for Methylmercury in Surface Water Analyzed by
Battelle Marine Sciences Laboratory for the September 1999 Wet Season (M5)
Entered by mwb /njs 02/04/00
                          Checked by: njs 4-13-
Sampling Station
ID
M5-878-SWB
Method Blank
Instrument Blank
QA-671-SWB(QA)
QA-671-SWB(QA-DUP)
M5-746-SWB (QA)
M5-746-SWB(QAMS)
M5-746-SWB(QAMSD)
M5-920-SWB (QA)
M5-920-.V,',; 	 VMS)
M5-920-SWB (QA MSB)
Dorm-2 (SRM)
StdlSO(ICV)
Stdl34(SVS)
Stdl34(SVS)
StdlSO(CCV)
StdlSO(CCV)
StdlSO(CCV)
StdlSO(CCV)
StdlSO(CCV)

Battelle
MSL Code
1405-61
BLK1 00699

1405-68
1405-68-DUP
1405-59
1405-59-MS
1405-59-MSD
1405-64
1405-64-MS
1405-64-MSD










Data Qualifier
Note


QC
Batch
100799MEB
100799MEB
Instrument
Peak
Height
855
196
Distilled
Sample
Volume(ml)
50.872
50.234
The Instrument Blanks were performed but, not reported






"DQO"
"DQO"



"M"






100799MEB
100799MEB
100799MEB
100799MEB
100799MEB
100799MEB
100799MEB
100799MEB
100799MEB
100799MEB
100799MEB
100799MEB
100799MEB
100799MEB
100799MEB
100799MEB
100799MEB

1329
1248
485
10284
10450
1053
10807
8027










50.889
50.196
49.59
50.065
50.408
51.002
49.284
50.317










Volume
Analyzed
(ml)
50.872
50.234

50.889
50.196
49.59
50.065
50.408
51.002
49.284
50.317
0.025
0.025
0.04
0.04
0.025
0.025
0.025
0.025
0.03

Distillation
Correction
Factor
0.777
0.777

0.777
0.777
0.777
0.777
0.777
0.777
0.777
0.777










Y intercept
386
386

386
386
386
386
386
386
386
386










Slope
(factor)
67.4
67.4

67.4
67.4
67.4
67.4
67.4
67.4
67.4
67.4










Blank
Correction
Factor
0
0

0
o
o
0
o
o
o
o










Hg
Concentration
ng/L
0.18
-0.07

0.35
0.33
0.04
3.78
3.81
0.25
4.04
2.90
3.75
99.8
3.00
1.20
69.3
86.8
91.8
88.2
76.5

DETECTION
LIMIT
ng/L
0.0251
0.0254

0.0251
0.0254
0.0257
0.0255
0.0253
0.025
0.0259
0.0254










TRUE
CONG






3.49
3.46

3.54
3.47
4.47
87.3
3.12
3.12
87.3
87.3
87.3
87.3
87.3

%R






107.1
109.1

107.0
76.4
83.9
114.3
96.2
38.5
79.4
99.4
105.2
101.0
87.6

Relative
Percent
Difference




-7.61


0.98


-32.80










"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5)  1999 Samples for Critical Parameters Analyzed by Battelle
With the 10% Full QA/QC Review
Total Methylmercury in Surface Water
                                            Sampling Station ID
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
   Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
   Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                      Notes
M5-622-SWB
M5-633-SWB
M5-643-SWB
M5-656-SWB
1405-115
M5-622-SWB
surface water = SW
09/30/99
10/12/99
10/13/99
101399MEB
49.402
49.402
aliquot
1
4.61
ng/L (ppt)
1631/1630
Niewolny
0.0226
1405-124
M5-633-SWB
surface water = SW
09/29/99
10/12/99
10/13/99
101399MEB
50.657
50.657
aliquot
1
0.18
ng/L (ppt)
1631/1630
Niewolny
0.022
1405-132
M5-643-SWB
surface water = SW
09/29/99
10/13/99
10/14/99
101499MEB
50.666
50.666
aliquot
1
0.48
ng/L (ppt)
1631/1630
Niewolny
0.0248
1405-142
M5-656-SWB
surface water = SW
09/28/99
10/13/99
10/14/99
101499MEB
49.418
49.418
aliquot
1
0.245
ng/L (ppt)
1631/1630
Niewolny
0.0255
NR
LIMS
Yes
NR
LIMS
Yes
NR
LIMS
Yes
NR
LIMS
Yes
1405-115
101399MEB
Good
NR
All Good
All Good
All Good
0.0226 and >
0.9989
1405-124
101399MEB
Good
NR
All Good
All Good
All Good
0.022 and >
0.9989
1405-132
101499MEB
Good
NR
All Good
"M"
All Good
0.0248 and >
0.9991
1405-142
101499MEB
Good
NR
All Good
"M"
All Good
0.0255 and >
0.9991
NR
LIMS


NR N
LIMS LII
"]\

R NR
VIS LIMS
A" "M"

"*" Method blank is above the true MDL, but less than 3 times the MDL.
The instrument blanks were performed but, not reported.
-------
                                      M5-622-SWB
M5-633-SWB
M5-643-SWB
M5-656-SWB
Narrative Description (Attached)
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation Criteria
                Applied Qualifiers [
15 I/Waters
X
X
X
X
X
X
X
X
15 I/Waters
X
X
X
X
X
X
X
X
15 I/Waters
X
X
X
X
X
X
X
X
15 I/Waters
X
X
X
X
X
X
X
X
X
X
NR
X
X
X
NR
X
X
NR
X
X
X
NR
X
X
NR
X
X
X
NR
X
X
NR
X
X
X
NR
X
X
X
NA
X
X
X
X
NA
X
X
X
X
NA
X
X
X
X
NA
X

X
X
ng/L
X
X
ng/L
X
X
ng/L
X
X
ng/L

NR
NR
NR
NR
NR
NR
NR
NR



"M"
"M"
X =  Attached or Verified

Data Qualifiers
"J"   Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5)  1999 Samples for Critical Parameters Analyzed by Battelle
With the 10% Full QA/QC Review
Total Methylmercury in Surface Water
                                            Sampling Station ID
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
   Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
   Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                      Notes
M5-661-SWB
M5-672-SWB
M5-684-SWB
M5-693-SWB
1405-147
M5-661-SWB
surface water = SW
09/29/99
10/14/99
10/15/99
101599MEB
50.489
50.489
aliquot
1
0.34
ng/L (ppt)
1631/1630
Niewolny
0.0234
1405-157
M5-672-SWB
surface water = SW
09/27/99
10/18/99
10/19/99
101999MEB
50.707
50.707
aliquot
1
0.39
ng/L (ppt)
1631/1630
Niewolny
0.0213
1405-8
M5-684-SWB
surface water = SW
09/26/99
09/29/99
09/30/99
093099MEB
50.042
50.042
aliquot
1
0.2
ng/L (ppt)
1631/1630
Niewolny
0.0214
1405-17
M5-693-SWB
surface water = SW
09/25/99
09/30/99
10/01/99
100199MEB
50.083
50.083
aliquot
1
0.09
ng/L (ppt)
1631/1630
Niewolny
0.0211
NR
LIMS
Yes
NR
LIMS
Yes
NR
LIMS
Yes
NR
LIMS
Yes
1405-147
101599MEB
Good
NR
All Good
"M"
All Good
0.0234 and >
0.9976
1405-157
101999MEB
Good
NR
All Good
"M"
All Good
0.0213 and >
0.996
1405-8
093099MEB
Good
NR
All Good
"M"
All Good
0.0214 and >
0.99952
1405-17
100199MEB
Good
NR
All Good
All Good
All Good
0. 0211 and >
0.99768
NR
LIMS
"M"

NR N
LIMS LII
"M" "J

R NR
VIS LIMS
A"

"*" Method blank is above the true MDL, but less than 3 times the MDL.
The instrument blanks were performed but, not reported.
-------
                                      M5-661-SWB
M5-672-SWB
M5-684-SWB
M5-693-SWB
Narrative Description (Attached)
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation Criteria
                Applied Qualifiers [
15 I/Waters
X
X
X
X
X
X
X
X
15 I/Waters
X
X
X
X
X
X
X
X
15 I/Waters
X
X
X
X
X
X
X
X
15 I/Waters
X
X
X
X
X
X
X
X
X
X
NR
X
X
X
NR
X
X
NR
X
X
X
NR
X
X
NR
X
X
X
NR
X
X
NR
X
X
X
NR
X
X
X
NA
X
X
X
X
NA
X
X
X
X
NA
X
X
X
X
NA
X

X
X
ng/L
X
X
ng/L
X
X
ng/L
X
X
ng/L

NR
NR
NR
NR
NR
NR
NR
NR

"M"
"M"
"M"

X=  Attached or Verified

Data Qualifiers
"J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria
were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5)  1999 Samples for Critical Parameters Analyzed by Battelle
With the 10% Full QA/QC Review
Total Methylmercury in Surface Water
                                            Sampling Station ID
Laboratory Records
Data Report (Attached)
           Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
               Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                    Analyst
         Method Detection limit
Data Report (Verified)
   Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
           Laboratory ID Code
                 QC Batch ID
               Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
   Data Entry Checked by Another
        All Calculation Checked
               QC Limits Met

                      Notes
M5-703-SWB
M5-712-SWB
M5-726-SWB
M5-738-SWB
1405-25
M5-703-SWB
surface water = SW
09/24/99
09/30/99
10/01/99
100199MEB
49.631
49.631
aliquot
1
0.26
ng/L (ppt)
1631/1630
Niewolny
0.0213
1405-33
M5-712-SWB
surface water = SW
09/24/99
10/18/99
10/19/99
100599MEB
49.446
49.446
aliquot
1
0.09
ng/L (ppt)
1631/1630
Niewolny
0.0238
1405-43
M5-726-SWB
surface water = SW
09/23/99
10/05/99
10/06/99
100699MEB
49.411
49.411
aliquot
1
0.1
ng/L (ppt)
1631/1630
Niewolny
0.0239
1405-142
M5-738-SWB
surface water = SW
09/22/99
10/05/99
10/06/99
100699MEB
50.223
50.223
aliquot
1
0.04
ng/L (ppt)
1631/1630
Niewolny
0.0235
NR
LIMS
Yes
NR
LIMS
Yes
NR
LIMS
Yes
NR
LIMS
Yes
1405-25
100199MEB
Good
NR
All Good
All Good
All Good
0.0213 and >
0.99768
1405-33
100599MEB
Good
NR
All Good
All Good
All Good
0.0238 and >
0.9992
1405-43
100699MEB
Good
NR
34.62
"M"
All Good
0.0239 and >
0.9978
1405-142
100699MEB
Good
NR
34.62
"M"
All Good
0.0235 and >
1.9978
NR
LIMS


NR
LIMS


NR
LIMS
"M", "DQO"

NR
LIMS
"M", "DQO"

"*" Method blank is above the true MDL, but less than 3 times the MDL.
The instrument blanks were performed but, not reported.
-------
                                      M5-703-SWB
M5-712-SWB
M5-726-SWB
M5-738-SWB
Narrative Description (Attached)
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation Criteria
                Applied Qualifiers [
15 I/Waters
X
X
X
X
X
X
X
X
15 I/Waters
X
X
X
X
X
X
X
X
15 I/Waters
X
X
X
X
X
X
X
X
15 I/Waters
X
X
X
X
X
X
X
X
X
X
NR
X
X
X
NR
X
X
NR
X
X
X
NR
X
X
NR
X
X
X
NR
X
X
NR
X
X
X
NR
X
X
X
NA
X
X
X
X
NA
X
X
X
X
NA
X
X
X
X
NA
X

X
X
ng/L
X
X
ng/L
X
X
ng/L
X
X
ng/L

NR
NR
NR
NR
NR
NR
NR
NR



"M", "DQO"
"M", "DQO"
X=  Attached or Verified

Data Qualifiers
"J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria
were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5) 1999 Samples for Critical Parameters Analyzed by Battelle
With the 10% Full QA/QC Review
Total Methylmercury in Surface Water
                            Sampling Station ID
Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                     Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
   Data Entry Checked by Another
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RPD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
   Data Entry Checked by Another
        All Calculation Checked
                QC Limits Met

                      Notes
M5-823-SWB
M5-920-SWB
1405-161
M5-823-SWB
surface water = SW
09/30/99
10/18/99
10/19/99
101999MEB
50.069
50.069
aliquot
1
1.25
ng/L (ppt)
1631/1630
Niewolny
0.0216
1405-68
M5-920-SWB
surface water = SW
09/23/99
10/06/99
10/07/99
100799MEB
51.002
50.002
aliquot
1
0.25
ng/L (ppt)
1631/1630
Niewolny
0.025
NR
LIMS
Yes
NR
LIMS
Yes
1405-161
101999MEB
Good
NR
All Good
"M"
All Good
0.0216 and >
0.9976
1405-68
100799MEB
Good
NR
-32.8
"M"
All Good
0.025 and >
0.9981
NR
LIMS
"M"
NR
LIMS
"M", "DQO"
                            *" Method blank is above the true MDL, but less than 3 times the MDL.
                            The instrument blanks were performed but, not reported.
-------
                                      M5-823-SWB
M5-920-SWB
Narrative Description (Attached)
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation Criteria
                Applied Qualifiers [
15 I/Waters
X
X
X
X
X
X
X
X
15 I/Waters
X
X
X
X
X
X
X
X
X
X
NR
X
X
X
NR
X
X
NR
X
X
X
NR
X
X
X
NA
X
X
X
X
NA
X

X
X
ng/L
X
X
ng/L

NR
NR
NR
NR

"M"
"M", "DQO"
X =  Attached or Verified

Data Qualifiers
"J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2"  Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
Soil - SERC
-------
SERC Lab / EPA REMAP results
Mineral Content and Ash Free Dry Weight
       Date:    12/(K"">
  Sample Type:    Sediment
                                Data Entered by LCL 03/16/00
                           Data Entry Checked by: NJS 3-17-00
                                                                                                                           o Inorganic Content
                                                                                                                                               % Organic Content
Sample ID
M5-622-SDF
M5-623-SDF
M5-624-SDF
M5-625-SDF
M5-626-SDF
M5-627-SDF
M5-628-SDF
M5-630-SDF
M5-631-SDF
M5-632-SDF
M5-633-SDF
M5-634-SDF
M5-635-SDF
M5-636-SDF
M5-637-SDF
M5-638-SDF
M5-639-SDF
M5-640-SDF
M5-641-SDF
M5-642-SDF
M5-643-SDF
M5-644-SDF
M5-645-SDF
M5-646-SDF
M5-647-SDF
M5-648-SDF
M5-649-SDF
M5-650-SDF
M5-651-SDF
M5-652-SDF
M5-653-SDF
M5-654-SDF
M5-655-SDF
M5-656-SDF
M5-657-SDF
M5-658-SDF
M5-659-SDF
M5-660-SDF
M5-661-SDF
M5-662-SDF
M5-663-SDF
M5-664-SDF
M5-665-SDF
M5-666-SDF
M5-667-SDF
M5-668-SDF
M5-669-SDF
M5-670-SDF
M5-671-SDF
M5-672-SDF
M5-673-SDF
M5-674-SDF
M5-675-SDF
M5-676-SDF
M5-677-SDF
Collection
Date
09/30/99
09/30/99
09/30/99
09/30/99
09/30/99
09/30/99
09/29/99
09/28/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/28/99
09/29/99
09/28/99
09/29/99
09/29/99
09/30/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/27/99
09/28/99
09/27/99
09/27/99
09/29/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/26/99
09/27/99
09/27/99
09/26/99
09/26/99
09/28/99
09/26/99
Collection
Time
1125
915
1018
1257
908
1050
1716
1520
1414
1010
1115
1510
1216
1405
1210
1630
1715
1116
1615
1011
910
1145
1447
1515
1102
1300
1620
1158
1410
959
1300
1145
1028
900
1751
1722
1205
1450
857
1610
1330
1100
1710
1655
1545
1207
1000
850
850
1100
1400
1025
1130
925
1310
Digestion
Date
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/09/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
Hold Time
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
Time Since
Digestion
70
70
70
70
70
70
71
72
71
71
71
71
71
71
71
71
72
71
72
71
71
70
72
72
72
72
72
72
72
72
72
72
72
72
73
72
73
73
71
73
73
73
73
73
73
73
73
73
78
77
77
78
78
76
78
Technician
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
CB/SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
Vial
Weight
(g)
1.0034
1
0.9994
0.9969
0.9896
0.9871
0.9907
0.9974
0.9972
0.9953
0.9941
1.0032
1.0006
0.9976
0.995
0.9918
0.9997
1.0028
1.0046
1.006
0.9976
1.0065
0.9986
0.9981
1.0001
1.0013
1.0003
1.003
1.0073
1.0057
1.0026
1.0011
0.9973
0.9973
1.0034
1.0033
1.0063
1.0032
1.0034
1.005
1.0064
1.0033
1.0025
1.0046
1.0034
1.0006
0.9997
1.0051
0.9971
1.0043
1.0126
1.0143
1.0121
1.011
1.0056
Sample Weight
(g)
0.0257
0.0247
0.025
0.0251
0.0254
0.0252
0.0248
0.0261
0.0247
0.0246
0.0247
0.025
0.0259
0.0254
0.0263
0.0253
0.0255
0.0245
0.0248
0.025
0.0248
0.025
0.0251
0.0252
0.0254
0.0248
0.0251
0.0248
0.0258
0.0256
0.0252
0.0243
0.0259
0.0259
0.0254
0.0257
0.0246
0.0245
0.0251
0.0248
0.0251
0.0248
0.0252
0.0251
0.247
0.0245
0.0254
0.0251
0.0251
0.0245
0.0248
0.0255
0.0251
0.0256
0.0255
Dried Cup +
Sed (g)
1.0192
1.0013
1.0009
0.9978
0.9912
0.988
0.9922
1.0003
0.9976
1.002
0.9972
1.0065
1.0017
0.9994
1.0009
0.9978
1.004
1.0048
1.0136
1.0085
1.0091
1.0022
1.0024
1.0023
1.0027
1.0041
1.0039
1.0056
1.0194
1.0089
1.0238
1.0039
1.003
1.0051
1.0094
1.0052
1.0115
1.0145
1.0106
1.0064
1.0141
1.0133
1.0058
1.0073
1.0066
1.004
1.0026
1.0119
1.0023
1.0056
1.0293
1.0159
1.0144
1.0137
1.0083
Ashed Sed.
(g)
0.0158
0.0013
0.0015
0.0009
0.0016
0.0009
0.0015
0.0029
0.0004
0.0067
0.0031
0.0033
0.0011
0.0018
0.0059
0.0060
0.0043
0.0020
0.0090
0.0025
0.0115
-0.0043
0.0038
0.0042
0.0026
0.0028
0.0036
0.0026
0.0121
0.0032
0.0212
0.0028
0.0057
0.0078
0.0060
0.0019
0.0052
0.0113
0.0072
0.0014
0.0077
0.0100
0.0033
0.0027
0.0032
0.0034
0.0029
0.0068
0.0052
0.0013
0.0167
0.0016
0.0023
0.0027
0.0027
Mineral
Content
(Fraction)
0.6148
0.0526
0.0600
0.0359
0.0630
0.0357
0.0605
0.1111
0.0162
0.2724
0.1255
0.1320
0.0425
0.0709
0.2243
0.2372
0.1686
0.0816
0.3629
0.1000
0.4637
-0.1720
0.1514
0.1667
0.1024
0.1129
0.1434
0.1048
0.4690
0.1250
0.8413
0.1152
0.2201
0.3012
0.2362
0.0739
0.2114
0.4612
0.2869
0.0565
0.3068
0.4032
0.1310
0.1076
0.0130
0.1388
0.1142
0.2709
0.2072
0.0531
0.6734
0.0627
0.0916
0.1055
0.1059
°/o Mineral
Content
61.5
5.3
6.0
3.6
6.3
3.6
6.0
11.1
1.6
27.2
12.6
13.2
4.2
7.1
22.4
23.7
16.9
8.2
36.3
10.0
46.4
-17.2
15.1
16.7
10.2
11.3
14.3
10.5
46.9
12.5
84.1
11.5
22.0
30.1
23.6
7.4
21.1
46.1
28.7
5.6
30.7
40.3
13.1
10.8
1.3
13.9
11.4
27.1
20.7
5.3
67.3
6.3
9.2
10.5
10.6
Ash Free
Dry
Weight
0.3852
0.9474
0.9400
0.9641
0.9370
0.9643
0.9395
0.8889
0.9838
0.7276
0.8745
0.8680
0.9575
0.9291
0.7757
0.7628
0.8314
0.9184
0.6371
0.9000
0.5363
1.1720
0.8486
0.8333
0.8976
0.8871
0.8566
0.8952
0.5310
0.8750
0.1587
0.8848
0.7799
0.6988
0.7638
0.9261
0.7886
0.5388
0.7131
0.9435
0.6932
0.5968
0.8690
0.8924
0.9870
0.8612
0.8858
0.7291
0.7928
0.9469
0.3266
0.9373
0.9084
0.8945
0.8941
% Ash Free Dry
Weight Content
38.5
94.7
94.0
96.4
93.7
96.4
94.0
88.9
98.4
72.8
87.4
86.8
95.8
92.9
77.6
76.3
83.1
91.8
63.7
90.0
53.6
117.2
84.9
83.3
89.8
88.7
85.7
89.5
53.1
87.5
15.9
88.5
78.0
69.9
76.4
92.6
78.9
53.9
71.3
94.4
69.3
59.7
86.9
89.2
98.7
86.1
88.6
72.9
79.3
94.7
32.7
93.7
90.8
89.5
89.4
-------
Sample ID
M5-678-SDF
M5-679-SDF
M5-680-SDF
M5-681-SDF
M5-682-SDF
M5-683-SDF
M5-684-SDF
M5-685-SDF
M5-686-SDF
M5-687-SDF
M5-688-SDF
M5-689-SDF
M5-690-SDF
M5-691-SDF
M5-692-SDF
M5-693-SDF
M5-694-SDF
M5-695-SDF
M5-696-SDF
M5-697-SDF
M5-698-SDF
M5-699-SDF
M5-700-SDF
M5-701-SDF
M5-702-SDF
M5-703-SDF
M5-704-SDF
M5-705-SDF
M5-706-SDF
M5-707-SDF
M5-708-SDF
M5-709-SDF
M5-708D-SDF
M5-709D-SDF
M5-710-SDF
M5-711-SDF
M5-712-SDF
M5-714-SDF
M5-715-SDF
M5-716-SDF
M5-718-SDF
M5-719-SDF
M5-720-SDF
M5-722-SDF
M5-723-SDF
M5-724-SDF
M5-725-SDF
M5-726-SDF
M5-727-SDF
M5-728-SDF
M5-729-SDF
M5-730-SDF
M5-731-SDF
M5-732-SDF
M5-733-SDF
M5-734-SDF
M5-735-SDF
M5-738-SDF
M5-740-SDF
M5-741-SDF
M5-742-SDF
M5-743-SDF
M5-744-SDF
Collection
Date
09/26/99
09/26/99
09/27/99
09/26/99
09/26/99
09/26/99
09/26/99
09/26/99
09/25/99
09/25/99
09/26/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/26/99
09/25/99
09/25/99
09/25/99
09/26/99
09/25/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/23/99
09/24/99
09/24/99
09/24/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/22/99
09/23/99
09/23/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
Collection
Time
1213
1335
900
1410
1615
850
1530
1434
915
1035
1527
1205
1350
1554
1200
1139
1702
1400
1510
1637
1030
1635
1750
1740
918
1655
1615
1725
1555
1500
900
1330
900
1330
1430
1115
905
1715
1145
1310
1030
1715
0
1600
1500
1442
1323
1230
1216
1350
1027
1120
1725
917
910
1540
1700
1410
1245
1534
1418
1130
1224
Digestion
Date
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/13/99
2/14/99
2/14/99
2/14/99
2/14/99
2/14/99
2/14/99
2/14/99
2/14/99
2/14/99
2/14/99
2/14/99
2/14/99
2/14/99
2/14/99
2/15/99
2/14/99
2/14/99
2/14/99
2/14/99
2/15/99
2/14/99
2/14/99
2/15/99
Hold Time
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
Time Since
Digestion
78
78
77
78
78
78
78
78
79
79
78
79
79
79
79
79
79
79
79
78
79
79
79
78
79
80
80
80
80
80
80
80
80
80
80
80
80
81
80
80
81
82
82
82
82
82
82
82
82
82
82
82
83
82
83
83
83
83
83
84
83
83
84
Technician
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
SLH/JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
Vial
Weight
(g)
1.0054
1.001
1.003
0.9994
1.006
.0062
.0088
.0074
.0068
.0087
.0116
1.013
.0104
.0141
.0156
.0204
.0213
0.9956
0.9917
0.9943
0.9993
0.9962
0.9998
.0216
.0195
.0196
.0208
.0217
.0217
.0193
.0147
.0139
.0145
.0179
.0077
.0086
.0158
.0136
.0098
.0087
.0095
.0134
.0152
.0181
.0206
.0269
.0302
.0304
.0312
.0279
.0239
.0229
0.9909
0.9889
0.9923
0.9872
0.988
1.0042
1.0026
0.9904
0.9919
0.9957
0.987
Sample Weight
(g)
0.0252
0.0248
0.0249
0.0255
0.0255
0.0248
0.0258
0.0249
0.0257
0.0246
0.0254
0.025
0.0257
0.0247
0.0247
0.0259
0.0245
0.0255
0.0257
0.0245
0.0251
0.0251
0.0251
0.0254
0.0254
0.0251
0.0246
0.0257
0.0253
0.0246
0.0253
0.0256
0.0247
0.0254
0.0253
0.0246
0.025
0.0253
0.0248
0.0246
0.0248
0.0255
0.0246
0.025
0.0255
0.0247
0.0251
0.0254
0.0246
0.0253
0.0247
0.0255
0.0256
0.0253
0.0245
0.0257
0.0252
0.025
0.0251
0.0248
0.0254
0.025
0.0252
Dried Cup +
Sed (g)
1.0073
1.0045
1.0057
1.004
1.0122
1.009
1.0137
1.0092
1.0095
1.0108
1.0131
1.0174
1.0129
1.0156
1.0177
1.0255
1.0233
1.005
0.9951
0.9977
1.0016
0.9991
1.0044
1.0251
1.0338
1.0372
1.032
1.0244
1.0386
1.0324
1.0202
1.0327
1.0212
1.0365
1.0244
1.014
1.0321
1.0275
1.0265
1.0167
1.0263
1.0284
1.0297
1.0335
1.0394
1.0323
1.0444
1.0343
1.0476
1.0439
1.0388
1.0255
1.0071
0.9968
1.0059
0.9953
1.0057
1.0171
1.019
1.0074
1.0116
1.0124
0.9941
Ashed Sed.
(g)
0.0019
0.0035
0.0027
0.0046
0.0062
0.0028
0.0049
0.0018
0.0027
0.0021
0.0015
0.0044
0.0025
0.0015
0.0021
0.0051
0.0020
0.0094
0.0034
0.0034
0.0023
0.0029
0.0046
0.0035
0.0143
0.0176
0.0112
0.0027
0.0169
0.0131
0.0055
0.0188
0.0067
0.0186
0.0167
0.0054
0.0163
0.0139
0.0167
0.0080
0.0168
0.0150
0.0145
0.0154
0.0188
0.0054
0.0142
0.0039
0.0164
0.0160
0.0149
0.0026
0.0162
0.0079
0.0136
0.0081
0.0177
0.0129
0.0164
0.0170
0.0197
0.0167
0.0071
Mineral
Content
(Fraction)
0.0754
0.1411
0.1084
0.1804
0.2431
0.1129
0.1899
0.0723
0.1051
0.0854
0.0591
0.1760
0.0973
0.0607
0.0850
0.1969
0.0816
0.3686
0.1323
0.1388
0.0916
0.1155
0.1833
0.1378
0.5630
0.7012
0.4553
0.1051
0.6680
0.5325
0.2174
0.7344
0.2713
0.7323
0.6601
0.2195
0.6520
0.5494
0.6734
0.3252
0.6774
0.5882
0.5894
0.6160
0.7373
0.2186
0.5657
0.1535
0.6667
0.6324
0.6032
0.1020
0.6328
0.3123
0.5551
0.3152
0.7024
0.5160
0.6534
0.6855
0.7756
0.6680
0.2817
% Mineral
Content
7.5
14.1
10.8
18.0
24.3
11.3
19.0
7.2
10.5
8.5
5.9
17.6
9.7
6.1
8.5
19.7
8.2
36.9
13.2
13.9
9.2
11.6
18.3
13.8
56.3
70.1
45.5
10.5
66.8
53.3
21.7
73.4
27.1
73.2
66.0
22.0
65.2
54.9
67.3
32.5
67.7
58.8
58.9
61.6
73.7
21.9
56.6
15.4
66.7
63.2
60.3
10.2
63.3
31.2
55.5
31.5
70.2
51.6
65.3
68.5
77.6
66.8
28.2
Ash Free
Dry
Weight
0.9246
0.8589
0.8916
0.8196
0.7569
0.8871
0.8101
0.9277
0.8949
0.9146
0.9409
0.8240
0.9027
0.9393
0.9150
0.8031
0.9184
0.6314
0.8677
0.8612
0.9084
0.8845
0.8167
0.8622
0.4370
0.2988
0.5447
0.8949
0.3320
0.4675
0.7826
0.2656
0.7287
0.2677
0.3399
0.7805
0.3480
0.4506
0.3266
0.6748
0.3226
0.4118
0.4106
0.3840
0.2627
0.7814
0.4343
0.8465
0.3333
0.3676
0.3968
0.8980
0.3672
0.6877
0.4449
0.6848
0.2976
0.4840
0.3466
0.3145
0.2244
0.3320
0.7183
% Ash Free Dry
Weight Content
92.5
85.9
89.2
82.0
75.7
88.7
81.0
92.8
89.5
91.5
94.1
82.4
90.3
93.9
91.5
80.3
91.8
63.1
86.8
86.1
90.8
88.4
81.7
86.2
43.7
29.9
54.5
89.5
33.2
46.7
78.3
26.6
72.9
26.8
34.0
78.0
34.8
45.1
32.7
67.5
32.3
41.2
41.1
38.4
26.3
78.1
43.4
84.6
33.3
36.8
39.7
89.8
36.7
68.8
44.5
68.5
29.8
48.4
34.7
31.5
22.4
33.2
71.8
-------
Sample ID
M5-745-SDF
M5-746-SDF
M5-747-SDF
M5-823-SDF
M5-828-SDF
M5-838-SDF
M5-848-SDF
M5-859-SDF
M5-868-SDF
M5-878-SDF
M5-890-SDF
M5-908-SDF
M5-920-SDF
M5-932-SDF
M5-944-SDF
Collection
Date
09/22/99
09/22/99
09/22/99
09/30/99
09/29/99
09/29/99
09/28/99
09/28/99
09/27/99
09/26/99
09/25/99
09/24/99
09/23/99
09/23/99
09/22/99
Collection
Time
1120
948
942
0
0
0
0
0
0
0
0
0
0
0
1224
Digestion
Date
2/15/99
2/14/99
2/14/99
2/14/99
2/15/99
2/14/99
2/14/99
2/14/99
2/14/99
2/14/99
2/15/99
2/14/99
2/14/99
2/15/99
2/14/99
Hold Time
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
Time Since
Digestion
84
83
83
75
77
76
77
77
78
79
81
81
82
83
83
Technician
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
JL
Vial
Weight
(g)
0.9821
1.0016
1.0022
1.0002
0.9842
1.0004
0.9988
0.9994
1.0013
0.9835
0.9859
0.9869
0.9891
0.9881
1.0031
Sample Weight
(g)
0.025
0.0253
0.0256
0.0252
0.0254
0.0257
0.025
0.0256
0.0254
0.0253
0.0253
0.0257
0.0254
0.0255
0.0249
Dried Cup +
Sed (g)
0.9981
1.0163
1.0226
1.0023
0.9856
1.005
1.0016
1.0044
1.0038
0.9851
0.9882
0.9933
1.002
0.9955
1.0085
Ashed Sed.
(g)
0.0160
0.0147
0.0204
0.0021
0.0014
0.0046
0.0028
0.0050
0.0025
0.0016
0.0023
0.0064
0.0129
0.0074
0.0054
Mineral
Content
(Fraction)
0.6400
0.5810
0.7969
0.0833
0.0551
0.1790
0.1120
0.1953
0.0984
0.0632
0.0909
0.2490
0.5079
0.2902
0.2169
% Mineral
Content
64.0
58.1
79.7
8.3
5.5
17.9
11.2
19.5
9.8
6.3
9.1
24.9
50.8
29.0
21.7
Ash Free
Dry
Weight
0.3600
0.4190
0.2031
0.9167
0.9449
0.8210
0.8880
0.8047
0.9016
0.9368
0.9091
0.7510
0.4921
0.7098
0.7831
% Ash Free Dry
Weight Content
36.0
41.9
20.3
91.7
94.5
82.1
88.8
80.5
90.2
93.7
90.9
75.1
49.2
71.0
78.3
R:\wp_files\2110-247Veport\pdf\Final Draft\Appendix QSeptember 1999 DR\[afdw-bd.xls]AFDW SOIL
-------
 10 % Recalculated Results for Methylmercury in Soil Samples Analyzed by
Florida International University Laboratory for the September 1999 Wet Season (M5)
Entered by mwb 4-11 -00
Sampling Station
ID
M5-622-SDF-A
M5-622-SDF-B
M5-622-SDF-C
M5-622-SDF-D

Blank-1
Blank-2
ccv

M5-633-SDF-A
M5-633-SDF-B
M5-633-SDF-C
M5-633-SDF-D

Blank-1
Blank-2
ccv
ccv

M5-643-SDF-A
M5-643-SDF-B
M5-643-SDF-C
M5-643-SDF-D

Blank-1
Blank-2
ccv

Data Qualifier
Note











"M"
M"








"M"
M'





QC
Batch
022100a
0221 OOa
0221 OOa
0221 OOa

0221 OOa
0221 OOa
0221 OOa

032000b
032000b
032000b
032000b

032000b
032000b
032000b
032000b

0221 OOb
0221 OOb
0221 OOb
0221 OOb

0221 OOb
0221 OOb
0221 OOb

Wet
Sample
Weight (g)
4.495
4.606
4.538
4.317





4.537
4.922
4.963
4.842






5.477
4.590
4.550
4.760





Diy/Wet
Weight
Ratio
0.021
0.021
0.021
0.021





0.123
0.123
0.123
0.123






0.250
0.250
0.250
0.250





First
Extraction
Volume(ml)
4.2
4.2
4.2
4.2

3.8
4.0


3.4
3.6
3.6
4.0

4.0
4.0



3.2
3.0
3.0
3.0

3.0
4.0


Back
Extraction
Volume(ml)
0.6
0.6
0.6
0.6

0.8
0.8


0.6
0.6
0.6
0.6

0.6
0.6



0.6
0.6
0.6
0.6

0.6
0.6


Final
Extraction
Volume(ul)
200
200
200
200

200
200


200
200
200
200

200
200



200
200
200
200

200
200


Spiked
Concentration
(ng/g)


7.87
8.27



2.50



1.23
1.26



3.75
3.75



0.66
0.63



2.50

MeHg
Peak
Area
7.70
9.92
11.05
14.34

0.00
0.00
6.880


12.76
15.07
15.76

0.00
0.00
6.590
7.740

14.80
12.96
16.67
19.58

0.00
0.00
10.04

Y intercept
0.62
0.62
0.62
0.62

0.62
0.62
0.62

0.50
0.50
0.50
0.50

0.50
0.50
0.50
0.50

0.61
0.61
0.61
0.61

0.61
0.61
0.61

Slope
2.36
2.36
2.36
2.36

2.36
2.36
2.36

2.44
2.44
2.44
2.44

2.44
2.44
2.44
2.44

3.20
3.20
3.20
3.20

3.20
3.20
3.20

MeHg
Concentration
(ng/g)
13.72
17.24
19.50
26.60

0.00
0.00
2.92

0.00
4.00
4.68
4.52

0.00
0.00
2.70
3.17

1.76
1.96
2.54
2.86



3.14

AVE
MeHg Cone.
(ng/g)

15.48

23.05






4.00

4.60







1.86

2.70





%RPD

-22.8

-30.8






NA

3.6







-10.8

-11.6





MR


73.45
113.09



116.61



NA
48.38



72.02
84.59



118.94
142.19



125.50

AVE
%R



93.27








48.38









130.56





Final
Result
ng/g



16.60








8.27









1.42





Data Qualifiers
"R2" Correlation Coefficient is out of QAPP limits.
"M" Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B" Analyte concentration in the associated blank was >3 times the MDL.
"H" Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
 10 % Recalculated Results for Methylmercury in Soil Samples Analyzed by
Florida International University Laboratory for the September 1999 Wet Season (M5)
Entered by mwb 02/02/00
Sampling Station
ID
M5-653-SDF-A
M5-653-SDF-B
M5-653-SDF-C
M5-653-SDF-D

Blank-1
Blank-2
ccv

M5-663-SDF-A
M5-663-SDF-B
M5-663-SDF-C
M5-663-SDF-D

Blank-1
Blank-2
ccv
ccv

M5-673-SDF-A
M5-673-SDF-B
M5-673-SDF-C
M5-673-SDF-D

Blank-1
Blank-2
ccv
ccv

M5-683-SDF-A
M5-683-SDF-B
M5-683-SDF-C
M5-683-SDF-D

Blank-1
Blank-2
ccv

Data Qualifier
Note







"DQO (KR)11



"M"
M"








"M"
M'




"DQO"



"M"
M'



"DQO11

QC
Batch
22800
22800
22800
22800

22800
22800
22800

022500b
022500b
022500b
022500b

022500b
022500b
022500b
022500b

0221 OOa
0221 OOa
0221 OOa
0221 OOa

0221 OOa
0221 OOa
0221 OOa
0221 OOa

30300a
30300a
30300a
30300a

30300a
30300a
30300a

Wet
Sample
Weight (g)
6.060
5.583
6.381
5.437





5.209
4.609
5.109
4.830






5.076
4.834
4.997
5.058






5.186
4.518
4.524
5.182





Diy/Wet
Weight
Ratio
0.447
0.447
0.447
0.447





0.125
0.125
0.125
0.125






0.202
0.202
0.202
0.202






0.0868
0.0868
0.0868
0.0868





First
Extraction
Volume(ml)
2.6
2.6
2.8
2 2

4.0
4.0


3.8
4.0
4.0
3.2

3.8
4.0



4.0
4.2
4.0
3.6

4.4
4.0



4.0
3.2
4.0
4.0

3.2
4.0


Back
Extraction
Volume(ml)
0.6
0.6
0.6
0.6

0.6
0.6


0.6
0.6
0.6
0.6

0.6
0.6



0.6
0.6
0.6
0.6

0.6
0.6



0.6
0.6
0.6
0.6

0.6
0.6


Final
Extraction
Volume(ul)
200
200
200
200

200
200


200
200
200
200

200
200



200
200
200
200

200
200



200
200
200
200

200
200


Spiked
Concentration
(ng/g)


0.26
0.31







1.17
1.24



2.50
2.50



0.74
0.73



2.50
2.50



1.91
1.67



2.50

MeHg
Peak
Area

2.17
9.87
6.94

0.00
0.00


6.77
5.78
8.33
6.97

0.00
0.00
8.480
7.050

6.97
6.52
8.13
7.41

0.00
0.00
6.060
6.880

1.54
0.84
7.60
7.58

0.00
0.00
9.310

Y intercept
-0.02
-0.02
-0.02
-0.02

-0.02
-0.02


0.13
0.13
0.13
0.13

0.13
0.13
0.13
0.13

0.52
0.52
0.52
0.52

0.52
0.52
0.52
0.52

0.45
0.45
0.45
0.45

0.45
0.45
0.45

Slope
5.90
5.90
5.90
5.90

5.90
5.90


3.02
3.02
3.02
3.02

3.02
3.02
3.02
3.02

1.99
1.99
1.99
1.99

1.99
1.99
1.99
1.99

2.66
2.66
2.66
2.66

2.66
2.66
2.66

MeHg
Concentration
(ng/g)
0.00
0.09
0.35
0.37

0.00
0.00


1.51
1.38
1.80
1.99

0.00
0.00
2.81
2.33

1.42
1.33
1.69
1.69

0.00
0.00
3.05
3.46

0.54
0.42
3.03
2.64

0.00
0.00
3.50



0.09

0.36






1.45

1.90







1.38

1.69







0.48

2.84





%RPD

NA

-4.9






8.7

-10.1







6.7

0.0







24.4

13.8





%R


NA
87.80







24.75
48.94



112.32
93.38



35.56
48.74



121.81
138.29



130.67
132.95



140.00

AVE
%R



87.80








36.84









42.15









131.81





Final
Result
ng'g



0.11








3.93









3.27









0.36





Data Qualifiers
"R2" Correlation Coefficient is out of QAPP limits.
"M" Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B" Analyte concentration in the associated blank was >3 times the MDL.
"H" Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
 10 % Recalculated Results for Methylmercury in Soil Samples Analyzed by
Florida International University Laboratory for the September 1999 Wet Season (M5)
Entered by mwb 4-11 -00
Sampling Station
ID
M5-693-SDF-A
M5-693-SDF-B
M5-693-SDF-C
M5-693-SDF-D

Blank-1
Blank-2
ccv

M5-703-SDF-A
M5-703-SDF-B
M5-703-SDF-C
M5-703-SDF-D

Blank-1
Blank-2
ccv
ccv

M5-714-SDF-A
M5-714-SDF-B
M5-714-SDF-C
M5-714-SDF-D

Blank-1
Blank-2
ccv

Data Qualifier
Note

"DQO"
"M"
"M"



"DQO"


"DQO"

"M"



"DQO (KR)11
"DQO (KR)11



"M"
"M"



"DQO (KR)11

QC
Batch
30300b
30300b
30300b
30300b

30300b
30300b
30300b

030700a
030700a
030700a
030700a

030700a
030700a
030700a
030700a

032300a
032300a
032300a
032300a

032300a
032300a
032300a

Wet
Sample
Weight (g)
5.279
4.996
5.201
5.347





5.368
5.250
5.548
5.521






4.908
4.629
4.865
5.835





Dry/Wet
Weight
Ratio
0.0876
0.0876
0.0876
0.0876





0.213
0.213
0.213
0.213






0.186
0.186
0.186
0.186





First
Extraction
Volume(ml)
3.2
3.0
3.2
3.2

3.2
4.0


2.0
2.0
2.0
1.6

4.0
4.0



3.4
3.4
3.4
3.4

4.0
4.0


Back
Extraction
Volume(ml)
0.6
0.6
0.6
0.6

0.6
0.6


0.6
0.6
0.6
0.6

0.6
0.6



0.6
0.6
0.6
0.6

0.8
0.8


Final
Extraction
Volume(ul)
200
200
200
200

200
200


200
200
200
200

200
200



200
200
200
200

200
200


Spiked
Concentration
(ng/g)


1.65
1.60



2.50



0.63
0.64








0.83
0.69





MeHg
Peak
Area
0.52
0.74
8.71
8.39

0.00
0.00
9.400

1.50
1.02
4.40
4.05

0.00
0.00



1.36
1.47
5.17
5.70

0.00
0.00


Y intercept
.39
.39
.39
.39

.39
.39
.39

0.21
0.21
0.21
0.21

0.50
0.50



-0.07
-0.07
-0.07
-0.07

-0.07
-0.07


Slope
2.59
2.59
2.59
2.59

2.59
2.59
2.59

2.66
2.66
2.66
2.66

2.44
2.44



.71
.71
.71
.71

.71
.71


MeHg
Concentration
(ng/g)
0.23
0.36
3.84
3.60

0.00
0.00
3.63

0.41
0.29
1.17
1.35

0.00
0.00



0.43
0.49
1.64
1.51





AVE
MeHg Cone.
(ng/g)

0.29

3.72






0.35

1.26







0.46

1.57





%RPD

-46.4

6.5






35.9

-14.5







-13.6

8.4





«


219.29
202.46



145.17



119.92
166.08








145.88
147.26





AVE
%R



210.87








143.00









146.57





Final
Result
ng/g



0.14








0.24









0.31





Data Qualifiers
"R2" Correlation Coefficient is out of QAPP limits.
"M" Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B" Analyte concentration in the associated blank was >3 times the MDL.
"H" Analysis digestion performed after holding times have expired.
"MR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
 10 % Recalculated Results for Methylmercury in Soil Samples Analyzed by
Florida International University Laboratory for the September 1999 Wet Season (M5)
Entered by mwb 02/02/00
Sampling Station
ID
M5-726-SDF-A
M5-726-SDF-B
M5-726-SDF-C
M5-726-SDF-D

Blank-1
Blank-2
ccv
ccv

M5-738-SDF-A
M5-738-SDF-B
M5-738-SDF-C
M5-738-SDF-D

Blank-1
Blank-2
ccv
ccv

M5-828-SDF-A
M5-828-SDF-B
M5-828-SDF-C
M5-828-SDF-D

Blank-1
Blank-2
ccv
ccv

M5-944-SDF-A
M5-944-SDF-B
M5-944-SDF-C
M5-944-SDF-D

Blank-1
Blank-2
ccv

Data Qualifier
Note


"M"
"M"













"DQO"
"DQO"



"M"
"M"







"DQO"
"M"
"M"



"DQO11

QC
Batch
30800
30800
30800
30800

30800
30800
30800
30800

022500b
022500b
022500b
022500b

022500b
022500b
022500b
022500b

040400b
040400b
040400b
040400b

040400b
040400b
040400b
040400b

31000
31000
31000
31000

31000
31000
31000

Wet
Sample
Weight (g)
5.183
4.935
5.010
4.804






5.101
5.139
5.038
5.370






5.022

5.030







4.386
4.482
5.594
5.626





Diy/Wet
Weight
Ratio
0.0819
0.0819
0.0819
0.0819






0.2806
0.2806
0.2806
0.2806






0.0453

0.0453







0.0785
0.0785
0.0785
0.0785





First
Extraction
Volume(ml)
4.2
4.0
4.2
4.2

4.0
4.0



3.6
4.2
4.2
4.2

3.8
4.0



4.0

4.0


4.0
4.0



4.0
4.0
4.0
4.0

3.2
4.0


Back
Extraction
Volume(ml)
0.6
0.6
0.6
0.6

0.6
0.6



0.6
0.6
0.6
0.6

0.6
0.6



0.6

0.6


0.6
0.6



0.6
0.6
0.6
0.6

0.6
0.6


Final
Extraction
Volume(ul)
200
200
200
200

200
200



200
200
200
200

200
200



200

200


200
200



200
200
200
200

200
200


Spiked
Concentration
(ng/g)


1.83
1.91



2.50
2.50



0.53
0.50



2.50
2.50



3.29




2.50
2.50



1.71
1.70



2.50

MeHg
Peak
Area
2.36
1.93
7.88
7.45

0.00
0.00
6.210
6.240


2.08
6.01
6.59

0.00
0.00
8.480
7.050

5.66

8.36


0.00
0.00
6.310
5.700

1 .88
0.40
5.69
6.85

0.00
0.00
9.310

Y intercept
0.11
0.11
0.11
0.11

0.11
0.11
0.13
0.13

0.27
0.27
0.27
0.27

0.27
0.27
0.27
0.27

0.39

0.39


0.52
0.52
0.52
0.52

0.61
0.61
0.61
0.61

0.61
0.61
0.61

Slope
2.24
2.24
2.24
2.24

2.24
2.24
3.02
3.02

2.04
2.04
2.04
2.04

2.04
2.04
2.04
2.04

2.21

2.21


1.99
1.99
1.99
1.99

1.94
1.94
1.94
1.94

1.94
1.94
1.94

MeHg
Concentration
(ng/g)
0.98
0.89
3.40
3.35

0.00
0.00
2.06
2.07

0.00
0.28
0.83
0.85

0.00
0.00
4.16
3.46

4.69

6.92


0.00
0.00
3.17
2.86

1.17
0.24
2.78
3.33

0.00
0.00
4.80



0.94

3.38







0.28

0.84

















0.71

3.06





%RPD

10.3

1.4







"NA"

-2.8

















131.1

-17.9





MR


132.09
129.12



82.25
82.65



"NA"
114.03



166.27
138.24



67.68




126.83
114.57



94.16
181.59



191.96

AVE
%R



130.61









114.03



















137.88





Final
Result
ng'g



0.72









0.25








6.93










0.51





Data Qualifiers
"R2" Correlation Coefficient is out of QAPP limits.
"M" Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B" Analyte concentration in the associated blank was >3 times the MDL.
"H" Analysis digestion performed after holding times have expired.
"MR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
SERC Mercury Lab / EPA REMAP results
Methyl Mercury Analysis
: Analysis not performed
: Analysis not required
: Averaged Results
     Data Entered by: MWB  3-30-00
Data Entry Checked by: NJS 4-7-00
Sampling Station
ID
M5-622-SDF
M5-623-SDF
M5-624-SDF
M5-625-SDF
M5-626-SDF
M5-627-SDF
M5-628-SDF
M5-628-SDF
QA-630-SDF
M5-631-SDF
M5-632-SDF
M5-633-SDF
QA-634-SDF
M5-635-SDF
QA-636-SDF
M5-637-SDF
M5-638-SDF
M5-639-SDF
M5-640-SDF
M5-641-SDF
M5-642-SDF
M5-643-SDF
M5-644-SDF
QA-645-SDF
M5-646-SDF
M5-647-SDF
M5-648-SDF
M5-649-SDF
M5-650-SDF
QA-651-SDF
QA-652-SDF
M5-653-SDF
M5-654-SDF
M5-655-SDF
M5-656-SDF
M5-657-SDF
M5-658-SDF
M5-659-SDF
M5-660-SDF
M5-661-SDF
M5-662-SDF
M5-663-SDF
M5-664-SDF
M5-665-SDF
M5-666-SDF
M5-667-SDF
M5-668-SDF
M5-669-SDF
M5-670-SDF
QA-671-SDF
M5-672-SDF
M5-673-SDF
M5-674-SDF
M5-675-SDF
M5-676-SDF
M5-677-SDF
M5-678-SDF
M5-679-SDF
M5-680-SDF
M5-681-SDF
QA-682-SDF
M5-683-SDF
M5-684-SDF
M5-685-SDF
M5-686-SDF
M5-687-SDF
M5-688-SDF
M5-689-SDF
M5-690-SDF
M5-691-SDF
Matrix
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
Analysis
Method






































































Collection
Date
09/30/99
09/30/99
09/30/99
09/30/99
09/30/99
09/30/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/28/99
09/29/99
09/28/99
09/29/99
09/29/99
09/30/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/27/99
09/28/99
09/27/99
09/27/99
09/29/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/26/99
09/27/99
09/27/99
09/26/99
09/26/99
09/28/99
09/26/99
09/26/99
09/26/99
09/27/99
09/26/99

09/26/99
09/26/99
09/26/99
09/25/99
09/25/99
09/26/99
09/25/99
09/25/99
09/25/99
Time
1125
915
1018
1257
908
1050
1716
1716

1414
1010
1115

1216

1210
1630
1715
1116
1615
1011
910
1145

1515
1102
1300
1620
1158


1300
1145
1028
900
1751
1722
1205
1450
857
1610
1330
1100
1710
1655
1545
1207
1000
850

1100
1400
1025
1130
925
1310
1213
1335
900
1410

850
1530
1434
915
1035
1527
1205
1350
1554
Digestion
Date
02/21/00
02/21/00
02/21/00
02/21/00
02/21/00
02/21/00
02/21/00
04/04/00

02/21/00
02/21/00
03/20/00

02/21/00

02/21/00
04/04/00
02/21/00
02/21/00
02/21/00
02/21/00
02/21/00
02/21/00

02/25/00
03/20/00
02/28/00
03/20/00
02/28/00


02/28/00
02/28/00
02/29/00
02/29/00
03/20/00
02/29/00
02/29/00
02/29/00
02/29/00
02/29/00
02/29/00
02/29/00
03/02/00
03/02/00
03/02/00
03/02/00
03/02/00
04/04/00

03/02/00
03/02/00
03/02/00
03/02/00
03/02/00
03/20/00
03/03/00
03/03/00
03/03/00
03/03/00
03/24/00
03/03/00
03/03/00
03/03/00
03/03/00
03/03/00
03/03/00
03/03/00
03/03/00
03/03/00
Run
Date
02/21/00
02/21/00
02/21/00
02/21/00
02/21/00
02/21/00
02/21/00
04/04/00

02/21/00
02/21/00
03/20/00

02/21/00

02/21/00
04/04/00
02/21/00
02/21/00
02/21/00
02/21/00
02/21/00
02/21/00

02/25/00
03/20/00
02/28/00
03/20/00
02/28/00


02/28/00
02/28/00
02/29/00
02/29/00
03/20/00
02/29/00
02/29/00
02/29/00
02/29/00
02/29/00
02/29/00
02/29/00
03/02/00
03/02/00
03/02/00
03/02/00
03/02/00
04/04/00

03/02/00
03/02/00
03/02/00
03/02/00
03/02/00
03/20/00
03/03/00
03/03/00
03/03/00
03/03/00
03/24/00
03/03/00
03/03/00
03/03/00
03/03/00
03/03/00
03/03/00
03/03/00
03/03/00
03/03/00
Holding
Time (Days)
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
Time Elapsed
From Dig
144
144
144
144
144
144
145
188

145
145
173

145

145
188
146
145
146
145
145
144

150
174
153
174
153


153
153
154
154
175
154
155
155
153
155
155
155
157
157
157
157
157
190

157
157
158
158
156
176
159
159
158
159

159
159
159
160
160
159
160
160
160
MeHg
Units (ng/g)
16.51
1.46
7.11
0.33
12.80
2.46
10.73
8.81
0.39
0.73
41.75
8.20
1.36
8.57
0.00
1.71
19.72
4.30
7.17
6.45
0.23
1.43
24.05
0.00
4.10
3.73
3.1
6.9
0.86
1.16
2.67
0.10
4.21
1.58
2.73
3.63
0.00
4.15
1.67
0.23
0.15
3.90
5.52
0.27
3.77
4.37
0.57
0.39
0.00
2.42
2.55
3.29
0.00
5.50
0.34
4.16
0.40
0.16
0.81
0.59
0.23
0.36
0.32
0.25
0.00
0.67
0.94
0.33
0.11
0.52
QA/QC
Batch ID
022100a
022100a
0221003
0221003
0221003
0221003
0221003
040400b
31500
0221003
0221003
032000b
31500
022100b
31500
022100b
040400b
022100b
022100b
022100b
022100b
022100b
022100b
31500
022500b
032000b
22800
032000b
22800
31500
31500
22800
22800
22900
22900
032000b
22900
22900
22900
22900
22900
22900
22900
30200
30200
30200
30200
30200
040400b
31500
30200
30200
30200
30200
30200
032000b
303003
303003
303003
303003
0324003
303003
303003
303003
303003
303003
30300b
30300b
30300b
30300b
QA Data
%R






































































%RPD
22.8
51.7
6.4
40.0
21.0
27.2
10.6
NA
2.4
38.5
4.4
NA
29.1
5.1
0.0
1.7
NA
2.5
12.6
7.5
NA
10.8
0.22
0.0
9.6
36.0
31
15.5
NA
28.0
0.9
NA
7.9
20.7
17.5
5.2
0.0
6.1
0.5
24.1
5.0
9.0
20.0
38.6
16.0
20.8
35.6
7.6
NA
51.6
14.8
6.5
0.0
17.1
34.6
35.7
48.9
NA
44.6
NA
NA
25.0
0.0
17.4
0.0
4.7
NA
0.0
NA
NA
Matrix %R
93.6
157.6
115.1
167.7
102.7
132.5
76.9
68.36
107.6
131.6
67.87
48.7
116.4
79.7
115.2
102.1
71.61
84.1
115.2
47.31
140.8
130.2
38.01
105.2
144.3
86.45
122.2
108.89
204.5
86.2
85
93.65
117.9
57.8
97.9
84.64
126.19
51.67
121.3
127.4
134.1
37.1
30.9
160.5
74.7
59.6
127.8
135.8
87.71
101.5
90.4
41.9
136.01
79.7
155.5
110.95
116.8
176.7
125.2
54.6
78.1
132.1
126.1
91.3
141
129.4
129.2
170.7
141
167.7

Notes






































































-------
M5-692-SDF
M5-693-SDF
M5-694-SDF
M5-695-SDF
QA-696-SDF
M5-697-SDF
QA-698-SDF
M5-699-SDF
M5-700-SDF
M5-701-SDF
M5-702-SDF
M5-703-SDF
M5-704-SDF
M5-705-SDF
M5-706-SDF
M5-707-SDF
M5-708-SDF
M5-709-SDF
QA-710-SDF
M5-711-SDF
M5-712-SDF
M5-714-SDF
M5-715-SDF
M5-716-SDF
M5-718-SDF
QA-719-SDF
M5-720-SDF
M5-722-SDF
M5-723-SDF
M5-724-SDF
M5-725-SDF
M5-726-SDF
M5-727-SDF
M5-728-SDF
M5-729-SDF
M5-730-SDF
M5-731-SDF
M5-732-SDF
M5-733-SDF
M5-734-SDF
M5-735-SDF
M5-738-SDF
M5-740-SDF
M5-741-SDF
M5-742-SDF
M5-743-SDF
M5-744-SDF
M5-745-SDF
M5-746-SDF
M5-747-SDF
M5-823-SDF
M5-828-SDF
M5-838-SDF
M5-848-SDF
M5-859-SDF
M5-868-SDF
M5-878-SDF
M5-890-SDF
M5-908-SDF
M5-920-SDF
M5-932-SDF
M5-944-SDF

M5-639-FCF
M5-640-FCF
M5-656-FCF
M5-666-FCF
M5-681-FCF
M5-683-FCF
M5-698-FCF
M5-699-FCF
M5-700-FCF
M5-712-FCF
M5-726-FCF

M5-729-PSF
M5-731-PSF
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD

FC
FC
FC
FC
FC
FC
FC
FC
FC
FC
FC

PS
PS













































































09/25/99
09/25/99
09/25/99
09/25/99
09/25/99
09/26/99
09/25/99
09/25/99
09/25/99
09/26/99
09/25/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99

09/24/99
09/24/99
09/23/99
09/24/99
09/24/99
09/24/99

09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/22/99
09/23/99
09/23/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/30/99
09/28/99
09/29/99
09/28/99
09/27/99
09/27/99
09/26/99
09/25/99
09/24/99
09/23/99
09/23/99
09/22/99

09/28/99
09/29/99
09/28/99
09/27/99
09/26/99
09/26/99

09/25/99
09/25/99
09/24/99
09/23/99

09/23/99
09/22/99
1200
1139
1702
1400

1637

1635
1750
1740
918
1655
1615
1725
1555
1500
900
1330

1115
905
1715
1145
1310
1030

0
1600
1500
1442
1323
1230
1216
1350
1027
1120
1725
917
910
1540
1700
1410
1245
1534
1418
1130
1224
1120
948
942
0

0
0
0
0
0
0
0
0
0
1224






850



905
1230



03/03/00
03/03/00
03/03/00
03/03/00

03/03/00

03/03/00
03/07/00
03/07/00
03/07/00
03/07/00
03/07/00
03/07/00
03/07/00
03/20/00
03/07/00
03/07/00
03/24/00
03/07/00
03/23/00
03/23/00
03/07/00
03/23/00
03/07/00
03/24/00
03/07/00
03/07/00
03/07/00
03/07/00
03/08/00
03/08/00
03/08/00
03/08/00
03/08/00
03/08/00
03/23/00
03/08/00
03/08/00
03/08/00
03/09/00
03/09/00
03/09/00
03/09/00
03/09/00
03/09/00
03/09/00
03/09/00
03/09/00
03/09/00
02/21/00
04/04/00
02/21/00
02/21/00
02/21/00
03/10/00
03/10/00
03/10/00
03/10/00
03/10/00
03/10/00
03/10/00

03/23/00
03/23/00
03/23/00
03/23/00
03/23/00
02/25/00
03/23/00
03/23/00
03/23/00
02/25/00
02/25/00

03/30/00
03/30/00
03/03/00
03/03/00
03/03/00
03/03/00

03/03/00

03/03/00
03/07/00
03/07/00
03/07/00
03/07/00
03/07/00
03/07/00
03/07/00
03/20/00
03/07/00
03/07/00
03/24/00
03/07/00
03/23/00
03/23/00
03/07/00
03/23/00
03/07/00
03/24/00
03/07/00
03/07/00
03/07/00
03/07/00
03/08/00
03/08/00
03/08/00
03/08/00
03/08/00
03/08/00
03/23/00
03/08/00
03/08/00
03/08/00
03/09/00
03/09/00
03/09/00
03/09/00
03/09/00
03/09/00
03/09/00
03/09/00
03/09/00
03/09/00
02/21/00
04/04/00
02/21/00
02/21/00
02/21/00
03/10/00
03/10/00
03/10/00
03/10/00
03/10/00
03/10/00
03/10/00

03/23/00
03/23/00
03/23/00
03/23/00
03/23/00
02/25/00
03/23/00
03/23/00
03/23/00
02/25/00
02/25/00

03/30/00
03/30/00
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28

28
28
28
28
28
28
28
28
28
28
28

28
28
160
160
160
160

159

160
164
163
164
165
165
165
165
178
165
165

165
181
182
165
181
165

166
166
166
166
167
167
167
167
167
167
183
167
167
168
169
169
169
169
169
169
169
169
169
169
144
189
145
146
147
165
166
167
168
169
169
170

177
176
177
178
179
152
36608
180
180
154
155

189
190
1.03
0.14
0.57
0.26
0.44
0.27
1.13
0.55
0.36
0.08
0.09
0.24
0.21
0.84
0.06
0.67
0.20
0.08
0.15
0.00
0.00
0.31
0.13
0.41
0.12
0.38
0.00
0.00
0.00
0.57
0.06
0.72
0.09
0.16
0.19
2.31
0.00
0.58
0.17
0.70
0.13
0.26
0.10
0.00
0.12
0.11
0.66
0.28
0.12
0.00
0.88
6.95
4.65
7.34
7.40
0.18
0.71
0.23
0.27
0.00
0.49
0.51

38.16
0.00
0.00
9.53
5.87
3.38
0.00
2.34
4.35
0.58
0.79

0.00
0.00
30300b
30300b
30300b
30300b
31500
30300b
31500
30300b
030700a
030700a
0307003
0307003
0307003
0307003
0307003
032000b
0307003
0307003
0324003
0307003
0323003
0323003
030700b
0323003
030700b
0324003
030700b
030700b
030700b
030700b
30800
30800
30800
30800
30800
30800
0323003
30800
30800
30800
30900
30900
30900
30900
30900
30900
30900
30900
30900
30900
31000
040400b
31000
31000
31000
31000
31000
31000
31000
31000
31000
31000

2300b
2300b
2300b
2300b
2300b
0225003
2300b
2300b
2300b
0225003
0225003

33000
33000













































































7.6
44.8
20.0
23.1
64.1
51.3
11.9
3.6
3.8
NA
25.0
34.3
19.4
7.1
NA
11.9
33.3
66.7
13.3
0.0
0.0
13.0
NA
17.2
41.7
13.5
0.0
0.0
0.0
15.4
11.8
10.6
60.0
33.3
NA
3.9
0.0
10.5
11.1
NA
0.0
NA
0.0
0.0
18.2
13.3
8.2
4.9
13.3
0.0
26.2
NA
16.1
3.4
9.8
25.0
26.5
34.4
50.0
0.0
9.4
132.4

5.2
0.0
0.0
NA
43.9
14.3
0.0
24.1
NA
37.5
24.3

NA
NA
139.96
211.01
130.5
152.6
88.2
145.04
112
150.1
145.3
154.4
168.5
145.4
142.8
151.97
164.5
98.98
165.4
147.3
101.5
47
162.2
146.7
91.95
17.2
93.7
99.15
95.02
100.1
103.4
114.3
139.4
130.9
114.4
116.2
102.3
122.5
109.8
130.2
105.1
130.2
80.3
108.8
70.5
10705
89.7
64.7
111.1
73.2
63.2
71.77
164
67.45
182.8
92.4
42.6
131.5
117.3
136.6
109.4
92.8
131.3
138.3

91.8
156.2
157.39
171.72
95.59
95
106.84
113.87
79.79
96.9
131.53

93.5
108.8













































































-------
M5-735-PSF
M5-740-PSF
M5-741-PSF
M5-742-PSF
M5-743-PSF
M5-744-PSF
M5-745-PSF
M5-746-PSF
M5-747-PSF
M5-747-PSF

PS
PS
PS
PS
PS
PS
PS
PS
PS
PS












09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99









942


03/30/00
03/30/00
03/30/00
03/30/00
03/30/00
04/04/00
04/04/00
03/30/00
02/21/00
04/04/00

03/30/00
03/30/00
03/30/00
03/30/00
03/30/00
04/04/00
04/04/00
03/30/00
02/21/00
04/04/00

28
28
28
28
28
28
28
28
28
28

190
190
190
190
190
195
195
190
152
195

0.00
0.00
0.00
0.00
0.07
0.70
0.38
0.00
0.15
0.85

33000
33000
33000
33000
33000
040400a
040400a
33000
0221003
0404003












NA
NA
NA
NA
NA
NA
NA
NA
33.3
NA

68.65
84.17
72.03
85.07
92.15
170.5
123
72.86
155.9
64.41












-------
10 % Recalculated Results for Total Phosphorus in Soil/Sediment
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by MWB 4-7-00
Checked by   NJS 4-14-00
Sample
M5-622-SDF
M5-643-SDF
M5-663-SDF
Sample
Citrus Leaves
Citrus Leaves
CCV
CCV
CCV
CCV
CCV
M5-636-SDF
M5-636-SDF-D
M5-658-SDF
M5-658-SDF-D
Blanks
QA/QC
Batch
EPA1124C
"
"
QA/QC
Batch
EPA1124C
"
"
"
"
"
"
"
"
"
"
"
Qualifier
Note



Qualifier
Note











"B (NR)"
Dilution
Factor
1
1
1
Dilution
Factor
1
1
1
1
1
1
1
1
1
1
1

Weight
grams
0.0251
0.0250
0.0249
Weight
grams
0.0255
0.0254





0.0248
0.0248
0.0256
0.0250

Peak Height
u in
5174
19003
9844
Peak Height
urn
74272
77618
58953
60170
61820
62375
63064
14348
13873
18825
17280

Slope
u in
2664.3945
2664.3945
2664.3945
Slope
urn
2664.3945
2664.3945
2664.3945
2664.3945
2664.3945
2664.3945
2664.3945
2664.3945
2664.3945
2664.3945
2664.3945

Sample
Results
ug/g (ppm)
77.4
285.3
148.4
Sample
Results
ug/g (ppm)
1093.2
1146.9
22.1
22.6
23.2
23.4
23.7
217.1
210.0
276.0
259.4

Detection
Limit
ug/g (ppm)
0.06
0.06
0.06
Detection
Limit*3
ug/g (ppm)
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18


SPK
CONC
ug/g (ppm)
1300
1300
23.23
23.23
23.23
23.23
23.23





R%
84.09
88.22
95.25
97.21
99.88
100.78
101.89





RPD

-4.799






3.366

6.190

Sample
M5-633-SDF
M5-653-SDF
M5-738-SDF
Sample
Citrus Leaves
Citrus Leaves
CCV
CCV
CCV
CCV
M5-647-SDF
M5-647-SDF-D
M5-735-SDF
M5-735-SDF-D
Blanks
QA/QC
Batch
EPAM5-C
"
"
QA/QC
Batch
EPAM5-C

"
"
"
"
"
"
"
"
"
Qualifier
Note



Qualifier
Note










"B (NR)"
Dilution
Factor
1
1
1
Dilution
Factor
1
1
1
1
1
1
1
1
1
1

Weight
grams
0.0248
0.0248
0.0249
Weight
grams
0.0246
0.0245




0.0248
0.0248
0.0252
0.0252

Peak Height
urn
28422
8898
24785
Peak Height
urn
85425
78812
57788
63323
64574
65826
26200
25934
5318
4525

Slope
urn
2775.5208
2775.5208
2775.5208
Slope
inn
2775.5208
2775.5208
2775.5208
2775.5208
2775.5208
2775.5208
2775.5208
2775.5208
2775.5208
2775.5208

Sample
Results
ug/g (ppm)
412.9
129.3
358.6
Sample
Results
ug/g (ppm)
1251.1
1159.0
20.8
22.8
23.3
23.7
380.6
376.8
76.0
64.7

Detection
Limit
ug/g (ppm)
0.06
0.06
0.06
Detection
Limit*3
ug/g (ppm)
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18


SPK
CONC
ug/g (ppm)
1300
1300
23.23
23.23
23.23
23.23





R%
96.24
89.15
89.63
98.21
100.15
102.09





RPD

7.646

-9.140

-1.920

1.020

16.113

"B" Analyte concentration in the associated blank was >3 times the MDL.
"NR" Data ivu:; unavailable for review.
-------
10 % Recalculated Results for Total Phosphorus in Soil/Sediment
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by MWB 4-7-00
Checked by   NJS 4-14-00
Sample
M5-673-SDF
M5-683-SDF
Sample
Citrus Leaves
Citrus Leaves
CCV
CCV
CCV
CCV
M5-661-SDF
M5-661-SDF-D
M5-676-SDF
M5-676-SDF-D
M5-685-SDF
M5-685-SDF-D
Blanks
QA/QC
Batch
EPAM5-D
"
QA/QC
Batch
EPAM5-D
"
"
"
"
"
"
"
"
"
"
"
"
Qualifier
Note


Qualifier
Note












"B (NR)"
Dilution
Factor
1
1
Dilution
Factor
1
1
1
1
1
1
1
1
1
1
1
1

Weight
grams
0.0253
0.0254
Weight
grams
0.0246
0.0245




0.0245
0.0245
0.0248
0.0248
0.0245
0.0247

Peak Height
u in
8544
20297
Peak Height
urn
88147
82242
62262
65420
66646
64271
10723
10589
17309
21182
25317
23903

Slope
u in
2845.8136
2845.8136
Slope
urn
2845.8136
2845.8136
2845.8136
2845.8136
2845.8136
2845.8136
2845.8136
2845.8136
2845.8136
2845.8136
2845.8136
2845.8136

Sample
Results
ug/g (ppm)
118.7
280.8
Sample
Results
ug/g (ppm)
1259.1
1179.6
21.9
23.0
23.4
22.6
153.8
151.9
245.3
300.1
363.1
340.1

Detection
Limit
ug/g (ppm)
0.06
0.06
Detection
Limit*3
ug/g (ppm)
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18


SPK
CONC
ug/g (ppm)
1300
1300
23.23
23.23
23.23
23.23







R%
96.86
90.74
94.18
98.96
100.81
97.22







RPD

6.5





1.3

-20.1

6.6

"B" Analyte concentration in the associated blank was >3 times the MDL.
"NR" Data was unavailable for review.
-------
10 % Recalculated Results for Total Phosphorus in Soil/Sediment
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by MWB 4-10-00
Checked by   NJS 4-14-00
Sample
M5-693-SDF
M5-703-SDF
M5-714-SDF
M5-726-SDF
M5-828-SDF
M5-944-SDF
Sample
Citrus Leaves
Citrus Leaves
CCV
CCV
CCV
CCV
CCV
CCV
CCV
CCV
M5-868-SDF
M5-868-SDF-D
M5-702-SDF
M5-702-SDF-D
M5-714-SDF
M5-714-SDF-D
M5-725-SDF
M5-725-SDF-D
Blanks
QA/QC
Batch
EPAM5-A
"
"
"
"
"
QA/QC
Batch
EPAM5-A
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
Qualifier
Note






Qualifier
Note


















"B (NR)"
Dilution
Factor
1
1
1
1
1
1
Dilution
Factor
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1

Weight
grams
0.0249
0.0245
0.0251
0.0245
0.0252
0.0254
Weight
grams
0.0246
0.0245








0.0246
0.0246
0.025
0.025
0.0251
0.0251
0.0248
0.0248

Peak Height
u in
12431
7407
28159
15762
12391
18729
Peak Height
urn
73703
67110
54639
58541
59855
60497
60628
57545
65184
64668
36375
37471
10068
10923
28159
26819
19440
18209

Slope
u in
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162
Slope
urn
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162
2680.2162

Sample
Results
ug/g (ppm)
186.3
112.8
408.6
240.0
183.5
275.1
Sample
Results
ug/g (ppm)
1117.8
1022.0
20.4
21.8
22.3
22.6
22.6
21.5
24.3
24.1
551.7
568.3
150.3
163.0
418.6
398.7
292.5
273.9

Detection
Limit
ug/g (ppm)
0.06
0.06
0.06
0.06
0.06
0.06
Detection
Limit*3
ug/g (ppm)
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18
0.18


SPK
CONC
ug/g (ppm)
1300
1300
23.23
23.23
23.23
23.23
23.23
23.23
23.23
23.23









R%
85.99
78.62
87.76
94.02
96.13
97.17
97.38
92.42
104.69
103.87









RPD

8.958









-2.968

-8.146

4.875

6.539

"B" Analyte concentration in the associated blank was >3 times the MDL.
"NR" Data was unavailable for review.
-------
SERC Lab / EPA REMAP results
Total Phosphorus (TP) in Soil by EPA Method 365.1 (modified)
: Analysis not performed

: Analysis not required

: Average of Two
     Data Entered by:   njs  03-22-00 mwb 03-27-0
Data Entry Checked by: njs 03-28-00
Sampling Station
ID
M5-623-SDF
M5-630-SDF
M5-633-SDF
M5-634-SDF
M5-637-SDF
M5-640-SDF
M5-641-SDF
M5-644-SDF
M5-646-SDF
M5-647-SDF
M5-648-SDF
M5-649-SDF
M5-650-SDF
M5-651-SDF
M5-653-SDF
M5-655-SDF
M5-657-SDF
M5-659-SDF
M5-660-SDF
M5-661-SDF
M5-664-SDF
M5-666-SDF
M5-667-SDF
M5-668-SDF
M5-671-SDF
M5-672-SDF
M5-673-SDF
M5-674-SDF
M5-676-SDF
M5-677-SDF
M5-678-SDF
M5-679-SDF
M5-680-SDF
M5-681-SDF
M5-682-SDF
M5-683-SDF
M5-684-SDF
Matrix
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
Collection
Date
09/30/99
09/28/99
09/29/99
09/29/99
09/29/99
09/29/99
09/28/99
09/30/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/27/99
09/27/99
09/27/99
09/29/99
09/27/99
09/27/99
09/27/99
09/27/99
09/26/99
09/27/99
09/27/99
09/26/99
09/28/99
09/26/99
09/26/99
09/26/99
09/27/99
09/26/99
09/26/99
09/26/99
09/26/99
Time
915
1520
1115
1510
1210
1116
1615
1145
1515
1102
1300
1620
1158
1410
1300
1028
1751
1205
1450
857
1100
1655
1545
1207
850
1100
1400
1025
925
1310
1213
1335
900
1410
1615
850
1530
Digestion
Date
11/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
Run
Date
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
Time Elapsed
From Dig
43
45
44
44
44
44
45
43
45
45
45
45
45
45
45
45
46
46
46
44
46
46
46
46
47
46
46
47
45
47
47
47
46
47
47
47
47
Holding
Time (D:iy:;'»
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
Phosphorus
Units (ppm, ug/g)
173
176
413
533
401
596
368
477
421
379
236
298
355
202
129
638
368
362
580
153
209
288
386
234
205
288
119
499
273
288
305
265
330
135
215
281
137
Detection
Limit (ppm)
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
QA/QC
Batch ID
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
QAData
%R %RPD Matrix %R Sample RPD
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
7.3
7.3
7.3
7.3
7.3
7.3
7.3
7.3
7.3
7.3
7.3
7.3
7.3
7.3
7.3
7.3
7.3
7.3
7.3
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.2
92.7
92.7
92.7
92.7
92.7
92.7
92.7
92.7
92.7
92.7
92.7
92.7
92.7
92.7
92.7
92.7
92.7
92.7
92.7
93.8
93.8
93.8
93.8
93.8
93.8
93.8
93.8
93.8
93.8
93.8
93.8
93.8
93.8
93.8
93.8
93.8
93.8









1.02









1.26








20.1









Notes









Averaged Result









Averaged Result








Averaged Result








-------
Sampling Station
ID
M5-685-SDF
M5-686-SDF
M5-687-SDF
M5-688-SDF
M5-689-SDF
M5-690-SDF
M5-691-SDF
M5-733-SDF
M5-734-SDF
M5-735-SDF
M5-738-SDF
M5-740-SDF
M5-741-SDF
M5-742-SDF
M5-743-SDF
M5-622-SDF
M5-624-SDF
M5-625-SDF
M5-626-SDF
M5-627-SDF
M5-628-SDF
M5-631-SDF
M5-632-SDF
M5-635-SDF
M5-636-SDF
M5-638-SDF
M5-639-SDF
M5-642-SDF
M5-643-SDF
M5-645-SDF
M5-647-SDF
M5-652-SDF
M5-654-SDF
M5-656-SDF
M5-658-SDF
M5-662-SDF
M5-663-SDF
M5-665-SDF
M5-669-SDF
M5-670-SDF
M5-708-SDF
M5-744-SDF
Matrix
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
Collection
Date
09/26/99
09/25/99
09/25/99
09/26/99
09/25/99
09/25/99
09/25/99
09/23/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/22/99
09/30/99
09/30/99
09/30/99
09/30/99
09/30/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/29/99
09/28/99
09/29/99
09/29/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/28/99
09/27/99
09/27/99
09/27/99
09/27/99
09/27/99
09/24/99
09/22/99
Time
1434
915
1035
1527
1205
1350
1554
910
1540
1700
1410
1245
1534
1418
1130
1125
1018
1257
908
1050
1716
1414
1010
1216
1405
1630
1715
1011
910
1447
1102
959
1145
900
1722
1610
1330
1710
1000
850
900
1224
Digestion
Date
11/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
1 1/12/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/18/99
11/15/99
Run
Date
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/24/99
11/19/99
Time Elapsed
From Dig
47
48
48
47
48
48
48
53
54
54
54
54
54
54
54
49
49
49
49
49
50
50
50
50
50
50
51
50
50
51
51
51
51
51
51
52
52
52
52
52
55
54
Holding
Time (D:iy:;'»
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
Phosphorus
Units (ppm, ug/g)
352
436
402
268
192
177
386
162
334
70
359
120
119
78
42
77
267
179
243
417
285
226
552
271
214
741
453
372
285
409
396
430
384
298
268
291
148
263
236
150
162
162
Detection
Limit (ppm)
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
QA/QC
Batch ID
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-D
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPAM5-C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPA1124C
EPAM5-A
QAData
%R %RPD Matrix %R Sample RPD
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
115
105
6.2
6.2
6.2
6.2
6.2
6.2
6.2
7.3
7.3
7.3
7.3
7.3
7.3
7.3
7.3
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
4.6
8.4
93.8
93.8
93.8
93.8
93.8
93.8
93.8
92.7
92.7
92.7
92.7
92.7
92.7
92.7
92.7
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
86.2
82.3
6.56








16.11














3.37









6.19








Notes
Averaged Result








Averaged Result














Averaged Result









Averaged Result







-------
Sampling Station
ID
M5-745-SDF
M5-746-SDF
M5-747-SDF
M5-823-SDF
M5-828-SDF
M5-838-SDF
M5-848-SDF
M5-859-SDF
M5-868-SDF
M5-878-SDF
M5-890-SDF
M5-908-SDF
M5-920-SDF
M5-932-SDF
M5-944-SDF
M5-693-SDF
M5-694-SDF
M5-695-SDF
M5-696-SDF
M5-697-SDF
M5-698-SDF
M5-699-SDF
M5-700-SDF
M5-701-SDF
M5-702-SDF
M5-703-SDF
M5-704-SDF
M5-705-SDF
M5-706-SDF
M5-707-SDF
M5-709-SDF
M5-710-SDF
M5-711-SDF
M5-712-SDF
M5-714-SDF
M5-715-SDF
M5-716-SDF
M5-718-SDF
M5-719-SDF
M5-720-SDF
M5-722-SDF
M5-723-SDF
Matrix
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
SD
Collection
Date
09/22/99
09/22/99
09/22/99
09/30/99
09/29/99
09/29/99
09/28/99
09/27/99
09/27/99
09/26/99
09/25/99
09/24/99
09/23/99
09/23/99
09/22/99
09/25/99
09/25/99
09/25/99
09/25/99
09/26/99
09/25/99
09/25/99
09/25/99
09/26/99
09/25/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/24/99
09/23/99
09/24/99
09/24/99
09/24/99
09/23/99
09/23/99
09/23/99
09/23/99
Time
1120
948
942
0
0
0
0
0
0
0
0
0
0
0
1224
1139
1702
1400
1510
1637
1030
1635
1750
1740
918
1655
1615
1725
1555
1500
1330
1430
1115
905
1715
1145
1310
1030
1715
0
1600
1500
Digestion
Date
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
Run
Date
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
Time Elapsed
From Dig
54
54
54
46
47
47
48
49
49
50
51
52
53
53
54
51
51
51
51
50
51
51
51
50
51
52
52
52
52
52
52
52
52
52
53
52
52
52
53
53
53
53
Holding
Time (D:iy:;'»
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
28
Phosphorus
Units (ppm, ug/g)
26
72
96
132
183
124
177
169
560
224
179
175
157
378
275
186
191
82
141
95
279
225
195
158
157
113
142
231
192
691
133
166
178
232
409
109
246
115
172
122
77
85
Detection
Limit (ppm)
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
QA/QC
Batch ID
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
QAData
%R %RPD Matrix %R Sample RPD
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
105
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3








-2.97















-8.15









4.87








Notes








Averaged Result






Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
-------
Sampling Station
ID
M5-724-SDF
M5-725-SDF
M5-726-SDF
M5-727-SDF
M5-728-SDF
M5-729-SDF
M5-730-SDF
M5-731-SDF
M5-732-SDF
Matrix
SD
SD
SD
SD
SD
SD
SD
SD
SD
Collection
Date
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/23/99
09/22/99
09/23/99
Time
1442
1323
1230
1216
1350
1027
1120
1725
917
Digestion
Date
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
11/15/99
Run
Date
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
11/19/99
Time Elapsed
From Dig
53
53
53
53
53
53
53
54
53
Holding
Time (D:iy:;'»
28
28
28
28
28
28
28
28
28
Phosphorus
Units (ppm, ug/g)
158
283
240
119
132
240
494
91
419
Detection
Limit (ppm)
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
QA/QC
Batch ID
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
EPAM5-A
QAData
%R
105
105
105
105
105
105
105
105
105
%RPD
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
8.4
Matrix %R
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
82.3
Sample RPD

6.54








Notes
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
Sample was label as SPF and Reported as SDF
-------
May  1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                Station ID    M5-622-SDF
Soil/Sediment
Laboratory Records
Data Report (Attached)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Calibration % R (high and low range)
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
09/30/99
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
09/30/99
02/21/00
02/21/00
X
SD = SF = S = Soil
09/30/99
11/18/99
11/24/99

X
SD = SF = S = Soil
09/30/99
12/09/99
12/09/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppm
CVAF


4.495,4.606
200ul
aliquot
See Worksheets
16.6
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
77
ug/g
EPA 365.1
Angel
0.06
0.025 g
0.025 g
0.025 g
NA
38.5
%
ASTM D2974-87
SG/JL
0

X
SD = SF = S = Soil
09/30/99



80
80
80
No Data Reviewed

g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL



28 days
SOP
Yes (FTN Associates)
No (Goal Only)
Yes (FTN Assoc rates)
Yes (FTN Assocrates)
No (Goal Only)
Yes (FTN Associates)
Yes (FTN Associates)
NA




FIU/SERC Laboratory uses the same ID as the Sampling Station ID








022100a
NA
All Good
Good
All Good
Good
0.2 ng/g and>
0.9815
EPA1124C
NA in Soils
"NR"
<20RPD
All Good
Good
60 ppm and >
0.9964

12/09/99
NA
NA
None Reported
NA
NA
NA
NA












Battelle Lab
SOP
Yes
"R2"
Yes
X
"B (NR)11
Yes
X
"DQO (NR)11


No Data Reviewed
                      Notes No descriptive narratives were provided by FIU.
                           Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
                           Total Phosphorus and MEHG were digested past the holding time goals. Holding time is a goal only.
                           Bulk Density data was not provided for review or reporting.
-------
                     Station ID    M5-622-SDF
                                        Total Hg
                                                 MeHg
Total Phosphorus
AFDW
Bulk Density
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations  From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection  Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
X

Not Noted
Internal COC












X
X
X
X
X
X
X
X
X
X
X
X
NA
X
X









X
X
ng/g
X
X
ug/g
X
X
%


g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
Applied Qualifiers|_
                                                                  "R2"
                                                                                                             "DQO (NR)11
X = Attached or Verified


Data Qualifiers

" J"  Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met

"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May  1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                Station ID    M5-633-SDF
Soil/Sediment
Laboratory Records
Data Report (Attached)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Calibration % R (high and low range)
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
09/29/99
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
09/29/99
03/20/00
03/20/00
X
SD = SF = S = Soil
09/29/99
11/12/99
11/19/99

X
SD = SF = S = Soil
09/29/99
12/09/99
12/09/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppm
CVAF


4.537, 4.922
200ul
aliquot
See Worksheets
8.2
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
413
ug/g
EPA 365.1
Angel
0.06
0.025 g
0.025 g
0.025 g
NA
87.4
%
ASTM D2974-87
SG/JL
0

X
SD = SF = S = Soil
09/29/99



80
80
80
No Data Reviewed

g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL



28 days
SOP
Yes (FTN Associates)
No (Goal Only)
Yes (FTN Assoc rates)
Yes (FTN Assocrates)
No (Goal Only)
Yes (FTN Associates)
Yes (FTN Associates)
NA




FIU/SERC Laboratory uses the same ID as the Sampling Station ID








032000b
NA
All Good
Good
48.70%
Good
0.2 ng/g and>
0.9808
EPAM5-C
NA in Soils
"NR"
<20RPD
All Good
Good
60 ppm and >
0.9965

12/09/99
NA
NA
None Reported
NA
NA
NA
NA












Battelle Lab
SOP
Yes
"R2", "M"
Yes
X
"B (NR)11
Yes
X
"DQO (NR)11


No Data Reviewed
                      Notes No descriptive narratives were provided by FIU.
                           Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
                           Total Phosphorus and MEHG were digested past the holding time goals. Holding time is a goal only.
                           Bulk Density data was not provided for review or reporting.
-------
                     Station ID    M5-633-SDF
                                        Total Hg
                                                 MeHg
Total Phosphorus
AFDW
Bulk Density
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations  From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection  Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
X

Not Noted
Internal COC












X
X
X
X
X
X
X
X
X
X
X
X
NA
X
X









X
X
ng/g
X
X
ug/g
X
X
%


g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
Applied Qualifiers|_
                                                                "R2", "M"
                                                                                                             "DQO (NR)11
X = Attached or Verified


Data Qualifiers

" J"  Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met

"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May  1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                Station ID    M5-643-SDF
Soil/Sediment
Laboratory Records
Data Report (Attached)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Calibration % R (high and low range)
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
09/29/99
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
09/29/99
02/21/00
02/21/00
X
SD = SF = S = Soil
09/29/99
11/18/99
11/24/99

X
SD = SF = S = Soil
09/29/99
12/09/99
12/09/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppm
CVAF


5.477, 4.590
200ul
aliquot
See Worksheets
1.4
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
285
ug/g
EPA 365.1
Angel
0.06
0.025 g
0.025 g
0.025 g
NA
53.6
%
ASTM D2974-87
SG/JL
0

X
SD = SF = S = Soil
09/29/99



80
80
80
No Data Reviewed

g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL



28 days
SOP
Yes (FTN Associates)
No (Goal Only)
Yes (FTN Assoc rates)
Yes (FTN Assocrates)
No (Goal Only)
Yes (FTN Associates)
Yes (FTN Associates)
NA




FIU/SERC Laboratory uses the same ID as the Sampling Station ID








022100b
NA
All Good
Good
130.56
Good
0.2 ng/g and>
0.9914
EPA1124C
NA in Soils
"NR"
<20RPD
All Good
Good
60 ppm and >
0.9964

12/09/99
NA
NA
None Reported
NA
NA
NA
NA












Battelle Lab
SOP
Yes
"R2", "M"
Yes
X
"B (NR)11
Yes
X
"DQO (NR)11


No Data Reviewed
                      Notes No descriptive narratives were provided by FIU.
                           Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
                           Total Phosphorus and MEHG were digested past the holding time goals. Holding time is a goal only.
                           Bulk Density data was not provided for review or reporting.
-------
                     Station ID    M5-643-SDF
                                        Total Hg
                                                 MeHg
Total Phosphorus
AFDW
Bulk Density
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations  From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection  Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
X

Not Noted
Internal COC












X
X
X
X
X
X
X
X
X
X
X
X
NA
X
X









X
X
ng/g
X
X
ug/g
X
X
%


g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
Applied Qualifiers|_
                                                                "R2", "M"
                                                                                                             "DQO (NR)11
X = Attached or Verified


Data Qualifiers

" J"  Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met

"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May  1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                Station ID    M5-653-SDF
Soil/Sediment
Laboratory Records
Data Report (Attached)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Calibration % R (high and low range)
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
09/28/99
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
09/28/99
02/28/99
02/28/99
X
SD = SF = S = Soil
09/28/99
11/12/99
11/19/99

X
SD = SF = S = Soil
09/28/99
12/09/99
12/09/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppm
CVAF


6.060, 5.583
200ul
aliquot
See Worksheets
0.1
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
129
ug/g
EPA 365.1
Angel
0.06
0.025 g
0.025 g
0.025 g
NA
15.9
%
ASTM D2974-87
SG/JL
0

X
SD = SF = S = Soil
09/28/99



80
80
80
No Data Reviewed

g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL



28 days
SOP
Yes (FTN Associates)
No (Goal Only)
Yes (FTN Assoc rates)
Yes (FTN Assocrates)
No (Goal Only)
Yes (FTN Associates)
Yes (FTN Associates)
NA




FIU/SERC Laboratory uses the same ID as the Sampling Station ID








22800
NA
All Good
Good
All Good
Not Reviewed
0.2 ng/g and>
0.9985
EPAM5-C
NA in Soils
"NR"
<20RPD
All Good
Good
60 ppm and >
0.9965

12/09/99
NA
NA
None Reported
NA
NA
NA
NA












Battelle Lab
SOP
Yes
"DQO (NR)"
Yes
X
"B (NR)11
Yes
X
"DQO (NR)11


No Data Reviewed
                      Notes No descriptive narratives were provided by FIU.
                           Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
                           Total Phosphorus and MEHG were digested past the holding time goals. Holding time is a goal only.
                           Bulk Density data was not provided for review or reporting.
-------
                     Station ID    M5-653-SDF
                                        Total Hg
MeHg
                                                                  Total Phosphorus
AFDW
Bulk Density
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations  From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection  Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
X

Not Noted
Internal COC












X
X
X
X
X
X
X
X
X
X
X
X
NA
X
X









X
X
ng/g
X
X
ug/g
X
X
%


g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
Applied Qualifiers|_
                                                               "DQO (NR)"
                                            "DQO (NR)11
X = Attached or Verified


Data Qualifiers

" J"  Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met

"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May  1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                Station ID    M5-663-SDF
Soil/Sediment
Laboratory Records
Data Report (Attached)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Calibration % R (high and low range)
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
09/27/99
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
09/27/99
02/29/00
02/29/00
X
SD = SF = S = Soil
09/27/99
11/18/99
11/24/99

X
SD = SF = S = Soil
09/27/99
12/09/99
12/09/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppm
CVAF


5.209, 4.609
200ul
aliquot
See Worksheets
3.9
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
148
ug/g
EPA 365.1
Angel
0.06
0.025 g
0.025 g
0.025 g
NA
69.3
%
ASTM D2974-87
SG/JL
0

X
SD = SF = S = Soil
09/27/99



80
80
80
No Data Reviewed

g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL



28 days
SOP
Yes (FTN Associates)
No (Goal Only)
Yes (FTN Assoc rates)
Yes (FTN Assocrates)
No (Goal Only)
Yes (FTN Associates)
Yes (FTN Associates)
NA




FIU/SERC Laboratory uses the same ID as the Sampling Station ID








022500b
NA
All Good
Good
36.84%
Good
0.2 ng/g and>
0.9871
EPA1124C
NA in Soils
"NR"
<20RPD
All Good
Good
60 ppm and >
0.9964

12/09/99
NA
NA
None Reported
NA
NA
NA
NA












Battelle Lab
SOP
Yes
"R2", "M"
Yes
X
"B (NR)11
Yes
X
"DQO (NR)11


No Data Reviewed
                      Notes No descriptive narratives were provided by FIU.
                           Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
                           Total Phosphorus and MEHG were digested past the holding time goals. Holding time is a goal only.
                           Bulk Density data was not provided for review or reporting.
-------
                     Station ID    M5-663-SDF
                                        Total Hg
                                                 MeHg
Total Phosphorus
AFDW
Bulk Density
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations  From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection  Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
X

Not Noted
Internal COC












X
X
X
X
X
X
X
X
X
X
X
X
NA
X
X









X
X
ng/g
X
X
ug/g
X
X
%


g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
Applied Qualifiers|_
                                                                "R2", "M"
                                                                                                             "DQO (NR)11
X = Attached or Verified


Data Qualifiers

" J"  Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met

"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May  1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                Station ID    M5-673-SDF
Soil/Sediment
Laboratory Records
Data Report (Attached)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Calibration % R (high and low range)
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
09/27/99
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
09/27/99
03/02/00
03/02/00
X
SD = SF = S = Soil
09/27/99
11/12/99
11/19/99

X
SD = SF = S = Soil
09/27/99
12/09/99
12/09/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppm
CVAF


5.076, 4.834
200ul
aliquot
See Worksheets
3.3
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
119
ug/g
EPA 365.1
Angel
0.06
0.025 g
0.025 g
0.025 g
NA
32.7
%
ASTM D2974-87
SG/JL
0

X
SD = SF = S = Soil
09/27/99



80
80
80
No Data Reviewed

g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL



28 days
SOP
Yes (FTN Associates)
No (Goal Only)
Yes (FTN Assoc rates)
Yes (FTN Assocrates)
No (Goal Only)
Yes (FTN Associates)
Yes (FTN Associates)
NA




FIU/SERC Laboratory uses the same ID as the Sampling Station ID








022100a
NA
All Good
Good
All Good
Good
0.2 ng/g and>
0.9815
EPAM5-D
NA in Soils
"NR"
<20RPD
All Good
Good
60 ppm and >
0.9973

12/09/99
NA
NA
None Reported
NA
NA
NA
NA












Battelle Lab
SOP
Yes
"R2"
Yes
X
"B (NR)11
Yes
X
"DQO (NR)11


No Data Reviewed
                      Notes No descriptive narratives were provided by FIU.
                           Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
                           Total Phosphorus and MEHG were digested past the holding time goals. Holding time is a goal only.
                           Bulk Density data was not provided for review or reporting.
-------
                     Station ID    M5-673-SDF
                                        Total Hg
                                                 MeHg
Total Phosphorus
AFDW
Bulk Density
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations  From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection  Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
X

Not Noted
Internal COC












X
X
X
X
X
X
X
X
X
X
X
X
NA
X
X









X
X
ng/g
X
X
ug/g
X
X
%


g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
Applied Qualifiers|_
                                                                  "R2"
                                                                                                             "DQO (NR)11
X = Attached or Verified


Data Qualifiers

" J"  Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met

"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May  1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                Station ID    M5-683-SDF
Soil/Sediment
Laboratory Records
Data Report (Attached)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Calibration % R (high and low range)
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
09/26/99
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
09/26/99
03/03/00
03/03/00
X
SD = SF = S = Soil
09/26/99
11/12/99
11/19/99

X
SD = SF = S = Soil
09/26/99
12/13/99
12/13/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppm
CVAF


5.186,4.518
200ul
aliquot
See Worksheets
0.36
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
77
ug/g
EPA 365.1
Angel
0.06
0.025 g
0.025 g
0.025 g
NA
88.7
%
ASTM D2974-87
SG/JL
0

X
SD = SF = S = Soil
09/26/99



80
80
80
No Data Reviewed

g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL



28 days
SOP
Yes (FTN Associates)
No (Goal Only)
Yes (FTN Assoc rates)
Yes (FTN Assocrates)
No (Goal Only)
Yes (FTN Associates)
Yes (FTN Associates)
NA




FIU/SERC Laboratory uses the same ID as the Sampling Station ID








30300a
NA
All Good
Good
131.81%
140%
0.2 ng/g and>
0.9823
EPAM5-D
NA in Soils
"NR"
<20RPD
All Good
Good
60 ppm and >
0.9973

12/13/99
NA
NA
None Reported
NA
NA
NA
NA












Battelle Lab
SOP
Yes
"R2", "M", "DQO"
Yes
X
"B (NR)11
Yes
X
"DQO (NR)11


No Data Reviewed
                      Notes No descriptive narratives were provided by FIU.
                           Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
                           Total Phosphorus and MEHG were digested past the holding time goals. Holding time is a goal only.
                           Bulk Density data was not provided for review or reporting.
-------
                     Station ID    M5-683-SDF
                                        Total Hg
MeHg
                                                                  Total Phosphorus
AFDW
Bulk Density
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations  From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection  Data/Time
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
X

Not Noted
Internal COC







Validation Criteria





X
X
X
X
X
X
X
X
X
X
X
X
NA
X
X









X
X
ng/g
X
X
ug/g
X
X
%


g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Applied Qualifiers|_
                                                             "R2", "M", "DQO"
                                            "DQO (NR)11
X = Attached or Verified


Data Qualifiers

" J"  Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met

"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May  1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                Station ID    M5-693-SDF
Soil/Sediment
Laboratory Records
Data Report (Attached)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Calibration % R (high and low range)
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
09/25/99
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
09/25/99
03/03/00
03/03/00
X
SD = SF = S = Soil
09/25/99
11/15/99
11/19/99

X
SD = SF = S = Soil
09/25/99
12/13/99
12/13/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppm
CVAF


5.279, 4.996
200ul
aliquot
See Worksheets
0.14
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
186
ug/g
EPA 365.1
Angel
0.06
0.025 g
0.025 g
0.025 g
NA
80.3
%
ASTM D2974-87
SG/JL
0

X
SD = SF = S = Soil
09/25/99



80
80
80
No Data Reviewed

g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL



28 days
SOP
Yes (FTN Associates)
No (Goal Only)
Yes (FTN Assoc rates)
Yes (FTN Assocrates)
No (Goal Only)
Yes (FTN Associates)
Yes (FTN Associates)
NA




FIU/SERC Laboratory uses the same ID as the Sampling Station ID








30300b
NA
All Good
-46.4
210.87%
145.17%
0.2 ng/g and>
0.9397
EPAM5-A
NA in Soils
"NR"
<20RPD
All Good
Good
60 ppm and >
0.995

12/13/99
NA
NA
None Reported
NA
NA
NA
NA












Battelle Lab
SOP
Yes
"R2", "DQO", "M"
Yes
X
"B (NR)11
Yes
X
"DQO (NR)11


No Data Reviewed
                      Notes No descriptive narratives were provided by FIU.
                           Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
                           Total Phosphorus and MEHG were digested past the holding time goals. Holding time is a goal only.
                           Bulk Density data was not provided for review or reporting.
-------
                     Station ID    M5-693-SDF
                                        Total Hg
MeHg
                                                                  Total Phosphorus
AFDW
Bulk Density
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations  From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection  Data/Time
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
X

Not Noted
Internal COC







Validation Criteria





X
X
X
X
X
X
X
X
X
X
X
X
NA
X
X









X
X
ng/g
X
X
ug/g
X
X
%


g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Applied Qualifiers|_
                                                             "R2", "DQO", "M"
                                            "DQO (NR)11
X = Attached or Verified


Data Qualifiers

" J"  Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met

"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May  1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                Station ID    M5-703-SDF
Soil/Sediment
Laboratory Records
Data Report (Attached)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Calibration % R (high and low range)
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
09/24/99
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
09/24/99
03/07/00
03/07/00
X
SD = SF = S = Soil
09/24/99
11/15/99
11/19/99

X
SD = SF = S = Soil
09/24/99
12/13/99
12/13/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppm
CVAF


5.368, 5.250
200ul
aliquot
See Worksheets
0.24
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
113
0
EPA 365.1
Angel
0.06
0.025 g
0.025 g
0.025 g
NA
29.9
%
ASTM D2974-87
SG/JL
0

X
SD = SF = S = Soil
09/24/99



80
80
80
No Data Reviewed

g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL



28 days
SOP
Yes (FTN Associates)
No (Goal Only)
Yes (FTN Assoc rates)
Yes (FTN Assocrates)
No (Goal Only)
Yes (FTN Associates)
Yes (FTN Associates)
NA




FIU/SERC Laboratory uses the same ID as the Sampling Station ID








030700a
NA
All Good
35.9
143
Not Reported
0.2 ng/g and>
0.9925
EPAM5-A
NA in Soils
"NR"
<20RPD
All Good
Good
60 ppm and >
0.995

12/13/99
NA
NA
None Reported
NA
NA
NA
NA












Battelle Lab
SOP
Yes
"R2", "M", "DQO"
Yes
X
"B (NR)11
Yes
X
"DQO (NR)11


No Data Reviewed
                      Notes No descriptive narratives were provided by FIU.
                           Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
                           Total Phosphorus and MEHG were digested past the holding time goals. Holding time is a goal only.
                           Bulk Density data was not provided for review or reporting.
-------
                     Station ID    M5-703-SDF
                                        Total Hg
MeHg
                                                                  Total Phosphorus
AFDW
Bulk Density
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations  From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection  Data/Time
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
X

Not Noted
Internal COC







Validation Criteria





X
X
X
X
X
X
X
X
X
X
X
X
NA
X
X









X
X
ng/g
X
X
ug/g
X
X
%


g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Applied Qualifiers|_
                                                             "R2", "M", "DQO"
                                            "DQO (NR)11
X = Attached or Verified


Data Qualifiers

" J"  Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met

"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May  1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                Station ID    M5-714-SDF
Soil/Sediment
Laboratory Records
Data Report (Attached)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Calibration % R (high and low range)
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
09/23/99
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
09/23/99
03/23/00
03/23/00
X
SD = SF = S = Soil
09/23/99
11/15/99
11/19/99

X
SD = SF = S = Soil
09/23/99
12/13/99
12/13/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppm
CVAF


4.908, 4.629
200ul
aliquot
See Worksheets
0.31
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
409
ug/g
EPA 365.1
Angel
0.06
0.025 g
0.025 g
0.025 g
NA
45.1
%
ASTM D2974-87
SG/JL
0

X
SD = SF = S = Soil
09/23/99



80
80
80
No Data Reviewed

g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL



28 days
SOP
Yes (FTN Associates)
No (Goal Only)
Yes (FTN Assoc rates)
Yes (FTN Assocrates)
No (Goal Only)
Yes (FTN Associates)
Yes (FTN Associates)
NA




FIU/SERC Laboratory uses the same ID as the Sampling Station ID








032300a
NA
All Good
Good
146.26%
Not Reported
0.2 ng/g and>
0.9935
EPAM5-A
NA in Soils
"NR"
<20RPD
All Good
Good
60 ppm and >
0.995

12/13/99
NA
NA
None Reported
NA
NA
NA
NA












Battelle Lab
SOP
Yes
"R2", "M", "DQO"
Yes
X
"B (NR)11
Yes
X
"DQO (NR)11


No Data Reviewed
                      Notes No descriptive narratives were provided by FIU.
                           Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
                           Total Phosphorus and MEHG were digested past the holding time goals. Holding time is a goal only.
                           Bulk Density data was not provided for review or reporting.
-------
                     Station ID    M5-714-SDF
                                        Total Hg
MeHg
                                                                  Total Phosphorus
AFDW
Bulk Density
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations  From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection  Data/Time
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
X

Not Noted
Internal COC







Validation Criteria





X
X
X
X
X
X
X
X
X
X
X
X
NA
X
X









X
X
ng/g
X
X
ug/g
X
X
%


g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Applied Qualifiers|_
                                                             "R2", "M", "DQO"
                                            "DQO (NR)11
X = Attached or Verified


Data Qualifiers

" J"  Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met

"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May  1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                Station ID    M5-726-SDF
Soil/Sediment
Laboratory Records
Data Report (Attached)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Calibration % R (high and low range)
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
09/23/99
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
09/23/99
03/08/00
03/08/00
X
SD = SF = S = Soil
09/23/99
11/15/99
11/19/99

X
SD = SF = S = Soil
09/23/99
12/14/99
12/14/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppm
CVAF


5.183,4.935
200ul
aliquot
See Worksheets
0.72
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
240
ug/g
EPA 365.1
Angel
0.06
0.025 g
0.025 g
0.025 g
NA
84.6
%
ASTM D2974-87
SG/JL
0

X
SD = SF = S = Soil
09/23/99



80
80
80
No Data Reviewed

g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL



28 days
SOP
Yes (FTN Associates)
No (Goal Only)
Yes (FTN Assoc rates)
Yes (FTN Assocrates)
No (Goal Only)
Yes (FTN Associates)
Yes (FTN Associates)
NA




FIU/SERC Laboratory uses the same ID as the Sampling Station ID








30800
NA
All Good
Good
130.61%
Good
0.2 ng/g and>
0.9995
EPAM5-A
NA in Soils
"NR"
<20RPD
All Good
Good
60 ppm and >
0.995

12/14/99
NA
NA
None Reported
NA
NA
NA
NA












Battelle Lab
SOP
Yes
"M"
Yes
X
"B (NR)11
Yes
X
"DQO (NR)11


No Data Reviewed
                      Notes No descriptive narratives were provided by FIU.
                           Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
                           Total Phosphorus and MEHG were digested past the holding time goals. Holding time is a goal only.
                           Bulk Density data was not provided for review or reporting.
-------
                     Station ID    M5-726-SDF
                                        Total Hg
                                                 MeHg
Total Phosphorus
AFDW
Bulk Density
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations  From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection  Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
X

Not Noted
Internal COC












X
X
X
X
X
X
X
X
X
X
X
X
NA
X
X









X
X
ng/g
X
X
ug/g
X
X
%


g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
Applied Qualifiers|_
                                                                  "M"
                                                                                                             "DQO (NR)11
X = Attached or Verified


Data Qualifiers

" J"  Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met

"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May  1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                Station ID    M5-738-SDF
Soil/Sediment
Laboratory Records
Data Report (Attached)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Calibration % R (high and low range)
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
09/22/99
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
09/22/99
03/09/00
03/09/00
X
SD = SF = S = Soil
09/22/99
11/12/99
11/19/99

X
SD = SF = S = Soil
09/22/99
12/14/99
12/14/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppm
CVAF


5.101,5.139
200ul
aliquot
See Worksheets
0.26
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
359
ug/g
EPA 365.1
Angel
0.06
0.025 g
0.025 g
0.025 g
NA
48.4
%
ASTM D2974-87
SG/JL
0

X
SD = SF = S = Soil
09/22/99



80
80
80
No Data Reviewed

g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL



28 days
SOP
Yes (FTN Associates)
No (Goal Only)
Yes (FTN Assoc rates)
Yes (FTN Assocrates)
No (Goal Only)
Yes (FTN Associates)
Yes (FTN Associates)
NA




FIU/SERC Laboratory uses the same ID as the Sampling Station ID








022500b
NA
All Good
Good
All Good
166, 114
0.2 ng/g and>
0.9871
EPAM5-C
NA in Soils
"NR"
<20RPD
All Good
Good
60 ppm and >
0.9965

12/14/99
NA
NA
None Reported
NA
NA
NA
NA












Battelle Lab
SOP
Yes
"R2", "DQO"
Yes
X
"B (NR)11
Yes
X
"DQO (NR)11


No Data Reviewed
                      Notes No descriptive narratives were provided by FIU.
                           Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
                           Total Phosphorus and MEHG were digested past the holding time goals. Holding time is a goal only.
                           Bulk Density data was not provided for review or reporting.
-------
                     Station ID    M5-738-SDF
                                        Total Hg
MeHg
                                                                 Total Phosphorus
AFDW
Bulk Density
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations  From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection  Data/Time
              Laboratory ID Code
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
X

Not Noted
Internal COC












X
X
X
X
X
X
X
X
X
X
X
X
NA
X
X









X
X
ng/g
X
X
ug/g
X
X
%


g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Validation Criteria
Applied Qualifiers|_
                                                               "R2", "DQO"
                                            "DQO (NR)11
X = Attached or Verified


Data Qualifiers

" J"  Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met

"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May  1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                Station ID    M5-828-SDF
Soil/Sediment
Laboratory Records
Data Report (Attached)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Calibration % R (high and low range)
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
09/28/99
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
09/28/99
04/04/00
04/04/00
X
SD = SF = S = Soil
09/28/99
11/15/99
11/19/99

X
SD = SF = S = Soil
09/28/99
12/15/99
12/15/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppm
CVAF


5.022
200ul
aliquot
See Worksheets
6.9
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
184
ug/g
EPA 365.1
Angel
0.06
0.025 g
0.025 g
0.025 g
NA
94.5
%
ASTM D2974-87
SG/JL
0

X
SD = SF = S = Soil
09/28/99



80
80
80
No Data Reviewed

g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL



28 days
SOP
Yes (FTN Associates)
No (Goal Only)
Yes (FTN Assoc rates)
Yes (FTN Assocrates)
No (Goal Only)
Yes (FTN Associates)
Yes (FTN Associates)
NA




FIU/SERC Laboratory uses the same ID as the Sampling Station ID








040400b
NA
All Good
Not Reported
67.68%
Good
0.2 ng/g and>
0.9942
EPAM5-A
NA in Soils
"NR"
<20RPD
All Good
Good
60 ppm and >
0.995

12/15/99
NA
NA
None Reported
NA
NA
NA
NA












Battelle Lab
SOP
Yes
"R2", "M","DQO(NR)"
Yes
X
"B (NR)11
Yes
X
"DQO (NR)11


No Data Reviewed
                      Notes No descriptive narratives were provided by FIU.
                           Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
                           Total Phosphorus and MEHG were digested past the holding time goals. Holding time is a goal only.
                           Bulk Density data was not provided for review or reporting.
-------
                     Station ID    M5-828-SDF
                                        Total Hg
                                                 MeHg
                         Total Phosphorus
AFDW
Bulk Density
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations  From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection  Data/Time
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
X

Not Noted
Internal COC







Validation Criteria





X
X
X
X
X
X
X
X
X
X
X
X
NA
X
X









X
X
ng/g
X
X
ug/g
X
X
%


g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Applied Qualifiers|_
|  "R2", "M","DQO(NR)"  |
                                                                                                             "DQO (NR)11
X = Attached or Verified


Data Qualifiers

" J"  Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met

"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
May  1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                Station ID    M5-944-SDF
Soil/Sediment
Laboratory Records
Data Report (Attached)
Total Hg
MeHg
Total Phosphorus
AFDW
Bulk Density
Laboratory ID Code
Sampling Location ID
Sample Type
Collection Date
Digestion Date
Analysis Date
QC Batch ID
Digestion Volume
Total Volume
Sample Volume Analyzed
Dilution
Results
Measuring Unit
EPA Method
Analyst
Method Detection limit
Data Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
Holding Time Met
QC Report (Attached)
Laboratory ID Code
QC Batch ID
Method Blanks
Instrument Blanks
Duplicates (RPD)
Matrix Spike Recoveries (75-125)
Calibration % R (high and low range)
Detection Range
Correlation Coefficient (>0.995)
QC Report (Verified)
Lab Data Entry Checked by Analyst
All Calculation Checked
QC Limits Met
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
SD = SF = S = Soil
09/22/99
Not Analyzed
Battelle Lab
X
SD = SF = S = Soil
09/22/99
03/10/00
03/10/00
X
SD = SF = S = Soil
09/22/99
11/15/99
11/19/99

X
SD = SF = S = Soil
09/22/99
12/14/99
12/14/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.





ppm
CVAF


4.386, 4.482
200ul
aliquot
See Worksheets
0.51
ng/g
CVAF
JL
0.2 ng/g
0.025 g
0.025 g
Aliquot
1
275
ug/g
EPA 365.1
Angel
0.06
0.025 g
0.025 g
0.025 g
NA
78.3
%
ASTM D2974-87
SG/JL
0

X
SD = SF = S = Soil
09/22/99



80
80
80
No Data Reviewed

g/mL
ASTM D453 1-86
SG/JL
0.001 g/mL



28 days
SOP
Yes (FTN Associates)
No (Goal Only)
Yes (FTN Assoc rates)
Yes (FTN Assocrates)
No (Goal Only)
Yes (FTN Associates)
Yes (FTN Associates)
NA




FIU/SERC Laboratory uses the same ID as the Sampling Station ID








31000
NA
All Good
131.1
137.88%
191.96%
0.2 ng/g and>
0.9831
EPAM5-A
NA in Soils
"NR"
<20RPD
All Good
Good
60 ppm and >
0.995

12/14/99
NA
NA
None Reported
NA
NA
NA
NA












Battelle Lab
SOP
Yes
"R2", "M", "DQO"
Yes
X
"B (NR)11
Yes
X
"DQO (NR)11


No Data Reviewed
                      Notes No descriptive narratives were provided by FIU.
                           Battelle Laboratory has been assigned to be the main laboratory for Total Hg in soils
                           Total Phosphorus and MEHG were digested past the holding time goals. Holding time is a goal only.
                           Bulk Density data was not provided for review or reporting.
-------
                     Station ID    M5-944-SDF
                                        Total Hg
MeHg
                                                                  Total Phosphorus
AFDW
Bulk Density
Narrative Description (Attached) The Narrative Section will be written after all of the analyses are completed
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations  From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection  Data/Time
          Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
             Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
           All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)
X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID

Internal COC
Hglab
Internal COC
Not Noted
Internal COC
X
X
Not Noted
X

Not Noted
Internal COC







Validation Criteria





X
X
X
X
X
X
X
X
X
X
X
X
NA
X
X









X
X
ng/g
X
X
ug/g
X
X
%


g/mL

NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Applied Qualifiers|_
                                                             "R2", "M", "DQO"
                                            "DQO (NR)11
X = Attached or Verified


Data Qualifiers

" J"  Concentration reported should be considered an estimate.  The data are acceptable for the use as determined by specific data users but certain QC criteria were not met

"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"  Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
Fish - SERC
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb4-13-00
                      Checked by
Sample
M5-622FSF-1

M5-622FSF-2

M5-622FSF-3

M5-622FSF-4

M5-622FSF-5

M5-622FSF-6

M5-622FSF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM1
DORM1
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV10-
CCV-11
CCV-12
CCV-13
CCV-14
QC
Batch
HO21JF1
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
Qualifier
Note
1^2=0.9989


































Instrument
Reading
Peak Height
126.6
125.9
122.6
122
117.6
119
106.4
103.3
124.2
123.9
110.3
110.1
128.4
127.5
1.4
1.5
0.6
0.4
0.7
39.8
40.3
79.5
79.4
77.4
75.8
76.7
77.2
75.7
75.8
75.5
75.8
81.9
82.1
82.2
82.0
Slope
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
0.3961
Hg
Concentration
(PPt)
319.6
317.8
309.5
308.0
296.9
300.4
268.6
260.8
313.6
312.8
278.5
278.0
324.2
321.9
3.5
3.8
1.5
1.0
1.8
100.5
101.7
200.7
200.5
195.4
191.4
193.6
194.9
191.1
191.4
190.6
191.4
206.8
207.3
207.5
207.0
Vol.
added
(mL)
1
1
0.5
0.5
0.5
0.5
1
1
0.5
0.5
0.5
0.5
1
1
1
1
0.5
0.5
1
0.1
0.1














Average
Reagent
Blank (ng)
0.1925
0.1925
0.1925
0.1925
0.1925
0.1925
0.1925
0.1925
0.1925
0.1925
0.1925
0.1925
0.1925
0.1925





0.1925
0.1925














Corrected Hg
Concentration
(ng)
19.94
19.83
37.88
37.69
36.33
36.76
16.73
16.24
38.38
38.28
34.06
34.00
20.23
20.09
0.22
0.24
0.19
0.12
0.11
60.40
61.16














Weight
offish
fe)
0.2070
0.2070
0.2109
0.2109
0.2712
0.2712
0.1219
0.1219
0.1490
0.1490
0.1634
0.1634
0.1009
0.1009





0.0126
0.0126














Hg
Concentration
ppb
96.34
95.81
179.60
178.72
133.94
135.55
137.25
133.20
257.55
256.93
208.44
208.06
200.49
199.07




0.0018
4793.39
4853.80
0.2007
0.2005
0.1954
0.1914
0.1936
0.1949
0.1911
0.1914
0.1906
0.1914
0.2068
0.2073
0.2075
0.2070
Averaged
Result
ppb

96.08

179.16

134.75

135.23

257.24

208.25

199.78

0.23

0.16
0.0018

4823.60














Averaged
Reported
Result (ppb)













172.93



0.193
0.0018

4823.60













0.196
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)



















4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%



















104.20
105.52
100.35
100.23
97.70
95.68
96.82
97.45
95.56
95.68
95.30
95.68
103.38
103.64
103.76
103.51
Standard
Deviation




















42.72













0.0069
Relative
Standard
Deviation




















0.9













3.51
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-13-00
                        Checked by
Sample
M5-633FSF-1

M5-633FSF-2

M5-633FSF-3

M5-633FSF-4

M5-633FSF-5

M5-633FSF-6

M5-633FSF-7

Method Blank-1

Method Blank-0. 5

Instrument Blank
DORMS
DORMS
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-1 1
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
CCV-17
CCV-18
CCV-19
CCV-20
CCV-2 1
CCV-22
QC
Batch
HO22JF1
11
"
"
11
11
"
"
"
"
"
"
"
"
"
"
"
"
"

"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
"
Qualifier
Note
1^2=1.0000


















11 M"
11 M"






















Instrument
Reading
Peak Height
25.9
26.1
15.6
15.9
47.1
46.8
17.8
17.1
11.2
10.8
13.7
13.2
11.3
11.3
0.5
0.3
0.6
0.2
0.5
71.5
25.6
82.1
81.4
82
81.7
79.7
79.9
80.3
81.1
81.2
81.4
81.7
81.9
79.3
79.4
76.3
77.8
78.7
80.1
80.1
81.5
79.4
79.7
Slope
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
0.4090
Hg
Concentration
(PPt)
63.3
63.8
38.1
38.9
115.2
114.4
43.5
41.8
27.4
26.4
33.5
32.3
27.6
27.6
1.2
0.7
1.5
0.5
1.2
174.8
62.6
200.7
199.0
200.5
199.8
194.9
195.4
196.3
198.3
198.5
199.0
199.8
200.2
193.9
194.1
186.6
190.2
192.4
195.8
195.8
199.3
194.1
194.9
Vol.
added
(mL)
1
1
0.2
0.2
0.5
0.5
0.5
0.5
0.5
0.5
1
1
1
1
1
1
0.5
0.5
1
0.1
0.1






















Average
Reagent
Blank (ng)
0.0925
0.0925
0.0925
0.0925
0.0925
0.0925
0.0925
0.0925
0.0925
0.0925
0.0925
0.0925
0.0925
0.0925





0.0925
0.0925






















Corrected Hg
Concentration
(ng)
3.90
3.93
11.46
11.69
14.07
13.98
5.26
5.05
3.28
3.16
2.02
1.94
1.65
1.65
0.08
0.05
0.18
0.06
0.08
105.32
37.65






















Weight
offish

0.1699
0.1699
0.2727
0.2727
0.1349
0.1349
0.1287
0.1287
0.1183
0.1183
0.0728
0.0728
0.0774
0.0774





0.0125
0.0125






















Hg
Concentration
ppb
22.9
23.1
42.0
42.9
104.3
103.6
40.9
39.2
27.7
26.7
27.7
26.7
21.3
21.3




0.0012
8425.8
3012.0
0.2007
0.1990
0.2005
0.1998
0.1949
0.1954
0.1963
0.1983
0.1985
0.1990
0.1998
0.2002
0.1939
0.1941
0.1866
0.1902
0.1924
0.1958
0.1958
0.1993
0.1941
0.1949
Averaged
Result
ppb

23.03

42.45

103.98

40.06

27.18

27.19

21.29

0.06

0.12
0.0012

5718.89






















Averaged
Reported
Result (ppb)













40.74



0.091
0.0012

5718.889





















0.196
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6

3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)




















4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%




















65.48
100.37
99.51
100.24
99.88
97.43
97.68
98.17
99.14
99.27
99.51
99.88
100.12
96.94
97.07
93.28
95.11
96.21
97.92
97.92
99.63
97.07
97.43
Standard
Deviation




















3828.09





















0.0036
Relative
Standard
Deviation




















66.9





















1.85
"M"  Anaryte exhibits potential matrix effect based on matrix spike n
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-13-00
                      Checked by
Sample
M5-643FSF-1

M5-643FSF-2

M5-643FSF-3

M5-643FSF-4

M5-643FSF-5

M5-643FSF-6

M5-643FSF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM 7
DORM 7
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV10-
CCV-11
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
CCV-17
CCV-18
CCV-19
CCV-20
CCV-2 1
CCV-22
CCV-23
CCV-24
QC
Batch
HO26JF1
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"

11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
Qualifier
Note
1^2=0.9998












































Instrument
Reading
Peak Height
3.1
3.1
31.5
31.1
25.2
25
15.1
15.3
71.2
70.8
5.6
5.8
4.3
4.5
0.50
0.40
0.10
0.00
0.2
38.8
39.7
77.4
77.5
75.8
77.4
73.3
75.1
76.5
74.7
74.5
73.7
75.9
75.9
82.2
82.3
84.1
84.2
83.9
82.7
79.5
80.4
78.1
79.9
78.5
76.9
Slope
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
0.3912
Hg
Concentration
(PPt)
7.9
7.9
80.5
79.5
64.4
63.9
38.6
39.1
182.0
181.0
14.3
14.8
11.0
11.5
1.3
1.0
0.3
0.0
0.5
99.2
101.5
197.9
198.1
193.8
197.9
187.4
192.0
195.6
191.0
190.4
188.4
194.0
194.0
210.1
210.4
215.0
215.2
214.5
211.4
203.2
205.5
199.6
204.2
200.7
196.6
Vol.
added
(mL)
0.2
0.2
0.2
0.2
0.5
0.5
1
1
1
1
1
1
0.5
0.5
1
1
0.5
0.5
1
0.1
0.1
























Average
Reagent
Blank (ng)
0.0425
0.0425
0.0425
0.0425
0.0425
0.0425
0.0425
0.0425
0.0425
0.0425
0.0425
0.0425
0.0425
0.0425





0.0425
0.0425
























Corrected Hg
Concentration
(ng)
2.36
2.36
24.36
24.05
7.88
7.82
2.39
2.42
11.42
11.36
0.86
0.89
1.31
1.37
0.08
0.06
0.03
0.00
0.03
59.76
61.15
























Weight
offish
fe)
0.567
0.567
0.2718
0.2718
0.1505
0.1505
0.087
0.087
0.1084
0.1084
0.0681
0.0681
0.0574
0.0574





0.0127
0.0127
























Hg
Concentration
ppb
4.2
4.2
89.6
88.5
52.4
51.9
27.5
27.8
105.4
104.8
12.6
13.1
22.8
23.9




0.00051
4705.85
4815.08
0.1979
0.1981
0.1938
0.1979
0.1874
0.1920
0.1956
0.1910
0.1904
0.1884
0.1940
0.1940
0.2101
0.2104
0.2150
0.2152
0.2145
0.2114
0.2032
0.2055
0.1996
0.2042
0.2007
0.1966
Averaged
Result
ppb

4.16

89.04

52.16

27.65

105.09

12.86

23.36

0.07

0.02
0.0005

4760.46
























Averaged
Reported
Result (ppb)













44.90



0.044
0.0005

4760.46























0.200
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6

3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)




















4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%




















104.68
98.93
99.05
96.88
98.93
93.69
95.99
97.78
95.48
95.22
94.20
97.01
97.01
105.06
105.19
107.49
107.62
107.23
105.70
101.61
102.76
99.82
102.12
100.33
98.29
Standard
Deviation




















77.24























0.0087
Relative
Standard
Deviation




















1.6























4.36
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-14-00
                      Checked by
Sample
M5-653FSF-1

M5-653FSF-2

M5-653FSF-3

M5-653FSF-4

M5-653FSF-5

M5-653FSF-6

M5-653FSF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM 14
DORM 14
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV10-
CCV-11
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
CCV-17
CCV-18
CCV-19
CCV-20
CCV-2 1
CCV-22
QC
Batch
HO28JF1
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
Qualifier
Note
1^2=0.9982










































Instrument
Reading
Peak Height
3.3
2.9
5.5
5
4.1
3.9
8.9
7.6
3.4
3.2
4.6
4.4
4.4
3.7
0.3
0.3
0.7
0.6
0.7
39
38.5
74.5
75.7
73.1
73.2
76.2
75.4
75
74.9
70.9
71.2
74.4
74.2
74.4
74.4
74.1
73.7
74.1
74.1
73.8
74.6
73.4
74.1
Y Intercept
Slope
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
0.4039
Hg
Concentration
(PPt)
8.2
7.2
13.6
12.4
10.2
9.7
22.0
18.8
8.4
7.9
11.4
10.9
10.9
9.2
0.7
0.7
1.7
1.5
1.7
96.6
95.3
184.5
187.4
181.0
181.2
188.7
186.7
185.7
185.4
175.5
176.3
184.2
183.7
184.2
184.2
183.5
182.5
183.5
183.5
182.7
184.7
181.7
183.5
Vol.
added
(mL)
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.5
0.5
1
0.1
0.1






















Average
Reagent
Blank (ng)
0.1225
0.1225
0.1225
0.1225
0.1225
0.1225
0.1225
0.1225
0.1225
0.1225
0.1225
0.1225
0.1225
0.1225





0.1225
0.1225






















Corrected Hg
Concentration
(ng)
0.39
0.33
0.74
0.66
0.52
0.49
1.27
1.06
0.41
0.38
0.60
0.56
0.56
0.45
0.05
0.05
0.21
0.18
0.11
58.10
57.36






















Weight
offish
fe)
0.0926
0.0926
0.1051
0.1051
0.0923
0.0923
0.1377
0.1377
0.0722
0.0722
0.0728
0.0728
0.0533
0.0533





0.011
0.011






















Hg
Concentration
ppb
4.2
3.6
7.0
6.3
5.6
5.3
9.2
7.7
5.6
5.2
8.2
7.7
10.6
8.5




0.0017
5282.03
5214.17
0.1845
0.1874
0.1810
0.1812
0.1887
0.1867
0.1857
0.1854
0.1755
0.1763
0.1842
0.1837
0.1842
0.1842
0.1835
0.1825
0.1835
0.1835
0.1827
0.1847
0.1817
0.1835
Averaged
Result
ppb

3.90

6.63

5.43

8.46

5.43

7.96

9.55

0.05

0.20
0.0017

5248.10






















Averaged
Reported
Result (ppb)













6.77



0.122
0.0017

5248.10





















0.183
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)



















4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%



















114.83
113.35
92.23
93.71
90.49
90.62
94.33
93.34
92.84
92.72
87.77
88.14
92.10
91.85
92.10
92.10
91.73
91.24
91.73
91.73
91.36
92.35
90.86
91.73
Standard
Deviation




















47.99





















0.0031
Relative
Standard
Deviation




















0.9





















1.67
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-14-00
                      Checked by
Sample
M5-663FSF-1

M5-663FSF-2

M5-663FSF-3

M5-663FSF-4

M5-663FSF-5

M5-663FSF-6

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM 15
DORM 15
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-1 1
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
CCV-17
CCV-18
CCV-19
CCV-20
CCV-2 1
CCV-22
QC
Batch
HO28JF2
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
Qualifier
Note
1^2=0.9990








































Instrument
Reading
Peak Height
171.8
172.4
127.1
133.7
88.5
89.5
86
87.7
67.4
67.2
69.8
62.5
1.2
1
2.1
1.4
0.65
38.6
37.8
89.7
91.8
82.3
88.6
88.3
89.3
80.1
88.8
90.4
89.7
77.5
86.2
87.3
86.4
77.5
86
84.7
85.6
77.7
84.2
85.6
85.5
Slope
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
0.4316
Hg
Concentration
(ppt)
398.1
399.4
294.5
309.8
205.1
207.4
199.3
203.2
156.2
155.7
161.7
144.8
2.8
2.3
4.9
3.2
1.5
89.4
87.6
207.8
212.7
190.7
205.3
204.6
206.9
185.6
205.7
209.5
207.8
179.6
199.7
202.3
200.2
179.6
199.3
196.2
198.3
180.0
195.1
198.3
198.1
Vol.
added
(mL)
1
1
1
1
1
1
1
1
1
1
0.5
0.5
1
1
0.5
0.5
1
0.1
0.1






















Average
Reagent
Blank (ng)
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325





0.3325
0.3325






















Corrected Hg
Concentration
(ng)
24.74
24.83
18.22
19.18
12.59
12.73
12.22
12.47
9.51
9.48
19.56
17.48
0.18
0.15
0.60
0.40
0.09
53.60
52.48






















Weight
offish
(g)
0.1356
0.1356
0.112
0.112
0.1073
0.1073
0.1079
0.1079
0.0964
0.0964
0.1626
0.1626





0.0109
0.0114






















Hg
Concentration
ppb
182.48
183.13
162.68
171.28
117.29
118.65
113.26
115.56
98.61
98.30
120.29
107.50




0.0015
4917.1
4603.4
0.2078
0.2127
0.1907
0.2053
0.2046
0.2069
0.1856
0.2057
0.2095
0.2078
0.1796
0.1997
0.2023
0.2002
0.1796
0.1993
0.1962
0.1983
0.1800
0.1951
0.1983
0.1981
Averaged
Result
ppb

182.81

166.98

117.97

114.41

98.46

113.90

0.16

0.50
0.0015

4760.27






















Averaged
Reported
Result (ppb)











132.42



0.330
0.0015

4760.27





















0.198
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)

















4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%

















106.89
100.07
103.92
106.35
95.34
102.64
102.29
103.45
92.79
102.87
104.73
103.92
89.78
99.86
101.14
100.09
89.78
99.63
98.12
99.17
90.01
97.54
99.17
99.05
Standard
Deviation


















221.82





















0.0098
Relative
Standard
Deviation


















4.7





















4.95
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-14-00
                      Checked by
Sample
M5-673FSF-1

M5-673FSF-2

M5-673FSF-3

M5-673FSF-4

M5-673FSF-5

M5-673FSF-6

M5-673FSF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM 22
DORM 22
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-1 1
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
QC
Batch
HO29JF1
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
Qualifier
Note
1^2=0.9993




































Instrument
Reading
Peak Height
139.5
141
95.7
105.5
90.7
90.8
44.5
47.3
137.5
137.4
61.7
67.7
59.2
59.5
0.9
0.7
0.6
0.6
0.15
32.7
34.9
83.4
83.7
74.9
82.8
80.8
80.4
74.2
80.7
83.2
82.4
77.8
83
82.2
82.7
77.3
83
Slope
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
0.4124
Hg
Concentration
(PPt)
338.3
341.9
232.1
255.8
219.9
220.2
107.9
114.7
333.4
333.2
149.6
164.2
143.5
144.3
2.2
1.7
1.5
1.5
0.4
79.3
84.6
202.2
203.0
181.6
200.8
195.9
195.0
179.9
195.7
201.7
199.8
188.7
201.3
199.3
200.5
187.4
201.3
Vol.
added
(mL)
0.5
0.5
0.5
0.5
1
1
0.2
0.2
1
1
0.5
0.5
1
1
1
1
0.5
0.5
1
0.1
0.1
















Average
Reagent
Blank (ng)
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325





0.3325
0.3325
















Corrected Hg
Concentration
(ng)
41.27
41.72
28.21
31.13
13.52
13.54
32.36
34.42
20.67
20.66
18.07
19.86
8.71
8.76
0.14
0.11
0.18
0.18
0.02
47.48
50.70
















Weight
offish
fe)
0.1786
0.1786
0.1504
0.1504
0.0999
0.0999
0.1894
0.1894
0.1001
0.1001
0.1476
0.1476
0.0764
0.0764





0.0126
0.0126
















Hg
Concentration
ppb
231.10
233.60
187.57
207.00
135.37
135.52
170.87
181.73
206.52
206.37
122.42
134.55
114.02
114.62




0.0004
3768.3
4023.6
0.2022
0.2030
0.1816
0.2008
0.1959
0.1950
0.1799
0.1957
0.2017
0.1998
0.1887
0.2013
0.1993
0.2005
0.1874
0.2013
Averaged
Result
ppb

232.35

197.29

135.44

176.30

206.44

128.49

114.32

0.12

0.18
0.0004

3895.95
















Averaged
Reported
Result (ppb)













170.09



0.151
0.0004

3895.95















0.196
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)



















4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%



















81.92
87.47
101.12
101.48
90.81
100.39
97.96
97.48
89.96
97.84
100.87
99.90
94.33
100.63
99.66
100.27
93.72
100.63
Standard
Deviation




















180.52















0.0075
Relative
Standard
Deviation




















4.6















3.82
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-14-00
                      Checked by
Sample
M5-683FSF-1

M5-683FSF-2

M5-683FSF-3

M5-683FSF-4

M5-683FSF-5

M5-683FSF-6

M5-683FSF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM 26
DORM 26
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-1 1
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
CCV-17
CCV-18
CCV-19
CCV-20
QC
Batch
HO01KF1
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
Qualifier
Note
1^2=0.9998








































Instrument
Reading
Peak Height
118.1
117
96.6
96.3
86.8
87.3
110.4
109.5
42.8
41.9
65.5
66.4
105.2
105.2
0.5
0.4
0.3
0.2
0.2
37.4
37.7
89.2
88.2
86.7
89
89
88.7
88.8
88.5
87.2
88.4
82.4
89.3
86.9
87.7
88.1
87.1
85.9
86
85.7
85.7
Slope
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
0.4151
Hg
Concentration
(PPt)
284.5
281.9
232.7
232.0
209.1
210.3
266.0
263.8
103.1
100.9
157.8
160.0
253.4
253.4
1.20
0.96
0.72
0.48
0.48
90.1
90.8
214.9
212.5
208.9
214.4
214.4
213.7
213.9
213.2
210.1
213.0
198.5
215.1
209.3
211.3
212.2
209.8
206.9
207.2
206.5
206.5
Vol.
added
(mL)
0.5
0.5
0.5
0.5
0.2
0.2
0.5
0.5
0.5
0.5
1
1
1
1
1
1
0.5
0.5
1
0.1
0.1




















Average
Reagent
Blank (ng)
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325
0.3325





0.3325
0.3325




















Corrected Hg
Concentration
(ng)
34.66
34.34
28.29
28.20
63.03
63.39
32.38
32.11
12.35
12.08
9.61
9.75
15.63
15.63
0.08
0.06
0.09
0.06
0.03
54.00
54.43




















Weight
offish
fe)
0.1167
0.1167
0.1212
0.1212
0.1936
0.1936
0.1369
0.1369
0.0867
0.0867
0.0917
0.0917
0.0804
0.0804





0.0109
0.0109




















Hg
Concentration
ppb
297.02
294.23
233.43
232.69
325.55
327.44
236.53
234.58
142.44
139.37
104.78
106.27
194.45
194.45




0.0005
4953.9
4993.8
0.2149
0.2125
0.2089
0.2144
0.2144
0.2137
0.2139
0.2132
0.2101
0.2130
0.1985
0.2151
0.2093
0.2113
0.2122
0.2098
0.2069
0.2072
0.2065
0.2065
Averaged
Result
ppb

295.62

233.06

326.49

235.55

140.90

105.53

194.45

0.07

0.07
0.0005

4973.85




















Averaged
Reported
Result (ppb)













218.80



0.071
0.0005

4973.85



















0.211
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)



















4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%



















107.69
108.56
107.44
106.24
104.43
107.20
107.20
106.84
106.96
106.60
105.03
106.48
99.25
107.56
104.67
105.64
106.12
104.91
103.47
103.59
103.23
103.23
Standard
Deviation




















28.27



















0.0041
Relative
Standard
Deviation




















0.6



















1.94
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-14-00
                      Checked by
Sample
M5-693FSF-1

M5-693FSF-2

M5-693FSF-3

M5-693FSF-4

M5-693FSF-5

M5-693FSF-6

M5-693FSF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM 31
DORM 31
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-1 1
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
QC
Batch
HO02KF1
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
Qualifier
Note
1^2=0.9996




































Instrument
Reading
Peak Height
60.2
64.5
69.7
70
30.2
31.6
5.5
5.6
68.5
74.5
37.1
37.2
51.8
54.6
0.5
0.4
0.3
0.4
0.6
40.3
40
83.8
85.1
79.7
86
86.7
86.9
82.3
88.1
89.4
89.7
88.2
91.3
95.4
95.3
86.5
95
Slope
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
0.4174
Hg
Concentration
(PPt)
144.2
154.5
167.0
167.7
72.4
75.7
13.2
13.4
164.1
178.5
88.9
89.1
124.1
130.8
1.20
0.96
0.72
0.96
1.44
96.6
95.8
200.8
203.9
190.9
206.0
207.7
208.2
197.2
211.1
214.2
214.9
211.3
218.7
228.6
228.3
207.2
227.6
Vol.
added
(mL)
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.5
0.5
1
0.1
0.1
















Average
Reagent
Blank (ng)
0.3325
0.3325
0.0875
0.0875
0.0875
0.0875
0.0875
0.0875
0.0875
0.0875
0.0875
0.0875
0.0875
0.0875





0.0875
0.0875
















Corrected Hg
Concentration
(ng)
8.75
9.40
10.43
10.48
4.47
4.68
0.74
0.76
10.25
11.16
5.51
5.53
7.73
8.15
0.08
0.06
0.09
0.12
0.09
58.13
57.70
















Weight
offish
fe)
0.0549
0.0549
0.0425
0.0425
0.0373
0.0373
0.0095
0.0095
0.0608
0.0608
0.0397
0.0397
0.0699
0.0699





0.0126
0.0126
















Hg
Concentration
ppb
159.45
171.27
245.47
246.54
119.86
125.52
78.17
79.76
168.61
183.51
138.85
139.23
110.60
116.65




0.0014
4613.7
4579.3
0.2008
0.2039
0.1909
0.2060
0.2077
0.2082
0.1972
0.2111
0.2142
0.2149
0.2113
0.2187
0.2286
0.2283
0.2072
0.2276
Averaged
Result
ppb

165.36

246.01

122.69

78.97

176.06

139.04

113.62

0.07

0.10
0.0014

4596.47
















Averaged
Reported
Result (ppb)













148.82



0.086
0.0014

4596.47















0.211
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)



















4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%



















100.30
99.55
100.38
101.94
95.47
103.02
103.86
104.10
98.59
105.53
107.09
107.45
105.65
109.37
114.28
114.16
103.62
113.80
Standard
Deviation




















24.32















0.0109
Relative
Standard
Deviation




















0.5















5.15
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-14-00
                      Checked by
Sample
M5-703FSF-1

M5-703FSF-2

M5-703FSF-3

M5-703FSF-4

M5-703FSF-5

M5-703FSF-6

M5-703FSF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM 29
DORM 29
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-1 1
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
CCV-17
CCV-18
CCV-19
CCV-20
QC
Batch
HO05KF1
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
Qualifier
Note
1^2=0.9991








































Instrument
Reading
Peak Height
38.4
38.7
46.9
47
58.7
59.1
97.7
97.7
52.7
54.7
92.5
93.2
84.8
84.5
0.6
0.8
0.3
0.3
0.35
33.4
33.2
79.2
79.5
85
85.2
83.9
85
85.5
82.6
84.8
83
83.6
86.3
84.2
85.3
83.3
83.9
82.9
83.6
83
83.3
Slope
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
Hg
Concentration
(PPt)
97.1
97.8
118.6
118.8
148.4
149.4
247.0
247.0
133.2
138.3
233.8
235.6
214.4
213.6
1.52
2.02
0.76
0.76
0.88
84.4
83.9
200.2
201.0
214.9
215.4
212.1
214.9
216.1
208.8
214.4
209.8
211.3
218.1
212.8
215.6
210.6
212.1
209.6
211.3
209.8
210.6
Vol.
added
(mL)
0.1
0.1
0.1
0.1
0.5
0.5
0.5
0.5
0.5
0.5
1
1
1
1
1
1
0.5
0.5
1
0.1
0.1




















Average
Reagent
Blank (ng)
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025





0.1025
0.1025




















Corrected Hg
Concentration
(ng)
58.43
58.89
71.39
71.54
18.15
18.27
30.27
30.27
16.28
16.90
14.63
14.74
13.40
13.35
0.10
0.13
0.09
0.09
0.06
50.81
50.50




















Weight
offish
fe)
0.2116
0.2116
0.223
0.223
0.0806
0.0806
0.103
0.103
0.0736
0.0736
0.0796
0.0796
0.0849
0.0849





0.0109
0.0109




















Hg
Concentration
ppb
276.13
278.29
320.11
320.80
225.17
226.71
293.93
293.93
221.24
229.69
183.77
185.17
157.86
157.29




0.0009
4661.3
4633.3
0.2002
0.2010
0.2149
0.2154
0.2121
0.2149
0.2161
0.2088
0.2144
0.2098
0.2113
0.2181
0.2128
0.2156
0.2106
0.2121
0.2096
0.2113
0.2098
0.2106
Averaged
Result
ppb

277.21

320.46

225.94

293.93

225.46

184.47

157.58

0.11

0.09
0.0009

4647.30




















Averaged
Reported
Result (ppb)













240.72



0.102
0.0009

4647.30



















0.211
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)



















4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%



















101.33
100.72
100.10
100.48
107.43
107.68
106.04
107.43
108.06
104.40
107.18
104.90
105.66
109.07
106.42
107.81
105.28
106.04
104.78
105.66
104.90
105.28
Standard
Deviation




















19.78



















0.0045
Relative
Standard
Deviation




















0.4



















2.14
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-14-00
                      Checked by
Sample
M5-703FSF-1

M5-703FSF-2

M5-703FSF-3

M5-703FSF-4

M5-703FSF-5

M5-703FSF-6

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM 37
DORM 37
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-1 1
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
CCV-17
CCV-18
CCV-19
CCV-20
CCV-2 1
CCV-22
QC
Batch
HO09KF1
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
Qualifier
Note
1^2=0.9999








































Instrument
Reading
Peak Height
35.3
36.4
41.4
41.3
58.2
58
104.9
103.5
54.5
54
92.3
93.3
0.5
0.3
0.3
0.4
0.3
42.2
42.6
75.7
76.2
82.5
83.1
83.6
83.8
82.8
83.6
80.7
80.8
73.6
74.6
72.3
72.3
72.9
73.9
0.7
0.5
0.5
0.1
75.8
77.2
Slope
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
Hg
Concentration
(PPt)
91.8
94.7
107.7
107.4
151.4
150.8
272.8
269.2
141.7
140.4
240.1
242.7
1.30
0.78
0.78
1.04
0.78
109.8
110.8
196.9
198.2
214.6
216.1
217.4
217.9
215.3
217.4
209.9
210.1
191.4
194.0
188.0
188.0
189.6
192.2
1.8
1.3
1.3
0.3
197.1
200.8
Vol.
added
(mL)
0.1
0.1
0.1
0.1
0.5
0.5
0.5
0.5
0.5
0.5
1
1
1
1
0.5
0.5
1
0.1
0.1






















Average
Reagent
Blank (ng)
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900





0.0900
0.0900






















Corrected Hg
Concentration
(ng)
55.27
57.00
64.84
64.68
18.53
18.46
33.47
33.02
17.34
17.18
15.03
15.20
0.08
0.05
0.10
0.13
0.05
66.09
66.72






















Weight
offish
fe)
0.2116
0.2116
0.223
0.223
0.0806
0.0806
0.103
0.103
0.0736
0.0736
0.0796
0.0796





0.014
0.014






















Hg
Concentration
ppb
261.20
269.35
290.75
290.04
229.88
229.08
324.92
320.58
235.66
233.48
188.86
190.92




0.0008
4720.8
4765.6
0.1969
0.1982
0.2146
0.2161
0.2174
0.2179
0.2153
0.2174
0.2099
0.2101
0.1914
0.1940
0.1880
0.1880
0.1896
0.1922
0.0018
0.0013
0.0013
0.0003
0.1971
0.2008
Averaged
Result
ppb

265.28

290.39

229.48

322.75

234.57

189.89

0.07

0.11
0.0008

4743.19






















Averaged
Reported
Result (ppb)











255.39



0.089
0.0008

4743.19





















0.166
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)

















4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%

















102.63
103.60
98.44
99.09
107.28
108.06
108.71
108.97
107.67
108.71
104.94
105.07
95.71
97.01
94.02
94.02
94.80
96.10
0.91
0.65
0.65
0.13
98.57
100.39
Standard
Deviation


















31.68





















0.0804
Relative
Standard
Deviation


















0.7





















48.31
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-14-00
                      Checked by
Sample
M5-714FSF-1

M5-714FSF-2

M5-714FSF-3

M5-714FSF-4

M5-714FSF-5

M5-714FSF-6

M5-714FSF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM 29
DORM 29
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-1 1
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
CCV-17
CCV-18
CCV-19
CCV-20
QC
Batch
HO05KF1
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
Qualifier
Note
1^2=0.9991








































Instrument
Reading
Peak Height
119.5
120.4
86.9
86.7
71.6
70.1
99.9
101
121.2
120.3
119.4
118.9
111.2
110
0.6
0.8
0.3
0.3
0.35
33.4
33.2
79.2
79.5
85
85.2
83.9
85
85.5
82.6
84.8
83
83.6
86.3
84.2
85.3
83.3
83.9
82.9
83.6
83
83.3
Slope
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
0.3956
Hg
Concentration
(PPt)
302.1
304.3
219.7
219.2
181.0
177.2
252.5
255.3
306.4
304.1
301.8
300.6
281.1
278.1
1.52
2.02
0.76
0.76
0.88
84.4
83.9
200.2
201.0
214.9
215.4
212.1
214.9
216.1
208.8
214.4
209.8
211.3
218.1
212.8
215.6
210.6
212.1
209.6
211.3
209.8
210.6
Vol.
added
(mL)
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
1
1
1
1
1
1
0.5
0.5
1
0.1
0.1




















Average
Reagent
Blank (ng)
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025
0.1025





0.1025
0.1025




















Corrected Hg
Concentration
(ng)
37.05
37.33
26.92
26.85
22.16
21.69
30.96
31.30
37.58
37.30
18.91
18.83
17.61
17.42
0.10
0.13
0.09
0.09
0.06
50.81
50.50




















Weight
offish
fe)
0.1451
0.1451
0.1138
0.1138
0.1586
0.1586
0.1611
0.1611
0.1041
0.1041
0.0880
0.0880
0.0649
0.0649





0.0109
0.0109




















Hg
Concentration
ppb
255.36
257.29
236.52
235.98
139.72
136.78
192.17
194.29
361.01
358.32
214.91
214.01
271.28
268.34




0.0009
4661.3
4633.3
0.2002
0.2010
0.2149
0.2154
0.2121
0.2149
0.2161
0.2088
0.2144
0.2098
0.2113
0.2181
0.2128
0.2156
0.2106
0.2121
0.2096
0.2113
0.2098
0.2106
Averaged
Result
ppb

256.32

236.25

138.25

193.23

359.66

214.46

269.81

0.11

0.09
0.0009

4647.30




















Averaged
Reported
Result (ppb)













238.28



0.102
0.0009

4647.30



















0.211
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)



















4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%



















101.33
100.72
100.10
100.48
107.43
107.68
106.04
107.43
108.06
104.40
107.18
104.90
105.66
109.07
106.42
107.81
105.28
106.04
104.78
105.66
104.90
105.28
Standard
Deviation




















19.78



















0.0045
Relative
Standard
Deviation




















0.4



















2.14
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-14-00
                      Checked by
Sample
M5-714FSF-1

M5-714FSF-2

M5-714FSF-3

M5-714FSF-4

M5-714FSF-5

M5-714FSF-6

M5-714FSF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM 37
DORM 37
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-1 1
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
CCV-2 1
CCV-22
QC
Batch
HO09KF1
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
Qualifier
Note
1^2=0.9999






































Instrument
Reading
Peak Height
129.5
133.1
88.5
89
82.4
82
111.7
108.9
121
124.6
129.5
127.8
110.4
108
0.5
0.3
0.3
0.4
0.3
42.2
42.6
75.7
76.2
82.5
83.1
83.6
83.8
82.8
83.6
80.7
80.8
73.6
74.6
72.3
72.3
72.9
73.9
75.8
77.2
Slope
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
Hg
Concentration
(PPt)
336.8
346.2
230.2
231.5
214.3
213.3
290.5
283.2
314.7
324.1
336.8
332.4
287.1
280.9
1.30
0.78
0.78
1.04
0.78
109.8
110.8
196.9
198.2
214.6
216.1
217.4
217.9
215.3
217.4
209.9
210.1
191.4
194.0
188.0
188.0
189.6
192.2
197.1
200.8
Vol.
added
(mL)
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
1
1
1
1
1
1
0.5
0.5
1
0.1
0.1


















Average
Reagent
Blank (ng)
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900





0.0900
0.0900


















Corrected Hg
Concentration
(ng)
41.34
42.49
28.22
28.38
26.27
26.14
35.64
34.75
38.62
39.77
21.13
20.85
18.00
17.61
0.08
0.05
0.10
0.13
0.05
66.09
66.72


















Weight
offish
fe)
0.1451
0.1451
0.1138
0.1138
0.1586
0.1586
0.1611
0.1611
0.1041
0.1041
0.0880
0.0880
0.0649
0.0649





0.014
0.014


















Hg
Concentration
ppb
284.88
292.82
247.99
249.39
165.63
164.83
221.24
215.68
370.96
382.03
240.10
236.93
277.33
271.27




0.0008
4720.8
4765.6
0.1969
0.1982
0.2146
0.2161
0.2174
0.2179
0.2153
0.2174
0.2099
0.2101
0.1914
0.1940
0.1880
0.1880
0.1896
0.1922
0.1971
0.2008
Averaged
Result
ppb

288.85

248.69

165.23

218.46

376.50

238.51

274.30

0.07

0.11
0.0008

4743.19


















Averaged
Reported
Result (ppb)













258.65



0.089
0.0008

4743.19

















0.203
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)



















4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%



















102.63
103.60
98.44
99.09
107.28
108.06
108.71
108.97
107.67
108.71
104.94
105.07
95.71
97.01
94.02
94.02
94.80
96.10
98.57
100.39
Standard
Deviation




















31.68

















0.0115
Relative
Standard
Deviation




















0.7

















5.67
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-14-00
                      Checked by
Sample
M5-726FSF-1

M5-726FSF-2

M5-726FSF-3

M5-726FSF-4

M5-726FSF-5

M5-726FSF-6

M5-726FSF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM 37
DORM 37
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-1 1
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
CCV-2 1
CCV-22
QC
Batch
HO09KF1
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
Qualifier
Note
1^2=0.9999






































Instrument
Reading
Peak Height
56.8
57.4
26.3
26.4
44.1
44.3
21.3
21.1
38.5
40.7
15
14.8
22.4
22.3
0.5
0.3
0.3
0.4
0.3
42.2
42.6
75.7
76.2
82.5
83.1
83.6
83.8
82.8
83.6
80.7
80.8
73.6
74.6
72.3
72.3
72.9
73.9
75.8
77.2
Slope
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
0.3845
Hg
Concentration
(PPt)
147.7
149.3
68.4
68.7
114.7
115.2
55.4
54.9
100.1
105.9
39.0
38.5
58.3
58.0
1.30
0.78
0.78
1.04
0.78
109.8
110.8
196.9
198.2
214.6
216.1
217.4
217.9
215.3
217.4
209.9
210.1
191.4
194.0
188.0
188.0
189.6
192.2
197.1
200.8
Vol.
added
(mL)
0.2
0.2
0.2
0.2
0.2
0.2
1
1
1
1
1
1
1
1
1
1
0.5
0.5
1
0.1
0.1


















Average
Reagent
Blank (ng)
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900
0.0900





0.0900
0.0900


















Corrected Hg
Concentration
(ng)
44.67
45.14
20.64
20.71
34.66
34.82
3.40
3.37
6.22
6.58
2.37
2.33
3.58
3.56
0.08
0.05
0.10
0.13
0.05
66.09
66.72


















Weight
offish
fe)
0.2004
0.2004
0.1542
0.1542
0.1778
0.1778
0.1063
0.1063
0.0667
0.0667
0.0720
0.0720
0.1005
0.1005





0.014
0.014


















Hg
Concentration
ppb
222.91
225.27
133.82
134.33
194.95
195.84
31.98
31.68
93.23
98.63
32.89
32.43
35.62
35.46




0.0008
4720.8
4765.6
0.1969
0.1982
0.2146
0.2161
0.2174
0.2179
0.2153
0.2174
0.2099
0.2101
0.1914
0.1940
0.1880
0.1880
0.1896
0.1922
0.1971
0.2008
Averaged
Result
ppb

224.09

134.08

195.39

31.83

95.93

32.66

35.54

0.07

0.11
0.0008

4743.19


















Averaged
Reported
Result (ppb)













107.07



0.089
0.0008

4743.19

















0.203
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)



















4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%



















102.63
103.60
98.44
99.09
107.28
108.06
108.71
108.97
107.67
108.71
104.94
105.07
95.71
97.01
94.02
94.02
94.80
96.10
98.57
100.39
Standard
Deviation




















31.68

















0.0115
Relative
Standard
Deviation




















0.7

















5.67
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-14-00
                      Checked by
Sample
M5-738FSF-1

M5-738FSF-2

M5-738FSF-3

M5-738FSF-4

M5-738FSF-5

M5-738FSF-6

M5-738FSF-7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM 47
DORM 47
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-1 1
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
CCV-17
CCV-18
QC
Batch
HO12KF1
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
Qualifier
Note
1^2=0.9994






































Instrument
Reading
Peak Height
21.5
21.1
17.9
18.2
18.7
18.7
18.9
18.9
29.8
29.8
28
28.1
15.4
14.9
1.2
0.9
0.1
0.5
0.5
48.3
48.5
80.2
80.8
75.5
79.8
79.8
79.6
79.5
79.8
76.8
80
79.2
79.6
74.9
79.8
78.1
78
76.9
78.4
Slope
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
0.4012
Hg
Concentration
(PPt)
53.6
52.6
44.6
45.4
46.6
46.6
47.1
47.1
74.3
74.3
69.8
70.0
38.4
37.1
2.99
2.24
0.25
1.25
1.25
120.4
120.9
199.9
201.4
188.2
198.9
198.9
198.4
198.2
198.9
191.4
199.4
197.4
198.4
186.7
198.9
194.7
194.4
191.7
195.4
Vol.
added
(mL)
0.5
0.5
0.5
0.5
0.2
0.2
1
1
1
1
1
1
1
1
1
1
0.5
0.5
1
0.1
0.1


















Average
Reagent
Blank (ng)
0.1275
0.1275
0.1275
0.1275
0.1275
0.1275
0.1275
0.1275
0.1275
0.1275
0.1275
0.1275
0.1275
0.1275





0.1275
0.1275


















Corrected Hg
Concentration
(ng)
6.46
6.34
5.36
5.45
14.00
14.00
2.84
2.84
4.55
4.55
4.27
4.29
2.29
2.21
0.19
0.14
0.03
0.15
0.08
72.47
72.77


















Weight
offish
fe)
0.1478
0.1478
0.1318
0.1318
0.1996
0.1996
0.0906
0.0906
0.1315
0.1315
0.0317
0.0317
0.0707
0.0707





0.0152
0.0152


















Hg
Concentration
ppb
43.73
42.90
40.67
41.37
70.12
70.12
31.35
31.35
34.62
34.62
134.68
135.17
32.40
31.29




0.0012
4767.6
4787.3
0.1999
0.2014
0.1882
0.1989
0.1989
0.1984
0.1982
0.1989
0.1914
0.1994
0.1974
0.1984
0.1867
0.1989
0.1947
0.1944
0.1917
0.1954
Averaged
Result
ppb

43.32

41.02

70.12

31.35

34.62

134.93

31.85

0.16

0.09
0.0012

4777.45


















Averaged
Reported
Result (ppb)













55.31



0.128
0.0012

4777.45

















0.196
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)



















4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%



















103.64
104.07
99.95
100.70
94.09
99.45
99.45
99.20
99.08
99.45
95.71
99.70
98.70
99.20
93.34
99.45
97.33
97.21
95.84
97.71
Standard
Deviation




















13.98

















0.0042
Relative
Standard
Deviation




















0.3

















2.14
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-14-00
                      Checked by
Sample
M5-828FSF-1

M5-828FSF-2

M5-828FSF-3

M5-828FSF-4

M5-828FSF-5

M5-828FSF-6

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM 49
DORM 49
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-1 1
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
CCV-17
CCV-18
CCV-19
CCV-20
CCV-2 1
CCV-22
CCV-23
CCV-24
QC
Batch
HO16KF1
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
Qualifier
Note
1^2=1.0000










































Instrument
Reading
Peak Height
83.9
84.1
24.8
24.6
54.1
53
152.9
152.9
67.8
67.7
107.9
108.6
1
0.5
0.2
0.2
0.55
49.5
49.8
85.7
86.6
85.8
86.1
84.8
84.6
82.3
85.4
87.7
88.1
86.1
90
90
90.7
86.1
89.8
90.4
90.9
86.8
90.8
89.6
89.7
89.6
89.5
Slope
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
0.4302
Hg
Concentration
(PPt)
195.0
195.5
57.6
57.2
125.8
123.2
355.4
355.4
157.6
157.4
250.8
252.4
2.32
1.16
0.46
0.46
1.28
115.1
115.8
199.2
201.3
199.4
200.1
197.1
196.7
191.3
198.5
203.9
204.8
200.1
209.2
209.2
210.8
200.1
208.7
210.1
211.3
201.8
211.1
208.3
208.5
208.3
208.0
Vol.
added
(mL)
0.5
0.5
0.1
0.1
0.1
0.1
1
1
1
1
0.5
0.5
1
1
0.5
0.5
1
0.1
0.1
























Average
Reagent
Blank (ng)
0.0850
0.0850
0.0850
0.0850
0.0850
0.0850
0.0850
0.0850
0.0850
0.0850
0.0850
0.0850





0.0850
0.0850
























Corrected Hg
Concentration
(ng)
23.90
23.96
34.68
34.40
75.75
74.20
22.31
22.31
9.84
9.83
30.77
30.97
0.15
0.07
0.06
0.06
0.08
69.30
69.72
























Weight
offish
fe)
0.1472
0.1472
0.2229
0.2229
0.2527
0.2527
0.0928
0.0928
0.0316
0.0316
0.1142
0.1142





0.016
0.016
























Hg
Concentration
ppb
162.39
162.77
155.57
154.31
299.74
293.64
240.37
240.37
311.51
311.05
269.40
271.15




0.0013
4331.1
4357.4
0.1992
0.2013
0.1994
0.2001
0.1971
0.1967
0.1913
0.1985
0.2039
0.2048
0.2001
0.2092
0.2092
0.2108
0.2001
0.2087
0.2101
0.2113
0.2018
0.2111
0.2083
0.2085
0.2083
0.2080
Averaged
Result
ppb

162.58

154.94

296.69

240.37

311.28

270.27

0.11

0.06
0.0013

4344.26
























Averaged
Reported
Result (ppb)











239.36



0.084
0.0013

4344.26























0.204
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)

















4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%

















94.15
94.73
99.60
100.65
99.72
100.07
98.56
98.33
95.65
99.26
101.93
102.39
100.07
104.60
104.60
105.42
100.07
104.37
105.07
105.65
100.88
105.53
104.14
104.25
104.14
104.02
Standard
Deviation


















18.58























0.0056
Relative
Standard
Deviation


















0.4























2.76
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-14-00
                      Checked by
Sample
M5-944FSF-1

M5-944FSF-2

M5-944FSF-3

M5-944FSF-4

M5-944FSF-5

M5-944FSF-6

M5-944FSF7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM 52
DORM 52
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-10
CCV-1 1
CCV-12
CCV-13
CCV-14
CCV-15
CCV-16
CCV-17
CCV-18
QC
Batch
HO15KF1
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
"
11
11
"
Qualifier
Note
1^2=0.9999






































Instrument
Reading
Peak Height
98
96.1
38.6
39.8
77.6
77.6
66.3
70.1
36.7
36.8
30.5
32.6
23.3
23.5
2.8
2.6
0.4
0.4
0.6
41.3
40.7
83.4
84.2
79.2
82.9
83.2
82.5
82
82.3
82.3
82.7
82
82.8
81.1
81.8
78.9
80
80.1
79.7
Slope
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
Hg
Concentration
(PPt)
234.5
230.0
92.4
95.2
185.7
185.7
158.7
167.7
87.8
88.1
73.0
78.0
55.8
56.2
6.70
6.22
0.96
0.96
1.44
98.8
97.4
199.6
201.5
189.5
198.4
199.1
197.4
196.2
196.9
196.9
197.9
196.2
198.1
194.1
195.7
188.8
191.4
191.7
190.7
Vol.
added
(mL)
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.5
0.5
1
0.1
0.1


















Average
Reagent
Blank (ng)
0.2625
0.2625
0.2625
0.2625
0.2625
0.2625
0.2625
0.2625
0.2625
0.2625
0.2625
0.2625
0.2625
0.2625





0.2625
0.2625


















Corrected Hg
Concentration
(ng)
14.51
14.22
5.56
5.74
11.44
11.44
9.73
10.31
5.27
5.29
4.34
4.65
3.25
3.28
0.42
0.39
0.12
0.12
0.09
59.33
58.46


















Weight
offish
fe)
0.0872
0.0872
0.0773
0.0773
0.0754
0.0754
0.0842
0.0842
0.0389
0.0389
0.0434
0.0434
0.0361
0.0361





0.0136
0.0136


















Hg
Concentration
ppb
166.41
163.13
71.88
74.22
151.67
151.67
115.59
122.39
135.48
135.87
99.90
107.19
90.03
90.86




0.0014
4362.5
4298.9
0.1996
0.2015
0.1895
0.1984
0.1991
0.1974
0.1962
0.1969
0.1969
0.1979
0.1962
0.1981
0.1941
0.1957
0.1888
0.1914
0.1917
0.1907
Averaged
Result
ppb

164.77

73.05

151.67

118.99

135.67

103.54

90.45

0.41

0.12
0.0014

4330.70


















Averaged
Reported
Result (ppb)













119.74



0.262
0.0014

4330.70

















0.196
Detection
Limn7*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)



















4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%



















94.84
93.45
99.78
100.74
94.76
99.19
99.55
98.71
98.11
98.47
98.47
98.95
98.11
99.07
97.03
97.87
94.40
95.72
95.84
95.36
Standard
Deviation




















45.01

















0.0037
Relative
Standard
Deviation




















1.0

















1.89
-------
10 % Recalculated Results for Total Mercury in Fish Tissue
Analyzed by Florida International University (SERC) for the September 1999 Wet Season (M5)
Entered by mwb 4-14-00
Checked by
                                        NJS 4-14-00
Sample
M5-944FSF-1

M5-944FSF-2

M5-944FSF-3

M5-944FSF-4

M5-944FSF-5

M5-944FSF-6

M5-944FSF7

METHOD BLK-1

METHOD BLK-0.5

Instrument Blank
DORM 52
DORM 52
CCV-1
CCV-2
CCV-3
CCV-4
CCV-5
CCV-6
CCV-7
CCV-8
CCV-9
CCV-1 0
CCV-1 1
CCV-1 2
CCV-1 3
CCV-1 4
CCV-1 5
CCV-1 6
CCV-1 7
CCV-1 8
QC
Batch
HG15KF1
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
Qualifier
Note
1*2=0.9999






































Instrument
Reading
Peak Height
98
96.1
38.6
39.8
77.6
77.6
66.3
70.1
36.7
36.8
30.5
32.6
23.3
23.5
2.8
2.6
0.4
0.4
0.6
41.3
40.7
83.4
84.2
79.2
82.9
83.2
82.5
82
82.3
82.3
82.7
82
82.8
81.1
81.8
78.9
80
80.1
79.7
Slope
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
0.4179
Hg
Concentration
(HP*)
234.5
230.0
92.4
95.2
185.7
185.7
158.7
167.7
87.8
88.1
73.0
78.0
55.8
56.2
6.70
6.22
0.96
0.96
1.44
98.8
97.4
199.6
201.5
189.5
198.4
199.1
197.4
196.2
196.9
196.9
197.9
196.2
198.1
194.1
195.7
188.8
191.4
191.7
190.7
Vol.
added
(mL)
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
0.5
0.5
1
0.1
0.1


















Average
Reagent
Blank (ng)
0.26 5
0.26 5
0.26 5
0.26 5
0.26 5
0.26 5
0.26 5
0.26 5
0.26 5
0.26 5
0.26 5
0.26 5
0.26 5
0.26 5





0.2625
0.2625


















Corrected Hg
Concentration
(ng)
14.51
14.22
5.56
5.74
11.44
11.44
9.73
10.31
5.27
5.29
4.34
4.65
3.25
3.28
0.42
0.39
0.12
0.12
0.09
59.33
58.46


















Weight
offish
(s>
0.0872
0.0872
0.0773
0.0773
0.0754
0.0754
0.0842
0.0842
0.0389
0.0389
0.0434
0.0434
0.0361
0.0361





0.0136
0.0136


















Hg
Concentration
ppb
166.41
163.13
71.88
74.22
151.67
151.67
115.59
122.39
135.48
135.87
99.90
107.19
90.03
90.86




0.0014
4362.5
4298.9
0.1996
0.2015
0.1895
0.1984
0.1991
0.1974
0.1962
0.1969
0.1969
0.1979
0.1962
0.1981
0.1941
0.1957
0.1888
0.1914
0.1917
0.1907
Averaged
Result
ppb

164.77

73.05

151.67

118.99

135.67

103.54

90.45

0.41

0.12
0.0014

4330.70


















Averaged
Reported
Result (ppb)













119.74



0.262
0.0014

4330.70

















0.196
Detection
Limit/*3
ppb
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
3.2/9.6
SPK
CONC
(ppb)



















4600
4600
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
R%



















94.84
93.45
99.78
100.74
94.76
99.19
99.55
98.71
98.11
98.47
98.47
98.95
98.11
99.07
97.03
97.87
94.40
95.72
95.84
95.36
Standard
Deviation




















45.01

















0.0037
Relative
Standard
Deviation




















1.0

















1.89
-------
September (M5) 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RSD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                      Notes
M5-622-FSF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
09/30/99
10/25/99
10/25/99
X
FS = FI = Fh = Fish
09/30/99
10/13/99
10/13/99
X
FS = FI = Fh = Fish
09/30/99
10/13/99
10/13/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
170
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
See Database
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
See Database
g
Measurement
MB
NA
Yes (FTN Associates)
Yes (FTN Associates)
Yes
No
NA
Yes
No
NA
Yes
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG21JF1
All Good
Good
<20 RSD
All Good
All Good
3. 2 ppb and >
0.9989
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (FTN Associates)
Yes (FTN Associates)


NA
NA


NA
NA


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M5-622-FSF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation  Criteria
                Applied Qualifiers [
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA




X = Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not
met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5) 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RSD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                      Notes
M5-633-FSF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
09/29/99
10/26/99
10/26/99
X
FS = FI = Fh = Fish
09/29/99
10/14/99
10/14/99
X
FS = FI = Fh = Fish
09/29/99
10/14/99
10/14/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
41
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
See Database
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
See Database
g
Measurement
MB
NA
Yes (FTN Associates)
Yes (FTN Associates)
Yes
No
NA
No (Goal Only)
No
NA
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG22JF1
All Good
Good
<20 RSD
65.48%
All Good
3. 2 ppb and >
1
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (FTN Associates)
Yes (FTN Associates)
"M"

NA
NA


NA
NA


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M5-633-FSF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation  Criteria
                Applied Qualifiers [
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA

"M"


X = Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not
met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5) 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RSD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                      Notes
M5-643-FSF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
09/29/99
10/27/99
10/27/99
X
FS = FI = Fh = Fish
09/29/99
10/19/99
10/19/99
X
FS = FI = Fh = Fish
09/29/99
10/19/99
10/19/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
45
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
See Database
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
See Database
g
Measurement
MB
NA
Yes (FTN Associates)
Yes (FTN Associates)
Yes
No
NA
No (Goal Only)
No
NA
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG26JF1
All Good
Good
<20 RSD
All Good
All Good
3. 2 ppb and >
0.9998
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (FTN Associates)
Yes (FTN Associates)


NA
NA


NA
NA


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M5-643-FSF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation  Criteria
                Applied Qualifiers [
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA




X = Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not
met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5) 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RSD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                      Notes
M5-653-FSF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
09/28/99
10/27/99
10/27/99
X
FS = FI = Fh = Fish
09/28/99
10/21/99
10/21/99
X
FS = FI = Fh = Fish
09/28/99
10/21/99
10/21/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
8.2
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
See Database
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
See Database
g
Measurement
MB
NA
Yes (FTN Associates)
Yes (FTN Associates)
Yes
No
NA
No (Goal Only)
No
NA
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG28JF1
All Good
Good
<20 RSD
All Good
All Good
3. 2 ppb and >
0.9982
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (FTN Associates)
Yes (FTN Associates)


NA
NA


NA
NA


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M5-653-FSF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation  Criteria
                Applied Qualifiers [
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA




X = Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not
met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5) 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RSD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                      Notes
M5-663-FSF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
09/27/99
11/02/99
11/02/99
X
FS = FI = Fh = Fish
09/27/99
11/22/99
11/22/99
X
FS = FI = Fh = Fish
09/27/99
11/22/99
11/22/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
130
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
See Database
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
See Database
g
Measurement
MB
NA
Yes (FTN Associates)
Yes (FTN Associates)
No (Goal Only)
No
NA
No (Goal Only)
No
NA
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG21JF1
All Good
Good
<20 RSD
All Good
All Good
3. 2 ppb and >
0.999
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (FTN Associates)
Yes (FTN Associates)
"H"

NA
NA


NA
NA


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M5-663-FSF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation  Criteria
                Applied Qualifiers [
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA

"H"


X = Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not
met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5) 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RSD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                      Notes
M5-673-FSF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
09/27/99
11/08/99
11/08/99
X
FS = FI = Fh = Fish
09/27/99
10/25/99
10/25/99
X
FS = FI = Fh = Fish
09/27/99
10/25/99
10/25/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
170
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
See Database
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
See Database
g
Measurement
MB
NA
Yes (FTN Associates)
Yes (FTN Associates)
No (Goal Only)
No
NA
No (Goal Only)
No
NA
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG29JF1
All Good
Good
<20 RSD
All Good
All Good
3. 2 ppb and >
0.9993
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (FTN Associates)
Yes (FTN Associates)


NA
NA


NA
NA


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M5-673-FSF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation  Criteria
                Applied Qualifiers [
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA




X = Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not
met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5) 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RSD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                      Notes
M5-683-FSF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
09/26/99
11/04/99
11/04/99
X
FS = FI = Fh = Fish
09/26/99
10/27/99
10/27/99
X
FS = FI = Fh = Fish
09/26/99
10/27/99
10/27/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
220
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
See Database
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
See Database
g
Measurement
MB
NA
Yes (FTN Associates)
Yes (FTN Associates)
No (Goal Only)
No
NA
No (Goal Only)
No
NA
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG01JF1
All Good
Good
<20 RSD
All Good
All Good
3. 2 ppb and >
0.9998
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (FTN Associates)
Yes (FTN Associates)
"H"

NA
NA


NA
NA


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M5-683-FSF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation  Criteria
                Applied Qualifiers [
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA

"H"


X = Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not
met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5) 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RSD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                      Notes
M5-693-FSF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
09/25/99
10/27/99
10/27/99
X
FS = FI = Fh = Fish
09/25/99
10/27/99
10/27/99
X
FS = FI = Fh = Fish
09/25/99
10/27/99
10/27/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
150
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
See Database
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
See Database
g
Measurement
MB
NA
Yes (FTN Associates)
Yes (FTN Associates)
No (Goal Only)
No
NA
No (Goal Only)
No
NA
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG02KF1
All Good
Good
<20 RSD
All Good
All Good
3. 2 ppb and >
0.9996
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (FTN Associates)
Yes (FTN Associates)
"H"

NA
NA


NA
NA


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M5-693-FSF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation  Criteria
                Applied Qualifiers [
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA

"H"


X = Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not
met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5) 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RSD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                      Notes
M5-703-FSF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
09/24/99
11/05/99
11/05/99
X
FS = FI = Fh = Fish
09/24/99
10/27/99
10/27/99
X
FS = FI = Fh = Fish
09/24/99
10/27/99
10/27/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
250
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
See Database
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
See Database
g
Measurement
MB
NA
Yes (FTN Associates)
Yes (FTN Associates)
No (Goal Only)
No
NA
No (Goal Only)
No
NA
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG05KF1
All Good
Good
<20 RSD
All Good
All Good
3. 2 ppb and >
0.9991
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (FTN Associates)
Yes (FTN Associates)
"H"

NA
NA


NA
NA


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M5-703-FSF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation  Criteria
                Applied Qualifiers [
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA

"H"


X = Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not
met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5) 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RSD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                      Notes
M5-714-FSF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
09/23/99
10/25/99
10/25/99
X
FS = FI = Fh = Fish
09/23/99
11/01/99
11/01/99
X
FS = FI = Fh = Fish
09/23/99
11/01/99
11/01/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
240
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
See Database
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
See Database
g
Measurement
MB
NA
Yes (FTN Associates)
Yes (FTN Associates)
No (Goal Only)
No
NA
No (Goal Only)
No
NA
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG05KF1
All Good
Good
<20 RSD
All Good
All Good
3. 2 ppb and >
0.9991
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (FTN Associates)
Yes (FTN Associates)
"H"

NA
NA


NA
NA


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M5-714-FSF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation  Criteria
                Applied Qualifiers [
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA

"H"


X = Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not
met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5) 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RSD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                      Notes
M5-726-FSF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
09/23/99
11/09/99
11/09/99
X
FS = FI = Fh = Fish
09/23/99
11/02/99
11/02/99
X
FS = FI = Fh = Fish
09/23/99
11/02/99
11/02/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
110
174.1
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
See Database
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
See Database
g
Measurement
MB
NA
Yes (FTN Associates)
Yes (FTN Associates)
No (Goal Only)
No
NA
No (Goal Only)
No
NA
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG09KF1
All Good
Good
<20 RSD
All Good
All Good
3. 2 ppb and >
0.9999
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (FTN Associates)
Yes (FTN Associates)
"H"

NA
NA


NA
NA


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M5-726-FSF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation  Criteria
                Applied Qualifiers [
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA

"H"


X = Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not
met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5) 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RSD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                      Notes
M5-738-FSF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
09/22/99
11/12/99
11/12/99
X
FS = FI = Fh = Fish
09/22/99
11/04/99
11/04/99
X
FS = FI = Fh = Fish
09/22/99
11/04/99
11/04/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
57
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
See Database
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
See Database
g
Measurement
MB
NA
Yes (FTN Associates)
Yes (FTN Associates)
No (Goal Only)
No
NA
No (Goal Only)
No
NA
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG12KF1
All Good
Good
<20 RSD
All Good
All Good
3. 2 ppb and >
0.9994
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (FTN Associates)
Yes (FTN Associates)
"H"

NA
NA


NA
NA


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M5-738-FSF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation  Criteria
                Applied Qualifiers [
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA

"H"


X = Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not
met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5) 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RSD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                      Notes
M5-828-FSF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
09/29/99
11/16/99
11/16/99
X
FS = FI = Fh = Fish
09/29/99
11/08/99
11/08/99
X
FS = FI = Fh = Fish
09/29/99
11/08/99
11/08/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
240
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
See Database
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
See Database
g
Measurement
MB
NA
Yes (FTN Associates)
Yes (FTN Associates)
No (Goal Only)
No
NA
No (Goal Only)
No
NA
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG16KF1
All Good
Good
<20 RSD
All Good
All Good
3. 2 ppb and >
1
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (FTN Associates)
Yes (FTN Associates)
"H"

NA
NA


NA
NA


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
-------
                     Station ID
M5-828-FSF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation  Criteria
                Applied Qualifiers [
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA

"H"


X = Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not
met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
September (M5) 1999 Samples for Critical Parameters Analyzed by SERC
With the 10% Full QA/QC Review
                 Station ID


Laboratory Records
Data Report (Attached)
            Laboratory ID Code
          Sampling Location ID
                 Sample Type
               Collection Date
                Digestion Date
                Analysis Date
                 QC Batch ID
             Digestion Volume
                Total Volume
       Sample Volume Analyzed
                    Dilution
                     Results
               Measuring Unit
                 EPA Method
                     Analyst
         Method Detection limit
Data Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
             Holding Time Met
QC Report (Attached)
            Laboratory ID Code
                 QC Batch ID
                Method Blanks
             Instrument Blanks
             Duplicates (RSD)
 Matrix Spike Recoveries (75-125)
    Blank Spike/CCV Recoveries
              Detection Range
  Correlation Coefficient (>0.995)
QC Report (Verified)
     Lab Data Entry Checked by Analyst
        All Calculation Checked
                QC Limits Met

                      Notes
M5-944-FSF Fish
Total Hg
Length
Weight
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
X
FS = FI = Fh = Fish
09/22/99
11/15/99
11/15/99
X
FS = FI = Fh = Fish
09/22/99
11/08/99
11/08/99
X
FS = FI = Fh = Fish
09/22/99
11/08/99
11/08/99
The Batch Numbers are referenced by the Sample ID range. They are specific to this project.
7 Fish
7 Fish
Aliquot
500-1000
120
ppb
CVAF
FDL/JL
3. 2 ppb
NA
7 Fish
7 Fish
NA
See Database
mm
Measurement
MB
NA
NA
7 Fish
7 Fish
NA
See Database
g
Measurement
MB
NA
Yes (FTN Associates)
Yes (FTN Associates)
No (Goal Only)
No
NA
No (Goal Only)
No
NA
No (Goal Only)
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
HG15KF1
All Good
Good
<20 RSD
All Good
All Good
3. 2 ppb and >
0.9999
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
By: Date/Time
NA
NA
NA
NA
NA
NA
NA
Yes (FTN Associates)
Yes (FTN Associates)
"H"

NA
NA


NA
NA


No descriptive narratives were provided by FIU.
Holding time goals set for the length and weight measurements are guidelines only.
Documentation on how the fish samples were stored (Frozen, 4 C, preserved) was not provided.
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                     Station ID
M5-944-FSF
Fish
             Total Samples/Matrix
              Methods/Parameters
        Range of Samples analyzed
           Holding Time Summary
              Analytical Problems
        QA/QC Acceptance Limits
          Integrity of Data Quality
             Deviations From SOP
                     Observations
Sample Management Records
             Sampling Location ID
                           Matrix
       Preservative  (Acid, Temp..)
             Collection Data/Time
              Laboratory ID Code
         Sample Handling/Storage
                Log-in Procedures
Raw Data (Attached)
              Sample Work Sheets
                 Sample Run Logs
              Instrument Raw Data
                     Bench Sheets
          Sample Preparation Logs
Raw Data (Verified)
            Sample ID Transferred
          All Calculation Checked
                   Measuring Unit
PE Results (Attached)
                     Organization
          Performance  (Pass/Fail)

Validation  Criteria
                Applied Qualifiers [
Total Hg
Length
Weight
The Narrative Section will be written after all of the analyses are completed



























X
X
Not Noted
X
X
X
Not Noted
X
X
X
Not Noted
X
FIU/SERC Laboratory uses the same ID as the Sampling Station ID
Samples kept in the Hg laboratory area.
Internal COC
Internal COC

Internal COC
X
X
X
X
X
X
Notes are the raw data and the instrument data.
X
X
X
X
X

X

X
X
ppb
X
X
mm
X
X
g

NA
NA
NA
NA
NA
NA

"H"


X = Attached or Verified


Data Qualifiers

" J"   Concentration reported should be considered an estimate. The data are acceptable for the use as determined by specific data users but certain QC criteria were not
met
"Reject"  Batch QC data did not meet DQO required accuracy/precision criteria required to allow use as stated
"R2" Correlation Coefficient is out of QAPP limits.
"M"   Analyte exhibits potential matrix effect based on matrix spike recovery outside of 75 to 125% range.
"B"  Analyte concentration in the associated blank was >3 times the MDL.
"H"  Analysis digestion performed after holding times have expired.
"NR" Data was unavailable for review.
"DQO" Precision and/or Accuracy results are out of the Data Quality Objective/QAPP control limits.
-------
INTERLABORATORY COMPARISONS
-------
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-------
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-------
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-------
September 1999 Samples
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September 1999 Samples

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-------
     September 1999 Samples
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-------
     September 1999 Samples
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05 400
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-------
September 1999 Samples
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-------
                                    APPENDIX D: Data Files

The following are Microsoft Excel spreadsheet files. These files should be able to load into a variety of other spreadsheet
applications such Lotus 123, etc.You may need to specify within your application the file format (Excel *.xls).

       P12join7FINAL.xls (multimedia chemistry data)

       EPAM4M5.xls (diatom data)

       NEWPAFIELD~JRl.xls (macrophyte presence/absence data)

       ugacy45doml.xls (aerial photo interp. of dominant vegetation (areas))

       CYCLE4sec.xls (aerial photo secondary vegetation)

       CYCLE5sec.xls (aerial photo secondary vegetation)

       CYCLE4secP.xls (aerial photo percent secondary vegetation)

       CYCLE5secP.xls (aerial photo percent secondary vegetation)

       JRcljsagmorphclean.xls (macrophyte morphological data)

       Guts_individual_fish.xls


The following files contain several 1x1 km map files (Adobe Acrobat pdf files)

       Cycle 4, Everglades Agricultural Area (maps-cycle4-eaa.pdf )

       Cycle 4, Everglades National Park (maps-cycle4-enp.pdf )

       Cycle 4, Water Conservation Area 1 (maps-cycle4-wcal.pdf  )

       Cycle 4, Water Conservation Area 2 (maps-cycle4-wca2.pdf  )

       Cycle 4, Water Conservation Area 3 (maps-cycle4-wca3.pdf  )

       Cycle 5, Everglades Agricultural Area (maps-cycle5-eaa.pdf )

       Cycle 5, Everglades National Park (maps-cycle5-enp.pdf )

       Cycle 5, Water Conservation Area 1 (maps-cycle5-wcal.pdf  )

       Cycle 5, Water Conservation Area 2 (maps-cycle5-wca2.pdf  )

       Cycle 5, Water Conservation Area 3 (maps-cycle5-wca3.pdf  )
-------