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4.7	Purgeable Organic Matrix Standard Spiking Solution

4.7.1	Prepare a spiking solution in methanol that contains the
following compounds at a concentration of 250 ug/10.0 mL:

Pttmablo Organic?

1,1-dichloroethene

trichloroethene

chlorobenzene

toluene

benzene

4.7.2	Matrix spikes also serve as duplicates; therefore, add an
aliquot of this solution to each of two portions from one
sample chosen for spiking.

4.8	BFB Standard - Prepare a 25 ng/uL solution of BF8 in methanol.

4.9	Great care must be taken to maintain the integrity of all standard
solutions. Store all standard solutions at -10*C to -20*0 in screw-cap
amber bottles with teflon liners.

5. Calibration

5.1	Assemble a purge and trap device that meets the specification in
paragraph 3.6. Condition the trap overnight at 180*C in the purge mode
with an inert gas flow of at least 20 cm/min. Daily, prior to use,
condition the traps for 10 minutes while backflushing at 180*C with the
column at 220®C.

5.2	Connect the purge and trap device to a gas chromatograph. The gas
chromatograph must be operated using temperature and flow rate
parameters equivalent to those in paragraph 7.1.2. Calibrate the purge
and trap-GC/MS system using the internal standard technique (paragraph

5.3).

5.3	Internal standard calibration procedure. The three internal standards
are bromochloromethane, 1,4-difluorobenzene, and chlorobenzene - dj, at
50 ug/L at time of purge. Separate initial and continuing calibrations
must be performed for water samples, and medium level soil samples.

5.3.1	Prepare calibration standards at a minimum of five
concentration levels for each TCL parameter and each surrogate
compound. The concentration levels are specified in Exhibit E.
Standards may be stored up to 24 hours, if held in sealed vials
with zero headspace at -10*C to -20*C and protected from light.
If not so stored, they must be discarded after an hour.

5.3.2	Prepare a spiking solution containing each of the internal
standards using the procedures described in paragraphs 4.4 and
4.5. It is recommended that the secondary dilution standard be
prepared at a concentration of 25 ug/mL of each internal
standard compound. The addition of 10 uL of this standard to

D-20/VOA

2/88

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5.0 mL of sample or calibration standard would be equivalent of
50 ug/L.

5.3.3 Tune the GC/MS system to meet the criteria in Exhibit E by

injecting BFB. Analyze each calibration standard, according to
paragraph 7, adding 10 uL of internal standard spiking solution
directly to the syringe. Tabulate the area response of the
characteristic ions against concentration for each compound and
internal standard and calculate relative response factors (RRF)
for each compound using equation 1.

Cis

*»•1 -» " xi. x c;

5.3.4

5.3.5

Where:
Ax -

Area of the characteristic ion for the compound
to be measured.

Aig - Area of the characteristic ion for the

specific internal standard from Exhibit E

Cis - Concentration of the internal standard.

Cx - Concentration of the compound to be measured.

The average relative response factor (RRF) must be calculated
for all compounds. A system performance check must be made
before this calibration curve is used. Five compounds (the
system performance check compounds) are checked for a minimum
average relative response factor. These compounds (the SPCCi
are chloromethane, 1,1-dichloroethane, bromoform,
1,1,2,2-tetrachloroethane, and chlorobenzene. Six compounds
(the calibration check compounds, CCC) are used to evaluate the
curve. These compounds the (CCC) are 1,1-Dichloroethene
Chloroform, 1,2,-Dichloropropane, Toluene, Ethylbenzene and
Vinyl Chloride. Calculate the % Relative Standard Deviation
(%RSD) of RRF values over the working range of the curve, a
minimum %RSD for each CCC must be met before the curve is

valid.

%RSD - Standard deviation x 100

mean

S.. instructions for For. VI, InitUl Calibration Dtt. for .ore

details

Check of the calibration curve must be performed once every 12
hours. These criteria are described in detail in the
instructions for Form VII, Continuing Calibration Check, (see
Exhibit B, Section III). The minimum relative response factor
for the system performance check compounds must be checked, if
this criteria is met, the relative response factor of all

D-21/VQA

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compounds are calculated and reported. A percent difference of
the dally relative response factor (12 hour) compared to the
average relative response factor from the initial curve is
calculated. The maximum percent difference allowed for each
compound flagged as 'CCC' in Form V1X is checked. Only after
both these criteria are met can sample analysis begin.

5.3.6 Internal standard responses and retention times in all

standards must be evaluated during or immediately after data
acquisition. If the retention time for any internal standard
changes by more than 30 seconds from the latest daily (12 hour)
calibration standard, the chromatographic system must be
inspected for malfunctions, and corrections made as required.
The extracted ion current profile (EICF) of the internal
standards must be monitored and evaluated for each standard.
If the EICF area for any internal standard changes by more than
a factor of two (-50% to +100%), the mass spectrometric system
must be inspected for malfunction and corrections made as
appropriate. When corrections are made, re-analysis of samples
analyzed while the system was malfunctioning is necessary.

6. GC/MS Operating Conditions

6.1 These performance tests require the following instrumental parameters:

7. Sample Analysis
7.1 Water Samples

7.1.1	All samples and standard solutions must be allowed to warm to
ambient temperature before analysis.

7.1.2	Recommended operating conditions for the gas chromatograph

Packed column conditions: Carbopak B (60/80 mesh) with 1%
SP-1000 packed in a 6 foot by 2 mm ID glass column with helium
carrier gas at a flow rate of 30 cm/min. Column temperature
is isothermal at 45*C for 3 minutes, then programmed at 8*C per
minute to 220®C and held for 15 minutes. Injector temperature
is 200-225*C. Source temperature is set according to the
manufacturer's specifications. Transfer line temperature is
25Q-300*C. The recommended carrier gas is helium at 30
cm /sec. (See EPA Method 5.2.4.2 for capillary column
condition.)

7.1.3 After achieving the key ion abundance criteria, calibrate the
system daily as described in Exhibit E,

Electron Energy:
Mass Range:

Scan Time:

70 Volts (nominal)

35 - 260

to give at least 5 scans per peak
and not to exceed 3 seconds per scan.

D-22/V0A

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7.1.4	Adjust the purge gas (helium) flow rate to 25-40 cm3/min.
Variations from this flow rate may be necessary to achieve
better purging and collection efficiencies for some compounds,
particularly chloromethane and bromoform.

7.1.5	Remove the plunger from a 5 mL syringe and attach a closed
syringe valve. Open the sample or standard bottle which has
been allowed to come to ambient temperature, and carefully pour
the sample into the syringe barrel to just short of
overflowing. Replace the syringe plunger and compress the
sample. Open the syringe valve and vent any residual air while
adjusting the sample volume to 5.0 mL. This process of taking
an aliquot destroys the validity of the sample for future
analysis so if there is only one VQA vial, the analyst should
fill a second syringe at this time to protect against possible
loss of sample integrity. This second sample is maintained
only until such a time when the analyst has determined that the
first sample has been analyzed properly. Filling one 20 mL
syringe would allow the use of only one syringe. If a second
analysis is needed from the 20 mL syringe, it must be analyzed
within 24 hours. Care must also be taken to prevent air from
leaking into the syringe.

7.1.6	The purgeable organics screening procedure (Section III), if
used, will have shown the approximate concentrations of major
sample components. If a dilution of the sample was indicated,
this dilution shall be made just prior to GC/MS analysis of the
sample. All steps in the dilution procedure must be performed
without delays until the point at which-the diluted sample is

in a gas tight syringe.

7.1.6.1 The following procedure will allow for dilutions
near the calculated dilution factor from the
screening procedure:

All dilutions are made in volumetric
flasks (10 mL to 100 mL).

Select the volumetric flask that will
allow for the necessary dilution.
Intermediate dilutions may.be necessary
for extremely large dilutions.

Calculate the approximate volume of
reagent water which will be added to
the volumetric flask selected and add
slightly less than this quantity of
reagent water to the flask.

Inject the proper aliquot from the
syringe prepared in paragraph 7.1.5
into the volumetric flask. Aliquots of
less than 1 mL increments are
prohibited. Dilute the flask to the

7.1.6.1.1

7.1.6.1.2

7.1.6.1.3

7.1.6.1.4

D-23/VOA

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mark with reagent water. Cap the
flask, invert, and shake three times.

7.1.6.1.5	Fill a 5 mL syringe with the diluted
sample as in paragraph 7.1.5.

7.1.6.1.6	If this is an intermediate dilution,
use it and repeat above procedure to
achieve larger dilutions.

7.1.7 Add 10.0 uL of the surrogate spiking solution (4.6) and 10.0 uL
of the internal standard spiking solution (5.3.2) through the
valve bore of the syringe, then close the valve. The surrogate
and internal standards may be mixed and added as a single
spiking solution. The addition of 10 uL of the surrogate
spiking solution to 5 mL of sample is equivalent to a
concentration of 50 ug/L of each surrogate standard.

Attach the syringe-syringe valve assembly to the syringe valve
on the purging device. Open the syringe valves and inject the
sample into the purging chamber.

Close both valves and purge the sample for 11.0 + 0.1 minutes
at ambient temperature.

At the conclusion of the purge time, attach the trap to the
chromatograph, adjust the device to the desorb mode, and begin
the gas chromatographic temperature program. Concurrently,
introduce the trapped materials to the gas chromatographic
column by rapidly heating the trap to 180*C while backflushing
the trap with an inert gas between 20 and 60 cm /min for four
minutes. If this rapid heating requirement cannot be met, the
gas chromatographic column must be used as a secondary trap by
cooling it to 30*C (or subambient, if problems persist) instead
of the recommended initial temperature of 45"C.

While the trap is being desorbed into the gas chromatograph,
empty the purging chamber. Wash the chamber with a minimum of
two 5 mL flushes of reagent water to avoid carryover of
pollutant compounds.

After desorbing the sample for four minutes, recondition the
trap by returning the purge and trap device to the purge mode.
Wait 15 seconds, then close the syringe valve on the purging
device to begin gas flow through the trap. The trap
temperature should be maintained at 180"C. Trap temperatures
up to 220*C may be employed, however the higher temperature
will shorten the useful life of the trap. After approximately
seven minutes, turn off the trap heater and open the syringe
valve to stop the gas flow through the trap. When cool, the
trap is ready for the next sample.

If the Initial analysis of a sample or a dilution of a sample
has concentration of TCL compounds that exceeds the initial

7.1.8

7.1.9

7.1.10

7.1.11

7.1.12

7.1.13

D-24/VOA

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calibration range, the sample must be reanalyzed at a higher
dilution. Note: For total xylenes, where three isomers are
quantified as two peaks, the calibration range of each peak
should be considered separately, e.g., a diluted analysis is
not required for total xylenes unless the concentration of
eithfer peak separately exceeds 200 ug/L. Secondary ion
quantitation is only allowed when there are sample
interferences with the primary ion. If secondary ion
quantitation is used, document the reasons in the Case
Narrative. When a sample is analyzed that has saturated ions
from a compound, this analysis must be followed by a blank
reagent water analysis. If the blank analysis is not free of
interferences, the system must be decontaminated. Sample
analysis may not resume until a blank can be analyzed that is
free of interferences.

7 1 14 For water samples, add 10 uL of the matrix spike solution

(paragraph 4.7) to the 5 mL of sample purged. Disregarding any
dilutions, this is equivalent to a concentration of 50 ug/L of
each matrix spike standard.

7 1 15 All dilutions must keep the response of the major constituents
(previously saturated peaks) in the upper half of the linear
range of the curve.

7.2 Soil/Sediment Samples

_ -tjnroaches may be taken to determine whether the low level or

medium level method may be followed.

o Assume the sample is low level and analyze a 5 g sample.

Use the X factor calculated from the optional hexadecane
° screen (Section III, paragraph 6.2.1.3).

If „..k« M. saturated from th. an.ly.ia of . 5 g aaapl., « smaller

II peass	analyzed to prevent saturation. However, the

*"f}* I	1« 1 «• I* ¦-»«« than 1 g aampl. ,lz.

smallest samp	saturation, the medium level method must be used.

is needed to prevent

7.2.1 Low Level Soil Method

Th* low level soil method is based on purging a heated

„*-/ aoii sample mixed with reagent water containing the
*®^!ate and internal standards. Analyze all reagent blanks
and standards under the same conditions as the samples.

Use 5 grans of sample or use the X Factor to determine the
sample size for purging.

If the X Factor is 0 (no peaks noted on the
° hexadecane screen), analyze a 5 g sample.

Tf the V Factor is between 0 and 1.0, analyze a
° minimum of a 1 g sample.

D-25/VOA

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7.2.1.1	The GC/MS system should be set up as in 7.1.2-7.1.4.
This should be done prior to the preparation of the
sample to avoid loss of volatiles from standards and
sample. A heated purge calibration curve must be
prepared and used for the quantitation of all
samples analyzed with the low-level method. Follow
the initial and daily calibration instructions (5.3)
except for the addition of a 40*C purge temperature.

7.2.1.2	To prepare the reagent water containing the
surrogates and internal standards, remove the
plunger from a 5 mL "Luerlock" type syringe equipped
with a syringe valve and fill until overflowing with
reagent water. Replace the plunger and compress the
water to vent trapped air. Adjust the volume to 5.0
mL. Add 10 uL each of the surrogate spiking
solution (4.6) and the internal standard solution to
the syringe through the valve. (Surrogate spiking
solution and internal standard solution may be mixed
together). The addition of 10 uL of the surrogate
spiking solution to 5 g of soil/sediment is
equivalent to 50 ug/kg of each surrogate standard.

7.2.1.3	The sample (for volatile organics) consists of the
entire contents of the sample container. Do not
discard any supernatant liquids. Mix the contents
of the sample container with a narrow metal spatula.
Veigh the amount determined in 7.2.1 into a tared
purge device. Use a top loading balance. Note and
record the actual weight to the nearest 0.1 g.

7.2.1.4	Immediately after weighing the sample, weigh 5-10 g
of the sediment into a tared crucible. Determine
the percent moisture by drying overnight at 105*C.

Allow to cool in a desiccator before weighing.
Concentrations of individual analytes will be
reported relative to the dry weight of sediment.

Percent moisture

g 
-------
7.2.1.7 Proceed with the analysis as outlined in 7.1.10

7.1.13. Use 5 mL of the same reagent water as the
reagent blank.

7 2.1.8 For low level soils/sediment add 10 uL of the matrix
spike solution (4.7) to the 5 mL of water (7.2.1.2).
The concentration for a 5 g sample would be
equivalent to 50 ugAg of each matrix spike
standard.

7.2.2 Medium Level Soil Method

The medium level soil method is based on extracting the soil/
sediment sample with methanol. An aliquot of the methanol
extract is added to reagent water containing the surrogate and
internal standards. This is purged at ambient temperature. All
oles with an X Factor >1.0 should be analyzed by the medium
samp nethod jf saturated peaks occurred or would occur when
ae^8g san,pie was analyzed, the medium level method must be

used.

7 2 2 1 The GC/MS system should be set up as in 7.1.2 -
'	7 14. This should be done prior to the addition of

the methanol extract to reagent water. Initial and
continuing calibrations (5.3) are performed by
adding standards in methanol to reagent water and
purging at ambient temperature.

7 9 9 2 The sample (for volatile organics) consists of the
entire contents of the sample container. Do not
discard any supernatant liquids. Mix the contents
of the sample container with a narrow metal spatula.
Weigh 4 g (wet weight) into a tared 15 mL vial. Use

top loading balance. Note and record the actual
weight to the nearest 0.1 g. Determine the percent
moisture as in 7.2.1.4.

7.2.2.3

7.2.2.4

Quickly add 9.0 mL of methanol, then 1 o mL of a
surrogate spiking solution to the vial' ca„ 5
shake for 2 minutes. NOTE: Steps 7 2 2 1 d
7.2.2 2 »u.t b. p.rfor..d r.pidly to .void L, „f
volatile organics. These steps must be berfaliL!!
a laboratory free of solvent fumes. P	ln

Using a disposable pipette, transfer approximate,
mL of extract into a GC vial for storage	y 1

remainder may be disposed of. Transfer 6
approximately 1 mL of the reagent methanol to a rr
vial for use as the method blank for each cas
set of 20 samples, whichever is more frequent6 °Z
These extracts may be stored in the dark at 4'c
(±2'C) prior to analysis.

D-27/VOA

2/88
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The addition of a 100 uL aliquot of each of these
extracts in paragraph 7.2.2.6 will give a
concentration equivalent to 6,200 ug/kg of each
surrogate standard.

7.2.2.5 The following table can be used to determine the
volume of methanol extract to add to the 5 mL of
reagent water for analysis. If the Hexadecane
screen procedure was followed, use the X factor
(Option B) or the estimated concentration (Option A)
to determine the appropriate volume. Otherwise,
estimate the concentration range of the sample from
the low level analysis to determine the appropriate
volume. If the sample was submitted as a medium
level sample, start with 100 uL.

All dilutions must keep the response of the major
constituents (previously saturated peaks) in the
upper half of linear range of the curve.

Estimated	.	Take this Volume of

X Fflgtftr	Concentration Range1	Methanol EXtMCt

0 * n	u«Ag	«L

- 5.0	500 - 10,000	100

°*5 " 100	1000 - 20,000	50

" „50 0	5000 - 100,000	10

12*5 * 250	25,000 - 500,000	100 of 1/50 dilution3

Calculate appropriate dilution factor for concentrations exceeding the table.

1 Actual concentration ranges could be 10 to 20 times higher than this if
the compounds are halogenated and the estimates are from GC/F1D.

The volume of methanol added to the 5 mL of water being purged should be
kept constant. Therefore, add to the 5 mL syringe whatever volume of
methanol is necessary to maintain a volume of 100 uL added to the syringe.

3

Dilute an aliquot of the methanol extract and then take 100 uL for

analysis.

Remove the plunger from a 5 mL "Luerlock" type
syringe equipped with a syringe valve and fill until
overflowing with reagent water. Replace the plunger
and compress the water to vent trapped air. Adjust
the volume to 4.9 mL. Pull the plunger back to 5 mL
to allow volume for the addition of sample and
standards. Add 10 uL of the internal standard
solution. Also add the volume of methanol extract
determined in 7.2.2.5 and a volume of methanol
solvent to total 100 uL (excluding methanol in
standards).

D-28/V0A

2/88
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Attach the syringe-syringe valve assembly to the
syringe valve on the purging device. Open the
syringe valve and inject the water/methanol sample
into the purging chamber.

Proceed with the analysis as outlined in 7.1.9 -
7.1.13. Analyze all reagent blanks on the same
instrument as the samples. The standards should
also contain 100 uL of methanol to simulate the
sample conditions.

For a matrix spike in the medium level sediment/soil
samples, add 8.0 mL of methanol, 1.0 mL of surrogate
spike solution (4.6), and 1.0 mL of matrix spike
solution (4.7) in paragraph 7.2.2.2. This results
in a 6,200 ug/kg concentration of each matrix spike
standard when added to a 4 g sample. Add a 100 uL
aliquot of this extract to 5 mL of water for purging
(as per paragraph 7.2.2.6).

8. Qualitative Analysis

8.1 The compounds listed in the Target Compound List (TCL), Exhibit C,

shall be identified by an analyst competent in the interpretation of
mass spectra (see Bidder Responsibility description) by comparison of
the sample mass spectrum to the mass spectrum of a standard of the
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.

8.1.1	For establishing correspondence of the GC relative retention
time (RRT), the sample component RRT must compare within +0.06
RRT units of the RRT of the standard component. For reference,
the standard must be run on the same shift as the sample. If
coelution of interfering components prohibits accurate
assignment of the sample component RRT from the total ion
chromatogram, the RRT should be assigned by using extracted ion
current profiles for ions unique to the component of interest.

8.1.2	For comparison of standard and sample component mass spectra,
mass spectra obtained on the Contractor's GC/MS are required.
Once obtained, these standard spectra may be used for
identification purposes, only if the Contractor's GC/MS meets
the daily tuning requirements for BFB. These standard spectra
may be obtained from the run used to obtain reference RRTs.

8.1.3	The requirements for qualitative verification by comparison of
mass spectra are as follows:

8.1.3.1 All ions present in the standard mass spectra at a
relative intensity greater than 10% (most abundant

7.2.2.7

7.2.2.8

7.2.2.9

D-29/VOA

2/88
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ion in the spectrum equals 100%) ftiust be present in
the sample spectrum.

8.1.3.2	The relative intensities of ions specified in
8.1.3.1 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 abundance must be
between 30 and 70 percent).

8.1.3.3	Ions greater than 10% in the aflfflBlS spectrum but r.ot
present in the standard spectrum must be considered
and accounted for by the analyst making the
comparison. In Task III, the verification process
should favor false negatives. All compounds meeting
the identification criteria must be reported with
their spectra. For all compounds below the CRQL
report the actual value followed by a "J", e.g.,

"3J."

8.1.4 If a compound cannot be verified by all of the criteria in
8.1.3.3, but in the technical judgement of the mass spectral
interpretation specialist, the identification is correct, then
the Contractor shall report that identification and proceed
with quantification in 9.

8.2 A library search shall be executed for non-TCL sample components for
the purpose of tentative identification. For this purpose, the 1985
release of the National Bureau of Standards Mass Spectral Library (or
more recent release), containing 42,261 spectra, shall be used.

Computer generated library search routines must not use normalization
routines that would misrepresent the library or unknown spectra when
compared to each other.

8.2.1	Up to 10 nonsurrogate organic compounds of greatest apparent
concentration not listed in Exhibit C for the purgeable organic
fraction shall be tentatively identified via a forward search
of the NBS mass spectral library. (Substances with responses
less than 10% of the internal standard are not required to be
searched in this fashion). 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
wist not use normalization routines that would misrepresent the
library or unknown spectra when compared to each other.

8.2.2	Guidelines for making tentative identification:

8.2.2.1	Relative intensities of major ions in the reference
spectrum (ions greater than 10% of the most abundant
ion) should be present in the sample spectrum.

8.2.2.2	The relative intensities of the major ions should
agree within ± 20%. (Example: For an ion with an

D-30/VOA

2/88
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abundance of 50 percent of the standard spectra, the
corresponding sample ion abundance must be between
30 and 70 percent.)

Molecular ions present in reference spectrum should
be present in sanple spectrum.

Ions present in the sample spectrum but not in the
reference spectrum should be reviewed for possible
background contamination or presence of co-eluting
compounds.

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 or co-eluting compounds.
Data system library reduction programs can sometimes
create these discrepancies.

8.2.3 If in the technical judgement of the mass spectral

interpretation specialist, no valid tentative identification
can be made, the compound should be reported as unknown. The
mass spectral specialist should give additional classification
of the unknown compound, if possible (i.e. unknown aromatic,
unknown hydrocarbon, unknown acid type, unknown chlorinated
compound). If probable molecular weights can be distinguished,
include then.

9. Quantitative Analvsla

9.1	TCL components identified shall be quantified by the internal standard
method. The internal standard used shall be that which is listed in
Exhibit E, Table 2.1. The E1CP area of the characteristic ions of
analytes listed in Tables 2 and 3 in this Section are used.

9.2	Internal standard responses and retention times in all standards must
be evaluated during or immediately after data acquisition. If the
retention time for any internal standard changes by more than 30
seconds from the latest daily <12 hour) calibration standard, the
chromatographic system must be inspected for malfunctions, and
corrections made as required. The extracted ion current profile (EICF)
of the internal standards must be monitored and evaluated for each
sample, blank, matrix spike and matrix spike duplicate. If the EI CP
area for any internal standard changes by more than a factor of two
(-50% to +100*), the mass spectrometrie system must be inspected for
malfunction and corrections made as appropriate. When corrections are
made, reanalysis of samples analysed while the system was
malfunctioning is necessary.

9.2.1 If after re-analysis, the EI CP areas for all internal standards
are inside the contract limits (-50% to +100*), then the
problem with the first analysis is considered to have been
within the control of the laboratory. Therefore, only aubmit
data from the analysis, with EICPs within the contract limits.

8.2.2.3

8.2.2.4

8.2.2.5

D-31/V0A

2/88
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This is considered the initial analysis and must be reports
such on all data deliverables.

9.2.2 If the re-analysis of the •aBPj* d°" contJact'limitrf^both
i.e., the EICP areas are outside the contract xim

analyses, then submit the EICP data and samp * . .

analyses. Distinguish between the initial	1. «uffixes

re-analysis on .11 d.f d.Uv.r.bl...

•peclfled In Exhibit B. DocuMnC In th. Ca«e N.rr.tlv.
inspection and corrective actions taken.

9.3 The relative response factor (RRF) from the daily stancUrd analysis is
used to calculate the concentration in the sample. se
response factor as determined in paragraph 5.3.3 and ^e *quations
below. When TCL compounds are below contract require 1	ort

lintt. (CRQL) t>ut th. .p«tr. —t th.	report

the concentration with a "J." For example, If I
concentration of 3 ug/L is calculated, report as 3J.

Water

(Vd,)

Concentration	ug/L -

Where:
*x "

Ais "

*s "

Vo "

Area of the characteristic ion for the compound to be

measured	.

Area of th. characteristic Ion for th. .pacific Internal
standard from Exhibit E.

Amount of lnt.m.1 st.nd.rd .ddad In nanog»« 
VoIum of w.t.r purged In tiJlUlttli WW <«*• Into
account any dilutions)

Sediment/Soil fined? nn. l«vel)

Concentration	ugAg "	(ftilF)

Sediment/Soil flow level)

(V'V

Concentration	ug/kg " (Alfl) (kAr') (Wg) (t)

(Dry weight basis)

Where:

A_, I_, A*. - same as for water, above

Vt	- Volvo. of total .xtr.ct 
-------
W,

D

s

~ Volume of extract added (uL) for purging

-	100 - »

100

-	Weight of sample extracted (g) or purged

9.4 An estimated concentration for non-TCL components tentatively

identified shall be quantified by the internal standard method. For
quantification, the nearest internal standard free of interferences
shall be used.

9.4.1 The formula for calculating concentrations is the same as in

paragraph 9.3. 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 relative response
factor (RRF) of one (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.

9.5	Xylenes (o-,m-, & p- isomers) are to be reported as Xylenes (total).
Since o- and p-Xylene overlap, the Xylenes must be quantitated as
m-Xylene. The concentration of all Xylene isomers must be added
together to give the total.

9.6	1,2-Dichloroethene (trans and cis stereoisomers) are to be reported as
1,2-Dichloroethene (total). The concentrations of both isomers must be
added together to give the total.

9.7	Calculate surrogate standard recovery on all samples, blanks and
spikes. Determine if recovery is within limits and report on
appropriate form.

9.7.1 Calculation for surrogate recovery.

9.7.2 If recovery is not within limits, the following is required:

o Reanalyze the sample if none of the above reveal a
problem.

9.7.3 If the reanalysis of the sample solves the problem, then the
problem was within the laboratory's control. Therefore, suili

Where:

Qd - quantity determined by analysis

Qa - quantity added to sample

o Check to be sure there are no errors in calculations,

surrogate solutions and internal standards. Also, check
instrument performance.

D-33/VQA

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submit data from the analysis with surrogate spike recoveries
within the contract limits. This shall be considered the
initial analysis and shall be reported as such on all data
deliverables.

9-7.4 If the reanalysis of the sample does not solve the problem,

i.e., surrogate recoveries are outside the contract limits for
both analyses, then submit the surrogate spike recovery data
and the sample data from both analyses. Distinguish between
the initial analysis and the reanalysis on all data
deliverables, using the sample suffixes specified in Exhibit B.

9.7.5 If the sample with surrogate recoveries outside the limits is
the sample used for the matrix spike and matrix spike
duplicate, and the surrogate recoveries of the matrix spike and
matrix spike duplicate show the same pattern (i.e., outside the
limits), then the sample, matrix spike, and matrix spike
duplicate do not require reanalysis. Document in the narrative
the similarity in surrogate recoveries.

Table 2

Characteristic Ions for Surrogate and

Internal Standards	for Volatile Organic Compounds

Compound		Primary Ion	SlfUfTtflirr Tonfs)

SVRfiOGATE STAPPARPS	174 176

4-Bromofluorobenzene	95 ^Q2

1,2-Dichloroethane d-4	65 _ft ,QQ

Toluene d-8	98 /U'

1PTSPPM. STANPARP?	49 130 51

Bromochloromethane	128 ' ^ jg

1,4-Difluorobenzene	114 '

Chlorobenzene d-5	117 '

D-34/V0A

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Table 3

Characteristic Ions for Volatile TCL Compounds

Parameter

Primary TftTl*

Secondary

	Ipn(g)

Chloromethane

50

52



Bromomethane

94

96



Vinyl chloride

62

64



Chloroethane

64

66



Methylene chloride

84

49, 51, 86



Acetone

43

58



Carbon disulfide

76

78



1,1-Dichloroethene

96

61, 98



1,1-Dichloroethane

63

65, 83, 85, 98,

100

1,2-Dichloroethene

96

61, 98



Chloroform

83

85



1,2-Dichloroethane

62

64, 100, 98



2-Butanone

72

57



1,1,1-Trichloroethane

97

99, 117, 119



Carbon tetrachloride

117

119, 121



Vinyl acetate

43

86



Bromodichloromethane

83

85



1,1,2,2-Tetrachloroethane

83

85, 131, 133,

166

1,2-Dichloropropane

63

65, 114



trans-1,3-Dichloropropene

75

77



Trichloroethene

130

95, 97, 132



Dibromochloromethane .

129

208, 206



1,1,2-Trichloroethane

97

83, 85, 99, 132

, 134

Benzene

78





cis-1,3-Dichloropropene

75

77



Bromoform

173

171, 175, 250, 252,

254, 256

2-Hexanone

43

58, 57, 100



4-Methy1-2-pentanone

43

58, 100



Te trachloroe thene

164

129, 131, 166



Toluene

92

91



Chlorobenzene

112

114



Ethyl benzene

106

91



Styrene

104

78, 103



Total xylenes

106

91



* The primary ion should be used unless interferences are present, in which
case, a secondary ion may be used.

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IV

ap"«"t o^_£«ir »/4 ml
foam	0A

- Q.^

Ny Mm */4 m.

oo

(.

Stool

'"'l 13X molecular
' ¦ sieve purge

Purge fw
How control

10mm gloss frit
medium porosity

n§m% 1.

Pocking procedure

Gloss _
froffi omm

Grade 15
Silica gol ®tffl

Construction

Jones 18cm

Gloss 8mm

14ft T^foot resistence
wire wropped solid

YHotmocoupb/sotdtoBor

Tubing 25 cm.
a 105 in. 10.
0.125 in. 0.0.
stoinloss stool

Trap inlot

Trop pockings end construction to include dasorb cofioiiktf

D-36/VOA

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IV.

Corriar gas flow control
Prossuro roguhtor

Purga gas
flow controi

t3X mohcutor

ttOVO iUtOt

Uguid uytctiofi pom

Column ovon

p- Confirmatory column
To datactor
"^-Analytical column

optional 4-port column
salaction vaha
Trap Mot
Masistanca wira

^Haatar control

Nota:

Alt knot batwoon

Wop and GC
should bo haatod
to 80°C

ngwiS. Schematic of purga and trop dovico — purgo

Carrier gos flow contra/^
Prossuro regulator

Purge gas

flow control

13X moiocufor
' filter

Liguid Ujoction porta CQhtm„ ^

T1"1"! 1.— Confirmatory column
I / To datactor

"^-Analytical column

optional 4-port column

Hootor control

7>S

Nota:

All linos t
trap and GC
should bo haotod
to 96*C

R|un 4. Schematic at purgo and trap device — dasorb moda

D-37/VOA

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IV.

PURGE INLET FITTING

SAMPLE OUTLET FITTING



3" * 6mm Q.O. GLASS TUBING

SEPTUM

CAP

Wfur« S. Low Soils laplnger

D-38/VOA

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exhibit d

ANALYTICAL METHODS
FOR SEMIVOLATILES

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Table of Contents

£fiiS.

SECTION I - INTRODUCTION 	 D-3/SV

SECTION II - SAMPLE PREPARATION AND STORAGE		 D-5/SV

PART A - SAMPLE STORAGE AND HOLDING TIMES 	D-6/SV

PART B - SAMPLE PREPARATION FOR EXTRACTABLE

SEMIVOLATILES (BNA) IN WATER 	 D-7/SV

PART C - PROTOCOLS FOR SOIL/SEDIMENT 	 D-12/SV

1.	Medium Level Preparation for
Screening and Analysis of

Semivolatiles (BNA) 	 D-12/SV

2.	Low Level Preparation for
Screening and Analysis of

Semivolatiles (BNA) 	 D-16/SV

SECTION III - SCREENING OF SEMIVOLATILE ORGANIC EXTRACTS 	 D-27/SV

SECTION IV - GC/MS ANALYSIS OF SEMIVOLATILES 	D-31/SV

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SECTION I

INTRODUCTION

The analytical methods that follow are designed to analyze water, soil and
sediment from hazardous waste sites for the organic compounds on the Target
Compound List (TCL) (See Exhibit C). The methods are based on EPA Method 625
(Base/Neutrals and Acids).

The methods are divided Into the following sections: sample preparation,
screening and analysis. Sample preparation covers sample extraction and
cleanup techniques. As described in the screening section, a portion of the
extracts may be screened on a gas chromatograph with appropriate detectors to
determine the concentration level of organics. The analysis section contains
the GC/MS analytical methods for organics.

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1.

Method for the Determination of F.xt-r^etable Samivolatllpg (Base /Neutral
and Acld^ Organic Compounds.

1.1	Scope and Application

This nethod covers the detemination of a number of organic compounds
that are partitioned into an organic solvent and are amenable to gas
chromatography. These TCL compounds and the contract required
quantitation limits are listed in Exhibit C.

Problems have been associated with the following compounds covered by
this method. Dichlorobenzidine and 4-chloroaniline can be subject to
oxidative losses during solvent concentration. This is especially true
in the soil/sediment method when concentrating the methylene chloride/
acetone extraction solvent. Hexachlorocyclopentadiene is subject to
thermal decomposition in the inlet of the gas chromatograph, chemical
reaction in acetone solution and photochemical decomposition.
N-nitrosodiphenylamine decomposes in the gas chromatographic inlet
forming diphenylamina and, consequently, cannot be separated from
diphenylamine native to the sample.

1.2	The method Involves solvent extraction of the matrix sample
characterization to determine the appropriate analytical protocol to be
used, and GC/MS analysis to determine semivolatile (BNA) organic
compounds present in the sample.

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SECTION II
SAMPLE PREPARATION AND STORAGE

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EARX-A - SAMPLE STORAGE AND HOLDING TTMF.S

1.	Procedures for Sample Storage

1.1	The samples must be protected from light and refrigerated at 4*C (±2*C)
from the time of receipt until extraction and analysis.

1.2	After analysis, extracts and unused sample volume must be protected
from light and refrigerated at 4*C (±2*C) for the periods specified in
the contract schedule.

2.	Contract Required Holding Tlm««

2.1 If separatory funnel or sonication procedures are employed for

extractions for semivolatile analyses, extraction of water samples
shall be completed within 5 days of VTSR (Validated Time of Sample
Receipt), and extraction of soil/sediment samples shall be completed
within 10 days of VTSR. If continuous liquld*liquid extraction
procedures are employed, extraction of water samples shall be started
within 5 days of VTSR.

Extracts of either water or soil/sediment samples must be analyzed
within 40 days following extraction.

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PART & - SAMPLE "PREPARATION FOR EXTRACTABLE SEMIVOIATTT.F.S (BNA1 TW UATBP

1.	finnimarv

A measured volume of simple, approximately one liter, is serially
extracted with methylene chloride at a pH greater than 11 and again at
pH less than 2, using a separatory funnel or a continuous extractor.
The methylene chloride extracts are dried and concentrated separately
to a volume of 1 mL.

2.	Interferences

2.1 Method interferences may be caused by contaminants in solvents,

reagents, glassware and other sample processing hardware, that lead to
discrete artifacts and/or elevated baselines in the total ion current
profiles (TICPs). All of these materials must be routinely
demonstrated to be free from interferences under the conditions of the
analysis by running laboratory reagent blanks. Matrix Interferences
may be caused by contaminants that are coextracted from the sample.
The extent of matrix interferences will vary considerably from source
to source.

3.	Apparatus and Materials

3.1 Glassware (Brand names and catalog numbers are included for
illustration purposes only).

3.1.1	Separatory funnel - 2,000 mL, with teflon stopcock.

3.1.2	Drying column - 19 mm ID chromatographic column with coarse
frit. (Substitution of a small pad of Pyrex glass wool for the
frit will prevent cross contamination of sample extracts.)

3.1.3	Concentrator tube - Kuderna-Danish, 10 mL, graduated (Kontes
K-570050-1025 or equivalent). Calibration must be checked at
the volumes employed in the test. Ground glass stopper is used
to prevent evaporation of extracts.

3.1.4	Evaporative flask - Kuderna-Danish, 500 mL (Kontes K-570001-
0500 or equivalent). Attach to concentrator tube with springs.

3.1.5	Snyder column - Kuderna-Danish, Three-ball macro (Kontes
K-503000-0121 or equivalent).

3.1.6	Snyder column - Kuderna-Danish, Two<¦ ball micro (Kontes K569001-
0219 or equivalent).

3.1.7	Vials - Amber glass, 2 mL capacity with Teflon-lined screw cap.

3.1.8	Continuous liquid-liquid extractors - Equipped with Teflon or
glass connnecting joints and stopcocks requiring no lubrication
(Hershberg-tfolf Extractor-Ace Glass Company, Vine land, NJ P/N
6841-10 or equivalent.)

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3.2	Silicon carbide boiling chips - approximately 10/40 mesh. Heat to
400*C for 30 ainutes or Soxhlet extract with methylene chloride.

3.3	Vater bath - Heated, with concentric ring cover, capable of temperature
control (± 2*C). The bath should be used in a hood.

3.4	Balance - Analytical, capable of accurately weighing ± 0.0001 g.

3.5	Nitrogen evaporation device equipped with a water bath that can be
maintained at 35-40*C. The N-Evap by Organomation Associates, Inc.,
South Berlin, HA (or equivalent) is suitable.

4. Reagents

4.1	Reagent water - Reagent water is defined as a water in which an
interferent is not observed at or above the CRQL of each parameter of
interest.

4.2	Sodium hydroxide solution (10N) - Dissolve 40 g NaOH in reagent water
and dilute to 100 mL.

4.3	Sodium thiosulfate - (ACS) Granular.

4.4	Sulfuric acid solution (1+1) - Slowly add 50 mL of	(sp gr.1.84)
to 50 mL of reagent water.

4.5	Acetone, methanol, methylene chloride - Pesticide quality or
equivalent.

4.6	Sodium sulfate - (AGS) Powdered, anhydrous. Purify by heating at 400"C
for four hours in a shallow tray, cool in a desiccator and store in a
glass bottle. Baker anhydrous powder, catalog #73898 or equivalent.

4.7	Surrogate standard spiking solution.

4.7.1	Surrogate standards are added to all samples and calibration
solutions; the compounds specified for this purpose are
phenol-dg; 2,4,6 tribromophenol; 2-fluorophenol;
nitrobenzene-dj; terphenyl- *14 and 2-fluorobiphenyl. Two
additional surrogates, one base/neutral and one acid, may be
added.

4.7.2	Prepare a surrogate standard spiking solution that contains the
base/neutral compounds at a concentration of 100 ug/mL, and the
acid compounds at 200 ug/mL. Store the spiking solutions at
4*C (+2*C) in Teflon-sealed containers. The solutions should
checked frequently for stability. These solutions must be
replaced after twelve months, or sooner if comparison with
quality control check samples Indicates a problem.

4.8	BNA Matrix standard spiking solution. The matrix spike solution
consists of:

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Bana/Nmitralg

1.2,4-trichlorobenzene
acenaphthene
2,4-dinitrotoluene
pyrene

N-ni troso - di - n- propylamine
1,4 - dlchlorobenzene

Ac Ida

pentachlorophenol
phenol

2-chlorophenol

4-chloro-3-methylphenol

4-nierophenol

Prepare a spiking solution Chat contains each of the base/neutral
conpounds above at 100 ug/1,0 mL in methanol and the acid compounds at
200 ug/1.0 ml in nethanol. Analyze duplicate aliquots of a sample
spiked with BNA matrix spiking solution.

5. Sample Extraction - Separator*

5.1	Samples may be extracted using separatory funnel techniques. If
emulsions prevent acceptable solvent recovery with separatory funnel
extraction, continuous extraction (paragraph 6.) may be used. The
separatory funnel extraction scheme described below assumes a sample
volume of 1-liter.

5.2	Using a 1-liter graduated cylinder, measure out a 1-liter sample
aliquot and place it into a 2-liter separatory funnel. Pipet 1.0 mL
surrogate standard spiking solution into the separatory funnel and mix
well. Check the pH of the sample with wide range pH paper and adjust to
pH >11 with 10N sodium hydroxide. Add 1.0 mL of BNA matrix spiking
solution to each of two 1-liter portions from the sample selectedi for
spiking.

5.3	Add 60 mL methylene chloride to the separatory funnel and extract the
sample by shaking the funnel for two minutes, with periodic venting to
release excess pressure. Allow the organic layer to separate from the
water phase for a minimum of 10 minutes. If the emulsion interface
between layers is more than one-third the volume of the solvent layer,
the analyst must employ mechanical techniques to complete the phase
separation. The optimum technique depends upon the sample, and may
include: stirring, filtration of the emulsion through glass wool,
centrifugation or other physical methods.

Collect the methylene chloride extract in a 250-mL Erlenmeyer flask. If
the emulsion cannot be broken (recovery of less than 80% of the
methylene chloride, corrected for the water solubility of methylene
chloride), transfer the sample, solvent and emulsion into the
extraction chamber of a continuous extractor. Proceed as described in
paragraph 6.3.

5.4	Add a second 60-mL volume of methylene chloride to the sample bottle
and repeat the extraction procedure a second tipe, combining the
extracts in the Erlenmeyer flask. Perform a third extraction in the
same manner. Label the combined extract as the base/neutral fraction.

5.5	Adjust the pH of the aqueous phase to less than 2 using sulfuric acid
(1 + 1). Serially extract three times with 60-mL aliquots of methylene

D-9/SV

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chloride, as per paragraph 5.3. Collect and combine the extracts in a
250-mL Erlenmeyer flask and label the combined extract as the acid
fraction.

5.6	Assemble a Kuderna-Danish (K-D) concentrator by attaching a 10-mL
concentrator tube to a 500-mL evaporative flask. Other concentration
devices or techniques nay be used in place of the K-D, if equivalency
is demonstrated for all extractable organics listed in Exhibit C.

5.7	Transfer the individual base/neutral and acid fractions by pouring
extracts through separate drying columns containing about 10 cm of
anhydrous granular sodium sulfate, and collect the extracts in the
separate K-D concentrators. Rinse the Erlenmeyer flasks and columns
with 20 to 30 mL of methylene chloride to complete the quantitative
transfer.

5.8	Add one or two clean boiling chips and attach a three-ball Snyder
column to the evaporative flask. Pre-wet the Snyder column by adding
about 1 mL methylene chloride to the top of the column. Place the K-D
apparatus on a hot water bath (80* to 90*C) so that the concentrator
tube is partially immersed in the hot water, and the entire lower
rounded surface of the flask is bathed with hot vapor. Adjust the
vertical position of the apparatus and the water temperature as
required to complete the concentration in 10 to 15 minutes. At the
proper rate of distillation, the balls of the column will actively
chatter but the chambers will not flood with condensed solvent. When
the apparent volume of liquid reaches 1 mL, remove the K-D apparatus
from the water bath and allow it to drain and cool for at least 10
minutes. Remove the Snyder column and rinse the flask and its lower
joint into the concentrator tube with 1-2 mL of methylene chloride. A
5-mL syringe is recommended for this operation.

5.9	Micro Snyder column technique - Add another one or two clean boiling
chips to the concentrator tube and attach a two-ball micro Snyder
column. Pre-wet the Snyder column by adding about 0.5 mL of methylene
chloride to the top of the column. Place the K-D apparatus on a a hot
water bath (80* to 90*C) so that the concentrator tube is partially
immersed in the hot water. Adjust the vertical position of the
apparatus and the water temperature as required to complete the
concentration in 5 to 10 minutes. At the proper rate of distillation
the balls of the column will actively chatter but the chambers will not
flood with condensed solvent. When the apparent volume of liquid
reaches about 0.5 mL, remove the K-D apparatus from the water bath and
allow it to drain for at least 10 minutes while cooling. Remove the
Snyder column and rinse its flask and its lower joint into the
concentrator tube with 0.2 mL of methylene chloride. Adjust the final
volume to 1.0 mL with methylene chloride. If GC/MS analysis will not
be performed immediately, stopper the concentrator tube and store
refrigerated. If the extracts will be stored longer than two days,
they should be transferred to individual Teflon-sealed screw cap
bottles and labeled base/neutral or acid fraction, as appropriate.

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5.10 Nitrogen blowdown technique (taken from ASTM Method D3086)

The following method may be used for final concentration, instead of
the procedure outlined in paragraph 5.9. Place the concentrator tube
in a warm water bath (35*C) and evaporate the solvent volume to just
below 1 mL using a gentle stream of clean, dry nitrogen filtered
through * column of activated carbon). Caution: New plastic tubing
must not be used between the carbon trap and the sample, as it may
introduce interferences. The internal wall of the tube must be rinsed
down several times with methylene chloride during the operation and the
final volume brought to 1 mL with methylene chloride. During
evaporation, the tube solvent level must be kept below the water level
of the bath. The extract must never be allowed to become dry.

6.	Sample Extraction - Continuous Ltauid-Llould Extractor

6.1	Check the pH of the sample with wide-range pH paper and adjust to pH 11
with 10 N sodium hydroxide. Transfer a 1-liter sample aliquot to the
continuous extractor; using a pipet, add 1 mL of surrogate standard
spiking solution and mix well.

6.2	Add 500 mL of methylene chloride to the distilling flask. Add
sufficient reagent water to ensure proper operation and extract for 18
hours. Allow to cool, then detach the boiling flask and dry.

Concentrate the extract as in paragraphs 5.6 through 5.8. Hold the
concentrated extract for combining with the acid extract (see paragraph
6.4).

6.3	Add 500 mL of methylene chloride to a clean distilling flask and attach
it to the continuous extractor. Carefully adjust the pH of the aqueous
phase to less than 2 using sulfuric acid (1 + 1). Extract for 18
hours. Dry and concentrate the extract as described in paragraphs 5.6
through 5.8. Hold the concentrated extract and label as the acid
extract.

6.3.1 If the base/neutral and/or acid extracts cannot be concentrated
to a final volume of 1 mL, dilute the more concentrated extract
to the final volume of the least concentrated extract.

7.	The samples extracts are ready for GC/MS analysis. Proceed to Section
IV, GC/MS Analysis of Semivolatiles. If high concentrations are
suspected (e.g., highly colored extracts), the optional GC/FID screen
in Section III is recommended.

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PARI C - PROTOCOLS FOR SOIL/SEDIMENT

It is mandatory that all soil/sediment samples be characterized as to
concentration level so that the appropriate analytical protocol is chosen to
ensure proper quantitation limits for the sample. Mote that the terms "low
level" and "medium level" are not used here as a judgement of degree of
contamination but rather as a description of the concentration ranges that
are encompassed by the "low" and "medium" level procedures.

The laboratory is at liberty to determine the method of characterization.
The following two screening methods may be used for soil/sediment sample
characterization:

o Screen an aliquot from the "low level" 30 g extract or an aliquot from
the "medium level" 1 g extract.

o Screen using either GC/FID or GC/MS as the screening instrument.

The concentration ranges covered by these two procedures may be considered to
be approximately 330 ug/kg - 20,000 ug/kg for the low level analysis and
>20,000 ug/kg for medium level analysis for SNA extractables. For soils
only, the extract for pesticide/PCB analysis may be prepared from an aliquot
of the extract for semivolatiles, or in a separate extraction procedure. If
it is prepared from the semivolatile extract, refer to Exhibit D PEST for the
procedures for extraction of pesticides/PCBs.

Screen from the Medium Level Method

Take 5.0 mL from the 10.0 mL total extract and concentrate to 1.0 mL and
screen. If the sample concentration is >20,000 ug/kg proceed with GC/MS
analysis of the organics. If the sample concentration is <20,000 ug/kg
discard the medium level extract and follow the low level method.

Screen from Low Level Method

Take 5.0 mL from the 300 mL (approximate) total extract from the 30 g sample
and concentrate to 1.0 mL and screen. If the concentration is >20,000 ug/kg
in the original sample, discard the 30 g extract and follow the medium level
methods for organics, using medium level surrogates. If the sample
concentration is <20,000 ug/kg, proceed with concentration and the remainder
of the low level method.

1- Medium Level Preparation for Screening and Analysis of Semlvolatlleg

Ml

1.1 Scope and Application

This procedure is designed for the preparation of sediment/soil samples
which may contain organic chemicals at a level greater than 20,000
ug/kg.

1.1.1. The extracts and sample allquots prepared using this method are
screened by GC/MS or FID, using capillary columns for
base/neutral and acid priority pollutants, and related organic
chemicals. The results of these screens will determine whether

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sufficient quantities of pollutants are present to warrant
analysis by low or medium protocol.

1.1.2 If the screenings indicate no detectable pollutants at the

lower limits of quantitation, the sample should be prepared by
the low level protocol in Section II, Part C, paragraph 2.

1.2	Summary of Method

1.2.1. Approximately 1 g portions of sediment/soil are transferred to
vials and extracted with methylene chloride. The methylene
chloride extract is screened for extractable organics by GC/FID
or GC/MS.

1.2.2	If organic compounds are detected by the screen, the methylene
chloride extract is analyzed by GC/MS for extractable organics.

1.2.3	If no organic compounds are detected by the medium level
screen, then a low level sample preparation is required.

1.3	Interferences

1.3.1. Method interferences may be caused by contaminants in solvents,
reagents, glassware, and other sample processing hardware that
lead to discrete artifacts and/or elevated baselines in the
total ion current profiles. All of these materials must be
routinely demonstrated to be free from interferences under the
conditions of the analysis by running laboratory reagent
blanks. Matrix interferences may be caused by contaminants that
are coextracted from the sample. The extent of matrix
interferences will vary considerably from source to source.

1.4	Limitations

1.4.1. The procedure is designed to allow quantitation limits for
screening purposes as low as 20,000 ug/kg for extractable
organics. For analysis purposes, the quantitation limits are
20,000 ug/kg for extractable organics. If peaks are present
based on the GC/FID screen, the sample is determined to require
a medium level analysis by GC/MS. Some samples may contain
high concentrations of chemicals that Interfere with the
analysis of other components at lower levels; the quantitation
limits in those cases may be significantly higher.

1.4.2 These extraction and preparation-procedures were developed for
rapid and safe handling of high concentration hazardous waste
samples. The design of the methods thus does t»ot stress
efficient recoveries or low limits of quantitation of all
components. Rather, the procedures were designed to screen at
moderate recovery end sufficient sensitivity, a broad spectrum
of organic chemicals. The results of the analyses thus may
reflect only a minimum of the amount actually present in some
samples.

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1.5 Reagents

1.5.1. Sodium Sulfate - anhydrous powdered reagent grade, heated at
400*C for four hours, cooled in a desiccator, and stored in a
glass bottle Baker anhydrous powder, catalog # 73898 or
equivalent.

1.5.2	Methylene chloride. Pesticide residue analysis grade or
equivalent.

1.5.3	Methanol. Pesticide residue analysis grade or equivalent.

1.5.4	Acetone. Pesticide residue analysis grade or equivalent.

1.5.5	Base/Neutral and Acid Surrogate Standard Spiking Solution

The compounds specified are phenol-dg, 2,4,6-tribromophenol,
2-fluorophenol, nitrobenzene-dg, terphenyl-dj* *nd
2-fluorobipheny 1. Prepare a solution containing these
compounds for base/neutral surrogates at a concentration of 100
ug/1.0 mL, and for acid surrogate standards at a concentration
of 200 ug/1.0 mL in methanol. Store the spiking solutions at
4*C (±2*C) in Teflon-sealed containers. The solutions should
be checked frequently for stability. These solutions must be
replaced after twelve months, or sooner, if comparison with
quality control check samples Indicates a problem.

1.5.6	Base/Neutral and Acid Matrix Standard Spiking solution.

Prepare a spiking solution in methanol that contains the
following compounds at a concentration of 100 ug/1.0 mL for
base/neutrals and 200 ug/1.0 mL for acids. Store the spiking
solutions at 4*C (±2*C) in Teflon-sealed containers. The
solutions should be checked frequently for stability. These
solutions must be replaced after twelve months, or sooner, if
comparison with quality control check samples indicates a
problem.

Bfigg Wwtralft	Addi

1,2,4-trlchlorobenzene	pentachlorophenol

acenaphthene	phenol

2,4-dinitrotoluene	2-chlorophenol

pyrene	4-chloro-3-methylphenol

N-nitroso-di-n-propylamine	4-nitrophenol

1,4-dichlorobenzene

1.6 Equipment

1.6.1. Glass scintillation vials, at least 20 mL, with screw cap and
teflon or aluminum foil liner.

1-6.2 Spatula. Stainless steel or Teflon.

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1.6.3	Balance capable of weighing 100 g to ± 0.01 g.

1.6.4	Vials and caps, 2 mL for GC auto sampler.

1.6.5	Disposable pipets, Pasteur; glass wool rinsed with methylene
chloride.

1.6.6	15-mL concentrator tubes.

1.6.7	Ultrasonic cell disruptor, Heat Systems Ultrasonics, Inc.,

Model W-385 SONICATOR (475 Watt with pulsing capability, No.
200 1/2 inch tapped disruptor horn plus No. 207 3/4 inch tapped
disruptor horn, and No. 419 1/8 inch standard tapered MICROTIP
probe), or equivalent device with a minimum of 375 Watt output
capability. NOTE: In order to ensure that stifficient energy
is transferred to the sample during extraction, the MICROTIP
probe must be replaced if the tip begins to erode. Erosion of
the tip is evidenced by a rough surface.

1.6.8	Sonabox acoustic enclosure - recommended with above disruptors
for decreasing cavitation sound.

1.6.9	Test tube rack.

1.6.10	Oven, drying.

1.6.11	Desiccator.

1.6.12	Crucibles, porcelain.

1.7 Medium Level Sample Preparation.

1.7.1. Transfer the sample container into a fume hood. Open the

sample vial. Decant and discard any water layer and then mix
the sample. Transfer approximately 1 g (record weight to the
nearest 0.1 g) of sample to a 20-mL vial. Vipe the mouth of
the vial with a tissue to remove any sample material. Record
the exact weight of sample taken. Cap the vial before
proceeding with the next sample to avoid any
cro ss-contamination.

1.7.1.1 Transfer 50 g of soil/sediment to 100 mL beaker.

Add 50 mL of water and stir for 1 hour. Determine
pH of sample with glass electrode and pH meter while
stirring. Report pH value on appropriate data
sheets. If the pH of the soil is greater than 11 or
less than 5, contact the Deputy Project Officer
cited in the contract for Instructions on how to
handle the sample. Document the instructions in the
Case Narrative. Discard this portion of •ample.

1.7.2 Immediately after weighing the sample for extraction, weigh
5-10 g of the sediment into a tared crucible. Determine the
percent moisture by drying overnight at 105*C. Allow to cool

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in a desiccator before weighing. Concentrations of individual
analytes will be reported relative to the dry weight of
sediment.

g of sample - g of dry sample x 100 _ % aoistuce
g of sample

1.7.3	Add 2.0 g of anhydrous powdered sodium sulfate to sample in the
20 mL vial from paragraph 1.7.1 and mix well.

1.7.4	Surrogate Standards are added to all samples, spikes, and
blanks. Add 1.0 mL of surrogate spiking solution to sample
mixture.

1.7.5	Add 1.0 mL of matrix standard spiking solution to each of two 1
g portions from the sample chosen for spiking.

1.7.6	Immediately add 9.0 mL of methylene chloride to the sample and
disrupt the sample with the 1/8 inch tapered MICROTIP
ultrasonic probe for 2 minutes at output control setting 5, in
continuous mode. (If using a sonicator other than Models W-375
or W-385, contact the Project Officer for appropriate output
settings). Before extraction, make certain that the sodium
sulfate is free flowing and not a consolidated mass. As
required, break up large lumps with a clean spatula, or yery
carefully with the tip of the unenergized probe.

1.7.6.1. Add only 8.0 mL of methylene chloride to the matrix
spike samples to achieve a final volume of 10 mL.

1.7.7	Loosely pack disposable Pasteur pipets with 2-3 cm glass wool
plugs. Filter the extract through the glass wool and collect
5.0 mL in a concentrator tube.

1.7.8	Concentrate the extract to 1.0 mL by the nitrogen blowdown
technique described in paragraph 2.7.3.

1.7.9	Transfer the concentrate to an autosampler vial for GC/FID or
GC/MS capillary column screening. If the concentrate is
screened, the quantitation limits should be approximately
20,000 ug/kg.

1.7.10	Proceed to Section III, paragraph 1.

Low Level Preparation f™- Screening and Analysis of Senivolatileg (BNA)
Summary of Method

A 30 gram portion of sediment is mixed with anhydrous powdered sodium
sulfate and extracted with 1:1 methylene chloride/acetone using an
ultrasonic probe. If the optional low level screen is used, a portion
of this dilute extract is concentrated fivefold and is screened by
GC/FID or GC/MS. If peaks are present at greater than 20,000 ug/kg,
discard the extract and prepare the sample by the medium level method.

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If no peaks are present at greater than 20,000 ug/kg, the extract is
concentrated. An optional gel permeation column cleanup nay be used
before analysis.

2.2	Interferences

Method Interferences nay be caused by contaninants in solvents,
reagents, glassware and other sample processing hardware that lead to
discrete artifacts and/or elevated baselines in the total ion current
profiles.

All of these naterials must be routinely denonstrated to be free from
interferences under the conditions of the analysis by running
laboratory reagent blanks. Matrix interferences nay be caused by
contaninants that are coextracted from the sanple. The extent of
matrix interferences will vary considerably fron source to source.

2.3	Apparatus and Materials

2.3.1	Apparatus for determining percent moisture

2.3.1.1	Oven, drying

2.3.1.2	Desiccator

2.3.1.3	Crucibles, porcelain

2.3.2	Disposable Pasteur glass pipets, 1 mL

2.3.3	Ultrasonic cell disruptor, Heat Systems - Ultrasonics, Inc.
Model 385 SONIGATOR (475 Watt with pulsing capability, No. 305
3/4 inch tapped high gain "Q" disruptor horn or No. 208 3/4
inch standard solid disruptor horn), or equivalent device with
a nininun of 375 Watt output capability. NOTE: In order to
ensure that sufficient energy is transferred to the sample
during extraction, the horn must be replaced if the tip begins
to erode. Erosion of the tip is evidenced by a rough surface.

2.3.3.1 Sonabox acoustic enclosure - recommended with above
disruptors for decreasing cavitation sound.

2.3.4	Beakers, 400 mL

2.3.5	Vacuum filtration apparatus

2.3.5.1	Buchner funnel.

2.3.5.2	Filter paper, Vhatman No. 41 or equivalent.

2.3.6	Kudema-Danish (K-D) apparatus.

2.3.6.1 Concentrator tube - 10 mL, graduated (Kontes
K-570040-1025 or equivalent).

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2.3.6.2	Evaporative flask - 500 mL (Kontes K-570001-0500 or
equivalent).

2.3.6.3	Snyder column - three-ball macro (Kontes
K-503000-0121 or equivalent).

2.3.6.4	Snyder column - two-ball micro (Kontes
K-569001-0219) or equivalent).

2.3.7	Silicon carbide boiling chips - approximately 10/40 mesh. Heat
to 400*C for 30 minutes or Soxhlet extract with methylene
chloride.

2.3.8	tfater bath - heated, with concentric ring cover, capable of
temperature control (±2*C). The bath should be used in a hood.

2.3.9	Balance, capable of accurately weighing ± 0.01 g.

2.3.10	Vials and caps, 2 mL for GC auto sampler.

2.3.11	Balance - Analytical, capable of accurately weighing ± O.OOOlg.

2.3.12	Nitrogen evaporation device equipped with a water bath that can
be maintained at 35-40*C. The N-Evap by Organomation
Associates, Inc., South Berlin, MA (or equivalent) is suitable.

2.3.13	Gel permeation chromatography (GPC) cleanup device. NOTE: GPC
cleanup is highly raeommendad for all extracts for low level
soils.

2.3.13.1	Automated system

2.3.13.1.1	Gel permeation chromatograph Analytical
Biochemical Labs, Inc. GPC Autoprep
1002 or equivalent including:

2.3.13.1.2	25 mm ID X 600 - 700 mm glass column
packed with 70 g of Bio-Beads SX-3.

2.3.13.1.3	Syringe, 10 mL with Luer-Lock fitting.

2.3.13.1.4	Syringe filter holder and filters -
stainless steel and TFE, Gelman 4310 or
equivalent.

2.3.13.2	Manual system assembled from parts. (Vise, R.H.,
Bishop, D.F., Williams, R.T. & Austern, B.M. "Gel
Permeation Chromatography in the GC/MS Analysis of
Organics in Sludges" U.S. EPA, Municipal
Environmental Research Laboratory - Cincinnati, Ohio
45268)

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2.3.13.2.1

25 mm ID X 600 - 700 mm heavy wall
glass column packed with 70 g of
BIO-Beads SX-3.

2.3.13.2.2	Pump: Altex Scientific, Model No.
1001A, seaipreparative, solvent
metering system. Pump capacity - 28
mL/min.

2.3.13.2.3	Detector: Altex Scientific, Model No.
153, with 254 m UV source and 8-ul
semi-preparative flowcells (2-mm
pathlengths)

2.3.13.2.4	Microprocessor/controller: Altex
Scientific, Model No. 420,
Microprocessor System Controller, with
extended memory.

2.3.13.2.5	Injector: Altex Scientific, Catalog
No. 201-56, sample injection valve,
Tefzel, with 10 mL sample loop.

2.3.13.2.6	Recorder: Linear Instruments, Model
No. 385, 10-inch recorder.

2.3.13.2.7	Effluent Switching Valve: Teflon
slider valve, 3-way with 0.060" ports.

2.3.13.2.8	Supplemental Pressure Gauge with
connecting Tee: U.S.Gauge, 0-200 psi,
stainless steel. Installed as a
"downstream" monitoring device between
column and detector.

Flow rate was typically 5 mL/min. of
methylene chloride. Recorder chart
speed was 0.50 cm/min.

2.3.14

2.3.15

Pyrex glass wool.

Pasteur pipets, disposable.

2.4 Reagents

2.4.1	Sodium Sulfate - anhydrous powdered reagent grade, heated at
400*C for four hours, cooled in a desiccator, and stored in a
glass bottle. Baker anhydrous powder, catalog #73898 or
equivalent.

2.4.2	Methylene chloride, methanol, acetone, isooctane, 2-propanol
and benzene pesticide quality or. equivalent.

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2.4.3

Reagent water - Reagent water Is defined as a water in which an
interferent is not observed at or above the CRQL of each
parameter of interest.

2.4.4	GPC calibration solutions:

2.4.4.1	Com oil - 200 mg/mL in methylene chloride.

2.4.4.2	Bis(2-ethylhexylphthalate) and pentachlorophenol 4.0
mg/mL in methylene chloride.

2.4.5	Sodium Sulfite, reagent grade.

2.4.6	Surrogate standard spiking solution.

2.4.6.1 Base/neutral and acid surrogate solution.

2.4.6.1.1	Surrogate standards are added to all
samples, blanks, matrix spikes, matrix
spike duplicates, and calibration
solutions; the compounds specified for
this purpose are phenol-de,

2,4,6-tribroaophenol, 2-fluorophenol,
nitrobenzene-d^, terpheny1-di^ and
2-fluorobiphenyl. Two additional
surrogates, one base/neutral and one
acid may be added.

2.4.6.1.2	Prepare a surrogate standard spiking
solution at a concentration of 100
ug/1.0 mL for base/ neutral and 200
ug/1.0 mL for acids in methanol. Store
the spiking solutions at 4*C (±2*C) in
Teflon-sealed containers. The
solutions must be replaced after twelve
months, or sooner if comparison with
quality control check samples indicate
a problem.

2.4.7 Matrix standard spiking solutions.

^2.4.7.1 Base/neutral and acid matrix spiking solution
consists of:

Base/Neutrala (100 ug/1.0 mL)

1,2,4-trichlorobenzene
acenaphthene
2,4- dinitro toluene
pyrene

N-nitroso-di-n-propylamine
1,4-dichlorobenzene

Acids (200 ug/1.0 mL)

pentachlorophenol
phenol

2-chlorophenol
4•chloro-3-methylphenol
4-nitrophenol

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Prepare a spiking solution that contains each of the
above in methanol. Store the spiking solutions at
4*C (±2*C) in Teflon-sealed containers. The
solutions should be checked frequently for
stability. These solutions must be replaced after
twelve months, or sooner if comparison with quality
control check samples indicate a problem.

Matrix spikes also serve as duplicates, therefore,
add volume specified in Sample Extraction section to
each of two 30-g portions from one sample chosen for
spiking.

2.5 Low Level Sample Preparation

2.5.1 Decant and discard any water layer on a sediment sample. Mix

samples thoroughly, especially composited samples. Discard any
foreign objects such as sticks, leaves, and rocks.

2.5.1.1 Transfer 50 g of soil/sediment to 100 mL beaker. Add
50 mL of water and stir for 1 hour. Determine pH of
sample with glass electrode and pH meter while
stirring. Report pH value on appropriate data
sheets. If the pH of the soil is greater than 11 or
less than 5, contact the Deputy Project Officer
cited in tiie contract for instructions on how to
handle the sample. Document the instructions in the
Case Narrative. Discard this portion of sample.

2.5.2 The following steps should be performed rapidly to avoid loss

of the more volatile extractables. Weigh approximately 30 g of
sample to the nearest 0.1 g into a 400-mL beaker and add 60 g
of anhydrous powdered sodium sulfate. Mix well. The sample
should have a sandy texture at this point. Immediately, add
100 mL of 1:1 methylene chloride - acetone to the sample, then
add the surrogates according to paragraph 2.5.2.3.

2.5.2.1	Immediately after weighing the sample for
extraction, weigh 5-10 g of the sediment into a
tared crucible. Determine the percent moisture by
drying overnight at 105*C. Allow to cool in a
desiccator before weighing. Concentrations of
individual analytes will be reported relative to the
dry weight of sediment.

g of sample - g of dry sample

	g 6{		 * 100 - % moisture

2.5.2.2	Weigh out two 30 g (record weight to nearest 0.1 g)
portions for use as matrix and matrix spike
duplicates according to 2.5.2. When using GPC
cleanup, add 2.0 1L of the base/neutral and acid
matrix spike to each of two portions. When not

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vising GPC cleanup, add 1.0 mL of base/neutral and
acid matrix spike to each of the other two portions.

2.5.2.3 When using GPC, add 1.0 mL of base/neutral and acid
surrogate standard to the sample. When not using
GPC, add 0.5 mL of BNA surrogate standard to the
sample.

2.5.3	Place the bottom surface of the tip of the 3/4 inch disruptor
horn about 1/2 inch below the surface of the solvent but above
the sediment layer.

2.5.4	Sonicate for 1 1/2 minutes with the W-385 (or 3 minutes with
the W-375), using No. 208 3/4 inch standard disruptor horn with
output control knob set at 10 (or Ho. 305 3/4 inch tapped high
gain "Q" disruptor horn at 5) and mode switch on "1 sec. pulse"
and % duty cycle knob set at 50%. Do NOT use MICROTIP probe.
(If using a sonicator other than Models ff-375 or W-385, contact
the Project Officer for appropriate output settings).

2.5.5	Decant and filter extracts through Whatman #41 filter paper
using vacuum filtration or centrifuge and decant extraction
solvent.

2.5.6	Repeat the extraction two more times with 2 additional 100 mL
portions of 1:1 methylene chloride - acetone. Before each
extraction, Bake certain that the sodium sulfate is free
flowing and not a consolidated mass. As required, break up
large lumps with a clean spatula, or very carefully with the
tip of the probe. Decant off the extraction solvent after each
sonication. On the final sonication, pour the entire sample
into the Buchner funnel and rinse with 1:1 methylene chloride -
acetone.

2.5.6.1 If the sample is to be screened from the low level
method, take 5.0 mL and concentrate to 1.0 mL
following paragraph 2.7.2 or 2.7.3. Note that the
sample volume in this case is 5.0 mL not 10,0 mL as
given in 2.7.2. Screen the extract as per Section
III, paragraph 1., "Screening of Extractable Organic
Extracts." Transfer the remainder of the 1 mL back
to the total extract from paragraph 2.5.6 after
GC/FID or GC/MS screening. (CAUTION: To minimize
sample loss, autosamplers which pre-flush samples
through the syringe should not be used.)

2.5.7	Transfer the extract to a Kuderna-Danish (K-D) concentrator
consisting of a 10 mL concentrator tube and a 500 mL
evaporative flask. Other concentration devices or techniques
may be used if equivalency is demonstrated for all extractable
compounds listed in Exhibit C.

2.5.8	Add one or two clean boiling chips to the evaporative flask and
attach a three-ball Snyder column. Pre-wet the Snyder column

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by adding about 1 mL methylene chloride to the top. Place the
K-D apparatus on a hot water bath (80 to 90'C) so that the
concentrator tube Is partially Immersed In the hot water and
the entire lower rounded surface of the flask Is bathed with
hot vapor. Adjust the vertical position of the apparatus and
the water temperature as required to complete the concentration
In 10 to 15 minutes. At the proper rate of distillation the
balls of the column will actively chatter but the chambers will
not flood with condensed solvent. When the apparent volume of
liquid reaches 1 mL, remove the K-D apparatus and allow It to
drain and cool for at least 10 minutes, and make up to 10 mL
volume with methylene chloride.

2.5.9 If GPC cleanup is not used proceed to paragraph 2.7.

2.6. Extract Cleanup

2.6.1 GPC Setup and Calibration

2.6.1.1	Packing the column - Place 70 g of Bio Beads SX-3 in
a 400 mL beaker. Cover the beads with methylene
chloride; allow the beads to swell overnight (before
packing the columns). Transfer the swelled beads to
the column and start pumping solvent through the
column, from bottom to top, at 5.0 mL/min. After
approximately 1 hour, adjust the pressure on the
column to 7 to 10 psi and pump an additional 4 hours
to remove air from the column. Adjust the column
pressure periodically as required to maintain 7 to

10	psi.

2.6.1.2	Calibration of the column - Load 5 mL of the corn

011	solution into sample loop No. 1 and 5 mL of the
phthalatephenol solution into loop No. 2. Inject
the com oil and collect 10 mL fraction (i.e.,
change fraction at 2•minute intervals) for 36
minutes. Inject the phthalate-phenol solution and
collect 15 mL fractions for 60 minutes. Determine
the corn oil elution pattern by evaporation of each
fraction to dryness followed by a gravimetric
determination of the residue. Analyze the
phthalate-phenol fractions by GC/FID on the DB-5
capillary column, a UV spectrophotometer or a GC/MS
system. Plot the concentration of each component in
each fraction versus total eluent volume (or time)
from the injection points. Choose a "dump time"
which allows 2^5% removal of the com oil and >85%
recovery of the bis(2-ethylhexyl)-phthalate. Choose
the "collect time" to extend at least 10 minutes
after the elution of pentachlorophenol. Wash the
column at least 15 minutes between samples. Typical
parameters selected are: Dump time, 30 minutes (150
mL), collect time, 36 minutes (180 mL) and wash
time, 15 minutes (75 mL). The column can also be

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calibrated by the use of a 254 mm UV cet&ctor in
place of gravimetric and GC analyses of fractions.
Measure the peak areas at various elution times to
determine appropriate fractions.

The SX-3 Bio Beads column may be reused for several
months, even if discoloration occurs. System
calibration usually remains constant over this
period of time if column flowrate remains constant.

2.6.2	GPC Extract Cleanup

Prefilter or load all extracts via the filter holder to avoid
particulates that might stop the flow. Load one 5.0 mL aliquot
of the extract onto the GPC column. Do not apply excessive
pressure when loading the GPC. Purge the sample loading tubing
thoroughly with solvent between extracts. After especially
dirty extracts, run a GPC blank (methylene chloride) to check
for carry-over. Process the extracts using the dump, collect
and wash parameters determined from the calibration and collect
the cleaned extracts in 400 mL beakers tightly covered with
aluminum foil. The phthalate-phenol calibration solution shall
be taken through the cleanup cycle with each set of 23 extracts
loaded into the GPC. The recovery for each compound must be
2:85%. This must be determined on a GC/FID, using a DB-5
capillary column, a UV recording spectrophotometer or a GC/MS
system. A copy of the printouts of standard and check solution
are required as deliverables with each case. Show % recovery
on the copy.

2.6.3	Concentrate the extract as per paragraphs 2.5.7 and 2.5.8.

2.7 Final Concentration of Extract with Optional Extract Splitting
Procedure

If the extract in 2.5.8 is to be used only for semivolatile analysis,
it must be concentrated to a volume of 1.0 mL, following the procedure
in 2.7.2.1.

If the extract in 2.5.8 is to be used for both semivolatile and
pesticide/PCB analyses, then it must be split into two portions,
that case, follow the procedure in 2.7.1 to obtain the pesticide
portion, and follow that with the procedure in 2.7.2.2 to obtain
semivolatile portion.

Refer to Exhibit D PEST for specific instructions regarding the
treatment of extracts for pesticide analysis.

2.7.1 If the same extract is used for both semivolatile and

pesticide/PCB analyses, to split out the pesticide extract,
transfer 0.5 mL of the 10 mL methylene chloride extract from
2.5.8 to a separate concentrator tube. Add 5 mL of hexane and
a silicon carbide boiling chip and mix using vortex mixer.
Attach a two-ball micro-Snyder column. Pre-wet the Snyder

In
the

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column by adding 0.5 aL of hexane to the top of the column.
Place the K-D apparatus on a hot water bath (80 - 90*C) so that
the concentrator tube Is partially immersed in the hot water.
Adjust the vertical position of the apparatus and the water
temperature as required to complete the concentration in 5 to
10 minutes. Concentrate the extract to an apparent volume of
less than 1 mL. Use Nitrogen blowdown (see 2.7.3) to reduce
the volume to 0.5 mL. Add 0.5 mL of acetone. The pesticide
extract must now be passed through an alumina column to remove
the BNA surrogates and polar interferences. Proceed to
paragraph 2.8 of the pesticide/PCB method (Exhibit D PEST).

2.7.2 Concentration of the semivolatile extract.

2.7.2.1	If the extract in 2.5.8 was not split to obtain a
portion for pesticide analysis, reattach the
micro-Snyder column to the concentrator tube used in
2.5.8 which contains the 10 mL extract and add a
fresh silicon carbide boiling chip to the
concentrator tube. Pre-wet the Snyder column with
0.5 mL of methylene chloride. Place the K-D
apparatus on the hot water bath (80 - 90*C) so that
the concentrator tube is partially immersed in the
hot water. Adjust the vertical position of the
apparatus and the water temperature as required to
complete the concentration in 5 to 10 minutes. When
the apparent volume of the liquid reaches 0.5 mL,
remove the K-D apparatus from the water bath and
allow it to drain for at least 10 minutes while
cooling. Remove the Snyder column and rinse the
lower joint into the concentrator tube with 0.2 mL
of methylene chloride. Adjust the final volume to
1.0 mL with methylene chloride. If GPC cleanup was
used, this 1.0 mL represents a two-fold dilution to
account for only half of the extract going through
the GPC.

2.7.2.2	If the extract in 2.5.8 ££& split in 2.7.1 to obtain
a portion for pesticide analysis, reattach the
micro-Snyder column to the concentrator tube used in
2.5.8 which contains the 9.5 mL extract and add a
fresh silicon carbide boiling chip to the
concentrator tube. Pre-wet the Snyder column with
0.5 mL of methylene chloride. Place the K-D
apparatus on the hot water bath (80 - 90*C) so that
the concentrator tube in partially immersed in the
hot water. Adjust the vertical position of the
apparatus and the water temperature as required to
complete the concentration in 5 to 10 minutes. When
the apparent volume of the liquid reaches 0.5 mL,
remove the K-D apparatus from the water bath and
allow it to drain for.at least 10 minutes while
cooling. Remove the Snyder column and rinse the
lower joint into the concentrator tube with 0.2 mL

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of methylene chlorid«. Adjust the final volume to
0.95 nL with nethylene chloride. If GPC cleanup was
used, this 0.95 nL represents a twofold dilution to
account for only half of the extract going through
the GPC, and therefore, the sample detection limit
for the sample would be 2x CRQL (see Exhibit B).

2.7.3	Nitrogen blowdown technique (taken from ASTM Method D 3086).
The following method may be used for final concentration of the
BNA extract instead of the procedures in paragraph 2.7.2.

Place the concentrator tube in a warm water bath (35*C) and
evaporate the solvent volume to below 1 mL using a gentle
stream of clean, dry nitrogen (filtered through a column of
activated carbon). Caution: New plastic tubing must not be
used between the carbon trap and the sample, since it may
introduce Interferences.

The internal wall of the tube must be rinsed down several times
with methylene chloride during the operation. During
evaporation, the tube solvent level must be kept below the
water level of the bath. The extract must never be allowed to
become dry.

If the extract in 2.5.8 was not split for both semivolatile and
pesticide analyses, bring the final volume of the extract to
1.0 mL with methylene chloride. This represents a ten-fold
concentration. If Che extract in 2.5.8 was split in 2.7.1,
then bring the final volume of the semivolatile portion to 0.95
mL with methylene chloride. This represents a similar ten-fold
concentration. In either case, if GPC cleanup techniques were
employed, the final volume (1.0 or 0.95 mL) represents a
two-fold dilution to account for Che fact that only half the
extract went through the GPC.

2.7.4	Store all extracts at 4*C (±2*C) in the dark in Teflon-sealed
containers.

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SECTION III

SCREENING OF SEMIVOLATILE
ORGANIC EXTRACTS

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1.

Snimnar^ of Method

1.1

2.
2.1

3.

3.1

3.2

can be prepared from pure standard materials or purchased
solutions.

3.2.1.1	Prepare stock standard solutions by accurately
weighing about 0.0100 g of pure material. Dissolve
the material in pesticide quality methylene
chloride and dilute to volume in a 10 mL volumetric
flask. Larger volumes may be used at the
convenience of the analyst. If compound purity is
assayed at 96% or greater, the weight may be used
without correction to calculate the concentration
of the stock standard. Commercially prepared stock
standards may be used at any concentration if they
are certified by the manufacturer or by an
independent source and are traceable to

EMSL/LV-supplied standards.

3.2.1.2	Transfer the stock standard solutions into Teflon
sealed screw-cap bottles. Store at -10*C to -20*C
and protect from light. Stock standard solutions
should be checked frequently for signs of
degradation or evaporation, especially just prior
to preparing calibration standards from them.

Stock standard solutions must be replaced after six
months or sooner if comparison with quality control

The solvent extracts of water and sediment/soil are screened on a gas
chromatograph/flame ionization detector (GC/FID) using a fused silica
capillary column (FSCC). The results of the screen will determine the
concentration of extract taken for GC/MS analysis.

Apparatus and Materials

Gas chromatograph - An analytical system complete with a temperature
programmable gas chromatograph and all required accessories including
syringes, analytical columns, and gases. The injection port must be
designed for on-column injection when using packed columns and for
splitless injection when using capillary columns.

2.1.1	Above GC equipped with flame ionization detector.

2.1.2	GC column - 30 m x 0.32 mm, 1 micron film thickness, silicone
coated, fused silica capillary column (J & V Scientific DB-S
or equivalent).

fteftgSTitg

Methylene chloride - pesticide residue analysis grade or equivalent.

GC calibration standard. Prepare a standard solution containing
phenol, phenanthrene and di-n-octylphthalate.

3.2.1 Stock standard solutions (1.00 ug/uL)-Stock standard solutions

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check samples indicates a problem. Standards
prepared from gases or reactive compounds such as
styrene must be replaced after two months, or
sooner if comparison with quality control'check
samples indicates a problem.

3.2.2 Prepare a working standard mixture of the three compounds in
methylene chloride. The concentration must be such that the
volume injected equals 50 ng of each compound. The storage
and stability requirements are the same as specified in
3.2.1.2.

4.	GC Calibration

4.1 At the beginning of each 12 hour shift, inject the GC calibration
standard. The following criteria must be:

4.1.1	Standardized for half scale response from 50 ng of
phenanthrene.

4.1.2	Adequately separates phenol from the solvent front.

4.1.3	Minimum of quarter scale response for 50 ng of
di-n-octylphthalate.

5.	GC/FID Screening

5.1	Suggested GC operating conditions:

Initial Column Temperature Hold - 50*C for 4 minutes
Column Temperature Program - 50 - 280*C at 8 degrees/min.

Final Column Temperature Hold - 280*C for 8 minutes
Injector - Grob-type, splitless
Sample Volume - 1 uL - 2 uL

9

Carrier Gas - Helium at 30 cm /sec

5.2	Inject the GC calibration standard and ensure the criteria specified in
4. are met before injecting samples. Estimate the response for 10 ng
of phenanthrene.

5.3	Inject the appropriate extracts from Section II, including blanks.

6.	Interpretation of Chronatograms
6.1 Water

6.1.1 If no sample peaks are detected, or all are less than full

scale deflection, the undiluted extract is analyzed on GC/MS.

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6 12 If any sample peaks are greater than full scale deflection,

calculate the dilution necessary to reduce the major peaks to
between half and full scale deflection. Use this dilution
factor to dilute the extract for GC/MS analysis.

6.2 Soil/Sediment

6 2 1 If no sample peaks from the extract (from low or medium level
preparation) are detected, or all are less than 10% full scale
deflection, the sample must be prepared by the low level
protocol, Section II, Part C, paragraph 2.

6.2.2	Peaks are detected at greater than 10% full scale deflection
and less than or equal to full scale deflection.

6.2.2.1	If the screen is from the medium level extract,
proceed with GC/MS analysis of this extract with
appropriate dilution if necessary.

6.2.2.2	If screen is from the low level extract, discard
extract and prepare sample by medium level method
for GC/MS analysis.

6.2.3	Peaks are detected at greater than full scale deflection:

6.2.3.1	If the screen is from the medium level preparation,
calculate the dilution necessary to reduce the
major peaks to between half and full scale
deflection. Use this dilution factor to dilute the
extract. This dilution is analyzed by GC/MS for
extractable organic*.

6.2.3.2	If the screen i« from the low level preparation,
discard the extract and prepare a sample by the
medium level method for GC/MS analysis.

7.	Analysis

7 1 Use the information from 6. to perform the GC/MS analysis of extracta-

bles in Section IV, GC/MS Analysis of Semivolatlles, paragraph 1.

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SECTION IV
GC/MS ANALYSIS OF SEHIVOIATILES

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1.	Swrnnnry of Method

This method is to be used for the GC/MS analysis of semivolatiles
screened by Section III protocols and for confirmation of
pesticides/PCBs identified by GC/EC, if concentrations permit.

2.	Apparatus and Materials

2.1 Gas chromatograph/aass spectrometer system.

2.1.1	Gas chromatograph - An analytical system complete with a
temperature programmable gas chromatograph suitable for
splitless injection and all required accessories including
syringes, analytical columns and gases.

2.1.2	Column - 30 m x 0.25 mm ID (or 0.32 mm) bonded-phase silicone
coated fused silica capillary column (J&W Scientific DB-5 or
equivalent). A film thickness of 1.0 micron is recommended
because of its larger capacity. A film thickness of 0.25
micron may be used.

2.1.3	Mass Spectrometer - Capable of scanning from 35 to 500 amu
every 1 second or less, utilizing 70 volts (nominal) electron
energy in the electron impact ionization mode and producing a
mass spectrum which meets all required criteria when 50 ng of
decafluorotriphenylphosphine (DFTPP) is injected through the GC
inlet. NOTE: DFTPP criteria must be met before any sample
extracts are analyzed. Any samples analyzed when DFTPP
criteria have not been met will require reanalysis at no cost
to the Government.

2.1.4	Data system - A computer system must be interfaced to the mass
spectrometer that allows the continuous acquisition and storage
on machine readable media of all mass spectra obtained
throughout the duration of the chromatographic program. The
computer must have software that allows searching any GC/MS
data file for ions of a specific mass and plotting such ion
abundances versus time or scan number. This type of plot is
defined as an Extracted Ion Current Profile (EICP). Software
must also be available that allows integrating the abundance in
any EICP between specified time or scan number limits.

3.	Reagents

3.1 Internal standards - 1,4 dichlorobenzene-, naphthalene-dg,

acenaphthene-d^Q, phenanthrene-d^g, chrysene-dj^. perylene-dj^ •

An internal standard solution can be prepared by dissolving 200 mg of
each compound in 50 mL of methylene chloride. It may be necessary to
use 5 to 10 percent benzene or toluene in this solution and a few
minutes of ultrasonic mixing in order to dissolve all the constituents.
The resulting solution will contain each standard at a concentration of
4000 ng/uL. A 10 uL portion of this solution should be added to each 1

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bL of sample extract. This will give a concentration of 40 ng/uL of
each constituent.

3.2 Prepare calibration standards at a minimum of five concentration

levels. Each calibration standard should contain each compound of
interest and each surrogate standard. (See GC/MS calibration in
Exhibit E for calibration standard concentration.)Great care must be
taken to maintain the integrity of all standard solutions. Store all
standard solutions at -10*C to -20*C in screw-cap amber bottles with
teflon liners. Fresh standards should be prepared every twelve months
at a minimum. The continuing calibration standard should be prepared
weekly and stored at 4*C (+2*C).

4. Calibration

4.1	Each GC/MS system must have the hardware tuned to meet the criteria
listed in Exhibit E for a 50 ng injection of decafluorotriphenyl
phosphine (DFTPP). No sample analyses can begin until all these
criteria are met. This criteria must be demonstrated each 12 hour
shift. DFTPP has to be injected to meet this criterion.
Post-acquisition manipulation of abundances is not acceptable.

4.2	The internal standards selected in paragraph 2.3.1 should permit most
components of interest in a chromatogram to have retention times of
0.80 to 1.20 relative to the Internal standards (see instructions for
Form VI, Initial Calibration Data). Use the base peak ion from the
specific internal standard as the primary ion for quantification, found
in Exhibit E, Table 2.2. If interferences are noted, use the next most
Intense ion as the secondary ion, i.e. For 1,4-dichlorobenzene-d^ use
m/z 152 for quantification.

4.2.1 The internal standards are added to all calibration standards
and all sample extracts just prior to analysis by GC/MS. A 10
uL aliquot of the internal standard solution should be added to
a 1 mL aliquot of calibration standards.

4.3	Analyze 1 uL of each calibration standard and tabulate the area of the
primary characteristic ion against concentration for each compound
including the surrogate compounds. Calculate relative response factors
(RRF) for each compound using Equation 1.

RRF - -— X —	Equation 1.

is cx

Where:

Ax - Area of the characteristic ion for the compound to be measured.

A^s - Area of the characteristic ion for the specific internal
standard from Exhibit E.

C^g - Concentration of the internal standard (ng/uL).

Cx - Concentration of the compound to be measure^ (ng/uL).

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4.3.1	The average relative response factor (RRF) should be calculated
for all compounds. A system performance check must be made
before this calibration curve is used. Four compounds (the
system performance check compounds) are checked for a minimum
average relative response factor. These compounds (the SFCC)
are N-nitroso-di-n-propylamine, heXachlorocyclopentadiene,
2,4-dinitrophenol, 4-nitrophenol. See instructions in Exhibit
E for Form VI, Initial Calibration Data for more details.

4.3.2	A % Relative Standard Deviation (%RSD) is calculated for
thirteen compounds labeled the Calibration Check Compounds
(CCC) on Form VI SV and in Table 2.3, Exhibit E, III SV. A
maximum % RSD is also specified for these compounds. These
criteria must be met for the calibration curve to be valid.

4.4	A check of the calibration curve must be performed once every 12 hours
during analysis. These criteria are described in detail in the
instructions for Form VII, Calibration Check. The minimum relative
response factor for the system performance check compounds must be
checked. If this criteria is met, the relative response factors of all '
compounds are calculated. A percent difference of the daily (12 hour)
relative response factor compared to the average relative response
factor from the initial curve is calculated. A maximum percent
difference is allowed for each compound flagged as 'CCC' on Form VII.

Only after both these criteria are met can sample analysis begin.

4.5	Internal standard responses and retention times in all standards must
be evaluated during or immediately after data acquisition. If the
retention time for any internal standard changes by more than 30
seconds from the latest daily (12 hour) calibration standard, the
chromatographic system must be Inspected for malfunctions, and
corrections made as required. The extracted ion current profile (EICF)
of the internal standards must be monitored and evaluated for each
standard. If EICP area for any internal standard changes by more than
a factor of two (-50% to +100%), the mass spectrometric system must be
inspected for malfunction and corrections made as appropriate. When
corrections are made, reanalysis of samples analyzed while the system
was malfunctioning is necessary.

5. GC/MS Analysis

5.1	The following instrumental parameters are required for all performance
tests and for all sample analyses:

Electron Energy - 70 volts (nominal)

Mass Range	- 35 to 500 amu

Scan Time	- not to exceed 1 second per scan

5.2	Confoine 0.5 mL of the base/neutral extract and 0.5 mL of acid from the
water extract prior to analysis.

5.3	Internal standard solution is added to each sample extract. For water
and/or medium soil extracts, add 10 uL of internal standard solution to
each accurately measured 1.0 mL of sample extract. If the low soil

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extracts required a pesticide split (see Section II, Part C, paragraph
2.7), add 9.5 uL of internal standard solution to each accurately
measured 0.95 oL of sample extract. Analyze the 1.0 mL extract by
GC/MS using a bonded-phase silicone-coated fused silica capillary
colum. The recommended GC operating conditions to be used are as
follows:

Initial Column Temperature Hold
Column Temperature Program

Final Column Temperature Hold
Injector Temperature
Transfer Line Temperature
Source Temperature

Injector
Sample Volume
Carrier Gas

40*C for 4 minutes

40-270*C at 10
degrees/mih.

270*C for 10 minutes

250-300'C

250-300*C

according to
manufacturer's
specifications

Grob-type, splitless

1 - 2 uL

%

Helium at 30 cm /sec

NOTE: Make any extract dilution indicated by
characterization prior to the addition of internal standards.
If any further dilutions of water or soil/sediment extracts are
made, additional internal standards must be added to maintain
the required 40 ng/uL of each constituent in the extract
volume. If the concentration on the column of any compound
exceeds the initial calibration range, the extract must be
diluted and reanalyzed. See Exhibit E, Section III, SV, Part 6.
Secondary ion quantitation is only allowed when there are
sample interferences with the primary ion. If secondary ion
quantitation is performed, document the reasons in the Case
Narrative.

6. tWLltatlv Analysis

6.1 The compounds listed in the Target Compound List (TCL), Exhibit C,

shall be identified by an analyst competent in the interpretation of
mass spectra (see PreAward Bid Confirmation description) by comparison
of the sample mass spectrum to the mass spectrum of a standard of the
suspected compound. Two criteria must be satisfied to verify the
identifications: (1) elution of the sample component at the GC
relative retention time as the standard component, and (2)
correspondence of the sample component and standard component mass
spectra.

6.1.1 For establishing correspondence of the GC relative retention

tine (RRT), the sample component RRT must compare within ±0.06
RRT units of the RRT of the standard component. For reference,
the standard must be run o» t&i tame shift §s the sample. If
eoelutlon of interfering components prohibits accurate

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assignment of the sample component RRT from the total Ion
chromatogram, the RRT should be assigned by using extracted ion
current profiles for ions unique to the component of interest.

6.1.2	For comparison of standard and sample component mass spectra,
mass spectra obtained on the contractor's GC/MS are required.
Once obtained, these standard spectra may be used for
identification purposes, only if the contractor's GC/MS meets
the DFTPP daily tuning requirements. These standard spectra
may be obtained from the run used to obtain reference RRTs.

6.1.3	The requirements for qualitative verification by comparison of
mass spectra are as follows:

6.1.3.1	All ions present in the standard mass spectra at a
relative intensity greater -than 10% (most abundant
ion in the spectrum equals 100%) must be present in
the sample spectrum.

6.1.3.2	The relative intensities of ions specified in (1)
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.)

6.1.3.3	Ions greater than 10% in the	spectrum but not
present in the standard spectrum must be considered
and accounted for by the analyst making the
comparison. In Task III, the verification process
should favor false positives. All compounds meeting
the identification criteria must be reported with
their spectra. For all compounds below the CRQL
report the actual value followed by "J", e.g. "3J."

6.1.4	If a compound cannot be verified by all of the criteria in
6.1.3, but in the technical judgement of the mass spectral
interpretation specialist, the identification is correct, then
the Contractor shall report that identification and proceed
with quantification in 7.

A library search shall be executed for non-TCL sample components for
the purpose of tentative Identification. For this purpose, the 1985
release of the National Bureau of Standards Mass Spectral Library (or
more recent release), containing 42,261 spectra, shall be used.

v

6.2.1 Up to 20 nonsurrogate organic compounds of greatest apparent
concentration not listed in Exhibit C for the combined base/
neutral/acid fraction shall be tentatively identified via a
forward search of the NBS mass spectral library. (Substances
with responses less than 10% of the nearest internal standard
are not required to be searched in this fashion). Only after
visual comparison of sample spectra with the nearest library
searches will the mass spectral interpretation specialist

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assign a tentative identification. NOTE: Computer generated
library search routines oust not vise normalization routines
that would misrepresent the library or unknown spectra when
compared to each other.

6.2.2 Guidelines for making tentative identification:

6.2.2.1	Relative intensities of major ions in the reference
spectrum (ions greater than 10% of the most abundant
ion) should be present in the sample spectrum.

6.2.2.2	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.)

6.2.2.3	Molecular ions present in reference spectrum should
be present in sample spectrum.

6.2.2.4	Ions present in the sample spectrum but not in the
reference spectrum should be reviewed for possible
background contamination or presence of co-eluting
compounds.

6.2.2.5	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 or coeluting compounds.
NOTE: Data system library reduction programs can
sometimes create these discrepancies.

6.2.3 If in the technical judgement of the mass interpretation

spectral specialist, no valid tentative Identification can be
made, the compound should be reported as unknown. The mass
spectral specialist should give additional classification of
the unknown compound, if possible (i.e., unknown phthalate,
unknown hydrocarbon, unknown acid type, unknown chlorinated
compound). If probable molecular weights can be distinguished,
include them.

Quantitation

TCL 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 (see Exhibit E, Tables 2.1
and 2.2). The EICP area of characteristic ions of analytes listed in
Tables 4, 5 and 6 are used.

Internal standard responses and retention times in all samples must be
evaluated during or immediately after data acquisition. If the
retention time for any internal standard changes by more than 30
seconds from the latest daily (12 hour) calibration standard, the
chromatographic system must be inspected for malfunctions, and

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corrections	as required. The extracted ion current profile (E1CP)

of the internal standards must be monitored and evaluated for each
sample, blank, matrix spike and matrix spike duplicate. The criteria
are described in detail in the instructions for Form VIII, Internal
Standard Area Summary. If the EICP area for any internal standard
changes by more than a factor of two (-50% to +100%), the mass
spectrometric system must be inspected for malfunction and corrections
made as appropriate. If the analysis of a subsequent sample or
standard indicates that the system is functioning properly, then
corrections may not be required. The samples or standards with EICP
areas outside the limits must be re-analyzed, and treated according to
7.1.1 and 7.1.2 below. If corrections are made, then the laboratory
must demonstrate that the mass spectrometric system is functioning
properly. This must be accomplished by the analysis of a standard or
sample that does meet the EICP criteria. After corrections are made,
the re-analysis of samples analyzed while the system was malfunctioning
is required.

7.1.1	If after re-analysis, the EICP areas for all internal standards
are inside the contract limits (>50% to +100%), then the
problem with the first analysis is considered to have been
within the control of the laboratory. Therefore, only submit
data from the analysis with EICPs within the contract limits.
This is considered the initial analysis and must be reported as
such on all data deliverables.

7.1.2	If the r,0-analysis of the sample does not solve the problem,
i.e., the EICP areas are outside the contract limits for both
analyses, then submit the EICP data and sample data from both
analyses. Distinguish between the initial analysis and the
re-analysis on all data deliverables, using the sample suffixes
specified in Exhibit B. Document in the Case Narrative all
inspection and corrective actions taken.

7.2 The relative response factor (RRF) 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 relative
response factor is calculated using the secondary ion. When TCL
Compounds are below contract required quantitation limits (CRQL) but
the spectra meets the identification criteria, report the concentration
with a "J." For example, if CRQL is 10 ug/L and concentration of 3 ug/L
is calculated, report as "3J."

7.2.1 Calculate the concentration in the sample using the relative
response factor (RRF) as determined in paragraph 4.3 and the
- following equation:

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Water

(V(i8)(vt)

Concentration ug/L - (Ais) (RRF) (VQ) (V^)

- Area of the characteristic ion for the compound to be
measured

Ai# - Area of the characteristic ion for the internal standard
Is - Amount of internal standard injected in nanograms (ng)
VQ - Volume of water extracted in milliliters (mL)
V^ - Volume of extract injected (uL)

Vt - Volume of total extract

(Use 2000 uL or a factor of this when dilutions are made. The
2,000 uL is derived from combining half of the 1 mL BN extract
and half of the 1 mL A extract.)

S9ll/S»4iirant

Concentration ug/kg
(Dry weight basis)

Where:

(V^sXV

(A1,)(RRF)(Vi)(Ws)(D)

Ax,I8,A£>	- Same as given for water, above

Vt	- Volume of low level total extract (Use 1000

uL or a factor of this when dilutions are
made. If GPC cleanup is used, the volume is
2,000 uL. The 1000 uL is derived from
concentrating the 9.5 mL extract to 0.95
mL.)

- OR -

Vt	- Volume of medium level extract (Use 2,000 uL

or a factor of this when dilutions are made.
The 2,000 uL is derived from concentrating 5
mL of the 10 mL extract to 1 mL.)

V£	- Volume of extract injected (uL)

D	- 100 - » moisture

100

Vs	- Weight of sample extracted (grams)

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An estimated concentration for non-TCL components tentatively
identified shall be quantified by the internal standard method. For
quantification, the nearest internal standard free of interferences
shall be vised.

7 3 1 The formula for calculating concentrations is the same as in

paragraph 7.2.1. 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 relative response
factor (RRF) of one (1) 1® 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.

Calculate surrogate standard recovery on all samples, blanks and
spikes. Determine if recovery is within limits and report on
appropriate form.

7.4.1	If recovery is not within limits (i.e., if two surrogates from
either base/neutral or acid fractions are out of limits fit if
recovery of any one surrogate in either fraction is below 10%),
the following is required.

o Check to be sure there are no errors in calculations,
surrogate solutions and internal standards. Also, check
instrument performance.

o Reanalyze the sample if none of the above reveal a problem.

7.4.2	If the reanalysis of the sample solves the problem, then the
problem was within the laboratory's control. Therefore, only
submit data from the analysis with surrogate spike recoveries
within the contract windows. This shall be considered the
Initial analysis and shall be reported as such on all data
deliverables.

7.4.3	If none of the steps in 7.4.1 or 7.4.2 solve the problem, then
reextract and reanalyze the sample. If the reextraction and
reanalysis of the sample solves the problem, then the problem
was within the laboratory's control. Therefore, only submit
data from the analysis with surrogate spike recoveries within
the contract windows. This shall be considered the initial
analysis and shall be reported as such on all data
deliverables.

7.4.4	If the reextraction and reanalysis of the sample does not solve
the problem, i.e., the surrogate recoveries are outside the
contract limits for both analyses, then submit the surrogate
spike recovery data and the sample analysis data from analysis
of both sample extracts. Distinguish between the initial
analysis and the reanalysis on all data deliverables, using the
sample suffixes specified in Exhibit B.

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7.4.5

If the sample with »nr»

the sample used for the°m«*e< recoverl-es outside the limits is
«nd the surrogate recoveriel J*"!?* matrix sPike duplicate
spike duplicate show „	®atrix spike and matrix

duplicate do nfl£ require're-analysis matrlX 8plke

Document in the narrative th« .{.n .

recoveries.	similarity in surrogate

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Table 4.

Characteristic Ions for Semivolatile TCL Compounds

Parameter

Primacy I
-------
parameter

Tabl« 4. (continued)

Characteristic Ions for Seaivolatile TCL Compounds

2-Nitroaniline
Dimethyl Fhthalate
Acenaphthylene

3-Nitroaniline
Acenaphthene

2,4-Dinitrophenol

4-Nitrophenol
Dibenzofuran

2,4-Dinitrotoluene

2,6-Dinitrotoluene

Diethylphthalate

4-Chloropheny1-phenylether

Fluorene

4-Nitroaniline

4,6-Dini tro-2 - Me thylpheno1

N-Nitrosodiphenylaoine

4-Bromophenyl-phenylether

Hexachlorobenzene

Pentach1oropheno1

phenanthrene

Anthracene

Di-N-Butylphthalate

Fluor anthene

Pyrene

Butylbenzylphthalate

3,3'-Dichlorobenzidine

Benzo(a)Anthracene

bis(2-Ethylhexy1)Fhthalate

Chrysene

Di-N-Octyl Fhthalate
Benzo (b ) Fluor anthene
Benzo (k) Fluor anthene
Benzo(a)Pyrene
Indeno(1,2,3-cd)Pyrene
Dibenz(a, h)Anthracene
Benzo(g, h, i)Perylene

imarv ion



65

92, 138

163

194, 164

152

151, 153

138

108, 92

153

152, 154

184

63, 154

109

139, 65

168

139

165

63, 182

165

89, 121

149

177, 150

204

206, 141

166

165, 167

138

92, 108

198

182, 77

169

168, 167

248

250, 141

284

142, 249

266

264, 268

178

179, 176

178

179, 176

149

150, 104

202

101, ioo

202

101, ioo

149

91, 206

252

254, 126

228

229, 226

149

167, 279

228

226, 229

149

•

252

253, 125

252

253, 125

252

253, 125

276

138, 227

278

139, 279

27fr

138, 277

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Table 5.

Characteristic Ions for Pesticides/PCBs
Parameter	Primary Ion	Secondary TftnfftX

Alpha-BHC

183

181, 109

Beta-BHC

181

183, 109

Delta-BHC

183

181, 109

Gamma-BHC (Lindane)

183

181, 109

Heptachlor

100

272, 274

Aldrin

66

263, 220

Heptachlor Epoxide

353

355, 351

Endosulfan I

195

339, 341

Dieldrin

79

263, 279

4,4'-DDE

246

248, 176

Endrin

263

82, 81

Endosulfan II

337

339, 341

4,4'-DDD

235

237, 165

Endosulfan Sulfate

272

387, 422

4,4'-DDT

235

237, 165

Methoxychlor

227

228

Chlordane (alpha and/or gamma)

373

375, 377

Toxaphene

159

231, 233

Aroclor-1016

222

260, 292

Aroclor-1221

190

222, 260

Aroclor-1232

190

222, 260

Aroclor-1242

222

256, 292

Aroclor-1248

292

362, 326

Aroclor-1254

292

362, 326

Aroclor-1260

360

362, 394

Endrin Ketone

317

67, 319

D-44/SV

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Table 6.

Characteristic Ions for Surrogates and
Internal Standards for Semivolatile Compounds

SURROGATES	tVlmVr Ion	PffMldflTY Jpnfg)

Phenol-d5	99	42, 71

2-Fluorophenol	112	64

2,4,6-Tribronophenol	330	332, 141

d-5 Nitrobenzene	82	128, 54

2-Fluorobipheny1	172	171

Terphenyl	244	122, 212

INTERNAL STANDARDS

1,4-Dichlorobenzene-d^	152	115

Naphthalene-dg	136	68

Acenapthene-djn	164	162, 160

Fhenanthrene-d^g	138	94, 80

Chrysene-d12	240	120, 236

Perylene-d12	264	260, 265

D-45/SV

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exhibit D
analytical methods

FOR PESTICIDES/PCBs

D-l/PEST

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at Contmti

Page

SECTION I INTRODUCTION	D-3/PEST

SECTION II SAMPLE PREPARATION AND STORAGE	D-5/PEST

PART A SAMPLE STORAGE AND MOLDING TIMES 	 D-6/PEST

PART B SAMPLE PREPARATION FOR PESTICIDES/PCBa

IN HATER 	 D-7/PEST

PART C PROTOCOLS FOR SOIL/SEDIMENT	D-14/PEST

1.	Madiua Laval Praparation for Analyais

of Paatlclda/PCBa	D-14/PEST

2.	Low Laval Praparation for Analysis

of Paatlclda/TCBa	D-19/PEST

SECTION III SCREENING OF PESTICIDE/PCB EXTRACTS	D-31/PEST

SECTION IV GC/EC ANALYSIS OF PESTICIDES/PCBa	D-33/PEST

D-2/PEST

7	2/88
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SECTION I

INTRODUCTION

analytical aethods that follow are designed Co analyse water, soil and
sediaent from hazardous waate alcaa for Cha organic compounds on the Target
CoapoundLlat (TCL) (Sac Exhibit C). The aethoda are baaed on EPA Method 608
(Peatlcldea and PCBa).

The aethoda are divided Into the following .actions: saaple preparation,
screening and analysis. Saiipla preparation covers sanple extraction and
cleanup techniques. As described in the screening section, a portion of the
extracts aey be screened on a gaa chroaatograph with appropriate detector to
determine the concentration level of pesticides/PCBs. The analyaia aection
contains the gas chroaatograph/electron capture detector (GC/BC) aethod for
pesticides and PCBs.

D-3/PEST

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1. Method for tha Dafniilnatlon of Pesticides

1.1	Scope and Application

This method covers tha determination of cartain TCL organochloride
pestlcidea and polychlorlnatad biphanyla aa llatad In Exhibit C. Tha
contract required quantitation liiiti are also listed In Exhibit C.
Because weathering and/or diffarent foraulatlons of chlordane usually
modify the chromatographic pattern exhibited by technical chlordane,
the use of this method is not appropriate for the determination of
technical chlordane.

The analyaia of the isomers alpha chlordane and gaama chlordane by this
method ifl, appropriate however.

1.2	The method involves aolvent extraction of the matrix, analyaia of the
extract on a gas chromatograph/electron capture detector (GC/EC) using
a packed column, or wide bore capillary column; and confirmation on a
GC/EC uaing either a aecond packed column, or wide bore capillary
column, or narrow bore capillary column. If concentration permita,
confirmation is to be done on GC/MS.

D-4/PEST

Rev. 5/89
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SECTION II
SAMPLE PREPARATION AND STORAGE

D-5/PEST

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PART A - SAMPLE STORAGE AWD HOLDING TIMES

1.	Procedure* for Sample Storage

1.1	The samples oust be protected from light and refrigerated at 4*C (+
2*C) from the tine of receipt until extraction and analysis.

1.2	After analysis, extracts and unused sample volume oust be protected
from light and refrigerated at 4* C (± 2* C) for the periods specified
in the contract schedule.

2.	Remiired Holding Tines

2.1	If separatory funnel or sonication procedures are employed for
extractions for pesticide/ FCB analyses, extraction of water samples
shall be completed within 5 days of VTSR (Validated Time of Sample
Receipt), and extraction of soil/ sediment samples shall be completed
within 10 days of VTSR. If continuous liquid-liquid extraction
procedures are employed, extraction of water samples shall be started
within 5 days of VTSR.

2.2	Extracts of either water or soil/sediment samples must be analyzed
within 40 days following extraction.

D-6/PEST

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PART B - SAMPLE PREPARATION TOR PESTICIDES /PrWg IN WATER

1.	»f Method

A measured volume of sample, approximately one-liter, is solvent
extracted with methylene chloride using a separatory funnel or a
continuous extractor. The methylene chloride extract is dried,
exchanged to hexane and adjusted to a final volume of 10 mL.

2.	Intirfortnctg

2.1	Method interferences may be caused by contaminants in solvents,
reagents, glassware, and other sample processing hardware that lead to
discrete artifacts and/or elevated baselines in gas chromatograms. All
of these materials must be routinely demonstrated to be free from
Interferences under the conditions of the analysis by running
laboratory reagent blanks. Interferences by phthalate esters can pose
a major problem in pesticide analysis when using the electron capture
detector. These compounds generally appear in the chromatogram as broad
elutlng peaks. Common flexible plastics contain varying amounts of
phthalates. These phthalates are easily extracted or leached from such
materials during laboratory operations. Cross-contamination of clean
glassware routinely occurs when plastics are handled. Interferences
from phthalates can best be minimized by avoiding the use of plastics
in the laboratory. Exhaustive cleanup of reagents and glassware may be
required to eliminate background phthalate contamination.

2.2	Matrix interferences may be caused by contaminants that are coextracted
from the sample. The extent of matrix interferences will vary
considerably from source to source, depending upon the nature and
diversity of the site being sampled. The cleanup procedures In
paragraphs 7.1 thru 7.5 must be used to overcome such Interferences to
attempt to achieve the CRQLs. The cleanup procedures in paragraph 8.1
through 8.5 may be used to remove sulfur interferences.

3.	Apparatus and Materials

3.1 Glassware (Brand names and catalog numbers included for illustration
purposes only).

3.1.1	Separatory funnel - 2000 mL with Teflon stopcock.

3.1.2	Drying column • Chromatographic column approximately 400 mm
long x 19 on ID, with coarse frit. (Substitution of a small
pad of disposable Pyrex glass wool for the frit will help
prevent cross-contamination of sample extracts.)

3.1.3	Concentrator tube - Kuderna-Danish, 10 mL, graduated (Kontes
K-570050-1025 or equivalent). Calibration must be checked at
the volumes employed in the test. Ground glass stopper is used
to prevent evaporation of extracts.

3.1.4	Evaporative flask - Kuderna-Danish, 500 mL (Kontes K-570001-
0500 or equivalent). Attach to concentrator tube with springs.

D-7/MST

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3.1.5	Snyder coition - Kuderna-Danish, Three-ball macro (Kontes
K-503000-0121 or equivalent).

3.1.6	Snyder colunn - Kude ma-Danish, Two-ball micro {Kontes
K-569001-0219 or equivalent).

3.1.7	Continuous liquid-liquid extractors - Equipped with Teflon or
glees connecting joints end stopcocks requiring no lubrication.
(Hershberg-Wolf Extractor-Ace Glass Company, Vineland, NJ P/N
6841-10, or equivalent.)

3.1.8	Vials - Amber glass, 10 to 15 mL capacity, with Teflon-lined
screw cap.

3.1.9	Bottle or test tube - 50 mL with Teflon-lined screw cap for
sulfur removal.

3.1.10	Chromatographic column for alumina - 8 mL (200 mm X 8 mm ID)
Polypropylene column (Kontes K-420160 or equivalent) or 6 mL
(150 mm x 8 mm ID) glass column (Kontes K-420155 or equivalent)
or 5 mL serological pipettes plugged with a small piece of
Pyrex glass wool in the tip. The Kontes columns may be plugged
with Pyrex glass wool or a polyethylene porous disk (Kontes
K-420162).

3.2	Pyrex glass wool - Pre-rinse glass wool with appropriate solvents to
ensure its cleanliness.

3.3	Silicon carbide boiling chips - Approximately 10/40 mesh. Heat to
400*C for 30 minutes or Soxhlet extrect with methylene chloride.

3.4	Vater bath - Heated, with concentric ring cover, capable of temperature
control (± 2*C). The bath should be used in a hood.

3.5	Balance - Analytical, capable of accurately weighing ± 0.0001 g.

3.6	Nitrogen evaporation device equipped with a water bath that can be
maintained at 35-40*C. The N-Evap by Organomatlon Associates, Inc.
South Berlin, MA (or equivalent) is suitable.

4. Reaaanta

4.1	Reagent water - Reagent water is defined as a water in which an
interferent is not observed at or above the CRQL of each parameter of
interest.

4.2	Acetone, hexsne, isooctane (2,2,4-trimethylpentane), methylene chloride
Pesticide quality or equivalent.

4.3	Sodium sulfate"- (ACS) granular, anhydrous. Purify by heating at 400*C
for 4 hours in a shallow tray.

4.4	Alumina - Neutral, Super I Voelm (Universal Scientific, Incorporated,
Atlanta, Georgia) or equivalent. Prepare activity III by adding 7%

D-8/PEST

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(v/w) reagent water to the Super I neutral alumina. Tumble or shake in
a wrist action shaker for a minimum of 2 hours or preferably overnight.
There should be no lumps present. Store in a tightly sealed glass
container. A 25 cycle soxhlet extraction of the alumina with methylene
chloride is required if a solvent blank analyzed by the pesticide
technique indicates any interferences for the compounds of interest.

4.4.1 Alumina Equivalency Check. Test the alumina by adding the BNA
surrogates (see Exhibit D SV) in 1:1 acetone/hexane to the
alumina and following paragraph 7.1. The tribromophenol should
not be detected by CC/EC if the alumina and its activation are
acceptable. Also check recovery of all single component
pesticides following the same procedure. The percent recovery
for all single component pesticides must be ^80%, except for
endosulfan sulfate which must be ^60% and endrin aldehyde which
is not recovered. The data must be retained by the laboratory
and made available for inspection during on-site evaluations.
If the alumina deactivated with 7% (v/w) reagent water does not
prove adequate to remove the BNA surrogates and other
Interferences, the alumina may be deactivated with as much as
9% reagent water, so long as the criteria for tribromophenol
and the recovery of all single component pesticides can be met.

4.5	Sodium hydroxide solution (ION)-(ACS). Dissolve 40 g NaOH in reagent
water and dilute to 100 mL.

4.6	Tetrabutylanmoniuar (TBA) - Sulfite reagent. Dissolve 3.39 g
tetrabutylammonlum hydrogen sulfate in 100 mL distilled water. To
remove Impurities, extract this solution three times with 20 mL
portions of hexane. Discard the hexane extracts, and add 25 g sodium
sulfite to the water solution. Store the resulting solution, which is
saturated with sodium sulfite, in an amber bottle with a Teflon-lined
screw cap. This solution can be stored at room temperature for at
least one month.

4.7	Pesticide surrogate standard spiking solution.

4.7.1	The surrogate standard is added to all samples and calibration
solutions; the compound specified for this purpose is
dlbutylchlorendate.

4.7.2	Prepare a surrogate standard spiking solution at a
concentration of 1 ug/1.00 mL in acetone. Store the spiking
solutions at 4*C (± 2*C) in Teflon-sealed containers. The
solutions should be checked frequently for stability. These
solutions oust be replaced after twelve months, or sooner, if
comparison with quality control check samples indicates a
problem.

4.8	Sulfuric acid solution (1+1)-(ACS). Slowly, add 50 mL H2SO4 (sp. gr.
1.84) to 50 mL of reagent water.

D-9/PEST

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4.9 Pesticide matrix standard spiking solution. Prepare a spiking solution
of aceton* or methanol that contains the following pesticides in the

Matrix spikes are also to serve as duplicates by spiking two 1-liter
portions from the one sample chosen for spiking.

4.10 See Exhibit A for a susnary of the quality control requirements of this
contract. See Exhibit E for contract-required quality
assurance/quality control procedures.

5.	Extraction - Separatory Funnel

5.1	Samplea may be extracted using separatory funnel techniques. If
emulsions prevent acceptable solvent recovery with separatory funnel
extractions, continuous liquid-liquid extraction (paragraph 6.1) may be
used. The separatory funnel extraction scheme described below assumes
a sample volume of one liter.

5.2	Using a 1-liter graduated cylinder, measure out a 1-liter sample
aliquot and place it into a 2-liter separatory funnel. Check the pH of
the sample with wide range pH paper and adjust to between 5 and 9 pH
with 10 N sodium hydroxide and/or 1:1 sulfuric acid solution. (NOTE:
Recovery of dibutylchlorendate will be low if pH is oucside this range.
Alpha-BHC, gama-BHC, Endosulfan I and II and Endrin are subject to
decomposition under alkaline conditions and therefore may not be
detected if the pH is above 9.) Pipet 1.0 mL surrogate standard
spiking solution into the separatory funnel and mix well. Add 1.0 mL
of pesticide matrix spiking solution to each of two 1-liter portions
from the sample selected for spiking.

5.3	Add 60 mL methylene chloride to the separatory funnel and extract the
sample by shaking the funnel for two minutes, with periodic venting to
»!•••• axcess pressure. Allow the organic layer to separate from the
water phase for a minimum of 10 minutes. If the emulsion interface
between layers is more than one-third the volume of the solvent layer,
th* analyst must employ mechanical techniques to complete the phase
separation. The optimum technique depends upon the sample, and may
include: stirring, filtration of the emulsion through glass wool,
centrifugation or other physical means. Drain methylene chloride into
a 250 mL Erlenmeyer flask.

5.4	Add a second 60 mL volume of methylene chloride to the sample bottle
and repeat the extraction procedure a second time, combining the
•'tracts in the Erlenmeyer flask. Perform a third extraction in the
same manner.

concentrations specified

Pcitlcldo

Lindane

Heptachlor

Aldrin

Dieldrln

Endrin

4,4' DDT

uy/1.0 mL

0.2
0.2
0.2
0.5
0.5
0.5

D-10/PEST

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5.5	Assemble a Kuderna-Danish (K-D) concentrator by attaching a 10-mL
concentrator tuba to a 500-mL evaporative flask. Other concentration
devices or techniques may be used in place of the K-D if equivalency is
demonstrated for all pesticides listed in Exhibit C.

5.6	Pour the combined extract through a drying column containing about 10
cm of anhydrous granular sodium sulfate, and collect the extract in the
K-D concentrator. Rinse the Erlenmeyer flask and column with 20 to 30
mL of methylene chloride to complete the quantitative transfer.

5.7	Add one or two clean boiling chips to the evaporative flask and attach
a three-ball Snyder column. Pre-vet the Snyder column by adding about
1 mL methylene chloride to the top. Place the K-D apparatus on a hot
water bath (80 to 90*C) so that the concentrator tube is partially
Immersed in the hot water and the entire lower rounded surface of the
flask is bathed with hot vapor. Adjust the vertical position of the
apparatus and the water temperature as required to complete the
concentration in 10 to 15 minutes. At the proper rate of distillation,
the balls of the column will actively chatter but the chambers will not
flood with condensed solvent. Vhen the apparent volume of liquid
reaches 1 mL, remove the K-D apparatus. Allow it to drain and cool for
at least 10 minutes.

5.8	Momentarily remove the Snyder column, add 50 mL of hexane and a new
boiling chip and re-attach the Snyder column. Pre-wet the column by
adding about 1 mL of hexane to the top. Concentrate the solvent
extract as before. The elapsed time of concentration should be 5 to 10
minutes. Vhen the apparent volume of liquid reaches 1 mL, remove the
K-D apparatus and allow it to drain and cool at least 10 minutes.

5.9	Remove the Snyder column, rinse the flask and its lower joint into the
concentrator tube with 1 to 2 mL of hexane. If sulfur crystals are a
problem, proceed to paragraph 8.1; otherwise continua to paragraph
5.10.

5.10	Nitrogen blowdown technique (taken from ASTM Method D 3086)

Place the concentrator tube in a warm water bath (35*C) and evaporate
the solvent volume to 0.5 mL using a gentle stream of clean, dry
nitrogen (filtered through a column of activated carbon). Caution:
New plastic tubing must not be used between the carbon trap and the
sample, as it may Introduce interferences. The Internal wall of the
tube must be rinsed down several times with hexane during the operation
and the final volume brought to 0.5 mL. During evaporation, the tube
solvent level must be kept below the water level of the bath. The
•xtract must never be allowed to become dry.

5.11	Dilute the extract to 1 mL with acetone and proceed to 7.1 (Alumina
Column Cleanup).

6. Sample Extraction - Continuous Llould-Llould Extractor

6.1 Vhen experience with a sample from a given source Indicates that a

serious emulsion problem will result, or if an emulsion is encountered

D-11/PEST

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in paragraph 5.3 using a scparatory funnal, a continuous extractor
should be used.

6.2	Using a 1-liter graduated cylinder, measure out a 1-liter sample
aliquot and place it into the continuous extractor. Pipet 1.0 mL
surrogate standard spiking solution into the continuous extractor and
mix veil. Check the pH of the sample with wide range pH paper and
adjust to between 5 and 9 pH with ION sodium hydroxide and/or 1:1
sulfuric acid solution.

6.3	Add 500 mL of methylene chloride to the distilling flask. Add
sufficient reagent water to ensure proper operation and extract for 18
hours. Allow to cool, then detach the boiling flask and dry.

Concentrate the extract as in paragraphs 5.5 through 5.11.

7.	AIuhIm Column Cleanup

7.1	Add 3 g of activity III neutral alumina to the 10-mL chromatographic
column. Tap the column to settle the alumina. Do not pre-wet the
alumina.

7.2	Transfer the 1 mL of hexane/acetone extract from paragraph 5.11 to the
top of the alumina using a disposable Pasteur pipet. Collect the
eluate in a clean 10-mL concentrator tube.

7.3	Add 1 mL of hexane to the original extract concentrator tube to rinse
it. Transfer these rinsings to the alumina column. Elute the column
with an additional 9 mL of hexane. Do not allow the column to go dry
during the addition and elution of the sample.

7.4	Adjust the extract to a final volume of 10 mL using hexane.

7.5	The pesticide/PCB fraction is ready for analysis. Proceed to Section
IV, paragraph 3. Store the extracts at 4*C (±2*C) in the dark in
Teflon-sealed containers until analyses are performed.

8.	Optional Sulfur

8.1	Concentrate the hexane extract from paragraph 5.9 to 1 mL.

8.2	Transfer the 1 mL to a 50 mL clear glass bottle or vial with a
Teflon-lined screw cap. Rinse the concentrator tube with 1 mL of
hexane, adding the rinsings to the 50 mL bottle,

8.3	Add 1 mL TSA-sulfite reagent and 2 mL 2-propanol, cap the bottle, and
shake for at least 1 min. If the sample is colorless or if the initial
color is unchanged, and if clear crystals (precipitated sodium sulfite)
are observed, sufficient sodium sulfite is present. If the
precipitated sodium sulfite disappears, add more crystalline sodium

D-12/PEST

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sulfite in approximately 100 mg portions until a solid residue remains
after repeated shaking.

8.4 Add 5 mL distilled water and shake for at least 1 minute. Allow the
sample to stand 5-10 minutes. Transfer the hexane layer (top) to a
concentrator ampule and go back to paragraph 5.10.

D-13/PEST

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PART C - fPOTOCOLS FOP SOTT./SEDIMENT

It Is mandatory that all soil/sedlment samples be characterized as to
concentration laval so that the appropriate analytical protocol nay be chosen
to ensure proper quantitation limits for the sample.

The use of GC/EC methods is recommended for screening soil/sediment samples
for pesticides/PCBs, however, the Contractor is at liberty to determine the
specific method of characterization.

Note that the terms "low level" and "medium level" are not used here as a
Judgement of degree of contamination but rather as a description of the
concentration ranges that are encompassed by the "low" and "medium" level
procedures.

The concentration range covered by the low level analysis may be considered
to be less than 1000 ug/kg of pesticides/PCBs. The concentration range
covered by the medium level analysis is greater than 1000 ug/kg.

1.	Level Preparation for Analysis of Pesticides/PCBs In

fiftfT/Wi-ent

1.1 Scope and Application

This procedure is designed for the preparation of sediment/soil samples

which may contain pesticides/PCBs at a level greater than 1,000 ug/kg.

1.1.1	Samples to be prepared and analyzed by this method should have
been screened by GC/EC techniques. The results of those
screens will determine whether sufficient quantities of
pesticides/PCBs are present to warrant analysis by the medium
level protocol.

1.1.2	If the screenings indicate no detectable pollutants at a level
of quantitation of 1000 ug/kg, the sample should be prepared by
the low level protocol in this Section.

1.1.3	If the extract for pesticide/PCB analysis is to be prepared
from an aliquot of the semlvolatlle extract, also refer to the
specific Instructions in Exhibit D SV.

1.2 Summary of Method

1.2.1	Portions of soll/sedlment are extracted and screened by methods
of the Contractor's choice.

1.2.2	If pestlcldes/PCBs are detected in the screen at levels above
approximately 1000 ug/kg• • 1 g sample is extracted with 10.0
mL of hexane for analysis by GC/EC.

1.2.3	If no pesticides/PCBs are detected above 1000 ug/kg, then the
sample shall be prepared by the low level protocol.

D-14/PEST

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1.3 Interferences

1.3.1 Method intirftctnesi may be caused by contaminants In solvents,
reagents, glassware and other sample processing hardware that
lead to discrete artifacts and/or elevated baselines in the
total ion current profiles. All of these materials must be
routinely demonstrated to be free from interferences under the
conditions of the analysis by running laboratory reagent
blanks. Matrix interferences may be caused by contaminants tna
are coextracted from the sample. The extent of matrix
interferences will vary considerably from source to source.

1.4	Limitations

1.4.1 The procedure is designed to allow quantitation limits as low
as 1000 ug/fcg f©* p«sticides/PCBs. If peaks are present base
on GC screen, the sample is determined to require a medium
level analysis by GC/EC. Some samples may contain high
concentrations of chemicals that interfere with the analysis o
other components at lower levels; the quantitation lialt* in
those cases may be significantly higher.

1.5	Reagents

1.5.1	Sodium Sulfate - anhydrous powdered reagent grade, heated at
400*C for four hours, cooled in a desiccator and stored in a
glass bottle Baker anhydrous powder, catalog # 73898 or
equivalent.

1.5.2	Methylene chloride. Pesticide residue analysis grade or
equivalent.

1.5.3	Hexane. Pesticide residue analysis grade or equivalent.

1.5.4	Methanol. Pesticide residue analysis grade or equivalent.

1.5.5	Acetone. Pesticide residue analysis grade or equivalent.

1.5.6	Pestlcide/PCB Surrogate Standard Spiking solution.

1.5.6.1 The compound specified is dibutylchlorendate.

Prepare a solution at a concentration of 20 ug/l.o
mL in methanol. Store the spiking solutions at 4
(±2*C) in Teflon-sealed containers. The solutions
should be checked frequently for stability. These
solutions must be replaced after twelve months, or
sooner, if comparison with quality control check
samples indicates a problem.

1.5.7	Pestlcide/PCB Matrix Standard Spiking solution

1.5.7.1 Prepare a spiking solution in methanol that contains
the following pesticides in the concentrations
•peclflad below. Store the spiking solutions at 4 C

D-15/PEST

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(±2*C) in Teflon-sealed container!. Tht solution*
should be checked frequently for stability. These
solutions aust be replaced after twelve months, or
sooner, if comparison with quality control check
saaples indicates a problea.

Pesticide	Ut/l.OllL

lindane	2.0

heptachlor	2.0

aldrin	2.0

dieldrin	5.0

endrin	5.0

4,4' DDT	5.0

1.5.8 Alumina - neutral, super I Voela (Universal Scientific,

Atlanta, GA) or equivalent. Prepare activity III by adding 7%
(v/w) reagent water to the Super I neutral aluaina. Tuable or
shake on a wrist action shaker for a ainlaua of 2 hours or
preferably overnight. There should be no lunps present. Store
in a tightly sealed glass container. A 25 cycle soxhlet
extraction of the aluaina with methylene chloride is required
if a solvent blank analyzed by the pesticide techniques
indicates any interferences for the coapounds of Interest.

1.5.8.1 Aluaina Equivalency Check. Test the aluaina by

adding the BNA surrogates (see Exhibit D SV) in 1:1
ace tone/hexane to the aluaina and following
paragraph 2.8.1. The tri-bromophenol should not be
detected by GC/EC if the aluaina and its activation
are acceptable. Also check recovery of all single
coaponent pesticides following the saae procedure.
The percent recovery for all single coaponent
pesticides aust be £80%, except for endosulfan
sulfate which aust be £60% and endrin aldehyde which
is not recovered. The data aust be retained by the
laboratory and aade available for inspection during
on-site evaluations. If the aluaina deactivated
with 7% (v/w) reagent water does not prove adequate
to reaove the BNA surrogates and other
interferences, the aluaina aay be deactivated with
as auch as 9« reagent water, so long as the criteria
for trlbroaophenol and the recovery of all single
coaponent pesticides can be aet.

1.5.9 Reagent Vater - Reagent water Is defined as water in which an
lnterferent Is not observed at or above the CRQL of each
parameter of interest.

1.6 Equipment

1.6.1	Glass scintillation vials, at least 20 aL, with screw cap and
teflon or aluainua foil liner.

1.6.2	Spatula. Stainless steel or Teflon.

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1.6.3	Balance capable of weighing 100 g to Che nearest 0.01 g.

1.6.4	Vials and caps, 2 mL for GC auto sampler.

1.6.5	Disposable pipettes, Pasteur; glass wool rinsed with methylene
chloride.

1.6.6	15-mL concentrator tubes.

1.6.7	Ultrasonic cell disruptor, Heat Systems•Ultrasonics, Inc.,
Model tf-385 SONIGATOR (475 Watt with pulsing capability. No.
200 1/2 inch tapped disruptor horn, and No. 419 1/8 inch
standard tapered M1CR0TIP probe), or equivalent device with a
minimum of 375 Watt output capability. NOTE: In order to
ensure that sufficient energy is transferred to the sample
during extraction, the MICROTIP probe must be replaced if the
tip begins to erode. Erosion of the tip is evidenced by a
rough surface.

1.6.8	Sonabox acoustic enclosure - recommended with above disruptors
for decreasing cavitation sound.

1.6.9	Test tube rack.

Oven, drying.

Desiccator.

Crucibles, porcelain.

Chromatography column for alumina. 8 mL (200 mm & 8 mm ID)
Polypropylene column (Kontes K-420160 or equivalent) or 6 mL
(150 mm X 8 am ID) glass column (Kontes K-420155 or equivalent)
or 5 mL serological pipettes plugged with a small piece of
Pyrex glass wool in the tip. (Pyrex glass wool shall be
pre-rinsed with appropriate solvents to insure its
cleanliness). The Kontes columns may be plugged with Pyrex
glass wool or a polyethylene porous disk (Kontes K-420162).

Sample Preparation

1.7.1 Medium Level preparation for analysis of Pesticide/PCBs
(Determine results of GC/EC screen before proceeding.)

1.7.1.1 Transfer the sample container into a fume hood.

Open the sample vial and mix the sample. Transfer
approximately 1 g (record weight to nearest 0.1 g)
of saaq>le to a 20 mL vial, tfipe the mouth of the
vial with a tissue to remove any sample material.
Record the exact weight of the sample taken. Cap
the vial before proceeding with the next sample to
avoid any cross contamination.

1.6.10

1.6.11

1.6.12

1.6.13

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1.7.1.1.1 Transfer 50 g of soil/sediment to 100

mL beaker. Add 50 mL of water and stir
for 1 hour. Determine pH of sample
with glass electrode and pH meter while
stirring. Report pH value on
appropriate data sheets. If the pH of
the soil is greater than 11 or less
than 5, contact the Deputy Project
Officer cited in the contract for
Instructions on how to handle the
sample. Document the instructions in
the Case Narrative. Discard this
portion of sample. NOTE: Recovery of
dibutylchlorendate will be low if pH is
outside this range.

1.7.1.2	Add at least 2 g of anhydrous powdered sodium
sulfate to the sample and mix well.

1.7.1.3	Surrogate standards are added to all samples, spikes
and blanks. Add 50 uL of surrogate spiking solution
to the sample mixture.

1.7.1.4	Add 1.0 mL of matrix standard spiking solution to
each of two 1 g portions from the sample chosen for
spiking.

1.7.1.5	Ionediately add 10.0 mL (only 9.0 mL for the matrix
spike sample) of hexane to the sample and disrupt
the sample with the 1/8 inch tapered MICROTIP
ultrasonic probe for 1 minute with the V-385 (or 2
minutes with the W-375) with output control setting
at 5 and mode switch on "1 sec. pulse" and % duty
cycle set at 50%. (If using a sonicator other than
Models W-375 or V-385, contact the Project Officer
for appropriate output settings.) Before
extraction, make certain that the sodium sulfate is
free flowing and not a consolidated mass. As
rsquired, break up large lumps with a clear spatula,
or very carefully with the tip of the unenergized
probe.

1.7.1.6	Loosely pack disposable Pasteur pipettes with 2-3 cm
glass wool plugs. Filter the extract through the
glass wool and collect at approximately 5 mL in a
concentrator tube.

1.7.1.7	Transfer 1.0 mL of the hexane extract to a glass
concentrator tube and concentrate to 0.5 mL using
Nitrogen blowdown. Add 0.5 mL of acetone to 0.5 mL
of hexane extract. Swirl to mix. The pesticide
extract must now be passed through an alumina column
to remove polar interferences.

D-18/PEST

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1.7.1.8 Follow the procedures for low level soil sediment
preparation outlined In paragraphs 2.8.1.1 through
2.8.3.3 for alumina cleanup and sulfur removal.

2. Low Level Preparation for Analysis of Pesticides/PCBs in Snil/S«diim»nt

2.1	Summary of Method

2.1.1 If based on the results of a GC/EC screen, no pestlcldes/PCBs
are present in the sample above 1000 ug/kg, a 30 gram portion
of soil/ sediment is mixed with anhydrous powdered sodium
sulfate and extracted with 1:1 methylene chloride/acetone using
an ultrasonic probe. The extract is concentrated and an
optional gel permeation column cleanup may be used. The
extract is cleaned up using a micro alumina column and analyzed
by GC/EC for pesticides.

2.2	Interferences

2.2.1 Method Interferences may be caused by contaminants in solvents,
reagents, glassware and other sample processing hardware that
lead to discrete artifacts and/or elevated baselines in the
total ion current profiles. All of these materials must be
routinely demonstrated to be free from interferences under the
conditions of the analysis by running laboratory reagent
blanks. Matrix interferences may be caused by contaminants
that are coextracted from the sample. The extent of matrix
interferences will vary considerably from source to source.

2.3 Apparatus and Materials

2.3.1 Apparatus for determining percent moisture

2.3.1.1	Oven, drying.

2.3.1.2	Desiccator.

2.3.1.3 Crucibles, porcelain.

2.3.2	Disposable Pasteur glass pipettes, 1 mL

2.3.3	Ultrasonic cell dlsruptor, Heat Systems • Ultrasonics, Inc.
Model W-385 S0NICAT0R (475 watt with pulsing capability, No.
305 3/4 inch tapped high gain "Q" dlsruptor horn or No. 208 3/4
inch standard solid dlsruptor horn), or equivalent device with
a minimum of 375 watt output capability. NOTE: In order to
ensure that sufficient energy is transferred to the sample
during extraction, the probe must be replaced if the tip begins
to erode. Erosion of the tip is evidenced by a rough surface.

2.3.3.1 Sonabox acoustic enclosure - recommended with above
dlsruptors for decreasing cavitation sound.

2.3.4	Beakers, 400 mL

D-19/PEST

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2.3.5	Vacuus filtration apparatus

2.3.5.1	Buchner funnel.

2.3.5.2	Flltar paper, Vhataan No. 41 or aqulvalant.

2.3.6	Kudarna-Danish (K-D) apparatus.

2.3.6.1	Concentrator tube - 10 aL, graduated (Kontes
K-570040-1025 or equivalent).

2.3.6.2	Evaporative flask - 500 aL (Kontes K-570001-0500 or
equivalent).

2.3.6.3	Snyder coluan - three-ball macro (Kontes
K-503000-0121 or equivalent).

2.3.6.4	Snyder coluan - two-ball aicro (Kontes
K-569001-0219) or equivalent).

2.3.7	Silicon carbide boiling chips - approximately 10/40 aesh. Heat
to 400*C for 30 ainutes or Soxhlet extract with aethylene
chloride.

2.3.8	Water bath - heated, with concentric ring cover, capable of
teaperature control (±2*C). The bath should be used in a hood.

2.3.9	Balance, capable of accurately weighing ±0.01 g.

2.3.10	Vials and caps, 2 aL for GC auto saapler.

2.3.11	Balance - Analytical, capable of accurately weighing ± 0.0001
g-

2.3.12	Nitrogen evaporation device equipped with a water bath that can
be aaintained at 35-40*C. The N-Evap by Organoaation
Associates, Inc. South Berlin, MA (or equivalent) is suitable.

2.3.13	Gel peraeation chroaatography (GPC) cleanup device. NOTE: GPC
cleanup ia highly fifiT**"»ndad for all extracts for low level
soils.

2.3.13.1 Autoaated systea

2.3.13.1.1	Gel peraeation chroaatograph Analytical
Biocheaical Labs, Inc. GPC Autoprep
1002 or equivalent including:

2.3.13.1.2	25 am ID X 600 - 700 m glass coluan
packed with 70 g of Bio-Beads SX-3.

2.3.13.1.3	Syringe, 10 aL with Luer-Lock fitting.

D-20/PEST

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2.3.13.1.4 Syringe filter holder and filters

stainless steel end TFE, Gelman 4310 or
equivalent.

2.3.13.2 Manual systen assembled froa parts. (Vise, R.H.,
Bishop, D.F., Williaae, R.T. & Austern, B.M. "Gel
Peraeation Chromatography in the GC/MS Analysis of
Orgastics In Sludges" U.S. EPA, Municipal
Environmental Research Laboratory - Cincinnati, Ohio
45268.)

2.3.13.2.1	25 on ID X 600 - 700 m heavy wall
glass coluan packed with 70 g of
BIO-Beads SX-3.

2.3.13.2.2	Puap: Altex Scientific, Model No.
1001A, sealpreparative, solvent
aetering systea.

Puap capacity - 28 aL/aln.

2.3.13.2.3	Detector: Altex Scientific, Model No.
153, with 254 na UV source and 8-ul
seal-preparative flowcells (2-aa
pathlengths)

2.3.13.2.4	Microprocessor/controller: Altex
Scientific, Model No. 420,
Microprocessor Systea Controller, with
extended aeaory.

2.3.13.2.5	Injector: Altex Scientific, catalog
No. 201-56, saaple injection valve,
Tefzel, with 10 aL saaple loop.

2.3.13.2.6	Recorder: Linear Instruments, Model
No. 385, 10-inch recorder.

2.3.13.2.7	Effluent Switching Valve: Teflon
slider valve, 3-way with 0.060" ports.

2.3.13.2.8	Suppleaental Pressure Gauge with
connecting Tee: U.S.Gauge, 0-200 psi,
stainless steel. Installed as a

"downstreaa" aonltorlng device between
coluan and detector. Flow rate was
typically 5 aL/ain. of aethylene
chloride. Recorder chart speed was
0.50 ca/ain.

2.3.14 Chromatography coluan for aluaina. 8 aL (200 aa & 8 am ID)
Polypropylene coluan (Kontes K-420160 or equivalent) or 6 aL
(150 aa X 8 aa ID) glass coluan (Kontes K-420155 or equivalent)
or 5 aL serological pipettes plugged with a saw 11 piece of
Pyrex glass wool in the tip. (Pyrex glass wool shall be

D-21/PEST

2/88
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pre-rinsed with appropriate solvents to assure its
cleanliness). The Kontes columns may be plugged with Pyrex
glass wool or a polyethylene porous disk (Kontes K-420162).

2.3.15	Pyrex glass wool.

2.3.16	Bottle or test tube, 50 mL with Teflon-lined screw cap for
sulfur removal.

2.3.17	Pasteur pipettes, disposable.

2.4 Reagents

2.4.1	Sodium Sulfate - anhydrous powdered reagent grade, heated at
400*C for four hours, cooled in a desiccator, and stored in a
glass bottle. Baker anhydrous powder, catalog #73898 or
equivalent.

2.4.2	Methylene chloride, hexane, acetone, isooctane, 2-propanol and
benzene - pesticide quality or equivalent.

2.4.3	Alumina - neutral, super I Woelm (Universal Scientific,

Atlanta, GA) or equivalent. Prepare activity III by adding 7%
(v/w) reagent water to the Super I neutral alumina. Tumble or
shake on a wrist action shaker for a minimum of 2 hours or
preferably overnight. There should be no lumps present. Store
in a tightly sealed glass container. A 25 cycle soxhlet
extraction of the alumina with methylene chloride is required
if a solvent blank analyzed by the pesticide techniques
indicate any interferences for the compounds of interest.

2.4.3.1 Alumina Equivalency Check. Test the alumina by

adding the BNA surrogates (see Exhibit D SV) in 1:1
acetone/hexane to the alumina and following
paragraph 2.8.1. The tribromophenol should not be
detected by GC/EC if the alumina and its activation
are acceptable. Also check recovery of all single
component pesticides following the same procedure.
The percent recovery for all single component
pesticides must be £80%, except for endosulfan
sulfate which must be £60% and endrin aldehyde which
is not recovered. The data must be retained by the
Contractor and made available for inspection during
on-site evaluations. If the alumina deactivated with
7% (v/w) reagent water, does not prove adequate to
remove the BNA surrogates and other interferences,
the alumina may be deactivated with as much as 9%
reagent water, so long as the criteria for
tribromophenol and the recovery of all single
component pesticides can be met.

2.4.4 Reagent water - Reagent water is defined as water in which an
interferent is not observed at or above the CRQL of each
parameter of interest.

D-22/PEST

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2.4.5	Tetrabutylammonium (TEA) - sulfite reagent. Dissolve 3.39 g
tetrabutylammonium hydrogen sulfate in 100 mL distilled water.
To remove impurities, extract this solution three times with 20
mL portions of hexane. Discard the hexane extracts and add 25
g sodium sulfite to the water solution. Store the resulting
solution, which is saturated with sodium sulfite, in an amber
bottle with a Teflon-lined screw cap. This solution can be
stored at room temperature for at least one month.

2.4.6	GPC calibration solutions:

2.4.6.1	Com oil - 200 mg/mL in methylene chloride.

2.4.6.2	Bis(2-ethylhexylphthalate) and pentachlorophenol -
4.0 mg/mL in methylene chloride.

2.4.7	Sodium Sulfite, reagent grade.

2.4.8	Surrogate standard spiking solution.

2.4.8.1 Pesticide surrogate standard spiking solution.

2.4.8.1.1	The surrogate standard is added to all
samples, blanks, matrix spike, matrix
spike duplicates and calibrations
solutions; the compound specified for
this purpose is dibutylchlorendate.

2.4.8.1.2	Prepare a surrogate standard spiking
solution at a concentration of 20
ug/1.0 mL in methanol. Store the
spiking solutions at 4*C (±2*C)
Teflon-sealed containers. The
solutions should be checked frequently
for stability. These solutions must be
replaced after twelve months, or sooner
if comparison with quality control
check samples indicates a problem.

2.4.9	Matrix standard spiking solutions.

2.4.9.1 Pesticide matrix standard spiking solution. Prepare
a spiking solution in methanol that contains the
following pesticides in the concentrations specified
below. Store spiking solutions at 4*C (±2*) in
Teflon-sealed containers. The solutions should be
checked frequently for stability. These solutions
must be replaced after twelve months, or sooner if
comparison with quality control check samples
indicate a problem.

D-23/PEST

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Paafclclde	Ut/l.ff BL

lindane	2.0

heptachlor	2.0

aldrin	2.0

dieldrin	5.0

•ndrin	5.0

4,4' DDT	5.0

Matrix spikes are also to serve as duplicates,
therefore, add volume specified in Sample Extraction
section to each of two 30 g portions from one sample
chosen for spiking.

2.5 Sample Extraction

2.5.1	Decant and discard any water layer on a sediment sample. Mix
samples thoroughly, especially composited samples. Discard any
foreign objects such as sticks, leaves and rocks.

2.5.1.1 Transfer 50 g of soil/sediment to 100 mL beaker.

Add 50 mL of water and stir for 1 hour. Determine
pH of sample with glass electrode and pH meter while
stirring. Report pH value on appropriate data
sheets. If the pH of the soil is greater than 11 or
less than 5, contact the Deputy Project Officer
cited in the contract for instructions on how to
handle the sample. Document the instructions in the
Case Narrative. Discard this portion of sample.
NOTE: Recovery of dibutylchlorendate will be low if
pH is outside this range.

2.5.2	The following step should be performed rapidly to avoid loss of
the more volatile extractables. Weigh approximately 30 g of
sample to the nearest 0.1 g into a 400-mL beaker and add 60 g
of anhydrous powdered sodium sulfate. Mix well. The sample
should have a sandy texture at this point. Immediately, add
100 mL of 1:1 methylene chloride - acetone to the sample.

2.5.2.1	Immediately after weighing the sample for
extraction, weigh 5-10 g of the sediment into a
tared crucible. Determine the percent moisture by
drying overnight at 105*C. Allow to cool in a
desiccator before weighing. Concentrations of
individual analytes will be reported relative to the
dry weight of sediment.

g of sample - g of dry sample

	g o{ MaapU	 x 100 - % moisture

2.5.2.2	Weigh out two 30 g (record weight to nearest 0.1 g)
portions for use as matrix and matrix spike
duplicates. Follow 2.5.2. Vhen using GPC cleanup,
add 800 uL of the pesticide matrix spike to each of

D-24/PEST

2/88
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2.5.3

2.5.4

2.5.5

2.5.6

2.5.7

2.5.8

the other two portions. When not using GPC cleanup,
sdd 400 uL of the pesticide matrix spike to each of
the two portions.

2.5.2.3 Vhen using GPC, add 200 uL of pesticide surrogate to
the sample. When not using GPC, add 100 uL of
pesticide surrogate to the sample.

Place the bottom surface of the tip of the 3/4 inch disruptor
horn about 1/2 inch below the surface of the solvent but above
the sediment layer.

Sonicate for 1 1/2 minutes with the W-385 (or 3 minutes with
the W-375), using No. 208 3/4 inch standard disruptor horn with
output control knob set at 10 (or No. 305 3/4 inch tapped high
gain "Q" disruptor horn at 5) and mode switch on "1 sec. pulse"
and % duty cycle knob set at 50%. Do NOT use MICROTIP probe.
(If using a sonicator other than Models W-375 or U-385, contact
the Project Officer for appropriate output settings).

Decant and filter extracts through Whatman #41 filter paper
using vacuum filtration or centrifuge and decant extraction
solvent.

Repeat the extraction two more times with 2 additional 100 mL
portions of 1:1 methylene chloride - acetone. Before each
extraction, make certain that the sodium sulfate is free
flowing and not a consolidated mass. As required, break up
large lumps with a clean spatula, or very carefully with the
tip of the unenergized probe. Decant off the extraction
solvent after each sonication. On the final sonication, pour
the entire sample into the Buchner funnel and rinse with 1:1
methylene chloride - acetone.

Transfer the extract to a Kuderna-Danish (K-D) concentrator
consisting of a 10 mL concentrator tube and a 500 mL
evaporative flask. Other concentration devices or techniques
may be used if equivalency is demonstrated for all extractable
and pesticide compounds listed in Exhibit C.

Add one or two clean boiling chips to the evaporative flask and
attach a three-ball Snyder column. Pre-wet the Snyder column
by adding about 1 mL methylene chloride to the top. Place the
K-D apparatus on a hot water bath (80 to 90*C) so that the
concentrator tube is partially immersed in the hot water and
the entire lower rounded surface of the flask is bathed with
hot vapor. Adjust the vertical position of the apparatus and
the water temperature as required to complete the concentration
in 10 to 15 minutes. At the proper rate of distillation the
balls of the column will actively chatter but the chambers will
not flood with condensed solvent. When the apparent volume of
liquid reaches 1 mL, remove the K-D apparatus and allow it to
drain and cool for at least 10 minutes, and make up to 10 mL
volume with methylene chloride.

D-25/PBST	2/88
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2.5.9 If GPC cleanup is not used proceed to paragraph 2.7.

2.6. Extract Cleanup

2.6.1 GPC Setup and Calibration

2.6.1.1	Packing the coluan - Place 70 g of Bio Beads SX-3 in
a 400 nL beaker. Cover the beads with methylene
chloride; allow the beads to swell overnight (before
packing the columns). Transfer the swelled beads to
the coluan and start punping solvent through the
coluan, froa bottoa to top, at 5.0 oL/ain. After
approxiaately 1 hour, adjust the pressure on the
column to 7 to 10 psi and puop an additional 4 hours
to remove air from the column. Adjust the coluan
pressure periodically as required to maintain 7 to

10	psi.

2.6.1.2	Calibration of the column - Load 5 mL of the com

011	solution into sample loop Ho. 1 and 5 mL of the
phthalate-phenol solution into loop No. 2. Inject
the corn oil and collect 10 mL fraction (i.e.,
change fraction at 2-minute intervals) for 36
minutes. Inject the phthalate-phenol solution and
collect 15 mL fractions for 60 minutes. Determine
the corn oil elution pattern by evaporation of each
fraction to dryness followed by a gravimetric
determination of the residue. Analyze the
phthalate-phenol fractions by GC/FID on the DB-5
capillary column, a UV spectrophotometer or a GC/MS
system. Plot the concentration of each component in
each fraction versus total eluent volume (or time)
from the injection points. Choose a "dump time"
which allows £85% removal of the corn oil and £85%
recovery of the bis(2-ethylhexyl)-phthalate. Choose
the "collect time" to extend at least 10 minutes
after the elution of pentachlorophenol. Vash the
column at least 15 minutes between samples. Typical
parameters selected are: Dump time, 30 minutes (150
mL), collect time, 36 minutes (180 mL), and wash
time, 15 minutes (75 mL). The column can also be
calibrated by the use of a 254 mm UV detector in
place of gravimetric and GC analyses of fractions.
Measure the peak areas at various elution times to
determine appropriate fractions.

The SX-3 Bio Beads column may be reused for several
months, even if discoloration occurs. System
calibration usually remains constant over this
period of time if column flow rate remains constant.

D-26/PEST

2/88
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2.6.2 GPC Extract Cleanup

Prefilter or load all extracts via the filter holder to avoid
particulates that might stop the flow. Load one 5.0 mL aliquot
of the extract onto the GPC column. Do not apply excessive
pressure when loading the GPC. Purge the sample loading tubing
thoroughly with solvent between extracts. After especially
dirty extracts, run a GPC blank (methylene chloride) to check
for carry-over. Process the extracts using the dump, collect
and wash parameters determined from the calibration and collect
the cleaned extracts in 400 mL beakers tightly covered with
aluminum foil. The phthalate-phenol calibration solution shall
be taken through the cleanup cycle with each set of 23 extracts
loaded into the GPC. The recovery for each compound must be
£85%. This must be determined on a GC/FID, using a Dfi-5
capillary column, a UV recording spectrophotometer or a GC/MS
system. A copy of the printouts of standard and check solution
are required as deliverables with each case. Show % recovery
on the copy.

2.6.2.1 If GPC cleanup of samples is required because of

poor GC/ EC chromatography in Section IV, dilute the
extract to 10 mL with methylene chloride and perforin
GPC cleanup as per paragraph 2.6.2. The reagent
blank accompanying the samples should be included,
unless only one or a partial group of samples
requires cleanup. In this case, set up a new
reagent blank with 10 mL of methylene chloride and
appropriate surrogate standard added.

2.6.3 Concentrate the extract as per paragraphs 2.5.7 and 2.5.8.

Final Concentration of Extract with Optional Extract Splitting
Procedure

If the extract in 2.5.8 is to be used only for pesticide/PCB analysis,
it must be concentrated to a volume of 1.0 mL, following the procedure
in 2.7.1.

If the extract in 2.5.8 is to be used for both semlvolatile and
pesticide/ PCB analyses, then it must be split into two portions. In
that case, follow the procedure in 2.7.1 to obtain the pesticide
portion, and follow that with the procedure in 2.7.2 to obtain the
semlvolatile portion. Refer to Exhibit D SV for specific instructions
regarding the treatment of extracts for semlvolatile analysis.

2.7.1 If the extract is to be used only for the pesticide/PCB

analysis, or if the same extract is used for both semlvolatile
and pesticide/ PCB analyses, to split out the pesticide/PCB
extract, transfer 0.5 mL of the 10 mL methylene chloride
extract to a separate concentrator tube. Add 5 mL of hexane
and a silicon carbide boiling chip and mix using vortex mixer.
Attach a two-ball micro-Snyder column. Pre-wet the Snyder
column by adding 0.5 mL of hexane to the top of the column.

D-27/PEST

2/88
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Place the K-D apparatus on a hot water bath (80 - 90*C) so that
the concentrator tube is partially Immersed In the hot water.
Adjust the vertical position of the apparatus and the water
temperature as required to complete the concentration in 5 to
10 minutes. Concentrate the extract to an apparent volume of
less than 1 mL. Use Nitrogen blowdown (see 2.7.3) to reduce
the volume to 0.5 mL. Add 0.5 mL of acetone. The pesticide
extract must now be passed through an alumina column to remove
the BNA surrogates and polar interferences. Proceed to
paragraph 2.8.

2.7.2	If the extract in 2.5.8 jaa split in 2.7.1 to obtain a portion
for pesticides analysis, the portion for semivolatile analysis
must be treated according to the procedures in Exhibit D SV,
Section II, Part C, paragraph 2.7.2.2.

2.7.3	Nitrogen blowdown technique (taken from ASTM Method D 3086).
Place the concentrator tube in a warm water bath (35*C) and
evaporate the solvent volume to below 1 mL using a gentle
stream of clean, dry nitrogen (filtered through a column of
activated carbon). Caution: New plastic tubing must not be used
between the carbon trap and the sample, since it may introduce
interferences.

The internal wall of the tube must be rinsed down several times
with hexane during the operation. During evaporation, the tube
solvent level must be kept below the water level of the bath.
The extract must never be allowed to become dry. If GPC
cleanup techniques were employed, the 0.5 mL volume represents
a two-fold dilution to account for the fact that only half the
extract went through the GPC, and therefore, the sample
detection limit would be 2x CRQL (see Exhibit B).

2.7.4	Store all extracts at 4*C (±2*C) in the dark in Teflon-sealed
containers until all analyses are performed.

2.8 Pesticide/PCB

2.8.1 Alumina Column Cleanup

All samples prepared from the same extract as used for the
semivolatile analysis must be taken through this cleanup
technique to eliminate BNA surrogates that will interfere in
the GC/EC analysis.

2.8.1.1	Add 3 g of activity III neutral alumina to the 10 mL
chromatographic column. Tap the column to settle
the alumina. Do not pre-wet the alumina.

2.8.1.2	Transfer the 1.0 mL of hexane/acetone extract from
paragraph 2.7.1 to the top of the alumina using a
disposable Pasteur pipette. Collect the eluate in a
clean, 10 mL concentrator tube.

D-28/PEST

2/88
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2.8.1.3	Add 1 bL of hexane to the original extract
concentrator tube to rinse it. Transfer these
rinsings to the alumina column. Elute the column
with an additional 9 mL of hexane. Do not allow the
column to go dry during the addition and elution of
the sample.

2.8.1.4	Concentrate the extract to 1.0 mL following either
paragraph 2.7.1 or 2.7.3, using hexane where
methylene chloride is specified. When concentrating
medium level extracts, the Nitrogen blowdown
technique should be used to avoid contaminating the
micro Snyder column.

2.8.2	Observe the appearance of the extract.

2.8.2.1	If crystals of sulfur are evident or sulfur is
expected to be present, proceed to paragraph 2.8.3.

2.8.2.2	If the sulfur is not expected to be a problem,
transfer the 1.0 mL to a GC vial and label as
Festicide/PCB fraction. The extract is ready for
GC/EC analysis. Proceed to Section IV. Store the
extracts at 4*C (±2*C) in the dark until analyses
are performed.

2.8.3	Optional $ulfur Cleanup

2.8.3.1	Transfer the 1.0 mL from paragraph 2.8.2 to a 50 mL
clear glass bottle or vial with a Teflon-lined screw
cap. Rinse the concentrator tube with 1.0 mL of
hexane, adding the rinsings to the 50 mL bottle. If
only a partial set of samples requires sulfur
cleanup, set up a new reagent blank with 1.0 mL of
hexane and take it through the sulfur cleanup.

Include the surrogate standards.

2.8.3.2	Add 1 mL TBA-sulfite reagent and 1 mL 2-propanol,
cap the bottle, and shake for at least 1 min. If
the sample is colorless or if the initial color is
unchanged, and if clear crystals (precipitated
sodium sulfite) are observed, sufficient sodium
sulfite is present. If the precipitated sodium
sulfite disappears, add more crystalline sodium
sulfite in approximately 100 mg portions until a
solid residue remains after repeated shaking.

2.8.3.3	Add 5 mL distilled water and shake for at least 1
min. Allow the sample to stand for 5-10 min. and
remove the hexane layer (top) for analysis.
Concentrate the hexane to 1.0 mL as per paragraphs

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2/88
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2.7.1 and 2.7.3 using hexane where methylene
chloride is specified. The temperature for the
water bath should be about 80*C for the micro Snyder
column technique. Continue as outlined in paragraph
2.8.2.2.

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SECTION III
SCREENING OF PESTICIDE/PCB EXTRACTS

D-31/PEST

2/88
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1. It is mandatory that all soil/sediment samples be characterized as to
concentration level so that the appropriate analytical protocol may be
chosen to ensure proper quantitation limits for the sample.

The use of GC/EC methods is recommended for screening soil/sediment
samples for pesticides/PCBs. The contractor is at liberty to determine
the specific method of characterization. The protocols for sample
preparation (Section II) and sample analysis (Section IV) are broken
down by concentration level.

2. The terms "low level" and "medium level" are not used as a judgement of
the degree of contamination, but rather as a description of the
concentration ranges that are encompassed by the "low" and "medium"
protocols.

The concentration range encompassed by the low level protocols may be
considered to be appropriate for those samples with less than 1000
ug/kg of pesticides/ PCBs. The concentration range encompassed by the
medium level protocols may be considered to appropriate for those
samples with more than 1000 ug/kg of pesticides/PCBs.

D-32/PEST

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SECTION IV
CC/EC ANALYSIS OP PKSTICIDBS/PCB«

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2/88
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1.

Summary of Mat-hod

1.1 The hexane extracts of water and soil/sediment are analyzed on a gas

chromatograph/electron capture detector (GC/EC). If pesticides or PCBs
are tentatively identified, a second GC/EC analysis is required using
an alternate column. Quantitation must be on a packed column or a wide
bore capillary column (ID >0.32 mm), whereas, confirmation can be on a
packed column, a wide bore capillary column or a narrow bore capillary
column. NOTE: To determine that no pesticides/PCBs are present at or
above the contract required quantitation limit is, a form of
quantitation.

2.	Interferences

2.1 Method interferences nay be caused by contaminants in solvents,

reagents, glassware, and other sample processing hardware that lead to
discrete artifacts and/or elevated baselines in gas chromatograms. All
of these materials must be routinely demonstrated to be free from
interferences under the conditions of the analysis by running
laboratory method blanks.

3.	Apparatus And Materials

3.1 Gas chromatograph - An analytical system complete with gas

chromatograph and all required accessories including syringes,
analytical columns, gases, electron capture detector and strip-chart
recorder with recording integrator. A data system is required for
measuring peak areas or peak heights and recording retention times. An
electrolytic conductivity detector is also acceptable if the required
quantitation limits are met. Overlapping peaks on rhrnnat-ograms are not
acceptable.

3.1.1 Quantitation and/or confirmation columns.

3.1.1.X Column 1 - Gas Chrom Q (100/120 mesh) or equivalent
coated with 1.5% 0V-17/1.95% OV-210 or equivalent
packed in a 1.8m long x 4 an ID (6 an OD) glass
column.

NOTE: The 2mm ID column cited in Table 7 as Column
1 will not adequately separate dibutylchlorendate
and endrin ketone.

3.1.1.2	Column 2 - Gas Chrom Q (100/120 mesh) or equivalent
coated with 3% OV-1 or-equivalent packed in a 1.8 m
long x 2 mm ID (6 mm OD) glass column.

3.1.1.3	Column 3 - Gas Chrom Q (80/100 mesh) or equivalent
coated with 5% OV-210 or equivalent packed in a 1.8
m long x 2 mm ID (6 an OD) glass column.

3.1.1.4	Vide bore capillary columns (ID >0.32 ¦¦) may be
employed for these analyses in place of packed
columns. Strictly speaking, there are no
equivalent wide bore columns for the mixed phase

D-34/PEST

Rev. 5/89
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Column 1 above. However, wide bore columns such as
DB-5 or DB-1701 may provide equivalent performance.
It Is the responsibility of the Contractor to
demonstrate the equivalence of any wide bore
columns employed for these analyses. Equivalence is
demonstrated by meeting all of the performance
criteria for pesticide analyses given in Exhibit D
and E. Such data should be kept on file by the
laboratory, and be available during on-site
evaluations.

Confirmation column only. Column • 30 m X 0.25 mm ID, 0.25
micron film thickness, bonded-phase silicone coated, fused
silica capillary column (J&W Scientific DB-5 or DB-1701 or
equivalent). NOTE: DB-1701 provides better separation of TCL

D-34a/PEST

Rev. 9/88
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pesticides. Column 10 n x 0.32 mm ID, 1 micron film thickness
has been used.

3.2 Balance - analytical, capable of accurately weighing ±0.0001 g.

4. Rtmntl

4.1	Isooctane (2,2,4-trimethylpentane), hexane and toluene - Pesticide
quality or equivalent.

4.2	Stock standard solutions (1.00 ug/uL) - Stock standard solution can be
prepared fron pure standard materials or purchased as certified
solutions.

4.2.1	Prepare stock standard solutions by accurately weighing about
0.0100 g of pure material. Dissolve the material in toluene,
dilute to volume in a 10 mL volumetric flask with isooctane.
Larger volumes can be used at the convenience of the analyst.
If compound purity is certified at 96% or greater, the weight
can be used without correction to calculate the concentration
of the stock standard. Commercially prepared stock standards
can be used at any concentration if they are traceable to
EMSL/LV supplied standards.

4.2.2	Transfer the stock standard solutions into a bottle/vial with
Teflon-lined septa. Store at 4*C (±2*C) and protect from
light. Stock standard solutions must be replaced after twelve
months, or sooner if comparison with check standards indicate a
problem.

4.3	Working standards solutions - Prepare mixtures of standards diluted
with hexane that will provide approximately half scale response for all
the compounds of Interest. This should be at the attenuation setting
capable of achieving the contract-required quantitation limits (Exhibit
C). (This would be approximately 0.01 ng/uL for aldrin.) Two mixtures
of the Individual component standards are recommended to prevent
co-elutlon of components on packed columns. However, all Individual
component standards may be included in one mixture on packed or
capillary columns if the laboratory demonstrates that the components
may be separated with nft overlap of peaks. Include dibutylchlorendate
in all standard mixtures. All multicomponent standards, i.e., PCB
Aroclors and toxaphene must be in separate solutions with the exception
of Aroclors 1016/1260. Include dibutylchlorendate in all
multicomponent standard mixtures.

4.3.1 Evaluation Standard Mixtures - Prepare working standard

mixtures diluted with hexane containing aldrin, endrin, 4,4'
DDT and dibutylchlorendate to evaluate the GC coluan. Prepare
three concentration levels to provide the following criteria:

4.3.1.1 Low level will be approximately 20t above base line
(Evaluation Standard Mix A).

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4.3.1.2	Mid level will be approximately half scale
(Evaluation Standard Mix B).

4.3.1.3	High level will be approximately full scale
(Evaluation Standard Mix C). (Dibutylchlorendate
mist be 0.1 ng/uL to correspond with 100% surrogate
recovery in 10 nL final volume. This may be
slightly greater than full scale but should still be
in linear range).

4.3.2 Individual Standard Mixtures - These include all single

component TCL pesticides plus alpha chlordane, gamma chlordane,
endrin ketone, endrin aldehyde and dibutylchlorendate (see
paragraph 6.1.4 for suggested mixtures). Alpha and gamma
chlordane should be in Mixture B to avoid overlap with other
pesticides.

5. Calibration

5.1	The gas chromatographic system must be calibrated using the external
standard technique for all packed columns used for quantitation.

5.2	External standard calibration procedure:

5.2.1 Prepare calibration standards at a minimum of three

concentration levels for each parameter of interest by adding
volumes of one or more stock standards to a volumetric flask
and diluting to volume with hexane. One of the external
standards should be at a concentration near, but above, the
CRQL and the other concentrations should correspond to the
expected range of concentrations found in real samples or
should define the working range of the detector. This should be
done on each quantitation column and each instrument at the
beginning of the contract period and each time a new column is
installed. The data must be retained by the laboratory and
made available for inspection during on-site evaluations.

5.2.2 Using injections of 2 to 5 uL of each calibration standard,
tabulate peak height or area responses against the mass
Injected. The results can be used to prepare a calibration
curve for each compound.

6- GC/EC Primary Analysis (Quantitation may be performed on primary or
confirmatlon analyses.)

Adjust oven temperature and carrier gas flow rates so that the
retention time for 4,4'-DDT is equal to or greater than 12 minutes.

Table 7 provides examples of operating conditions for the gas
chromatograph. Separation should be £ 25% resolution between peaks.
Percent resolution is calculated by dividing the height of the valley
by the peak height of the smaller peak being resolved, multiplied by
100. This criterion must be considered when determining whether to
quantitate on the Primary Analysis or the Confirmation Analysis. When

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this criterion cannot be met, quantitation is adversely affected
because of the difficulty in determining where to establish the
baseline.

6.1 Inject 2 to 5 uL of the sample or standard extract using the

solvent-flush technique or auto sampler. Smaller (1.0 uL) volumes can
be injected only if automatic devices are employed. Record the volume
injected to the nearest 0.05 uL and the total extract volume. NOTE:
Dibutylchlorendate recovery may be calculated from a capillary or
packed column GC/EC meeting all QC requirements for quantitation.
However, matrix spike duplicates must be quantitated on a packed column
or wide bore capillary column.

6.1.1	Inject Individual Standard Mix A and B and all multiresponse
pesticides/PCBs at the beginning of each 72 hour sequence.
(See paragraph 6.1.3.5) To establish the RT window within each
72-hour sequence for the pesticide/PCB of interest, use the
absolute RT from the above chromatograms as the mid-point, and
± three times the standard deviation calculated in Exhibit E
for each compound. Individual Standard Mix A and B are analyzed
alternately and intermittently throughout the analysis as shown
in 6.1.3.5. Any pesticide outside of its established retention
time window requires immediate investigation and correction
before continuing the analysis. The laboratory must reanalyze
all affected samples.

6.1.2	Sample analysis of extracts from Section II, Sample
Preparation, can begin when linearity and degradation QA/QC
requirements specified in Exhibit E have been met.

NOTE: The 10.0% RSD linearity criterion is only required on
the column(s) being used for pesticide/PCBs quantitation. If a
column is used for surrogate quantitation only, the 10.0% RSD
is required only for dibutylchlorendate.

Analyze samples in groups of no more than 5 samples. After the
analysis of the first group of up to 5 samples, analyze
Evaluation Mix B. Analyze another group of up to 5 samples,
followed by the analysis of Individual Mix A or B. Subsequent
groups of up to 5 samples may be analyzed by repeating this
sequence, alternately analyzing Evaluation Mix B and Individual
Mix A or B between the groups as shown in 6.1.3.5. The
Pesticide/PCB analytical sequence must end with Individual Mix
A and B regardless of the number of samples analyzed (see
6.1.3.5).

If a multiresponse pesticide/PCB is> detected in either of the
preceding groups of 5 samples, the appropriate multiresponse
pesticide/PCB may be substituted for Individual Mix A or B. All
standards listed in 6.1.3.5 must be included for every Case and
must be analyzed within the same 72-hour period as the samples,
with the exception of Aroclors 1221 and 1232 which are analyzed
at a minimum of once per month (see footnote in 6.1.3.5). If
the samples are split between 2 or more instruments, the

D-37/PEST

Rev. 9/88
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complete set of standards oust be analyzed on each Instrument
with the same 72-hour requirement. All standards must be
analyzed prior to the samples to avoid the effects of poor
chromatography caused by the unsuspected injection of a highly
concentrated sample.

6.1.3 Paragraphs 6.1.3.1 - 6.1.3.5 contain GC performance criteria.
If it is determined during the course of a 72-hour sequence
that one or more of the criteria have been violated, stop the
run and take corrective action (see Exhibit E, Section III
PEST, 4.3.3.8). After the corrective action has been taken,
the 72-hour sequence may be restarted as follows. If a
standard violated the criterion, restart the sequence with that
standard, determine that the criteria have been met and
continue with sample analyses, according to 6.1.3.5. If a
sample violated the criterion, restart the sequence with the
standard that would have followed that group of samples
(thereby preserving the sequence of standards in 6.1.3.5),
determine that the criteria have been met and continue with
sample analyses, according to 6.1.3.5.

If it is determined after the completion of a 72-hour sequence
that one or more of the criteria have been violated, proceed as
follows. If a standard violated the criterion, all samples
analyzed after that standard must be re-analyzed as part of a
new 72-hour sequence. If a subsequent standard in the original
sequence met all the criteria, then only those samples analyzed
between the standard that did not meet the criterion and the
standard that did Met the criterion must be re-analyzed as
part of a new 72-hour sequence. If only samples violated the
criteria, then those samplas must be re-analyzed as part of a
new 72-hour sequence.

6.1.3.1 Differences in the Calibration Factors for each

standard in Individual Standard Mix A and B must not
exceed 20.0% (15.0% for any standard compound used
for quantitation) during the 72-hour Primary
Analysis. Calculate the % difference using the
initial Individual Standard Mix versus all
subsequent Individual Standard Nixes analyzed during
the 72-hour sequence. (The equations for
calculation of Calibration Factor and % difference
are in Exhibit E, Section III PEST, paragraph
4.3.4.2.) NOTE: To determine that no
pestlcides/PCBs are present at or above the contract
required quantitation limit • form of
quantitation.

The retention time shift of dibutylchlorendate in
any standard or sample must be less than 2.0%
difference for packed columns, less than 1.5%
difference for wide bore capillary columns (ID
greater than 0.32 mm) and less than 0.3% difference

D-38/PEST

2/88
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for narrow bore capillary columns (ID less than 0.32
mm) .

6.1.3.2	Samples must also be repeated if the degradation of
DDT and/or endrin exceeds 20.0% respectively on the
intermittent analysis of Evaluation Standard Mix B.

6.1.3.3	All pesticide standards must fall within the
established 72-hour retention time windows.

6.1.3.4	Highly colored extracts may require a dilution.

6.1.3.5	The 72-hour sequence must be as follows.

72-Hour Sequence for Festicide/PCB Analysis:

1.	Evaluation Standard Mix A

2.	Evaluation Standard Mix B

3.	Evaluation Standard Mix C

4.	Individual Standard Mix A*

5.	Individual Standard Mix B*

6.	Toxaphene

7.	Aroclors 1016/1260

8.	Aroclor 1221**

9.	Aroclor 1232**

10.	Aroclor 1242

11.	Aroclor 1248

12.	Aroclor 1254

13.	5 samples

14.	Evaluation Standard Mix B

15.	5 samples

16.	Individual Standard Mix A or B

17.	5 samples

18.	Evaluation Standard Mix B

19.	5 samples

20.	Individual Standard Mix A or B
(whichever not run in step 16)

21.	5 samples

22.	Repeat the above sequence starting
with Evaluation Standard Mix B (step
14 above).

23.	Pesticide/PCB analysis sequence must
end with the analyses of both
Individual Standard Mix A and B
regardless of number of samples
analyzed.

~These may be combined into one mixture (see
paragraph 4.3).

**Aroclors 1221 and 1232 must be analyzed on each
instrument and each column at a minimum of once per
month.

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Copies of these chromatograms must be submitted for
sample analyses performed during the applicable
month.

6.1.4 Suggested groups of compounds and concentrations for Individual
Standard Mi* A and B follow, which are recommended to prevent
overlap of compounds on the two packed columns (3% OV-1 and
1.5% OV-17/1.95% OV-210). Some of the compounds overlap on the
5% OV-210 column (see Table 7). The concentration is based on
a 5 uL injectira.

Individual



Individual



Standard Mix A

ny/uL

Standard Mix B

ny/uL

gamma-BHC

0.005

alpha-BHC

0.005

heptachlor

0.010

beta-BHC

0.010

aldrin*

0.010

delta-BHC

0.010

heptachlor epoxide

0.010

aldrin*

0.010

endosulfan I

0.010

p,p'-DDE

0.010

dieldrin

0.010

endrin

0.010

p.p'-DDT

0.020

p,p'-DDD

0.020

endrin aldehyde

0.025

endosulfan sulfate

0.020

endosulfan II

0.020

endrin ketone

0.020

methoxychlor

0.100

alpha chlordane

0.010

dibutylchlorendate

0.050

guana chlordane

0.010





dibutylchlorendate

0.050

*For RRT determination.

6.1.5 Inject the method blank (extracted with each set of samples) on
every Instrument and GC column on which the samples are
analyzed.

6.2 Evaluation of Chromatograms.

6.2.1	Consider the sample negative when its peaks, depending on the
pesticide's response factor, result in concentrations less than
the required quantitation level. The sample is complete at .
this point. Confirmation is not required.

6.2.2	Tentative identification is made when the unknown's retention
time matches the retention time of a corresponding standard
that was chromatographed on the same instrument within a

72-hour period.

6.2.3	Determine if any pesticides/PCBs listed in Exhibit C are
present. Pattern recognition techniques, based on chromatograms
of standards, are recommended for the identification of PCB
compounds.

6.2.3.1 If the response for any of these compounds is 100%
or less of full scale, the extract is ready for
confirmation and quantitation.

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2/88
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If Che response for any compound Is greater than
full scale, dilute the extract so that the peak will
be between 50 and 100% full scale and reanalyze on
the packed column. Use this dilution also for
confirmation and quantitation.

For dilution >10 fold. Also inject an aliquot of a
dilution 10 fold more concentrated to determine if
other compounds of Interest are present at lower
concentrations.

Computer reproductions of chromatograms manipulated
to ensure all peaks are on scale over a 100 fold
range are an accepted substitute. However, this can
be no greater than a 100 fold range. This is to
prevent retention time shifts by column or detector
overload. Linearity must be demonstrated over the
100 fold range using higher concentrations of the
evaluation mixture.

6.2.4	Quantitation may be performed on the primary analysis, with the
exception of toxaphene and possibly the DDT series. If DDT
exceeds the 10.0% RSD linearity criterion, then quantitations
for any DDE, DDD and DDT in a sample must be on the
confirmation analysis. Toxaphene must always be quantltated on
the confirmation analysis. See Exhibit E for special QC
requirements for quantitation.

6.2.5	If identification of compounds of interest are prevented by the
presence of Interferences, further cleanup is required. If
sulfur is evident go to Sulfur Cleanup (Section II, Part B,
paragraph 8.). If unknown interferences or poor chromatography
are noted only in the sample chromatogram, it is recommended
that gel permeation chromatography cleanup (Section II, Part C,
paragraph 2.6) be applied.

6.2.6	Vhen selecting a GC column for confirmation and/or
quantitation, be sure that none of the compounds to be
conflrmed/quantitated overlap, i.e., do not select the 3% OV-1
column if DDE and dieldrin are to be confirmed and/or
quantltated. Vhen samples are very complex, it may be
necessary to use all three packed columns to achieve adequate
separation (£25% resolution) of all compounds being
quantltated.

7. GC/EC ConfjnMMon Analysis

7.1 Confirmation Analysis is to confirm the presence of all compounds

tentatively identified in the Primary Analysis. Therefore, the only
standards that are required are the Evaluation Standard Mixes (to
check linearity and degradation criteria) and standards of all
compounds to be confirmed. The linearity criterion on the confirmation
column for pesticides is not required unless the column is used for
quantitation. The 72-hour sequence in 6.1.3.5 is, therefore, modified

6.2.3.2

6.2.3.3

6.2.3.4

D-41/PEST

2/88
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to fit each case. Quantitation nay be performed on the confirmation
analysis. If toxaphene or DDT i» to be quantitated, additional
linearity requirements are specified in 7.3.1.

7.2 Table 7 provides examples of operating conditions for the gas

chromatograph. Separation should be £25% resolution between peaks.
Percent resolution is calculated by dividing the height of the valley
by the peak height of the smaller peak being resolved, multiplied by
100. This criterion must be considered when determining whether to
quantitate on the Primary Analysis or the Confirmation Analysis. When
this criterion cannot be met, quantitation is adversely affected
because of the difficulty in determining where to establish the
baseline.

For a fused silica capillary column (FSCC) confirmation, there must be
>25 percent resolution (valley) between the following pesticide pairs:

o beta-BHC and delta-BHC
o Dieldrin and 4,4'-DDT
o 4,4'-DDD and Endrin Aldehyde
o Endosulfan Sulfate and 4,4'-DDT

All QC requirements specified in Exhibit E must be adhered to, i.e.,
the £12 min. retention time for 4,4'-DDT, the criteria for 4,4'-DDT and
endrin degradation, linearity, calibration factor for standards and
retention time shift for dibutylchlorendate. The retention time
criterion for 4,4'-DDT does not have to be met if the confirmation
column is OV-1 or OV-101. Apply instructions from 6.1.3 to the
confirmation analysis.

7.3 Inject 2 to 5 uL (1-2 uL for capillary columns) of the sample extract
and standards using the solvent-flush technique or auto samplers. A
volume of 1 uL can be injected only if automatic devices are employed.
Record the volume injected to the nearest 0.05 uL and the total extract
volume. The detector attenuation must provide peak response equivalent
to the Primary Analysis response for each compound to be confirmed.

7.3.1 Begin the Confirmation Analysis GC sequence with the three

concentration levels of Evaluation Standard Mixes A, B and C.
The exception to this occurs when toxaphene and/or DDT series
are to be confirmed and quantitated. There are four
combinations of pesticides that could occur, therefore, the
following sequences must be followed depending on the
situation.

7.3.1.1 Toxaphene only - Begin the sequence with Evaluation
Mix B to check degradation, followed by three
concentration levels of toxaphene. Check linearity
by calculating %RSD.

If £10.0% RSD, use the appropriate equation in
paragraph 8 for calculation. If >10.0% RSD, plot a
standard curve and determine the ng for each sample
in that set from the curve.

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7.3.1.2	DDT, DDE, DDD only - Begin the sequence with
Evaluation Mix B. Then inject three concentration
levels of a standard containing DDE, DDD and DDT.
Calculate linearity and follow the requirements
specified in 7.3.1.1 for each compound to be
quantitated.

7.3.1.3	DDT series and toxaphene - Begin the sequence with
Evaluation Mix B. Then inject three concentration
levels of toxaphene and another three levels of the
DDT series. Calculate linearity and follow the
requirements specified in 7.3.1.1 for each compound
to be quantitated. NOTE: Capillary quantitation
would be allowed only in this situation.

7.3.1.4	Other pesticldes/PCBs plus DDT series and/or
toxaphene — Begin the sequence with Evaluation
Standard Mixes A, B and C. Calculate linearity on
the four compounds in the Evaluation Standard mixes.
If DDT and/or one or more of the other compounds are
>10.0% RSD and/or degradation exceeds the criterion,
corrective maintenance as outlined in Exhibit E,
Section III PEST, paragraph 4.3.3.8, should be
performed before repeating the above chromatography
evaluations. If only DDT exceeds the linearity
criterion and one or more of the DDT series is to be
quantitated, follow 7.3.1.2 (do not repeat
Evaluation Mix B).

If none of the DDT series Is to be quantitated and
DDT exceeds the 10.0% RSD, simply record the % RSD
on the proper form. Any time toxaphene is to be
quantitated, follow 7.3.1.1.

7.3.2	After the linearity standards required in 7.3.1 are injected,
continue the confirmation analysis sequence by injecting
standards for all compounds tentatively identified in the
primary analysis, to establish the 72-hour retention time
windows. (See paragraph 6.1.1.) Analyze all confirmation
standards for a case at the beginning, at intervals specified
In 7.3.3 and at the and. Any pesticide outside of its
established retention time window requires immediate
investigation and correction before continuing the analysis.
The laboratory must reanalyze all samples which follow the
standard that exceeds the criterion.

7.3.3	After Injection of the appropriate standards (see 7.3.2), begin
injection of samples. Analyze groups of 5 samples. Analyze
Evaluation Mix B after the first group of 5 samples. After the
second group of 5 samples, analyze a standard pertaining to the
samples in the preceding groups (I.e., substitute standards
pertaining to the preceding samples for Individual Mix A or B
in 6.1.3.5). Continue analyzing groups of 5 samples,
alternately analyzing Evaluation Mix B and standards pertaining

D-43/PEST

2/88
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to the preceding samples between groups of 5 samples. The
alternating standard's calibration factors must be within 15.0%
of each other if quantitation is performed. Deviations larger
than 15.0% require the laboratory to repeat the analyses of
samples which were analyzed after the standard that exceeded
the criterion. The 15.0% criterion only pertains to compounds
being quantitated.

If more than one standard is required to confirm all compounds
tentatively identified in the Primary Analysis, alternate the
standards with Evaluation Mix B. Samples must also be repeated
if the degradation of either DDT and/or endrin exceeds 20.0% on
the intermittent Evaluation Standard Mix B.

If the samples are split between 2 or more instruments, all
standards and blanks pertaining to those samples must be
analyzed on each instrument.

7.3.4 Inject the method blank (extracted with each set of samples) on
every GC and GC column on which the samples are analyzed.

7.4 Evaluation of Chromatograms

7.4.1	A compound tentatively identified in the primary analysis is
confirmed if the retention time from the confirmation analysis
falls within the retention time window of a corresponding
standard* that was chromatographed on the same instrument within
a 72-hour period.

7.4.2	Quantitation should be on the packed column or wide bore
capillary column chromatogram (primary or confirmation) that
provides the best separation from interfering peaks. NOTE: To
determine that no pesticides/PCBS are present at or above the
contract required quantitation limit jj. * form of quantitation.

7.4.2.1 Quantitation of Chlordane - Because weathering

and/or different formulations of chlordane usually
modify the pattern exhibited by technical chlordane,
this method is not appropriate for determining
technical chlordane. Instead, standards for alpha
chlordane and gamma chlordane are used for
quantitation, and each isomer of chlordane is
reported separately.

7.4.3	Computer reproductions of chromatograms that are attenuated to
ensure all peaks are on scale over a 100 fold range are
acceptable. However, this can be no greater than a 100 fold
range. This is to prevent retention time shifts by column or
detector overload. Also, peak response must be >25% of full
scale deflection to allow visual pattern recognition of
multicomponent compounds, and individual compounds must be
visible.

D-44/PEST

Rev. 9/88
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If identification of compounds of interest are prevented by the
presence of interferences, further cleanup is required. If
sulfur is evident, go to Sulfur Cleanup (Section II, Part B,
paragraph 8).

If unknown interferences or poor chromatography are noted only
in the sample chromatogram, it is recommended that gel
permeation chromatography cleanup (Section II, Part C,
paragraph 2.6) be applied.

Calculate surrogate standard recovery on all samples, blanks
and spikes unless the surrogate was diluted out. Determine if
recovery is within limits and report on Form II. See formula
for calculation in 8.3.

If TCL pesticide/PCB compounds were identified in the unspiked
sample from which the matrix spike and matrix spike duplicate
were prepared, confirmation analysis is required for the matrix
spike and matrix spike duplicate. If TCL pesticide/PCfi
compounds were not identified in. the unspiked sample,
confirmation of the matrix spike and matrix spike duplicate is
not required. Calculate matrix spike duplicate recoveries and
report on Form III (see Exhibit B, Section III).

8. Calculations

8.1 Calculate the concentration in the sample using the following equation
for external standards. Response can be measured by the manual peak
height technique or by automated peak height or peak area measurements
from an Integrator.

8.1.1	Water

(Q(I,)(V,.)

Concentration ug/L - (Ag)(V^)(Vs)

Where:

a - Response for the parameter to be measured.

A - Response for the external standard.

V8 - Volume of total extract (uL) (take into account

' any dilutions)

I . Amount of standard injected in nanograms (ng)
vf - Volume of extract injected (uL)

V* - Volume of water extracted (mL)

8.1.2	fit^m^t/Soil

(V(I.)(Vt)

Concentration	ugAg " (AB)(Vj)(W8)(D)

(Dry weight basis)

7.4.4

7.4.5

7.4.6

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Where:

same as given above in 8.1.1

Volune of low level total extract
(Use 20,000 uL or a factor of this when
dilutions are made other than those accounted
for below):

o 1/20 total extract taken for pesticide
analysis (derived from 0.5 mL of 10 mL
extract)

o final concentration to 1.0 mL for pesticide
analysis

- or -

V -	Volume of Medium level total extract

(Use 10,000 uL or a factor of this when
dilutions are made.)

D _	100 - % moisture (% moisture from Section II,

100	Part C)

Wa -	Weight of sample extracted (g)

8.2	For multicomponent mixtures (chlordane, toxaphene and PCBs) match
retention times of peaks in the standards with peaks in the sample.
Quantitate every identifiable peak (>50» of the total area must be
used) unless interference with individual peaks persist after cleanup.
Add peak height or peak area of each identified peak in the
chromatogram. Calculate as total response in the sample versus total
response in the standard.

8.3	Calculation for surrogate and matrix spike recoveries.

Percent Recovery — Qa

-J- X 100%

where,

- quantity determined by analysis
Qa - quantity added to sample.

Be sure all dilutions are taken into account. Soil/Sediment has a
20-fold dilution factor built into the method when accounting for
one-twentieth of extract taken for pesticide analysis and final
dilution to 1 mL.

8.4	Report results in micrograms per liter or micrograms per kilogram

without correction for recovery data.

Ay, I#»As,VjL -

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GC/MS Confirmation of Pesticides

Any compounds confirmed by two columns must also be confirmed by GC/MS

if the concentration is sufficient for detection by GC/MS. The

following paragraphs should be used as guidance when determining if a

pestlcide/PCB compound can be confirmed by GC/MS.

9.1.1	The GC/MS analysis normally requires a minimum concentration of
10 ng/uL in the final extract, for each single component
compound. For the BNA extract of a water sample, a
concentration of 10 ng/uL in extract is approximately 20 ug/L
(ppb) in the sample. For the BNA extract of a low level soil
sample, the equivalent sample concentration would be
approximatly 170 ug/Kg if no GPC was performed. For the BNA
extract of a medium soil, the equivalent sample concentration
is on the order of 10,000 ug/Kg.

9.1.2	The pesticide extract and associated blank should be analyzed
by GC/MS as per Exhibit D SV, Section IV, paragraph 5.

9.1.3	The confirmation may be from the GC/MS analysis of the
semlvolatile extracts (sample and blank). However, if the
compounds are not detected in the semlvolatile extract even
though the concentration Is high enough, a GC/MS analysis of
the pesticide extract is required.

9.1.4	A reference standard for the compound must also be analyzed by
GC/MS. The concentration of the reference standard must be at
a level that would demonstrate the ability to confirm the
pesticides/PCBs Identified by GC/EC. Use the sample
concentration calculated from the GC/EC results as guidance.
The concentration of the reference standards must be no greater
than the sample extract concentration predicted from the GC/EC
sample concentration. For Instance, as in paragraph 9.1.1
above, a 20 ug/L sample result from GC/EC requires a 10 ng/uL
GC/MS reference standards in order to demonstrate adequate
sensitivity for a water sample.

9.1.5	In the event the GC/MS does not confirm the presence of the
pesticides/PCBs identified by GC/ECD, those compounds should be
reported as not detected. The minimum quantitation limits ("U"
values) should be adjusted to reflect the interferences. The
inability to confirm the compounds by GC/MS must be noted in
the Case Narrative.

9.1.6	For GC/MS confirmation of multicomponent pesticides and PCBs,
required deliverables are spectra of 3 major peaks of
multicomponent compounds from samples and standards.

9.1.7	Quantitation by GC/MS must use the characteristic quantitation
ions for pesticides/PCBs given in Table 5 of Exhibit D SV.

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Table 7

Examples of Orders of Elution of Pesticides/PCBs

Parameter

alpha-BHC
gamma-BHC
beta-BHC
Heptachlor
delta-BHC
Aldrin

Heptachlor epoxide

Endosulfan 1

4,4'-DDE

Dieldrln

Endrln

4,4*-DDD

Endosulfan 11

4,4'-DDT

Endrin aldehyde

Endosulfan sulfate

Endrln ketone

gamma Chlordane

alpha Chlordane

Toxaphene

Aroclor-1016

Aroclor-1221

Aroclor-1232

Aroclor-1242

Aroclor-1248

Aroclor-1254

Aroclor-1260

methoxychlor

dlbutvlchlorendate

Column 1

Column 2

Column 3

1.45

1.64

1.86

1.86

1.94

2.37

2.18

1.76

2.75

2.27

3.21

2.55

2.55

2.01

2.80

2.76

4.01

2.93

4.31

4.98

5.53

5.46

6.26

7.08

6.37

7.51

6.03

6.74

7.38

8.59

8.25

8.35

10.14

10.08

9.53

10.57

10.14

8.35

12.88

12.06

12.75

11.55

13.64

9.53

21.11

16.73

11.09

31.27

22.70

-

33.16

4.77

5.74

5.25

5.24

6.39

5.70

mr

mr

mr

mr

mr

mr

mr

mr

mr

mr

mr

mr

mr

mr

mr

mr

mr

mr

mr

mr

mr

mr

mr

mr

24.07

19.60

18.12

21.80

27.21

22.26

mr - multlrespouse compounds.

Column 1 conditions: Gas Chrom Q (80/100 mesh) or equivalent coated with
1.5% OV-17/1.95% OV-210 or equivalent packed in a 1.8 m long x 2 mm ID (6 mm
OD) glass column with 5% methane/95% argon carrier gas at a flow rate of 30
mL/min. (HP 5880) Column temperature, isothermal at 192*C. 2 mm ID column
with 80/100 mesh does not adequately resolve dibutyl chlorendate and endrin
ketone.

Column 2 conditions: Gas Chrom Q (100/120 mesh) or equivalent coated with 3%
OV-1 or equivalent packed in a 1.8 m long x 2 mm ID (6 m OD) glass column
with 5% methane/95% argon carrier gas at a flow rate of 30 mL/min. (30
mL/min makeup gas). (Tracor 222). Column temperature, isothermal at 194*C.

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Table 7 (continued)

OV-2T0	i . ^r°" Q <80/100 —h) or equivalent co.t.d with 5«

-IKCOD) gl... colunn with 5% .ethane/

HP5840 Colimn*^ g" " " V "" o£ 30 "L/"ln- <30 »v»tn. ..k.-up g«s).
Hr5B40. Column temperature, Isothermal at 183'C.

Capillary column 1 condition.: 30 m x 0.25 mm ID, 0.25 micron film thickness,

fused silica DB-5 (or equivalent) splitless mode

Helium carrier gas: 4 mL/min at 280*C and 25 PSI
Septum purge: 15 mL/min
Split vent: none

Initial temperature: 160*C, initial hold - 2 mln
Program at 5*C/min

Final temperature: 270*C, final hold - 4 min
Injection port temperature: 225*C

Capillary column 2 conditions: 10 m * 0.32 mm ID, 1 micron film thickness,

fused silica DB-1701, splitless mode

Helium carrier gas: 4 mL/min at 280*C and 25 PSI
Septum purge: 15 mL/min
Split vent: none

Initial temperature: 160*C, initial hold - 3 min

Program at 10*C/min to 240*C

Program from 240 to 270*C at 5#C/min

Final Hold: 4 min

Injection port temperature: 235*C

D-49/PEST

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exhibit e

QUALITY ASSURANCE/QUALITY CONTROL REQUIREMENTS

E-l

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Table of Contents

Section	£&&&

I INTRODUCTION 	E-3

II QA/QC STANDARD OPERATING PROCEDURES 	 E-4

III QA/QC REQUIREMENTS

Volatiles (VOA) QA/QC Requirements 	E-10/VOA

Semivolatiles (SV) QA/QC Requirements 	E-28/SV

Pesticides/PCBs (PEST) QA/QC Requirements 	E-47/PEST

IV ANALYTICAL STANDARDS 	E-65

V LABORATORY EVALUATION PROCEDURES 	E-67

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SECTION I

INTRODUCTION

The purpose of the Quality Assurance/Quality Control (QA/QC) program outlined
herein is the definition of procedures for the evaluation and documentation
of subsampling, analytical methodologies, and the reduction and reporting of
data. The objective is to provide a uniform basis for subsampling, sample
handling, Instrument conditions, methods control, performance evaluation, and
analytical data generation and reporting.

The scope of the program is for all laboratory operations (from sample
receipt, through analysis, to data reduction/reporting) applied to trace
organics samples. The scope includes those audit procedures used to evaluate
the application of the procedures defined within this QA/QC program.

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SECTION II
QA/QC STANDARD OPERATING PROCEDURES

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1.	The Contractor shall have a written QA/QC standard operating procedures
(SOP) which describes the in-house procedures that he employs to
guarantee, to the extent possible, the quality of all analysis
activities. It should describe the quality assurance and the quality
control procedures used during the analysis. Each Contractor should
prepare his own SOPs to suit the needs of his organization as he has
best determined. The QA/QC SOP should contain the essential elements
described in this section.

2.	Elements of a OA/OC SOP

2.1	All routine laboratory tasks should have written QA/QC Standard
Operating Procedures. Standard Operating Procedures should be detailed
documents describing who does what, when, where, how, and why. They
shall be sufficiently complete and detailed to ensure that:

2.1.1	Data of known quality and integrity are generated.

2.1.2	The loss of data due to out-of-control conditions is minimized.

2.2	Standard Operating Procedures shall be:

2.2.1 Adequate to establish the traceability of standards,
instrumentation, samples, and environmental data.

2.2.2	Simple, so a user with basic education, experience and/or
training can properly use them.

2.2.3	Complete enough so the user can follow the directions in a
stepwise manner.

2.2.4	Consistent with sound scientific principles.

2.2.5	Consistent with current EPA regulations, guidelines, and
contract requirements.

2.2.6	Consistent with the instrument manufacturer's specific
instruction manuals.

2.3	Standard Operating Procedures shall also provide for documentation
sufficiently complete to:

2.3.1	Record the performance of all tasks and their results.

2.3.2	Explain the cause of missing data.

2.3.3	Demonstrate the validation of data each time they are recorded
calculated, or transcribed.

2.4	To accomplish these objectives, Standard Operating Procedures should
address the major elements upon which the final quality of the
Contractor's work depends. In the following descriptions these six
major areas have been divided into sub-elements, where applicable.

These elements include but are not limited to:

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2.4.1

Organization and personnel,

2.4.2

Facilities and equipment,

2.4.3

Analytical methodology,

2.4.4

Sample custody procedures,

2.4.5

Quality control, and

2.4.6

Data handling.

3. Organization and Personnel

3.1	QA Policy and Objectives - Each organization should have a written
quality assurance policy that should be made known to all organization
personnel. Objectives should be established to produce data that meet
contract requirements in terms of completeness, precision, accuracy,
representativeness, documentation, and comparability. The SOP should
require the preparation of a specific QA plan for the analysis.

3.2	QA Organization - The organization and management of the QA function
should be described in the Contractor's SOP. Reporting relationships
and responsibilities should be clearly defined. A QA Coordinator or
Supervisor should be appointed and his responsibilities established. A
description of the QC paperwork flow should be available. There should
be a clear designation of those who are authorized to approve data and
results. Responsibilities for taking corrective action should be
assigned to appropriate management personnel.

3.3	Personnel training - It is highly desirable that there be a training
program for employees. This system should include motivation toward
producing data of acceptable quality and should involve "practice work"
by the new employee. The quality of this work can be immediately
verified and discussed by the supervisor, with appropriate corrective
action taken.

3.4	Document Control and Revisions. The SOP should include a system for

documenting:

3.4.1

Calibration procedures,

3.4.2

Analytical procedures,

3.4.3

Computational procedures,

3.4.4

Quality control procedures,

3.4.5

Bench data,

3.4.6

Operating procedures, or any changes to these procedures, and

3.4.7

Laboratory notebook policy.

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3.5 Procedures for making revisions to technical procedures or documents
must be clearly defined, with the lines of authority indicated.
Procedural revisions should be written and distributed to all affected
individuals, thus ensuring implementation of changes.

4.	Facilities and Equipment

4.1	Procurement and Inventory Procedures - Purchasing guidelines for all
equipment and reagents having an effect on data quality should be
well-defined and documented. Similarly, performance specifications
should be documented for all items of equipment having an effect on
data quality. Once any item which is critical to the analysis such as
an in situ instrument, or reagent is received and accepted by the
organization, documentation should be retained of the type, age, and
acceptance status of the item. Reagents should be dated upon receipt
in order to establish their order of use and to minimize the
possibility of exceeding their useful shelf life.

4.2	Preventive Maintenance - Preventive maintenance procedures should be
clearly defined and written for each measurement system and required
support equipment. When maintenance activity is necessary, it should
be documented on standard forms maintained in logbooks. A history of
the maintenance record of each system serves as an indication of the
adequacy of maintenance schedules and parts inventory.

5.	Analytical Methodology

5.1	Calibration and Operating Procedures - Calibration is the process of
establishing the relationship of a measurement system output to a known
stimulus. In essence, calibration is a reproducible reference point to
which all sample measurements can be correlated. A sound calibration
SOP should Include provisions for documentation of frequency,
conditions, standards, and records reflecting the calibration history
of a measurement system.

5.1.1 The accuracy of the calibration standards is an important point
to consider since all data will be in reference to the
standards used. An SOP for verifying the accuracy of all
working standards against primary grade standards should be
routinely followed.

5.2	Feedback and corrective action - The SOP should specify the corrective
action that is to be taken when an analytical or sampling error is
discovered or the analytical system is determined to be out of control.
The SOP should require documentation of the corrective action and
notification of the analyst of the error and correct procedures.

6.	Sample Cuafcndv

6.1 Sample custody is a part of any good laboratory or field operation.
Where samples may be needed for legal purposes, "chain-of-custody"
procedures, as defined in Exhibit F must be used. However, at a
minimum, the following sample custody procedures should be addressed in
the QA/QC SOP.

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6.2 Chain-of-custody In laboratory operations

6.2.1	Identification of responsible party to act as sample custodian
at the laboratory facility authorized to sign for incoming
field samples, obtain documents of shipment (e.g., bill of
lading number or mail receipt), and verify the data entered
onto the sample custody records.

6.2.2	Provision for a laboratory sample custody log consisting of
serially numbered standard lab-tracking report sheets.

6.2.3	Specification of laboratory sample custody procedures for
sample handling, storage and dispersement for analysis.

7. Pvality Control

7.1	Quality Control Procedures - The quality control procedures used during
analysis should be described and must conform to those described in
Exhibit E. The quality control checks routinely performed during
sample analysis include method blank analysis to establish analyte
levels, duplicate analysis to establish analytical precision, spiked
and blank sample analysis to determine analytical accuracy. The
frequency of these quality control checks are defined in the contract.
Limits of acceptance or rejection are also defined for analysis and
control charts should be used. Confirmation procedures should be
described in the SOP.

7.2	Control Checks and Internal Audits - A good SOP will make provision for
and describe control checks and internal audits by the Contractor.
Several approaches are used for control checks. These include:

7.2.1	Reference material analysis. Analytical reference materials
are available from several commercial and government sources,
or they may be prepared in-house. The chemical analysis of
theste materials has been well established. Such materials can
be analyzed alongside routine samples and the results used to
check the accuracy of analytical procedures.

7.2.2	Blank analysis. The procedures and the frequency of blank
analyses are defined in the contract.

7.2.3	Matrix spike and matrix spike duplicate analysis. The
procedures and the frequency of matrix spike analyses are
defined in the contract.

7.2.4	Internal audits. Internal audits should be periodically
conducted to evaluate the functioning of the QA SOP. This
involves an independent check of the performance of the
laboratory analysts to determine if prescribed procedures are
closely followed.

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8.

Data Handling

8.1	Data Handling, Reporting, and Recordkeeping - Data handling, reporting
and recordkeeping procedures should be described. Data handling
reporting includes all procedures used to record data on standard
forms, and in laboratory notebooks. The reporting format for

types of bench data should be described and the forms provided The
contents of notebooks should be specified.

8.1.1 Recordkeeping of this type serves at least two useful

functions: (1) it makes possible the reanalysis of a set of
data at a future time, and (2) it may be used in support of the
experimental conclusions if various aspects of the analv.l.
called into question.

8.2	Data Validation - Data validation procedures, defined ideally as a set
of computerized and manual checks applied at various appropriate level
of the measurement process, should be in written form and clearly
defined for all measurement systems.

8.2.1	Criteria for data validation must be documented and include
limits on:

8.2.1.1	Operational parameters such as GC conditions;

8.2.1.2	Calibration data;

8.2.1.3	Special checks unique to each measurement, e.g.,
successive values/averages;

8.2.1.4	Statistical tests, e.g., outliers; and

8.2.1.5	Manual checks such as hand calculations.

8.2.2	The limits defined in the contract ensure a high probability of
detecting invalid data for either all or the majority of the
measurement systems. The required data validation activities
(GC operating conditions, analytical precision, etc.) should be
recorded on standard forms in a logbook.

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SECTION III
VOLATILES QA/QC REQUIREMENTS

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This section outlines the minimum quality control (QC) operations necessary
to satisfy the analytical requirements associated with the determination of
volatile organic TCL compounds in water and soil/sediment samples. These QC
operations are as follows:

o	Documentation of GC/MS Mass Calibration and Abundance Pattern

o	Documentation of GC/MS Response Factor Stability

o	Internal Standard Response and Retention Time Monitoring

o	Method Blank Analysis

o	Surrogate Spike Response Monitoring

0	Matrix Spike and Matrix Spike Duplicate Analysis

1	- TUNING AND GC/MS MASS CALIBRATION
1. Summary

It is necessary to establish that a given GC/MS meets the standard mass
spectral abundance criteria prior to initiating any on-going data
collection. This is accomplished through the analysis of
p-Bromofluorobenzene (BFB).

Definition: The twelve (12) hour time period for GC/MS system tuning,
standards calibration (initial or continuing calibration criteria) and
method blank analysis begins at the moment of Injection of the BFB
analysis that the laboratory submits as documentation of a compliant
tune. The time period ends after twelve (12) hours has elapsed
according to the system clock.

1.1 p-Bromofluorobenzene (BFB)

1.1.1	Each GC/MS system used for the analysis of volatile TCL
compounds must be hardware tuned to meet the abundance criteria
listed in Table 1.1 for a maximum of a 50 nanogram injection of
BFB. Alternately, add 50 ng of BFB solution to 5.0 ml of
reagent water and analyze according to Exhibit D VOA, Section
IV. BFB shall not be analyzed simultaneously with any
calibration standards or blanks. This criterion must be
demonstrated daily or for each twelve-hour time period,
whichever is more frequent. If required, background subtraction
must be straightforward and designed only to eliminate column
bleed or instrument background ions. Background subtraction
actions resulting in spectral distortions for the sole purpose
of meeting the contract specifications are unacceptable.

NOTE: All instrument conditions must be identical to those used
in sample analysis, except that a different temperature program
may be used.

1.1.2	BFB criteria MUST be met before any standards, samples, or
blanks are analyzed. Any samples analyzed when tuning criteria

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have not been net nay require reanalysis aC no cost to the
Agency.

1.1.3 Whenever the Contractor takes corrective action which may

change or affect the tuning criteria for BFB (e.g., Ion source
cleaning or repair, etc.), the tune must be verified
Irrespective of the twelve-hour tuning requirements.

TABLE 1.1. BFB KEY IONS AND ABUNDANCE CRITERIA

Mass	Ion Abundance Criteria

SO	15.0-40.0 percent of the base peak

75	30.0-60.0 percent of the base peak

95	base peak, 100 percent relative abundance

96	5.0-9.0 percent of the base peak

173	less than 2.0 percent of mass 174

174	greater than 50.0 percent of the base peak

175	5.0-9.0 percent of mass 174

176	greater than 95.0 percent but less than 101.0
percent of mass 174

177	5.0 - 9.0 percent of mass 176

1.2 Documentation

The Contractor shall provide documentation of the calibration In the
form of a bar graph spectrum and as a mass listing.

1.2.1 The Contractor shall complete a Form V (GC/HS Tuning and Mass
Calibration) each time an analytical system Is tuned. In
addition, all standards, samples, blanks, matrix spikes, and
matrix spike duplicates analyzed during a particular tune must
be summarized In chronological order on the bottom of the
appropriate Form V. Detailed instructions for the completion
of Form V are in Exhibit B, Section III.

PART 2 - CALIBRATION OF THE GC/MS SYSTEM

2. Summary

Prior to the analysis of samples and required blanks and after timing
criteria have been met, the GC/MS system must be initially calibrated
at a minimum of five concentrations to determine the linearity of
response utilizing TCL compound standards. Once the system has been
calibrated, the calibration must be verified each twelve (12) hour time
period for"each GC/MS system.

2.1 Prepare calibration standards as described In Exhibit D VOA, Section
IV, to yield the following specific concentrations:

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2.1.1 Volatile TCL Coapounds

Initial calibration of volatile TCL coapounds ia required at
20, SO, 100, 150 and 200 ug/L. Surrogate and internal
standarda shall be used with each of the calibration standards.
Utilizing the analytical protocol specified in Exhibit D this
will result in 100-1000 total ng analyzed. If an analyte
saturate* at the 200 ug/L concentration level, and the GC/MS
systea is calibrated to achieve a detection sensitivity of no
less than 5 ug/L, the laboratory auat docuaent it in the Case
Narrative, and attach a quantitation report and RIC. In this
Instance, the laboratory should calculate the results based on
a four-point initial calibration for the specific analvta that
saturates. The use of separate calibration aeChods which
reflect the two different low and aadlua soil/sediaent aethods
is required. Secondary Ion quantitation is only allowed when
there are aaaple interferences with the prlaary ion. If
secondary ion quantitation is used, docuaent the reaaons in the
Case Narrative. Analyse all aethod blanks and standarda under
the saae conditions as the saaples.

2.2	The USEPA plans to develop perforaance based criteria for response
factor data acquired during this prograa. To accoapllsh this goal, the
Agency has specified both the concentration levels for initial
calibration and has also specified the specific internal standard to be
used on a compound-by-coapound basis for quantitation (see Table 2.1).
Establishment of standard calibration procedures is necessary and
deviations by the Contractor will not be allowed.

2.3	Analyze each calibration standard and tabulate the area of the priaary
characteristic ion (Exhibit D V0A, Table 3) against concentration for
each coapound including all contract required surrogate coapounds. The
relative retention tiaes of each coapound in each calibration run
should agree within 0.06 relative retention tlae units. Late eluting
coapounds usually will have auch better agreeaent.

Using Table 2.1 and Equation 2.1, calculate the relative response

factors (RRF) for each coapound at each concentration level.

RRF - -x-	Eq. 2.1

Ais °x

where,

Ax - Area of the characteristic ion for the coapound to be
aeasured.

Ais - Area of the characteristic ion for the specific Internal
standarda froa Table 2.1 or 2.2.

cis ~ Concentration of the Internal standard (ng/uL).

Cx - Concentration of the coapound to be aeasured (ng/uL).

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TABLE 2.1. VOLATILE INTERNAL STANDARDS WITH CORRESPONDING
TCL ANALYTES ASSIGNED FOR QUANTITATION

Broaochloroaethane	1,4-Difluorobenzene	Chlorobenzene-

ChloroiM thane
Bromome thane
Vinyl Chloride
Chioroe thane
Methylene Chloride
Acetone

Carbon Disulfide
1,1-Dichloroethene

1.1-Dichloroethane

1,2•Dichloroethene(tot
Chloroform

1.2-Dichloroethene
2-Butanone

1,2-Dichloroethane-d^
(aurr)

1.1.1-Trichloroethane
Carbon Tetrachloride
Vinyl Acetate
Broaodlchloroae thane
1,2-Dichloropropane
trans-1,3-Dichloropropene
Trichloroethene
Dibroaochloroaethane

1.1.2-Trichloroethane
,) Benzene

cis-1,3-Dichloropropene
Broaoforn

2-Hexanone

4-Me thy1-2-Pentanone
Tetrachloroethene

1,1,2,2-Tetrachloroethane

Toluene

Chlorobenzene

Ethylbenzene

Styrene

Xylene(total)

Bronofluorobenzene

(aurr)

Toluene-dg (surr)

(•urr) - surrogate compound

2.3.1 Using the relative response factors (RRF) from the initial

calibration, calculate the percent relative standard deviations
(%RSD) for compounds labeled on Form VI as Calibration Check
Compounds and shown in Table 2.2 (see 2.6.2), using Equation
2.2 below.

SD

%RSD - 	 X 100	Eq. 2.2

x

where,

RSD - Relative Standard Deviation

SD	— Standard Deviation of initial relative

response factors (per compound)

J L

'	N-l

r (x, - x)2

mean of initial relative response factors
(per compound)

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2.4

Th. »RSD for «»ch Individual CUbr.elon Ch.ck Compound «u.t be
liSA than or equal to 30.0 percent. This criteria	k-

for the initial calibration to be valid.

A system performance check iiuat be performed to ensure that minimum

average relative response factors are met before the calibration curve

IS USQd.

2.4.1 For volatiles, the five System Performance Check Compounds
(SPCCs) are: chloromethane, 1,1-dichloroethane, bromoform,
1,1,2,2-tetrachloroethane and chlorobenzene. Tha minimum
acceptable average relative response factor (RRF) for these
compounds is 0.300, 0.250 for Bromoform. These compounds
typically have RRFs of 0.4-0.6 and are used to check compound
instability and check for degradation caused by contaminated
lines or active sites in the system. For instance:

o Chloromethane - this compound is the most likely
compound to be lost if the purge flow is too fast.

o Bromoform - this compound is one of the compounds most
likely to be purged very poorly if the purge flow is too
slow. Cold spots and/or active sites in the transfer
lines may adversely affect response. Response of the
quantitation ion (m/z 173) is directly affected by the
tuning of BFB at ions m/z 174/176. Increasing the m/z
174/176 ratio may improve bromoform response.

o Tetrachloroethane, 1,1-Dichloroethane - These compounds
can be deteriorated by contaminated transfer lines in
purge and trap systems and/or active sites in trapping
materials.

2.4.2 The initial calibration is valid only after both the %RSD for

CCC compounds and the minimum RRF for SPCC have been met. Only
after both these criteria are met can sample analysis begin.

2.5 Documentation

Once the initial calibration is validated, calculate and report the
average relative response factor (RRF) and percent relative standard
deviation (%RSD) for all TCL compounds. The Contractor shall complete
and submit Form V (the GC/MS tune for the initial calibration) and Form
VI (Initial Calibration Data) for each instrument used to analyze
samples under this protocol. Detailed instructions for completion of
Form VI are in Exhibit B, Section III.

2.6 Continuing Calibration

A calibration standard(s) containing all volatile TCL compounds,
including all required surrogates, Bust be performed each twelve hours
during analysis (see definition of twelve hour time period, paragraph
1 of this Section). Compare the relative response factor data from
the standards each twelve hours with the average relative response

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factor fron the initial calibration for a specific instrument. A
system performance chaek must ba made aach twelve hours. If the SFCC
critarla ara mat, a comparison of relative response factors is made for
all conpounds. This is the iim ehack that ia applied during the
initial calibration (Fora VI). If the alninun relative response
factors ara not set, the system must ba evaluated and corrective action
Bust be taken before sample analysis begins.

2.6.1	Some possible problems are standard mixture degradation,
injection port inlat contamination, contamination at the front
end of the analytical column, and active sites in the column or
chromatography system. This check must be met before analysis
begins. The minimum relative response factor (RRF) for
volatile System Performance Check Compounds (SFCC) is 0.300
(0.250 for Bromoform).

2.6.2	Calibration Check Compounda (CCC)

After the system performance check is met, Calibration Check
Compounds listed in Table 2.2 are used to check the validity of
the initial calibration. Calculate the percent difference
using Equation 2.3.

SRFt - RRFC

« Difference - 			 x 100 Eq. 2.3

SRFX

where

BRFf - average ralatlve response factor from initial
calibration

RRFe - relative response factor from current
calibration check standard

2.6.2.1 If the percent difference for any compound is

greater than 20%, the laboratory should consider
this a warning limit. If the percent difference for
each CCC Is lass than or equal to 25.0%, the initial
calibration la assumed to be valid. If the criteria
are not met (>25.0% difference), for any one
calibration check compound, corrective action MUST
be taken. Problems similar to those listed under
SPCC could affect this criteria. If no source of
the problem can be determined after corrective
action has been taken, a new Initial five point
calibration MOST ba generated. These criteria MUST
be met before ssmple analysis begins.

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TABLE 2.2 VOLATILE CALIBRATION CHECKCOMPOUNDS

1.1-Dichloroethene
Chloroform

1.2-Dichloropropane
Toluene
Ethylbenzene
Vinyl Chloride

2.6.3 Concentration Levels for Continuing Calibration Check

The USEPA plans to evaluate the long term stability of relative
response factors during this progran. Standardization among
contract laboratories is necessary to reach these long term
goals. Along with contract specified concentrations for initial
calibration, the USEPA is requiring specific concentrations for
each continuing calibration standard(s).

2.6.3.1 The concentration for each volatile TCL compound in
the continuing calibration standard(s) is 50 ug/L.

2.7 Documentation

The Contractor shall complete and submit a Form VII for each GC/MS syst
utilized for each twelve hour time period. Calculate and report the ^
relative response factor and percent difference («D) for all compounds
Ensure that the minimum RRF for volatile SPCCs is 0.300 «nd 0.250 for
Bromoform. The percent difference (%D) for each CCC compound must be
less than or equal to 25.0 percent. Additional instructions for
completing Form VII are in Exhibit B, Section III.

FART.2 - METHOD BLANK ANALYSIS

3. Summary

3.1

3.2

3.1.1

A method blank is a volume of deionized, distilled laboratory water f
water samples, or a purified solid matrix for soil/sediment samples °r
carried through the entire analytical scheme. The method blank volum
weight must be approximately equal to the sample volumes or sample ' °T

weights being processed.

Method blank analysis must be performed at the following frequency -

For the analysis of volatile TCL compounds, a method blank
analysis must be performed once for each 12-hour time period
See Part 1, paragraph 1 for the definition of the 12-hour time
period. The method blank 0UC£ be analyzed after the calibratio

standard(s).	n

It is the Contractor's responsibility to ensure that method interferon
caused by contaminants in solvents, reagents, glassware, and other samel*
processing hardware that lead to discrete artifacts and/or elevated *
baselines in gas chromatograms be minimized.

S-17/™	Rev. 9/88
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3.2.1	For the purposes of this protocol, an acceptable laboratory
method blank should meet the criteria of paragraphs 3.2.1.1 and
3.2.1.2.

3.2.1.1	A method blank for volatile analysis must contain
less than or equal to five times (5X) the Contract
Required Quantitation Limit (CRQL from Exhibit C) of
methylene chloride, acetone, toluene, and
2-butanone.

3.2.1.2	For all other TCL compounds not listed above, the
method blank must contain less than or equal to the
Contract Required Quantitation Limit of any single
TCL analyte.

3.2.2	If a laboratory method blank exceeds these criteria, the
Contractor must consider the analytical system to be out of
control. The source of the contamination must be investigated
and appropriate corrective measures MUST be taken and
documented before further sample analysis proceeds. All
samples processed with a method blank that is out of control
(i.e., contaminated) MUST be reextracted/repurged and
reanalyzed at no additional cost to the Agency. The Laboratory
Manager, or his designee, must address problems and solutions
in the Case Narrative (Exhibit B).

~.3	Documentation

The Contractor shall report results of method blank analysis using the
Organic Analysis Data Sheet (Form I) and the form for tentatively
identified compounds (Form I, TIC). In addition, the samples
associated with each method blank must be summarized on Form IV (Method
Blank Summary). Detailed instructions for the completion of these
forms can be found in Exhibit B, Section III.

3.3.1 The Contractor shall report All, sample concentration data as
UNCORRECTED for blanks.

Mil - SURROGATE SPIKE fSSl ANALYSIS

~.

Surrogate standard determinations are performed on all samples and
blanks. All samples and blanks are fortified with surrogate spiking
compounds before purging or extraction in order to monitor preparation
and analysis of samples.

4.1 Each sample, matrix spike, matrix spike duplicate, and blank are spiked
with surrogate compounds prior to purging or extraction. The surrogate
spiking compounds shown in Table 4.1 are used to fortify each sample,
matrix spike, matrix spike duplicate, and blank with the proper
concentrations. Performance based criteria are generated from
laboratory results. Therefore, deviations from the spiking protocol
will not be permitted.

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TABLE 4.1 SURROGATE SPIKING COMPOUNDS

Compounds

Amount in Sample/Extract*
	(before anv ootional dilution^

Fraction

Vater Low/Medium Soil

Toluene-dg VOA
4-Bromofluorobenzene VOA
l,2-Dichloroethane-d4 VOA

50 ug 50 ug
50 ug 50 ug
50 ug 50 ug

* At the time of injection.



4.2 Surrogate spike recovery must be evaluated by determining whether the
concentration (measured as percent recovery) falls inside the contract
required recovery limits listed in Table 4.2.

TABLE 4.2 CONTRACT REQUIRED SURROGATE SPIKE RECOVERY LIMITS

Fraction Surrogate Compound

Vater Low/Medium Soil

VOA	Toluene-dg	88-110	81-117

VOA	4-Bromofluorobenzene	86-115	74-121

VOA	lt2-Dichloro«thane-d^	76-114	70-121

4.3 Treatment of surrogate spike recovery information Is according to
paragraphs 4.3.1 through 4.3.2.

4.3.1 Method Blank Surrogate Spike Recovery

The laboratory must take the actions listed below if recovery
of any one surrogate compound in the volatiles fraction of the
method blank is outside of the required surrogate spike
recovery limits.

4.3.1.1	Check calculations to ensure that there are no
errors; check internal standard and surrogate
spiking solutions for degradation, contamination,
etc; also check instrument performance.

4.3.1.2	Reanalyze the blank or extract if steps in 4.3.1.1
fail to reveal the cause of the noncompliant
surrogate recoveries.

4.3.1.3	If the blank is a methanol extract for medium level
soil samples, reextract and reanalyze the blank if
steps in 4.3.1.2 fall to reveal the cause of the
noncompliant surrogate recoveries.

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4.3.1.4 If the measures listed in 4.3.1.1 thru 4.3.1.3 fail
to correct the problem, the analytical system must
be considered out of control. The problem MUST be
corrected before continuing.

This may mean recalibrating the instrumentation but
it may also mean more extensive action. The
specific corrective action is left up to the GC/MS
operator. When surrogate recovery(ies) in the blank
is outside of the contract required windows, all
samples associated with that blank MUST be
reanalyzed at no additional cost to the Agency.

4.3.2 Sample Surrogate Spike Recovery

The laboratory must take the actions listed below if recovery
of any one surrogate compound in the volatiles fraction of the
sample is outside of the contract surrogate spike recovery
limits.

4.3.2.1 The Contractor laboratory shall document (in this
instance, document means to write down and discuss
problem and corrective action taken in the Case
Narrative (see Exhibit B) deviations outside of
acceptable quality control limits by taking the
following actions:

4.3.2.1.1	Check calculations to ensure that there
are no errors; check internal standard
and surrogate spiking solutions for
degradation, contamination, etc; also
check instrument performance.

4.3.2.1.2	If the steps in 4.3.2.1.1 fail to
reveal a problem, then reanalyze the
sample or extract. If reanalysis of the
sample or extract solves the problem,
then the problem was within the
laboratory's control. Therefore, only
submit data from the analysis with
surrogate spike recoveries within the
contract windows. This shall be
considered the initial analysis and
shall be reported as such on all data
deliverables.

4.3.2.1.3	If the sample was a soil extracted with
methanol and the steps in 4.3.2.1.2
fail to solve the problem, then
reextract and reanalyze the sample. If
the reextraction and reanalysis solves
the problem, then the problem was in
the laboratory's control. Therefore,
only submit data from the extraction

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and analysis with surrogate spike
recoveries within the contract windows.
This shall be considered the initial
analysis and shall be reported as such
on all data deliverables.

4.3.2.1.4 If the reextraction and/or reanalysis
of the sample does not solve the
problem; i.e., surrogate recoveries are
outside the contract windows for both
analyses, then submit the surrogate
spike recovery data and the sample data
from both analyses according to
paragraph 4.4. Distinguish between the
initial analysis and the reanalysis on
all data deliverables, using the sample
suffixes specified in Exhibit B.

4.4 Documentation

The Contractor is required to report surrogate recovery data for the
following:

o	Method Blank Analysis

o	Sample Analysis

o	Matrix Spike/Matrix Spike Duplicate Analyses

o	All sample reanalyses that substantiate a matrix effect

The surrogate spike recovery data are summarized on the Surrogate Spike
Percent Recovery Summary (Form II). Detailed instructions for the
completion of Form II are in Exhibit B, Section III.

PARI 5 - MATRIX SPIKE/MATRIX SPIKE DUPLICATE ANALYSIS (MS/MSD^

5.	Summary

In order to evaluate the matrix effect of the sample upon the
analytical methodology, the USEPA has developed the standard mixes
listed in Table 5.1 to be used for matrix spike and matrix spike
duplicate analyses. These compounds are subject to change depending
upon availability and suitability for use as matrix spikes.

5.1 MS/MSD Frequency of Analysis

A matrix spike and matrix spike duplicate must be performed for each
group of samples of a similar matrix, once:

o each Case of field samples received, OR

o each 20 field samples in a Case, OR

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o each group of field samples of a similar concentration level
(soils only), OR

o each 14 calendar day period during which field samples in a
Case were received (said period beginning with Che receipt of
the first sample in that Sample Delivery Group)t

wMehavar is most frequent.

5.2 Use the compounds listed in Table 5.1 to prepare matrix spiking

solutions according to protocols described in Exhibit D VOA. The
analytical protocols in Exhibit D VOA stipulate the amount of matrix
splicing solution to be added to the sample aliquots. Each method
allows for optional dilution steps which must be accounted for when
calculating percent recovery of the matrix spike and matrix spike
duplicate samples.

TABLE 5.1. MATRIX SPIKING SOLUTIONS

Volatlles

Chlorobenzene	1,1-Dichloroethene

Toluene	Trichloroethene

Benzene

5.2.1 Samples requiring optional dilutions and chosen as the matrix
spike/ matrix spike duplicate samples, must be analyzed at the
same dilution as the original unsplked sample.

5.3	Individual component recoveries of the matrix spike are calculated
using Equation 5.1.

Matrix Spike	SSR - SR

Percent Recovery			x 100 Eq. 5.1

SA

where,

SSR — Spike Sample Results

SR - Sample Result

SA — Spike Added From Spiking Mix

5.4	Relative Percent Difference (RPD)

The Contractor is required to calculate the relative percent difference
between the matrix spike and matrix spike duplicate. The relative
percent differences (RPD) for each component are calculated using
Equation 5.2.

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Di - D2

RPD -		 X 100	Eq. 5.2

/2

where,

RPD - Relative Percent Difference

D^ - First Sample Value

~ Second Sample Value (duplicate)

5.5 Documentation

The matrix spike (MS) results (concentrations) for nonspiked volatile
TCL compounds shall be reported on Form I (Organic Analysis Data Sheet)
and the matrix spike percent recoveries shall be summarized on Form III
(MS/MSD Recovery). These values will be used by EPA to periodically
update existing performance based QC recovery limits (Table 5.2).

The results for nonspiked volatile TCL compounds in the matrix spike
duplicate (MSD) analysis shall be reported on Form I (Organic Analysis
Data Sheet) and the percent recovery and the relative percent
difference shall be summarized on Form III (MS/MSD Recovery). The RPD
data will be used by EPA to evaluate the long term precision of the
analytical method. Detailed instructions for the completion of Form III
are in Exhibit B, Section III.

TABLE 5.2. MATRIX SPIKE RECOVERY LIMITS

Fraction

Matrix Spike Compound

Water

Soil/Sediment

VOA

1,1-Dichloroethene

61-145

59-172

v6a

Trichlorethene

71-120

62-137

VOA

Chlorobenzene

75-130

60-133

VOA

Toluene

76-125

59-139

VOA

Benzene

76-127

66-142

PART S - SAMPLE ANALYSIS

The intent of Part 6 is to provide the Contractor with a brief summary
of ongoing QC activities involved with sample analysis. Specific
references are provided to help the Contractor meet specific reporting
and deliverables requirements of this contract.

6.1 Sample Analysis

Samples can be analyzed upon successful completion of the initial QC
activities. When twelve (12) hours have elapsed since the Initial tune

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was completed, it is necessary to conduct an instrument tune and
calibration check analysis (described in Part 2 of this Section). Any
major system maintenance, such as a source cleaning or installation of
a new column, may necessitate a retune and recalibration irrespective
of the twelve-hour requirement (see Initial Calibration, Part 2).

Minor maintenance should necessitate only the calibration verification
(Continuing Calibration, Part 2)

6.1.1 Internal Standards Evaluation - Internal standard responses and
retention times in all samples must be evaluated immediately
after or during data acquisition. If the retention time for
any internal standard changes by more than 30 seconds, the
chromatographic system must be inspected for malfunctions, and
corrections made as required. The extracted ion current
profile (EICP) of the internal standards must be monitored and
evaluated for each sample, blank, matrix spike, and matrix
spike duplicate. The criteria are described in detail in the
instructions for Form VIII, Internal Standard Area Summary (see
Exhibit B, Section III). If the extracted ion current profile
(EICP) area for any internal standard changes by more than a
factor of two (-50* to 100%), from the latest daily (12 hour
time period) calibration standard, the mass spectrometric
system must be inspected for malfunction, and corrections made
as appropriate. Breaking off 1 foot of the column (when using
capillary column) or cleaning the injector sleeve (when using
either packed or capillary column) will often improve high end
sensitivity for the late eluting compounds; repositioning or
repacking the front end of the column will often improve front
end column performance. Poor injection technique can also lead
to variable IS ratios. When corrections are made, re-analysis
of samples analyzed while the system was malfunctioning is
necessary.

6.1.1.1	If after reanalysis, the EICP areas for all internal
standards are Inside the contract limits (-50% to
+100%), then the problem with the first analysis is
considered to have been within the control of the
laboratory. Therefore, only submit data from the
analysis with EICPs within the contract limits.

This is considered the initial analysis and must be
reported as such on all data deliverables.

6.1.1.2	If the reanalysis of the sample does not solve the
problem, i.e., the EICP areas are outside the
contract limits for both analyses, then submit the
EICP data and sample data from both analyses.
Distinguish between the initial analysis and the
reanalysis on all data deliverables, using the
sample suffixes specified in Exhibit B. Document in
the Case Narrative all inspection and corrective
actions taken.

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6.1.2 Each Analytical run must also be checked for saturation. The
level at which an individual compound will saturate the
detection system is a function of the overall system
sensitivity and the mass spectral characteristics of that
compound. The initial method calibration (Part 2) requires
that the system should not be saturated for high response
compounds at 200 ug/L for VOA TCL compounds.

6.1.2.1 If the on-column concentration of any compound in
any sample exceeds the initial calibration range,
that sample must be diluted, the internal standard
concentration readjusted, and the sample reinjected,
as described in specific methodologies in Exhibit D
VOA. Note: For total xylenes, where three isomers
are quantified as two peaks, the calibration of each
peak should be considered separately, i.e., a
diluted analysis is not required for total xylenes
unless the concentration of either peak separately
exceeds 200 ug/L. Secondary ion quantitation is
only allowed when there are sample matrix
interferences with the primary ion. If secondary
ion quantitation is performed, document the reasons
in the Case Narrative.

6.1.2.2 If the dilution of the sample causes any compound

detected in the first analysis to be undetectable in
the second analysis, then the results of both
analyses shall be reported on separate Forms I,
according to the instructions in Exhibit B.

6.1.3 Qualitative Analysis

The compounds listed in the Target Compound List (TCL), Exhibit
C, shall be identified by an analyst competent in the
interpretation of mass spectra, by comparison of the suspect
mass spectrum to the mass spectrum of a standard of the
suspected compound. Two criteria must be satisfied to verify
the Identifications: (1) elutlon 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 (Exhibit D, Section IV).

6.1.3.1 For establishing correspondence of the GC relative
retention time (RRT), the sample component RRT must
compare within ±0.06 RRT units of the RRT of the
standard component. For reference, the standard must
be run on the same shift as the sample.

6.1.3.2 For comparison of standard and sample component mass
spectra, mass spectra obtained on the Contractor's
GC/MS are required. The BFB tuning requirements
listed in Part 1 of this Section must be met on that
same GC/MS.

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6.1.3.2.1 The requirements for qualitative

verification by comparison of mass
spectra are as follows:

o All ions present in the standard

mass spectra at a relative intensity
greater than 10% (most abundant ion
in the spectrum equals 100%) must be
present in the sample spectrum.

o The relative intensities of ions
specified in the above paragraph
must agree within ±20% between the
standard and sample spectra.

o Ions greater than 10% in the sample
spectrum but not present in the
standard spectrum must be considered
and accounted for by the analyst
making the comparison. When GC/MS
computer data processing programs
are used to obtain the sample
component spectrum, both the
processed and the raw spectra must
be evaluated. In Task III, the
verification process should favor
false positives (Exhibit D, Section
IV).

6.1.3.2.2 If a compound cannot be verified by all
of the criteria in 6.1.3.2.1, but in
the technical judgement of the mass
spectral interpretation specialist the
identification is correct, the
Contractor shall report the
identification and proceed with the
quantitation.

6.1.3.3 A library search shall be executed for nonsurrogate
and non-TCL sample components for the purpose of
tentative identification. For this purpose, the
1985 or most recent available version of the
National Bureau of Standards Mass Spectral Library,
containing 42,261 spectra should be used.

6.1.4 Quantitation

6.1.4.1 TCL components identified shall be quantitated by
the internal standard method. The internal
standards used shall be the ones assigned in Table
2.1 of this Section. The EICP area of characteristic
ions of TCL analytes are used (Exhibit D VOA,

Section IV).

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6.1.4.2	An estimated concentration for non-TCL components
tentatively identified shall be quantitated by the
internal standard method. For quantification, the
nearest internal standard free of Interferences must
be used.

6.1.4.3	Calculate surrogate standard recovery (see Fart 4)
for all surrogate compounds in all samples, blanks,
matrix spikes, and matrix spike duplicates. If
recovery is within contractual limits, report on
Form II (see Exhibit B). If recovery is outside
contractual limits, take specific steps listed in
Surrogate Spike Recoveries (Part 4).

6.1.4.4	Calculate matrix spike and matrix spike duplicate
percent recovery (see Part 5 of this Section) for
all compounds and report results on Form III (see
Exhibit B). Calculate Relative Percent Differences
(RPDs) for all matrix spiking compounds and report
results on Form III. Ensure that the proper
frequency of MS/MSD analysis is maintained.

6.1.5 Reporting and Deliverables

Refer to Exhibit B of this Statement of Work for specific
details on contract deliverables and reporting formats.

Exhibit B contains specific instructions for completing all
required•Forms, as well as a detailed itemization of reporting
and deliverables requirements. Exhibit H contains the format
requirements for delivery of data in computer-readable format.

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SECTION III SV

S EMIVOLATILES QA/QC
REQUIREMENTS

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This Section outlines the minimum quality control (QC) operations necessary
to satisfy the analytical requirements associated with the determination of
semivolatile organic TCL compounds in water and soil/sediment samples. These
QC operations are as follows:

o Documentation of GC/MS Mass Calibration and Abundance Pattern
o Documentation of GC/MS Response Factor Stability
o Internal Standard Response and Retention Time Monitoring
o Method Blank Analysis
o Surrogate Spike Response Monitoring
o Matrix Spike and Matrix Spike Duplicate Analysis

PART 1 - TUNING AND GC/MS MASS CALIBRATION

1. Summary

It is necessary to establish that a given GC/MS meets the standard mass
spectral abundance criteria prior to initiating any on-going data
collection. This is accomplished through the analysis of
Decafluorotriphenylphosphine (DFTPP).

Definition: The twelve (12) hour time period for GC/MS system tuning
and standards calibration (initial or continuing calibration criteria)
begins at the moment of injection of the DFTPP analysis that the
laboratory submits as documentation of a compliant tune. The time
period ends after twelve (12) hours has elapsed according to the system
clock.

1.1 Decafluorotriphenylphosphine (DFTPP)

1.1.1	Each GC/MS system used for the analysis of semivolatile or
pesticide TCL compounds must be hardware tuned to meet the
abundance criteria listed in Table 1.2 for a 50 ng injection of
decafluorotriphenylphosphine (DFTPP). DFTPP may be analyzed
separately or as part of the calibration standard. The
criteria must be demonstrated daily or for each twelve (12)
hour period, whichever is more frequent, before samples can be
analyzed. DFTPP must be Injected to meet this criterion. If
required, background subtraction must be straightforward and
designed only to eliminate column bleed or instrument
background ions. Background subtraction actions resulting in
spectral distortions for the sole purpose of meeting the
contract specifications are unacceptable. NOTE: All
instrument conditions must be identical to those used in sample
analysis, except that a different temperature program may be
used.

1.1.2	Whenever the Contractor takes corrective action which may
change or affect the tuning criteria for DFTPP (e.g., ion
source cleaning or repair, etc.), the tune must be verified
irrespective of the 12-hour tuning requirements.

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TABLE 1.2. DFTPP KEY IONS AND ION ABUNDANCE CRITERIA

Mass Ion Abundance Criteria

51	30.0 - 60.0 percent of mass 198

68	less than 2.0 percent of mass 69

70	less than 2.0 percent of mass 69

127	40.0 - 60.0 percent of mass 198

197	less than 1.0 percent of mass 198

198	base peak, 100 percent relative abundance

199	5.0 - 9.0 percent of mass 198
275	10.0 - 30.0 percent of mass 198

365	greater than 1.00 percent of mass 198

441	present but less than mass 443

442	greater than 40.0 percent of mass 198

443	17.0 • 23.0 percent of mass 442

1.2 Documentation

The Contractor shall provide documentation of the calibration in the
form of a bar graph spectrum and as a mass listing.

1.2.1 The Contractor shall complete a Form V (GC/MS Tuning and Mass
Calibration) each time an analytical system is tuned. In
addition, all samples, standards, blanks, matrix spikes, and
matrix spike duplicates analyzed during a particular tune must
be summarized in chronological order on the bottom of the
appropriate Form V. Detailed instructions for the completion
of Form V are found in Exhibit B, Section III.

PART 2 - CALIBRATION OF THE CC/MS SYSTEM

2. Summary

Prior to the analysis of samples and required blanks and after tuning
criteria have been met, the GC/MS system must be initially calibrated
at a minimum of five concentrations to determine the linearity of
response utilizing TCL compound standards. Once the system has been
calibrated, the calibration must be verified each twelve (12) hour time
period for each GC/MS system.

2.1 Prepare calibration standards as described in Exhibit D SV, Section IV,
to yield the following specific concentrations:

2.1.1 Semivolatile TCL Compounds

Initial calibration of semivolatile TCL compounds is required
at 20, 50, 80, 120, and 160 total nanograms. If an analyte
saturates at the 160 total nanogram concentration level, and
the GC/MS system is calibrated to achieve a detection
sensitivity of no less than the CRQL, the laboratory must
document it on Form VI and in the Case Narrative, and attach a
quantitation report and RIC. In this instance, the laboratory

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should calculate the results based on a four-point initial
calibration for the specific analvte. The use of a secondary
ion for quantitation is only allowed when there are sample
interferences with the primary ion. If secondary ion
quantitation is performed, document the reasons in the Case
Narrative. Nine compounds: Benzoic Acid, 2,4-Dinitrophenol,
2,4,5-Trichlorophenol, 2-Nitroaniline, 3-Nitroaniline,
4-Nitroaniline, 4-Nitrophenol, 4,6-Dinitro-2-Methylphenol, and
Pentachlorophenol will only require a four-point Initial
calibration at 50, 80, 120, and 160 total nanograms since
detection at less than 50 nanograms per injection is difficult.

2.2	The USEFA plans to develop performance based criteria for response
factor data acquired during this program. To accomplish this goal, the
Agency has specified both the concentration levels for initial
calibration and has also specified the specific internal standard to be
used on a compound-by-compound basis for quantitation (Table 2.2).
Establishment of standard calibration procedures is necessary and
deviations by the Contractor will not be allowed.

2.3	Analyze each calibration standard and tabulate the area of the primary
characteristic ion (Exhibit D SV, Table 4) against concentration for
each compound including all contract required surrogate compounds. The
relative retention times of each compound in each calibration run
should agree within 0.06 relative retention time units. Late eluting
compounds usually will have much better agreement.

Using Table 2.2, calculate the relative response factors (RRF) for each
compound at each concentration level using Equation 2.1.

Ajc Cls

RRF - _ x —	Eq. 2.1

Ais cx

where,

Ax - Area of the characteristic ion for the compound to be
measured.

A^g - Area of the characteristic ion for the specific internal

standards from Table 2.1 or 2.2.

Cl8 - Concentration of the internal standard (ng/uL).
Cx — Concentration of the compound to be measured (ng/uL).

2.3.1 Using the relative response factors (RRF) from the initial

calibration, calculate the percent relative standard deviations
(%RSD) for compounds labeled on Form VI as Calibration Check
Compounds and shown in Table 2.3 (see 2.6.2) using Equation
2.2.

%RSD - SD X 100	Eq. 2.2

"x

where,

RSD - Relative Standard Deviation

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SD — Standard Deviation of initial response factors
(per compound)

where: SD —

N-l

x - mean of initial relative response factors (per
compound)

The %RSD for each individual Calibration Check Compound must be
less than or equal to 30.0 percent. This criteria must be met
for the initial calibration to be valid.

2.4	A system performance check must be performed to ensure that minimum
average relative response factors are met before the calibration curve
is used.

2.4.1	For semivolatiles, the System Performance Check Compounds
(SPCCs) are: N-Nitroso-Di-n-Propylamine,

Hexachlorocyclopentadiene, 2,4-Dinitrophenol and 4-Nitrophenol.
The minimum acceptable average relative response factor (RRF)
for these compounds is 0.050. SPCCs typically have very low
RRFs (0.1-0.2) and tend to decrease in response as the
chromatographic system begins to deteriorate or the standard
material begins to deteriorate. These compounds are usually
the first to show poor performance. Therefore, they must meet
the minimum requirement when the system is calibrated.

2.4.2	The initial calibration is valid only after both the %RSD for
CCC compounds and the minimum RRF for SPCC have been met. Only
after both these criteria are met can sample analysis begin.

2.5	Documentation

Once the initial calibration is validated, calculate and report the
average relative response factor (REP) and percent relative standard
deviation (%RSD) for all TCL compounds. The Contractor shall complete
and submit Form V (the GC/MS tune for the initial calibration) and Form
VI (Initial Calibration Data) for each instrument used to analyze
samples under this protocol. Detailed instructions for completion of
Form VI are in Exhibit B, Section III.

2.6	Continuing Calibration

A calibration standard(s) containing all semivolatile TCL compounds,
including all required surrogates, must be analyzed each twelve hours
during analysis (see definition of twelve hour time period, paragraph
1. of this Section). Compare the relative response factor data from
the standards each twelve hours with the average relative response
factor from the initial calibration for a specific instrument. A
system performance check must be made each twelve hours. If the SPCC

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TABLE 2.2. SEMIVOLATILE INTERNAL STANDARDS WITH CORRESPONDING TCL ANALYTES ASSIGNED FOR QUANTITATION

1,4-Dichlorobenzene-d^ Naphthalene-dg Acenaphthene-d^Q Phenanthrene-d^Q Chrysene-d^ Perylene-d^

Phenol

bis(2-Chloroethyl)
ether

2-Chlorophenol

1.3-Dichlorobenzene

1.4-Dichlorobenzene
Benzyl Alcohol

1,2 •Dichlorobenzene
2-Hethylphenol
bis(2-Chlorolso-

propyl)ether
4-Hethylphenol
N-nitroso-Di-n-

propylaaine
Hexachloroethane
2-Fluorophenol

(surr)

Phenol-dg (surr)

Nitrobenzene
Isophorone
2-Nitrophenol
2,4-Diaethyl-
phenol
Benzoic acid
bis(2-Chloro-
ethoxy)aethane
2,4-Dichloro-
phenol

1,2,4-Trichloro-
benzene
Naphthalene
4-Chloroaniline
Hexachloro-
butadiene
4-Chloro-3-
nethylphenol
2-Methylnaphth-

alene
Nitrobenzene-dj
(surr)

Hexachlorocyclo•
pentadiene
2,4,6-Trichloro-
phenol

2.4.5-Trichloro-
phenol

2-Chloronaphthalene

2-Nitroaniline
Diaethyl Phthalate
Acenaphthylene

3-Nitroaniline
Acenaphthene
2,4-Dinitrophenol

4-Nitrophenol
Dibenzofuran

2,4-Dinitrotoluene
2,6-Dinitrotoluene
Diethyl Phthalate
4-Chloropheny1
phenyl ether
Fluorene
4-Nitroaniline
2 * Fluorobiphenyl
(surr)

2.4.6-Tribrono
Phenol (surr)

4,6-Dinitro-2-
¦ethylphenol
N-nitrosodi-
phenylaaine
1,2-Diphenylhy-
drazine
4-Bronophenyl
Phenyl Ether
Hexachloro-
benzene
Pentachloro-
phenol
Phenanthrene
Anthracene
Di-n-butyl
Phthalate
Fluoranthene

Pyrene
Butylbenzyl
Phthalate
3,3'-Dichloro-
benzidine
Benzo(a)*

anthracene
bis(2•ethylhexy1)

Phthalate
Chrysene
Terphenyl-dj^
(surr)

Di-n-octyl
Phthalate
Benzo (b ) f luor -

anthene
Benzo(k)fluor-
anthene
Benzo(a)pyrene
Indeno(1,2,3-cd)

pyrene
Dibenz(a,h)
anthracene
Benzo(g,h,i)
perylene

Surr - surrogate conpound
-------
criteria are net, a comparison of relative response factors is made for
all compounds. This is the same check that is applied during the
initial calibration (Form VI). If the minimum relative response
factors are not met, the system must be evaluated and corrective action
must be taken before sample analysis begins.

2.6.1 Some possible problems are standard mixture degradation,

injection port inlet contamination, contamination at the front
end of the analytical column, and active sites in the column or
chromatography system. This check must be met before analysis
begins. The minimum relative response factor (RRF) for
semivolatile System Performance Check Compounds (SPCC) is
0.050.

2.6.2 Calibration Check Compounds (CCC)

After the system performance check is met, Calibration Check
Compounds listed in Table 2.3 are used to check the validity of
the initial calibration. Calculate the percent difference
using Equation 2.3.

RRFj - RRFC

% Difference - 			 x 100	Eq. 2.3

where,

RRFX

RRFj - average response factor from initial
calibration.

RRFC - response factor from current verification check
standard.

2.6.2.1 If the percent difference for any compound is

greater than 20%, the laboratory should consider
this a warning limit. If the percent difference for
each CCC is less than or equal to 25.0%, the initial
calibration is assumed to be valid. If the criteria
are not met (>25.0% difference), for any one
calibration check compound, corrective action MUST
be taken. Problems similar to those listed under
SPCC could affect this criteria. If no source of
the problem can be determined after corrective
action has been taken, a new initial five point
calibration MUST be generated. These criteria MUST
be met before sample analysis begins.

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TABLE 2.3. CALIBRATION CHECK COMPOUNDS

Base/Neutral Fraction	Acid Fraction

Acenaphthene

1,4-Dichlorobenzene

Hexachlorobutadiene

N-Nitroso-di-n-phenylanine

Di-n-octylphthalate

Fluoranthene

Benzo(a)pyrene

4-Chloro-3-Methylphenol
2,4-Dichlorophenol
2-Nitrophenol
Phenol

Pentachlorophenol
2,4,6-Trichlorophenol

2.6.3 Concentration Levels for Continuing Calibration Check

The USEPA plans to evaluate the long tern stability of response
factors during this program. Standardization among contract
laboratories is necessary to reach these long term goals. Along
with contract specified concentrations for initial calibration,
the USEPA is requiring specific concentrations for each
continuing calibration standard(s).

2.6.3.1 The concentration for each semivolatile TCL compound
in the continuing calibration standard(s) is 50
total nanograms for all compounds.

2.7 Documentation

The Contractor shall complete and submit a Form VII for each GC/MS
system utilized for each twelve hour time period. Calculate and report
the relative response factor and percent difference (tD) for all
compounds. Ensure that the minimum RRF for semivolatile SPCCs is
0.050. The percent difference (%D) for each CCC compound must be less
than or equal to 25.0 percent. Additional instructions for completing
Form VII are found in Exhibit B, Section III.

PART 3 - METHOD BLANK ANALYSIS

3. Summary

A method blank is a volume of deionized, distilled laboratory water for
water samples, or a purified solid matrix for soil/sediment samples,
carried through the entire analytical scheme (extraction,
concentration, and analysis). For soil/sediment samples, a solid
matrix suitable for semivolatile analyses is available from EMSL/LV.
The method blank volume or weight must be approximately equal to the
sample volumes or sample weights being processed.

3.1 Method blank analysis must be performed at the following frequency.

3.1.1 For the analysis of semivolatile TCL compounds, a method blank
analysis must be performed once:

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o each Case, OR

o each 14 calendar day period during which samples In a Case
are received (said period beginning with the receipt of the
first sample in that Sample Delivery Group), OR

o each 20 samples in a Case, Including matrix spikes and
reanalyses, that are of similar matrix (water or soil) or
similar concentration (soil only), OR

o whenever samples are extracted by the same procedure

(separatory funnel, continuous liquid-liquid extraction, or
sonication),

whichever is most freouent. on each GC/MS or GC system used to
analyze samples.

3.2 It is the Contractor's responsibility to ensure that method

interferences caused by contaminants in solvents, reagents, glassware,
and other sample processing hardware that lead to discrete artifacts
and/or elevated baselines in gas chromatograms be minimized.

3.2.1 For the purposes of this protocol, an acceptable laboratory

method blank should meet the criteria of paragraphs 3.2.1.1 and
3.2.1.2.

3.2.1.1	A method blank for semlvolatile analysis must
contain less than or equal to five times (5X) the
Contract Required Quantitation Limit (CRQL from
Exhibit C) of the phthalate esters in the TCL.

3.2.1.2	For all other TCL compounds not listed above, the
method blank must contain less than or equal to the
Contract Required Quantitation Limit of any single
TCL analyte.

3.2.2 If a laboratory method blank exceeds these criteria, the

Contractor must consider the analytical system to be out of
control. The source of the contamination must be investigated
and appropriate corrective measures MUST be taken and
documented before further sample analysis proceeds. All
samples processed with a method blank that is out of control
(i.e., contaminated) MUST be reextracted and reanalyzed at no
additional cost to the Agency. The Laboratory Manager, or his
designee, must address problems and solutions in the Case
Narrative (Exhibit B).

3.3 Documentation

The Contractor shall report results of method blank analysis using the
Organic Analysis Data Sheet (Form I) and the form for tentatively
identified compounds (Form I, TIC). In addition, the samples
associated with each method blank must be summarized on Form IV (Method

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Blank Summary). Detailed Instructions for the completion of these
forms are in Exhibit B, Section III.

3.3.1 The Contractor shall report AU sample concentration data as
UNCORRECTED for blanks.

PART 4 - SURROGATE SPTKE (SSt ANAT.VSTS

4. Summary

Surrogate standard determinations are performed on all samples and
blanks. All samples and blanks are fortified with surrogate spiking
compounds before purging or extraction in order to monitor preparation
and analysis of samples.

4.1 Each sample, matrix spike, matrix spike duplicate, and blank are spiked
with surrogate compounds prior to extraction. The surrogate spiking
compounds shown in Table 4.1 are used to fortify each sample, matrix
spike, matrix spike duplicate, and blank with the proper
concentrations. Performance based criteria are generated from
laboratory results. Therefore, deviations from the spiking protocol
will not be permitted.

TABLE 4.1. SURROGATE SPIKING COMPOUNDS

Amount in Sample Extract*
Compounds	fhafor* inv optional

Fraction	Vater	Low/Medium Soil

Nitrobenzene-d^	BNA	SO ug	SO ug

2 - Fluorobiphenyl	BNA	50 ug	50 ug

p-Terphenyl-d14	BNA	50 ug	50 ug

Phenol-d^	BNA	100 ug	100 ug

2-Fluorophenol	BNA	100 ug	100 ug

2,4,6-Trlbromophenol	BNA	100 ug	100 ug

* At the time of injection.

4.2 Surrogate spike recovery must be evaluated by determining whether the
concentration (measured as percent recovery) falls inside the contract
required recovery limits listed in Table 4.2.

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TABLE 4.2. CONTRACT REQUIRED SURROGATE SPIKE RECOVERY LIMITS

Fraction Surrogate Compound	Water	Low/Medium Soil

BNA	Nitrobenzene-de	35-114	23-120

BNA	2-Fluorobiphenyl	43-116	30-115

BNA	p-Terphenyl-djA	33-141	18-137

BNA	Phenol-de	10-94	24-113

BNA	2-Fluorophenol	21-100	25-121

BNA	2,4,6-Tribromophenol	10-123	19-122

4.3 Treatment of surrogate spike recovery information is according to
P&ragraphs 4.3.1 through 4.3.2.

4.3.1 Method Blank Surrogate Spike Recovery

The laboratory oust take the actions listed below if recovery
of any one surrogate compound in either the base/neutral or
acid fraction is outside of contract surrogate spike recovery
limits.

4.3.1.1	Check calculations to ensure that there are no
errors; check internal standard and surrogate
spiking solutions for degradation, contamination,
etc; also check instrument performance.

4.3.1.2	Reanalyze the blank extract if steps in 4.3.1.1 fail
to reveal the cause of the noncompliant surrogate
recoveries.

4.3.1.3	Reextract and reanalyze the blank.

4.3.1.4	If the measures listed in 4.3.1.1 thru 4.3.1.3 fail
to correct the problem, the analytical system must
be considered to be out of control. The problem
MUST be corrected before continuing. This may mean
recalibrating the instrumentation but it may also
mean more extensive action. The specific corrective
action is left up to the GC/MS operator. When
surrogate recovery(ies) in the blank is outside of
the contract required windows, all samples
associated with that blank MUST be reanalyzed at no
additional cost to the Agency.

4.3.2 Sample Surrogate Spike Recovery

The laboratory must take the actions listed below if either of
the following conditions exists:

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o Recovery of any one surrogate compound in either base
neutral or acid fraction is below 10%.

o Recoveries of two surrogate compounds in either base
neutral or acid fractions are outside surrogate spike
recovery limits.

4.3.2.1 The Contractor shall document (in this instance,

document means to write down and discuss the problem
and corrective action taken in the Case Narrative,
see Exhibit B) deviations outside of acceptable
quality control limits and take the following
actions:

4.3.2.1.1	Check calculations to ensure that there
are no errors; check internal standard
and surrogate spiking solutions for
degradation, contamination, etc.; also
check instrument performance.

4.3.2.1.2	If the steps in 4.3.2.1.1 fall to
reveal a problem, then reanalyze the
extract. If reanalysis of the extract
solves the problem, then the problem
was within the laboratory's control.
Therefore, only submit data from the
analysis with surrogate spike
recoveries within the contract windows.
This shall be considered the initial
analysis and shall be reported as such
on all data deliverables.

4.3.2.1.3	If the steps in 4.3.2.1.2 fail to solve
the problem, then reextract and
reanalyze the sample. If the
reextractlon and reanalysis solves the
problem, then the problem was in the
laboratory's control. Therefore, only
¦ubmlt data from the extraction and
analysis with surrogate spike
recoveries within the contract windows.
This shall be considered the Initial
analysis and shall be reported as such
on all data deliverables.

If the reextractlon and reanalysis of
the sample does not solve the problem;
i.e., surrogate recoveries are outside
the contract windows for both analyses,
then submit the surrogate spike
recovery data and the sample data from
both analyses according to paragraph
4.4. Distinguish between the initial
analysis and the reanalysis on all data

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deliverables, using the sample suffixes
specified in Exhibit B.

4.4 Documentat ion

The Contractor shall report surrogate recovery data for the following:

o	Method Blank Analysis

o	Sample Analysis

o	Matrix Spike/Matrix Spike Duplicate Analyses

o	All sample reanalyses that substantiate a matrix effect

The surrogate spike recovery data is summarized on the Surrogate Spike
Percent Recovery Summary (Form II). Detailed instructions for the
completion of Form II are in Exhibit B, Section III.

PART 5 ¦ MATRIX SPIKE/MATRIX SPIKE DUPLICATE ANALYSIS fMS/MSm

5. Siinrniarv

In order to evaluate the matrix effect of the sample upon the
analytical methodology, the USEPA has developed the standard mixes
listed in Table 5.1 to be used for matrix spike and matrix spike
duplicate analyses. These compounds are subject to change depending
upon availability and suitability for use as matrix spikes.

5.1	MS/MSD Frequency of Analysis

A matrix spike and matrix spike duplicate must be performed for each
group of samples of a similar matrix, once:

o each Case of field samples received, OR
o each 20 field samples in a Case, OR

o each group of field samples of a similar concentration level
(soils only), OR

o each 14 calendar day period during which field samples in a
Case were received (said period beginning with the receipt of
the first sample in that Sample Delivery Group),

whichever is most freouent.

5.2	Use the compounds listed in Table 5.1 to prepare matrix spiking
solutions according to protocols described in Exhibit D SV. The
analytical protocols in Exhibit D SV stipulate the amount of matrix
spiking solution to be added to the sample aliquots prior to
extraction. Each method allows for optional dilution steps which must
be accounted for when calculating percent recovery of the matrix spike
and matrix spike duplicate samples.

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TABLE 5.1. MATRIX SPIKING SOLUTIONS

Base/Neutrals

1,2,4-Trichlorobenzene
Acenaphthene
2,4 - D ini tr o to luene
Pyrene

N-Nltroso-Di-n-Propylamine
1,4-Dichlorobenzene

Acids

Pentachlorophenol
Phenol

2-Chlorophenol

4-Chloro-3-Methylphenol

4-Nitrophenol

5.2.1 Samples requiring optional dilutions and chosen as the matrix
spike/ matrix spike duplicate samples, must be analyzed at the
same dilution as the original unspiked sample.

5.3	Individual component recoveries of the matrix spike are calculated
using Equation 5.1.

SSR - SR

Matrix Spike Percent Recovery - 	 x 100	Eq. 5.1

SA

where

SSR — Spike Sample Results

SR — Sample Result

SA - Spike Added from spiking mix

5.4	Relative Percent Difference (RPD)

The Contractor is required to calculate the relative percent difference
between the matrix spike and matrix spike duplicate. The relative
percent differences (RPD) for each component are calculated using
Equation 5.2.

D1 - D2

RPD - 	 x 100	Eq. 5.2

(D1 ~ D2)/2

where

RPD — Relative Percent Difference

D1 - First Sample Value

D2 — Second Sample Value (duplicate)

5.5	Documentation

The matrix spike (MS) results (concentrations) for nonsplked
semivolatlle TCL compounds shall be reported on Form I (Organic
Analysis Data Sheet) and the matrix spike percent recoveries shall be
summarized on Form III (MS/MSD Recovery). These values will be used by

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EPA to periodically update existing performance based QC recovery
limits (Table 5.2).

The results for nonspiked semivolatile TCL compounds in the matrix
spike duplicate (MSD) analysis shall be reported on Form I (Organic
Analysis Data Sheet) and the percent recovery and the relative percent
difference shall be summarized on Form III (MS/MSD Recovery). The RPD
data will be used by EPA to evaluate the long term precision of the
analytical method. Detailed instructions for the completion of Form
III are in Exhibit B, Section III.

TABLE 5.2. MATRIX SPIKE RECOVERY LIMITS*

Fraction Matrix Spike Compound	Water Soil/Sediment

BN

1,2,4-Trichlorobenzene

39-98

38-107

BN

Acenaphthene

46-118

31-137

BN

2,4-Dinitrotoluene

24-96

28-89

BN

Pyrene

26-127

35-142

BN

N-Nitroso-Di-n-Propylamine

41-116

41-126

BN

1,4-Dichlorobenzene

36-97

28-104

Acid

Pentachlorophenol

9-103

17-109

Acid

Phenol

12-89

26-90

Acid

2-Chlorophenol

27-123

25-102

Acid

4-Chloro- 3-Methylphenol

23-97

26-103

Acid

4-Nitrophenol

10-80

11-114

PART 6 - SAMPLE ANALYSTS
6. Summary

The intent of Part 6 is to provide the Contractor with a brief summary
of ongoing QC activities involved with sample analysis. Specific
references are provided to help the Contractor meet specific reporting
and deliverables requirements of this contract.

6.1 Sample Analysis

Samples can be analyzed upon successful completion of the initial QC
activities. When twelve (12) hours have elapsed since the initial tune
was completed, it is necessary to conduct an instrument tune and
calibration check analysis (described in Part 2 of this Section). Any
major system maintenance, such as a source cleaning or installation of
a new column, may necessitate a retune and recalibration (see Initial
Calibration, Part 2). Minor maintenance should necessitate only the
calibration verification (Continuing Calibration, Part 2).

6.1.1 Internal Standards Evaluation - Internal standard responses and
retention times in all samples must be evaluated Immediately
after or during data acquisition. If the retention time for

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any internal standard changes by nore than 30 seconds, the
chromatographic system must be inspected for malfunctions, and
corrections made as required. The extracted ion current
profile (EICP) of the internal standards must be monitored and
evaluated for each sample, blank, matrix spike, and matrix
spike duplicate. The criteria are described in detail in the
Instructions for Form VIII, Internal Standard Area Summary (see
Exhibit B, Section III). If the extracted ion current profile
(EICP) area for any Internal standard changes by more than a
factor of two (-50% to 100%), from the latest daily (12 hour
time period) calibration standard, the mass spectrometric
system must be inspected for malfunction, and corrections made
as appropriate. Breaking off 1 foot of the colunti; or cleaning
the Injector sleeve will often improve high end sensitivity for
the late elutlng compounds; repositioning or repacking the
front end of the column will often improve front end column
performance. Poor injection technique can also lead to
variable IS ratios. When corrections are made, reanalysis of
samples analyzed while the system was malfunctioning is
necessary.

6.1.1.1	If after reanalysis, the EICP areas for all internal
standards are inside the contract limits (-50% to
+100%), then the problem with the first analysis is
considered to have been within the control of the
laboratory. Therefore, only submit data from the
analysis with EICPs within the contract limits. This
is considered the initial analysis and must be
reported as such on all data deliverables.

6.1.1.2	If the reanalysis of the sample does not solve the
problem, i.e., the EICP areas are outside contract
limits for both analyses, then submit the EICP data
and sample data from both analyses. Distinguish
between the initial analysis and the reanalysis on
all data deliverables, using the sample suffixes
specified in Exhibit B. Document in the Case
Narrative all Inspection and corrective actions
taken.

6.1.2 Each analytical run must also be checked for saturation. The
level at which an individual compound will saturate the
detection system is a function of the overall system
sensitivity and the mass spectral characteristics of that
compound. The Initial method calibration (Part 2) requires
that the system should not be saturated for high response
compounds at 160 nanograms for semivolatile TCL compounds.

6.1.2.1 If the on-column concentration of any compound in
any sample exceeds the Initial calibration range,
that sample must be diluted, the Internal standard
concentration readjusted, and the sample reinjected,
as described in specific methodologies in Exhibit D
SV. Secondary ion quantitation is only allowed when

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there are sample matrix interferences with the
primary ion.

6.1.2.2 If the dilution of the sample causes any compound

detected in the first analysis to be undetectable in
the second analysis, then the results of both
analyses shall be reported on separate Forms I,
according to the instructions in Exhibit B.

Qualitative Analysis

The semivolatile compounds listed in the Target Compound List
(TCL), Exhibit C, shall be identified by an analyst competent
in the interpretation of mass spectra, by comparison of the
suspect mass spectrum to the mass spectrum of a standard of the
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 (see Exhibit D SV, Section IV).

6.1.3.1	For establishing correspondence of the GC relative
retention time (RRT), the sample component RRT must
compare within ±0-06 RRT units of the RRT of the
standard component. For reference, the standard
must be run on the same shift as the sample.

6.1.3.2	For comparison of standard and sample component mass
spectra, mass spectra obtained on the Contractor's
GC/MS are required. The DFTPP tuning requirements
listed in Fart 1 must be met on the same GC/MS.

6.1.3.2.1 The requirements for qualitative

verification by comparison of mass
spectra are as follows:

o All ions present in the standard

•ass spectra at a relative Intensity
greater than 10% (most abundant ion
in the spectrum equals 100%) must be
present in the sample spectrum.

o The relative intensities of ions
specified in the above paragraph
must agree within ±20% between the
standard and sample spectra.

o Ions greater than 10% in the
spectrum but not present in the
standard spectrum must be considered
and accounted for by the analyst
making the comparison. Vhen GC/MS
computer data processing programs
are used to obtain the sample

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component spectrum, both the
processed and the raw spectra must
be evaluated. In Task III, the
verification process should favor
false negatives (Exhibit D SV,
Section IV).

6.1.3.2.2 If a compound cannot be verified by all
of the criteria in 6.1.3.2.1, but in
the technical Judgement of the mass
spectral interpretation specialist the
identification is correct, the
Contractor shall report the
identification and proceed with the
quantitation.

6.1.3.3 A library search shall be executed for nonsurrogate
and non-TCL sample components for the purpose of
tentative identification. For this purpose, the 1985
or most recent available version of the National
Bureau of Standards Mass Spectral Library,
containing 42,261 spectra, should be used.

6.1.4 Quantitation

6.1.4.1	Semivolatile TCL components identified shall be
quantitated by the internal standard method. The
internal standards used shall be the ones assigned
in Table 2.2 of this Section. The EICP area of
characteristic ions of TCL analytes are used
(Exhibit D SV, Section IV).

6.1.4.2	An estimated concentration for non-TCL components
tentatively Identified shall be quantitated by the
internal standard method. For quantification, the
nearest internal standard free of interferences must
be used.

6.1.4.3	Calculate surrogate standard recovery (see Part 4)
for all surrogate compounds on all samples, blanks,
matrix spikes, and matrix spike duplicates. If
recovery is within contractual limits, report on
Form II (see Exhibit B, Section III). If recovery
is outside contractual limits, take specific steps
listed in Surrogate Spike Recoveries (Part 4).

6.1.4.4	Calculate matrix spike and matrix spike duplicate
percent recovery (see Part 5) for all compounds and
report results on Form III (see Exhibit B, Section
III). Calculate Relative Percent Differences (RPDs)
for all matrix spiking compounds and report results
on Form III. Ensure that the proper frequency of
MS/MSD analysis is maintained.

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6.1.5

Reporting and Deliverables

Refer to Exhibit B of this Statement of Work for specific
details on contract deliverables and reporting formats. Exhibit
B contains specific instructions for completing all required
Forms, as well as a detailed itemization of reporting and
deliverables requirements. Exhibit H contains the format
requirements for delivery of data in computer-readable format.

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SECTION III PEST

PESTICIDES/PCBs QA/QC
REQUIREMENTS

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This Section outlines the minimum quality control (QC) operations necessary
to satisfy the analytical requirements associated with the determination of
pestlclde/PCB organic TCL compounds in water and soil/sediment samples.

These QC operations are as follows:

o	Method Blank Analysis

o	Surrogate Spike Response Monitoring

o	Matrix Spike and Matrix Spike Duplicate Analysis

o	Specific QA/QC for Pesticide Analysis

PART 1 - METHOD BLANK ANALYSIS

1. Summary

A method blank is a volume of delonized, distilled laboratory water for
water samples, or a purified solid matrix for soil/sediment samples,
carried through the entire analytical scheme (extraction,
concentration, and analysis). For soil/sediment samples, a solid
matrix suitable for pesticide analyses is available from EMSL-LV. The
method blank volume or weight must be approximately equal to the sample
volumes or sample weights being processed.

1.1	Method blank analysis must be performed at the following frequency:

1.1.1 For the analysis of pestlclde/PCB TCL compounds, a method blank
analysis must be performed once:

o each Case, OR

o each 14 calendar day period during which samples In a Case
are received (said period beginning with the receipt of the
first sample in that Sample Delivery Group), OR

o each 20 samples in a Case, Including matrix spike and
re^nalyses that are of similar matrix (water or soil) or
similar concentration (soil only), OR

o whenever samples are extracted by the same procedure
(separatory funnel or continuous extraction),

whichever is most frequent, on each GC/MS or GC system used to
analyze samples.

1.2	It is the Contractor's responsibility to ensure that method
interferences caused by contaminants in solvents, reagents, glassware,
and other,sample processing hardware that lead to discrete artifacts
and/or elevated baselines in gas chromatograms be minimized.

1.2.1 For the purposes of this protocol, an acceptable laboratory
method blank should meet the criteria of paragraph 1.2.1.1.

1.2.1.1 The method blank must contain less than or equal to
the Contract Required Quantitation Limit of any
single pestlclde/PCB Target Compound (Exhibit C).

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1.2.2 If a laboratory method blank exceeds these criteria, the

Contractor oust consider the analytical system to be out of
control. The source of the contamination must be investigated
and appropriate corrective measures MUST be taken and
documented before further sample analysis proceeds. All
samples processed with a method blank that is out of control
(i.e., contaminated) MUST be reextracted and reanalyzed at no
additional cost to the Agency. The Laboratory Manager, or his
designee, must address problems and solutions in the Case
Narrative (Exhibit B).

1.3 Documentation

The Contractor shall report results of method blank analysis using the
Organic Analysis Data Sheet (Form I). In addition, the samples
associated with each method blank must be summarized on Form IV (Method
Blank Summary). Detailed instructions for the completion of these
forms can be found in Exhibit B, Section III.

1-3.1 The Contractor shall report AT.T. sample concentration data as
UNCORRECTED for blanks.

PART 2 - SURROGATE SPIKE fSS) ANALYSIS

2.	Simimar-y

Surrogate standard determinations are performed on all samples and
blanks. All samples and blanks are fortified with surrogate spiking
compounds before purging or extraction in order to monitor preparation
and analysis of samples.

2.1 Each sample, matrix spike, matrix spike duplicate, and blank are spiked
with surrogate compounds prior to extraction. The surrogate spiking
compounds shown in Table 4.1 are used to fortify each sample, matrix
spike, matrix spike duplicate, and blank with the proper
concentrations. Performance based criteria are generated from
laboratory results. Therefore, deviations from the spiking protocol
will not be permitted.

TABLE 4.1. SURROGATE SPIKING COMPOUND

Amount in Sample Extract*

Compound		(before any optional dilutions)

Fraction	Vater	Low/Medium Soil

Dibutylchlorendate	Pest.	0.1 ug	0.1 ug

* At the time of injection.

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2.2 Surrogate spike recovery must be evaluated by determining whether the
concentration (measured as percent recovery) falls inside the advisory
recovery limits listed in Table 4.2.

TABLE 4.2. ADVISORY SURROGATE SPIKE RECOVERY LIMITS







Low/Medium

Fraction

Surrogate Compound

Water

Soil/Sediment

Pest.

Dibutylchlorendate

(24-154)*

(20-150)*

* These limits are for advisory purposes only. They are not used to

determine if a sample should be reanalyzed. When sufficient data becomes
available, the USEPA may set performance based contract required windows.

2.3 Documentation

The Contractor shall report surrogate recovery data for the following:

o Method Blank Analysis
o Sample Analysis

o Matrix Spike/Matrix Spike Duplicate Analyses

The surrogate spike recovery data is summarized on the Surrogate Spike
Percent Recovery Summary (Form II). Detailed instructions for the
completion of Form II are in Exhibit B, Section III.

fART 3 - MATRIX SPIKE/MATRIX SPIKE DUPLICATE ANALYSIS (MS/MSD^

3. Summary

In order to evaluate the matrix effect of the sample upon the
analytical methodology, the USEPA has developed the standard mixes
listed in Table 5.1 to be used for matrix spike and matrix spike
duplicate analyses. These compounds are subject to change depending
upon availability and suitability for use as matrix spikes.

3.1 MS/MSD Frequency of Analysis

A matrix spike and matrix spike duplicate must be performed for each
group of .samples of a similar matrix, once:

o each Case of field samples received, OR
o each 20 field samples in a Case, OR

o each group of field samples of a similar concentration level (soils
only), OR

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o each 14 calendar day period during which field samples In a Case
were received (said period beginning with the receipt of the first
sample In that Sample Delivery Group),

whichever la most frequent.

3.2 Use the compounds listed in Table 5.1 to prepare matrix spiking

solutions according to protocols described in Exhibit D PEST. The
analytical protocols in Exhibit D PEST stipulate the amount of matrix
spiking solution to be added to the sample aliquots prior to
extraction. Each method allows for optional dilution steps which must
be accounted for when calculating percent recovery of the matrix spike
and matrix spike duplicate samples.

TABLE 5.1. MATRIX SPIKING SOLUTIONS

Pesticides
Heptachlor Lindane
Aldrin	Endrin

Dieldrin 4,4'-DDT

3.2.1 Samples requiring optional dilutions and chosen as the matrix
spike/matrix spike duplicate samples, must be analyzed at the
same dilution as the original unspiked sample.

3.3	Individual component recoveries of the matrix spike are calculated
using Equation 5.1.

SSR - SR

Matrix Spike Percent Recovery - 	 x 100	Eq. 5.1

SA

where

SSR - Spike Sample Results

SR - Sample Result

SA - Spike Added from spiking mix

3.4	Relative Percent Difference (RPD)

The Contractor is required to calculate the relative percent difference
between the matrix spike and matrix spike duplicate. The relative
percent differences (RPD) for each component are calculated using
Equation 5.2.

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RPD - 	1	1— x 100	Eq. 5.2

(Dx + D2)/2

where

RPD - Relative Percent Difference

D^ - First Sample Value

D2 - Second Sample Value (duplicate)

3.S Documentation

The matrix spike (MS) results (concentrations) for nonspiked
pesticide/PCB TCL compounds shall be reported on Form I (Organic
Analysis Data Sheet) and the matrix spike percent recoveries shall be
summarized on Form III (MS/MSD Recovery). These values will be used by
EPA to periodically update existing performance based QC recovery
limits (Table 5.2).

The results for nonspiked pesticide/PCB TCL compounds in the matrix
spike duplicate (HSD) analysis shall be reported on Form I (Organic
Analysis Data Sheet) and the percent recovery and the relative percent
difference shall be summarized on Form III (MS/MSD Recovery). The RPD
data will be used by EPA to evaluate the long term precision of the
analytical method. Detailed instructions for the completion of Form
III are in Exhibit B, Section III.

TABLE 5.2. MATRIX SPIKE RECOVERY LIMITS*

Fraction Matrix Spike Compound Vater	Soil/Sediment

Pest.

Lindane

56-123

46-127

Pest.

Heptachlor

40-131

35-130

Pest.

Aldrin

40-120

34-132

Pest.

Dieldrin

52-126

31-134

Pest.

Endrin

56-121

42-139

Pest.

4,4'-DDT

38-127

23-134

* These limits are for advisory purposes only. They are not to be

used to determine if a sample should be reanalyzed. When sufficient
multi-lab data are available, standard limits will be calculated.

PARI 4 - PESTICIDE OA/OC REQUIREMENTS
4. Simrniarv

Part 4 summarizes ongoing QC activities involved with pesticide/PCB
analysis that were detailed in Parts 1, 2 and 3 of this Section, and
describes the additional QA/QC procedures required during the analysis
of pesticide/PCBs that are not covered in Parts 1, 2, and 3.

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4.1	The Contractor must perform the following:

4.1.1	Method Blank analysis as per Part 1 of this Section.

4.1.2	Spike all standards, samples, blanks, matrix spike and matrix
spike duplicate samples with the surrogate spike compound
(dibutylchlorendate) as per Part 2 of this Section.

4.1.3	Matrix Spike/Matrix Spike duplicate analysis as per Part 3 of
this Section.

4.2	The external standard quantitation method must be used to quantitate
all pesticides/PCBs. Before performing any sample analysis, the
laboratory is required to determine the retention time window for each
pesticide/PCB target compound listed in Exhibit C and the surrogate
spike compound, dibutylchlorendate. These retention time windows are
used to make tentative identification of pesticides/PCBs during sample
analysis.

4.2.1	Prior to establishing retention time windows, the GC operating
conditions (oven temperature and flow rate) must be adjusted
such that 4,4'-DDT has a retention time of > 12 minutes on
packed GC columns, except on OV-1 or 0V-101 columns.

Conditions listed in Table 7, Exhibit D PEST, Section IV may be
used to achieve this criteria.

4.2.2	Establish retention time windows as follows:

4.2.2.1	At the beginning of the contract and each time a new
GC column is installed, make three injections of all
single component pesticides mixtures, multi-response
pesticides, and PCBs throughout the course of a 72-
hour period. The concentration of each
pesticide/PCB should be sufficient to provide a
response that is approximately half scale. The
three injections of each compound should be made at
approximately equal intervals during the 72-hour
period, (e.g., each compound should be injected near
the beginning, near the middle, and near the end of
the 72-hour period).

4.2.2.2	Verify the retention time shift for
dibutylchlorendate in each standard. The retention
time shift between the initial and subsequent
standards must be less than 2.0% difference for
packed columns, less than 1.5% difference for wide
bore capillary columns (ID greater than 0.32 mm),
and less than 0.3% difference for narrow bore
capillary columns (ID less than 0.32 mm). If this
criterion is not met, continue injecting replicate
standards to meet this criterion.

4.2.2.3	Calculate the standard deviation of the three
absolute retention times for each single component

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pesticide. For multiresponse peaiiciufca	ui tCBs

choose one major peak from Che envelope	and

calculate the standard deviation of the	three
retention times for that peak.

4.2.2.4 The standard deviations determined in 4.2.2.3 shall
be used to determine the retention time windows for
a particular 72-hour sequence. Apply plus or minus
three times the standard deviations in 4.2.2.3 to
the retention time of each pesticide/PCB determined
for the first analysis of the pesticide/PCB standard
in a given 72 hour analytical sequence. This range
of retention times defines the retention time window
for the compound of interest for that 72-hour
sequence. NOTE: By definition, the retention time
of a pesticide/PCB from the first analysis of that
compound in the 72 hour sequence is the center of
the retention time window. Do not use the retention
time measured in 4.2.2.1 as the center of the
retention time window. The experience of the
analyst should weigh heavily in the interpretation
of chromatograms. For multiresponse pesticide/PCBs,
the analyst should utilize the retention time window
but should primarily rely on pattern recognition.

For example, the three injections of aldrin in
4.2.2.1 have a mean retention time of 1.40 minutes
and a standard deviation of .0.01 minutes. The
retention time of the aldrin standard at the
beginning of the 72-hour sequence begun today is
1.51 minutes. Three times the standard deviation
(0.01) is applied to the retention time of aldrin
from the sequence begun today, e.g., 1.51 ± 3(0.01)
- 1.48-1.54. If aldrin has a retention time of 1.60
minutes at the beginning of the next 72-hour
sequence, then the retention time window becomes:
1.60 + 3(0.01) - 1.57-1.63 for that 72-hour
sequence.

4.2.2.5 In those cases where the retention time window for a
particular pesticide/PCB is less than 0.01 minutes,
the laboratory may substitute whichever of the
following formulae apply.

o For packed columns, the retention time window of
the particular pesticide/PCB shall be calculated
as + 1% of the Initial retention time of the
compound in the 72-hour sequence.

o For wide bore capillary columns (ID greater than
0.32 mm), the retention time window of the
particular pesticide/PCB shall be calculated as
+ 0.75% of the initial retention time of the
compound in the 72-hour sequence.

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o For narrow bore capillary columns (ID less than
0.32 mm), the retention tine window of the
particular pesticide/PCB shall be calculated as
1 0.15% of the Initial retention time of the
conpound in the 72-hour sequence.

Regardless of whether the retention time windows are
calculated by the method in 4.2.2.4 or 4.2.2.5, the
retention time windows must be reported as a range
of values, not as, for example, 1.51 minutes ± 1%.

The laboratory must calculate retention time windows
for each pesticide/PCB on each GC column used at the
beginning of the program and whenever a new GC
column is installed. The data must be retained by
the laboratory and made available during an on-site
laboratory evaluation.

4.3 Primary GC Column Analysis

4.3.1	Primary Analysis establishes whether or not pesticides/PCBs are
present in the sample, and establishes a tentative
identification of each compound. Quantitation may be performed
on the primary analysis if the analysis meets all of the QC
criteria specified for quantitation. NOTE: To determine that
no pestic^des/PCBs are present at or above the contract
required quantitation limit la a form of quantitation.

4.3.2	Separation should be 25 percent resolution between peaks.

This criteria must be considered when determining whether to
quantitate on the Primary Analysis or the Confirmation
Analysis. When this criterion cannot be met, quantitation is
adversely affected because of the difficulty in determining
where to establish the baseline.

4.3.3	Evaluation Standard Mixtures

4.3.3.1	Prepare Evaluation Standard Mixes A, B, and C
(Aldrin, Endrin, 4,4'-DDT and Dibutylchlorendate) at
the 3 concentration levels described in Exhibit D
PEST. Analyze the three Evaluation Standard Mixes
sequentially at the beginning of each seventy-two
(72) hour period (See Figure 4.1).

4.3.3.2	Calculate the Calibration Factor (ratio of the total
area to the mass Injected) for each compound in
Evaluation Standard Mix A, B and C using Equation
4.1.

Calibration	Total Area of Peak

Factor	¦ 	 Eq.4.1

Mass Injected (in nanograms)

4.2.2.6

4.2.2.7

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4.3.3.3 Using the Calibration Factors from 4.3.3.2 above,
calculate the percent relative standard deviation
(%RSD) for each compound at the three concentration
levels using Equation 4.2. The percent relative
standard deviation for Aldrin, Endrin, and
Dlbutylchlorendate oust be less than or equal to
10.0 percent. If the %RSD exceeds 10.0% for
4,4'-DDT, see Section 4.5.4.4.

Note: The 10.0% RSD linearity criteria pertains
only to columns being used for Pesticide/PCB
quantitation. If a column is used only for surrogate
quantitation, the 10.0% RSD is only required for
Dlbutylchlorendate.

% Relative	SD

Standard Deviation - —— x 100 Eq. 4.2

x

/" "
where Standard Deviation (SD) - /E (xi - x)

1-1 	

N-l

x - mean of initial three Calibration Factors (per
compound).

4.3.3.4	Evaluate the chromatogram from the analysis of the
Evaluation Mix B. The appearance of peaks in
addition to the four main pesticide peaks Indicates
a breakdown of Endrin and/or 4,4'-DDT.

4.3.3.5	Calculate the percent breakdown for Endrin and/or
4,4'-DDT on the mixed phase (1.5% OV-16/1.95% OV-210
or equivalent) GC column using Equations 4.3 and
4.4. The percent breakdown for Endrin or 4,4'-DDT
must not exceed 20.0 percent. Corrective action
must be taken before analysis continues.

% breakdown Total DDT degradation peak area1(DDE + DDD)

for			-	 x 100 Eq. 4.3

4,4'-DDT	Total DDT peak area1 (DDT + DDE + DDD)

Total Endrin degradation peak areas1
% breakdown	(Endrin Aldehyde + Endrin Ketone)

for Endrin - 			-	 X 100 Eq. 4.4

Total Endrin Peak Area1(Endrin +

Endrin Aldehyde + Endrin Ketone)

' The term peak height may be substituted for the term peak area.

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Calculate the percent breakdown for Endrin and/or
4,4'-DDT on the OV-1 or equivalent GC column using
Equations 4.3 and 4.4 The percent breakdown for
Endrin or 4,4'-DDT oust not exceed 20.0 percent.
Corrective action oust be taken before analysis
continues.

If there is evidence of a peak at the retention time
for Endrin aldehyde/4,4'-DDD (which coelute on the
OV-1 or equivalent GC column), calculate a combined
percent breakdown for Endrin/4,4'-DDT using Equation
4.5. The combined Endrin/4,4'-DDT percent breakdown
must not exceed 20.0 percent, else corrective action
must be taken before analysis continues.

Total Endrin/DDT degradation peak areas
Combined	(DDD, DDE, Endrin Aldehyde, Endrin Ketone)

% breakdown - 		—	x 100 Eq, 4.5

Total Endrin/DDT degradation peak area^

(Endrin, Endrin Aldehyde, Endrin Ketone,

DDD, DDE, DDT)

4.3.3.8 Suggested Maintenance

Corrective measures may require any one or more of

the following remedial actions:

4.3.3.8.1	Packed columns - For instruments with
off-column injection; replace the
demister trap, clean and deactivate the
glass injection port insert or replace
with a cleaned and deactivated insert.
Inspect the injection end of the column
and remove any foreign material (broken
glass from the rim of the column or
pieces of septa). Replace the glass
wool with fresh deactivated glass wool.
Also, it may be necessary to remove the
first few millimeters of packing
material if any discoloration is noted,
also swab out the inside walls of the
column if any residue is noted. If
these procedures fail to eliminate the
degradation problem, it may be
necessary to deactivate the metal
injector body (described below) and/or
repack/replace the column.

4.3.3.8.2	Capillary columns - Clean and
deactivate the glass injection port
insert or replace with a cleaned and

4.3.3.6

4.3.3.7

^ The term peak height may be substituted for the term peak area.

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deactivated Insert. Break off the
first few inches, up to one foot, of
the injection port side of the column.
Remove the column and solvent backflush
according to the manufacturer's
instructions. If these procedures fail
to eliminate the degradation problem,
it may be necessary to deactivate the
metal injector body and/or replace the
column.

4.3.3.8.3 Metal Injector Body • Turn off the oven
and remove the analytical column when
the oven has cooled. Remove the glass
Injection port insert (instruments with
off-column injection or Grob). Lower
the injection port temperature to room
temperature. Inspect the injection
port and remove any noticeable foreign
material.

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 and then toluene, catching the
rinsate in the beaker.

Prepare a solution of deactivating
agent (Sylon-CT or 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 replace the
GC column.

4.3.4 Individual Standard Mixtures A and B

4.3.4.1	Prepare Individual Standard Mixtures A and B
containing the single component pesticides. These
may be divided into the groups suggested in Exhibit
D PEST, which are recommended to prevent overlap of
compounds on two of the packed columns. One mixture
of all of the single component pesticides is
acceptable when using capillary column. Prepare
separate solutions of all multi-response pesticides
and PCBs. (Aroclor 1016 and Aroclor 1260 may be
combined in a single mixture.)

4.3.4.2	Analyze Individual Standard Mixtures A and B and all
multi-response pesticide/PCBs at the beginning of

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each 72 hour period (see Figure 4.1) and analyze
Individual Standard Mixtures A and B at the
intervals specified in the analytical sequence in
Figure 4.1, and whenever sample analysis is
completed. The Calibration Factor for each standard
quantitated (Individual Standard Mix A or B)
(Equation 4.6), must not exceed a 15.0 percent
difference for a quantitation run nor exceed a 20.0
percent difference for a confirmation run during the
72 hour period. Calculate percent difference using
Equation 4.7. Deviations greater than 15.0 percent
require the laboratory to repeat the samples
analyzed following the quantitation standard that
exceeded the criterion.

NOTE: Aroclors 1221 and 1232 must be analyzed at a
minimum of once a month on each instrument and each
column. Copies of these chromatograms must be
submitted with each case for instruments and columns
used to quantitate samples in that case, when
Identity of these two pesticides (Aroclor 1221 and
1232) has been confirmed.

Total Area of Peak*

Calibration Factor - Mass injected (in nanograms)

* For multlresponse pesticides/PCBs use
area of all peaks used for quantitation.

R1 " R2

Percent Difference - 	 x 100	Eq. 4.7

R1

where

- Calibration Factor from first analysis

R.2 - Calibration Factor from second or subsequent
analysis

4.4 Sample Analysis (Primary GC Column)

4.4.1	Samples are analyzed per the sequence described in Figure 4.1.

4.4.2	The retention time shift for Dibutylchlorendate must be
evaluated after the analysis of each sample. The retention
time shift must be less than 2.0% difference for packed GC
columns between the initial standard analysis and any sample or
standard analyzed during the 72 hour period. The percent
difference for wide bore capillary columns (ID greater than
0.32 mm) must be less than 1.5%. The percent difference for
narrow bore capillary columns (ID less than 0.32 nm) must be
less than 0.3% (Equation 4.8).

Eq. 4.6
the total

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PT • BT

Percent Difference (%D) - 	1—^	S	 x 100	Eq. 4.8

RTj

where

RTj - absolute retention time of Dibutylchlorendate in the
initial standard (Evaluation Standard Mix A).

RTg - absolute retention time of Dibutylchlorendate in the
sample or subsequent standard.

4.4.3	Evaluate the GC column throughout the analysis of samples by
injecting Evaluation Standard Mix B at the frequency outlined
in Figure 4.1.

4.4.4	Calculate the percent breakdown for 4,4'-DDT and Endrin
according to 4.3.3.5. Take corrective action when the
breakdown for 4,4'-DDT or Endrin exceeds 20.0 percent.

FIGURE 4.1 72 HOUR SEQUENCE FOR PESTICIDE/PCB ANALYSIS

1.	Evaluation Standard Mix A

2.	Evaluation Standard Mix B

3.	Evaluation Standard Mix C

4.	Individual Standard Mix A*

5.	Individual Standard Mix B*

6.	Toxaphene

7.	Aroclors 1016/1260

8.	Aroclor 1221**

9.	Aroclor 1232**

10.	Aroclor 1242

11.	Aroclor 1248

12.	Aroclor 1254

13.	5 Samples

14.	Evaluation Standard Mix B

15.	5 Samples

16.	Individual Standard Mix A or B

17.	5 Samples

18.	Evaluation Standard Mix B

19.	5 Samples

20.	Individual Standard Mix A or B (whichever not run in steo 16>

21.	5 Samples	K '

22.	Repeat the above sequence starting with Evaluation Standard Mix B (step

14 above;•

23.	Pesticide/PCB analysis sequence must end with the analysis of both

individual Standard Mix A ^ B regardless of nu»J« of ^iST*
analyzed.	v

*These may be one mixture.

« Aroclor. 1221 .nd 1232 mt h «n.lyz.d .t . .mi,*,,, of OT,a. n.r „onrh on

.S c! V T' COPl" 0t th,M

E-60/PEST

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4.4.5 If one or more compounds have a response greater than full
scale, the extract requires dilution according to the

specifications in Exhibit D PEST. If the dilution of the
extract causes any compounds tentatively identified in the
first analysis to be undetectable in the second analysis, then
the results of both analyses shall be reported on separate
Forms I, according to the instructions in Exhibit B. For
dilutions greater than 10-fold, also see the Instructions in
Exhibit D PEST.

Confirmation Analysis (GC/EC)

4 5 1 Confirmation Analysis is to confirm the presence of all
compounds tentatively identified in the Primary Analysis.
Therefore, the only standards that are required are the
Evaluation Standard Mixes (to check linearity and degradation
criteria) and standards of all compounds to be confirmed. The
72-hour sequence described in Figure 4.1 is, therefore,
modified to fit each case. Quantitation may be performed on
the confirmation analysis. If toxaphene or DDT is to be
quantitated, the linearity requirements are specified in

Section 4.5.4.

where to establish the Dasexin*.

4.5.2.1 For a fused silica capillary (FSCC) confirmation,
there must be > 25 percent resolution (valley)
between the following pesticide pairs:

4 5 2	should be > 25 percent resolution between peaks.

o	beta-BHC and delta-BHC

o	Dieldrin and 4,4'-DDT

o	4,4'-DDD and Endrin Aldehyde

o	Endosulfan Sulfate and 4,4'-DDT

4.5.3

OV-101.

E-61/PEST

Rev. 9/88
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following sequences must be followed depending on the
situation.

4.5.4.1 Toxaphene only - Begin the sequence with Evaluation
Mix B to check degradation, followed by three
concentration levels to toxaphene. Check linearity
by calculating %RSD. If < 10.0% RSD, use the
appropriate equation in Exhibit D PEST for
calculation. If >10.0% RSD, plot a standard curve
and determine the ng for each sample in that set
from the curve.

4.5.4.2	DDT, DDE, DDD only Begin the sequence with
Evaluation Mix B. Then inject three concentration
levels of a standard containing DDE, DDD and DDT.
Calculate linearity and follow the requirements
specified in 4.5.4.1 for each compound to be
quantitated.

4.5.4.3	DDT series and toxaphene - Begin the sequence with
Evaluation Mix B. Then inject three concentration
levels of toxaphene and another three levels of the
DDT series. Calculate linearity and follow the
requirements specified in 4.5.4.1 for each compound
to be quantitated.

4.5.4.4	Other pesticides/PCBs plus DDT series and/or
toxaphene Begin the sequence with Evaluation
Standard Mixes A, B and C. Calculate linearity on
the four compounds in the Evaluation Standards
mixes. If DDT and/or one or more of the other
compounds are >10.0% RSD and/or degradation exceeds
the criterion, corrective maintenance as outlined in
paragraph 4.3.3.8 should be performed before
repeating the above chromatography evaluations. If
DDT only exceeds the linearity criteria and one or
more of the DDT series is to be quantitated, follow
4.5.4.2 (do not repeat Evaluation Mix B). If none of
the DDT series is to be quantitated and DDT exceeds
the 10.0% RSD, simply record the % RSD on the proper
form. Anytime toxaphene is to be quantitated,
follow 4.5.4.1.

4.5.5 After the linearity standards required in 4.5.4 are injected,
continue the confirmation analysis Injection sequence with all
compounds tentatively identified during primary analysis to
establish the daily retention time windows during primary
analysis. Analyze all confirmation standards for a case at the
beginning, at intervals specified in 4.5.6, and at the end. Any
pesticide outside of its established retention time window
requires immediate investigation and correction before
continuing the analysis. The laboratory must reanalyze all
samples between the standard that exceeds the criterion and a
subsequent standard that meets the criterion.

E-62/PEST

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4.5.6	Begin injection of samples at this point of the Confirmation
Analysis sequence. Analyze groups of 5 samples with a standard
pertaining to the samples after each group (Evaluation Mix B is
required after the first 5 samples, and every 10 samples
thereafter, e.g., after 5, 15, 25, etc). The alternating
standard's calibration factors oust be within 15.0 percent of
each other if quantitation is performed. Deviations larger
than 15.0 percent require the laboratory to repeat the samples
analyzed between the standard that exceeds the criterion and a
subsequent standard that meets the criterion. The 15.0 percent
criterion only pertains to compounds being quantitated.

4.5.6.1	If more than one standard is required to confirm all
compounds tentatively identified in the Primary
Analysis, include an alternate standard after each
10 samples.

4.5.6.2	Samples must also be repeated if the degradation of
either DDT and/or Endrin exceed 20.0 percent on the
intermittent Evaluation Standard Mix B.

4.5.6.3	If the samples are split between 2 or more
instruments, all standards and blanks pertaining to
those samples must be analyzed on each instrument.

4.5.7	Inject the method blanks (extracted with each se& of samples)
on every GC and GC column on which the samples are analyzed.

4.5.8	If quantitation is performed on the confirmation analysis,
follow the instructions in 4.4.5 regarding dilution of extracts
and reporting results.

4.6 GC/MS Pesticide/PCB Confirmation

4.6.1	Any pesticide/PCB confirmed by two dissimilar GC columns must
also be confirmed by GC/MS if the concentration in the final
sample extract is sufficient for GC/MS analysis (based on
laboratory GC/MS detection limits).

4.6.1.1 Pesticides/PCBs may be confirmed utilizing the

extract prepared for semivolatile GC/MS analysis;
however, the absence of pesticide/PCBs in the
semivolatile extract would require the analysis of
the pesticide/PCB (fraction) extract.

4.6.2	The tuning and mass calibration criteria for DFTPP (50 ng) MUST
be met prior to any confirmation of pesticides/PCBs is
undertaken. Refer to the tuning and mass calibration
instruction for semivolatiles. The characteristic ions for
GC/MC analysis of pesticides/PCBs are given in Exhibit D SV,

Table 5.

E-63/PEST

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4.6.3 The pesticide/PCB sample extract(s) and the associated

pesticide/PCB blank(s), and reference standard(s) must be
analyzed by GC/MS.

4.7 Documentat ion

See Exhibit B for complete instructions for the completion of all
required forms and the Deliverable Index for all reporting and
deliverables requirements.

E-64/PEST

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SECTION IV

ANALYTICAL STANDARDS

The Environmental Protection Agency's Quality Assurance Materials Bank will
supply primary standards (calibration standards, surrogate standards, matrix
spiking standards, and internal standards), contingent upon their
availability, only for traceability and quantitative verification of
Contractor standards. It is emphasized that these primary standards are for
traceabilitv only There are insufficient quantities to have these available

standards. The Contractor is responsible for preparing

its oZ working standards from commercial sources.

Caution should b. exerdsad wh.n .i*lng ¦chasa	^

particularly th. oulticoapon.nt standards. Chemical reactions such as
acld/bas« reactions, Schlff base formations (reactions of aldehydes and
ketones with primal amines), hydrolysis, lsotoplc exchange, and others may

occur.

rJ,n caii or write directly to the QAMB (address and
EPA contract lab°* fouowing request form) to obtain reference standards,
phone number on th	hfsed on the reasonableness of the request and

Standards will be provided base	-rial laboratory that is not

their availability. Any	^ lab0r"0ry

currently under contract to EPA

^ — . list of available standards will be provided by
Upon award of a contract, a

the EMSL/LV upon request.

E-65

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QUALITY ASSURANCE MATERIALS BANK

REQUEST FOR REFERENCE STANDARDS

MAIL TOl

Telephone:

U.S. Environment*! Protection Ageno/
Quality Assurance Materials Bank (MD-8)
Research Triangle Park. NC 27711 USA

Requests ONLY:
Information:
Technical Assistance:

(919)541-4019
(FTS) 629-4019
(702) 545-2690
(FTS) 545-2690
(919)541-3951
(FTS) 629-39S1

Th« following reference standard* are required for our program:

Oat* R*qu«lt Recei ved_
Date of Shipment .

laboratory Cod* Number.
Request Number _______

Verified	

THIS (LOCK FOR AfiXNCY USt ONLY

Number
fteauired

Standard

Code
Number

Compound(l)

Solvent

Purity

Concentration
(|ig/ml)

































































































1









1































1









1 1

1



1 1

1



M««t« €Ofne*«t« •«»* m htM,
to««r -i

wmhtiik fl< r)mn»»w««ta
Miytic* VQOWW «WO> n> IM C*ttnM Ol -

to m a— amy ¦« bm aoorttorf tf tt.ii.rno wrumi .*q

0«u

hfuturi-

Request for Reference Standards

E-66

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SECTION V

LABORATORY EVALUATION PROCEDURES

This section outlines the procedures which will be used by the Proles
Officer or his authorized representative during the contract period of
performance to conduct laboratory audits to determine the Contractor'«
continuing ability to meet the terns and conditions of this contract Th*
evaluation process incorporates two major steps: 1) evaluaMnn i \
performance, and 2) on-site inspection of the laboratory to verify Continuity
of personnel, instrumentation and quality control requirements of the
contract. The following is a description of these two steps.

flUVT .1 - EVALUATION OF LABORATORY PERFORMANCE

1- Performance Evaluation Sample Analysis

1.1 The Performance Evaluation (PE) sample set will be sent to a
participating laboratory on a quarterly basis to verify the
laboratory's continuing ability to produce acceptable analytical
results. These samples will be provided either single blind
(recognizable as a PE material and of unknown composition), or double
blind (not recognizable as a PE material and of unknown composition)

If received as* a single blind, the Contractor is required to submit PE
sample data in a separate SDG package in accordance with Delivery
Schedule requirements for sample data. PE samples received as double
blind would be treated as routine samples and data would be submitted
in the SDG deliverables package per normal procedure.

1.2	When the PE data are received, results will be scored routinely for
identification and quantitation. Results of these scorings will be
provided to the Contractor. The government may adjust the scores on
any given PE sample to compensate for unanticipated difficulties with a
particular sample.

1.3	If a laboratory performs unacceptably, the laboratory will be
immediately notified by the Project Officer. A laboratory so notified
may expect, but the government is not limited to, the following
actions: a site visit, a full data audit, and/or laboratory analysis
of a second PE sample. Failure by the laboratory to take corrective
actions and/or failure of two successive PE sample analyses will
require that the laboratory discontinue analysis of samples until such
time as the Project Officer has determined that the laboratory may
resume analyses.

2. Organic Data Audit

2.1 Organic data audits are conducted on CLP Contractor's Reporting and

Deliverables packages by EMSL/LV. The organic data audit provides the
Agency with an in-depth inspection and evaluation of the Case data
packages with regard to achieving QA/QC acceptability.

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PART 7 ON-SITE LABORATORY EVALUATION

2. The on-site laboratory evaluation helps to ensure that all the

necessary quality control is being applied by the Contractor in order
to deliver a quality product.

2.1 Quality assurance evaluations allow the evaluators to determine that:

2.1.1 The organization and personnel are qualified to perform
assigned tasks,

2.1.2	Adequate facilities and equipment are available,

2.1.3	Complete documentation, including chain-of-custody of samples
is being implemented,

2.1.4	Proper analytical methodology is being used,

2.1.5	Adequate analytical Quality Control, including reference
samples, control charts, and documented corrective action
measures, is being provided, and

2.1.6	Acceptable data handling and documentation techniques are being
used.

2.2 The on-site visit also serves as a mechanism for discussing weaknesses
identified through the Performance Evaluation sample analysis or
through Contract Compliance Screening or other review of data
deliverables. Lastly, the on-site visit allows the evaluation team to
determine if the laboratory has implemented the recommended and/or
required corrective actions, with respect to quality assurance, made
during the previous on-site visit.

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EXHIBIT F

CHAIN-OF-CUSTODY, DOCUMENT CONTROL,
AND STANDARD OPERATING PROCEDURES

F-l

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1. 
-------
Document Control Procedures

The goal of the laboratory document control program is to assure that
all documents for a specified case will be accounted for when the
project is completed. Accountable documents used by contract
laboratories shall include, but not be limited to, logbooks, chain-
of-custody records, sample work sheets, bench sheets, and other
documents relating to the sample or sample analyses. The following
document control procedures have been established to assure that all
laboratory records are assembled and stored for delivery to EPA or
are available upon request from EPA prior to the delivery schedule.

2.1 Preprinted Data Sheets and Logbooks

Preprinted data sheets shall contain the name of the laboratory and
be dated and signed by the analyst or individual performing the work.
All documents produced by the laboratory which are directly related
to the preparation and analysis of EPA samples shall become the
property of the EPA and shall be placed in the case file. For that
reason, all observations and results recorded by the laboratory but
not on preprinted data sheets are entered into permanent laboratory
logbooks. The person responsible for the work shall sign and date
each entry and/or page in the logbook. When all data from a case is
compiled, copies of all EPA case-related logbook entries shall be
included in the documentation package. Analysts' logbook entries
must be in chronological order and shall include only one case per
page. Instrument? run logs shall be maintained so as to enable a
reconstruction of the run sequences of individual instruments.

Because the laboratory must provide copies of the instrument run logs
to EPA, the laboratory may exercise the option of using only
laboratory or SMO sample identification numbers in the logs for
sample ID rather than government agency or commercial client names.

Using laboratory or SMO sample IDs only in the run sequences will
assist the laboratory in preserving the confidentiality of commercial
clients.

2 . 2 Error Correction Procedure

All documentation in logbooks and other documents shall be in ink.
If an error is made, corrections shall be made by crossing a line
through the error and entering the correct information. Changes
shall be dated and initialed. No information shall be obliterated or

rendered unreadable.

2.3 Consistency of Documentation

Before releasing analytical results, the laboratorysh«U assemble
and cross-check the Information on .ample tags custody records lab
bench sheets, personal and Instrument logs and other relevant data
to ensure thit data pertaining to each particular .ample or case 1.
consistent throughout the ca«e file.

p-3	2/88
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2.4	Document Numbering and Inventory Procedure

In order to provide document accountability of the completed analysis
records, each item in a case shall be inventoried and assigned a
serialized number and identifier associating it to the case and
Region.

Case # - Region • Serialized number (For example: 75-2-0240)

The number of pages of each item must be accounted for if each page
is not individually numbered. All documents relevant to each case,
including logbook pages, bench sheets, mass spectra, chromatograms,
custody records, library search results, etc., shall be inventoried.
The laboratory shall be responsible for ensuring that all documents
generated are placed in the file for inventory and are delivered to
EPA. Figure 1 is an example of a document inventory.

2.5	Shipping Data Packages and Case Files

The Contractor shall have written procedures to document shipment of
deliverables packages to the recipients. Case File Purge shipments
require custody seals on the container(s) placed such that it cannot
be opened without damaging or breaking the seal. The Contractor
shall also document what was sent, to whom, the date, and the method
(carrier) used.

3. Standard Operating Procedures

The Contractor must have written standard operating procedures (SOPs)
for (1) receipt of samples, (2) maintenance of custody, (3) sample
storage, (4) tracking the analysis of samples, and (5) assembly of
completed data.

An SOP is defined as a written narrative step-wise description of
laboratory operating procedures including examples of laboratory
documentation. The SOPs must accurately describe the actual
procedures used in the laboratory, and copies of the written SOPs
shall be available to the appropriate laboratory personnel. These
procedures are necessary to ensure that analytical data produced
under this contract are acceptable for use in EPA enforcement case
preparation and litigation. The Contractor's SOPs shall provide
mechanisms and documentation to meet each of the following
specifications and shall be used by EPA as the basis for laboratory
evidence audits.

3.1	The Contractor shall have a designated sample custodian responsible
for receipt of samples and have written SOPs describing his/her
duties and responsibilities.

3.2	The Contractor shall have written SOPs for receiving and logging in
of the samples. The procedures shall include but not be limited to
documenting the following information:

F-4

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o Presence or absence of EPA chain-of-custody forms
o Presence or absence of airbills

° lists"06 °r abSenCe °f EPA Traffic Reports or SAS packing

o Presence or absence of custody seals on shipping and/or
sample containers and their condition

o Presence or absence of sample tags

o Sample tag ID numbers if not recorded on the chain-of-
custody record(s) or packing list(s)

o Condition of the shipping container

o Condition of the sample bottles

o Verification of agreement or nonagreement of information on
receiving documents

o Resolution of problems or discrepancies with the Sample
Management Office

3.3	The Contractor shall have written SOPs for maintenance of the
security of samples after log-in and shall demonstrate security of
the sample storage and laboratory areas. The SOPs shall specifically
include descriptions of all storage areas for EPA samples in the
laboratory, and steps taken to prevent sample contamination. The
SOPs shall include a list of authorized personnel who have access or
keys to secure storage areas.

3.4	The Contractor shall have written SOPs for tracking the work
performed on any particular sample. The tracking SOP shall include
the following:

3.4.1	a description of the documentation used to record sample
receipt, sample storage, sample transfers, sample
preparations, and sample analyses.

3.4.2	A description of the documentation used to record instrument
calibration and other QA/QC activities.

3.4.3	Examples of the document formats and laboratory documentation
used in the sample receipt, sample storage, sample transfer,
and sample analyses.

3.5	The Contractor shall have written SOPs for organization and assembly
of all documents relating to each EPA case, including technical and
managerial review. Documents shall be filed on a Case-specific
basis. The procedures must ensure that all documents including
logbook pages, sample tracking records, chromatographic charts,
computer printouts, raw data summaries, correspondence, and any other

F-5

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written documents having reference to the Case are compiled in one
location for submission to EPA. The system must include a document
numbering and inventory procedure.

3.6	The Contractor shall have written SOPs for laboratory safety.

3.7	The Contractor shall have written SOPs for cleaning of glassware used
in preparing and analyzing samples under this contract.

3.8	The Contractor shall have SOPs for traceability of standards used in
sample analysis QA/QC.

A. Handling of Confidential Information

A Contractor conducting work under this contract may receive EPA-
designated confidential information from the agency. Confidential
information must be handled separately from other documentation
developed under this contract. To accomplish this, the following
procedures for the handling of confidential information have been
established.

4.1	All confidential documents shall be under the supervision of a
designated document control officer (DCO).

4.2	Confidential Information

Any samples or information received with a request of confidentiality
shall be handled as "confidential." A separate locked file shall be
maintained to store this information and shall be segregated from
other nonconfidential information. Data generated from confidential
samples shall be treated as confidential. Upon receipt of
confidential information, the DCO logs these documents into a
Confidential Inventory Log. The information is then made available
to authorized personnel but only after it has been signed out to that
person by the DCO. The documents shall be returned to the locked
file at the conclusion of each working day. Confidential information
may not be reproduced except upon approval by the EPA Contracting
Officer. The DCO will enter all copies into the document control
system. In addition, this information may not be disposed of except
upon approval by the EPA Contracting Officer. The DCO shall remove
and retain the cover page of any confidential information disposed of
for one year and shall keep a record of the disposition in the
Confidential Inventory Log.

F-6

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Figure 1

Example
DOCUMENT INVENTORY

Document Control #*	Document Tvpb	# Pages

232-2-0001

Case File Document Inventory Sheet

1

232-2-0002

Chain-of-Custody Records

2

232-2-0003

Shipping Manifests

2

232-2-0004

Sample Tags

50

232-2-0005

SMO Inorganics Traffic Reports

10

232-2-0006

GC/MS spectra for sample B0310

20

232-2-0007

GC/MS spectra for sample B0311

20

232-2-0008

GC/MS spectra for sample B0319

20

232-2-0009

Analyst's logbook pages

6

232-2-0010

GC/MS library search worksheets

15

232-2-0011

GC instrument log pages

5

232-2-0012

GC/MS QC data sheets

4

etc.

etc.

etc.

~This number is to be recorded on each set of documents.

F-7

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EXHIBIT 
-------
GLOSSARY OF TERMS

ALIQUOT - a measured portion of a sample taken for analysis.

ANALYSIS DATE/TIME - the date and military time of the Injection of the
sample, standard, or blank into the GC/MS or GC system.

BAR GRAPH SPECTRUM - a plot of the mass-to-charge ratio (m/e) versus relative
intensity of the ion current.

BLANK - see Method Blank

4-BROMOFLUOROBENZENE (BFB) - compound chosen to establish mass spectral
tuning performance for volatile analyses.

CALIBRATION CHECK COMPOUNDS (CCC) - target compounds used to evaluate the
calibration stability (precision) of the GC/MS system. Maximum percent
deviations of the CCCs are defined in the protocol.

CASE - a finite, usually predetermined number of samples collected over a
given time period from a particular site. Case numbers are assigned by the
Sample Management Office. A case consists of one or more Sample Delivery
Groups.

CHARACTERIZATION - a determination of the approximate concentration range of
compounds of interest used to choose the appropriate analytical protocol.

CONCENTRATION LEVEL (low or medium) - characterization of soil samples or
sample fractions as low concentration or medium concentration is made on the
basis of the laboratory's preliminary screen, not on the basis of information
entered on the Traffic Report by the sampler.

CONFIRMATION ANALYSIS - see Primary Analysis.

CONTINUING CALIBRATION - analytical standard run every 12 hours to verify the
calibration of the GC/MS system.

CONTINUOUS LIQUID-LIQUID EXTRACTION - used herein synonymously with the terms
continuous extraction, continuous liquid extraction, and liquid extraction.

DAY - unless otherwise specified, day shall mean calendar day.

DECAFLUOROTRIPHENYLPHOSPHINE (DFTPP) - compound chosen to establish mass
spectral tuning performance for semivolatile analysis.

EXTRACTABLE - a compound that can be partitioned into an organic solvent from
the sample matrix and is amenable to gas chromatography. Extractables
include BNA and pesticide/PCB compounds.

IN-HOUSE - at the Contractor's facility.

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INITIAL CALIBRATION - analysis of analytical standards for a series of
different specified concentrations; used to define the linearity and dynamic
range of the response of the mass spectrometer to the target compounds.

INTERNAL STANDARDS - compounds added to every standard, blank, matrix spike,
matrix spike duplicate, sample (for VOAs), and sample extract (for
semivolatiles) at a known concentration, prior to analysis. Internal
standards are used as the basis for quantitation of thd target compounds.

LABORATORY - synonymous with Contractor as used herein.

MATRIX - the predominant material of which the sample to be analyzed is
composed. For the purpose of this SOW, a sample matrix is either water or
soil/sediment. Matrix is not synonymous with phase (liquid or solid).

MATRIX SPIKE - aliquot of a matrix (water or soil) fortified (spiked) with
known quantities of specific compounds and subjected to the entire analytical
procedure in order to indicate the appropriateness of the method for the
matrix by measuring recovery.

MATRIX SPIKE DUPLICATE - a second aliquot of the same matrix as the matrix
spike (above) that is spiked in order to determine the precision of the

method.

METHOD BLANK (previously termed reagent blank) - an analytical control
consisting of all reagents, internal standards and surrogate standards, that
is carried through the entire analytical procedure. The method blank is used
to define the level of laboratory background contamination.

NARRATIVE (Case Narrative) - portion of the data package which Includes
laboratory contract, Case and sample number identification, and descriptive
documentation of any problems encountered in processing the samples, along
with corrective action taken and problem resolution. Complete Case Narrative
specifications are included in Exhibit B.

PERCENT MOISTURE - an approximation of the amount of water in a soil/sediment
sample made by drying an aliquot of the sample at 105 C. The percent
moisture deterained in this manner also includes contributions from all
compounds that may volatilize at 105*C, including water. Percent moisture is
determined from decanted samples and from samples that are not decanted.

PRIMARY ANALYSIS - one of two types of pesticide/PCB analysis by GC/EC
PRIMARY ANALYSIS one	the confirmation Analysis. If the two analyses

fchniqu.., th. othar b.lng tha^onl	^ £lr,t ,„ly,ls

•ra run at aapara	.	aatabllah th* tantativa Identification of any

chronologically, and la uaadto	^	ln th.

« th. wo analyaaa «. ataultanaoua. aithar may b«

considered the Primary Analysis.

a.u	nrocedures to be followed with respect to

BtOTOCOL - daacrlbaa	Lthoda. data raportlng alui

aanpla racalpt	" '	u»ad aynonymoualy with Stataoant of Work

deliverables, and document control..	J J

(SOW).

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PURGE AND TRAP (DEVICE) • analytical technique (device) used to Isolate
volatile (purgeable) organlcs by stripping the compounds from water or soil
by a stream of Inert gas, trapping the compounds on a porous polymer trap,
and thermally desorblng the trapped compounds onto the gas chromatographic
column.

REAGENT WATER - water In which an interferent Is not observed at or above the
minimum quantitation limit of the parameters of Interest.

RECONSTRUCTED ION CHROMATOGRAM (RIC) - a mass spectral graphical
representation of the separation achieved by a gas chromatograph; a plot of
total Ion current versus retention time.

RECOVERY - a determination of the accuracy of the analytical procedure made
by comparing measured values for a fortified (spiked) sample against the
known spike values. Recovery is determined by the following equation:

measured value
%Rec ~ known value * 100%

RELATIVE RESPONSE FACTOR (RRF) - a measure of the relative mass spectral
response of an analyte compared to its Internal standard. Relative Response
Factors are determined by analysis of standards and are used in the
calculation of concentrations of analytes in samples. RRF is determined by
the following equation:

RRF -
Where

it x is

Ais

A — area of the characteristic ion measured

C — concentration

is - internal standard

x — analyte of Interest

RESOLUTION - also termed separation, the separation between peaks on a
chromatogram, calculated by dividing the height of the valley between the
peaks by the peak height of the smaller peak being resolved, multipled by
100.

SAMPLE - a portion of material to be analyzed that is contained in single or
multiple containers and identified by a unique sample number.

SAMPLE DELIVERY GROUP (SDG) - a unit within a single Case that is used to
Identify a group of samples for delivery. An SDG is a group of 20 or fewer
field samples within a Case, received over a period of up to 14 calendar
days. Data from all samples in an SDG are due concurrently. A Sample
Delivery Group is defined by one of the following, whichever occurs first:

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o Ctu; or

o Each 20 field samples within a Case; or

o Each 14-day calendar period during which field samples in a Case are
received, beginning with receipt of the first sample in the Case or SDG.

Samples may be assigned to Sample Delivery Groups by matrix (i.e., all soils
In one SDG, all waters in another), at the discretion of the laboratory.

SAMPLE NUMBER (EPA Sample Number) - a unique identification number designated
by EPA for each sample. The EPA sample number appears on the sample Traffic
Report which documents information on that sample.

SEMIVOLATILE COMPOUNDS - compounds smenable to analysis by extraction of the
sample with an organic solvent. Used synonymously with Base/Neutral/Acid
(BNA) compounds.

SOIL - used herein synonymously with soil/sediment and sediment.

STANDARD ANALYSIS - an analytical determination made with known quantities of
target compounds; used to determine response factors.

SURROGATES (Surrogate Standard) - compounds added to every blank, sample,
matrix spike, matrix spike duplicate, and standard; used to evaluate
analytical efficiency by measuring recovery. Surrogates are brominated,
fluorlnated, or isotoplcally labelled compounds not expected to be detected
in environmental media.

SYSTEM PERFORMANCE CHECK COMPOUNDS (SPCC) - target compounds designated to
aonltor chromatographic performance, sensitivity and compound instability or
degradation on active sites. Minimum response factor criteria for the SPCCs
are defined in the protocol.

TARGET COMPOUND LIST .(TCL) - a list of compounds designated by the Statement
of Vork (Exhibit C) for analysis.

TENTATIVELY IDENTIFIED COMPOUNDS (TIC) - compounds detected in samples that
are not target compounds, internal standards or surrogate standards. Up to
30 peaks (those greater than 10% of peak areas or heights of nearest internal
standards) are subjected to mass spectral library searches for tentative
idantification.

TIME - when required to record time on any deliverable item, time shall be
expressed as Military Time, i.e., a 24-hour clock.

TRAFFIC REPORT (TR) - an EPA sample identification form filled out by the
sampler, which accompanies the sample during shipment to the laboratory and
which documents sampla condition and receipt by the laboratory.

TWELVE-HOUR TIME PERIOD - The twelve (12) hour time period for GC/MS system
tuning, standards calibration (initial or continuing calibration), and method
blank analysis begins at the moment of injection of the DFTPP or BFB analysis
that the laboratory submits as documentation of compliant tune. The time
p«iod Inds afte/l2 hour, has -lapsed according to the system clock.

G-5

2/88
-------
VALIDATED TIME OF SAMPLE RECEIPT (VTSR) - the data on which a saopl* is
received at Che Contractor'* facility, as recorded on the shipper's delivery
receipt and Sample Traffic Report.

VOLATILE COMPOUNDS - compounds amenable to analysis by the purge and trap
technique. Used synonymously with purgeable compounds.

WIDE BORE CAPILLARY COLUMN - a gas chromatographic column with an internal
diameter (ID) that is greater than 0.32 mm. Columns with lesser diameters
are classified as narrow bore capillaries.

G-6

Rev. 9/88
-------
EXHIBIT H

DATA DICTIONARY AND FORMAT FOR DATA
DELIVERABLES IN COMPUTER-READABLE FORMAT

SECTION I: Description of Deliverables 	H-2

SECTION II: Format A Specifications 	H-3

SECTION III: Format B Specifications 	H-63

H-l	2/88
-------
SECTION I

npgrRTPTIOK of DELIVERABLE

1.	Introduct-1 on

1.1	Two file formats are specified for delivery of computer-readable data.
Format A Is oriented to the structure of the hardcopy reporting forms
required by the contract. Format B is oriented to the general data
required by the contract. Information sufficient to generate required
hardcopy forms is contained in either format.

1.2	The file or files for a Sample Delivery Group (SDG, see Exhibit A,
Section I, B) must be submitted on a diskette or diskettes (see
Deliverable, 2.1). Information on a diskette or diskettes for any
single SDG must be in one, and only one, of the two formats. The
format used is at the option of the laboratory. The option used must
be included in the File Name specification (paragraph 2.2).

1.3	Format A consists of variable length ASCII records, and Format B
consists of fixed-length 80-byte ASCII records.

1.4	All information for one SDG must be in one file If format A is used.
Use of Format B may require information for one SDG to be in a number
of files. Format; B may require more than one 360 K diskette for a
valid SDG.

2.	DclivgraMg

2.1	The file or files must be submitted on a 5-1/4 inch floppy diskette,
which may be either a double-sided, double density, 360 K-byte or a
high capacity 1.2 N-byte diskette. The diskette or diskettes must
contain all information relevant to one and only one SDG, and must
accompany the hardcopy package for the SDG submitted to the Sample
Management Office (see Exhibit B). Information on the diskette or
diskettes must correspond exactly with information submitted in the
hardcopy data package and on the hardcopy data package forms. Blank or
unused records in either format should not be Included on the
diskettes.

2.2	Each diskette must be Identified with an external label containing (in
this order) the following information:

Disk Density
File Name(s)

Laboratory Name (optional)

Laboratory Code
Case Number (where applicable)

SAS Number (where applicable)

H- 2

2/88
-------
The format for the File Name(s) must be XXXXX.ONY

where XXXXX is the SDG identifier

0	indicates Organics analysis

N	is a continuation number used to identify

multiple files corresponding to the same SDG.
For Format A, "N" must be "1". For Format B,
"N" must be "1" for the only, or first file of
the SDG, and must be incremented to "2", "3",
etc., for subsequent files of the SDG. "N"
cannot be greater than 9

Y	is "A" for Format A

or "B" for Format B

Dimensions of the label must be in the range 4-3/4" to 5" long by 1-1/4
to 1-1/2" wide.

H-2a

Rev. 4/89
-------
SECTION II

FORMAT A SPECTFTrATTfiM

1.	Format: Characteristics

1.1	Format A is based upon the structure of the hardcopy reporting forms
required by the contract. With two exceptions, Form Suffix and Record
Type, all fields in the fornat correspond directly with entries or
items on the hardcopy forms. The record structure is obtained by
taking entries in sequence from the appropriate hardcopy form. For
example, the Header record (page H-7) from Form 1A is a concatenation
of all entries on the hardcopy form that precede the reported results
and qualifiers.

1.2	All Format A fields are character. Alphanumeric values should be left
justified and numeric values should be right justified in appropriate
fields. Field lengths are such that all possible valid values can be
written to the file. The maximum format is specified for each field.
For example, "Numeric 13.3" is specified for "Result" on Detail Record
D1 of Form 1A (see page H-7). Numeric values reported may take any
form (e.g., integer 13, integer 3, real 13.3, real 5.1, etc.) provided
they do not exceed the specifications. (Requirements for the number of
significant figures to be reported on the appropriate hardcopy form are
given in the Form Instruction Guide, Exhibit B, Section III.)

2.	RgCgrfl lYPM

2.1	Format A consists of variable length ASCII records. The last two bytes
of each record must contain "carriage return" and "line feed",
respectively. Unused bytes in partially filled fields must be blank-
filled.

2.2	Format A has three types of records: Header Records, Detail Records
and Comment Records.

Typg

Header

Typg IP

H

C
-------
3.

Record Length

Table 3.1 summarizes the length and (in parantheses) the number of
records in Format A. The maximum number of detail and comment records
is shown, corresponding to a submission of hardcopy forms on which
information is written on all possible lines. The Form Totals are the
maximum lengths (excluding carriage return/line feed) required for a
complete set of each type of form.

Table 3 1 Formal- A Snimpflrv

Form

Record



Header





HI

121

1A

153a(l)b

35(34)

IB

168 (1)

35(33)

1C

168 (1)

35(32)

ID

168 (1)

35(27)

IE

155 (1)

71(30)

IF

170 (1)

71(30)

1(Total)

982 (6)

8670(186)

2A

67(1)

37(30)

2B

70(1)

37(30)

2C

67(1)

49(30)

2D

70(1)

49(30)

2E

67(1)

28(30)

2F

70(1)

28(30)

2(Total)

411(6)

6840(180)

3A

85(1)

70( 5)

3B

84(1)

70( 5)

3C

85(1)

70(11)

3D

88(1)

70(11)

3E

85(1)

70( 6)

3F

988(1)

70( 6)

3(Total)

519(6)

3080(44)

4A

123(1)

51(30)

4B

135(1)

55(30)

4C

177(1)

49(26)

4(Total)

435(3)

4454(86)

SA

115(1)

20(9)

5B

103(1)

21(13)

5(Total)

218(2)

453(22)

HI

Comment

£1

£2

61( 5)

72(1)

72(1)

61( 5)

72(1)

72(1)

61(11)

72(1)

72(1)

61(11)

72(1)

72(1)

61( 6)

72(1)

72(1)

61 ( 6)

72(1)

72(1)

2684(44)

432(6)

432(6)

72(1)

72(1)



72(1)

72(1)



72(1)

72(1)



216(3)

216(3)



59(24)





59(22)





2714(46)





H-4

2/88
-------
Form

Table 3.1 Format A Sin—rv
	Record



Header

Detail





HI

121

122

6A

173(1)

69(37)



6B

161(1)

69(37)



6C

161(1)

69(36)



6(Total)

495(3)

7590(110)



7A

129(1)

49(37)



7B

117(1)

49(37)



7C

117(1)

49(36)



7(Total)

363(3)

5390(110)



8A

115(1)

106(1)

69(26)

8B

103(1)

106(1)

69(22)

8C

103(1)

106(1)

69(22)

8D

101(1)

58(4)

36(14)

8E

103(1)

51(38)



8(Total)

525(5)

2488(45)

5334(84)

9

135(1)

72(27)



9(Total)

135(1)

1944(27)



10

145(1)

43(6)

43(6)

10(Total)

145(1)

258(6)

258(6)

Comment

£1

£2

72(1)
72(1)

72(1)
72(1)

b -	number of record* required for a form.

4.	Form Suffix

The fourth end fifth byte* of each record contain the form suffix (AA-
22) which must be unique (within a type of form (e.g., Form IA, Form
IIC* etc ) for each set of records that corresponds to one hardcopy
form. For example, the form suffix for records for the first
occurrence in the file of a Form 1C must be AA. The sedond occurrence
must be AB, and the twenty-eighth must be BA.

5.	tt.rnrd Listing

The remainder of thia section contains detailed specifications for
every record required for a full set of hardcopy forms.

H-5

2/88
-------
FORM I FILE DESCRIPTION
(FORM1)

H - 6

1/87 REV.
-------
VOLATILE 0R9ANICS ANALYSIS DATA SHEET - (FORM 1A)

HEADER RECORD 1 (HI)

COLUMN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

1- 3

3

FORM NUMBER

•1A*

4- 5

2

FORM SUFFIX

•AA'-'ZZ*

4- 7

2

RECORD TYPE

•HI'

e- 19

12

EPA SAMPLE NO.



20- 44

25

LAB NAME



45- 35

11

CONTRACT



56- (I

6

LAB CODE



62- 66

5

CASE NO.



67- 72

6

SAS NO.



73- 77

5

SDG NO.



78- 82

5

MATRIX

•SOIL ' OR 'HATER•

83- 94

12

LAB SAMPLE ID



95- 99

5

SAMPLE HT/VOL

NUMERIC 5.1

100-101

2

SAMPLE HT/VOL UNITS

•G • OR 'ML*

102-115

14

LAB FILE ID



116-118

3

LEVEL

•LOW' OR 'MED'

119-126

8

DATE RECEIVED

MM/DD/YY

127-128

2

XMOISTURE NOT DEC

NUMERIC 2

129-136

8

DATE ANALYZED

MM/DD/YY

137-140

4

COLUMN

•PACK' OR 'CAP •

141-148

8

DILUTION FACTOR

NUMERIC 8

149-153

5

CONCENTRATION UNITS

•UG/L ' OR 'UG/KG'

DETAIL RECORD 1 (Dl>





COLUMN CS>

LENGTH

CONTENTS

FORMAT/CONTENTS

1-3

3

FORM NUMBER

•1A*

4-5

2

FORM SUFFIX

•AA'-'ZZ*

6-7

2

RECORD TYPE

•Dl'

8-17

10

CAS NO.



18-30

13

RESULT

NUMERIC 13.3

31-35

5

QUALIFIER (Q)



H - 7	1/87 REV.
-------
SEHXVOLATXLE

ORGANICS

ANALTSIS DATA SHEET -

(FORM IB)

HEADER RECORD

i 1 (HI)





COLUMN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

	_______

	

———————————

	 	

1- 3

3

FORM NUMBER

' IB'

4- 5

2

FORM SUFFIX

'AA'-'ZZ*

6- 7

2

RECORD TYPE

•HI*

8- 19

12

EPA SAMPLE NO.



20- 44

25

LAB NAME



45- 55

11

CONTRACT



56- 61

6

LAB CODE



62- 66

5

CASE NO.



67- 72

6

SAS NO.



73- 77

5

SDG NO.



78- 82

5

MATRIX

•SOIL ' OR 'HATER'

83- 94

12

LAB SAMPLE ID



95- 99

5

SAMPLE HT/VOL

NUMERIC 5.1

100-101

2

SAMPLE HT/VOL UNITS

•G * OR 'ML'

102-115

14

LAB FILE ID



116-118

3

LEVEL

•LOH* OR 'MED'

119-126

8

DATE RECEIVED

MM/DD/YY

127-128

2

X MOISTURE NOT DEC

NUMERIC 2

129-130

2

X MOISTURE DEC

NUMERIC 2

131-138

8

DATE EXTRACTED

MM/DD/YY

139—142

4

EXTRACTION

*SEPF *, 'CONT' OR 'SONC'

143-150

8

DATE ANALYZED

MM/DD/YY

151

1

GPC CLEANUP

•Y' OR 'N'

152-155

4

PH

NUMERIC 4.1

156-163

8

DILUTION FACTOR

NUMERIC 8

164-168

5

CONCENTRATION UNITS

•UG/L ' OR 'UG/KG'

DETAIL RECORD 1 (Dl)





COLUMN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

——————

— — — —

— — — — — — — —— — — — — ——

———— 	_____________

1- 3

3

FORM NUMBER

'IB'

4- 5

2

FORM SUFFIX

'AA'-'ZZ*

6- 7

2

RECORD TYPE

'Dl'

8-17

10

CAS NO.

18-30

13

RESULT

NUMERIC 13.3

31-35

5

QUALIFIER (Q)



H - 8	1/87 REV.
-------
SEMIVOLATILE ORGANICS ANALYSIS DATA SHEET - (FORM 1C)

HEADER RECORD 1 (HI)

COLUMN (S) LENGTH CONTENTS

1-
4-
6-
8-
20-
45-
56-
62-
67-
73-
78-
83-
95-
100-
102-
116-
119-
127-
129-
131-
139-
143-

152-
156-
164-

3
5
7
19
44
55
61
66
72
77
82
94
99
101
115
118
126
128
130
138
142

150

151
155
163
168

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE

12	EPA SAMPLE NO.

25	LAB NAME

11	CONTRACT
6	LAB CODE

5	CASE NO.

6	SAS NO.
5	SDG NO.
5	MATRIX

12	LAB SAMPLE ID
5	SAMPLE MT/VOL

2	SAMPLE MT/VOL UNITS
LAB FILE ID

3	LEVEL

8	DATE RECEIVED

2	X MOISTURE NOT DEC

2	X MOISTURE DEC

8	DATE EXTRACTED

4	EXTRACTION

8	DATE ANALYZED

I	GPC CLEANUP

it	PH

8	DILUTION FACTOR

5	CONCENTRATION UNITS

FORMAT/CONTENTS
'1C'

•AA'-'ZZ'

'HI *

•SOIL * OR 'HATER *

NUMERIC 5.1
*G ' OR 'ML'

'LOW OR 'MED*

MM/DD/YY
NUMERIC 2
NUMERIC 2
MM/DD/YY

'SEPF'» 'CONT' OR 'SONC'

MM/DD/YY

'Y * OR 'N'

NUMERIC 4.1

NUMERIC 8

•UG/L ' OR 'UG/KG*

DETAIL RECORD 1 (Dl>

COLUMN 	LENGTH

1-3	3

4-5	2

6-7	2

8-17	10

18-30	13

31-35	5

CONTENTS

FORM NUMBER
FORM SUFFIX
RECORD TYPE
CAS NO.

RESULT

QUALIFIER (Q)

FORMAT/CONTENTS
• ic

•AA'-'ZZ*

' D1 •

NUMERIC 13.3

H - 9

1/87 REV.
-------
PESTICIDE ORGANICS ANALYSIS DATA SHEET - (FORM ID)

HEADER RECORD 1 (HI)

IOLUNN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

1- 3

3

FORM NUMBER

• ID'

4- 5

2

FORM SUFFIX

•AA'-'ZZ*

6- 7

2

RECORD TYPE

•HI*

8- 1?

12

EPA SAMPLE NO.



20- 44

25

LAB NAME



45- 55

11

CONTRACT



56- 61

6

LAB CODE



62- 66

5

CASE NO.



67- 72

6

SAS NO.



73- 77

5

SDG NO.



78- 82

5

MATRIX

•SOIL * OR •WATER'

83- 94

12

LAB SAMPLE ID



95- 99

5

SAMPLE WT/VOL

NUMERIC 5.1

100-101

2

SAMPLE WT/VOL UNITS

'G ' OR * ML *

102-115

14

LAB FILE ID



116-118

3

LEVEL

•LOW' OR 'MED*

119-126

8

DATE RECEIVED

MM/DD/YY

127-128

2

X MOISTURE NOT DEC

NUMERIC 2

129-130

2

X MOISTURE DEC

NUMERIC 2

131-138

8

DATE EXTRACTED

MM/DD/YY

139-142

4

EXTRACTION

•SEPF'» 'CONT' OR 'SONC'

143-150

8

DATE ANALYZED

MM/DD/YY

151

1

GPC CLEANUP

•Y * OR * N *

152-155

4

PH

NUMERIC 4.1

156-163

8

DILUTION FACTOR

NUMERIC 8

164-168

5

CONCENTRATION UNITS

•UG/L * OR *UG/KG'

DETAIL RECORD 1 (Dl)

COLUMN (S)	LENGTH

1-3	3

4-5	2

6-7	2

8-17	10

18-30	13

31-35	5

CONTENTS

FORM NUMBER
FORM SUFFIX
RECORD TYPE
CAS NO.

RESULT

QUALIFIER (Q)

FORMAT/CONTENTS
•ID*

'AA'-'ZZ'

•Dl'

NUMERIC 13.3

H - 10	1/87 REV,
-------
VOLATILE ORGANICS ANALYSIS DATA SHEET - (FORM IE)
TENTATIVELY IDENTIFIED COHPOUNDS

HEADER RECORD I (HI)

COLUMN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

——————————

—————

	———	



1-

- 3

3

FORM NUMBER

* IE *

4- 5

2

FORM SUFFIX

•AA'-'ZZ'

6-

- 7

2

RECORD TYPE

•HI *

8-

- 19

12

EPA SAMPLE NO.



20-

- 44

2 •»

LAB NAME



45-

- 55

11

CONTRACT



56-

- 61

6

LAB CODE



62-

- 66

5

CASE NO.



67-

¦ 72

6

SAS NO.



73-

- 77

5

SDG NO.



78-

¦ 82

5

MATRIX

'SOIL * OR 'WATER'

83-

¦ 94

12

LAB SAMPLE ID



95- 99

5

SAMPLE WT/VOL

NUMERIC 5.1

100-

¦101

2

SAMPLE NT/VOL UNITS

'G ' OR 'ML'

102-

¦115

14

LAB FILE ID



116-

-118

3

LEVEL

•LOW OR 'MED*

119-

-126

8

DATE RECEIVED

MM/DD/YY

127-128

2

X MOISTURE NOT DEC

NUMERIC 2

129-136

8

DATE ANALYZED

MM/DD/YY

137-

140

4

COLUMN

•PACK' OR 'CAP '

141-

148

8

DILUTION FACTOR

NUMERIC 8

149-

150

2

NUMBER TICS FOUND

NUMERIC 2

151-

155

5

CONCENTRATION UNITS

•UG/L * OR 'UG/KG'

DETAIL RECORD

1 (Dl)





COLUMN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

1-

3

3

FORM NUMBER

'IE'

4-

5

2

FORM SUFFIX

•AA'-'ZZ'

6-

7

2

RECORD TYPE

• Dl *

8-

9

2

SEQUENCE NUMBER

NUMERIC 2

10-

19

10

CAS NO.



20-

47

28

COMPOUND



48-

53

6

RT

NUMERIC 6.2

54-

66

13

ESTIMATED CONCENTRATION

NUMERIC 13.3

6 7-

71

5

QUALIFIER (Q)



H - 11

1/87 REV.
-------
SEMIVOLATILE ORCANICS ANALYSIS DATA SHEET - (FORM IF)
TENTATIVELY IDENTIFIED COMPOUNDS

HEADER RECORD 1 (HI)

COLUMN CS)

LENGTH

CONTENTS

1- 3

3

FORM NUMBER

4- 5

2

FORM SUFFIX

6- 7

2

RECORD TYPE

8- 19

12

EPA SAMPLE NO.

20- 44

25

I.AB NAME

45- 55

11

CONTRACT

56- 61

6

LAB CODE

62- 66

5

CASE NO.

67- 72

6

SAS NO.

73- 77

5

SDG NO.

78- 82

5

MATRIX

83- 94

12

LAB SAMPLE ID

95- 99

5

SAMPLE HT/VOL

100-101

2

SAMPLE HT/VOL UNITS

102-115

14

LAB FILE ID

116-118

3

LEVEL

119-126

8

DATE RECEIVED

127-128

2

X MOISTURE NOT DEC

129-130

2

X MOISTURE DEC

131-138

8

DATE EXTRACTED

139-142

4

EXTRACTION

143-150

8

DATE ANALYZED

151

1

GPC CLEANUP

152-155

4

PH

156-163

8

DILUTION FACTOR

164-165

2

NUMBER TICS FOUND

166-170

5

CONCENTRATION UNITS

FORMAT/CONTENTS
* IF *

•AA'-'ZZ'

•HI*

•SOIL ' OR 'HATER'

NUMERIC 5.1
•G ' OR 'ML'

'LOH' OR 'MED'

MM/DD/YY
NUMERIC 2
NUMERIC 2
MM/DD/YY

'SEPF'» *CONT' OR 'SONC'

MM/DD/YY

'Y* OR 'N *

NUMERIC 4.1

NUMERIC 8

NUMERIC 2

•UG/L ' OR 'UG/KG'

DETAIL RECORD 1 (Dl)

COLUMN (S) LENGTH CONTENTS

1- 3

3

4- 5

2

6- 7

2

8- 9

2

10-19

10

20-47

28

48-53

6

54-66

13

67-71

5

FORM NUMBER
FORM SUFFIX
RECORD TYPE
SEQUENCE NUMBER
CAS NO.

COMPOUND
RT

ESTIMATED CONCENTRATION
QUALIFIER 
-------
FORM IX FILE DESCRIPTION
(FORM2)

H -

13

1^87 REV.
-------
HATER VOLATILE SURROGATE RECOVERY - (FORM 2A)

HEADER RECORD 1 (HI)

COLUMN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

1- 3

3

FORM NUMBER

' 2A'

4- 5

2

FORM SUFFIX

*AA'-•ZZ*

6- 7

2

RECORD TYPE

'HI'

8-32

25

LAB NAME



33-43

11

CONTRACT



44-49

6

LAB CODE



50-54

5

CASE NO.



55-60

6

SAS NO.



61-65

5

SDG NO.



66

1

PAGE

NUMERIC 1

67

1

OF

NUMERIC 1

DETAIL RECORD 1 (Dl)





COLUMN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

	——

	

————	—	—	—_



1- 3

3

FORM NUMBER

' 2A *

4- 5

2

FORM SUFFIX

•AA'-'ZZ'

6- 7

2

RECORD TYPE

•Dl*

8- 9

2

SEQUENCE NUMBER

NUMERIC 2

10-21

12

EPA SAMPLE NO.



22-24

3

SI (TOL)

NUMERIC 3

25
26-28
29
30-32
33
34-36
37

3
1

51	OUT FLAG

52	(BFB)

52	OUT FLAG

53	(DCE)

S3 OUT FLAG
OTHER
TOTAL OUT

BLANK OR 'D* OR '«'
NUMERIC 3
BLANK OR *D' OR
NUMERIC 3
BLANK OR 'D' OR
NUMERIC 3
NUMERIC 1

H - 14

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SOIL VOLATILE SURROGATE RECOVERY - (FORM 2B)

HEADER RECORD 1 (HI)

COLUMN CS) LENGTH CONTENTS

1- 3
4- 5
6- 7
8-32
33-43
44-49
50-54
55-60
61-65
66-68

69

70

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE
25	LAB NAME

11	CONTRACT

6	LAB CODE

5	CASE NO.

6	SAS NO.
5	SDG NO.

3	LEVEL
1	PAGE

1	OF

FORMAT/CONTENTS
' 2B'

* AA'-'ZZ *

'HI'

'LOW* OR
NUMERIC 1
NUMERIC 1

MED'

DETAIL RECORD 1 (Dl)

%

COLUMN (S) LENGTH CONTENTS

1- 3
4- 5
6- 7
8- 9
10-21
22-24
25
26-28
29
30-32
33
34-36
37

3
2
2
2

FORM NUMBER
FORM SUFFIX
RECORD TYPE
SEQUENCE NUMBER
EPA SAMPLE NO.
SI (TOL)

51	OUT FLAG

52	(BFB)

52	OUT FLAG

53	(DCE)

S3 OUT FLAG
OTHER
TOTAL OUT

FORMAT/CONTENTS

•	2B'

•	AA * - * ZZ'

•	Dl*

NUMERIC 2
NUMERIC 3

BLANK OR 'D' OR '*•
NUMERIC 3

BLANK OR 'D' OR •«'
NUMERIC 3

BLANK OR 'D* OR '*•
NUMERIC 3
NUMERIC 1

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HATER SEMIVOLATILE SURROGATE RECOVERY - (FORM 2C)

HEADER RECORD 1 (HI)

COLUMN (S) LENGTH CONTENTS

I- 3
4- 5
6- 7
8-32
33-43
44-4 9
50-54
55-60
61-65

66

67

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE

25	LAB NAME

11	CONTRACT

6	LAB CODE

5	CASE NO.

6	SAS NO.
5	SDG NO.
1	PAGE

1	OF

FORMAT/CONTENTS
* 2C *

'AA'-'ZZ'
•HI*

NUMERIC 1
NUMERIC 1

DETAIL RECORD 1 (Dl)

COLUMN  LENGTH CONTENTS	FORMAT/CONTENTS

1- 3

3 FORM NUMBER

' 2C'





4- 5

2 FORM SUFFIX

•AA'-'ZZ*





6- 7

2 RECORD TYPE

• Dl*





8- 9

2 SEQUENCE NUMBER

NUMERIC 2





10-21

12 EPA SAMPLE NO.







22-24

3 SI (NBZ)

NUMERIC 3





25

1 SI OUT FLAG

BLANK OR 'D*

OR

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26-28

3 S2 (FBP)

NUMERIC 3





29

1 S2 OUT FLAG

BLANK OR 'D*

OR



30-32

3 93 < TPH)

NUMERIC 3





33

1 S3 OUT FLAG

BLANK OR 'D*

OR



34-36

3 S4 CPHL)

NUMERIC 3





37

1 S4 OUT FLAG

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OR



38-40

3 S5 (2FP)

NUMERIC 3





41

1 S5 OUT FLAG

BLANK OR 'D'

OR

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42-44

3 S6 (TBP)

NUMERIC 3





45

1 S6 OUT FLAG

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OR

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46-48

3 OTHER

NUMERIC 3





49

1 TOTAL OUT

NUMERIC 1





H - 16

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SOIL SEMIVOLATILE SURROGATE RECOVERY - (FORM 2D)

HEADER RECORD 1 (HI)

COLUMN (S) LENGTH CONTENTS

1- 3
4- 5
6- 7
8-32
33-43

50-54
55-60
61-65
66-68

69

70

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE
25	LAB NAME

11	CONTRACT

6	LAB CODE

5	CASE NO.

6	SAS NO.
5	SDG NO.

3	LEVEL
1	PAGE
1	OF

FORMAT/CONTENTS

•	2D'

*	AA'-'22 *

•HI •

'LOW OR 'MED'
NUMERIC 1
NUMERIC 1

DETAIL RECORD 1 (Dl)

COLUMN (S) LENGTH CONTENTS

1- 3
4- 5
6- 7
8- 9
10-21
22-24
25
26-28
29
30-32
33
34-36
37
38-40
41
42-44
45
46-48
49

3
2
2

2

12

3

3
1

FORM NUMBER
FORM SUFFIX
RECORD TYPE
SEQUENCE NUMBER
EPA SAMPLE NO.
SI (NBZ)

51	OUT FLAG

52	(FBP)

52	OUT FLAG

53	(TPH)

53	OUT FLAG

54	(PHL)

54	OUT FLAG

55	<2FP)

55	OUT FLAG

56	(TBP)

S6 OUT FLAG
OTHER
TOTAL OUT

FORMAT/CONTENTS
'2D'

'AA'-'ZZ*

•Dl'

NUMERIC 2

NUMERIC 3
BLANK OR 'D' OR
NUMERIC 3

BLANK OR *D' OR '«•

NUMERIC 3

BLANK OR *D* OR '«'
NUMERIC 3
BLANK OR 'D' OR
NUMERIC 3

BLANK OR *D* OR '*'
NUMERIC 3
BLANK OR *D' OR
NUMERIC 3
NUMERIC 1

H - 17

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HATER PESTICIDE SURROGATE RECOVERY - (FORM 2E)
HEADER RECORD 1 (HI)

COLUMN (S) LENGTH CONTENTS

FORMAT/CONTENTS

1- 3
<~- 5
6- 7
8-32
33-43
44-49
50-54
55-60
61-65

66

67

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE

25	LAB NAME

11	CONTRACT

6	LAB CODE

5	CASE NO.

6	SAS NO.
5	SD6 NO.
1	PAGE

1	OF

,2E*

•AA'-'ZZ*
•HI*

NUMERIC 1
NUMERIC 1

DETAIL RECORD 1 (Dl)

COLUMN (S)

LENGTH CONTENTS

FORMAT/CONTENTS

1- 3
4- 5
6- 7
8- 9
10-21
22-24
25
26-28

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE

2	SEQUENCE NUMBER
12	EPA SAMPLE NO.

3	SI (DBC)

1	SI OUT FLAG

3	OTHER

ZZ'

* ZE'
'AA'-'
*D1 •

NUMERIC 2

NUMERIC 3
BLANK OR 'D'
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OR

H - 18

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SOIL PESTICIDE SURROGATE RECOVERY - (FORM 2F)

HEADER RECORD I (HI)
COLUMN (S) LENGTH

1- 3
4- 5
6- 7
8-32
33-43
44-49
50-54
55-60
61-65
66-68

69

70

3
2

2
25
11

6

5

6
5

3
1
1

DETAIL RECORD 1 (Dl)
COLUMN (S) LENGTH

1- 3
4- 5
6- 7
8- 9
10-21
23-24
25
26-26

3
2
2

2

12

3
1
3

CONTENTS

FORM NUMBER
FORM SUFFIX
RECORD TYPE
LAB NAME
CONTRACT
LAB CODE
CASE NO.
SAS NO.
SDG NO.
LEVEL
PAGE
OF

CONTENTS

FORM NUMBER
FORM SUFFIX
RECORD TYPE
SEQUENCE NUMBER
EPA SAMPLE NO.
SI (DBC)

SI OUT FLAG
OTHER

FORMAT/CONTENTS

* 2F'

'AA'-'ZZ*
'HI *

•LOW OR
NUMERIC 1
NUMERIC 1

MED1

FORMAT/CONTENTS
• 2F *

' AA * -'ZZ'

•Dl*

NUMERIC 2

NUMERIC 3
BLANK OR 'D*
NUMERIC 3

OR

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FORM III FILE DESCRIPTION
(FORPI3)

H - 20

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HATER VOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY - CFORM3A)

HEADER RECORD 1 (HI)

COLUMN (S)

LENGTH

CONTENTS

	

—	

	

1- 3

3

FORM NUMBER

4- 5

2

FORM SUFFIX

6- 7

2

RECORD TYPE

8-32

25

LAB NAME

33-43

11

CONTRACT

44-49

6

LAB CODE

50-54

5

CASE NO.

55-60

6

SAS NO.

61-65

5

SDG NO.

66-77

12

MATRIX SPIKE -





EPA SAMPLE NO.

78-79

2

RPD* * OUTSIDE QC LIMITS

80-81

2

RPD: TOTAL

82-83

2

SPIKE RECOVERY: • OUT

84-85

2

SPIKE RECOVERY: TOTAL

DETAIL RECORD

1 (Dl)



COLUMN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

' 3A*
'AA*-'
'HI *

ZZ'

NUMERIC 2
NUMERIC 2
NUMERIC 2
NUMERIC 2

FORMAT/CONTENTS

1- 3

3

4- 5

2

«- 7

2

8-31

24

32-40

9

41-53

13

54-66

13

67-69

3

70

1

FORM NUMBER
FORM SUFFIX
RECORD TYPE
COMPOUND

SPIKE ADDED (UG/L)
SAMPLE CONC. (UG/L)
MS CONC.(UG/L)
MSX REC.

MSX REC. FLA6

* 3A'

•AA'-•ZZ'
*D1'

NUMERIC 9.3
NUMERIC 13.3
NUMERIC 13.3
NUMERIC 3
BLANK OR •«•

DETAIL RECORD 2 
-------
COMMENT RECORD 1 (CI)

COLUMN 	LEN6TH	CONTENTS	FORMAT/CONTENTS

1-3	3	FORM NUMBER	'3A*

«- 5	2	FORM SUFFIX	•AA'-'ZZ*

6-7	2	RECORD TYPE	*C1'

8-72	65	COMMENT LINE 1

COMMENT RECORD 2 CC2)

COLUMN (S) LENGTH

1-3	3

4-5	2

6-7	2

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CONTENTS

FORM NUMBER
FORM SUFFIX
RECORD TYPE
COMMENT LINE 2

FORMAT/CONTENTS

* 3A'

' AA' — 'ZZ'
*C2 *

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REV.
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SOIL VOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY - CFORM3B)

HEADER RECORD 1 (HI)

COLUMN (S) LENGTH CONTENTS

FORMAT/CONTENTS

1- 3
4- 5
6- 7
8-32
33-43
44-49
50-54
55-60
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66-77

78-80
81-82
83-84
85-86
87-88

3
2

2
25

11
6

5

6
5

12

3
2
2
2
2

FORM NUMBER
FORM SUFFIX
RECORD TYPE
LAB NAME
CONTRACT
LAB CODE
CASE NO.

SAS NO.

SDG NO.

MATRIX SPIKE -

EPA SAMPLE NO.

LEVEL

RPDJ ~ OUTSIDE QC LIMITS
RPD: TOTAL

SPIKE RECOVERY: « OUT
SPIKE RECOVERY: TOTAL

' 3B'

•AA'-'ZZ*
'HI'

' LOW OR 1
NUMERIC 2
NUMERIC 2
NUMERIC 2
NUMERIC 2

MED'

DETAIL RECORD 1 

COLUMN (S)

1- 3
4- 5
6- 7
8-31
32-40
41-53
54-66
67-69
70

3
2

2
24

9
13
13

3
1

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FORM NUMBER
FORM SUFFIX
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SAMPLE CONC. (UG/KG)
MS CONC. (UG/KG)
MS* REC.

MS* REC. FLAG

• 3B'

fAA'-'ZZ'
•Dl*

NUMERIC 9.3
NUMERIC 13.3
NUMERIC 13.3
NUMERIC 3
BLANK OR

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DETAIL RECORD 2 (D2)

COLUMN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

1- 5

3

FORM NUMBER

• 3B'

4- 5

2

FORM SUFFIX

'AA'-'ZZ*

6- 7

2

RECORD TYPE

' D2'

8-31

24

COMPOUND



32-40

9

SPIKE ADDED (UG/L)

NUMERIC 9.3

41-53

13

MSD CONC. (UG/KG)

NUMERIC 13.3

54-56

3

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NUMERIC 3

57

1

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BLANK OR

58-60

3

X RPD

NUMERIC 3

61

1

X RPD OUT FLAG

BLANK OR •«'

COMMENT RECORD 1 (CI)





COLUMN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

1- 3

3

FORM NUMBER

• 3B *

4- 5

2

FORM SUFFIX

•AA'-'ZZ'

6- 7

2

RECORD TYPE

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8-72

65

COMMENT LINE 1



COMMENT RECORD 2 (C2)





COLUMN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

1- 3

3

FORM NUMBER

' 3B'

4- 5

2

FORM SUFFIX

•AA'-'ZZ'

6- 7

2

RECORD TYPE

' C2'

8-72

65

COMMENT LINE 2



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HATER SEMIVOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE REC0VERY-(F0RM3C)

HEADER RECORD 1 (HI)

LUMN (S)

LENGTH

CONTENTS

1- 3

3

FORM NUMBER

4- 5

2

FORM SUFFIX

6- 7

2

RECORD TYPE

8-32

25

LAB NAME

33-43

11

CONTRACT

44-49

6

LAB CODE

50-54

5

CASE NO.

55-60

6

SAS NO.

61-65

5

SDG NO.

66-77

12

MATRIX SPIKE -





EPA SAMPLE NO.

78-79

2

RPD: * OUTSIDE QC LIMITS

80-81

2

RPD: TOTAL

82-83

2

SPIKE RECOVERY: « OUT

84-85

2

SPIKE RECOVERY: TOTAL

FORMAT/CONTENTS

' 3C *

'AA'-'ZZ'

HI

NUMERIC 2
NUMERIC 2
NUMERIC 2
NUMERIC 2

DETAIL RECORD 1 (Dl)

COLUMN (S)

1- 3
4- 5
6- 7
8-31
32-40
41-33
54-66
67-69
70

LENGTH CONTENTS

3
2

2
24

9
13
13

3
1

FORM NUMBER
FORM SUFFIX
RECORD TYPE
COMPOUND
SPIKE ADDED
SAMPLE CONC.

(UG/L)
(UG/L)

MS CONC. (UG/L)
MSX REC.

MSX REC. OUT FLAG

DETAIL RECORD 2 (D2)

COLUMN (S) LENGTH CONTENTS

1- 3
4- 5
6- 7
8-31
32-40
41-53
54-56
57
58-60
61

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE

COMPOUND

SPIKE ADDED (UG/L)
MSD CONC. (UG/L)
MSDX REC.

MSDX REC. OUT FLAG
X RPD

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NUMERIC 9.3
NUMERIC 13.3
NUMERIC 13.3
NUMERIC 3
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FORMAT/CONTENTS

•	3C'

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*	D2'

NUMERIC 9.3
NUMERIC 13.3
NUMERIC 3
BLANK OR *«'
NUMERIC 3
BLANK OR **'

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COMMENT RECORD 1 (CI)

COLUMN (S) LENGTH CONTENTS

FORMAT/CONTENTS

1- 3
<~- 5
6- 7
8-72

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE

65	COMMENT LINE 1

* 3C'

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LEN6TH CONTENTS

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1- 3

3

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4- 5

2

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6- 7

2

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8-72

65

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SOIL SEMIVOLATXLE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY - (FORM3D)

HEADER RECORD 1 (HI)

COLUMH (S) LEH6TH COHTENTS

1- 3
4- 5
6- 7
8-32
33-43

50-54
55-60
61-65
66-77

78-80
81-82
83-84
85-86
87-88

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE
25	LAB MAKE

11	CONTRACT
6	LAB CODE

5	CASE NO.

6	SAS NO.

5	SD6 NO.

12	MATRIX SPIKE -

EPA SAMPLE NO.

3	LEVEL

2	RPD: • OUTSIDE QC LIMITS

2	RPD: TOTAL

2	SPIKE RECOVERY: * OUT

2	SPIKE RECOVERY: TOTAL

FORMAT/CONTENTS
'3D *

'AA'-'ZZ*

•HI'

•LOW OR '
NUMERIC 2
NUMERIC 2
NUMERIC 2
NUMERIC 2

MED'

DETAIL RECORD 1 (Dl)

COLUMN CS) LEN6TH CONTENTS

FORMAT/CONTENTS

1- 3
4- 5
6- 7
8-31
32-40
41-53
54-66
67-69
70

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE
24	COMPOUND

9	SPIKE ADDED (U6/K6)

13	SAMPLE CONC. (UG/KG)

13	MS CONC. (UG/KG)

3	MS* REC.

1	MSX REC. OUT FLAG

•3D'

•AA'-'ZZ'
'Dl •

NUMERIC 9.3
NUMERIC 13.3
NUMERIC 13.3
NUMERIC 3
BLANK OR * * *

DETAIL RECORD 2 (D2)

COLUMN (S) LENGTH CONTENTS

FORMAT/CONTENTS

1- 3
4- 5
6- 7
8-31
32-40
41-53
54-56
57
58-60
61

FORM NUMBER
FORM SUFFIX
RECORD TYPE
COMPOUND

SPIKE ADDED (UG/KG)
MSD CONC. (UG/KG)
MSDX REC.

MSOX REC. OUT FLAG
X RPD

X RPD OUT FLAG

'3D*

•AA'-'ZZ'
•D2 •

NUMERIC 9.3
NUMERIC 13.3
NUMERIC 3
BLANK OR
NUMERIC 3
BLANK OR '*'

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COMMENT RECORD 1 (CI)

COLUMN (S)	LENGTH

1-3	3

4-5	2

6-7	2

8-72	65

CONTENTS

FORM NUMBER
FORM SUFFIX
RECORD TYPE
COMMENT LINE 1

FORMAT/CONTENTS
• 3D*

•AA'-'ZZ'

•CI '

COMMENT RECORD 2 

COLUMN  LENGTH CONTENTS

1-3	3

«- 5	2

6-7	2

8-72	65

FORMAT/CONTENTS

*	3D *

•AA'-'ZZ*

*	C2'

FORM NUMBER
FORM SUFFIX
RECORD TYPE
COMMENT LINE 2

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HEADER RECORD 1 (HI)

COLUMN (S) LENGTH CONTENTS

FORMAT/CONTENTS

1- 3
4- 5
6- 7
8-32
33-43

50-54
55-60
61-65
66-77

78-79
80-81
82-83
84-85

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE

25	LAB NAME

11	CONTRACT
6	LAB CODE

5	CASE NO.

6	SAS NO.

5	SD6 NO.

12	MATRIX SPIKE -

EPA SAMPLE NO.

2	RPD* • OUTSIDE QC LIMITS

2	RPD: TOTAL

2	SPIKE RECOVERY: • OUT

2	SPIKE RECOVERY: TOTAL

* 3E *

'AA'-'ZZ*
•Ml*

NUMERIC 2
NUMERIC 2
NUMERIC 2
NUMERIC 2

DETAIL RECORD 1 (Dl)

COLUMN (S) LENGTH CONTENTS

FORMAT/CONTENTS

1- 3

3

FORM NUMBER

* 3E'

4- 5

2

FORM SUFFIX

•AA'-'ZZ'

6- 7

2

RECORD TYPE

'Dl'

8-31

24

COMPOUND



32-40

9

SPIKE ADDED (UG/L)

NUMERIC 9.3

41-53

13

SAMPLE CONC. (UG/L)

NUMERIC 13.3

54-66

13

MS CONC. (UG/L)

NUMERIC 13.3

67-69

3

MSX REC.

NUMERIC 3

70

1

MSX REC. OUT FLAG

BLANK OR '«'

DETAIL RECORD 2 (D2)

COLUMN (S) LENGTH CONTENTS

FORMAT/CONTENTS

1- 3

3

FORM NUMBER

' 3E *

4- 5

2

FORM SUFFIX

•AA'-'ZZ*

6- 7

2

RECORD TYPE

*D2 *

8-31

24

COMPOUND



32-40

9

SPIKE ADDED (UG/L)

NUMERIC 9.3

41-53

13

MSD CONC.(UG/L)

NUMERIC 13.3

54-56

3

MSDX REC.

NUMERIC 3

57

1

MSDX REC. OUT FLAG

BLANK OR *«*

58-60

3

X RPD

NUMERIC 3

61

1

X RPD OUT FLAG

BLANK OR

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COLUMN (S)

LEN6TH CONTENTS

FORMAT/CONTENTS

1- 3
5

6- 7
8-72

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE

65	COMMENT LINE 1

• 3E *

•AA * —'ZZ•
•CI '

COMMENT RECORD 2 
-------
SOIL PESTICIDE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY - (F0RN3F)
HEADER RECORD 1 (HI)

COLUMN CS) LENGTH CONTENTS	FORMAT/CONTENTS

1- 3

3

FORM NUMBER

* 3F'

4- 5

2

FORM SUFFIX

'AA'-'ZZ*

6- 7

2

RECORD TYPE

•HI •

8-32

25

LAB NAME



33-43

11

CONTRACT



44-49

6

LAB CODE



50-54

5

CASE NO.



55-60

6

SAS NO.



61-65

5

SDG NO.



66-77

12

MATRIX SPIKE -

EPA SAMPLE NO.



78-80

3

LEVEL

'LOW OR 'MED'

81-82

2

RPD: • OUTSIDE QC LIMITS

NUMERIC 2

83-84

2

RPD: TOTAL

NUMERIC 2

85-86

2

SPIKE RECOVERY: • OUT

NUMERIC 2

87-88

2

SPIKE RECOVERY: TOTAL

NUMERIC 2

DETAIL RECORD 1 (Dl)

COLUMN (S) LENGTH CONTENTS	FORMAT/CONTENTS

1- 3

3

FORM NUMBER

' 3F •

4- 5

2

FORM SUFFIX

•AA'-'ZZ*

6- 7

2

RECORD TYPE

•Dl •

8-31

24

COMPOUND



32-40

9

SPIKE ADDED (UG/KG)

NUMERIC 9.3

41-53

13

SAMPLE CONC. (UG/KG)

NUMERIC 13.3

54-66

13

MS CONC. (UG/KG)

NUMERIC 13.3

67-69

3

MSX REC.

NUMERIC 3

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SPIKE ADDED (UG/KG)

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H - 31	1/87 REV.
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COHHENT RECORD 1 (CI)

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H - 32

1/87 REV.
-------
FORM XV FILE DESCRIPTION
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SEMIVOLATILE METHOD BLANK SUMMARY - (FORM 48)

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-------
PESTXCXOE METHOD BLANK SUMMARY - (FORM 4C>

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H - 36

1/87 REV.
-------
COMMENT RECORD 1 (CI)

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H - 57

1/87

REV.
-------
FORM V FILE DESCRIPTION
(F0RH5)

H - 38

1/87 REV.
-------
VOLATILE ORGANIC GC/MS TUNING AND MASS CALIBRATION - CFORMSA)
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110-113

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114

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115

1

OF



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1/87 REV.
-------
SEHXVOLATXLE

ORGANIC

CC/HS TUNING AND MASS CALIBRATION - (FORM5B)

OECAFLUOROTRIPHENYLPHOSPHZNE (DFTPP)



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66- 79

14

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80- 87

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102

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PAGE

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103

1

OF

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3

M/E

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11-16

6

X RELATIVE ABUNDANCE

NUMERIC 6.2

17-21

5

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NUMERIC 5.1

DETAIL RECORD 2 (D2)





COLUMN (S)

LENGTH

CONTENTS

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1- 3

3

FORM NUMBER

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«- 5

2

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2

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2

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EPA SAMPLE NO.



22-33

12

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34-47

14

LAB FILE ID



48-55-

8

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4

TIME ANALYZED

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H - AO

1/87 REV.
-------
FORM VI FILE DESCRIPTION
(FORM6)

H - 41

1/87 REV.
-------
VOLATILE ORGANICS INITIAL CALIBRATION DATA - (FORM 6A)

HEADER RECORD

1 (HI)



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LENGTH

CONTENTS

I- 3

3

FORM NUMBER

4- 5

2

FORM SUFFIX

6- 7

2

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25

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11

CONTRACT

44- 49

6

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50- 54

5

CASE NO.

55- 60

6

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61- 65

5

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66- 75

10

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8

CALIBRATION

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5

MATRIX

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3

LEVEL

100-103

4

COLUMN

104—117

14

RRF20 LAB

118-131

14

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132-145

14

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146-159

14

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160-173

14

RRF200 LAB

DETAIL RECORD

1 (Dl)



COLUMN (S)

LENGTH

CONTENTS

———	—	

	

	

1- 3

3

FORM NUMBER

4- 5

2

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6- 7

2

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27

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5

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40-44

5

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45-49

5

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50-54

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55-59

5

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60-64

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X RSD

ID
DATE
DATE

FILE
FILE
FILE
FILE
FILE

ID
ID
ID
ID
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FORMAT/CONTENTS

•	6A *

*	AA * — * ZZ'

•HI•

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NUMERIC 5.3
NUMERIC 5.3
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NUMERIC 5.3
NUMERIC 5.3
NUMERIC 5.1

H - 42

1/87 REV.
-------
SEMIVOLATILE ORGANICS INITIAL CALIBRATION DATA - (FORN 6B)

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LENGTH

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3

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2

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25

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33- 43

11

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6

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50- 54

5

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55- (0

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61- (5

5

SDG NO.





66- 75

10

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76- 83

8

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1

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84- 91

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92-105

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106-119

14

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120-133

14

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134-147

14

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148-161

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ID



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1 (Dl)







COLUMN (S)

LENGTH

CONTENTS



FORMAT/CONTENTS

1- 3

3

FORM NUMBER



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2

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27

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35-39

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NUMERIC 5.3

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5

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NUMERIC 5.3

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NUMERIC 5.3

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5

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NUMERIC 5.3

55-59

5

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NUMERIC 5.1

H - 43	1/87 REV.
-------
SEMIVOLATXLE ORGANICS INITIAL CALIBRATION DATA - (FORM 6C)

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LENGTH

CONTENTS

1- 3

3

FORM NUMBER

4- 5

2

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6- 7

2

RECORD TYPE

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25

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11

CONTRACT

44- 49

6

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50- 54

5

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6

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5

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66- 75

10

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76- 83

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8

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92-105

14

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120-133

14

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134-147

14

RRF120 LAB FILE ID

148-161

14

RRF160 LAB FILE ID

DETAIL RECORD

1 (Dl)



COLUMN (S)

LENGTH

CONTENTS

1- 3

3

FORM NUMBER

4- 5

2

FORM SUFFIX

6- 7

2

RECORD TYPE

8-34

27

COMPOUND

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45-49

5

RRF80

50-54

5

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55-59

5

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60-64

5

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65-69

5

X RSD

FORMAT/CONTENTS

' 6C *

'AA*ZZ'
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MM/DD/YY
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•Dl*

NUMERIC 5.3
NUMERIC 5.3
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NUMERIC 5.3
NUMERIC 5.3
NUMERIC 5.3
NUMERIC 5.1

H - 44

1/87 REV.
-------
FORM VII FILE DESCRIPTION
(FORM7)

H

- 4 5

1/87 REV.
-------
VOLATILE CONTINUING CALIBRATION CHECK - (FORM 7A)

HEADER RECORD 1 (HI)

OLUMN (S)

LENGTH

CONTENTS



	

—	

	——	

¦—

1- 3

3

FORM NUMBER



4- S

2

FORM SUFFIX



6- 7

2

RECORD TYPE



8- 32

25

LAB NAME



33- 43

11

CONTRACT



44- 49

6

LAB CODE



50- 54

5

CASE NO.



55- 60

6

SAS NO.



61- 65

5

SDG NO.



66- 75

10

INSTRUMENT ID



76- 83

8

CALIBRATION DATE



84- 87

4

CALIBRATION TIME



88-101

14

LAB FILE ID



102-109

8

INIT. CALIB. DATE

1

110-117

8

INIT. CALIB. DATE

2

118-122

5

MATRIX



123-125

3

LEVEL



126-129

4

COLUMN



FORMAT/CONTENTS
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*AA'-'22'

•HI*

MM/-DD/YY
HHMM

MM/DD/YY
MM/DD/YY

'SOIL • OR 'MATER*
•LOW OR 'MED'
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DETAIL RECORD 1 (Dl)

COLUMN  LENGTH CONTENTS

1- 3
4- 5
6- 7
8-3*
35-39
40-44
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3	FORH NUMBER

2	FORM SUFFIX

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5	X D

FORMAT/CONTENTS
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NUMERIC 5.3
NUMERIC 5.3
NUMERIC 5.1

H - 46

1/87 REV,
-------
SEMIVOLATILE CONTINUING CALIBRATION CHECK -

(FORH 7B)

HEADER RECORD 1 (HI)

COLUMN (S) LENGTH CONTENTS	FORMAT/CONTENTS

1- 3

3

FORM NUMBER

* 7B'

4- 5

2

FORM SUFFIX

*AA'- * ZZ'

6- 7

2

RECORD TYPE

•HI*

8- 32

25

LAB NAME



33- 43

11

CONTRACT



44- 49

6

LAB CODE



50- 54

5

CASE NO.



55- 60

6

SAS NO.



61- 65

5

SDG NO.



66- 75

10

INSTRUMENT ID



76- 83

8

CALIBRATION DATE

NM/DD/YY

84- 87

4

CALIBRATION TIME

HHMM

88-101

14

LAB FILE ID



102-109

8

INIT. CALIB. DATE 1

MM/DD/YY

110-117

8

INIT. CALIB. DATE 2

MM/'DD/'YY

DETAIL RECORD 1 (Dl)

COLUMN (S) LENGTH CONTENTS	FORMAT/CONTENTS

1- 3

3

FORM NUMBER

' 7B'

4- 5

2

FORM SUFFIX

*AA * - * ZZ *

6- 7

2

RECORD TYPE

•Dl •

8-34

27

COMPOUND



35-39

5

AVERAGE RRF

NUMERIC 5.3

40-44

5

RRF50

NUMERIC 5.3

45-49

5

X D

NUMERIC 5.1

H - 47

1/87 REV.
-------
SEMIVOIATILE CONTINUING CALIBRATION CHECK - (FORM 7C>

HEADER RECORD

1 (HI)





COLUMN (S>

LENGTH

CONTENTS

FORMAT/CONTENTS

1- 3

3

FORM NUMBER

• 7C*

4- 5

2

FORM SUFFIX

•AA'-•ZZ *

6- 7

2

RECORD TYPE

•HI'

8- 32

25

LAB NAME



33- 43

11

CONTRACT



44- 49

6

LAB CODE



50- 54

5

CASE NO.



55- 60

6

SAS NO.



61- 65

5

SDG NO.



66- 75

10

INSTRUMENT ID



76- 83

8

CALIBRATION DATE

MM/DD/YY

84- 87

4

CALIBRATION TIME

HHMM

88-101

14

LAB FILE ID



102-109

8

IN IT. CALIB. DATE 1

MM/DD/YY

110-117

8

INIT. CALIB. DATE 2

MM/DD/YY

DETAIL RECORD 1 (Dl)





COLUMN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

——————————

——————

	

	 ——		

1- 3

3

FORM NUMBER

' 7C *

4- 5

2

FORM SUFFIX

'AA * -'ZZ *

6- 7

2

RECORD TYPE

• Dl'

8-34

27

COMPOUND



35-39

5

AVERAGE RRF

NUMERIC 5.3

40—44

5

RRF50

NUMERIC 5.3

45-49

5

X D

NUMERIC 5.1

H - 48

1/87 REV.
-------
FORM VIII FILE DESCRIPTION
(FORMS)

H - 4?

1/87 REV.
-------
VOLATILE INTERNAL STANDARD AREA SUMMARY - (FORM BA)

HEADER RECORD 1 (HI)

LUMN (S)

LENGTH



1- 3

3

FORM NUMBER

4- 5

2

FORM SUFFIX

6- 7

2

RECORD TYPE

8- 32

25

LAB NAME

33- 43

11

CONTRACT

44- 49

6

lab code

50- 54

5

CASE NO.

55- 60

6

SAS NO.

61- 65

5

SDG NO.

66- 79

14

LAB FILE ID (STANDARD)

80- 87

8

DATE ANALYZED

88- 97

10

INSTRUMENT ID

98-101

4

TIME ANALYZED

102-106

5

MATRIX

107-109

3

LEVEL

110-113

4

COLUMN

114

1

PAGE

115

1

OF

FORMAT/CONTENTS

DETAIL RECORD 1 (Dl)

COLUMN (S) LENGTH CONTENTS

1- 3
4- 5

6- 7

«- 16

17- 22
23- 31
32- 37
38- 46
47- 52

S3- 61
42- 70
71- 7?

80- 88
89- 97
'8-106

FORM NUMBER
FORM SUFFIX
RECORD TYPE
12 HOUR STANDARD -

151	(BCM) AREA
RT

152	(DFB) AREA
RT

153	(CBZ) AREA
RT

UPPER LIMIT -

151	(BCM) AREA

152	(DFB) AREA

153	(CBZ) AREA
LOWER LIMIT -

151	(BCM) AREA

152	(DFB) AREA

153	(CBZ) AREA

*8A'

•AA'-'ZZ'

'HI *

mm/dd/yy

HHMM

'SOIL • OR * HATER'
•LOW OR 'MED*
•PACK' OR 'CAP '
NUMERIC 1
NUMERIC 1

FORMAT/CONTENTS

' 8A'

•AA'-'ZZ'
•Dl*

NUMERIC 9
NUMERIC 6.2
NUMERIC 9
NUMERIC 6.2
NUMERIC 9
NUMERIC 6.2

NUMERIC 9
NUMERIC 9
NUMERIC 9

NUMERIC 9
NUMERIC 9
NUMERIC 9

H - 50

1/87 REV.
-------
DETAIL RECORD 2 
-------
SEMIVOLATILE INTERNAL STANDARD AREA SUMMARY - (FORM SB)

HEADER RECORD 1 (HI)

COLUMN (S) LEN6TH CONTENTS	FORMAT/CONTENTS

1- 3

3

FORM NUMBER

*8B'

4- 5

2

FORM SUFFIX

•AA'-'ZZ'

6— 7

2

RECORD TYPE

•Hi*

8- 32

25

LAB NAME



33- 43

11

CONTRACT



44- 49

6

LAB CODE



50- 54

5

CASE NO.



55- 60

6

SAS NO.



61- 65

5

SDG NO.



66- 79

14

LAB FILE ID (STANDARD)



80- 87

8

DATE ANALYZED

MM/DD/YY

88- 97

10

INSTRUMENT ID



98-101

4

TIME ANALYZED

HHMM

102

1

PA6E

NUMERIC 1

103

1

OF

NUMERIC 1

DETAIL RECORD 1 (Dl)

COLUMN (S) LENGTH CONTENTS

FORMAT/CONTENTS

1- 3
<*- 5
6- 7

8- 16
17- 22
23- 31
32- 37
38- 46
47- 52

53- 61
62- 70
71- 79

80- 88
89- 97
98-106

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE

12 HOUR STANDARD -

151	(DCB) AREA
RT

152	(NPT) AREA
RT

153	(ANT) AREA
RT

UPPER LIMIT -

151	(DCB) AREA

152	(NPT) AREA

153	(ANT) AREA
LOWER LIMIT -

151	(DCB) AREA

152	(NPT) AREA

153	(ANT) AREA

•SB'

•AA'-'ZZ'
•Dl •

NUMERIC
NUMERIC
NUMERIC
NUMERIC
NUMERIC
NUMERIC

NUMERIC 9
NUMERIC 9
NUMERIC 9

NUMERIC 9
NUMERIC 9
NUMERIC 9

H - 52

1/87 REV.
-------
DETAIL RECORD 2 (02)

COLUMN (S)

1- 3
4- 5
«- 7
«- 9
10-21
22-30
31
32-37
38-46
47
48-53
54-62
63
64-6?

H - 53	1/87 REV.

LENGTH CONTENTS

FORMAT/CONTENTS

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE

2	SEQUENCE NUMBER

EPA SAMPLE NO.
IS1 (DCB) AREA

151	(DCB) AREA FLA6
RT

152	(NPT) AREA

152	(NPT) AREA FLA6
RT

153	(ANT) AREA
IS3 (ANT) AREA FLA6
RT

8B

AA-ZZ
D2

NUMERIC 2

NUMERIC 9
BLANK OR *m«
NUMERIC 6.2
NUMERIC 9
BLANK OR
NUMERIC 6.2
NUMERIC 9
BLANK OR
NUMERIC 6.2
-------
SEMIVOLATIIE INTERNAL

STANDARO AREA SUMMARY -

(FORM 8C)

HEADER RECORD 1 (HI)

COLUMN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

1-3	3	FORM NUMBER

4-5	2	FORM SUFFIX

6-7	2	RECORD TYPE

8- 32	25	LAB NAME

33- A3	II	CONTRACT

44- 49	6	LAB CODE

50- 54	5	CASE NO.

55- 60	6	SAS NO.

61- 65	5	SDG NO.

66- 79	14	LAB FILE ID (STANDARD)

80- 87	8	DATE ANALYZED

88- 97	10	INSTRUMENT ID

98-101	4	TIME ANALYZED

102	1	PAGE

103	1	OF

* 8C'

'AA * -•ZZ *
•HI'

MM/DD/YY
HHMM

NUMERIC 1
NUMERIC 1

DETAIL RECORD 1 (Dl)

COLUMN (S)

1-
4-
6-

3
5
7

8-16
17- 22
23- 31
32- 37
38- 46
47- 52

53- 61
62- 70
71- 79

80- 88
89- 97
98-106

LENGTH

3
2
2

CONTENTS

FORMAT/CONTENTS

FORM NUMBER
FORM SUFFIX
RECORD TYPE
12 HOUR STANDARD -

154	(PHN) AREA
RT

155	(CRY) AREA
RT

156	(PRY) AREA
RT

UPPER LIMIT -

154	(PHN) AREA

155	(CRY) AREA

156	(PRY) AREA
LOWER LIMIT -

154	(PHN) AREA

155	(CRY) AREA

156	(PRY) AREA

' 8C *

'AA'-'ZZ
•Dl'

NUMERIC
NUMERIC
NUMERIC
NUMERIC
NUMERIC
NUMERIC

NUMERIC 9
NUMERIC 9
NUMERIC 9

NUMERIC 9
NUMERIC 9
NUMERIC 9

H - 54

1/87 REV.
-------
DETAIL RECORD 2 
-------
PESTICIDE EVALUATION STANDARDS SUMMARY - (FORM 8D)

HEADER RECORD 1 (HI)

COLUMN (S)

LENGTH CONTENTS

FORMAT/CONTENTS

1-3	3	FORM NUMBER

4-5	2	FORM SUFFIX

6-7	2	RECORD TYPE

8- 32	25	LAB NAME

33- 43	11	CONTRACT

44- 49	6	LAB CODE

50- 54	5	CASE NO.

55- 60	6	SAS NO.

61- 65	5	SD6 NO.

66- 75	10	INSTRUMENT ID

76- 85	10	GC COLUMN ID

DATES OF ANALYSES

86- 93	8	FROM:

94-101	8	TO:

' 8D *

'AA'-'ZZ*

HI

MM/DD/YY
MM/DD/YY

DETAIL RECORD 1 (Dl)

COLUMN (S) LENGTH CONTENTS

1- 3
4- 5
6- 7
8-20
21-31
32-42
43-53
54-58

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE

13	PESTICIDE

11	CALIB. FACTOR

11	CALIB.

11	CALIB.

5	X RSD

EVAL MIX A
FACTOR EVAL MIX B
FACTOR EVAL MIX C

FORMAT/CONTENTS
•80*

'AA'-'ZZ'

• Dl*

NUMERIC 11
NUMERIC 11
NUMERIC 11
NUMERIC 5.1

DETAIL RECORD 2 (D2>

COLUMN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

1- 3
4- 5
6- 7
8- 9
10-17
18-21
22-26
27-31
32-36

3	FORM NUMBER
2	FORM SUFFIX
2	RECORD TYPE

2	SEQUENCE NUMBER

8	DATE ANALYZED

4	TItlE ANALYZED

5	ENDRIN

5	4,4*-DDT

5	COMBINED

* 8D'

•AA'-'ZZ'
' D2'

NUMERIC 2

MM/DD/YY

HHMM

NUMERIC 5.1
NUMERIC 5.1
NUMERIC 5.1

H - 56

1/87 REV.
-------
PESTICIDE EVALUATION STANDARDS SUMMARY - (FORM 8E)
EVALUATION OF RETENTION TIME SHIFT FOR DIBUTYLCHLORENDATE

HEADER RECORD 1 (HI)

COLUMN (S)

1- 3
4- 5
6- 7
8- 32
33- 43
44- 49
50- 54
55- 60
61- 65
66- 75
76- 85

86- 93
94-101

102

103

LENGTH CONTENTS

FORMAT/CONTENTS

3
2
2
25
11
6

5

6
5

10
10

8
8
1
1

FORM NUMBER
FORM SUFFIX
RECORD TYPE
LAB NAME
CONTRACT
LAB CODE
CASE NO.

SAS NO.

SDG NO.

INSTRUMENT ID
GC COLUMN ID
DATES OF ANALYSES
FROM:

TO»

PAGE
OF

' 8E'

'AA * -'ZZ*
•HI *

MM/DD/YY
MM/DD/YY
NUMERIC 1
NUMERIC 1

DETAIL RECORD 1 (Dl)

COLUMN (S)

LENGTH

CONTENTS

FORMAT/CONTENTS

1- 3

3

4- 5

2

6- 7

2

8- 9

2

10-21

12

22-33

12

34-41

8

42-45

4

46-50

5

51

1

FORM NUMBER
FORM SUFFIX
RECORD TYPE
SEQUENCE NUMBER
EPA SAMPLE NO.
LAB SAMPLE ID
DATE ANALYZED
TIME ANALYZED
X D
FLAG

* 8E '

'AA•-'ZZ'
•Dl •

NUMERIC 2

MM/DD/YY
HHMM

NUMERIC 5.1
BLANK OR **•

H - 57

1/87 REV.
-------
FORM IX FILE DESCRIPTION
CFORM9)

H -

58

1/87 REV.
-------
PESTICIDE/PCB STANDARDS SUMMARY - (FORM 9)

HEADER RECORD 1 (HI)

COLUMN (S) LENGTH CONTENTS	FORMAT/CONTENTS

1- 3

3

FORM NUMBER



. 9.

4- 5

2

FORM SUFFIX



'AA'-'ZZ*

6- 7

2

RECORD TYPE



•HI*

8- 32

25

LAB NAME





33- 43

11

CONTRACT





44- 49

6

LAB CODE





50 54

5

CASE HO.





55- 60

6

SAS NO.





61- 65

5

SDG NO.





66- 75

10

INSTRUMENT ID





76- 85

10

6C COLUMN ID





86- 93

8

DATE OF ANALYSIS

FROM:

MM/DD/YY

94-101

8

DATE OF ANALYSIS



MM/DD/YY

102-109

8

DATE OF ANALYSIS

TO:

MM/DD/YY

110-113

4

TIME OF ANALYSIS



HHMM

114-117

4

TIME OF ANALYSIS

FROM:

HHMM

118-121

4

TIME OF ANALYSIS

TO:

HHMM

122-133

12

EPA SAMPLE NO. (STANDARD)



134

1

PAGE



NUMERIC 1

135

1

OF



NUMERIC 1

DETAIL RECORD 1 (Dl)
COLUMN (S) LENGTH

I- 3

3

4- 5

2

6- 7

2

8-20

13

21-26

6

27-32

6

33-38

6

39-49

11

50-55

6

56-66

11

67

1

68-72

5

CONTENTS

FORM NUMBER
FORM SUFFIX
RECORD TYPE
COMPOUND
RT

RT WINDOW FROM:
RT WINDOW TO:
CALIBRATION FACTOR
RT

CALIBRATION FACTOR
QUANT
X D

FORMAT/CONTENTS

• 9*

•AA'-'ZZ'
'Dl *

NUMERIC 6.2
NUMERIC 6.2
NUMERIC 6.2
NUMERIC 11
NUMERIC 6.2
NUMERIC 11
'Y* OR 'N*
NUMERIC 5.1

H - 59

1/87 REV.
-------
FORM X FILE DESCRIPTION
(FORMIO)

H -

60

1/87 REV.
-------
PESTICIDE/PCB IDENTIFICATION - (FORM 10)

HEADER RECORD 1 (HI)

COLUMN (S)

1-
4-
6-
8-

20-
45-
56-
62-
67-
73-
78-
88-
98-
108-
118-
130-

3
5
7
1?
44
55
61
66
72
77
87
97
107
117
129

143

144

145

LENGTH CONTENTS

3	FORM NUMBER

2	FORM SUFFIX

2	RECORD TYPE

12	EPA SAMPLE NO.

25	LAB NAME

11	CONTRACT
6	LAB CODE

5	CASE NO.

6	SAS NO.

5	SDG NO.

10	GC COLUMN ID (1)

10	GC COLUMN ID (2)

10	INSTRUMENT ID (1)

10	INSTRUMENT ID (2)

12	LAB SAMPLE ID

14	LAB FILE ID (IF GC/MS)

1	PAGE

1	OF

FORMAT/CONTENTS

•10'

* AA'-' ZZ'
'HI'

NUMERIC 1
NUMERIC 1

DETAIL RECORD 1 (Dl)

COLUMN  LENGTH CONTENTS

1- 3
4- 5
6- 7
8- 9
10-23
24-29

30-35

36-41

42

43

3
2
2
2
14
6

6
1
1

FORM NUMBER
FORM SUFPIX
RECORD TYPE
SEQUENCE NUMBER
PESTICIDE/PCB
RETENTION TIME
COLUMN 1

RT WINDOW OF STANDARD
FROM:

TO:

QUANT?

GC/MS?

FORMAT/CONTENTS
'10'

* AA'-*ZZ'

•Dl*

NUMERIC 2

NUMERIC 6.2

NUMERIC 6.2
NUMERIC 6.2
•Y* OR 'N*
*Y' OR 'N'

H - 61

1/87 REV.
-------
DETAIL RECORD 2 

COLUMN (S)

LENGTH CONTENTS

FORMAT/CONTENTS

1- 3
4- 5
6- 7
8- 9
10-23
24-29

30-35

36-41

42

43

3
2
2
2
14
6

6
1
1

FORM NUMBER
FORM SUFFIX
RECORD TYPE
SEQUENCE NUMBER
PESTICIDE/PCB
RETENTION TIME
COLUMN 2

RT WINDOW OF STANDARD
FROM:

TO:

QUANT?

6C/MS?

•10'

'AA'- * ZZ *
* D2'

NUMERIC 2

NUMERIC 6.2

NUMERIC 6.2
NUMERIC 6.2
•Y* OR 'N'
'Y* OR 'N *

COMMENT RECORD 1 CC1)

.COLUMN (S) LENGTH CONTENTS	FORMAT/CONTENTS

1- 3

3

FORM NUMBER

•10'

4- 5

2

FORM SUFFIX

'AA'-'ZZ'

6- 7

2

RECORD TYPE

'CI •

8-72

65

COMMENT LINE 1



COMMENT RECORD 2 CC2)

COLUMN (S) LENGTH CONTENTS	FORMAT/CONTENTS

1- 3

3

FORM NUMBER

•10*

4- 3

2

FORM SUFFIX

'AA * -* ZZ *

6- 7

2

RECORD TYPE

' C2'

8-72

65

COMMENT LINE 2



H - 62

1/87 REV.
-------
SECTION III

FORMAT B SPECIFICATION

1.	Format Characteristics

1.1	Format B is based upon analytical results and ancillary information required by
the contract. All data generated by a single analysis are grouped together, and
the groups are aggregated to produce files that report data from an SDG.

1.2	Format B fields are separated by at least one blank byte. Field characteristics
and required justification of values are given in the detailed listing of record
types below.

2.	Rgcgrd Types

2.1	Format B consists of fixed-length 80-byte ASCII records. The last two bytes of
each record must contain "carriage return" and "line feed", respectively. Unused
bytes in partially filled fields must be blank-filled.

2.2	Format B consists of eleven record types than can be summarized in four groups:

Type	Name

10	Run Header

20	Sample Header

30	Results Record

90	Comments Record

Contents

Contains information pertinent to the whole
production run. See production run definition
below.

Contains sample-identifying information, or
corresponding information for calibrations, QC
samples, Instrument performance checks, etc.
Contains any final result on a sample, calibration,
or QC sample, and identifying information.

Contains free-form comments.

A type 20 record, representing a sample, contains the raw EPA Sample No. (the
Sample No. as given on the Traffic Report without any of the identifying
suffixes) which acts as an identifying label for the sample. A QC code indicates
whether the data are from an environmental sample, calibration, or QC sample; or
other calculated run-wide data such as mean response factors. A type 30 record,
representing an individual compound, contains a CAS code to identify the analyte,
surrogate, or internal standard. All 30 series records following that record
pertain to the same compound. See page H-82 for an example of the sequence of
record types.

3. Production Runs

A production run represents a "group" or "batch" of samples that are processed in
a continuous sequence under relatively stable conditions. Specifically:
Calibration — All samples in a run use the same initial calibration data.

Method number — Constant. Instrument conditions - Constant throughout a run.
Results obtained on different instruments cannot be combined in one run.

H-63

2/88
-------
Analyses from each fracCion consist of a separate production run, and are
reported in separate files. There will be a separate production run for each 72
hour sequence for pesticides for each GC column utilized. Thus, a full three
fraction analysis will consist of a minimum of four production runs, and could
consist of more.

4. Record Sequence (see page H-82)

4.1 A Run Header (type 10) record must be present once and once only (per file) as
the first record in a file.

4.2	Each environmental sample, calibration, or quality control sample is represented
by a group composed of type 20 and 21 records, which hold sample level
identifying information, followed by one type 30 record for each method analyte
or standard. The type 20 record holds a count for the number of method analytes
being determined, and includes all target compounds plus any tentatively
identified compounds. Type 20 records must occur in the order of sample
analysis. The type 20 records for quality control items have the additional rule
that the LF1 record must occur before the LF2 record, but the records need not be
adjacent. In addition, a type 20 record is used as a header for any additional
run-wide data that must be reported for each method analyte (such as mean
response factors). Unique identifiers given on page H-77 are used in place of
"QC codes" to indicate the type of data that follows. Type 30 records for each
analyte must occur in the order specified on hardcopy deliverable Form 6.

4.3	Type 90 comment records may be defined to occupy any position except before the
type 10 (header) record.

5. File/Record IntagiM t-y

All record types shall contain the following check fields to ensure file and
record integrity:

Record

Field

Field

Position

Ltngth

Contents

1-2

2

Record type or identifier

72-74

3

Record sequence number





within file

75-78

4

Record checksum

79-80

2

Will contain CR and LF

Rcmarfrg

"10" or as appropriate
000-999, repeated as
necessary

Four hexadecimal digits(*)

(*) The checksum is the sum of the thirty-five Integers that make up the data in
columns 1 to 70, when data are represented in the format 35A2 on processors which
store data bytes in left to right order. The Hum is taken modulo 65536 (216) and
represented as four hexadecimal digits. For processors which use an A70
character representation of data, the checksum is the sum of all the even
character position values plus 256 times the sum of all the odd character
position values.

H-64

2/88
-------
6. Dates and Times

Date or time-of-day information consists of successive groups of one or two
decimal digits, each separated by blanks. Dates are given in the order YY MM DD,
and times as HH MM. All hours oust be given as 0 to 23 using a 24 hour clock and
must be local time.

7. Multiple Volume Data

Format B data from an entire SDG may not fit onto a single diskette. If a single
production run is being split onto multiple diskettes, than all files must start
with a type 10 record, and the multiple type 10 records for each file of the same
production run must be identical. If it is necessary to split the data from a
single sample onto multiple diskettes, then the type 20 (and following) type
records for that sample must be repeated. In this situation, columns 7-30, which
collectively identify the sample, must be identical on each diskette.

8. Record Listing

Following is a listing of every record type required to report data from a single
SDG.

8.1 Format of the mandatory Production Run Header Record (Type 10)

Record	Field Field

Position	Length Contents	Remarks

1-2	2	Record type	"10"

3-18	16	blank

19-23

24-25

Measurement Type

blank

"GC/MS" for Volatiles and
Semivolatiles or "GC/EC"
for Pesticides.

26-30

31-35

Method Number

blank

"6241" for Volatiles; "625C"
for Semivolatiles; "6081"
for Pesticides

36-41
42-51

52-61
62

6	Lab ID

10	blank

10	Contract Number

1	blank

From EPA standard list or
Project Officer

Agency standard number

63-68	6	Instrument ID	e.g. 59951G; provided by

contract lab; left justi-
fied; must be unique and
permanent within lab. First
four characters are designa-
tor; fifth is sequence num-
ber; sixth !• lab assigned.

H-65

Rev. 9/88
-------
8.2 Format of the Chromatography Record (Type 11)
Use: To describe chromatograph conditions.
Position: Follows type 10.

Record	Field	Field

fggltlgn	Length	Contents

1-2	2	Record type

3	1	blank

4-11	8	Comaercial Column name

12-17	6	blank

18-21	4	Column inside

diameter (mm)

Remarks
"11"

Left justified. Column
ID, e.g. SP2330

Right justified

H-66

2/88
-------
8.3 Format of the mandatory Sample Header Data Record (Type 20)

Record

Field

Field



Position

L&n&Zh

Contents

Remarks

1-2

2

Record type

"20"

3-6

4

blank



7-11

5

EPA Sample I.D.

Left justified. Raw Sample







No. only; no suffixes.

12-15

4

blank



16

1

Sample Medium/Matrix Code

"0" if not applicable







"1" for water

17

1

blank

"H" for soil

18-20

3

QC code

Codes type of data to be

21

1

blank

reported (see page H-77)

22-24

3

Sample Qualifier

Code to qualify the results







of the entire sample

25

1

blank

analysis (see page H-79)

26-30

5

Case Number



31-39

9

blank



40-47

8

Date of Instrumental analysis

YY MM DD

48

1

blank



49-53

5

Hour, Min. of analysis

HH MM

54-56

3

blank



57

1

Sample Units Code

"L" - liters for water

58

1

blank

"K" - kilograms for soil

59-66

8

Sample Size

right justified;







see Note

67

1

blank



68-70

3

Analyte count

Numeric; 1-3 decimal digits;

right justified. Counts all
analytes including TIC's.

NOTE: Sample Size is the volume in liters for liquids and the wet weight in
kilograms for solids. The Sample Units Code indicates which units are in use
for the current sample. Leave blank if not applicable.

H-67

Rev. 9/88
-------
8.4 Format of Che Sample Header Data Record (Type 21)
Use: Continuation of type 20.

Position: Follows the type 20 to which it applies.

Record

Field

Field



Position

Length

Centtnti

Remarks

1-2

2

Record type

"21"

3-5

3

blank



6

1

Concentration level

"L" - low







"M" — medium

7

1

blank

(See note).

8

1

Clean-up Utilized

"G" or blank

9-11

3

blank



12

1

Extraction code

"S" - Separatory Funnel







"C" - Continuous Liq-Liq

13-17

5

blank

"N" - Sonication

18-23

6

SAS Number

Leave blank if none.

24

1

blank



25-35

11

Laboratory Data Descriptor

Lab File ID for Volatiles

36

37-44

45-47
48-55

1
8

3
8

blank

Date of Beginning of
Sanple Prep - Extraction
prior to analysis
blank

Date Sanple Received at Lab YY MM DD

or Semivolatiles; Lab Sample
ID for Pesticides.

YY MM DD

Note: The Concentration Level is an estimate of overall level for all analytes.

H-68

2/88
-------
8.5 Format of Che Sample Conditions Record (Type 22)

Use: Continuation of type 20. Used to describe additional sample conditions.
Position: Follows the type 20 and 21 to which it applies.

Record
Position

1-2
3

4-11
12

Field

Length

2
1

8

1

Field
Contents

Record type
blank

Date of associated

calibration

blank

Remarks

'22'

YY MM DD; see Note.

(Date of Source of the
response factors or
calibration factors used)

13-17
18

19-29

30

31-34
35

36-37
38

39-40
41

42-46
47

48-55

5

I

II

4

1

2

1

2
1

5
1

Time of associated

calibration

blank

Calibration File ID

blank

Sample pH
blank

Percent moisture
blank

HH MM

Lab File ID or Lab Sample
ID (pesticides) of continu-
ing calibration, or
"AVERAGE", position 21-27
and padded with blanks (if
mean used)

XX or XX.X, right justified

right justified; use
zero if not applicable

Decanted percent moisture right justified; use
blank	zero if not applicable

Extract Volume in ml
blank

Concentration/dilution
factor

e.g. 1.0 or 0.050

Right Justified;
e.g. 2000 or .001

Note: For average, use the date and time average was calculated.

H-69

2/88
-------
8.6 Format of the Associated Injection and Counter Record (Type 23)

Use: Continuation of type 20. Used to identify associated blanks and tunes,

and to count the number of surrogates and spikes outside QC limits and the
number of TIC compounds.

Position: Follows the type 20, 21, and 22 to which it applies.

Record

Field

Field



Position

Length

Contents

Remarks

1-2

2

Record type

"23"

3

1

blank



4

1

"P" or blank

Labels data as "tune" data.

5

1

blank

(if applicable)

6-13

8

Date of associated

YY MM DD. Acquisition date





DFTPP/BFB injection

of tune to be linked with

14

1

blank

this sample (if applicable).

15-19

5

Time of DFTPP/BFB injection

HH MM (if applicable)

20

1

blank



21-31

11

DFTPP/BFB Lab File ID

From instrument data system

32

1

blank

(if applicable)

33

1

"B" or blank

Labels data as "blank" data.

34

1

blank

(if applicable)

35-42

8

Date of associated

YY MM DD. Acquisition date

43



blank injection

of method blank to be linked

1

blank

with sample (if applicable).

44-48

5

Time of blank injection

HH MM (if applicable)

49

1

blank



50-60

11

Blank Lab File ID or

From instrument data system

61

1

blank Lab Sample ID

62



(pesticides)



1

upw

Identifies following counter

63





"P" - # of % Recoveries

1

blank

Outside of QC limits

64-65

2

Number of Percent Recoveries

Use the Counter from Form

66



Failing QC limits

2 or 3 for each sample.

1

blank

67

1

"T" or "R"

"T" - # of TIC compounds.

68





"R" - # of * RSD's outside

1

blank

limits

69-70

2

Number of TIC Compounds

From Form 1-E or 1-F

or # % RSD's Outside Limits or from Form 3

H- 70

2/88
-------
8.7 Format of the Results Data Record (Type 30)

Record	Field	Field

Position	Length Contents

1-2	2	Record type

3	1	blank

4	1	"C" or "I"

5	1	blank

6-14	9	CAS Number

15	1	blank

16-24	9	CAS Number Internal

Standard Utllllzed

25	1	blank

26-30	5	Units of measure

31	1	blank

32-34	3	Non-numeric result

35	1	blank

36-41	6	Numeric analytical result

42	1	blank or 'E'

43.45	3	Exponent

46	1	blank

47	1	Calculated Value Descriptor

48	1	blank

49.54	6	Related Calculated Value

55	1	blank or 'E'

56-58	3	Exponent

59	1	blank

60	1	Limit or QC Value

Descriptor

61	1	blank

62-66	5	Related Limit Value

67	1	blank or 'E'

68-70	3	Exponent

Remarks
"30"

Use "C" - CAS Number unless
identifying combined DDT and
Endrin, in which case use

M Jff

Right justified. Use
"COMBINED" for combined DDT
and Endrin.

Right justified

(Left justified) "UG/KG" for
Soil; "UG/L " for Water;
"PERCT" for percent

See page H-79 also called a
result qualifier

Right justified; fixed
point or scientific
notation

Blank field will be
interpreted as "+00"

Describes following value
(See page H-81)

Value of item described
Format same as 36-46.

Describes following value
(See page H-81)

Value of item described
above.

H-71

2/88
-------
8.8 Format of the Instrumental Data Readout Record (Type 31)

Use: To describe peak areas for Internal standards and DFTPP/BFB percent
abundances.

Position: Follows type 30 for Internal standards and DFTPP/BFB data.

Record	Field Field

Position	Length Contents	Remarks

1-2	2	Record type	"31"

3	1	blank

4	1	"M"	Indicates mass for DFTPP/BFB

5	1	blank	data.

6	1	Type of Value	A - Area (Internal Standards).

P - % Abundance of base
(DFTPP/BFB); S - % Abun-
7-9	3	blank	dance of secondary ion.

10-17	8	First Mass	Gives the DFTPP/BFB masses

18	1	blank	(right justified) e.g. 442.

19-28	10 First Area or % Abundance up to 10 decimal digits,

29	1	blank	right justified

30-37	8	Second Mass (DFTPP/BFB) Leave columns 30-68 blank

38	1	blank	for Internal Standards.

Up to three masses and

39-48	10 Second Percent Abundance percent abundances may be

49	1	blank	given on each record for

DFTPP/BFB data. Those ions
50-57	8	Third Mass	that require two % values

58	1	blank	must be listed twice.

59-68	10 Third Percent Abundance

H-72

2/88
-------
8.9 Format of the Auxiliary Data Record (Type 32)

Use: Used to report scan number and retention time (In minutes) for Internal
Standards and for TIC compounds. Used to report retention time data for
Pesticides.

Position: Follows type 30. (Record will only be required as specified above.)

Record	Field	Field

Position	Length	Contents	Remarks

1-2	2	Record type	"32"

3-8	6	blank

9-10	2	"RT"	Indicates retention time.

11	1	blank

12-21	10	Retention Time in Minutes	Fixed or Scientific nota-

22	1	blank	tion as in Record Type 30.

23-24	2	"SC" or "RF"	Indicates scan number for

GC/MS or RT "From" Value

25	1	blank	for Pesticides.

26-35	10	Scan Number or Retention	In minutes.

Time "From" Value

36	1	blank

37-38	2	"RO" or blank	Indicates RT "To" Value for

39	1	blank	Pesticides.

40-49	10	Retention Time "To" Value	In minutes.

H-73

2/88
-------
8.10 Format of the Name Record (Type 33)

Use: To carry an analyte name for a TIC compound.
Position: Follows type 30 for TIC compounds.

Record

Position

1-2
3

Field
Length

2
1

Field
Contents

Record type
blank

Remarks
"33"

4-70

67

Name of compound

H-74

2/88
-------
8.11 Format of the Comment Record (Type 90)

First Use:	To provide for multiple Result Qualifier Flags from hardcopy

deliverable Form 1.

Position: Ionediately follows the type 30 record to which It applies.

Record

Poiltlgn

1-2

3

4-8
9

10-12
13

Field
Length

2
1

5
1

3
1

Field
Contents

Record Type
blank

"FLAGS"
blank

Remarks
"90"

Identifies this as a Form 1
Flags record.

Second Result Qualifier Flag See H-79 for definitions,
blank

14-16
17

Third Result Qualifier Flag
blank

18-20
21

Fourth Result Qualifier Flag
blank

22-24

Fifth Result Qualifier Flag

Second Use: To provide for Operator-Entered Comments.
Position: May occur anywhere.

Record
Position

1-2
3-4

5-70

Field
Lenyth

2
2

66

Field
Contents

Record Type
blank

Any Comment

Remarks

¦90"

Blank in column 4 identifies
this as an operator comment

H-75

2/88
-------
9. Definitions of Varlou. Codmm Used In Format B Records

9.1 Quality Control and Related Codas (QCC) In Typa 20 Records

Note: These QCC appear In the QC code fields of type 20 records. They are used
to indicate the typa of data that are being reported.

Q££ Name	Definition

LRB LABORATORY (REAGENT)	The "Method Blank" (See Exhibit G).

BLANK

LSD LABORATORY SPIKE

DUPLICATE BACKGROUND
(ORIGINAL) VALUES

An environmental sample which is analyzed according
to the analytical method, and subsequently used for
the matrix spike and the matrix spike duplicate
(See Exhibit G).

LF1 LABORATORY SPIKED
SAMPLE - FINAL -
FIRST MEMBER

The "Matrix Spike" (See Exhibit G)

LF2 LABORATORY SPIKED
SAMPLE - FINAL -
SECOND MEMBER

The "Matrix Spike Duplicate" (See Exhibit G)

LPC LABORATORY PERFORMANCE A solution of DFTPP or BFB used to establish the
CHECK SOLUTION	mass spectral tuning performance (See Exhibit G).

(tune data)

CLM

CLS

CLC

INITIAL CALIBRATION
MULTI POINT

INITIAL CALIBRATION
SINGLE POINT

CONTINUING CHECK
CALIBRATION

The Initial Calibration for GC/MS (See Exhibit G),
or the Initial Evaluation Standard Mixes (A,
B, C) for Pesticides (See Exhibit D PEST).
Response factors (GC/MS) or Calibration Factors
(Pesticides) rather than concentrations will be
reported on the following type 30 records.

The Initial Individual Standard/Toxaphene/Aroclor
Mixes used to determine all calibration factors.
(See Exhibit D PEST).

The Continuing Calibration for GC/MS (See Exhibit
G), or the subsequent Individual/Evaluation Stan-
dard Mixes for Pesticides (See Exhibit D PEST).

H-76

2/88
-------
OCC Nan*

CLD DUAL PURPOSE
CALIBRATION

Definition

A calibration solution as above used both as an
initial calibration (CLM) and a continuing check
(CLC). [50 level initial calibration if needed
for Form 8]

blank

Unknown sample, not associated with any quality
control item.

The following QCC values are used on type 20 records which act as a header, and
indicate that additional (usually calculated) analyte specific data will be
present on type 30 (and following type) records. Usually these data will apply
to an entire production run, in which case they will appear immediately following
the type 10 record. If the data apply to only a portion of the samples in the
run, they should be placed immediately preceding the samples to which they apply.
Much of the rest of the information in the type 20 record may be blank,
indicating that these data do not apply to these results.

MNC MEAN VALUES FROM
CALIBRATIONS

SDR MATRIX SPIKE DUPLICATE
CALCULATED RESULTS

The data following represent mean values and
percent RSD's from the initial calibribration
(GC/MS) or the evaluation mixes (Pesticides).

The data following represent calculated QC
results for the triplicate of samples LSD,
LF1, and LF2. Data will consist of the LF1
percent recovery, the LF2 percent recovery,
and the percent RSD for each method analyte
that was spiked according to the analytical
method as is present on hardcopy deliverable
Form 3.

9.2 Codes For Sample Medium (Matrix, Source)

Medium

All Media, Specific Medium not Applicable. Use for
Calibrations, Tunes, etc.

Water
Soil

Code
0

1
H

H-77

2/88
-------
9.3 List of Sample and Result Qualifiers

Definition: A sample qualifier or a result qualifier (also called a non-
numeric result) consists of 3 characters which act as an
indicator of the fact and the reason that the subject analysis
(a) did not produce a numeric result, or (b) produced a numeric
result but it is qualified in some respect relating to the type
or validity of the result.

9.3.1 Sample Qualifiers
Qualifier full

RIN RE-ANALYZED

REX RE-PREPARED

REJ REJECTED

Definition

The indicated analysis results were
generated from a re-injection of
the same sample extract or aliquot.

The Indicated analysis results were
generated from a re-extraction of
the same sample.

The analysis results have been rejected
for an unspecified reason by the
laboratory. For initial calibration
data, these data were not utilized in
the calculation of the mean.

SPL SPLIT RESULTS	The indicated environmental sample

or calibration has been split into
more than one analysis, and the analysis
results are reported as more than
one group of results (multiple type
20 records).

SRN SPLIT RESULTS -	A combination of "SPL" and "RIN"

RE-ANALYZED

SRX SPLIT RESULTS -	A combination of "SPL" and "REX"

RE-PREPARED

9.3.2 Result Qualifiers

BDL BELOW DETECTABLE LIMITS

NAR NO ANALYSIS RESULT

AVG AVERAGE VALUE

Indicates compound was analyzed for but
not detected; (Form 1 "U" Flag).

There is no analysis result required for
this subject parameter.

Average value - used to report a range of
values.

H-78

2/88
-------
Qualifier Full Hant

Definition

CBC

CANNOT BE CALCULATED

The analysis result cannot be calculated
because an operand value is qualified.
Identifies analytes whose Internal Standard
is not found.

LTL LESS THAN LOVER

CALIBRATION LIMIT

GTL GREATER THAN UPPER
CALIBRATION LIMIT

LLS LESS THAN LOVER STANDARD

TIE TENTATIVELY IDENTIFIED
-ESTIMATED VALUE

REJ REJECTED

STD INTERNAL STANDARD

STB INTERNAL STANDARD

BELOV DETECTION LIMITS

FBK FOUND IN BLANK

MSP PERCENT RECOVERY

Actual value is known to be less than the
lower calibration range due to dilution.
(Form 1 "D" Flag)

Actual value is known to be greater than the
upper calibration range. (Form 1 -E" Flag)

The analysis result is less than the sample
quantitation limit. (Form 1 "J" Flag)

The indicated analyte is a tentatively
identified analyte; its concentration has
been estimated. (Form 1-E or 1-F "J" Flag)

Same definition as above.

The indicated compound is an internal
standard. There is no analysis result to
report.

A combination of "STD" and "BDL".

The indicated compound was found in the
associated method blank (LRB) as well as
the sample. (Form 1 "B" flag)

The following value represents the percent
recovery for the "MS" sample. The remaining
two values give the "MSD" percent recovery
and the Percent RPD.

CON CONFIRMED

TFB TENTATIVELY IDENTIFIED
AND FOUND IN BLANK

ALC ALDOL CONDENSATION

Pesticide identification has been confirmed
by GC/MS (Form 1 "C" Flag).

A Combination of "TIE" and "FBK" (Form 1-E
or 1-F "B" flag).

Labels a suspected Aldol Condensation
product for TIC's (Form 1-E or 1-F "A"
Flag).

H-79

2/88
-------
9.4 Calculated Value Descriptors

These codes appear in column 47
columns 49-58.

OiiaHfiar	P"] 1

A	AMOUNT ADDED

P	PERCENT RECOVERY

D	PERCENT DIFFERENCE

B

PERCENT BREAKDOWN

9.5 Limit or QC Value Descriptors

These codes appear in column 60
columns 62-70.

PvaUficr

U

Full Nama
UNDETECTED

PERCENT RSD

SURROGATE RECOVERY
PERCENT DIFFERENCE

of Type 30 records to identify the value in

Definition

Identifies the amount of matrix spike analyte
added (for QC codes "LF1" and "LF2").

Identifies the Percent Recovery of the "MSD"
Sample in the Matrix Spike Results Record
(for QC Code "SDR")

Identifies the Percent Difference of the
Dlbutylchlorendate retention time for
pesticides (as on Form 8-E).

Identifies the Percent Breakdown of DDT and/or
Endrin (as on Form 8-D).

of Type 30 records to identify the value in

Definition

Value is the corrected saople quantitation
limit (Form 1 "U" Value).

Value is the Percent RSD for the Matrix Spike
and Matrix Spike Duplicate (QC Code "SDR") or
for the Mean Response Factors (QC Code "MNC").

Value is the Percent Recovery for the indicated
Surrogate.

Value is the Percent Difference of the Result
of the Continuing Check from that of the
Initial Calibration (as on Form 7).

H-80

2/88
-------
10. Example of the Sequence of Record Types In a File

10	Contains Run Header information

11	Contains additional run-wide information if required.

20	Occurs once for each sample, calibration, mean response factor,
matrix spike duplicate result, etc. - Acts as a header.

21

22	Contains additional information for samples.

23

30	Occurs once for each final analytical result. Reports

the value being determined as defined by the type 20.

31	Reports any Instrumental data necessary.

32	Reports any auxiliary data necessary.

33	Reports component names if necessary.

30	Values for the next analyte or parameter being measured.

31	Additional data may vary for each parameter, and records

32	may occur in any order. Multiple occurrences of the

32	same record type, however, must be consecutive.

33

30	Continues for as many as are necessary.

31

32

33

30

31

32

33

20	Next Sample Header record - The following applies to the next

21	sample or other group of data.

22

30

31

32

33

31

32

33

etc.

30

20

21

30

31

32

33

etc.

H-81

2/88
-------
11. Format of Records for Specific Uses

11.1 Format of the Sample Header Data Record (Type 20) for Mean Response Factors

Record

Field

Field



Position

LsugSh

Contents

Remarks

1-2

2

"20"

Record Type

3-15

13

blank



16

1

"0"

All matrices

17

1

blank



18-20

3

"MNC"

Identifies Mean Response

21-66

46

blank

Factors

67-69

3

Analyte count

Numeric; 1-3 decimal

digits; right
justified.

11.2 Format of the Results Data Record (Type 30) for Mean Response Factors

Record

Field

Field



Position

Length

Contents

Remarks

1-2

2

"30"

Record Type

3

1

blank



4

1

"C"



5

1

blank



6-14

9

CAS Number

Right justified.

15

1

blank



16-24

9

CAS Number Internal

Right justified





Standard Utililzed



25-31

7

blank



32-34

3

"AVG"

Indicates Average Value

35

1

blank

36-41

6

Mean Response Factor

Right Justified; fixed

42

1

blank or 'E'

or scientific notation

43-45

3

Exponent

Blank field will be

46-59

14

blank

Interpreted as "+00"

60

1

"R"

Indicates Percent RSD

61

1

blank



62-66

5

Percent RSD



67

1

blank or 'E'



68-70

3

Exponent



H-82

2/88
-------
11.3 Format of the Sample Header Data Record (Type 20) for Matrix Spike Duplicates

Record
fogltlon

1-2
3-6

7-11
12-15

16

17

18-20
21-25

26-30
31-66

67-69

Field
Length

2

4

5
4

1
1

3
5

5

36

Field

Contents

"20"
blank

EFA Sample I.D.
blank

Sample Medium/Matrix Code
blank

"SDR"
blank

Case Number
blank

Analyte count

Remarks
Record Type

Left justified. Raw
Sample I.D. only;

no suffixes.
"1" for water
"H" for soil

Identifies Matrix Spike
Duplicate Results

Numeric; 1-3 decimal
digits; right
justified. Counts
number of spiked
analytes.

11.4 Format of the Counter Record (Type 23) for Matrix Spike Duplicates
Position: Follows the type 20 to which it applies.

Record
Position

1-2
3-61

62

63

64-65

66

67

68

69-70

Field
Length

2

59

1
1

2

1

1
1

Field
Contents

"23"
blank

«pn

blank

Number of Percent Recoveries

Failing QC limits

blank

"R"
blank

Number of % RSD's Outside
Limits

Remarks
Record Type

Identifies Number of %
Recoveries outside of

limits.

Use the counter from
Form 3 for each sample.

# of % RSD's outside
limits.

From Form 3.

H-83

2/88
-------
11.5 Format of Che Results Date Record (Type 30) for Matrix Spike Duplicates

Record

Field

Field



Position

Length

Contents

Remarks

1-2

2

"30"

Record type

3

1

blank



4

1

"C"



5

1

blank



6-14

9

CAS Number

Right justified.

15

1

blank



16-24

9

CAS Number Internal

Right justified





Standard Utililzed



25

1

blank



26-30

5

"PERCT"

Units are "Percent"

31

1

blank



32-34

3

"MSP"

Indicates Matrix Spike

35

1

blank

Percent recovery

36-41

6

"MS" Percent Recovery

Right justified; fixed

42

1

blank or 'E*

or scientific notation

43-45

3

Exponent

Blank field is

46

1

blank

interpreted as "+00"

47

1

npn

Indicates Matrix Spike

48

1

blank

Duplicate Percent Recovery

49-54

6

"MSD" Percent Recovery

Format same as 36-46.

55

1

blank or 'E'



56-58

3

Exponent



59

1

blank



60

1

"R"

Indicates Percent RSD

61

1

blank



62-66

5

Percent RSD



67

1

blank or 'E'



68-70

3

Exponent



H-84	2/88
-------
11.6 Format of eh* Sample Header Data Record (Type 20) for Pesticide Evaluation Mix B

Record

Field

Field



Sotltion

Length

Content!

Remarks

1-2

2

"20"

Record Type

3-6

4

blank

7-11

5

"EVALB"

Sample I.D.

12-15

4

blank



16

1

¦0"

All matrices

17

1

blank



18-20

3

"CLC"

Indicates Continuing







Check

21-25

5

blank

(Pesticide Standard)

26-30

5

Case Number



31-38

8

blank



39-46

8

Date of Instrumental analysis

YY MM DD

47

1

blank



48-52

5

Hour, Min. of analysis

HH MM

53-66

14

blank



67-69

3

Analyte count

Numeric; 1-3 decimal

digits; right
justified. Vill be
"2" or "4".

H-8S

2/88
-------
11.7 The following type 30 record occurs once if reporting "Combined" breakdown only-
or three times if reporting separate breakdowns for Endrin and DDT along with tb4
Combined value.

Format of the Results Data Record (Type 30) for Pesticide Evaluation Mix B
(Percent Breakdown Data From Form 8D)

Record
Position

Field

Length

Field
Contents

Remarks

1-2

2

"30"

Record Type

3

1

blank

4

1

"C" or "I"

Use "C" - CAS Number







unless identifying







combined DDT and







Endrin, in which case

5

1

blank

use "I"

6-14

9

CAS Number

Right justified. Use







"COMBINED" for combined

15-25

11

blank

DDT and Endrin.

26-30

5

"PERCT"

Units

31-46

16

blank



47

1

"B"

Identifies Percent

48

1

blank

Breakdown

49-54

6

Percent Breakdown of

Right justified; fixed





Indicated Compound(s)

scientific notation

55

1

blank or 'E'

Blank field will be

56-58

3

Exponent

Interpreted as "+00"

H-86

2/88
-------
11.8 Format of the Results Data Record (Type 30) for Pesticide Evaluation Mix B
(Evaluation Standards Summary Data From Form 8E)

Record

Field

Field



Position

Leneth

Contents

Remarks

1-2

2

"30"

Record Type

3

1

blank

4

1

"C"



5

1

blank



6-14

9

" 1770805"

CAS Number

15-25

11

blank



26-30

5

"PERCT"

Units

31-46

16

blank



47

1

"D"

Identifies Retention Time

48

1

blank

Percent Difference

49-54

6

Retention Time Shift

Right justified; fixed





Percent D

or scientific notation

55

1

blank or 'E'

Blank field is

56-58

3

Exponent

interpreted as "+00"

H-87	2/88
-------
11.9 Format of the Sample Header Data Records (Type 20-23) for Continuing Checks
Format

Record

Field

Field



Position

Length

Contents

Remarks

1-2

2

"20"



3-6

4

blank



7-13

7

Identifier

e.g., VTD050

14

1

Daily Sequence Number

From Exhibit B

15

1

blank



16

1

"0"

All matrices

17

1

blank



18-20

3

"CLC"

Indicates

21

1

blank

Continuing Check

22-24

3

Sample Qualifier

See page H-79

25

1

blank



26-30

5

Case Number



31-38

8

blank



39-46

8

Date of Instrumental analysis

YY MM DD

47

1

blank



48-52

5

Hour, Min. of analysis

HH MM

53-66

14

blank



67-69

3

Analyte count

Numeric; 1-3







decimal digits;







right justified.

Record

Field

Field



frsltien

Leneth

Contents

Remarks

1-2

2

"21"

Record Type

3-17

15

blank



18-23

6

SAS Number

Leave blank

24

1

blank

if none.

25-35

11

Lab File I.D.







H-88

2/88
-------
Record
Position

1-2

3

4

5

6-13
14

15-19
20

21-31

Field
L£D££ll

2
1

1
1

8

1

5

I

II

Field
Contents

-23"

blank

NpM

blank

Date of associated
DFTPP/BFB injection
blank

Time of DFTPP/BFB injection
blank

DFTPP/BFB Lab File ID

Remarks
Record Type

Labels data as
"tune" data.

YY MM DD.
Aquisition date
of tune to be
linked with this
calibration.
HH MM

From instrument
data system.

Record

Field

Field



Position

Length

Contents

Remarks

1-2

2

"30"



3

1

blank



4

1

«C"



5

1

blank



6-14

9

CAS Number

Right justified.

15

1

blank



16-24

9

CAS Number Internal

Right Justified.





Standard Utilized



25-31

7

blank



32-34

3

Non-numeric result

See page H-79;

35

1

blank

also called a







result qualifier.

36-41

6

Response Factor

Right justified;

42

1

blank or 'E'

fixed or scientific

43-45

3

Exponent

notation. Blank

46-59

14

blank

field will be inter







preted as "+00".

60

1

"D"

Identifies

61

1

blank

Percent Difference.

62-66

5

RF Percent Difference

From Initial

67

1

blank or 'E'

Calibration

68-70

3

Exponent

(from Form 7).

H-89

2/88
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