DISCHARGE MONITORING REPORT -
QUALITY ASSURANCE (DMR-QA) STUDY 18
To Participating Chemistry Laboratories:
In March of 1998, the U.S. Environmental Protection Agency (USEPA) Office of Enforcement and
Compliance Assurance sent announcement letters to designated National Pollutant Discharge
Elimination System (NPDES) permittees, informing them that the USEPA and related state
agencies were continuing the NPDES Discharge Monitoring Report - Quality Assurance (DMR-
QA) studies. These announcements contained the chemistry sample ordering form that you
subsequently submitted. The purpose of these studies is to evaluate the analytical and reporting
ability of laboratories routinely performing chemistry and whole-effluent toxicity self-monitoring
analyses required in the designated NPDES permits. For further information, please refer to the
Chemistry Laboratory Requirements on page 1 inside.
Participation of NPDES permittees in this program, including proper analyses, reporting and
record retention, is mandatory based on the authority of Section 308(a) of the Clean Water Act.
The Agency's legal opinions, dated August 11, 1977 and January 9, 1989, reaffirm this authority.
If you have questions regarding the DMR-QA, please contact your state DMR-QA coordinator,
whose name address and telephone number are listed in the attached Chemistry Laboratory
Instructions. These offices will play an important role in providing any subsequent study follow-
up action or guidance. Please include the complete name, address, USEPA Lab Code and
telephone number of your laboratory in all correspondence.
Thank you for your cooperation in this national program to improve the quality of NPDES self-
monitoring data.
Enclosures (3):
1) Chemistry Laboratory Instructions
2) NPDES Chemistry Laboratory Data Reporting Form
3) Chemistry Samples (per your request)
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DMR-QA CHEMISTRY LABORATORY INSTRUCTIONS
TABLE OF CONTENTS
"
Starts on Page:
Hi '
Chemistry Laboratory Requirements 1
i" '' '" 11 i
\t i11 in
Chemistry Sample/Information Replacement Order Form 2
iiiii1 i ' ' MI i
Ampul Disposal Information... 5
Reporting Chemistry Data:
Completing the NPDES Chemistry Laboratory Data Report Form 6
1 ' ' r i i ;""
What to Do With the Form After Completion 7
'i! " '
Sample Preparation Instructions... g
i " ij
Method Code Reference Guide ?*s
11
Material Safety Data Sheets (MSDS) 39
List of DMR-QA State Coordinators Back Page
ii i
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DMR-QA STUDY 18
CHEMISTRY LABORATORY REQUIREMENTS
1. Some tests you normally perform for your permittee may not be included in the DMR-QA Study. You are
only required to perform analyses which have been requested by a permittee, provided they are included
in the study. Participating laboratories are required to perform only one of each type of analysis.
regardless of the number of permittees that request it. Review the analytes listed below to determine
which analyses must be performed to satisfy the DMR-QA reporting requirements for each NPDES
Permittee you support. To the extent feasible, analyze each DMR-QA sample the same way you would
analyze a routine sample, i.e., usual analyst, usual analytical system, usual procedures, etc.
Chemistry Analytes: aluminum, arsenic, cadmium, (total) chromium, cobalt, copper, iron, lead, manganese,'mercury, nickel, selenium,
vanadium, zinc, pH, non-filterable residue (total suspended solids), oil and grease, ammonia nitrogen, nitrate nitrogen, orthophosphate,
total Kjeldahl nitrogen, total phosphorus, 5-day biochemical oxygen demand, chemical oxygen demand, total organic carbon, 5-day
carbonaceous biochemical oxygen demand, total cyanide, total phenolics (by the 4AAP method), and total residual chlorine.
2. Ensure that you have received the appropriate study samples, reporting forms and instructions:
1. Replacement samples, reporting forms or instructions may be acquired by returning the completed
Chemistry Sample / Information Replacement Form on the next page. If you have analytical problems, the
available concentrate volume in each ampul is usually sufficient to prepare a second sample1.
2. Unused samples may be handled in one of three ways:
Properly dispose of unused samples ensuring compliance with all federal, state and local
regulations governing waste management. For more information regarding waste disposal, see the
Ampul Disposal Information on page 3.
Return unopened ampuls to the USEPA Contractor, ManTech Environmental, in accordance with
49 CFR 173.4, and using the return address on the sample shipment (4907 S. Alston Ave.,
Durham, NC 27713).
Retain samples for internal quality control. If stored at room temperature and out of direct light,
unopened samples are stable for at least one year. A complete list of "true'Ycalculated values may
be obtained after the results of the study have been distributed to permittees, which is expected to
occur in January, 1999. Your permittees may request a copy by contacting their Regional/State
Coordinator. Users of a Personal Computer w/modem may use the USEPA Office of Research
and Development Electronic Bulletin Board, modem number (513) 569-7700 or (513) 569-7610. If
you need assistance with use of the Bulletin Board, call (513) 569-7272 (do not call this number for
general information regarding PE Studies).
3. Perform the analyses requested by your permittees; refer to the enclosed NPDES Chemistry Laboratory Data
Report Form for a convenient listing of the analyses available in the study.
4. Report the results of your analyses and additional required information as specified on page 6, Completing
the NPDES Chemistry Laboratory Data Report Form.
5. Submit your reporting form to the requesting permittees in accordance with the instructions on page 7, Chemistry
Laboratory Reporting Procedure.
6. After official evaluation of the study data by the USEPA, permittees will receive Performance Evaluation
Reports and laboratories will be asked by the supported NPDES permittee(s) to explain reported values that
were not within the study acceptance limits. Permittees will then provide this explanation to the appropriate
USEPA or State Agency.
1Not applicable for the pH, demand and residue samples.
1
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I I I I I
!,! ill; ! DMR-QA STUDY 18
'l I I II
CHEMISTRY SAMPLE / INFORMATION REPLACEMENT ORDER FORM
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If replacement samples, reporting form or instructions are needed, copy this form, complete the information and
return it as Indicated below.
ll
1. USEPA Chemistry Laboratory Code: If you are unsure of your USEPA Lab Code, it can be found on the label used to
de}tyer your ortginal shipment or the label on page 1 of your NPDES Chemistry Laboratory Data Report Form
i ii I I
(State Code + 5 digits, for example NC12345)
2. Shipping Address:
i
Laboratory Name
ii
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Contact Name
Phone (_
Title
111 I •«
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Lalwaiory Shipping Address (No PO Boxes)_
City
State
_Zip Code_
3, Sarpples: Check the appropriate block(s). You may order only one of each ampul (The same analytical result for
epc/j gnafyte may be reported to all your permittees to satisfy their reporting requirements).
' '"'' " '' '' '''' '' "'' ' "
Denjancj,
Q TotalCyanide
f. •;. I ii B.t IIKS:. .;:: I ml , :! iiiiillili jliil; I ii iiillii iii
Q Residue
Q Total Phenplics
O Nutrients #1
a PH
Q Nutrients #2
Toa
I !
U Oil & Grease
, . Q
Report Form
Q Trace Metals #1
Q DMR-QA Chemistry Laboratory Instructions
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^^^$3£J&&
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nijiji&rf
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completed form to the USEPA|Contractor: ManTech|Environmental (919) 406-2246 attn: Terry Bundy.
!'filii|l Illlillllll^ BIIM^
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AMPUL DISPOSAL INFORMATION
U.S. EPA WATER POLLUTION PERFORMANCE EVALUATION SAMPLES
WP
Inorganic
Ampul
Trace Metals conc-1
Solvent
5%HNO3/H2O
Trace Metals conc-2
5%HNO3/H2O
Other
Contents
aluminum
arsenic trioxide
cadmium
chromium trioxide
cobalt
copper
iron
lead nitrate
manganese
mercuric oxide
methyl mercury chloride
nickel
selenium dioxide
vanadium pentoxide
zinc oxide
beryllium
molybdenum trioxide
potassium antimony tartrate
silver nitrate
strontium nitrate
thallium nitrate
titanium
Chemical
Formula
AI
As2O3
Cd
CrO3
Co
Cu
Fe
Pb(NO3)2
Mn
HgO
CHSHgCI
Ni
SeO2
V2O5
ZnO
Be
MoO3
KSbC4H4O7
AgNO3
Sr(NO3}2
TINO3
Ti
Max. Cone.
mg/L Ampul
410
150
110
210
110
110
410
500
410
3.2
3.8
310
300
2000
260
110
150
270
160
97
130
40
Minerals conc-1 A
Minerals conc-1 B
pH-Minerals conc-2
H2O calcium chloride CaCI2+2H2O 41000
hydrochloric acid HCI 150
magnesium chloride MgCI2+6H2O 34000
H2O potassium chloride KCI 7800
potassium sulfate K2SO4 9100
sodium bicarbonate NaHCOS 20000
sodium chloride NaCI 11000
sodium fluoride NaF 910
sodium sulfate Na2SO4 19000
H2O hydrochloric acid HCI 1700
potassium dihydrogen phosphate KH2PO4 6800
potassium hydrogen phthalate KHC8H404 10000
sodium hydroxide NaOH 1900
sodium borate "borax" B4Na2O7+10H2O 4600
tris(hydroxymethyl) aminomethane "THAM" H2NC(CH2OH)3 6100
Nutrient-1
Nutrient-2
Phenolics
H2O
H2O
H2O
ammonium chloride
potassium dihydrogen phosphate
potassium nitrate
glycine
sodium B-glycerolphosphate
2-chlorophenol
2,4-dichlorophenol
2,4-dinitrrophenol
phenol
NH4CI 7600
KH2PO4 2400
KNO3 30000
NH2CH2COOH 19000
(HOCH2)2CHOPO(ONa)2 11000
+5H20
CIC6H4OH 210
CI2H3OH 270
(NO2)2C6H3OH 300
C6H5OH 310
Demands
H2O
glucose
glutamic acid
C6H1105CHO
HO2C2HNH2(CH2)2CO2H
6800
6800
Cyanide
H2O
potassium ferricyanide
potassium hydroxide
sodium hydroxide
K3Fe(CN)6
KOH
NaOH
230
29
29
Residual Chlorine
H2O
sodium hypochlorite "Clorox"
NaCIO
440
Residue (TSS-nonfilt)
earth+salt
solid mix
solid mix
infusorial earth (calcined powder)
sodium chloride
(a natural clay)
NaCI
Maximum
percent of mix
50
99
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DMR-QA STUDY 18
CHEMISTRY LABORATORY REPORTING PROCEDURE
1) Make photo copies of the completed NPDES Chemistry Laboratory Data Report Form (pink colored
form).
2) Retain the original form for your files,
3) Contract labs should send 1 copy to each NPDES Permittee {your clients) who requested your
participation, by September 4,1998, This date should allow each permittee enough time to meet
their reporting deadline of September 30, 1998).
4) In-house labs may disregard the NPDES Chemistry Laboratory Data Report Form and report
directly on the NPDES Permittee Data Report Form (orange colored form). This form will be sent
in a separate mailing to each NPDES Permittee during the summer of 1998).
5) Do not submit NPDES Chemistry Laboratory Report Forms (pink colored forms) to the USEPA
Contractor, USEPA or to a State Agency; NPDES Permittees must report using NPDES
Permittee Data Report Forms (orange colored forms).
; Chemistry Labs should report to each
• NPDES permittee that they do analysis for,
• who requested data for this study.
: Permittees will transfer appropriate results received
: from inhouse and/or contract labs to the NPDES
: Permittee Data Report Form and submit it to the
• USEPA Contractor to represent the quality of their
• routine DMR data.
Chemistry
La b o rato ry
(You)
r
NPDES Chemistry Laboratory
Data Report Form
(1 Copy)
NPDES
(your client)
f
NPDES Permittee
Data Report Form
(Original Form + 1 Copy)
EPA
Contractor
(ManTech
Environmental)
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!! ...... r ....... D!V!R,QA STUDY 18
GENERAL INSTRUCTIONS
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* Immegiately ugon receipt of samples, check for breakage and correctness of sets shipped; see list
of requested sets on the bottom of the report form label. To request replacements for broken
1^-^
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er f^or this rjiailing; to obtain answers to questions, call your State or regional coordinator
(see Itsflriciuded in these instructions)! Sample replacement takes at least 2 to 3 weeks.
:i : l ;J J ' ";; it ' ' : : L : : :: ii:: : ii: ; : ~ :" :J; :i: iili; ' : " : ' : : ' =™=B " ! ' " : :
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', j ,,_ ; ;, ', *, , j,,, , .Bead insjrucjjons,,,,carefully'before opening ampuls'.
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s the same way you would treat a routine sample, i.e., usual analyst,
|1analytical system, usual procedures, etc.
I L 'Sample.
' '''
j gQ§!ie you regort, provide results of a sinqje analysis, as wouldi be done with a routine
ga bg§| resyltej ampul solutions and reagent water should be at room temperature (near20c
= s ; ; |i i ii I
Centigrade) when used.
* ll'^: / Arjifaer-coloregJo|al resiqluai chlorine gmpuis as well as the clear cyanide ampuls should be stored
^^s^s^^. away from' light" until the analyst is' ready to use them.
...... ..... ...... ''' ...... ..... ......
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Bouiiyto ...... avoid ..... cuts ...... orflnji'gass'.' ...... A ..... suggested ...... procedure ..... is ..... to ...... wfaplhe" ampui .......
PaP®rltowe"1 and.sna^off the arnuitoatthe narrow part of the neck.
^;; ;Unless otrierv\«|e stated,'samples neednxrt be filtered. '"' ' '
Uge only Class A volurnetrics.
r V!
"Reagent water" is equivalent to Type II Reagent Water as specified in ANSI/ASTM Standard D
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II5S i!!!!,!!h!!'™!|||:
i,a _,^ , P:te§se, ^Pj^il&ErS;,!! PQly, °n,§ Soncentration jperanalyte.
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DMR-QA STUDY 1.8
TRACE METAL SAMPLE
An ampul containing 5% nitric acid (v\v) is provided for preparation of the study sample.
SAMPLE PREPARATION
To prepare sample 1, fill a 1-L volumetric flask approximately 3/4 full with reagent water, pipette
10.0 mL (which contains 0.5 ml_ of concentrated nitric acid) of ampul 1 and 1.0 ml_ of trace-metal-grade
concentrated nitric acid into the flask, dilute to volume with reagent water, and mix well. The resulting
samples should be analyzed for the following analytes at levels within the stated concentration ranges.
Analyte
Aluminum
Arsenic
Cadmium
Chromium
Cobalt
Copper
Iron
Lead
Manganese
Mercury
Nickel
Selenium
Vanadium
Zinc
Concentration, micrograms
| per liter (ug/L) after dilution
| <5000
<2000
<2000
<2000
<2000
<2000
<4000
<4000
<4000
<60
<4000
<4000
<11000
<4000
Notes:
Samples, standards and reagent water blanks should all have the same acid matrix. The solution
resulting from the above dilution will contain 0.15% v/v nitric acid; additional or different acids may
be used as appropriate for analytical procedures or to match standards.
Mercury is present as a mixture of organic and inorganic forms. If a cold vapor method is
used, an aliquot of the sample must be digested before analysis for mercury. However,
digestion of this sample for any other metal analysis in unnecessary.
Chromium should be determined only as total chromium. When chromium is analyzed by direct
air-acetylene AA, use of matrix modifiers or the less sensitive oxidizing flame may be necessary to
control interfering ions. Preferably, use a fuel-rich nitrous oxide-acetylene flame for best results.
Some analytes may occur at concentrations that are too low for determination with simple direct AA
and must be determined with ICP, furnace AA.^or AA after chelation extraction (where approved) to
produce reportable results.
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I '" 11 ' ' i !'
DMR-QA STUDY 18
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• With some methods (such as colorimetric chromium method 3500D from Reference 74),
preparatory extraction may be required to remove relatively high concentrations of interferences
-'-'I'liVi.ii
< • ;*" Bfc^jiise'many analysts will" use atomic absorption or inductively coupled plasma spectrometry,
s™^^^^ asp!ratibnslorllmeasuremehf.s may be obtained to determine an analyte concentration, as
' ;;: ji ; wstli.rpjjBoe.samples". ' \
if • •• i I = i i i* l^alforrrij was' used. ^ ^ _
;;,:,! ; ;;; ; ;; I:;! ; ;g,, > ; ;,; ;; ; ; ; • ; i; ; ;J „ ; ;; „: ;„; ; ;;; ;::i;3 ,;• ; , 1 ;, ; ;, ] ;;: |, ,,:,; ;i, ; ii; | il; 1 ;, £ i^(; ;! ;,,;,;>!.:,:; L;! ;;,^_ i .it; Li
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]t; : '. ; : JT : : ::7: '. " ; d! : ; '. : " CcJ^K^mpuls contain 5% nitric acid.
• : : : 7" : : : ::: "t : CORROSIVE/OXIDIZER -TOXIC -SEVERE IRRITANT
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-. i •= i - - jiS| =i ' j Material Safety Data Sheets are attached
! ; i • ' ' i • Ij rri jflg-gglgly foij^wing {Re sampfe preparatibri instructions.
,i, if'1!1' . - [• . ' . : !:!; •., " , .'. ,"" ,'':"•, ; - •.'•.' ,, : • ' „: '.. » !.i , . /I'1''1" '••,•' i
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DMR-QA STUDY 18
pH SAMPLE
SAMPLE PREPARATION
To prepare the pH sample, pour the contents of the pH ampul directly into a <50-ml_ beaker; do
not dilute before determining pH.
NOTES:
We acknowledge that, ideally: 1) the strong memory effects of the calibrating buffers are removed
by allowing the electrode(s) to soak in some of the sample prior to analysis, and 2) laboratories
should be able to use their entire routine analytical procedures in performance evaluation studies.
However, there are practical limits to the amount of pH sample we can provide to you in our
studies.
Therefore, we propose that you soak your electrode(s) in distilled water to remove the memory
effect of the calibration buffers before you analyze our pH sample as directed in the study
instructions. We believe this adjustment to your normal procedure is reasonable, effective and
should not adversely affect your chances of successful performance.
If you cannot produce a valid pH measurement from your analytical system using a sample of 20
mL (or 40 ml_ using the contents of an additional ampul which is available upon request), your
analytical system is beyond the scope of this study. For example, systems for continuous pH
measurement may require a minimum sample size which is incompatible with the current study
design. If your pH system is incompatible with the study design, you should discuss this with your
State DMR-QA Coordinator (see list at back of this set of instructions).
END OF INSTRUCTIONS FOR pH
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DMR-QA STUDY 18
NUTRIENT SAMPLES
Two ampuls containing reagent-water solutions are provided to prepare two separate samples.
Sample 1 will contain inorganic nitrogen and phosphorus and may be analyzed for ammonia nitrogen,
nitrate nitrogen, and orthophosphate phosphorus. Sample 2 will contain organically-bound forms and may
be analyzed for total Kjeldahl nitrogen and total phosphorus. When prepared according to instructions,
samples will contain <50 mg/L of each nutrient.
SAMPLE PREPARATION
To prepare sample 1, fill a 1-L volumetric flask approximately 3/4 full with ammonia-free, reagent
water, pipette 10.0 ml_ of ampul 1 solution into the flask, dilute to volume with reagent water, and mix well.
To prepare sample 2, repeat the procedure with ampul 2.
NOTES:
Solutions in ampuls were preserved by autoclaving the sealed ampuls. Because this preservative
treatment is not effective after ampuls are opened, open ampuls just before analysis.
If a solution is not to be analyzed within two days after preparation, preserve a sample aliquot with
0.2 mL of concentrated sulfuric acid per 100 mL of sample (pH <2) and store at 4°C until just
before analysis. Analyze the preserved sample as soon as possible within the maximum 28-day
holding time.
Report results as milligrams per liter with three figures.
END OF INSTRUCTIONS FOR NUTRIENTS
11
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DMR-QA STUDY 18
DEMAND SAMPLE
One ampul containing reagent-water solution is provided to prepare one sample. The sample may
be analyzed to determine 5-day biochemical oxygen demand (BOD), 5-day carbonaceous BOD (CBOD),
chemical oxygen demand (COD), and total organic carbon (TOG).
SAMPLE PREPARATION
To prepare the sample, fill a 1-L volumetric flask approximately 3/4 full with reagent water, pipette
20.0 mL from the ampul into the flask, dilute to volume with reagent water, and mix well. The sample is
ready for analysis to determine 5-day BOD, 5-day CBOD, COD and TOG. Each measured value should be
<300 mg/L.
NOTES:
• The ampul contains about 21 mL of solution; if clean dry pipettes are used, this is sufficient to
prepare the sample. More ampuls may be requested if both 5-day BOD and 5-day CBOD are to be
determined. If an additional sample is needed, complete the "Request for Sample Replacement"
sheet attached to the cover memorandum and submit as directed.
• The solution in this ampul was preserved by autoclaving the sealed ampul. Because this preserva-
tive treatment is not effective after the ampul is opened, open the ampul just before analysis.
• Begin the BOD and/or CBOD as soon as possible after sample preparation. If cooled to 4°C, the
maximum holding time for these analyses is 48 hours. If COD and/or TOG cannot be analyzed
within your usual holding time after sample preparation, an aliquot should be preserved (pH <2)
using 0.2 mL of concentrated sulfuric acid per 100 mL (or an equivalent amount of another acid
which is compatible with your chosen methods). This acid preserved portion should be stored at
4°C and analyzed as soon as possible within the 28-day maximum holding time.
• 5-day BOD and 5-day CBOD: For proper oxygen depletion, the sample should be tested in a
dilution series such as 4%, 8%, and 16%. Use a natural surface water, diluted domestic sewage,
or commercially available seeds for seeded dilution water and avoid entrainment of air. For a 5-
day CBOD, the use of a nitrifying inhibitor is recommended.
• Be sure to determine the "blank" BOD of your seeded dilution water so that the proper seed
correction can be made (See STANDARD METHODS, 17th edition, Page 5-6).
• Report results as milligrams per liter with three figures.
END OF INSTRUCTIONS FOR DEMAND
13
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DMR-QA STUDY 18
CYANIDE SAMPLE
One ampul containing a reagent-water solution is provided to prepare one sample.
SAMPLE PREPARATION
To prepare the sample, fill a 1-L volumetric flask approximately 3/4 full with reagent water and add 1 mL of
1N NaOH. Pipette 10.0 ml of the solution from the ampul into the flask, dilute to volume with reagent
water, and mix well.
NOTES:
• CAUTION: The sample should be analyzed as soon as possible after opening and diluting.
• The cyanide concentration will be <2 mg/L.
• To prevent a concentration change, the ampul and, even more importantly, the prepared sample
should not be exposed to sunlight or other ultraviolet light any longer than necessary. Therefore,
perform the analysis immediately after sample preparation.
• The specified addition of 1 mL of 1 normal sodium hydroxide is only a recommended minimum to
prevent the loss of cyanide. If another amount, or even another base (such as KOH) is part of the
analyst's "normal routine", it is his/her option to change the recommendation.
• Since all the cyanide is present in soluble forms, filtration of the sample is not necessary, however,
the sample will require distillation.
• The presence of a precipitate in the ampul is not a problem, unless it is blue in color.
• Report results as milligrams per liter with three figures.
END OF INSTRUCTIONS FOR CYANIDE
15
-------
DMR-QA STUDY 18
NON-FILTERABLE RESIDUE (TOTAL SUSPENDED SOLIDS) SAMPLE
One vial containing homogeneously mixed solids is provided to prepare one sample.
SAMPLE PREPARATION
To prepare the sample, fill a 1-L volumetric flask about 3/4 full with reagent water. Soon after
opening and without drying, weigh 500 mg of solids from the vial and quantitatively transfer to the volumetric
flask using a glass funnel and wash bottle filled with reagent water. After rinsing the glass funnel
thoroughly and removing it, dilute flask contents to volume with additional reagent water (see notes) and
mix by inverting the flask 10 times. Let the sample flask stand for 10 min and invert again 10 times.
Immediately after the second set of inversions, rapidly measure a 500-mL aliquot into a graduated cylinder
by repetitively mixing and pouring so as not to allow solids to settle in the flask before the transfer is
complete. Filter this 500-mL aliquot and determine the non-filterable residue (total suspended solids)
according to your chosen routine method.
NOTES:
Do not dry the vial contents prior to weighing the 500 mg of mixed solids. Weigh the solids as
received without any preparatory action.
If a significant portion of the weighed (500 mg) solids fails to disperse evenly and stubbornly floats
on the surface, add a few drops of diluted detergent to the partially filled sample preparation flask.
For example, dissolve approximately 10 mL of detergent in 100 mL of reagent water and mix.
Then add 2 drops of this diluted detergent to the sample preparation flask, mix, observe, and
repeat (if necessary) the 2 drop additions until the suspended sample appears to be dispersed
evenly. Choose a detergent which will rinse clean from the Gooch crucible and filter pad without
leaving a measurable residue requiring a blank subtraction. Possible conveniently accessible
choices might be Triton-X-100, or any house-hold liquid dish-washing detergent void of insoluble
ingredients. If your detergent fails to disperse the solids evenly and it was not Triton-X-100, try
Triton-X-100. If all else fails, request a new ampul.
CAUTION: The analysis should be performed soon after the 500 mL aliquot is obtained.
Report results as milligrams per liter with three figures.
Ampuls contain NaCI.
IRRITANT
Material Safety Data Sheets are attached
immediately following the sample preparation instructions.
END OF INSTRUCTIONS FOR NON-FILTERABLE RESIDUE
17
-------
DMR-QA STUDY 18
OIL AND GREASE SAMPLE
One ampul containing a solution of oil and grease in n-propanol and glycerol is provided to prepare
one sample.
SAMPLE PREPARATION
To prepare the sample, add 994 ml_ of reagent water and 5 mL of 1:1 hydrochloric acid into a 2-L
separatory funnel and mix. Pipette 1.0 mL of the ampul solution into the separatory funnel and mix well.
Analyze the sample using whatever analytical method you most often use on routine samples. Note that
data produced using hexane for extraction must be reported in a different place on the report form than
data produced using Freon for extraction.
NOTES:
To avoid a concentration change, the sample must be analyzed soon after the ampul has been
opened.
The sample should be analyzed with an approved gravimetric method, because it is not suitable for
an infrared method.
For calculations, assume that initial sample volume was 1000 mL.
Report results as milligrams per liter with three figures.
Ampuls contain n-propanol (flammable liquid)
and glycerol (irritant)
Material Safety Data Sheets are attached
immediately following the sample preparation instructions.
END OF INSTRUCTIONS FOR OIL AND GREASE
19
-------
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-------
DMR-QA STUDY 18
TOTAL PHENOLICS SAMPLE
One ampul containing a reagent-water solution is provided to prepare one sample.
SAMPLE PREPARATION
To prepare the sample, fill a 1-L volumetric flask approximately 3/4 full with reagent water. Pipette
10.0 mL from the ampul into the flask, dilute to volume with reagent water, and mix well. Analyze the
sample using a 4AAP method ONLY.
Notes:
• In each sample, the resulting total phenolic concentration will be <6 mg/L.
• The solution in the ampul was preserved by autoclaving the sealed ampul. Because this
preservative treatment is not effective after the ampul is opened, open the ampul just before analy-
sis.
« Do not report phenolic results determined with GC/MS, because GC/MS data are not equivalent to
data obtained with the 4AAP methods.
• Report results as milligrams per liter with three figures.
END OF INSTRUCTIONS FOR TOTAL PHENOLICS
21
-------
DMR-QA STUDY 18
TOTAL RESIDUAL CHLORINE SAMPLE
One ampul containing a reagent-water solution is provided to prepare one sample.
SAMPLE PREPARATION
To prepare the sample, fill a 1-L volumetric flask approximately 3/4 full with chlorine-free, reagent water.
Pipette 10.0 mL from the ampul into the volumetric flask, dilute to volume with reagent water, and mix well.
NOTES:
• In this sample, the resulting concentration of total residual chlorine will be <6 mg/L.
• To prevent a concentration change, the ampul and prepared sample should not be exposed to
sunlight or other strong light or agitation any longer than necessary. Therefore, perform the
analysis immediately after sample preparation.
• Report results as milligrams per liter with three figures.
END OF INSTRUCTIONS FOR TOTAL RESIDUAL CHLORINE
23
-------
DMR-QA STUDY 18
Method Code Reference Guide
Analyte
Method
Code Ref.-Method
Description
Trace Metals
Aluminum
(ICP)
(DCP)
Antimony
Arsenic
13
14
15
26
27
28
29
31
43
56
99
13
14
15
23
24
25
99
14
15
16
17
20
21
22
29
31
32
33
45
46
99
R19 - 200.7
R24 - 202.1
R24 - 202.2
R89 - 3111D
R89 - 3113B
R89 - 3500D
R89 - 3120B
R25 - D4190-82(88)
R79 - 1-3051-85
R80 - AES0029
Other
R24 - 204.1
R24 - 204.2
R19 - 200.7
R89 - 3111B
R89 - 3113B
R89 - 3120B
Other
R19
R24
R24
R24
R89
R89
R89
R89
- 200.7
- 206.2
- 206.3
- 206.4
- 3114B4d
- 3113B
- 3120B
- 3500C
R25 - D2972-88A
R25 - D2972-88B
R25 - D2972-88C
R79 - 1-3062-85
R79 - 1-3060-85
Other
Inductively Coupled Plasma
Atomic Absorption (AA):
Direct aspiration unless
otherwise noted
AA; Furnace
AA
AA; Furnace
Eriochrome Cyanine R
ICP
Direct Current Plasma
AA
DCP
AA
AA; Furnace
ICP
AA
AA; Furnace
ICP
ICP
AA; Furnace
AA; Gaseous hydride
Silver Diethyl-
dithiocarbamate
AA; Gaseous hydride
AA; Furnace
ICP
Silver Diethyl-
dithiocarbamate
Silver Diethyl-
dithiocarbamate
AA; Gaseous hydride
AA; Furnace
AA; Gaseous hydride
Silver Diethyl-
dithiocarbamate
25
-------
I,
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DMR-QA STUDY 18
'I!/
Analyt<
Method
Code
Ref.-Method
Description
Cadmium 13 R19
I, '' 14 R24
\ Ii 15 R24
20 R89
'21 R89
1 ' 22 R89
23 R89
24 R89
i 35 R25
'36 R25
I" , (37 R25
38 R2S
39 R25
44 R79
45 R79
i I'll 4 6 R,79
" 52 R8
'1,55 R81
l'i In i in1 5 6 R80
- 200.7
- 213.1
- 213.2
- 3111B
- 3111C
- 3113B
- 3120B
- 3500D
- D3557-90A
- D3557-90B
- D4l90-82(88)
- D3S"57"-9bC
- D3557-90D
-,. _ L _ LJ 1
- 1-3135-85
- 1-3136-85
- 1-1472-85
- p. 37
- 974.27
- AES0029
ICP
AA
AA; Furnace
AA
AA"; Chelation-extraction
AA; Furnace
ICP
Dithizone
AA
AA; Chelation-extraction
DCP '
Vbltametry
AA; Furnace
AA
AA
ICP "
AA
AA
DCP
M99 Other
i '
fchromium 13 R19
"i ,,'14 R24
" '] "III "115 R24
,i '1(16 R24
,('20 R89
i21 R89
i I1 2 2 Rg'9
'i j" ' ' ,l'23 R89
i ,i If 2 4 R89
1 ' ' '" 35 R25
I|M| " l"36 R25
ii38 R25
| 1 1 44 R79
ill 'i 5 5 R.8 IL
"! 56 R80
1 1 I
- 200.7
- 218.1
- 2is',2
- 218,3,
- 31llB
- 3111C
- 3113B
- 312'OB
- 3500D
- D1687-92B
- D4190-82(88)
- D1687-92C
- 1-3236-85
- 974.27
- AES0029
' i| j i i I 99 Other
IL ' ' I'll "
|
ICP
AA
AA; Furnace
AA; Chelation-extraction
AA
AA; Chelation-extraction
AA; Furnace
ICP
Diphenylcarbazide
AA
DCP
AA; Furnace
AA
AA
DCP
| |
1 i
ii
n i (PI
' II n i ii j
mill j i 1 III 1 i 1 1 i 1 ill ' 1 ll 1
(I 1,1
i
Ill
26
-------
DMR-QA STUDY 18
Method
Analvte Code
Cobalt 13
14
15
25
26
27
28
34
35
36
37
44
51
56
99
Copper 13
14
15
20
21
22
27
28
29
30
35
36
37
39
44-
45
52
54
56
57
99
Ref .
R19
R24
R24
R89
R89
R89
R89
R25
R25
R25
R25
R79
R8
R80
-Method
- 200.7
- 219.1
- 219.2
- 3111B
- 3111C
- 3113B
- 3120B
- D3558-90A
- D3558-90B
- D4190-82 (88)
- D3558-90C
- 1-3239-85
- p. 37
- AES0029
Description
ICP
AA
AA; Furnace
AA
AA; Chelation-extraction
AA; Furnace
ICP
AA
AA; Chelation-extraction
DCP
AA; Furnace
AA
AA
DCP
Other
R19
R24
R24
R89
R89
R89
R89
R89
R89
R25
R25
R25
R25
R25
R79
R79
R8
R41
R81
R80
- 200.7
- 220.1
- 220.2
- 3111B
- 3111C
- 3113B
- 3120B
- 3500D
- 3500E
- D1688-90C
- D1688-84A(88)
- D1688-90A
- D1688-90B
- D4190-82 (88)
- 1-3271-85
- 1-3270-85
- p. 37
- 8506
- 974.27
- AES0029
ICP
AA . . ,
AA; Furnace
AA
AA; Chelation-extraction
AA; Furnace
ICP
Neocuproine
Bicinchoninate
AA; Furnace
Neocuproine
AA
AA; Chelation-extraction
DCP
AA
AA
AA
Bicinchoninate
AA
DCP
Other
27
-------
DMR-QA STUDY 18 1
Method
Analvte Code
Manganese 13
14
15
20
21
22
28
29
35
36
37
38
43
54
56
57
58
99
Mercury 13
14
23
33
43
51
99
Molybdenum 13
14
15
23
24
25
42
52
99
Nickel 13
14
15
20
21
22
27
28
34
35
36
37
43
52
99
Ref . -Method
R19 - 200.7
R24 - 243.1
R24 - 243.2
R89 - 3111B
R89 - 3111-C
R89 - 3113B
R89 - 3120B
R89 - 3500D
R25 - D858-90A
R25 - D858-90B
R25 - D4190-82 (88)
R25 - D858-90C
R79 - 1-3454-85
R41 - 8034
R81 - 974.27
R81 - 920.203
R80 - AES0029
Other
R24 - 245.1
R24 - 245.2'
R89 - 3112B
R25 - D3223-91
R79 - 1-3462-85
R81 - 977.22
Other
R19 - 200.7
R24 - 246.1
R24 - 246.2
R89 - 3111D
R89 - 3113B
R89 - 3120B
R79 - 1-3490-85
R80 - AES0029
Other
R19 - 200.7
R24 - 249.1
R24 - 249.2
R89 - 3111B
R89 - 3111C
R89 - 3113B
R89 - 3120B
R89 - 3500D
R25 - D1886-90A
R25 - D1886-90B
R25 - D4190-82 (88)
R25 - D1886-90C
R79 - 1-3499-85
R80 - AES0029
Other
Description
ICP
AA
AA; Furnace
AA
•
AA; Chelation-extraction
AA; Furnace
ICP
Persulf ate
AA
AA; Chelation-extraction
DCP
AA; Furnace
AA
Periodate (pp. 2-113
2-117)
AA
Persulfate
DCP
Manual Cold Vapor
Automated Cold Vapor
Manual Cold Vapor
Manual Cold Vapor
Manual Cold Vapor
Manual Cold Vapor
ICP
AA
AA; Furnace
AA
AA; Furnace
ICP
AA
DCP
ICP
AA
AA; Furnace
AA
and
1
I
I
1
1
I
I
I
I
I
I
I
1
1
I
1
I
AA; Chelation-extraction 1
AA; Furnace
ICP
Heptoxime
AA
•
I
I
I
AA; Chelation-extraction I
DCP
AA; Furnace
AA
DCP
•
I
•
•
I
29
-------
•
Method
Analvte Code
Zinc 13
14
15
20
21
22
27
28
34
35
36
43
52
54
55
57
99
Nutrients :
Ammonia, 14
as Nitrogen 15
16
17
20
21
22
23
24
32
33
44
45
53
54
99
DMR-QA STUDY 18
Ref . -Method
R19 - 200.7
R24 - 289.1
R24 - 289.2
R89 - 3111B
R89 - 3111C
R89 - 3500F
R89 - 3120B
R89 - 3500E
R25 - D1691-90B -
R25 - D1691-90A
R25 - D4190-82(88)
R79 - 1-3900-85
R8 - p. 37
R41 - 8009
R81 - 974.27
R80 - AES0029
Other
R24 - 350.2
R24 - '350.3
R24 - 350.1
R24 - 350.2
R89 - 4500C
R89 - 4500E
R89 - 4500H
R89 - 4500G
R89 - 4500F
- R25 - D1426-89A
R25 - D1426-89B
R79 - 1-3520-85
R79 - 1-4523-85
R40 - 379-75WE
R81 - 973.49
Other
Description
ICP
AA
AA; Furnace
AA
AA; Chelation-extraction
Zincon
ICP
Dithizone
AA; Chelation-extraction
AA
DCP
AA
AA
Zincon (pp. 2-231 and 2-333)
AA
DCP
Titration
Electrode
Automated Phenate
Nesslerization
Nesslerization
Titration
Automated Phenate
Electrode
Electrode
Nesslerization
Electrode
Nesslerization
Automated Phenate
Automated Electrode
Nesslerization
31
-------
DMR-QA STUDY 18
Analvte
Kjeldahl
Nitrogen
Total
Phosphorus ,
as P
Method
Code
14
15
16
17
18
19
34
35
36
37
42
53
70
71
72
73
74
75
76
77
78
99
13
14
15
16
26
27
33
34
43
' 54
55
99
Ref . -Method
R24 - 351.3
R24 - 351.4
R24 - 351.2
R24 - 351.3
R24 - 351.3
R24 - 351.1
R25 - D3590-89A
R25 - D3590-89A
R25 - D3590-89A
R25 - D3590-89B
R26 - 1-4551-78
R81 - 973.48
R89 - 4500H
R89 - 4500B+E
R89 - 4500B+C
R89 - 4500B+F
R89 - 4500B+G
R89 - 4500C+E
R89 - 4500C
R89 - 4500C+F
R89 - 4500C+G
Other
R24 - 365.2
R24 - 365.3
R24 - 365.1
R24 - 365.4
R89 - 4500E
R89 - 4500F
R25 - D515-88A
R25 - D515-88B
R79 - 1-4600-85
R81 - 973.56
R81 - 973.55
Other
33
Description
Nesslerization
Pot entiome trie
Semi -automated Block
Digestion
Titration
Electrode
Automated Phenate
Titration
Nesslerization
Pot entiome trie
Semi-automated Block
Digestion
Automated Phenate
Titration
Automated Phenate
Macro Digestion + Titration
Macro Digestion +
Nesslerization
Macro Digestion + Electrode
Macro Digestion + Electrode
Semi -micro Digestion +
Titration
Semi-micro Digestion +
Nesslerization
Semi-micro Digestion +
Electrode
Semi-micro Digestion +
Electrode
Manual Ascorbic Acid
Reduction
Man. Ascorbic Acid Reduction
(2 reagents)
Automated Ascorbic Acid
Reduction
Semi -automated Block
Digestion
Manual Ascorbic Acid
Reduction
Automated Ascorbic Acid
Reduction
Manual Ascorbic Acid
Reduction
Semi -automated Block
Digestion
Automated Ascorbic Acid
Reduction
Automated Ascorbic Acid
Reduction
Manual Ascorbic Acid
Reduction
-------
DMR-QA STUDY 18
Analyte
Method
Code
Ref.-Method
Description
Total Cyanide
13
14
25
26
34
43
51
99
R24 - 335.2
R24. - 335.3
R89 - 4500D
R89 - 4500E
R25 - D2036-91A
R79 - 1-3300-85
R8 - p. 22
Other
Manual Spectrophotometric
Automated Spectro-
photometric
Titrimetric
Manual Spectrophotometric
Manual Spectrophotometric
Manual Spectrophotometric
Titration or Colorimetric
Non-filterable 12
Residue 24
(Total Suspended 42
Solids) 99
R24 - 160.2
R89 - 2540D
R79 - 1-3765-85
Other
Glass fiber 103° to 105°C
Glass fiber 103° to 105°C
Glass fiber 103° to 105°C
Oil and Grease
12 R24 - 413.1
13 R102 - 1664
23 R89 - 5520B
99 Other
Freon Extraction/Gravimetric
Hexane Extraction/
Gravimetric
Freon Extraction/Gravimetric
35
-------
DMR-QA STUDY 18
METHOD REFERENCES
R3 . "Standard Methods for the Examination of Water and Waste Water," 14th
ed., 1976. Available from the American Public Health Association,
1015 18th Street, N.W., Washington, DC 20036. •
R8. American National Standards on Photographic Processing Effluents,
April 2, 1975. Available from ANSI, 1430 Broadway, New York, NY
10018.
R19. "Inductively Coupled Plasma-Atomic Emission Spectrometric Method for
Trace Element Analysis of Water and Wastes," Appendix C, 40 CFR, Part
13 6 .
R24. "Methods of Chemical Analysis of Water and Wastes." U.S.
Environmental Protection Agency, NERL, Cincinnati, OH 45268, March,
1983 (EPA-600/4-79-020). Available from ORD Publications, CERI,
EPA, Cincinnati, OH 45268.
R25. Annual Book of ASTM Standards, Volumes 11.01 and 11.02 for Water,
merican Society for Testing and Materials, 1916 Race Street,
Philadelphia, PA 19103.
R26. Techniques of Water-Resources Investigation of the U.S. Geological
Survey, Chapter A-l, "Methods for Determination of Inorganic
Substances in Water and Fluvial Sediments," Book 5, 1979, Stock
#024-001-03177-9. Available from Superintendent of Documents, U.S.
Government Printing Office, Washington, D.C. 20402.
R40. Ammonia, Automated Electrode Method, Industrial Method Number
379-75WE, dated February 19, 1976, Bran & Luebbe (Technicon)
AutoAnalyzer II, Bran & Luebbe Analyzing Technologies, Inc.,
Elmsford, NY 10523.
R41. Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O.
Box 389, Loveland, CO 80537.
R42. COD Method, Oceanography International Corporation, 512 West Loop
P.O. Box 2980, College Station, TX 77840
R43 . Hydrogen Ion (pH) Automated Electrode Method, Industrial Method
Number 378-75WA, October, 1976, Bran & Luebbe (Technicon)
AutoAnalyzer II, Bran & Luebbe Analyzing Technologies, Inc.,
Elmsford, NY 10523.
R44. Iron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical
Company, P.O. Box 389, Loveland, CO 80537.
37
-------
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DMR-QA STATE COORDINATORS
' Alabama
E. John Williford
ALDept. ofEnv. Mgt.
1890 A. Cong. W.L. Dickinson Dr.
Montgomery, AL 36109
(334) 260-2700
Alaska
Karen Hoover
US EPA, Region X
OW-133
1200 Sixth Ave.
Seattle, WA 98101
(206) 553-1213
American Samoa
Sheila Wiegman
American Samoa EPA
Environmental Quality Commission
Pago Pago, AS 96799
(684) 633-2304
Arizona
Gary Brussels
AZ Dept. of Health Services
Environmental Lab Licensure
3443 North Central Ave., Suite 810
Phoenix, AZ 85012
(602) 255-3454
* Arkansas
Dick Cassat
AR Dept of Poll. Ctrl. & Ecology
8001 National Drive
Little Rock, AR 72209
(501) 682-0744
California
Bill Ray
CA State Water Res. Control Board
PO Box 944213
Sacramento, CA 95814-0100
(916)657-1123
Colorado
Carla Lenkey
CO Dept. of Public Division
Field Support Section
4300 S. Cherry Creek Dr.
Denver, CO 80222-1530
(303) 692-3603
Connecticut
Donald Gonyea
CT Dept. of Env. Protection
Water Management Bureau
PO Box 5066
Hartford, CT 06106-5066
(860) 424-3827
Delaware
Joe Mulrooney
DNR&EC
Water Pollution Branch
PO Box 1401
Dover, DE 19903
(302)739-5731
District of Columbia
William Ruby
Environmental Regulation Admin.
Water Resources Management Div.
2100 M.L. King Jr. Ave, SE
Washington, DC 20020
(202) 645-6601 ext. 3032
: Florida
Ed Sims
US EPA, Region IV
Water Management Div. (CWAES)
100 Alabama St., SW - Atlanta Federal
Center
Atlanta, GA 30303-3104
(404) 562-9768
Carlos Boueres
FL Dept. of Env. Protection
Quality Assurance Section
2600 Blear Stone Road, MS 6505
Tallahassee, FL 32399
(904) 488-2796
Georgia
Jeff Larson
GA Dept of Natural Resources
Env. Protection Div.
4244 Int. Pkwy, Suite 110 - Atlanta
Tradeport
Atlanta, GA 30354
(404) 362-2680
Guam
Jesus Salas
Guam EPA
PO Box 22439-GMF
Tiyan Barrigada, GU 96921
(671) 472-8863
Hawaii
Rendy Chow
HI Dept. of Health
State Laboratories Div.
2725 Waimano Home Rd.
Pearl City, HI 96782
(808) 453-6684
Idaho
Karen Hoover
US EPA, Region X
OW-133
1200 Sixth Ave.
Seattle, WA 98101
(206) 553-1213
* Illinos
Erin Rednour
niinois EPA
Bureau of Water
PO Box 19276
Springfield, IL 62702
(217) 782-9720
Indiana
Steve Kim
IN Dept. of Env. Mgt., OWM
Oper. Assist. & Training Section
PO Box 6015
Indianapolis, IN 46204
(317) 232-8793
Iowa
Charles Furrey
IA Dept. of Natural Resources
Henry A. Wallace Bldg.
900 E. Grand
DesMoines, IA 50319
(515) 281-4067
Kansas
Jack McKenzie
Kansas Dept. of Health & Env.
Laboratory Services & Research
Forbes Field Bldg. #740
Topeka,KS 66620-0001
(913) 296-1639
Kentucky
Donna Drury
KY Dept. for Env. Protection
Division of Water
14 Reilly Rd. Ft. Boone Plaza
Frankfort, KY 40601
(502) 564-3410 ext. 461
Louisana
Elaine Sorbet
LDEQ Water Lab
8618 GSRI
Baton Rouge, LA 70808
(504) 765-2406
Maine
David Dodge
ME Dept. of Env. Protection
Div. of Water Resource Regulation
State House, Station 17
Augusta, ME 04333
(207) 287-7659
fe Maryland
Marlene Patillo
MD Dept. of the Environment
Div. of Municipal Compliance
2500 Broening Highway
Baltimore, MD 21224
(410)631-3646
Melvin Knott
MD Dept. of the Environment
Industrial Wastewater Program
2500 Broening Highway
Baltimore, MD 21224
(410) 631-3906
Massachusetts
Ping Yee
MA Dept. of Env. Protection
Div. of Water Pollution Control
Training Center - Route 20
Milbury.MA 01527
(508)756-7281
* Michigan
Clyde Marion
US EPA, Region V
(WC-15J)
77 West Jackson Blvd.
Chicago, IL 60604
(312)353-5966
Minnesota
Kim Sandrock
MN Pollution Control Agency
520 Lafayette Road
St. Paul, MN 55155
(612) 296-7387
Mississippi
Phillip_Bass
MS Dept of Env. Quality
Office of Pollution Control
PO Box 10385
Jackson, MS 39204
(601) 961-5143
Missouri
Jack Pate
MO Dept. of Natural Resources
Water Pollution Control Program
205 Jefferson Street
Jefferson City, MO 65101
(573) 751-1399
Montana
Mike Pasichnyk
MT Dept of Environmental Quality
Water Protection Bureau
PO Box 200901
Helena, MT 59620-0901
(406) 444-5326
Nebraska
Chris Helms
Dept of Env. Quality
Water Quality Division
PO Box 98922
Lincoln, NE 68509-8922
(402) 471-2186
Nevada
Wendall McCurry
NV Div. of Environmental Protection
Bureau of Water Quality Planning
333 W. Nye Lane, Capitol Complex
Carson City, NV 89701
(702) 687-4670 ext. 3098
New Hampshire
Stephanie Larson
NH Dept. of Env. Services
Water Supply & Poll. Ctrl. Div.
P.O Box 95
Concord, NH 03301
(603)271-1493
* New Jersey
Linda Mauel
US EPA, Region n
2890 Woodbridge Ave. (MS-220)
Edison, NJ 08837-3679
(732) 321-6766
New Mexico
Patrick Hanson
NM Environmental Dept.
Rennels Bldg., Rm. N 2050
PO Box 26110
Santa Fe,NM 87501
(505) 827-2799
* NPDES Delegated State
Study 18
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