Form HI I I Q«;C. Report No. _ BUNKS LAB NAME _________ ____ CASE NO. DATE ____________________ UNITS Matrix Compound Metals: 1. Aluminum 2. Antinony 3. Arsenic 4. Barium 5. Beryllium 6* Cadmium 7. Calcium 8* Chromium 9. Cobalt 10 • Copper 11. Iron 12. Lead 13. Magnesium 14. Manganese 15. Mercury 16. Nickel 17. Potassium 18. Selenium 19. Silver 20. Sodium 21. Thallium 22. Vanadium 23. Zinc Other: Cyanide Initial Calibration Blank Value 4 • » . Continuing Calibration Blank Value 1 i • ! ; ! . Z 3 • • • , • • 4 • • Preparation Blank Matrix: Matrix: • ** • " • o. • • AR30I3U
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Form HI I IQ«;C. Report No. _
BUNKSLAB NAME _________ ____ CASE NO.DATE ____________________ UNITS
Matrix
Compound
Metals:1. Aluminum2. Antinony3. Arsenic4. Barium5. Beryllium6* Cadmium7. Calcium8* Chromium9. Cobalt10 • Copper11. Iron12. Lead13. Magnesium14. Manganese15. Mercury16. Nickel17. Potassium18. Selenium19. Silver20. Sodium21. Thallium22. Vanadium23. ZincOther:
Cyanide
InitialCalibrationBlank Value
4
•
» .
Continuing CalibrationBlank Value
1
i
•
! ;
! .
Z 3
•
•
•
,
•
•
4
•
•
Preparation BlankMatrix: Matrix:
•
**
• "
• o.•
•
AR30I3U
Fora VIIQ.C. Report No.
INSTRUMENT DETECTION LIMITS ANDLABORATORY CONTROL SAMPLE
' LAB NAME • CASE NO. DATELCS NO.
Compound
Iletala:1. Aluminum2* Antimony3. Arsenic4. J&arium5. Beryllium6. Cadmium7. Calcium8* Chromium9. Cobalt10. Copper11. Iron12. Lead13. Magnesium14. Manganese15. Mercury16. Nickel17* Potassium16. Selenium19. Silver20. Sodium21. Thallium22. Vanadium23. ZincOther:
Cyanide
Required DetectionLimits (CEDL)-UR/!
. 200601020055
5000105025100
5 .--. •5000
150.240
5000510
5000 . -:105020
10
Instrument DetectionLimits (IDD-ug/1ICP/AA FurnaceID* ____ !Df_ ___
9
•
MR
*
.
KR
Lab Control Sampleug/L mft/kc(circle one)
True Found ZR
•
•
s•
•
•
'•
•
KR - Hoc required
AR30I3UU• u 26
Fora VIIIQ.C. Report No*STANDARD ADDITION RESULTS
LAB HAMS ______- •_____' _____ CASS NO.DATS ___________________________ UNITS
SPASample t
•
•
Element
.
•
• •
— .
»
»
^
-.—
—
0 ADDASS.
•
•
1 ADOCON. ABS1
>
2 ADDCON. ABS.*
•
3 ADDCON. ABS.1
*
•
FINALCON.2
X*
»
'
r*
\^j
1 CON is the concentration added, A3S. is the instrument readout in absorbance orconcentration.
* Concentration as determined by MSA*"r" is the correlation coefficient.* - correlation coefficient is outside of control window of 0.995.
AR30I3I*5
.Form IXQ. C. Report No.
ICP SERIAL DILUTIONSLAB NAME ________ CASE NO.
EPA Sample No.DATE __________________ Lab Sample ID No.
Units _______Matrix
CompoundMetals:1 • Aluminum2. Antimony3. Arsenic4. Barium5. Beryllium6* Cadmium7. . Calcium6. Chromium9. Cobalt10. Copper11. Iron12. Lead13. Magnesium14. Manganese15. Nickel16. Potassium17. Selenium18. Silver19. Sodium20. Thallium21. Vanadium22. ZincOther:
Initial SampleConcentrationC I)
-•
.
•
'.• ..
-
- - * • " • •
' , ••' ''
.. . .
. .. „
Serial Dilution1Result(S)
•
- - - - -
•
. •
;
2 Difference2
*
s
« ™
.
*
*
•
1 Diluted cample concentration corrected for 1:4 dilution (see Exhibit D)2 Percent Difference - I1" sl x 100
INR - Not Required, Initial sample concentration less than 10 times IDLNA - Not Applicable, analyte not determined by ICF
AR30I3l<6
Fora XQC Report No.
HOLDING TIMES
LAB NAME
DATS __________________________ CASS NO.
2PASample No*
•
•
--
•
Matrix
„
DataReceived
•
.
•
MercuryPrep Date
•,
*
• .•
•
MercuryHolding Time
(Days)
•
•
•
CN PrepData
•
„
CNHolding Time
(Days)
•
V >
*,
•
. . . _ • /\ /
AR301347
Form XI (Quarterly)INSTRUMENT DETECTION.LIMITS; • J;
LAB NAME ' ' ____ DATE
ICP/Flame AA (Circle One) Model Number________ Furnace AA Number
Element
1. Aluminum
2* Antimony
3. Arsenic•
4. Barium
5. Beryllium
6. Cadmium
7. Calcium
8 • Chromium
9. Cobalt
10. Copper
11. Iron
12. Lead
Wavelength(nm)
••
CRDL(ug/L)
'200
=> 60
10
200
55
5000•
MO
50
25
100
5
IDL(ug/L)
•
Element
13. Magnesium
14. Manganese
15. Mercury
16. 'Nickel
17. Potassium
18. Selenium
19. Silver
20. Sodium
21. Thallium
22. Vanadium
23. Zinc -.
Wavelength(cm)
.•
.
CRDL(ug/L)
5000
15
0.2
40
5000t
5»
10
5000
10
50
20
IDL(ug/L)
Footnotes: e Indicate the instrument for vhlch the IDL applies with a "P" (for Iian "A" (for Flame AA),' or an T" (for Furnace AA) behind the IDL va.
• - • • ' •
• Indicate*elements commonly run with background correction (AA) witha "B" behind the analytical wavelength.
• If core than one ICP/Flame or Furnace AA is used, submit separateForms XI-XIII for each instrument.
COMMENTS:
Lab Manager
AR30I31*8
Fora XII (Quarterly)•
1C? Interelement. Correction Factors
LABORATORY_______________________-___ 1C? Model Number'DATE _____
Analyte
1* Antimony
2. Arsenic
3. Barium
4. Beryllium
5* Cadtaluo
6* Chromium
7. Cobalt
3. Copper •
9. Lead
10. Manganese*
11. Mercury
12. Xickel
13* Potassium
14. Selenium
15. Silver
16,. Sodiua
17. Thallium
13. Vanadium
19. Zinc
AnalyteWavelength(am)
*
•
.•
Interelement Correction Factorsfor
Al
*
Ca
•
•
•
Fe
.•
Mg
.
•
'
•
•
'
» "
s ,;
COMMENTS:
Manager———.—————flR3QI3>l9
Fore XIII (Quarterly)ICP Linear Ranges
LAB NAME __________•________________ ICP Model- Number .,__
DATE
Analyte
1. Aluminum
2. Antimony
3. Arsenic
4. Barium
5. Beryllium
6. Cadmium
7. Calcium
8. Chromium
9. Cobalt
10. Copper
11. Iron
12. Lead
IntegrationTine
(Seconds)
•
•
•
Concen-tration(ug/L)
•
Analyte
13. Magnesium
14. Manganese
IS. Mercury
16. Nickel•
17. Potassium
18. Selenium
19. Silver
20. Sodium
21. Thallium
22. Vanadium
23. Zinc
IntegrationTiae
(Seconds)
•
«
Concen-tration(ug/L)
.
f
» *
-
,
•
•
•
Footnotes: e Indicate elements not analyzed by ICP vith the notation "NA1
COMMENTS:
Lab Manager
AR30I350
Form XII (Quarterly) (cont'd)ICP Interelement Correction Factors
LABORATORY_________________________ ICP Model NumberDATE .
Analyte
1. Antimony
2* Arsenic
3* Barium
4, Beryllium
5. Cadmiua
6. Chromium
7. Cobalt
8. Copper
9. Lead
10. Manganese
11. Mercury
12. Nickel. - « .
13. Potassium
14. Selenium
15. Silver
16. Sodium
17. Thallium
13. Vanadium
19. Zinc
•
AnalyteWavelength(na)
,
•
•
•
Interelement Correction Factors .for
,
•
i
'
•
•
•
•
'
•
•
•
• *
•
•
« *
/
•
COMMENTS:
Lab Manager,
AR30I35I
EXHIBIT IV
Target Compound List (TCP and '•'* 'Contract Required Quantitation Limits (CRQD*
Quantitatlon Limits**_Water Low Soil/Sediment*
Volatiles____________ CAS Number______ug/L_________ug/Kg_____
1. Chloromethane 74-87-3 10 102. Bromomethane 74-83-9 10 103. Vinyl Chloride 75-01-4 10 104. Chloroethane 75-00-3 10 105. Methylene Chloride 75-09-2 5 5
6. Acetone 67-64-1 10 107. Carbon Disulfide 75-15-0 5 58. 1,1-Dlchloroethene 75-35-4 5 59. 1,1-Dichloroethane 75-34-3 5 510. 1,2-Dichloroethene (total) 544-59-0 5 5
11. Chloroform 67-66-3 5 512. 1,2-Dichloroethane 107.-06-2 5 5 .13. 2-Butanone 78-93-3 10 1014. 1,1,1-Trlchlorcethane 71-55-6 5 515. Carbon Tetrachloride 56-23-5 5 5 .
f 9
16. Vinyl Acetate 108-05-4 10 1017..Bromodichloromethane 75-27-4 5 518. 1,2-Dichlorcpropane 78-87-5 5 519. cis-l,3-Dlchloropropene 10061-01-5 5 520. Trichloroethene 79-01-6 5 5
*
21. Dibromochloromdthane 124-48-1 5 5.22. 1,1,2-Trichloroethane 79-00-5 5 523. Benzene 71-43-2 5 524. trans-1,3- 5 5
Dichloropropene 10061-02-625. Bromoform 75-25-2 5 5
26. 4-Hethyl-2-pentanone 108-10-1 10 1027. 2-Hexanone 591-78-6 10 1028. Tetrachloroethene 127-18-4 5 529. Toluene 108-88-3 5 530. 1,1,2,2-Tetrachloroethane 79-34-5 5 5
(continued)
1/87 Rev,
AR301352
Quantltation Limits**Low Soil/Sedimenta
Volatile*_____________CA5 Number_____ug/L________ug/Kg_____
31. Chlorobenzene 108-90-7 5 532. Ethyl Benzene 100-41-4 5 533. Styrene 100-42-5 5 534. Xylenes (Total) 1330-20-7 5 5
3Mediua Soil/Sediment Contract Required Quantitation Limits (CRQL) for VolatileTCL Compounds are 100 times the individual Low Soil/Sediment CRQL.
*Speclfic quantitation limits are highly matrix dependent. The quanticationlimits listed herein are provided for guidance and may not always be achievable.
**Quantitation limits listed for soil/sediment are based on vet weight. Thequantitation limits calculated by the laboratory for soil/sediment, calculatedon dry weight basis as required by the contract, will be higher.
1/87 Rev.
AR30I353
Target Compound List (TCL) andContract Required Quantitation Limits (CRQL)*
____Quantitation Limits**W a t e r L e v Soil/Sedimentb
Semlvolatiles________ CAS Number____ug/L________ug/Kg____
35. Phenol 108-95-2 10 33036. bis(2-Chloroethyl) ether 111-44-4 10 33037. 2-Chlorophenol 95-57-8 10 33038. 1,3-Dichlorobenzene 541-73-1 10 33039. 1,4-Dichlorobenzene <• 106-46-7 10 330
40. Benzyl alcohol 100-51-6 10 33041. 1,2-Dichlorobenzene 95-50-1 10 33042. 2-Methylphenol 95-48-7 10 33043. bis(2-Chlorolsopropyl)
ether 108-60-1 10 33044. 4-Methylphenol 106-44-5 10 330
45. N-Nitroso-di-n- /dlpropylamlne 621-64-7 10 330 • *
46. Eexachloroethane 67-72-1 10 33047. Nitrobenzene 98-95-3 10 33048. Isophorone 78-59-1 10 33049.,2-Nitrophenol , 88-75-5 10 330
50. 2,4-Dlmethylphenol 105-67-9 10 33051. Benzole acid 65-85-0 50 160052. bls(2-Chloroethoxy)
methane lll-91-l • 10 33053 2,4-Dichlorophenol 120-83-2 10 • 33054. 1,2,4-Trlchlorobenzene 120-82-1 10 330
55 Naphthalene 91-20-3 10 33056. 4-Chloroanillne 106-47-8 10 33057. Hexachlorobutadiene 87-68-3 10 33058. 4-Chloro-3-methylphenol
(para-chloro-meta-cresol) 59-50-7 10 33059. 2-Methylnaphtbalene 91-57-6 10 330
60. Hexachlorocyclopentadiene 77-47-4 10 33061. 2,4,6-Trlchlorophenol 88-06-2 10 33062. 2,4,5-Trichlorophenol 95-95-4 50 160063. 2-Chloronaphthalene 91-58-7 10 33064. 2-Nitroaniline 88-74-4 50 1600
(continued)
1/87 Rev.
AR30l35t»
.73. 2,4-Dinitrotoluene 121-14-2 10
84-66-2 10 330
Quantitation Limits**Water Low Soil /Sediment" '-" —
Senlvolatlles __________ CA5 Number ____ ug/L ________ ug/Kg _____ . j
65. Dimethylphthalata 131-11-3 10 330 |66. Acenaphthylene 203-96-3 10 33067. 2,6-Dlnltrotoluene 606-20-2 10 33068. 3-Nltroaniline 99-09-2 50 160069. Acenaphthene 83-32-9 10 330
70. 2,4-Dinltrophenol 51-28-5 50 160071. 4-Hitrophenol 100-02-7 50 160072. Dlbenzofuran 132-64-9 10 33073. 2,4-Dinitrotolue -- 0 33074. Dlethylphthalate
75. 4-Chlorophenyl-phenylether 7005-72-3 10 330
76. Fluorene 86-73-7 10 33077. 4-Nltroaniline 100-01-6 50 160073. 4,6-Dinltro-2-methylphenol 534-52-1 50 160079. N-nltrosodiphenylamlne 86-30-6 10 330
80. 4-Bromophenyl-phenylether 101-55-3 10 - 33031. Hexachlorobenzene 113-74-1 10 33082. Pentachlorophenol 87-36-5 50. 160083. Phenanthrene 85-01-8 10 33084. Anthracene 120-12-7 10 330
83. Di-n-butylphthalata 84-74-2 10 33086. Fluoranthene 206-44-0 10 33037. Pyrene * 129-00-0 10 33038. Butylbenzylphthalate 85-63-7 10 33039. 3,3f-Dichlorobenzldine 91-94-1 20 660
90. Benzo(a)anthracene 56-35-3 10 33091. Chrysene 213-01-9 10 33092. bis(2-Ethylhexyl)phthalate 117-81-7 10 33093. Di-n-octylphthalate 117-34-0 10 33094. Benzo(b)fluoranthene 205-99-2 10 330
(continued) \_J1/37 Rev.
AR30I355
^Quantitation Limits**
Low Soil/Sediment0Semlvolatiles _____ CAS Number ug/L ____ ug/Kg
95. Benro(k)fluoranthene 207-08-9 10 33096. Benzo(a)pyrene 50-32-8 10 33097. Indeno(l,2,3-cd)pyrene 193-39-5 10 33098. DibenzU.h) anthracene 53-70-3 10 33099. Benzo(g,h,i)perylene 191-24-2 10 330
^Medium Soil/Sediment Contract Required Quantitation Limits (CRQL) for Semi-Volatile TCL Compounds are 60 times the individual Low Soil/Sediment CRQL.
*Speci£ic quantitation limits are highly matrix dependent. The quantitationlimits listed herein are provided for guidance and may not always be achievable.
• • • :**Quantltation limits listed for soil/sediment are based on wet weight. Thequantitation limits calculated by the laboratory for soil/sediment, calculatedon dry weight basis as required by the contract, will be higher.
10/86
AR3DI356
Target Compound List (TCL) andContract Required Quantitation Limits (CRQL)* . .
Quantitation Limits**Water Low Soll/Sedimentc
_____Pestieides/PCBs________CAS Number____ug/L________ug/Kg ___t
100. alpha-BHC 319-84-6 0.05 3.0101. beta-BHC 319-35-7 0.05 8.0102. delta-BHC 319-36-3 0.05 8.0103. gamma-BHC (Undane) 53-39-9 0.05 3.0104. Heptachlor 76-44-8 0.05 8.0
105. Aldrln 309-00-2 0.05 8.0106. Heptachlor epoxide 1024-57-3 0.05 8.0107. Endosulfan I 959-98-3 0.05 3.0103. Dieldrin • 60-57-1 0.10 16.0109. 4,4'-DDE 72-55-9 0.10 16.0
110. Endrin 72-20-3 0.10 16.0111. Endosulfan II 33213-65-9 0.10 16.0112. 4.4'-DDD 72-54-8 0.10 16.0113. Endosulfan sulfate 1031-07-3 0.10 . 16.0114. 4,4'.-DDT 50-29-3 . 0.10 16.0
115. Methoxychlor 72-43-5 0.5 80.0 I116. Endrin ketone 53494-70-5 0.10 16.0 |117. alpha-Chlordane 5103-71-9 0.5 80.0118. gamma-Chlordane 5103-74-2 0.5 80.0119. Toxaphene 8001-35-2 1.0 160.0
120. Jlroclor-1016 12674-11-2 0.5 80.0121. Aroelor-1221 11104-23-2 0.5 80.0.122. Aroclor-1232 11141-16-3 0.5 80.0123. Aroelor-1242 53469-21-9 0.5 80.0124. Aroclor-1243 12672-29-6 0.5 80.0
125. Aroclor-1254 11097-69-1 1.0 160.0126. Aroclor-1260 . 11096-32-5 1.0 160.0
Soil/Sediment Contract Required Quantitation Limits (CRQL) for Pesticide/PCBTCL compounds are 15 times the individual Low Soil/Sedioent CRQL.
•
•Specific quantitation limits are highly matrix dependent. The quantitationlimits listed herein ate provided for guidance and may not always beachievable.
'•..**Quantitation Units listed for soil/sediment are based on wet weight. The quan-titation Limits calculated by the laboratory for soil/sediment, calculated onweight basis as required by the contract, will be higher.
1/87 Rev.
. - • AR301357
EXHIBIT Viii t
DELETED
AR30I358
EXHIBIT 71 IZI VOA
5.5 Documentation
The matrix spike (MS) results (concentrations) for nonspiked volatile TC"^compounds shall be reported on Form I (Organic Analysis Data Sheet) and \Jthe matrix spike percent recoveries shall be summarized on Form III (MS/MS*DRecovery). These values will be used by EPA to periodically update existingperformance based QC recovery Holts (Table 5.2). ,
4.
The results for nonspiked volatile TCL compounds in the matrix spikeduplicate (MSO) analysis shall be reported on Fora I (Organic AnalysisData Sheet) and the percent recovery and the relative percent differenceshall be summarized on Fora III (MS/USD Recovery). The RPD data will beused by EPA to evaluate the long tana precision of the analytical method.Detailed instructions for the completion of Fora III are in Exhibit B,Section III.
TABLE 5.2. MATRIX SPIKE RECOVERY LIMITS
Fraction Matrix Spike Compound Water . Soil/Sediment
VOA . 1,1-Dichloroathan* 61-145 59-172VOA . Trichlorethene 71-120 62-137.VOA I Chlorbbenzene . . :.... . . .'. 75-130 .60 133VOA::-:- •'-'• -Toluene-'': ' " ' '••"•••••. ;" 76-125 59-139VOA .• •'. Sanzene '•• . > 76-127 66-142
PART 6 - SAMPLE ANALYSIS6. Summary
Tha intent of Part 6 is to provide the Contractor with a brief summary ofongoing QC activities involved with sample analysis. Specific references
• are provided to help th« Contractor meat specific reporting and dellverablesrequirements of this contract.
6.1 Sample Analysis
Samples can be analyzed upon successful completion of the initial QCactivities. When twelve (12) hours have elapsad since thu inicial tunewas completed, it Is necessary :o conduct an instrument tune and calibra-tion check analysis (described in Part 2 of this Section). Any major systemmaintenance . such as a source cleaning or installation of a new column,. .vmay necessitate* a re tune and recallbratioh Irrespective of the twelve-hour ••*requirement (see Initial Calibration, Part 2). Minor maintenance~shculdnecessitate only the calibration verification (Continuing Calibration,Part 2)
•
6.1.1 Internal Standards Evaluation - Internal standard responses and re-tention times in all samples must b» evaluated Immediately after orduring data acquisition. If the retention time for any internal
... ,. • . . . - ,•"•_'•'•' ' " • ' ' . ' • . ' ' ' • " ' • ' '• • • - . - . - . 10/86 . '
AR30I359
uIll PEST
Documentation
The matrix spike (MS) results (concentrations) for nonspiked pesti-cide/PCB TCL compounds shall be reported on Form I (Organic AnalysisData Sheet) and the matrix spike percent recoveries shall be summarizedon Form III (MS/MSD Recovery). These values will be used by EPA toperiodically update existing performance based QC recovery limits(Table 5.2).
The results for nonspiked pestlcide/PCB TCL compounds in the matrixspike duplicate (HSD) analysis shall be reported on Form I (OrganicAnalysis Data Sheet) and the percent recovery and the relative percentdifference shall be summarized on Form III (MS/MSD Recovery). The RPDdata will be used by EPA to evaluate the long term precision of theanalytical method. Detailed instructions for the completion of FormIII are in Exhibit B, Section III.
TABLE 5.2. MATRIX SPIKE RECOVERY LIMITS*
Fraction Matrix Spike Compound Water Soil/Sediment
Pest. . Llhdane . 56-123 46-127Pes.ti.--••-: Heptachlor -. •. - 40-131 35-130Pest. Aldrin 40-120 34-132Fest. Dleldrln 52-126 31-134Pest. . Endrin • • 56-121 42-139Pest. 4,4'-DOT 38-127 23-134
* These limits are for advicory 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*
PART 4 - PESTICIDE QA/QC REQUIREMENTS
4. Summary .
Part 4 summarizes ongong QC activities Involved with pesticide/FCBanalysis that were detailed in Parts 1, 2 and 3 of this Section, anddescribes the additional QA/QC procedures required during the analysis ofpesticide/FCBs that are net covered in Parts 1, 2, and 3. .
4.1 The Contractor must perform the following:
4.1.1 Method Blank analysis as per Part 1 of this Section.
10/86AR30I360
TABLE 5.2. MATRIX SPIKE RECOVERY LIMITS
Fraction Matrix Spike Compound Water
BN 1,2,4-Trlchlorobenzene 39-93 33-107BN Acenaphthene 46-113 31-137BN 2,4-Dlnltrotoluene 24-96 -23-39BN Pyrena 26-127 35-142BN N-Nitroso-Oi-n-Propylamlne 41-116 41-126BN 1,4-Dlchlorobenzsne 36-97 23-104Acid Pentachlorophenol 9-103 17-109Acid Phenol 12-39 26-90Acid 2-Chlorophenol 27-123 25-102Acid 4-Chloro-3-Methylphenol 23-97 26-103Acid 4-Nltrophenol 10-30 11-114
PART 6 - SAMPLE ANALYSIS
6. Summary . . . . . •
The intent.of Part 6 is 'to provide the Contractor with a brief summary ofongoing QC activities involved with sample analysis. Specific references ar-provided to help the Contractor meet specific reporting and daliverables ,requirements of this contract. s—'
6.1 Sample Analysis
Samples can be analyzed upon successful completion of the initial QCactivities. When twelve (12) hours have elapsed since the initial tunewas completed, it is necessary to conduct an instrument tune and cali-bration check analysis (described in Part 2 of this Section). Any aajorsystea maintenance, such as a source cleaning or installation of a newcolumn, may necessitate a retuna and recalibratlon (see Initial Calibra-tion, Part 2). Minor maintenance should necessitate only the calibra-tion verification (Continuing Calibration, Part 2).
6.1.1 Internal Standards Evaluation - Internal standard response? and*retention times in all sampUs must be evaluated immediatelyafter or during data acquisition. If the retention time far anyInternal standard changes by aora than 30 seconds, the chromato-.graphic systea must be Inspected for malfunctions, and corrac-• '
. • tions made as required. The extracted ion current profile(EICP) of the internal standards must be racnitorad and evaluatedfsr each sample, blank, matrix spike, and matrix spike duplicate.The criteria are described in detail in tha instructions forFora VIII, Internal Standard Area Summary (see Exhbit 3, SectionIII). If the extracted ion current profile (EICP) area for anyinternal standard changes by more than a factor of two (-502 t
10/86
AR30I36I
EXHIBIT VIIIII VOA
TABLE 4.1. SURROGATE SPIKING COMPOUNDS
Amount in Sample/Extract*Compounds -: ' : • •______(before any optional dilutions)______
Fraction Water Low/Medium Soil
Toluene-dg VOA 50 ug 50 ug4-Bromofluorobenzene VOA 50 ug 50 ug1,2-Dichloroethane-d4 VOA 50 jig 50 ug ____
* At the time of injection.
4.2 Surrogate spike recovery must be evaluated by determining whether theconcentration (measured as percent recovery) falls inside the contractrequired recovery limits listed in Table 4.2.
• TABLE 4.2. CONTRACTREQUIRED SURROGATE SPIKE RECOVERY LIMITS- "
• ' Fraction'- ;" ' -Surrogate Compound' •' . Water ' Low/Medium Soil
VOA . Toluene-dg • • 88-110 81-117VOA 4-Bromofluorobenzene 86-115 74-121VOA l,2-Dichloroethane-d4 76-114 70-121
4.3 Treatment of surrogate, spike recovery information is according tcparagraphs 4.3*1 through 4.3.2.
4.3.1 Method Blank Surrogate Spike Recovery
The laboratory cust take the actions listed below if recovery ofany one surrogate compound in the volatiles fraction of the methodblank is outside of the required surrogate spike recovery limits.
4.3.1.1 . Check calculations to .ensure that there are no errors;, che. . ...".-. .-.. ';'••; Internal standard and surrogate- spiking solutions for ..' \.-..
•-.""' ' • • • • * • .'degradation, contamination, etc; also check instrument .performance.
•
£.3.1.2 Reanalyze the dlank or extract If steps in 4.3.1.1 failto reveal the cause of the noncompliant surrogate recover!
HR3dY962
Ill SV
PART 4 - SURROGATE SPIKE (SS) ANALYSIS
4. Summary O
Surrogate standard determinations are performed on all samples and blanks.All samples and blanks are fortified with surrogate spiking compoundsbefore purging or extraction in order to monitor preparation and analysisof samples.
4.1 Each sample, matrix spike, matrix spike duplicate, and blank are spikedwith surrogate compounds prior to extraction. The surrogate spikingcompounds shown in Table 4.1 ara used to fortify each sample, matrixspike, matrix spike duplicate, and blank with the proper concentrations.Performance based criteria ara generated froa laboratory results.Therefore, deviations froa the spiking protocol will not be permitted.
TABLE 4.1. SURROGATE SPIKING COMPOUNDS
Amount in Sample Extract*Compounds ____ (before any optional dilutions)________
Fraction Water Low/Medium Soil• ^ ^ MHM M MWi ^ V ^ ^ ^ ^ ^ M ^ ^ ^ ^ MVM B aBMBMn ^ B mi ^ MnBM ^ B Ma B H M ^ MHnM aMa BMHM BM H BMMMa ^ H ^
Nitrobenzene-d5 ..... -BNA. • - . - : . .---.SO'ug ...... . 50 ug . '2-Fluoroblphenyl'' BNA ' " '50 ug 50 ugp-Terphenyl-dj4 BNA . 50 ug 50 ugPhenol-d5 .. .. .BNA . . .. . 100. ug 100 ug2-Fluorophenol ' BNA 100 ug 100 ug2 4,6-Tri bromophenol__ BNA 100 ug___ 100 ug
* At the time of injection.
4.2 Surrogate spike recovery must be evaluated by determining whether theconcentration (measured as percent recovery) falls Inside the contractrequired recovery Halts listed in Table 4.2.
___ TABLE 4.2. CONTRACT REQUIRED SURROGATE SPIKE RECOVERY LIMITS ^_
Fraction Surrogate Compound Water Low/Mediua Soil
BNA ' 'Nitrobenzene-d'5 35-114 23-120 'BNA 2-Fluorobiphenyl 43-116 30-115BNA p-Terphenyl-dt4 33-141 18-137'BNA Phenol-d3 10-94 24-113BNA 2-Fluorophenol 21-100 25-121BNA .. 2,4,6-Tribromophenol O-123
I8/M AR30I363
Ill PEST
2.2 Surrogate spike recovery must be evaluated by determining whether the.concentration (measured as percent recovery) falls inside the advisoryrecovery limits listed in Table 4.2.
_____TABLE 4.2. ADVISORY SURROGATE SPIKE RECOVERY LIMITS_____________
Low/MediumFraction Surrogate Compound Water Soil/Sediment
Pest. Dibutylchlorendate (24-154)* (20-150)*
* These limits are for advisory purposes" only. They are not used to determineif 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 Analysiso Sample Analysis . / •o Matrix Spike/Matrix Spike Duplicate Analyses
. . . . . . . . . ? .•:••••.. A•/••••••;•./..••••.•••' •.•'• • • • • • . • . • • • • •The surrogate spike recovery data'is summarized on the Surrogate SpikePercent Recovery Summary (Torn II). Detailed Instructions for the
. .... . coop let ion. of Form. II are .in Exhibit. B, Section III.
PART 3 - MATRIX SPIKE/MATRIX SPIKE DUPLICATE ANALYSIS (MS/MSD)
3. Summary • . - ' ' • '
In order to evaluate the matrix effect of the sample upon the analyticalmethodology, the USEPA has developed the standard mixes listed in Table5.1 to be used for matrix spike and matrix spike duplicate analyses.These compounds are subject to change depending upon availability andsuitability for use as matrix spikes.
3.1 MS/MSD Frequency of Analysis
A matrix spike and matrix spike duplicate must be performed for eachgroup of saaples of a similar matrix, once:
•• ' o each Case of field samples received, OR V . ' -o each 20 field samples in a Case, ORo each group of saaples of a similar concentration level (soils
only), ORo each 14 calendar day period during which samples in a Case were
received (said, period beginning with the receipt of the firstsample in that Sample'Delivery Group),
whichever is cost frequent. •
40
EXHIBIT VIII
DELETED
47 AR30I365
EXHIBIT IX
Ill EC FORMSURROGATE RECOVERY
HATER MATRIXReview t Approval
LLI SAKPLE -=•-'NUMBER PERCENT RECOVERED Date
Fraction: ———VOLATILES-——— ———-————BASE UEUTRALS I ACIDS————— -PESTICIDES-08- 4-iroio D4-1.2 2-Fluoro Phenol Nitro 2-Fluoro 2,4,6- Ter Dibutyl Oxy
Coipoundi Toluene fluoro Oichloro phenol -OS benzene biphenyl Tribroio phenyl chlor chlor OUT OF SPECbenzene ethane -d5 phenol tJM endate dane d * YES)
8C liiits: 88-118 86-115 76-114 21-188 18-94 35-114 43-116 18-123 33-141 24-1S4 64-118 VOA BNA PEST Coetent
1838833
\mm1800883imm1888388
18838831883823 .13883831883333 r1883833
A - Surrogate recoveries are evaluated according to CLP. specifications. Saiples are re-extracted and re-analyzed ifthey fall outside of the CLP specifications.
AR30I366
LLI 9C FOR.1HATRII SPIKED DUPLICATE ANALYSIS
KATES MT8IX
Background LLII 1283311 Oati Revie» I ApprovalRatrix Spiki LLII !22i882Matrix Spike Oep. LLII 123B8B3 Oati ______________.
-———Spike It———— ————Spiki 12————— BC Halt Out ofOrganic Saiple Spiki Spiked Spike Recovery Spiked Spike Recovery for Spec
Contaiinant Caipound Result Added Result Recovered (X) Result Recovered (I) Recovery «*YesSroup (?pb) (ppb) (ppb) (ppb) (ppb) (ppb) Ion high
1,1 Dichlorosthani .10 23 NO a II ND 9 91 ill 1451Trichloraetheni NO 23 SO B 31 ND 8 81 71Z 1281
Volatile* 3en:sne ND 23 NO 1 il NO 3 IZ 731 1381Toluene .ID 23 NO 1 81 N9 8 81 761 1231ChlorobiMjne .10 25 NO 8 81 ND i 81 Til 1271
2-Chl:roph»ol HO 281 HO 9 81 HO 3 81 271 1231Phenol .10 289 SO 8 91 ND 9 91 121 391
Acids 4-Chloro-3-«ethylphenol ND 289 NO 9 91 ND 9 31 231 9714-Nitrcpher.ol MO 229 NO 9 91 ' NB 9 31 191 891Pentachlcrsohenol ND 239 NO 9 91 NO 9 31 911931
1.4-8icnlar:&snisneN-:1itr2i3Ci-fl-PropvUsi.*e
e l,2,4-Tric!il3robenzanetrail Acsnaohthsr.e
2~,4-2initr3toluaniDi-n-ButvlshthalatePyrene
LindaneHeotachlsr
ticides AiirinP.3--5DT
NONOSDNDNONBNO
N9•ID.10ND
139121139139189139139
9.9951.321.933.24
NONONDNDNDNOND
NDNONONO
913131813191
1 31
1 31I 31I 11! 91
NONDNONDNDNBNO
' NONONONO
9399999
9999
11919181919191
31919191
3el 97141! 1161•9Z 981461 1181241 961111 1171241 1271 •
!6Z 1231431 1311431 1231381 1271
Qieldrin NO 1.29 NO 9 11 ND 9 91 52! 1261Endrin NB 9.&1 NO 9 31 ND 9 91 !61 1211
NO - None Hetactid.
AR30I367
' L L I QC FQRHRATRIX SPIKED DUPLICATE ANALYSIS
HATER RATRIX
Data Review t Approval ______________ Date
LLI I 1888892 1888333Spiked Spiked Oup. Out of
Ccntatinant Result Result fiC Liiit SpecGroup Cotpound (ppb) (ppb) RPO for RPO «»yes
1,1 Oichloroethene NO ND 91 141Trichloroethene NO ND 91 141
Volatiles Benzene NO NO 81 111Toluene NO ND 81 131Chlorobenzcne NO NO 81 131
2-CMoropbenol NO ND 91 481Phenol NO NO 81 421
Acids 4-Chlcrc-3-nethylphenol NO NO 81 4214-Mitrophenol r NO NO 81 581Pcntachlorophenol ...,- : NO NO 11 381
l,4-9ichlorobenzcne NO NO 81 281!HitrcsDdi-n-PropyU»ine NO NO 81 381
Ba=; 1,2,4-Trichlorobenzens NO NO 81 2S1Neutrals Acinashthene •'•' < NO ND 81 31!
2,4-Dinitrotoluene ND NO 1! 281Si-n-Sutylphthalatf NO NO 3! 481Pyrtne ND ND 8! 311
Lindane ND NO 81 151Keptachlor NO ND 81 281
Pesticides Aldrin r NO NO 81 221p.p'-DOT ND KD 81 271Dicldrin NC NO 31 181Endrin . ND NO 8! 211
b° AR30I368
. EPA METHOD #624EXHIBIT X MATRIX SPIKE PERFORMANCE DATA
Trial Avg. std. Avg.Parameter 1 2 3 4 Valua Dev. % R^.
BenzeneBromodichloromathanaBromoformBromomethanaCarbon tatrachloridaChlorobenzeneChloroethane2-Chloroathylvinyl etherChloroformChloromethaneDibromochloromethane1 , l-Dichloroethane1 , 2-Dichloroethane1, 1-Dichloroethenetrans-l , 2-Dichloroethene1 , 2-Dichloropropanacis-l, 3 -Dichloropropenetrans-l, 3-DichloropropeneEthyl benzeneMethylene chloride1,1,2, 2-TetrachloroethaneTatracTxloroetheneTc ;na1, 1, 1-Trichloroethane1,1, 2-TrichloroethaneTrichloroetheneTrichlorofluoromethaneVinyl chloride
19.917.914.913.220.213.314.316.319.213.716.519.020.513.313.720.4IS. 64.9313.119.417.319.319.320.319.019.319.313.0
19.317.114.513.019.518.214.615.518.514.416.217.820.013.113.019.614.34.5717.413.617.319.218.419.313.513.613.912.8
19.316.715.212.019.113.313.215.713.03.4716.317.119.417.217.413.314.34.4517.713.018.419.013.513.318.913.717.811.0
19.318.114.411.420.313.412.615.313.310.516.317.419.217.317.619.914.14.4916.913.013.113.513.719.713.913.513.410.9
19.417.414.712.419.713.413.615.313.511.716.417.319.717.317.919.614.74.6317.513.517.919.113.719.613.318.713.611.9
'•. ;'?•Vlll. _l
0.2&-0.660.370.350.570.260.940.340.512.70.260.330.590.750.570.670.670.250.510.660.620.540.400.620.220.360.651.13
• t
877462999263799359323999
*39909PK-J3383939096949394949360
The theoretical valves for all parameters are 20 ppb except fortrans-l,3-dichloropropene which is 5.6 ppb.
This table was constructed to satisfy Section 8.2 of EPA 624,Fed. Reg/October 26, 1934.
BASE NEUTRAL AND ACID EXTRACTABLE ANALYSIS"EPA METHOD #625
MATRIX SPIKE PERFORMANCE DATA
Trial Avg. std. Avg.Parameter 1 2 3 4 Value Dev. * PPP.
AcenaphtheneAcenaphthyleneAnthraceneBenzo (a) anthraceneEenzo(b)fluoranthene ;Benzo (k) f luorantheneBenzo (a) pyreneBenzo (ghi) peryleneBenzyl butyl phthalateBis ( 2-chloroethyl) etherBis ( 2 -chloroethoxy) methaneBis (2-chloroisopropyl) etherBis ( 2 -e thy Ihexyl) phthalate4-Bromophenyl phenyl ether2 -Chloronaphthalene4-Chlorophenyl phenyl etherChryseneDibenzo ( a , h) anthraceneDi-n-butyl phthalate1 , 2-Dichlorobenzene1 , 3 -Dichlorobenzene1 , 4 -Dichlorobenzene3,3' -DichlorobenzidineDiethyl phthalateDimethyl phthalate2 , 4 -Dinitrotoluene2 , 6-Dinitrotoluene 'Di-n-octylphthalateFluoranthene
4y -
86.882.182.680.83.87.292.L06.89.980.699.388.783.771.296.92.576.980.578 . 666.760.161.287.374 . 868.985. B86.790.888.6
81.978.473.375.274.581.587.4103.84.180.795.5.81.079.375.890.488.972.074.672.164.559.559.985.870.367.678.979.184.180.4
83.581.673.569.786.287.596.118.85.781.597.685.781.167.593.591.75.495.973.568.166.274.481.170.967.281.276.887.687.5
82.781.172.377.876.467.491.5113.86.078.694.682.880.468.893.583.773.288.73.69.767.75.287.368.367.178.382.086.692.2
83.780.875.475.780.085.991.7110.86.480.496/864.681.170.893.389.074.484.874.367.363.267.785.471.167.781.161.287.387.2
2.151.654.814.445.502.943.526.692.461.232.113.381.873.65.2.293.842.199.232.922.213.958.252.942.720.833.404.272.774.94
63817576808692110868097. 858171938974857467636885716861818787
bi:
XBASE NEUTRAL AND ACID EXTRACTABLE ANALYSIS
EPA METHOD #625MATRIX SPIKE PERFORMANCE DATA
(Continued)
Trial Avg. std. Avg.Parameter 1 2 3 4 Value Dav. % Rec.
FluoreneHexachlorobenzeneHexachlorobutadieneHexachloroethanaIndeno (1,2, 3-cd) pyreneIsophoroneNaphthaleneNitrobenzeneN-Nitrosodi-n-propylaminePhenanthrenePyrene1,2, 4-Trichlorobenzene4-Chloro-3-methylphenol2rChlorophenol2 , 4-Dichlorophenol2 , 4-Dimethylphenol2 , 4-Dinitrophenol2-Methyl-4 , 6-dinitrophenol2-Nitrophenol4-NitrophenolPentachlorophenolPhenol2,4, 6-Trichlorophenol
84.967.356.557.0104.39.031.9106.93.4109.76.335.76.79.33.39.86.87.31.44.36.36.85.
73.364.759.157.594.584.078.1100.92.8*
97.972.631.378.76.31.43.93.93.32.47.92.36.87.
73.969.663.763.5116.87.382.999.797.091.175.391.573.34.35.33.92.91.34.50.36.39.83.
79.163.164.563.0105.36.431.4100.93.099.675.990.336.87.33.53.94.95.39.54.90.41.91.
80.467.661.060.3105.86.331.1101.'96.699.475.037.230.82.34.42.91.92.34.49.89.33.38.
2.992.063.303.433.792.152.033.052.577.381.674.374.43•4.932.993.413.593.423.564.273.002.452.50
306361601058781101.9799753'Bb S328442919234498938.88.
*1
.1I
The theoretical values for all parameters are 100 ppb.
This table was constructed to satisfy Section 3.2 of EPA 625,Federal Register, October 26, 1984.
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EXHIBIT XISOi- FOR THE MAINTENANCE OF
GAS CHROMATOGRAPH/MASS SPECTROMETER SYSTEMS
This SOP outlines both routine and non-routinemaintenance procedures to be used in the GC/MS lab at LancasterLaboratories, Inc. The Group Leader of GC/MS shall beresponsible for the implementation of this SOP.
I. Instrumentation
This SOP shall apply to the following instrumentation.
1. Finnigan OWA/1020 GC/MS System Serial number12777-0932 installed at LLI October, 1983.
'} 2. Finnigan 1020 GC/MS System Serial number 13270-0784installed at LLI August, 1984.
•' II. Routine Maintenance"1_ Routine maintenance procedures are outlined in "Finnigan
MAT. 1000 Series GC/MS System Operator's Manual" in thei Operator's Maintenance Section, page 4-1. More detailed
information can be found in "OWA/1020 Series Organics in Water1 Analyzer/1000 Series GC/MS Service Manual".
:i The routine maintenance procedures when completed shall .be entered onto the "GC/MS Routine Maintenance Log" sheet(Figure 1) by entering initials of person doing the work andthe date on which it was completed. A signed entry includingthe date and a detailed description of the maintenanceperformed shall also be made in the Instrument Maintenance Logof the appropriate instrument.
Weekly Maintenance
The GC septum (teflon face silicon rubber) shall bechanged at least once a veek or whenever maintenance isperforroc-d on the GC inlet pysten-.
AR30I377•J V
• . : : • .Maintenance on the CC injector end/or GC column ie
indicated by not being able to met specifications for thetailing factor of benzidine and pentachlorophenol as specifiedin EPA Method 1625. Another indication for injectormaintenance is that poor peak shape (badly tailing peaks) areobserved for the relatively active phenolic compounds,especially benzidine, 4-nitrophenol, and 2,4-dinitrophenol.The first step in cleaning the injector ie to remove the glassliner from the injector and heating it in a muffle furnace at500C for at least 3 hours or overnight. Thie oxidizes organiceadsorbed onto the liner. After cooling, the liner ic rinsedwith toluene, soaked in Sylon CT for approximately 1 minute(Sylon/CT is a silylation reagent available from Supelco),rinsed with toluene, and finally rinsed in nethanol to
»' "-.neutralize any residual Sylon CT reagent. This cleaned lineris then inserted into the GC capillary injector. If thechromatography remains poor after this procedure, perhaps theactivity in the chromatographic system ie in the GC column.Since the active cites are generally in the front section of*the column, they can be removed by cutting off approximately12-15 inches of the column head and discarding it. Afterassembly of the shortened column in the injector and thesubsequent injection of a test compound (BN or Acid Standard),and the activity problem remains, the column can be solventrinsed as per instructions that accompany the column whenreceived from the column vendor. If solvent rinsing does notsolve this activity problem, the column must be replaced.
In order to assure that the mechanical pump oil remainsfree of volatile compounds, the mechanical fore pumps shall bepurged according to page 4-13 of the OWA/1020 Operations Manualonce per week.
flR30!378
Monthly Maintenance
Several filter and fan units are located on the GC/MSSystem. The filters must be checked once per month to be sure ^~--that they are not clogged or are restricting air flow across ,/'
: the electronic components the air is to cool. If the filtersare dirty, they shall be cleaned by blowing compressed air in
"i the opposite direction of normal air flow to dislodge dustparticles. If the filter cannot be cleaned, it must be
; replaced. The filters to which this applies are located on thebottom of the card cage module and the filter inside the frontgrill on the disk drive. The heat exchanging radiator of therecirculating cooler used to cool the turbopump bearings mustalso be checked to be sure there are no obstructions to air
~i exchange and flow. The fans in the card cage, the powermodule, and the computer must also be checked to be sure they
'] are functioning normally.
* ' •"| Quarterly Maintenance
.. The mechanical rotary vane pump oil must be changed on aquarterly basis as outlined on page 4-13 or 1020 Operator's \^JManual. The oil used is Inland 15 Vacuum Pump Oil.
The absolute filter on the CMD disk drive shall bei changed on a quarterly basis as outlined on pages 10-16 of the
'"Cartridge Module Disk Drive for Finnigan MAT Incos and 1000•• . Series Data Systems" in the options section of the 1020
Operator's Manual.
Bimonthly Maintenance
During the routine analysis of samples on the GC/MSsystem, the ion source becomes coated with neutralizedcompounds which prevents proper interaction of the variouscharged surfaces of the source with the charged analyte ions.
6i
Therefore, the ion source must be periodically disassembled,cleaned and re-assembled. Ion source cleaning is generallyindicated by poor sensitivity and/or the inability to tune thesource to EPA tuning criteria. '
The ion source shall be cleaned at a minimum on abimonthly basis or more often as instrument performance woulddictate. Ion source cleaning is outlined in the MaintenanceSection of the 1020 Operator's Manual on pages 4-6 to 4-12.After ion source cleaning and reassembly of the ion source andpumping down the system, the analyst shall check variousparameters as indicated on the Poet Maintenance Checklist inthe 1020/OWA Operations Course Manual page 10-7.
Semi-Annual Maintenance
The turbo pump oil shall be changed on a semi-annualbasis. Instructions of how to perform this are found in the"Pfeiffer Manual Operating Instructions - Turbo Molecular PumpTPH 330, TPH 510", page 28 for the OWA (Ser. 112777) turbopump. The instructions for changing the bearing oil in the1020 (Serial # 13270) turbo pump are found on page 25 of the"Pfeiffer Manual Operating Instructions - Turbo-Molecular Pump,TPH 170, TPU 170". The oil used in this procedure ie PfeifferOiT12.
XII. Kon Routine Maintenance
Even with proper preventive maintenance performed on aroutine basis, equipment failure ie inevitable when workingwith GC/MS systems. >
Although it ie not possible to anticipate every eort ofequipment failure, the following general approach should beueed when encountering non-routine maintenance eituations.
1R30J380
7.. Check thrown t.hn 1020/OWA Operator's Manual,Service Manual, and Reference Manual fortroubleshooting helps that address the problem withwhich you are dealing. After studying the manuals,follow procedures described in an effort to solve *.jthe problem.
2. Technical help can also be obtained from FinniganMAT Technical Support by calling either(300) 354-9731 (Cincinnati, OH) or (300) 327-1061
... (San Jose, CA). If Technical Support cannot help• you, a service call is necessary.
1 3. To schedule service, call (301) 943-3817 (Rockville,MD) and ask for "service". David Painter is
] currently (August, 1985) the service manager forthis area.
I ' '4. In the event that replacement parts are indicated,
these can be ordered from San Jose, CA, by callingthe Finnigan MAT Parts Center at (408) 946-4343 withthe Finnigan MAT part number, part description and
' Lancaster Laboratories, Inc. P.O. Number. The partsgenerally can be obtained Federal Express next day
r service.
~] It is imperative that all service calls, maintenance and- repairs be recorded in the appropriate instrument maintenanceT log. The log entry shall include the date, a detailed
description of the action taken, and a full signature of theLancaster Laboratories, Inc. personnel involved.
In the event that a GC/MS system is inoperable, thefollowing persons shall be notified; GC/MS Group Leader,Organic Analysis Group Leader, Manager of Instrumental/Environmental Chemistry, and the Manager of Sample -Administration. This will allow for proper monitoring of theincoming workload and notification of possible turnaround timeincreases to prospective clients. When the instrument isfunctioning properly, the same persons shall be notified.
63 AR30I38I
w- GCKS ROUTINE MAINTENANCE LOGfor
FINNIGAN MODEL < _________SERIAL « _________
Record initials and actual date service was performed
Weekly
change gc eeptum
purge vaccuum pumpschange gc eeptumpurge vaccuum pumpschange gc septumpurge vaccuum pumpschange gc eeptum
purge vaccuun pumps
:",..
...
t
•
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AR30I382
EXHIBIT XIIWater & Soil for PurgeableOrganics by P&T/cc/MS #520Initiated Date 9/13/35Revised Date 10/1/86Page 3 of 10
Safety Precautions;-- The toxicity or carcinogenicity of each reagent used in
this method has not been precisely defined; however, eachchemical compound should be treated as a potential healthhazard. Exposure to these chemicals must be reduced to thelowest possible level by whatever means available. The—I • »
1 following parameters have tentatively been classified as known> or suspected carcinogens: benzene, carbon tetrachloride,"1 chloroform, 1,4-dichlorobenzene, and vinyl chloride.
• j Procedure:A. InstrumentaX Set—UP*
, The GC/MS is maintained in1 a stand-by condition when* it* is*not acquiring data. Generally, the computer* remains powered upin the stand-by mode. Should the computer have to be turnedon, it can be booted up by typing 11A 100160, carriage return, >/11A, L. froa the virtual console mode after the CMD disk drive
• "is turned on. The terminal, scope, and printer must also beturned on. After booting up and the system is in the MSDSexecutive (>) the proper parameters are entered into the datasystem using SCAN, GC, SYST, and ACQU before data acquisition
.: and data manipulation can be performed. Typical setting forthese programs are in Figures 2 and 3. The electrometer should
I then be turned on for about 15 minutes by typing ON in MSDS andallow it to equilibrate. The electrometer can then be zeroedby entering >MTUN and manually adjusting EZ so that the properamount of signal noise is observed. Figure 1 illustrates aproper zero setting using scan EZ to monitor noise of mass403. Following the zeroing, mass calibration is accomplishedby the CAH command. The cal gas override switch must be in theoff position during the mass calibration and then turned onafter CAH is completed. By using program SCAN, check to besure the correct scan program is entered as indicated on Figure v>2. The mass spectrometer is now ready to acquire data.
AR30I383
Water & Soil for PurgeableOrganice by P&T/GC/MS 1520Initiated Date 9/18/85Revised Date 10/1/86Page 4 of 10
The GC ie set for the volatile organic analysis byinstalling the 6 ft. x 1/8 in. glass column packed with 1%SP1000 on Carbopack B and setting the carrier flow to 30cc/min. By using the MSDS program GC, the following parametersare entered: zone temp. « 175, initial temp. « 45, final temp.«= 220, initial time = 2 min. temp, program « 10C/min., final
»time «» 10 Bin., separator temp « 250, manifold temp « 80, inj.mode B packed, fil/mul mode:- auto as indicated on Figure 2, GC
"] deecriptor.
| The Tekmar LSC-2 Liquid Sample Concentrator ie eet-upmanually by using the following conditions t purge pressure =
i 20 pei, purge flow « 40 ml/min:, purge « 11, deeorb = 04 -x 1, *bake « 07, 6 PI - 30C, SP2 « 45C, SP3 " 45C, SP4 -' 180C, SP5 «210C, auto/etep/hold « auto, desorb ready/deeorb preheat =
i hold, bake «* auto. The sorbent trap must be packed asdescribed in reference 1.
To be cure the system is ready for data acquisition andthat the heated zones are at proper temperatures, MSDS programSS should be run. Take note of the number of sectors remainingon the removable disk and be cure that adequate disk space ieavailable. Diek space can also be checked using > STAT/D andin ACQU. If the diek ie too full and must be changed, installold data diek, and prepare for use according to Appendix A.
Before acquisition of calibration standards or sample data,the mass spectrometer must be checked for proper tuning. Thisie done by analyzing an internal standard blank as described inSection D. Sample Analysis, which contains about 50 ppb of4-bromofluorobenzene (BFB) . The relative intensities of theobserved ions for BFB must fall within the following ranges:
HR30I381*
Water i Soil for PurgeableOrganics by P&T/GC/MS J520Initiated Date 9/13/35Revised Date 10/1/36Page 5 of 10
Relative Abundance50 15 - 40% mass 95
~ 75 30 - 60% mass 9595 base peak - 100%
* : 96 5-9% mass 95173 <2% mass 174174 , >50% mass 95
• 175 5-9% mass 174176 * >95% but <101% mass 174
I 177 5-9% mass 176The relative intensities of the BFB spectrum can be viewed
1 by running the procedure BFBCHECK or by manually obtaining aBFB spectrum in the CHRO program and using the L subcommand to
j obtain a mass listing at the apex of the BFB GC peak or toobtain an averaged or background corrected listing. To see ifthe BFB tuning intensity criteria listed above are satisfied,type B in the LIST program. If the BFB does not meet thecriteria listed above, the source must be retuned in programMTUNE and the internal standard blank reacquired. This processis repeated until the BFB criteria are met. Some guidelines
! for tuning an OWA are given in Appendix B. The area of mass123* of bromochloromethane of the internal standard blank must
'[ be >20,000 area counts to assure adequate sensitivity for allthe analytes in this method.
*«it
B. Instrumental Calibration:Individual stock standard solutions may be prepared for
instrumental calibration from pure standard materials bypipeting approximately 0.5 g (± .0001 g) of each pure standardmaterial- listed in Table 1 into separate 10 ml volumetricflasks that contain about 9.8 ml of MeOH. The volumetric flaskmust be dry around the top stopper joint so that accurateweights can be obtained. After the weight of the standard
> material is known, fill flask to 10 ml mark. Acrolein,
AR30I385
Water & Soil for PurgeableOrganics by PtT/GC/MS 1520Initiated Date 9/18/85Revised Date 10/1/86Page 6.bf 10
acrylonitrile, and 2-chloroethylvinylether are prepared asdescribed below as a separate mix due to the relative ORIGIN 11instability of these compounds. After all the individual fftetf)solutions are made, the concentration of each ie calculated inthe following manner: mg of analyte/0.010 1 « mg/1 or ppm ofanalyte in solution. A calculation of what volumee of these
• »approximately 50,000 ppm primary stock eolutions have to becombined and diluted to 50 ml to obtain a 1000 ppm secondaryetock mix in methanol is then calculated:
(ppm of primary etock solution) (X ml) « (1000 ppm) (50 ml)X ml « 50,000/ppm of primary etock.The 1000. ppm.secondary stock mixture ie then eealed in 1 ml
glaee ampules by using a propane torch. Standard etocke -of "theTable 1 compounds prepared and eealed in ampules as describedabove have been successfully used up to 6 months afterpreparation. Each vial is labeled and stored in the freezeruntil it ie needed.
The acrolein, acrylonitrile, and 2-chloroethylvinyletherstandard ie prepared fresh weekly by weighing out 0.01 g± .0001 g, which is about 1 drop of each compound in the same10 ml volumetric flask containing about 9.8 ml methanol toyield a etock solution of approximately 1000 ppm when broughtto volume with methanol. Typical volumes used in standardpreparation are given in Table 5.
A volatile organic internal-surrogate standard etockmixture ie made by weighing out in separate 10 ml volumetricflasks containing 9.8 ml of MeOH (as described above) 0.01 g (±0.0001 gwhich ie 1 drop) of bromochloromethane,d4-l,2-.dichloroethane, 1,4-difluorobenzene, dschlorobenzene,dg-toluene, and 4-bromofluorobenzene (BFB). Thie will yield a
65 AR30I386
Water & Soil for PurgeableOrganics by P&T/GC/MS 1520Initiated Date 9/13/85Revised Date 10/1/36
"i Page 7 of 10»
-i primary stock of approximately 1,000 ppm for each compound. A 0working internal standard mixture is then made by pipeting a
._, calculated volume of the primary internal standard stocks into• 25 ml of methanol which results in a 25 ppm surrogate-internal
standard working mix containing the six compounds. This mix is' then sealed in glass ampules and a fresh vial is opened on a
weekly basis or more frequently as needed. When 10 microliters~] of this working internal standard are spiked into 5 ml of) sample, the resultant spike level will be* 50 ppb for all"l compounds. An alternative source of this spiking solution is
Supelco. (Catalog 14-3376, 4-8835).i After preparation of the standard solutions, the instrument
is calibrated using the internal standard technique. Thecalibration standards are prepared Immediately before use as •
I they are generally not stable for over 1/2 hour in thevolumetric flask with headspace. The volumes used in standard
• preparation are described in Table 5 to prepare the threelevels of standards. It is important that the microliter
i volumes of stock solutions are spiked as far down into thebulbous portion of the flask with a fast, reproducible plungerstroke. After inverting the volumetric flask three or fourtimes, fill a 5 ml syringe with standard and spike with 10microliters of the working internal standard solution. Inject
' the 5 ml standard into the purge vessel and push the starti button to start the purge flow for the 11 minute purge cycle.
1 At this point, the data system must be set-up to acquiredata. This is done using the AC program as described in fullin the 5100 Series Application Software Operators Manual,
, Scanning and Acquisition Section. Under the conditions of thismethod, 1.000 scans of data must be collected. Files are namedin accordance with the guidelines established in Appendix C.
When the purge cycle is complete, the acquisition is set-upon the data system, and the white ready*light is illuminated on
' the GC, the data acquisition can be started by flipping the
•fir, AR30I387
i U j;:'"••'• Water & Soil for PurgeableOrganics by P&T/GC/MS $520;Initiated Date 9/18/85Revieed Date 10/1/E6Page 8 of 10
deeorb ready/desorb preheat switch momentarily to auto andreturn to the hold position. The data system then displaysACQU: If you desire to observe the real time data, type Ewhich gets you to the >, then type MAP/C and display 1000 Scans(01,1000). When 1000 scans of data have been acquired, thefile is complete and can be processed using the AUTOQUANsoftware of the OKA. A full discussion of the AUTOQUAN program
1 and the QUAN programs are found in the 5100 ApplicationsSoftware Operator's Manual, Quantitation Section. Appendix D
-, contains the actual procedure used to calibrate the system.The objective of using these programs ie to create a 3 pointcalibration response liet with a RSD <35% as described in
' Reference 1. :
] C. Sample Preparation:There ie no sample preparation step for the analysis of
water.For eoil analysis, 20 g (± .01 g) ie weighed out into a 40
ml glass teflon eealed screw top vial after which 20.0 ml ofmethanol ie added. The soil-solvent ie then shaken for 2minutes. The eoil ie then allowed to settle and the methanolicextract ie ready to be analyzed as described below.
D. Sample AnalysisFor a water sample, 5 ml of water to be analyzed ie poured
gently into a 5 ml eyringe with the barrel removed. Theplunger ie then put in place and the volume adjusted to5.0 ml. Ten microlitere of working internal standard are thenepiked into the eyringe and the contents of the eyringeinjected through the 3 way valve of the purge and trap into thepurge vessel. The purge flow is started and the data acquiredas described in the Instrumental Calibration Section.
flR30!388
EXHIBIT XIII
STANDARD OPERATING PROCEDUREFOR IL 951 ATOMIC ABSORPTION/
ATOMIC EMISSION SPECTROPHOTOMETER
~~i Routine operation of the IL 951 AA/AE Spectrophotometer:.,.v :..
('-IIgnition and extinguishing of flames should be carried out .
in accordance with the IL 951 operator's manual, table 3.2,3.5. and 3.6 on pp 3-24 through 3-26, and 3-29 through 3-32.Routine absorption operation should be performed according toSection 4, pp 4-1 through 4-52, of the operator's manual.
' Procedures for routine use of atomic emission are found inJ section 5.1 of the IL 951 operator's manual, pp 5-1 through"1 5-5. The procedure for Mercury determination by cold vapor is
found under the Special Techniques section of Atomic Absorptionj Methods Manual, Vol. 1, as is the procedure for Hydride
Generation.
'1.; See equipment information card regarding persons
responsible for these operations.
Materials required to perform these methods include thef IL 951 AA/AE Spectrophotometer, DI water, Baker instra-analyzed
acid, and standards prepared using stock solutions traceable to* ; NBS references or confirmed by either titrimetry or
• gravimetry. Instrumental conditions for each method may be._ found in the IL Atomic Absorption Methods Manual, Vol. 1.tj Required conditions and materials for instrumental operation* are found in the IL 951 operator's manual, sections 1.2 - 1.6
• on pp 1-1 through 1-6.
i Daily usage of the IL 951 is documented on the print out ofthe calibration curve. Other than the calibration curve,
: conditions of daily use are not documented but conditionsfollowed are in accordance with the IL Atomic AbsorptionMethods Manual, Vol. 1.
Calibration:f; f >' { •v r....- s •. '•
The procedure for calibration is found in the IL 951 (!.;.;operator's manual, pp 4-15 through 4-21. Materials requiredinclude prepared standards and blank. Calibration is carriedout each time a method is performed. Correction forinstrumental drift ie described in the IL 951 operator'smanual, pp 4-43 through 4-45. Documentation of eachcalibration is kept in AA standard curve notebook.
Maintenance:
Maintenance logbooks will be kept in accordance withStandard Operating Procedure QA-7 found in the departmentoperations manual. Section six of the IL 951 operator's manualdescribes routine maintenance as follows:
6.1 maintenance schedule, pp 6-1 through 6-3.6.2-6.5 description of routine maintenance, pp 6-3through 6-9.
Documentation for all maintenance ie found in themaintenance record. For non-routine maintenance or equipmentfailures consult section 3 of the IL 951 Instrument ServiceManual or call the current service representative at AlliedAnalytical'e message center (617) 890-4300.
RS/cfs
9/85
No. of SuggestedPlaces past Calibration
Element Decimal BGC Range (mo/1)
Aluminum 2 N 1.000-20^ Antimony (Flame) 2 Y 0.500-10
"1 Antimony (Hydride) 3 N 0.025-.20Arsenic (Hydride) 3 N 0.025-.20Barium 2 N 1.000-10
" i Beryllium 3 Y 0.010-1.0Bismuth (Flame) 1 Y 0.500-10Bismuth (Hydride) 3 N 0.025-.20Cadnium 3 Y 0.100-1.0Calcium 2 N 0.200-3.0Chromium 2 N 0.100-5.0
-, Cobalt 2 Y 0.100-2.5I Copper 2 Y 0.100-5.0
V Iron 2 N 0.100-5.0Lead 2 Y 0.100-5.0
1 Lithium 3 N 0.100-1.5Magnesium 3 N 0.100-2.0Manganese 3 N 0.100-2.5
1 Mercury (Cold vapor) 4 N 0.001-.02Molybdenum 1 N 0.500-10Nickel 2 , Y 0.100-2.5
-i Potassium 3 N ' 0.100-1.5Selenium (Flame) 1 Y 1.000-20
1 Selenium (Hydride) 3 N 0.025-.20Silicon 1 N 1.000-50Silver 3 Y 0.100-2.0
-i 4 Sodium 3 N 0.100-1.5Strontium 2 N 0.100-2
I Thallium 1 Y 0.100-5.0J T i n I N 0.500-20
Titanium 1 N 1.000-20^i Vanadium 1 N 0.500-5.0j Zinc 3 Y 0.100-2.5
CALIBRATIOI
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I
Dn 741C
8520
963•
OKI(R
• CALIBRATION PROCEDURE
NOTES: 1) This procedure is applicable for both AA and AE determinations.2) The following procedure is for simultaneous calibration of Channel A and B. If one selects
*1 single channel operation, Questions from only that 1 channel will appear.a. Perform steps c (page 4-5) through step g
(page 4-10), and select AA operation forboth channels, CONC mode, normal twochannel operation and display both chan-nels, i
'} b. When the CRT displays "Statistics" (page4-10) enter number of runs. Enter the num-ber of desired replicates and type of statis- ' ' •tics information to be displayed, i.e., mean,SO, & RSD or mean only.
c. Press STD/ • The CRT displays:
3Cattbrote1 ft2 B3 Both
1 A - A channel only.2 B - 6 channel only.3 Both - A and B channels.
4-15
. AR30I392
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I
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741C
8520
963•
)
d. Select single or dual channel opera-tion by Dressing tha desired number,and or ess ENTER, or simply pressENTER for Calibration #3 both chan-nels.
e. Aspirate a blank solution.• The CRT displays:
f. Press READ.
g. After tha desired number of replicatereadings, press READ to stop.
NOTE: This step automatically zeroes the absorbance reading of the blank, (i.e., 0.279 becomes 0.000).
4-16
AR30I393
1
CALIBRATION
DAOBn
•<C MM.
"9 '"
hn 741C
e520
963•
h. Press ENTER. • The measured absorbance for the blanksolution is set to zero and entered into themicrocomputer.
• The CRT displays:
Enter flbs•i Instrumen3 Clear old data
1 Instrument — this selection is used whenaspirating standardsolutions.
2 Keyboard — used to manually enterconcentrations and absorb-ances.
3 Clear Old Data - used to clear the CRT sonew CONC and absorb-ance values can be entered.
NOTE: After step h., operator selects one of the entries. If not, pressing ENTE R will default to "2 key-board."
AR30I39U
I IAI 1 1 1 1QBOO 0Q i _ O % » « CM**
.1 X
74XC
85X0
96X•
i. Unless manual entry of cal curve is desired, • The CRT displays the concentrationpress 1 and ENTER. and absorbances.
• After 1 or 2 is selected, the CRT displays.for example:
1^^________^__
Enter Std 1 Cone for Cu
Std Cu Abs Pb Abs0 0.000 0.000 0.000 0.0001
h — — —— — <
i
/
NOTES: 1) If manual entry is desired, see page 4-25.2) If entry "3" is selected, any calibration curves not stored in one of the storage registers will
be removed from the microcomputer. The CRT will display the following message and] the operator must now enter 1 or 2:
ClearedEnter abs. 31 Instrument2 Keyboard3 Clear Old Data
j. Enter the concentration of standard 1using the number keys, and press ENTER.
k. Enter the concentrations of tha remainingstandards of Channel A.
4-18
77
CALIBRATION
If
DAIOBin D33 Gl/p f»* _P****_
DO 1X1
741C
8520
963•
NOTES: 1) Standard No. 1 formats the decimal point (e.g., 0010,010.0,10.00) for the subsequentstandards entered.
2) Enter the concentration for all of the standards to be used in the calibration curve (up tofive standards per curve per channel).
I. After the desired number of standard con-centrations are entered for Channel A (upto five), press STD.
NOTE: If five standards have been entered for the A channel, omit step I. The standard entry will auto-matically switch to the B channel after the fifth concentration is entered.
m. Enter the B channel concentrations byrepeating steps h through k.
NOTE: If five standards have been entered, omit step n below. The microcomputer will automaticallyadvance through step n to the CRT display: ''Analyze STD 1."
n. Press STD. " The CRT displays:
o. Aspirate the standard..p. Press READ. 02.00 0.000 1.000 0.000q. After the desired number of replicate
readings are taken, press READ to stop.
Cu-D Cd
Analyze Std 1
Std Cu Abs Cd Abs0 00.00 0.000 0.000 0.00001.00 0.000 0.500 0.000
r. Press ENTER. • The CRT displays:
Cu-D CdAbs 0.160 0.215Mean 0.158 0.220Analyze Std 1Std Cu Abs Cd Abs0 00.00 0.000 00.00 0.0001 01.00 0.000 0.500 0.0002 02.00 0.000 1.000 0.000
1.19
Vfc OR30I396
mt «>c »~~ ».«..GAUD DQeCD Q
»a *»«EJJ rs. Repeat steps m and n for the remaining • The mean absorbance is entered into
standards. the microcomputer. ' -• The CRT displays:
1
^ i -Cu
_-M_M-_-v
Cd
Analyze Std 2
Std012
^ ——
Cu00.0001.0002.00
Abs0.0000.1530.000
Cd00.000.5001.000
Abs0.0000.2200.000, V
•
•
i
With the graphics option, when the cali-bration curve is completed, the CRT willdisplay the absorbance versus concentra- xtion plot.The absorbances of the calibration stand-ards will be displayed as O and the calcu-lated curve fit as a dotted line — accuracyof the curve fit can be evaluated by theproximity of the dotted line to the D.
$4
4-20
AR30I397
n
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741C
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963•
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THIS COMPLETES THE CALIBRATION PROCEDURE.
• After the desired number of standards areentered, the microcomputer will calculatethe curve, which will be displayed on theCRT (graphics option).
• The optional printer will reproduce:
Cu-D STD CONC MEAN1 01.00 0.1652 02.00 0.320
APP CONCSTD 1 01.00STD 2 02.00Cd STD CONC MEAN
1 0.500 0.2152 1.000 0.400
APP CONCSTD 1 0.500STD 2 1.000
Cu Cu-DMODE: AA. DB CONCSTATS #10I NT: AUTO T-01.0DL-0
• The CRT will display all of the data.
AR30I398
EXHIBIT XIV
ATTACHMENT 3
Method 200.7 CLP-H*INDUCTIVELY COUPLED PLASMA-ATOMIC EMISSION SPECTROMZTRIC METHOD
FOR TRACE ELEMENT ANALYSIS 0? WATER AND WASTES
1. Scooe and Application
1.1 Dissolved element, ara determined la flitare, and acidified samples.Appropriate steps must be taken in all analyses to aaaure thatpotential, interferences ara taken into account. Thia la especiallytrue when dissolved aollda .exceed 1300 mg/L. (See 3.)
•
1.2 Total elements are determined after appropriate digestion proceduresare performed. Since digestion, techniques increase the dissolved •solids content of the saaples, appropriate atepa must be taken tocorrect for potential interference effects. (See 5.)
1.3' Table 1 lists elements along with recommended wavelengths'and typicalestimated instrumental detection limits using .conventional pneumaticnebullzation. Actual working detected limits are sample dependentand as the sample matrix varies, these concentrations may also vary.In time, other elements may be added as more information becomesavailable and as required.
1.4 Because of the differences between various makes and models ofsatisfactory instruments, no detailed instrumental operatinginstructions can be provided. Instead, the analyst is referredto the instructions provided by the manufacturer of the particularinstrument.
2. Summary of Method• •
2.1 The method describes a technique for the simultaneous or sequentialmultielement determination of trace elements in solution. The basisof the method is the measurement of atomic emlsaion by an opticalspectroscopic technique. Samples are nebulized and the aerosolthat is produced is transported to the plasma torch where excitationoccurs. Characteristic atomic-line emission spectra are produced bya radio-frequency inductively coupled plasma (ICP). The spectra aredispersed by a grating spectrometer and the intensities of the lineare monitored by photomultiplier tubes. The photocurrents froa thephotomultipller tubes are.processed and controlled by a computersystem. A background correction technique is required to compensatefor variable background contribution to the determination of traceelements. Background must be measured adjacent to analyte lines on
*CL?-M Modified for the Contract Laboratory Program
.*i AR30I399
Method 200.7 CLP-M (cont.)'.- •- • " : > ? ' f r • . ' - r;'.v *
'samples during analysis. The position selected for the backgroundintensity measurement, on either or both sides of the analyticalline, will be determined by the complexity of the spectrum adjacentto the analyte line. The position used'must be free of spectral.interference and reflect the same change in background intensity asoccurs at the analyte wavelength measured. Background correction isnot required in cases of line broadening where a background correc-tion measurement would actually degrade the analytical result. Thepossibility of additional interferences named in S.I (and tests fortheir presence as described in 5.2) should also be recognized andappropriate corrections cade.
3. Definitions
3.1 Dissolved — Those elements which will pass through a 0*45 urnmembrane filter*
3.2. Suspended — Those elements which are retained by a 0.45 urnmembrane filter.
3'3 Tot-1 M The concentration determined, on an unfiltered cample *following vigorous digestion.
3.4 Instrumental detection limits — See Exhibit E, pages 2-4.'
3.5 Sensitivity — The slope of the analytical curve, i.e. functionalrelationship between emission intensity and concentration.
3.6 Instrument cheek standard — A multielement standard of knownconcentrations -prepared by the analyst to monitor and verifyinstrument performance on a daily basis. (See 7.6.1.)
- . . . •3.7 Interference cheek sample -— A solution containing both interfering
and analyte elements of known concentration that can be used*toverify background and interelement correction factors. (See 7.6.2.)
3.8 Quality control sample — A solution obtained from an outside sourcehaving known concentration values to be used to verify the calibra-tion standards. (See 7.6.3.)
•
3.9 Calibration standards — A series of known standard solutions usedby the analyst for calibration of the instrument (i.e., preparationof the'analytical curve). (See 7.4.)
3.10 Linear dynamic range-— The concentration range over which theanalytical curve remains linear as determined in Exhibit E.
3.11 Reagent blank — A volume of deionized, distilled water containingthe same acid matrix as the calibration standards carried throughthe entire analytical scheme. '(See 7.5.2.)
AR30UOO
Method 200.7 CLP-M (cone.)
3.12 Calibration blank — A volume of deionized, distilled water acidifl'with HN03 and HCi. (See 7.5.1.)
3.13 Method of standard addition — The standard addition techniqueinvolves the use of the unknown and the unknown plus-a-knovn amountof standard by adding known amounts of standard to one or morealiquots of the processed sample solution.
4.
4.1 The toxlcity or careiaogenicity of each reagent used in this methodhas not been precisely defined; however, each chemical compoundshould be treated as a potential health hazard. The laboratoryla responsible for maintaining a current awareness file of OSHAregulations regarding the safe handling of tha chemicals specifiedin this method. A reference file of material handling data sheetsshould also be made available to all personnel involved in thechemical analysis. Additional references to laboratory safety areavailable and have been identified (11.7, 11.3 and 11.9) for theinformation of the analyst. ,'
* • *
3." Interferences-M_-_-MMM^HA^MM-M_MM_l . *
3.1 Several types of interference effects may contribute to in-accuracies in the determination of trace elements. They can besummarized as follows:
5.1.1 Soeetral interferences can be categorized aa 1) overlap of""a spectral line froa another element; 2) unresolved overlapof molecular band spectra; 3) background contribution fromcontinuous or recombination -phenomena; and 4) backgroundcontribution from stray light froa the line emission of highconcentration elements. The first of these effects can becompensated by utilizing a computer correction of the rawdata, requiring the monitoring and measurement of the inter-fering element. The second effect may require selection ofan alternate wavelength. The third and fourth effects canusually be compensated by a background correction adjacentto the analyte line. In addition, users of simultaneousmulti-element Instrumentation must assume the responsibilityof verifying the absence of spectral Interference from anelement that could occur in a sample but for which there isno channel in the instrument array. Listed in Table 2 aresome interference effects for the recommended wavelengthsgiven in Table 1. The data in Table 2 are intended for useonly as a rudimentary guide for' the indication of potentialapectral interferences. For this purpose,, linear relations
• between concentration and intensity for the analytes* and theInterferents can be assumed. The Interference information,which was collected at the Ames Laboratory1, is expressed -"
.
1Anes Laboratory , US-OS, Iowa Stace University, Ames Iowa 50011
33-' HR30H.OI
Method 200.7 CLP-M (cont.)
analyte concentration equivalents (i.e. false analyte concen-trations) arising from 100 mg/L of the interferent element.The suggested use of this information is'as follows: Assumethat arsenic (at 193.696 nm) is to be determined in a samplecontaining approximately 10 ag/L of of aluminum. Accordingto Table 2, 100 mg/L of aluminum would yield a false signalfor arsenic equivalent to approximately 1.3 mg/L. Therefore,10 mg/L of aluminum would result in a false signal for arsenicequivalent to approximately 0.13 ag/L. The reader is cautionethat other analytical-systems may exhibit somewhat differentlevels of interference than those shown in Table 2, and thatthe interference effects must be*evaluated for each individualsystem. Only those interferents listed were investigated andthe blank spaces in Table 2 indicate that measurable inter-ferences were not observed from the interferent concentrationslisted in Table 3* Generally, interferences were discernibleif they produced peaks or background shifts corresponding ca2-5Z of the peaks generated by the analyte concentrations alsolisted in Table 3. S
At present, Information on the listed silver and potassiumwavelengths are not available but.it has been reported "thatsecond order energy from the magnesium 383.231 cm wavelengthinterferes with the listed potassium line at 766.491 cm.
•
5.1.2 Physical interferences are generally considered to be effectsassociated with the sample nebuliration and transport.proc-esses. Such properties as change in viscosity and surfacetension can cause significant inaccuracies especially insaaples which may contain high dissolved solids and/or acidconcentrations* The use of a peristaltic pump may lessenthese interferences. If these types of interferences areoperative, they oust be reduced by dilution of the sample.and/, or utilization of standard addition techniques. Anotherproblem which can occur from high dissolved solids is saltbuildup at the tip of the nebulizer. This affects aerosolflow rate causing instrumental drift. Vetting the argonprior to nebullzatlon, the use of a tip washer, or sampledilution have been used to control this problem. Also, it -has been reported that better control of the argon flow rateimproves instrument performance. This is accomplished withthe use of eass flow controllers. .•
5.1.3 Chemical Interferences are characterized by molecular com-pound formation, ionization effects and solute vaporizationeffects. Normally these effects are not pronounced with theICP technique, however, if observed they can be minimized bycareful selection of operating conditions (that Is, incidentpower, observation position, and ao forth), by buffering ofthe.sample, by matrix matching, and by atandard additionprocedures. , These types of interferences can be highlydependent on matrix type and the specific analyte element.
/1R30U02
Method 200.7 CLP-M (cone.)
5.2 ?or each group of samples of a similar matrix type and concentration(i.e., low, medium) for each Case of samples, or for each 20 lamplesreceived, whichever la more frequent, the following tests must beperformed prior to reporting concentration data for analyte element
5.2.1 Serial dilution — If the analyte concentration is suffi-ciently high (minimally a factor of 10 above the instrumentdetection limit after dilution), an analysia of a 1:4 dilutionmust agree within 10 percent of tha original determination.Serial dilution results must be reported on QC Report Form EC.Samples Identified as field Blanks cannot be used for serialdilution analysis*
If tha dilution analysis is not within 102, a chemical orphysical Interference effect should ba suspected, and thedata must be flsgged with an *!*•
6* Apparatus
6.1 Inductively Coupled Plasma-Atomic Emission Spectrometer.
6.1*1 Computer controlled atomic emission spectrometer with back-ground correction. ••
6*1*2 Radiofrequeney generator.• *
6.1.3 Argon gas supply, welding grade or better.
6.2 Operating conditions — Because of the differences between variousmakes and models of satisfactory instruments, no detailed operatinginstructions can be provided* Instead, .the analyst should follow theinstructions provided by tha manufacturer of the particular instrument.Sensitivity, instrumental detection limit, precision, linear dynamicrange, and interference effects must ba investigated and establishedfor each individual analyta line on that particular instrument. Allmeasurements must be within the instrument linear range where correc-tion factors are valid. Ift is the responsibility of the analyst toverify that tha instrument configuration and operating conditionsused satisfy the analytical requirements and to maintain quality con-trol data confirming instrument performance and analytical results.
7. Reagents and1 standards«* ••_• •M_MM _iM MHMM_« MM_i_M M •
t
7.1 Adda used in the preparation of standards and for sample processingmust be ultra-high purity grade or equivalent. Redistilled acidsare acceptable.
7.1.1 Acetic acid, cone, (sp gr 1.06).•
7.1.2 Hydrochloric acid, cone, (sp gr 1.19).
7.1.3 Hydrochloric acid. (1+1): Add 500 mL cone. HC1 (sp gr lto 400 mL deionized, distilled water and dilute to 1
dl. AR30U03
Method 200.7 CLP-M (cone.)5' .t;
7.1.4 Nitric acid, cone, (sp gr 1.41).
7.1.5 Nitric acid, (1+1): Add 500 mL cone. HNOj Cap gr'1.41) to400 mL deionized, distilled water and dilute to 1 liter.
7.2 Deionized. distilled water: Prepare by pasaing distilled waterthrough a mixed bed of cation and anion exchange resins. Usedeionized, distilled water for the preparation of all reagents,calibration standards and as dilution water* The purity of thiswater Bust be equivalent to ASTK Type XI reagent water of Specifi-cation 0 1193 (14.6).
' . ' . - • . . . . - V7.3 Standard stock solutions-pay be purchased or prepared from ultra-
high purity grade chemicals or Betels. All salts must be dried for1 h at 105* unless- otherwise specified.
• (
(CAUTION: Many metal salts are extremely toxic and aay be fatal ifswallowed. Wash hands thoroughly after handling.) Typical'stocksolution preparation procedures follow:
* • * •
7.3*1 Aluminum solution, stock, 1 aL • 100 ug Al: Dissolved 0.100g of aluminum metal in an acid mixture of 4 mL of (1+1) EC1and 1 mL of cone* HNOj in a beaker* Warm gently to effect •
' • solution* When solution is complete, transfer quantitativelyto a liter flask, add an additional 10 aL of (1+1) HCi anddilute to 1000 aL with deionized,'distilled water.
7.3.2 Antimony solution stock. 1 mL « 100 ug Sb: Dissolve 0.2669g K(SbO)C4tt40e in deionized distilled water, add 10 aL (1+1)HCI and dilute to 1000 mL with deionized, distilled water.
•• - . . . . , B
7.3.3 Arsenic solution, stock. 1 __. • 100 ug As: Dissolve 0.1320•g of AJ2°3 in 100 eL .of deionized, distilled water containing0.4 g NaOH. Acidify the solution with 2 mL cone. BNOj anddilute to 1,000 mL with deionized, distilled water.
7*3*4 Barium solution, stock, 1 aL • 100 ug Ba: Dissolve 0.1516 g' . BaCl2 (dried at 250'C for 2 hrs)-ic 10 mL deionized> distilled
water with 1 aL (1+1) HCI. Add 10.0 aL (1+1) HCI and diluteto 1,000 eL with deionized, distilled water.
7.3.5 Beryllium solution, stock, I aL • 100 ug Be: Do not dry*Dissolve 1.966 g BeSO^iUO, in deionized, distilled water,add 10.0 mL cone. HNOj and dilute to 1,000 aL with deionized,distilled water.
. * *
7.3.6 Boron solution, stock, 1 aL • 100 ug B: Do not dry. Dissolve0.5716 g anhydrous 1131503 in deionized, distilled water anddilute to 1,000 mL. Use a reagent meeting ACS specifications,keep the bottle tightly stoppered and store in a desiccatorto prevent the entrance of atmospheric moisture.
80 «R30|liOlf
Method 200.7 CLP-M (cont.)
7.3.7 Cadmium solution, stock., 1 mL • 100 ug Cd: Dissolve 0.1g CdO in a minimum amount of (1+1) -$03. Heat to Srate of dissolution. Add 10.0 mL cone. HNOj and dilute to1,000 mL with deionized,' distilled water.
7.3.3 Calelua solution, stock, 1 mL • 100 ug Ca: Suspend 0.2493 gCaO>3 dried at IBO'C for 1 h before weighing in deionlzed,distilled water and dissolve cautiously with a minimum amountof (1+1) HH03* Add 10.0 aL cone. -£03 and dilute to 1,000 aLwith deionized, distilled water*
7*3.9 Chromium solution, stock, 1 aL • 100 ug Cr: Dissolve 0.1923g of Cr03 in deionized, distilled water* When solution iscomplete acidify with 10 aL cone* HN03 and dilute to 1,000 mLwith deionized, distilled vatar.
.'7.3.10 Cobalt solution stock, 1 aL • 10 ug Cos Dissolve 0.1000 g
of cobalt metal in a minimum amount of (1+1) HNta* Add 10.0ml (1+1) HCI and dilute to 1,000 aL with deionized, diatilledwater.
.7.3.11 Copper solution, stock." 1 aL • 100 ug Cu: Dissolve 0.1252
g CuO In a minimum amount of (1+1) H2K)3* Add 10.0 aL cone.HK03 and dilute to 1,000 mL with deionized, distilled war--
7.3*12 Iron solution, stock, 1 aL • 100 ug ?e: Dissolve 07e203 in a warm mixture of 20 aL (1+1) HCI and 2 mL of cone.HM03* Cool, add an additional 5 aL of cone. HKOj and diluteto 1,000 aL with deionized, distilled water.
7.3.13 Lead solution, stock, 1 mL • 100 ug Pb: Dissolve 0.1599 gPb(N03)2 la a minimum amount of (1+1) HN03* Add 10.0 mL ofcone* HN03 and dilute to 1,000 mL with deionized, distilledwater*
7.3*14 Magnesium solution, stock, 1 aL * 1.00 ug Mg: Dissolve 0.1628f MgO in a minimum amount of (1+1) HH03. Add 10.0 aL cone.HN03 and dilute to 1,000 mL with deionized, distilled water.
7*3*15 Manganese solution, stock. 1 mL » 100 ug Mn: Dissolve O.lOOCg of manganese metal in the acid mixture, 10 mL cone. HCIand 1 mL cone. HN03, and dilute to 1,000 mL with deionizad,distilled water.
7.3.16 Molybdenum solution, stock, 1 mL * 100 ug Mo: Dissolve0.2043 g (NHt)2Mo04 in deionized, distilled water and diluteto 1,000 mL.
8V 1R30II.05
Method 200.7 CLP-M (cent.)
7.3.17 Nickel solution, stock. 1 mL • 100 ug Hi: Dissolve 0.1000 gof nickel octal in 10 aL hot cone. HNOj, cool and dilute to1,000 aL with deionized, distilled water.
7.3.1. Potassium solution, stock, 1 eL • 100 ug 1: Dissolve 0.1907g KC1, dried at 110*C, in deionized, distilled water. Diluteto 1,000 aL.
7.3.19 Selenium solution, stock, I aL « 100 ug Se: Do net dry.Dissolve 0*1727 g a SeOs (aetual assay 94.6X) in deionized,distilled water and dilute to 1,000 aL*
7.3.20 Silica solution, stock, 1 aL •» 100 ug S102: Do not dry.Dissolve 0.4730 g I S EUO in deionized, distilled water.Add 10.0 aL cone* HN03 and dilute to 1,000 eL with deionized,distilled water*
* • • •
7.3.21 Silver solution, stock. 1 ml - 100 ug Ag: Dissolve 0.1575 gAgN03 in .100 mL of deionized, distilled water and 10 eL cone.HN03. Dilute to 1,000 aL with deionized, distilled-water.
7.3.22 Sodium solution, stock. 1 aL • 100 ug Ra: Dissolve 0.2542 gNaCl in deionized, distilled water. Add 10.0 aL cone. ENC>3and dilute to 1,000 mL .with deionized, distilled water.
i _ . . *
7.3*23 Thallium solution, stock, 1 mL • 100 ug Tl: Dissolve 0.1303g T1N03 in deionized, distilled water. Add 10.0 mL cone.HNOj and dilute to 1,000 eL with deionized, distilled water.
7.3.24 Vanadium solution, stock, 1 aL • 100 ug V: Dissolve 0*2297N-4V03 in a Binleum amount of cone. HN03* Heat to iner'easerate of dissolution. Add 10.0 aL cone. HNOj and dilute to1,000 aL with deionized, distilled water.
7.3*25 Zinc solution, stock, 1 mL » 100 ug Zn: Dissolve 0.1245 gZnO in a minimum amount of dilute £2103. Add 10.0 eL cone.HN03 and dilute to 1,000 aL with deionized, distilled water*
.; ' -V- i- ' .
7.4 Mixed calibration standard solutions --• Prepare mixed ealibrationstandard solutions by combining appropriate volumes of the stocksolutions in volumetric flasks. (See 7.4.1 thru 7.4.5.) Add 2eL of (1+1) MN03 and 1U aL of (1+1) HCI and dilute to 100 aL withdeionized, distilled water. (See Notes 1 and 6.) Prior to pre-paring the mixed standards, each stock aolution should be analyzedseparately to determine possible spectral interference or thepresence of impurities. Care should be taken when preparing themixed standards that the elements are compatible a'nd stable.Transfer the mixed standard solutions to a FEF fluorocarbon orunused polyethylene bottle for storage. Fresh mixed standardsshould be prepared as needed with the realization that concentration
AR30U06
Method 20U.7 CLP-M (cont.)
can change on aging. Calibration standards oust be initiallyverified using a quality eontrol sample and monitored weekly foV—^atability (see 7.6.3). Although not specifically required, sometypical calibration standard combinations follow when uaing thosespecific wavelengths listed in Table 1.
7.4.1 Mixed standard solution I —'Manganese, beryllium, cadmium,lead, and zinc*
7*4,2 Mixed standard solution II — Barium, copper, iron, vanadiumand cobalt*
*9
7.4.3 Mixed atandard solution III — Molybdenum, silica,arsenic, and eelenium.
.7.4.4 Mixed atandard solution IV — Calcium, sodium, potassium,
aluminum, chromium and nickel./*
7*4*5 Mixed standard solution7 — Antimony, boron, magnesium,silver, and thallium.
HOTS 1: If tha addition of silver to the recommendedacid combination results in an initial precipitation
• add 15 aL of deionized distilled water and warm thflask until tha solution clears. .Cool and dilutev j100 mL with deioniaed, distilled water. For this ^acid combination tha silver concentration should belimited to 2 mg/L* Silver under these conditions, isstable in a tap water matrix for 30 days. Higherconcentrations of silver require additional HCI.
•
7.5 Two types of blanks are required for the analysis. • The calibrationblank (3.13) is used in establishing the analytical curve while thereagent blank (preparation blank, 3*12) is .used to correct forpossible contamination resulting froa varying amounts of the acidsused in the sample processing.
• • •7.5*1 The calibration blank is prepared by diluting 2 mL of (1+1)
HN-3 and 10 mL of (1+1) HCI to 100 aL with deionized,distilled water* (See Note 6.) Prepere a sufficientquantity to ba used to flush the systea -between standardsand samples.
7.5.2 The reagent blank (or preparation blank - See Exhibit E)must contain all the reagents end la the same volumes asused in the processing of the samples. The-reagent blankmust be carried through the complete procedure and containthe same acid concentration in the final solution as cb-sample solution used for analysis.
99 ' AR30U07
Method 200.7 CLP-M (cont.) -
;-' '' - , 9; ' . • - . - •
7.6 la addition the calibration standards, an instrument cheek standard(3.6), an interferenee check sample (3.7) and a quality controlsample (3..) are also required for the analyses.
' *
7.6.1 The Instrument check standard for continuing calibrationverifIcatlon is prepared by the analyst by combining com-patible elements at a concentration equivalent to the mid-point of their respective calibration curves. (See 10.1.3.)
7.6*2 The interference cheek sample is prepared by the analyse,or obtained from EPA if available (Exhibit E).
* . ' •
7.6.3 The quality control sample for tha initial calibrationverification should be prepared in the same acid matrixas tha calibration standards and in accordance with theinstructions provided by the supplier. EPA will eithersupply a quality control sample or information where oneof equal quality ean be procured* (See 10.1.1.')- , / *
8. Procedure•8*1 Set up instrument with proper operating parameters established in
Section 6.2. The instrument Bust be allowed to become thermallystable before beginning. This usually requires ac least 30 oin.of operation prior Co calibration.
8.2 Initiate appropriate operating configuration of computer.
ts.3 Profile and calibrate instrument according to instrument manufac-turer's recommended procedures, using mixed calibration standardsolutions such as chose described in Section 7*4. Flush the systeawith the calibration blank (7.5.1) between each standard. (SeeNOTE 7.) (Use the average intensity of multiple exposures for bothstandardization and sample analysis to reduce random error.)
NOTE 7: Forgboron concentrations greater than 500 ug/L extendedflush times of 1 to 2 minutes may be required.
t 8.4 Begin the sample run flushing the system with the calibration blanksolution (7.5.1) between each sample. (See NOTE 7.) Analyze the .~instrument check standard (7.6.1) and the'calibration blank (7.5.1)each 10 saaples*
9* Calculation
9.1 Reagent blanks (preparation blanks) should be treated .as specifiedin Exhibit E. '
9.2 If dilutions were performed, the appropriate faetor must be appliedto sample values.
9.3 Data must be reported in ug/L.
. • 0 AR30U08
•Method 200.7 CLP-M (cone.)
10. Quality Control (Instrumental)
10.1 -Cheek the instrument standardization by analyzing appropriatequality eontrol cheek standards as follows:
10.1.1 A quality control sample (7.6.3) must be used dally for theinitial calibration verification (5«e Exhibit E). A freshdilution of this sample shall be analyzed every week there-after to monitor their stability. If the results are notwithin +102 of the true value listed for the control sample,prepare""a new calibration standard and recalibrate the •instrument. If this does not correct the problea, prepare anew stock standard and a new calibration standard and repeattha calibration*
10.1.2 Analyze tha calibration blank (7.5.1) at a frequency of 102.. ' Tha resale should ba within +; contract required detection
levels (Exhibit C). If tha result is not within tha controllevel, terminate tha analysis, correct tha problea andrecalibrate tha instrument (See Exhibit 2). '*
10.1.3 For continuing calibration verification, analyze aa appro--priate instrument cheek standard (7.6.1) containing thaelements of interest ae a frequency of 102. This checkstandard is used to determine inst rumen? drift. If agree-ment is not within +,102 of the expected values, the analysik _/is out of conrrol. ""the analysis oust be terminated, theproblea corrected, tha instrument recalibrated, and thepreceding 10 sauples reanalyzed (See Exhibit Z).
* •
10.1.4 To verify int.relement and background eorreetioa factorsanalyze the 1C? Interference check sample (7.6.2) at thebeginning, and. end of the sample run or a almlmua of twiceper 8 hour work shift whichever is more frequent. The chacksample must b« analyzed initially at least 5 times repeti-tively eo establish % mean value and standard deviation.Results must fall within tha established eontrol limits. Ifnot, terminate the analysis, correct the problem, recalibratethe instrument, and reanalyze the samples (See Exhibit E).
11. Bibliography
• 1. Wlnge, R. X., V.J. Pet*r-f,a, and V.A. Fassel, "Inductively Coup?.edPlasma-Atomic Emission Sptctroscopy Prominent Lines," EPA-600/--79-017.
2. Winefordner, J.D., "Trace Analysis: Spectroscopic Methods fjr Elements,"Chemical Analysis, Vol. 46, pp. 41-'42.
AR30U09
' Method 200.7 CLP-M (cont.)
3* Handbook for Analytical Quality Control in Water and WastewaterLaboratories, EPA-600/4-79-019.
v_y •4. Garbarino, J.R. and Taylor, H.E., "An Inductively-Coupled Plasma
Atonic Emission Speetrometric Method for Routine Water QualityTesting,* Applied Spectres copy 3_3, No. 3(1979).
5. Methods for Chemical Analysis of Water and Wastes," EPA-600/4-79-020.
6* Annual Book of ASTM Standards, Pare 31*• ' . •
7. .'Carcinogens - Working With Carcinogens," Department'of Health,Education, and Welfare, Public Health Service, Cancer for DiseaseControl, National Institute for Occupational Safety and Health,Publication Ho. 77-206, Aug. 1977.
8. "OSEA Safety and Health Standards, General Industry," (29 CFR 1910),Occupational Safety and Health Administration, OSHA 2206, (Revised,January 1976)* /'
9* "Safety in Academic Chemistry Laboratories, American Chemical SocietyPublications, Cooaaittee on Chemical Safety, 3rd Edition, 1979.*
10. "Inductively Coupled .Plasma-Atomic Emission Speetrometric Method ofTrace Elements Analysis of Water and Waste", Method 200.7 modifiedby CLP Inorganic Data/Protocol Review Commie tee; original method by .Theodore D. Martin, EMSL/Clncinnaei.
9£.
Method 200.7 CLP-M (cone.)
TABLE 1 - RECOMMENDED WAVELENGTHS<2> AND ESTIMATEDINSTRUMENTAL DETECTION LIMITS
Estimated DetectionElement ' • Wavelength, nmCD Limit, ug/L<2)
Aluminum 308.213 43Antimony 206.833 • 32Arsenic 193.696 . 53Barium 435.403 2Beryllium 313.042 0.3
Boron 249.773 5Cadmium * 226.502 ' 4Calcium 317.933 10Chromium 267*716 7 /•Cobalt 228.616 7
•' .Coppei 324.734 6Iron 259.940 . • 7Lead 220.353 42Magnesium 279.079 30Manganese 257.610 • 2
Molybdenum 202.030 3Nickel 231.604 13Potassium 766.491 see"' .Sttlsniua 196.026 ' 75Silica (S102) 238.158 .53Silver 323.063 7Sodi'rr 533.995 29Thalilom 190.364 40Vanadium 292.402 3Zinc 213.856 2.
The wavelengths listed are recommended because of their sensitivity andoverall acceptance. Other wavelength may be substituted if they canprovide tha needed sensitivity and are treated with the same correctivetech'J.ques for spectral interference. (See 5.1.1). The use of alternate
must be 'reported (in na) wir'a the sample data.
(*) The estimated instrumental detection ."imits as shown are taken from"Inductively Coupled Plasma-Atomic Emission Spectroscopy-Promlnent Lines,"EPA-600/4-79-017. They are given as a guide for an instrumental limit.The actual method detection limits are sample dependent and may varythe sample matrix varies*
(3) Highly dependent on operating conditions and plasma position.
fiS AR30HH
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• •
' •*• . ' •
Method 200.7 CLP-H (cont)
TABLE 3. INTSajEXSHT AND AHAL1TE ELEMENTAL CONCENTRATIONS USEDTOR IMTEagERENCS MEASUREMENTS IH TABLS 2 (EXHIBIT D)
Analytes (mg/L) Interferents (mg/L)
Al 10 Al 1000As 10 Ca 1000B 10 Cr 200Ba 1 Ca 200Ba 1 ?• 1000Ca 1 Mg 1000Cd 10 Ma 200Co 1 Hi 200Cr 1 Ti 200"Cu 1 7 200Pe 1 .Mg 1 .Ma 1Mo 10Ha 10Hi 10Pb 10*Sb ' 10Se 10Si 1Tl * ' 107 1Zn 10
EXHIBIT XV
QUALITY ASSURANCE OPERATIONS MANUAL
Standard Operating Procedure.s QA-14
Title? Sample Log-in, Storage, and Disposal (Food Chemistryand Environmental)
Scope; This SOP will cover procedures used to log, store anddispose of samples received for analysis by the Food Chemistryand Environmental Chemistry Departments.
Purpose i one of the major objectives of our Quality AssuranceProgram is to ensure the accountability of the results that wereport. This means that we take every precaution to ensurethat the results reported do, in fact, refer to the sample wereceived, i.e. to avoid sample mix-up. It is important also toensure that the sample does not deteriorate, or otherwisechange its physical or chemical properties while awaitinganalysis or until it is discarded. The following proceduresare designed to accomplish these objectives.
Procedures;
I. Regular Samples
1. All samples which are to be analyzed by the FoodChemistry or Instrumentation/Environmental ChemistryDepartments shall be delivered to the Sample AdministrationGroup immediately upon receipt.
2. All client correspondence relating to samples(purchase orders, letters, etc.) shall also be transferred tothe Sample Administration Group.
3. Personnel of the Sample Administration Group shall logthe samples into the computer, as soon after receipt aspractical, but in no case later than 24 hours after receipt. ._The only exception to this will be samples received on ,Saturdays or Sundays, which will be refrigerated until log-inon Monday.
*
4. Samples requiring the addition of preservatives willbe logged-in immediately and delivered to tha Group Leader ofthe group performing the analyses, for addition ofpreservatives.
5. During tha process of computer log-in, a label shallbe printed with the pertinent information, which shall baimmediately attached to the sample container. The labelinformation shall include, but not be limited to:
» .
a. Computer generated LLI sample number.
b. Client name, account number, and sample designation.
c. Employee number of person entering sample.
d. Computer designated storage area. This will depend onsize of sample, need for special requirements forstorage (refrigeration, etc.) and nature of sample(e.g. locked storage for forensic samples).
e. List of analyses requested, by analytical methodnumber.
6. A designated storage time for the sample will beestablished by the computer according to programmedinstructions based on the type of sample and its nature(tendency to spoil or otherwise deteriorate with time). Thecomputer designated storage time may be overridden by theperson entering the sample, in accordance with clientinstructions or other considerations.
7. Immediately after sample entry, the samples will betransferred to the computer designated storage area to awaitanalysis.
8. Each day, the Computer Services Department willfurnish to all laboratory Departments a computer printoutlisting the samples awaiting analyses, the/ma lye ee to be run,and the location of the samples. Client name and the status ofsamples (incomplete, completed but not verified, or verified)is also designated in the printout.
9. Each day the Sample Administration Group will generatea "discard" printout which lists samples which should bediscarded in accordance with the designated storage timeallotment.
10. Each day the Sample Administration Group will deliverto the Group Leaders concerned all client correspondencerelating to samples. The client correspondence will beinitialed by the Group Leaders and returned to the SampleAdministration Group for filing. Filing shall bealphabetically, by client name.
II. Forensic Samples
Special sample handling procedures will be followed for"forensic samples." Forensic samples are those which are, ormay be, involved in a forensic dispute, i.e. a legal dispute, a•government hearing, or, in general, a confrontation between twoopposing factions. Such samples must be handled with a strict"chain-of-custody" procedure. A sample may be said to be "incustody" of an individual if it is in his/her possession,within his/her line of eight, or locked in a storage area withlimited access. A chain-of-custody procedure requiresdocumentation of receipt, transfer, and disposal of forensicsamples with full, legal signatures of all persons involved.The following special procedures will apply when forensicsamples are being handled in our laboratories.
98
1. If a client indicates that he wishes chain-of-custodydocumentation, or that the sample(s) are to be used in aforensic situation, client personnel will be contacted andinformed of the fee we charge to cover the cost ofdocumentation and special handling, and authorization toproceed will be requested.
The client will also be asked if he wants a copy of *>the chain-of-custody documentation. If he does, we will useeither the client-supplied form for documentation, or the LLIform designed for this purpose (copy attached).
Disposal instructions will also be requested of theclient. Disposal options are:
a. retention in locked storage at LLI for a variablelength:of time, not to exceed 1 year,
b. transfer to bonded storage at client's request""andexpense,
c. return to client, ord. disposal in the same manner as regular samples.
2. The use of the client form or LLI fora forchain-of-custody when requested by the client will be inaddition to our internal chain of custody records, which willbe maintained in a bound notebook kept by the SampleAdministration Group.
3. Sample receipt and log-in will proceed as in Part I,except that receipt will be acknowledged in thechain-of-custody notebook and on the forms, if required.
4. Immediately after log-in, the sample will be depositedin the computer designated storage area, which will be a lockedstorage area for all forensic saaples. Keys to the lockedstorage area will be kept by the Coordinator of SampleAdministration and her/his designated deputies. Said deputiesshall be personnel of the Sample Administration Group, or oneor more Group Leaders, or Managers of the Food Chemistry orInstrumentation/Environmental Chemistry Departments.
39 AR30IM7
5. Analysts wishififf€6-"w rk on forensic camples shallrequest the samples from the Sample Administration Group.Transfer of samples to the analyst will be documented in thechain-of-custody notebook, and any applicable forms.
6. Samples transferred to an analyst shall be kept in thelaboratory, in the custody of the analyst, .for the minimum timerequired for the analysis. Under no circumstances shall theybe left unattended overnight, but shall be transferred back tothe Sample Administration Group for locked storage overnight. .,
7. Transfer of samples from one analyst to another in thelaboratory shall be documented in the chain-of-custody notebookand any required forms.
8. Upon completion of analysis, the samples shall bereturned to the locked storage area under supervision of SampleAdministration Group personnel, and the return documented.Sample Administration Group personnel shall arrange fordisposal of forensic samples in accordance with the client'swishes. Final disposal of the samples shall also be documented.
3/85
100 flR30""8
EXHIBIT XVI
SAMPLE AND DATA ROUTING AT LANCASTER LABORATORIES, INC.
Action Personnel Involved
Sample Received at LLI Sample Administration
Sample is entered onto sample Sample Administrationmanagement system (lab IDnumber assigned, analysesscheduled, chain-of-custodystarted, storage locationassigned *
Sample stored in assigned Sample Administrationlocation (refrigerator,freezer, etc.)Removed from storage for ' Technical Personnel 'analysis; necessary aliquottaken and sample returned tostorage
Analysis performed according to Technical Personnelselected analytical method; rawdata recorded in notebook andtransferred to computer bychemist or technician*
Computer performs calculations as Data Processingprogrammed according to methods
Chemist or supervisor verifies Technical Personnelraw data (•
'!Computer generates final report Data Processingwhich is sent to client along Middle Managementwith any copies of raw data Corporate Managementrequested. Final reports arereviewed by supervisors priorto mailing*Analyses requiring the chemist's interpretation aayinvolve manual data reduction prior to entry onto thecomputer.
AR30UI9
^LI
AN
U
* t
3!
Cl
Ut>
-•;
*
EXHIBIT XVII
P«aF39MANC£ EVALUATION REPORT
WATER POLLUTION STUDY N'JMSER irfPOl
SQftATORYS PA009 -7-> AJ.'Z /->VfV£/$S*J?:J? /-A oS
SAMPLE REPORT TRUE ACCEPTANCEALYTES NUM3ES VALUE VALUE* LIMITS
TRACE METALS IN HICROGRAMS PER LITER:
UHINJK 1 392 390 303.- 517.2 143 156 109.- 211.
SENIC 1 2S5 250 189.- 326.2 75.2 73.0 55.2- 99.4
RYLLIUM 1 108 108 90.0- 12S.2 28.8 32.4 25.9- 39.1
DMIUM , 1 99.0 100 32.7- 115.2 49.0 50.0 40.4- 57.1
SALT t 201 204 170.- 239.2 64.5 67.9 53.6- 31.5
ROMTUM 1 96.4 90.0 69.5- 107.2 64.0 60.0 44.6- 72.6
P?ER 1 216 224 194.- 2*9,2 23.9 22.4 15.9- 28.8
3N 1 638 672 572.- 733.2 63.5 67.2 49.4- 82.5
RCU3Y 1 4.8 4.30 3.23-6.482 0.65 0.600 .231- .977
NSANESE I 241 252 220.- 277.2 61.8 63.0 51.9- 72.5
CKEL 1 245 245 205.- 284.2 49.5 49.0 37.1- 61.3
A3 1 307 315 260.- 365.2 80.5 34.0 65.5- 103.
7
E: li/i?/
WARNING PE9F02MANCLIMITS EVALUATION
331.- 490.121.- 198.
207.- 309.60.8- 93.9
94.9- 123.27.6- 37.4
86.7- 111.42.5- 55.0
179.- 230.57.2- 77.9
74.2- 103.43.1- 69.1
201.- 242.17.5- 27.2
593.- 713.53.4- 73.4
3.64- 6.07.325- .383
227.- 270.54.5- 69.9
215.- 274.40.1- 59.3
273.- 352.70.5- 98.2
3AS-3 UPON THEORETICAL CALCULATIONS. 3R A R£r£*£NCE VALUE WHEN
10?.AR30
ACCE»TA3IACC£PTA3I
ACCEPTA31ACCEPTA3I
' ACCEPTA3IACCE»TAdl
* ACC£»TA3IACCEPTA5I
ACC£«TA3iACCEPTA4I
ACC£?TA2'ACC£»TA3
ACC£BTA3ACCEPTA3
ACC2PT43ACCEPTAi
ACCE9TA3ACCc'TAi
ACCEPTA34CC£'TA3
ACCc?TASACC£?TA»
ACCS'TAJACCc9TA^
N5C?.3SA?Y
U20
EVALU1TICN RcPCRT 3ATE: li
HATER POLLUTION STUDY NUM3E* MP017
L133RAT3RY: PA009
-4MALYTES
TRACE METALS
•«ji •UTlltf
Vl^l&^TllM
ZINC
ANTI*4-?^Y
"LVER
iHALLIUM
OLY33ENUM
TRONTI'JM
ITANIU^
MINERALS IN
PH-UMITS
SPEC. C3NO.rUHHOS/CM AT 25 O
SAMPLENUM3E.R
IN MI<
• 12
12
12
34
34
34
34
34
34
MILLIS
34
12
REPORTVALUE
:RO£*AMS33.054.3
15941.3
30213.0
10325.5
10.26.15
47.514.5
33.421.2
43.04.5
13766.5
RAMS PER
8.344.43
356536
TRUEVALUE*
PER LIT
10060.0
15531.0
30419.0
10323.3
10.45.24
50.015.0
41.523.3
50.44.20
19563.3
LITER:3.964.39
373611
ACCEPT1NCELIMITS
E*:
30.2- 119.43.5- 75.1
120.- 192.12.0- 50.9
255.- 343.13.4- 25.7
70.6- 152.15.7- 44.5
7.57- 13.14.51- 7.93
34.4- 67.3U.l- 20.6
25.3- 57.011.1- 34.1
40.3- 57.42.76- 5.33
150.- 247.40.7- 101.
<EXCc»T AS
3. S3- 3.104.31- 4.50
335.- 410.540.- S6).
WARNINGLIMITS
85.1- 114.47.5- 71.1
130.- 132.17.2- 45.6
267.- 337.14.9- 24.2
31.5- 142.19.5- 40.3
3.36- 12.44.35- 7.55
33.9- 63.411.3- 19.1
29.3- 52.514.2- 30.9
43.1- 55.13.23- 5.46
163.- 234.50.1- 99.9
NOTED)
3.63- 9.044.33- 4.47
344.- 401.556.— 653.
PERFORMANCEsVALUATICN
ACCEPTA3LACCEPTA3L
ACCs'TAaLACC5PTA3L
•' ACCEPTAiLACCEPTA3L
' ACCs°TA3LACCEPTA3L
ACCr LACCEK^A
6CC=»T13LACCS'TAdL
JCCI'T13LACC£?TASL
ACCc°TASLACCE'TAiL
aCC='TS3LACCi3TA3L
4CCr*T43LACCz'TlSL
ACC:?TA3L»CC:»TAU
3ASSO UPON THEORETICAL CALCULATIONSt CR a ^ErE^rNCE VALUE WHEN
AR30U2I103
?£RF:RMANC£-EVALUATION REPORT SATE: n/i9/!HATER POLLUTION STUDY NUM3E3 WP017
33RAT33Y: PA009
A LYTESSAMPLENUMBER
REPORTVALUE
TR'J£VA'.Uc*
ACCE'TANCcLIMITS
WARNINGLIMITS
PERFORMANCEEV4LUATI3N
MINERALS IN MILLIGRAMS PER LITER.* (EXCEPT AS NOTED)
TOS AT 180 C
:ACA
AL HARDNESSCAC03)
.CIUH
lApESI'JM
'l
r'Q
•c?HI
LI
Jl
AM
HUM
ASSIUM
4L ALKALINITYCAC33)
.CRIOS
OR IDS
FATE
NUTRIENTS
3NIA-NITROGEN
12
12
12
12
12
12
12
12
12
12
222312
126150
45.21S.O
0.92724.9
14.150.3
5.3012.8
11.075.0
95.5105
3.180.53
17.260.5
IN MILLIGRAMS PER
12
0.881.88
232315
113142
46.015.0
0.91025.0
13.256.2
5.0013.0
9.9975.0
$4.0101
3.200.531
16.060.0
LITER:0.2002.00
154.- 390.230.- 385.
110.- 130.132.- 155.
40.0- 51.414.2- 19.2
.753- 1.12 -21.1- 23.3
11.3- 15.143.3- 62.3
3.95- 5.9410.3- 15.3
7.28- 14.567.4- 80.2
77.6- 93.393.1- 109.
2.69- 3.S6.430- .642
11.2- 19.747.4- 70.8
.0261- .4611.54- 2.44
133.- 360.293.- 372.
112.- 128.135.- 152.
41.4- 50.014.9- 13. S
.304- 1.0722.0- 27.4
11.3- 14.650.1- 61.0
4.20- 5.6911.4- 14.7
8.17- 1?.669.0- 73.6
79.5- 91.435.1- 107.
2.31- 3.54.457- .515
12.2- IS. 650.3- 67.3
.0784- .4091.65- 2.33
ACCE»TA3l
ACCEPTA3LACCE«»TA3L
"ACCE*TA3LACCEPTA3L
' ACC2»TA3L*CCE*TA3L
ACCEPTA3LSCC5PTA3L
ACC5PTA5LACCE'TAsL
4CC:»TA3L
ACCEPTA3LACCE'TASL
4CCEPTA3LACCE'TAiL
ACCE'TA3LACCEPT43L
NCT ACCcPTAjL»CC£?TA3L
SASE3 UPON THEORETICAL CALCULATIONS* 23 \ REFERENCE VALUE WHEN
104 flR30ll»22
P5RS0»MANC£ EVALUATION R£?ORT OATE: 11 /-
WATER POLLUTION STUDY NUH82R WP017
LABORATORY: P4009
MMALYTESSAMPLENUMBER
R£3QI»T TRUE ACCEPTANCEVALUr VALUe* LIMITS
WA9NINGLIMITS
PERFORMANCEEVALUATION
NUTRIENTS IM MILLIGRAMS PER LITER:
lITRATE-NITROGcN
IRTHO'HOSPHATE
XJsLDAHL-NlTROSzN
TOTAL PHOSPHORUS
DEMANDS IH
JB
1Z
-DAY 303
PC3»S IN *
rC3-A33CLOR 1015
C3-A30CLOR 1254
12
12
34
34
MILLIGRAMS
12
12
12
0.191.43
0.220.50
0.32.6
0.271.07
? = R
31473.4
12733.4
20745.5
0.2001.50
0.0200.600
0.6003.00
0.4001.00
LITERS
33134.2
13133.3
20451.3
.131-1.20-
.0036-..314-
.0721-1.94-
.307-
. SOS-
274. -60.6-
101.-25.3-
121.-23. S-
.2661.73
0363.633
1.224.33
.3101.23
361.36.6
155.40.5
237.75.0
.147-1.27-
.0076-..535-
.211-2.20-
. .232-.356-
295.-65.1-
103.-27.3-
142.-34.2-
.2491.71
0324.667
1.033.33
.4351.13
350.32.1
149.39.5
267.69.3
ACCePTAatACCEPTA31
HOT ACCEPTA51MOT ACCs'TAat
" ACCE'TAil
' ACC£?T45!ACC£?T4>1
iwi jS«S?1!ACCEPTA3
ICROGRAHS PER LIT23:
1
2
1.93
2.51
1.33
2.34
.329-
.337-
2.53
3.25
1.05-
1.23-
2.36
2.95
ACCsPTi-
ACC£»Tt!
HAS:} UPON THSORETICJL CALCULATIONS. OR A R£P£R£NC5 VALUE WH5N
AR30II»23
, PERFORMANCE EVALUATION RSPQRT OATE: ll/19/<
WATER POLLUTION STUDY NUM3£R *P017
LA33RATORY: PA009LAd—AN
,L
01
3D
SAMPLELYTeS NUHSER
REPORTVALUE
PESTICIDES IN MICROGR
RIN 1 02 0
L3RIN 12
12
OOf 12
** 1
-— — «^
rtt!
JEf
.HI
iTACHLOR i
2
ITACHLOR €?CXID6 1
203DANE 3
4
00
00
00
0
00
00
VOLATILE HALOCAR30NS
1,2 DICHLORDcTHANE 1
1 *CHI
1 v <
.3ROFORM I2
Lil TRICHLOROETHANE 12
TRUEVALUE*
AMS PER LITER:.537 0.590 ..106 0.125 .
.814
.211
.937
.263
.596
.114
1.12.239
.531
.214
.506
.116
7.451.39
00
00
60
0
00
00
.352
.232
.932
.266
.539
.095 .
1.31.2$! .
.571
.233 .
.511
.120 .
8.642.35
IX MICROGRAMS
S3.113.3
64.929.6
SO.O12.7
90.2
60.424.2
73.811.8
ACCEPTANCELIMITS
0473-0060-
.371-
.118-
.333-
.125-
.174-0452-
.457-0935-
.150-0358-
.205-0373-
4.07-1.09-
.900
.190
1.25.316
1.42.373
.352
.166
2.09.378
.337
.329
.738
.192
11.73.21
WARNINGLIMITS
.157-.0295-
.484-
.144-
.524-
.158-
.251-.0607-
.665-
.130-
.247-
.117-
.274-.0577-
5.04-1.36-
.791
.166
1.14.290
1.29.347
.765
.151
1.63.342
.751
.299
.670
.173
10.72.54
PERFQ3MANC:EVALUATION
ACC£?TA3LACCEPTA3L
ACCfPTASLACCEPTA3L
" ACCE*T43LACC£9TA3L
' ACCE?Ta3LACC£?T*iL
ACC£'TA3L
ACCEPTJ2LACC£'T45L
ACCESTA3L
ACC=3TS3LACCe?TA3L
PER LITER:49.3-9.54-
41.7-13.5-
46.2-5.32-
13?.24.1
83.133.6
104.20.6
51.1-11.4-
47.0-20.4-
53.5-7.23-
127.22.3
77.831.7
96.418.7
ACC5PT4-JL
ACC=?Ti3LACC=»T43L
ACCE'TJSL
BASED UPON THEORETICAL CALCULATIONS! C* A RES£RENCE VALUE WHEN
PERFORMANCE EVALUATION 'E^ORT 5AT«: 11•
WATER POLLUTION STUOY NUM3£R WP017
LA30R4TORY: PA009
SAMPLEANALYTES NUMBER
REPORTVALUE
TRUEVALUE*
VOLATILE HALOCAR30NS IN MIC30GRAMS
TRICHLOROsTHENE
CAR30NTETRACHLORIOE
TST1ACHLOR05TMENE
342MOOICHLORQMETHAMS
M»aMCHl3<IOI»TH»H
«3,D=3«
IsTHYLrNE CHLCSIOE
:*LM9.ltt*U
VOLATILE AROMAT
3-N""£ETHYL3EMIEME
TOLUENE
12.
12
12
12
12
12
12
12
ICS
12
12
12
55.515.3
93.310.2
52.411.0
30.719.3
76.323.7
93.222.6
11415.7
27.015.4
IN MICRO
7,4*43.0
9.3273.6
17.794.2
55.112.5
92.77.34
43.33.47
54.515.5
71.716.7
97.127.0
93.313.7
73.113.6
GRAMS c
7.7851.3
13.573.5
13.299.0
ACCEPTANCELIMITS
PER LITE?:
35.1- 73.35.25- 20.3
59.4- 123.1.37- 1«».9
23.3- 6*.l4.77- 13.5
53. 2- 115.10.3- 22. a
47.3- 113.10.6- 25.3
57.5- 157.16.5- 39.3
44.6- 14S.7.43- 23.3
42.2- 114.3.23- 13.7
»r* LITER:4.57- 11.734.3- 59.5
5.33- 16.450.1- 105.
11.3- 25.063.3- 133.
WARNINGLIMITS
40.7- 72.83. 05- 13.5
63.4- 120.3.62- 13.3
33.7- 59.75.33- 12.3
67.2- 103.11.9- 21.2
55.4- 104.12.5- 23.9
70.1- 144.19.5- 3o.«
57.6- 133.9.45- 21.2
51.3- 105.9.77- 1«.2
5.57- 10.333.9- 54.9
5.74- 15.057.3- 93.3
13.1- 23.372.3- 124.
EVALUATION
ACCEPTA31ACCEPTAal
ACCEPTA31ACCEPTAal
•• 4CC-PTA31
ACCSPTA31ACC£»TAV
4CC5' *3
ACCE°T45ACC£?TA3
ACCEPT:*4CC-PT43
ACCE»TA3
ACC=?T45
ACCiPTi!ACCsPTA;
4CC1PTA4CC5PT4
?ASEO UPON THEORETICAL C ALCULATI3NS t 0? A ?S=£RENC£ VALUE WHrN
AR30U25
PERFORMANCE EVALUATION R£»ORT DATE: li/19/UATE3 POLLUTION STUDY NUM3ER WP017
MORATORY: PAO'OS
*
1
I.
1
4
r i
SAMPLEULTTcS NUM3ER
VOLATILE AROMATICS
2-3ICHLOR03EMZENE
3-OICHLOR03ENZENS
4-DICHL3R03ENZENE
MISCELLANEOUS
TAL CYANIDEN MG/L)
^L-FILT£RA3Le RESIDUEv3N MG/L)
>1L AND GREASE3N MG/L)
~3TAL PHENOLICSIN XG/L)
12
12
12
REPORT TRUE ACCEPTANCEVALUE VALUE* LIMITS
WARNINGLIMITS
«• *\ m W ( •! M -1 \f
EVALUATION
IN MICROGRAMS PER LITER:
14.371.6
19.671.3
5.6853.7
PARAMETERS:i2
12
12
12
T1TAL RESIDUAL CHLORINE 1ON MS/L) 2
0.1250.1=7
13.356.3
17.566.5
0.2910.625
C.300.78
t 14.072.9
20.677.4
5.4654.6
i
0.1410.213
16.060.5
15.6: 68.4
0.314.750
0.2510.300
5.73- 23.237.6- 110.
5.39- 33.220.0- 121.
1.84- 9.7922.1- 39.7
.0854- .178.133- .284
10.2- 18.249.6- 63.4
5.53- 22.243.9- 80.2
.145- .511
.302- 1.16
.0460- .496.454- 1.17
8.03- 29.947.1- 101.
5.24- 29.334.0- 107.
2.90- 3.7336.2- 31.5
.0971- .166.152- .265
11.2- 17.251.3- 61.7
7.69- 20. 148.5- 75.7
.191- .465
.409- 1.05
.111- .432
.557- 1.07
ACCEPTASACCEPTA3
ACCEPTA3ACC£°TA5
•- ACCEPTA5ACCEPTA3
• •
ACCE»T43IACCEPTAsI
ACCEPTA31ACC£'TA2I
ACCEPT15IACCEPTASI
ACCEPTAalACC2PTA3I
ACC£PTA5!ACCEPT45I
SASE3 UPON THEORETICAL CALCULATIONS, OR A RcFEReNCE VALUE WHEN NECESSARY
flR30ll*26
UNITED STATES ENVIRONMENTAL PROTECTION AGENCYWASHINGTON. D.C. 20460
JUN t 1 1987
OFFICE OfSOLID WASTE AND EMERGENCY
To: Laboratories Participating in Pro-Award PerformanceEvaluation Samples for IFB's WA 87-J004
Dear Participant:
Enclosed are copies of your score sheet for the pre-award"Performance Evaluation Samples" for IFB's WA 87-J004 and theacceptance windows. -- •
The acceptable score for performance on those samples is 300points.
If you wish to have a debriefing, please contact Larry Butlerat EMSL-LV.
Sincerely,
X £Joan F. FiskNational Organics Program Manager
Enclosure
cc: Larry Butler, EMSL-LV
AR30U27
WP-1572C
VOA ONLYPREAUARD PERFORMANCE EVALUATION SAMPLE DATA SCORING
Laboratory Lancaster Laboratories. Inc. (LANCAS) #95_____
IFB _____VOA Only WA87-J004 ___________ Date 5-11-67 _______
SUMMARY:
I. Identification 150 points 150 pointsfor water for soil
a. Total number of I pts. deducted 0 0Water Soil
b. pts. awarded for I 150 150
II. Quantification
a. Total number of II pts deducted 0 0
b. pts. awarded for II _150 _150
Total points awarded for I and II, water and soil 600 out'of600 pts.
III. Quality Control 300 pts.
a. Total number of III pts. deducted 0_____
b. pts. awarded for III 300 out of300 pts
TV. Reporting/Deliverables 100 pts.
a. Total number of IV pts. deducted 0______
. b. pts. awarded for IV 100 out of100 pts
V. Score
a. Total number of I, II, III,1 and IV pts. awarded 1000 out of1000 pts.
b. Total pts. awarded , , .. 1000 out of1000 pts
VI. Number of days late 0
uo AR30U28
IMPORTANT: 1} Points deducted will not exceed the maximum possible number ofpoints.
I. Identification (150 points for water sample; 150 points for soil samples.
A. Target Compound List (TCL) identification (Water Water SoilSample • 100 pts. max.; Soil Sample - 100 pts. max.).
Number of compounds not identified ( 0/0 ) X 100 pts.(Number of compounds in study ( 8/8 )/10- ( 0/0 ) pts. ..ded. __0_ __0_
B. TCL false positives (Water Sample - 30 pts. max.;Soil Sample - 30 pts. max.)
Number of TCL false positives ( 0/0 ) X 3 points »( 0/0 ) points deducted 0 __o_
C. Tentatively Identified Compounds (TIC) identification(Water Sample • 10 pts. max.; Soil Sample * 10 pts. max.)
* •
Number of compounds not identified ( 0/0 ) X 10 pts.Number of compounds in study ( 6/4 )" ( 0/0 ) pts. ded. __0_ __0_
D. TIC false positives (Water Sample * 10 pts. max.;Soil Sample » 10 pts. max.)
Number of TIC false positives ( 0/0 ) X 1 point -( 0/0 ) points deducted __0_ __p_
Total number of I pts. deducted 0 __p_
II. Quantification of. the TCL (.150 points for water sample; 150 points forsoil sample)
A. TCL quantification include VOA(Water Sample » 150 pts. max.; Soil Sample » 150 pts. max.)
Number of compounds not within criteria ( 0/0 ) x 150 ptsNumber of compounds in study ( 3/8 )/5- ( 0/0 ) pts. ded. __0_ __0_
Total number of II pts deducted 0 __0_
AR30U29x> • « •
III. Quality Control (300 points)
i A. Instrument Quality Control (150 points) Number of—' Pts deducted
1. Tuning (50 points)*
b. BFB (50 pts. max.)
1. For any BFB performance tune analyzed separately oradded to reagent water with any critical ions abundanceratios outside criteria deduct a maximum of 25 points.(Critical key ions are: 95, U, 174, 175 176. 177.) __p__
2. For any BFB performance tune analyzed separately oradded to reagent water with any non-critical ions abund-ance ratios outside criteria deduct 2 points for each toa maximum of 25 points. (Non-critical key ions are: 50,75, 173.) __0_
3. Failure to perform a BFB tune at the 12-hour "~frequency, deduct a maximum of 50 pts. 0
2. Initial Calibration (50 points)t ,,,.... .• ..
a. For initial calibration data for VOA withSystem Performance Check Compound (SFCC) averagerelative response factor (RRF) less than 0.300
_J (less than 0.250 for Bromoform) (25 pts. max.)
# compounds not within criteria. ( 0 )Total number of compounds, (_10._.)X 25 pts « ( 0 ) pts. ded. __0_
b. For initial calibration data for VOA withCalibration Cheek Compound (CCC) percent relativestandard deviation greater than 30%, (25 pts. max.)
ft compounds net within criteria. ( 0 )Total number of compounds, (•12 )X 25 pts. • ( 0 ) pts..ded. __0_
e. Failure to perform initial calibration- will result inthe deduction of all the Quality Control points, whichequals 300. 0
AR30U30
Number^ ofPts. Deducted
3. Continuing Calibration (50 points)
a. -for continuing calibration data for VOA. withSystem Performance Check Compound (SPCC) average relativeresponse factor (RRF) less than 0.300(less than 0.250 for Bromoform). (25 pts. max.)
# compounds not within criteria. ( 0 >Total number of compounds, ( 10 ) •••J. 25 pts. • ( 0 ) pts. ded.
b. For continuing calibration data for VOA withCalibration Cheek Compound (CCC) percent relative standarddeviation greater than 25% (25 pts. max.)
it compounds not within criteria. ( 0 )Total number of compounds, ( 12 )X 25 pts. « (__0_) pts. ded.
i
c. Failure to perform continuing calibration will result inthe deduction of all the continuing calibration points,which equals 50 points.
B. Sample/Method Quality Control (150 points)«
1. Surrogate Spike recovery (60 points) NOTE: Do notinclude Method Blanks.
a. VOA (60 pts. max.)
Number of surrogate compound9 not within criteria ( 0 )Total number of VOA surrogate compounds (12 ).X 60 pts. » ( 0 ) pts. deducted
2. Method Blank Analyses (60 points)
Failure to perform the method blank analysis for any of thefractions will result in the deduction of 60 points.
a. VOA surrogate recovery (30 pts. max.)
Number of surrogate compounds not within criteria ( 0 )Total number of VOA surrogate compounds ( 6 )X 30 pts. - ( 0 ) pts. deducted.
flR30ll»3l
Number ofPts. Deducted
b. VOA method blank contamination (30 pts. max.).
* If one or more TCL compounds are detected in the methodblank above the contract required quantitation limit(5X the CRQL for methylene chloride, acetone, toluene,and 2-butanone) deduct the maximum points, 30. _ 0
3. Matrix Spike/Matrix Spike Duplicate (30 points)
a. Utilization of the wrong spiking concentration in one ormore of the fractions will result in the deduction of 30points.
b. Failure to perform matrix epike or matrix spikeduplicate analysis will result in the deduction of30 points. HR
Total number of III pts. deducted o
IV. Reporting and Deliverables (100 pbints) ' .
A. BFB (25 points max)
1. Mass listing and bar graph output submitted for eachinstrument and for every 12-hour period samples wereanalyzed. Deduct 25 points for any BFB violation. 0
B. EICs, Chromatograms, quantitation reports, and system print-outs (25 pts. max.)
1. Deduct 25 points if any of the required deliverables arenot submitted in aceordanee with .the statement of work. 0
C. Mass spectra (25 pts. max.)
1. Deduct -25 points if any of the required deliverables are• not submitted in accordance with the Statement of Work. 0
D. Contractual Forms (25 pts. max.) •
1. Deduct-25 points if any .of the required deliverablesare not submitted in aceordanee with the Statement of Work. 0
Total number of IV pts. deducted
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ATTACHMENT 2
ENVIRONMENTAL RESOURCES MANAGEMENT, INCORPORATEDSTANDARD OPERATING PROCEDURES
AR30U31*
TheERM Group
ORJGINAi
STANDARD OPERATING PROCEDURESFOR RI/FS-RELATED FIELD INVESTIGATIONS
AT THEKIMBERTON, PENNSYLVANIA NPL SITE
July 1987
Prepared By:
Environmental Resources Management, Inc.999 West Chester Pike
West Chester, Pennsylvania 19382
TheERM Group
TABLE OF CONTENTS
Page
Section 1 - Introduction 1-1
Section 2 - Stream Sampling Protocol 2-1
2.1 Preparation for Stream Sampling 2-12.2 Stream Sampling Procedures (Water) 2-12.3 Stream Sampling Procedures (Sediment) 2-22.4 Decontamination Procedure 2-32.5 Sample Preservation 2-42.6 In-Field Measurements 2-42.7 Procedure-Specific Health and Safety Plan 2-5
i Section 3 - Soil Sampling Protocol 3-1
3.1 Preparation for Soil Sampling 3-13.2 Soil Sampling Procedures 3-13.3 Decontamination Procedure 3-23.4 Sample Preservation 3-43.5 In-Field Measurements 3-43.6 Procedure-Specific Health and Safety Plan 3-4
Section 4 - ERM Health and Safety Program 4-1
4.1 Introduction 4-14.2 Medical Monitoring 4-14.3 Training 4-34.4 General Safety Practices 4-44.5 Decontamination 4-54.6 Level C - Generalized Personal Protection
Decontamination Procedure 4-64.7 Sampling Equipment and Sample Container
Decontamination 4-74.8 Location of Nearest Hospital 4-8
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The ERM Group
SECTION 1
INTRODUCTION
This document presents Environmental Resources Management, Inc.'s(ERM) site-specific Standard Operating Procedures (SOP) for thecollection of environmental samples relating to the Revised WorkPlan for Completion of the Remedial Investigation and FeasibilityStudy for the Kimberton, Pennsylvania NPL site. This document isintended to be an integral part of ERM's Quality AssuranceProject Plan (OAPP) which also includes the site-specific projectwork plan.
The samples collected in conjunction with the proposed work scopecan be categorized either as environmental samples or hazardoussamples. Samples collected from spills, lagoons, drums, andimpoundments are defined as hazardous samples due to the poten-tial for elevated contaminant concentration. Those samplesobtained from dilute sources such as runoff, surface and/orground water are categorized as environmental samples. Each ofthe aforementioned sample types requires specific samplingprocedures to insure the integrity of the samples and the safetyof the sampling personnel.
The proposed stream sampling falls within the above notedenvironmental sampling category. Specific sampling procedurespertaining to the streams investigation are outlined in Section2. The proposed subsurface soil resampling program is charac-terized as the collection of hazardous samples and is outlined inSection 3.
1-1 AR30U37
ThcERMQroap
SECTION 2
STREAM SAMPLING PROTOCOL
2.1 Preparation for Stream Sampling
Prior to the acquisition of both water and sediment samples fromsprings, seeps and streams, the following will be addressed:
Characterization of sample areas with respect tosurrounding topography, drainage pattern, andstream location.
Determination of specific equipment or proceduresrequired for the acquisition of statisticallyrepresentative samples or measurements.
- Characteristics of stream dynamics such ast depth,mixing zones, stagnation zones, aeration zones,and confluences.
Preliminary labeling and preparation of appropri-ate glass sample containers and chain-of-custodyforms.
Preparation of field and travel blanks. Thenumber of blanks will be established by LancasterLaboratories, Inc. of Lancaster, Pennsylvania.Field water blanks will be prepared by filling a40 ml glass vial with distilled water which hasequilibrated with ambient site meteorologicalconditions (i.e., temperature, baromtric pressure,etc.). Field equipment blanks (sediment samplesonly) will be acquired by collecting distilledwater in a 40 ml glass vial which has been pouredover the decontaminated sediment sampling equip-ment.
2.2 Stream Sampling Procedures (Water)
All samples will be collected as grab samples.
Stream samples will be obtained within the primarymixing zone, that is, from the primary flowchannel, at approximately one-half total streamdepth.
The ERM Group
Stagnant areas will not be sampled to avoid zonesof anomalous contaminant concentrations.
Spring samples will be collected as close aspossible to actual points of surface discharge toprevent chemical alteration of the ground water inambient meteorlogic conditions.
All samples will be collected with no headspace inlaboratory-sterilized 40 ml glass vials withTeflon septum-lined caps. Sampling personnel willutilize a clean pair of latex gloves for eachsample location.
Samples will be collected in duplicate to circum-vent resampling should post-sampling vial breakageoccur.
Sampling will be conducted from downstream toupstream stations to avoid suspending contaminantsinto the water column' from bottom sediments.
Sample containers will be rinsed three times withthe water to be sampled prior to sample procure-ment to equilibrate the container with the sampleenvironment.
Where possible, sampling will begin at thesuspected zone of lowest contamination and proceedto the zone of highest contamination.
- f . ' ,-. -
Immediately following sample procurement, thesamples will be labeled, logged on a chain-of-custody form, and secured on ice.
2.3 Stream Sampling Procedures (Sediment)
All samples will be collected as grab samples.
Sediment samples will be obtained within the primarymixing zone of the stream from a depth of 0 to 6 inchesbelow the stream bed.
- Sediments within stagnant or excessively aerated zonesof the stream will not be sampled.
All samples will-be collected with a decontaminatedthree-inch diameter stainless steel bucket auger.
2-2
TheERMGroup
Excess water will be decanted from the sample containerprior to sealing the sample in a laboratory-sterilizedone pint glass container with a teflon lined cap.
Samples will be collected in duplicate to precluderesampling should post-sampling container breakageoccur.
- Sampling will begin at the suspected zone of lowestcontamination and proceed to the zone of highestcontamination.
Immediately following sample procurement, the sampleswill be labeled, logged on a chain-of-custody form, andsecured on ice.
2.4 Decontamination Procedure
The potential for sample cross-contamination associated withstream water sampling has been minimized as a result of thefollowing planned procedures:
Sample containers will be utilized as sampling de-vices.
- Sample containers are precleaned and sealed at thelaboratory .
Sampling personnel will utilize a clean pair oflatex gloves at each sample location.
In light of this program, no specific sampling decontaminationprocedures have been incorporated into the stream water samplingprogram.
All non-disposable equipment used for the collection, prepara-tion, preservation, and storage of stream sediment samples willbe decontaminated in accordance with the following procedure:
- Removal of sediment from the equipment either with apressurized sprayer or a wash bottle and scrub brush(utilizing clean tap water);
Scrub equipment with an Alconox/tap water mixture;
Rinse equipment three times with clean tap water;
Rinse equipment with reagent-grade acetone;
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Triple rinse with deionized (distilled) water;
Allow equipment to air dry.
2.5 Sample Preservation
Generally, surface water samples exhibit increased stability incomparison to ground water samples, and tend to be in equilibriumwith atmospheric conditions. Therefore, samples from theaforementioned streams and seeps generally would not be expectedto undergo significant changes in water chemistry upon extractionfrom their environment. To insure proper preservation of bothstream water and sediment samples, all sample containers will bestored at 4'C until analyzed*
2.6 In-Field Measurements
In conjunction with the acquisition of surface water samples, thefollowing in situ measurements will be obtained:
pH, conductivity, and temperature
Stream and spring flow measurements
Stream and spring portable gas chromatograph analysis
2*6.1 Portable Gas Chromatograph Analysis
Stream and seep/spring samples collected in association with thestream monitoring program will be analyzed for trans-l,2-dichlor-oethene and trichloroethene using a Photovac 10S50 portable gaschromatograph. The 10S50 will be used to both quantitatively andqualitatively assess the presence of these two compounds viaheadspace analysis at ambient temperatures. A sensitive Photo-ionization Detector (PID) is used as the detector in the 10S50.
Appropriate copncentration level standards in water will beprepared from Supelco® stock standards (concentration of thestock standard is 200 mg/1). The 10S50 will be initiallycalibrated prior to the analysis of any samples. Recalibrationwill be performed periodically to account for compound retentiontime shifts due to changes in ambient temperature. Headspacemeasurements of laboratory pure distilled water will be analyzedto evaluate syringe cleanliness and carryover.
2-4
The ERM Group
Standards, samples, and blanks will be prepared by transferring a25 ml aliquot into a 40 ml screw cap vial with a teflon linedsepta. The cap will be .securely tightened and the sample willthen be shaken vigorously for sixty (60) seconds. This agitationprocess effectively drives volatile compounds into the headspaceof the vial. A gas-tight syringe is used to inject headspaceinto the chromatographic column via an injection port. The columnis a four foot (41) SE-30; 5% o'n 60/80 mesh Chromasorb G.
Trichloroethene and trans-l, 2-dichloroethene will be identifiedbased on comparison of retention times between tha standards andsamples. Integration of the area under the peak will be cor-related to that of the standard peak (at a known concentration)and the sample concentration calculated. Necessary dilutionfactors and injection volume variations will be used to correctraw sample concentrations. An example of the 10S50 chromatogramprint-out is presented in Figure B-2.
2.7 Procedure-Specific Health and Safety Plan
In accordance with ERM '3 Standard Operating Procedures, asite- and/or procedure-specific health and safety protocol mustbe developed for each task. The exposure potential associatedwith the proposed stream water and sediment sampling proceduresare minimal for the following reasons:
Based upon previous analyses (Ecology and Environ-ment, Inc., 1982 and Ground Water Technology,1982), the maximum contaminant levels associatedwith the on-site streams and springs fall belowthe established Threshold Limit Values (TLV) by aminimum of two orders of magnitude*
The source matrix (stream and/or spring) is inequilibrium with ambient atmospheric conditions;therefore, the potential for excessive volatiliza-tion within the associated breathing space isminimal.
The only plausible route of exposure is skincontact (hand and feet areas).
Field sampling personnel will wear rubber boots and gloves torestrict skin contact with the subject surface water thereforeeliminating the primary route of exposure.
AR30ll»U22-5
The ERM Group
SECTION 3
SOIL SAMPLING PROTOCOL
3.1 Preparation for Soil Sampling* •
Prior to the acquisition of soil samples from the on-site areasof concern (lagoons and potential drum storage area), thefollowing procedures will be performed:
Delineation of each sample area utilizing aerialphotograph interpretation and field measurements.
- Location of specific sample locations within eacharea of concern. Demarkation of sampling pointswill be accomplished with a permanent marker (woodor metal stake).
Decontamination of all sampling equipment with asteam cleaner prior to site access (i.e., drillrig, auger flights, split-spoon samplers).
Preliminary labeling and preparation of 4-ounceglass sample containers with Teflon-lined lids.
Preparation of field, travel and equipment blanks.The number of blanks will be established byLancaster Laboratories, Inc. Equipment blankswill be obtained by collecting distilled water ina 40 ml glass vial which has been poured over thedecontaminated split-spoon samplers.
Calibration.and charging of the Organic VaporAnalyzer (OVA). Isobutylene (100 ppm) is utilizedas a calibration gas.
3.2 Soil Sampling Procedures
Five sample stations will be established within each area ofconcern (one in each corner and positioned in the center). Soilsamples will be procured utilizing a continuous split-spoonsampling method (2-foot intervals). A representative sample fromeach two-foot interval of material will be sealed in a lab-oratory-sterilized four ounce glass container. Upon receipt at
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The ERM Group
the laboratory, and prior to analysis, all representative samplesfrom each area of concern will be composited. The specificsampling protocol is as follows:
ORIGINALSoil borings will be conducted utilizing a (3sd)truck-mounted hollow-stem auger drilling rig.
Soil samples will be procured with a 2-inch (I.D.)split-spoon sampler two feet in length. Thesplit-spoon will be advanced ahead of the augerflights at two-foot intervals.
Each time the split-spoon is extracted from theboring the soil will be scanned with an OVA todetermine the relative level of total volatileorganic compounds.
- Representative soils from each two-foot splitspoon sample will be procured in laboratorysterilized 4-ounce glass containers with teflon-lined lids.
Immediately following sample collection, thesamples will be labeled, logged on a chain-of-custody form and preserved on ice.
All individual samples from each area of concern(i.e., former lagoon) will be composited byLancaster Laboratories, at their facility,immediately prior to sample analysis.
All sampling equipment will be decontaminatedbetween each sample location*
Areas designated for investigation will be sampledin order from the suspected lowest to highestlevel of contamination based upon preliminarysampling by Groundwater Technology, Inc. in 1982.Since no data currently exists for Area 5, thislocation will be sampled last.
3*3 Decontamination Procedure
All non-disposable equipment used for sample collection, prepara-tion, preservation, and storage will be cleaned prior to theiruse and after each subsequent use. Unless the equipment andmaterials being used are disposable or of sufficient number so asnot to be reused during any one sampling period, decontaminationwill be conducted in the field.
3-2
The ERM Group
Three decontamination procedures will be utilized to facilitatethe acquisition of representative samples and minimize thepotential for cross-contamination. The first of these representsthe least stringent decontamination procedure and will be used toclean the split-spoon sampler between two-foot intervals at eachsoil boring location. This procedure is primarily required toobtain representative OVA readings from each interval. The augerdecontamination protocol will include:
Removal of soil from the split-spoon either with apressure sprayer or a wash bottle and scrub brush(utilizing clean tap water).
The second decontamination procedure will be conducted betweeneach soil boring and after encountering any anomalous layerswithin each area of concern (i.e., Lagoon 1, 2, etc.). Todecontaminate both the split-spoon and all sampling equipment,the following procedures will be conducted:
Removal of soil from the equipment with a pressur-ized sprayer or steam cleaner and brush, ifnecessary, (utilizing clean tap water).
Scrub sampling equipment with an Alconox/tap watermixture.
Rinse equipment either three times with clean tapwater or with a pressurized steam cleaner.
Final rinse with deionized (distilled) water." * r"
Allow equipment to air dry.
The last and most stringent decontamination procedure will beutilized to clean all sampling and associated equipment (i.e.,auger flights) prior to entering a new area of concern. Aspreviously stated, due to the ultimate analysis of only onecomposite soil sample per area of concern, this procedure is notrequired between each of the five soil borings within the areasof concern. The protocol is as follows:
Removal of soil from the equipment with a a steamcleaner (utilizing clean tap water).
Scrub sampling equipment with an Alconox/tap watermixture.
- Rinse equipment either three times with clean tapwater or with a pressurized steam cleaner.
3-3
The ERM Group
Triple rinse with deionized (distilled) water.
Allow equipment to air dry.
3.4 5a»ple Preservation
The preservation methodology which will be employed for all soilsamples is placement on ice and temperature maintenance at 4°C.
3.5 In-Field Measurements
Prior to conducting the in-field measurements, the samplers orfield team will review the operating manuals for pertinentinformation to guarantee proper calibration and standardizationof all instruments and probes. All subsequent field measurementswill ba conducted according to the procedures outlined in theappropriate operating manuals.
In conjunction with the collection of soil samples, the followingin situ measurements will ba procured:
Total VOC readings of each two-foot soil boringinterval below existing grade. Tha readings willba obtained with a Photovac OVA with a photo-ionization detector (PID) calibrates to isobutyl-ana (100 ppm) .
Continuous total VOC readings within fieldpersonnels' breathing space in accordance withERM 'a procedure-specific health and safety plan.
3.6 Procedure-Specific Health and Safety Plan
In accordance with ERM 'a standard Operating Procadures, atask-specific health and safety plan has baan developed for thasoil sampling program. Tha exposure potentials have bean basedon tha "worst-case" analyses collected in conjunction with tha1932 Groundwatar Technology preliminary lagoon investigation.
Tha minimal protection level proximal to any soil boring activitywill be Lavel D including tha following equipment:
Chemically-resistant clothing (Tyvex suits will bedonned if excessively dusty or muddy conditionsprevail)
AR30IH63-4
The ERM Group
Safety glasses
Inner latex gloves and outer nitrile gloves
Leather work boots and washable outer boots
- Dust masks if dusty conditions prevail
This minimal protection level will be upgraded to protection,,Level C under the following circumstances:
- 5 to 50 ppm total VOCs measured within theassociated breathing space will require donning ofhalf-face respirators and Tyvex suits.
50 to 250 ppm total VOCs measured within theassociated breathing space will require donning offull-face respirators and Tyvex suits.
The air quality within the breathing space proximal to thesampling areas will be monitored continuously with a PhotovacOVA. These readings will be recorded at fifteen-minute intervalsthroughout the course of the soil sampling program.
A predetermined disposal point will be designated for protectiveclothing, if necessary, prior to exiting the immediate investiga-tion area. Such clothing will be containerized on site forappropriate disposal if required.
A route map to the nearest hospital and a telephone for emergencyuse will be available within the plant building nearest to theinvestigation area. Emergency telephone numbers will be avail-able and posted at this location. Included are the followingnumbers:
POLICEEast Pikeland Township Police 935-2440Pennsylvania State Police 827-7461
FIREKimberton Fire Department 933-8966
AMBULANCEWest End Fire Company 933-3110
HOSPITALPhoenixville Hospital 933-9281
ERM West Chester 692-8606
AR30UI*?3—5
The ERM Group
SECTION 4
ERR HEALTH & SAFETY PROGRAM
4.1 Introduction
ERM has instituted a comprahansiva health and safety programdesigned to protect its employees from tha various potentialhazards associated with any fiald investigation. This sectiondiscusses the various components of tha ERM Health and SafetyProgram, detailing general protocols to ba followed throughoutapplicable field activities at tha Kimbarton, Pennsylvania NPLSita. Procedure-specific guidelines ara provided in the sub-sequent sections of this appendix.
4.2 Medical Monitoring
ERM has established a medical monitoring program to identify,monitor, and prevent health risks for employees potentiallyexposed to hazardous materials. All employees ara required to . ,participate in this program. This program has two essential • >—'components, routine health cara and emergency medical cara, asdacribed below:
1. Pre-employment examinations to establish the indiv-idual's state of health, baseline physiological data,and ability to wear personal protective equipment.
2. Annual physicals for fiald personnel.
3. Whenever a situation at a sita which may pose a sig-nificantly increased health risk to any personnel, orparsonnal exhibit currently job-related physicalconditions, tha Health and Safety Coordinator mayrecommend that such individuals consult with theexamining physician for examination and treatment inaccordance with good medical practice.
The baselina medical examinations include, but ara not limitedto, the following:
1. Complete medical and occupational/environmental historyand a physical medical examination
2. Pulmonary function tests, defined as FEV1 and FVC
4-1 AR30IH8
The ERM Group
3. An EKG — 12-lead
4. A chest X-ray (PA) with interpretation by NIOSH-certif-ied "B" reader (if recommended by examining physician)
5. A urinalysis — routine and microscopic
6. Chemzyme analysis (E/G ratio), SGIP, SCOT, alumalbumin,alkaline phosphatases, bilirubin (total), BUN, ere-'atinine ratio, calcium, CO2 content, cholesterol,chlorites, creatinine, globulin, glucose, LDH, phos-porous (inorganic), potassium, protein (total), sodium,triglycerides, uric acid, complete blood, count withdifferential and platelet count
7. Audiometric testing
8. Visual acuity (to be performed as part of the physicalexamination)
9. Other special tests
The need for special testing (i.,e., PCB levels, serum cho-lestrol, etc.) is determined by the examining physconsultation with ERM's Health and Safety Officer.
Annual physical examinations need not include EKG or chest X-rayunless either is recommended by the examining physician. Suchexaminations include an update rather than a complete medicalhistory of the individual.
Following the completion of each previously decribed medicalexamination, the following is conducted:
The examining physician or appropriate representativediscusses with each individual the results of theirmedical examination. In these discussions, any medicalcondition which warrants further evaluation or treat-ment, and any possible medical condition which couldhinder the employee from safely and efficientlycompleting his/her work with relationship to wearingpersonal protective clothing is discussed.
- The examining physician or appropriate representativenotifies ERM's Health and Safety Coordinator in writingthat the individual has undergone a complete medicalexamination. In addition, ERM's Health and SafetyOfficer is advised as to any medical condition that thephysician feels would adversely affect the individual's
AR30IH94-2
The ERM Group
ability to work under conditions requiring the use ofpersonal protective clothing. ERM's Health and SafetyOfficer than take appropriate action, if needed.
4.3 Training
Training is performed to ensure that personnel are:
aware of the hazardous aspects of work;
awara of the regulations and rules of conduct specificto on-site activities;
knowledgeable and comfortable with tha safe operatingprocedures, work practices, and emergency actionestablished at each sita; and
- confident regarding tha ability to respond to emerg-encies in a safa, aff active manner.
Therefore, tha training program is a "preventive" measure, ifimplemented and enforced, will help to reduce employee injury,illness, and accidents, thus decreasing tha likelihood of workercompensation claims, suits, and other legal actions.
An introductory training coursa is provided to all ERM employeesaccording to tha duties and area of naed undar the directsupervision of ERM's Health and Safety Coordinatopr. Thefollowing subjects ara covered during introductory training:
a. Overview of pertinent federal lawsb. Safety and health principlesc. Introduction to hazardous materialsd. Toxicologye. Dermal protectionf. Respiratory protection principlesg. Risk assessment and site safetyh. Sita operationsi. Monitoring instrumentsj. Decontamination principles
In addition, on-sita field refresher training is provided by orunder tha instruction of tha Haalth and Safety Coordinator.
Prior to the start of field activities, all subcontract personnelwill be informed of the hazards and potential exposures relatedto the planned activities and of the Haalth and Safety proceduresto be followed by ERM. v j
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4*4 General Safety Practices
The following are important safety precautions which will beenforced during this investigation:
1. Eating, drinking, chewing gum or tobacco, smoking, orany practice that increases that probability ofhand-to-mouth transfer and ingestion of material isprohibited in any area designated as contaminated. *
2. Hands and face must be thoroughly washed upon leavingthe work area and before eating, drinking, or any otheractivity.
3. Whenever decontamination procedures for outer garmentsare in effect, the entire body should be thoroughlywashed as soon as possible after the protective garmentis removed.
4. No excessive facial hair, which interferes with thesatisfactory fit of a mask-to-face seal, is allowed onpersonnel required to wear respiratory protectiveequipment.
5. Contact with contaminated surfaces or with surfacessuspected of being contaminated should be avoided.Whenever possible, one should not walk through puddles,mud, or other discolored surfaces; kneel on ground;lean, sit, or place equipment on drums, containers,vehicles, or the ground.
6. Medicine and alcohol can potentiate the effect fromexposure to toxic chemicals and should not be consumedby personnel involved in the site investigation.
7. Personnel and equipment in the contaminated areasshould be minimized, consistent with effective siteoperations.
8. Work areas for various operational activities should beestablished.
*. - i. r ' ' •• •9. Procedures for leaving the contaminated area must be
planned and'implemented prior to going to the site.Work areas and decontamination procedures must beestablished on the basis of prevailing site conditions.
10. Respirators will be issued for the exclusive use of oneworker and will be cleaned and disinfected after eachuse.
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11. Safety gloves and boots shall ba taped to the dis-posable, chemical-protective suits whan necessary.
12. All unsafe equipment left unattended will ba identifiedby a "DANGER, DO NOT OPERATE" tag.
13. Noise mufflers or ear plugs may be required' for all ERMpersonnel working around heavy equipment. Thisrequirement will ba at tha discretion of tha SitaSafaty Officer. Disposable, form-fitting plugs arepreferred.
14. Cartridges for air-purifying respirators will bachanged daily at a minimum.
15. Self-contained breathing apparatus (SCBA) and air-purifying respirators will be inspected daily by thaSita Safaty Officer.
4*5 Decontamination
In general, decontamination involves scrubbing with an Al-conox/water solution followed by clean watar rinses. Alldisposable items shall be disposed of in a dry waste drum.Certain parts of contaminated respirators, such as harnessassemblies and leather or clothing components, are difficult todecontaminate. If grossly contaminated, they may have to bediscarded. Rubber components can ba soaked in soap and watar andscrubbed with a brush. In addition to being decontaminated, allrespirators, non-disposable protactiva clothing, and otherpersonal articles must be sanitized before they can ba used againif they become soiled from exhalation, body oils, and per-spiration. The manufacturer's instructions should be followed insanitizing of all respirator equipment. If practical, protectiveclothing should ba machine-washed after a thorough deconta-mination; otherwise, it should ba cleaned by hand.
Decontamination procedures should match tha prescribed lava Is ofpersonal protection. A detailed discussion for tha establishmentof procedures required for procedure specific levels of personalprotection is presented in ensuing sections.
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4.6 Level C - Generalized Personal Protection Decontam-ination Procedure
The following describes the general decontamination proceduresfollowed by ERM for Level C Protection. These procedures areapplicable to Level D Protection with the exception of Step 8 -Respirator Removal.
Step 1 — Segregated Equipment Drop
Deposit equipment (tools, sampling devises, notebooks, mon-itoring instruments, radios, etc.) used on the site ontoplastic drop cloths.
Step 2 — Boot Wash
Wash boots with a solution of detergent and water.
Needed Equipment: Container (thirty gallons), decon-tamination solution (detergent/water), long-handled,soft-bristled scrub brushes.
Step 3 — Boot Rinse
Rinse off outside of boots.
Needed Equipment: Container (thirty gallons)/ high-pressurespray unit, and water.:
Step 4 — Glove Wash
Wash gloves off with a detergent/water solution.
Needed Equipment: Container (thirty gallons) and water/detergent solution.
Step S•— Glove Rinse
Rinse gloves off with water.
Needed Equipment: Container (thirty gallons), high-pressurespray unit, and water.
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Step 6 — Remove Outer Gloves and Boots Removal
Remova outer gloves and boots and deposit in a plastic-linedcontainer or store in designated area if not grosslycontaminated.
Needed Equipment: Container (twenty gallons) and plasticliners.
Step 7 — Tyvek or Coverall Removal
Remove Tyvek or coveralls and place in a plastic-linedcontainer.
Needed Equipment: Container (thirty gallons) and plasticliners.
Step 8 — Respirator Removal
Remove respirator and sanitize appropriate components.Discard cartridges after maximum of four hours use.
Needed Equipment: Table, soap, watar, container (5 gal),container with plastic linars (5-10 gal)
Step 9 — Inner Glova Removal
Remove inner gloves and discard into plastic lined con-tainer.
Needed Equipment: Container (5-10 gal), plastic liner.
Step 10 — Field Wash
Wash hands and faca.
Needed Equipment: Watar, soap, tables, and buckets.
4.7 Sampling Equipment and Sample Container Decontamination
All non-disposable sampling equipment will ba decontaminated withan Alconox/water solution followed by a clean water rinse. As anadded precaution against cross-contamination, all non-disposabla
4-7
The ERM Group
sampling equipment will be rinsed with distilled, deionizedwater. All disposable sampling equipment will be properlydisposed of in dry waste drums.
Before leaving the site, all sample containers will be thoroughlydecontaminated using an Alconox/water solution followed by aclean water rinse. The decontamination procedure should includea complete scrubbing of the container's surface to removepossible contamination. Care must be exercised to prevent damageto sample container identification labels.
All sampling equipment and sample containers will be allowed toair dry on a clean sheet of plastic.
4.8 Location of Nearest Hospital
The closest medical facility with respect to the Kimberton,Pennsylvania NPL site is the Phoenixville General Hospital. Thisfacility is reached by traveling east on Coldstream Rd., thennorth on Rt. 113, then east on Rt. 23. Total distance to thehospital is approximately 3*6 miles from the site. The route mapto the facility will be posted at the site throughout fieldactivities.
HR3QU554-8
ATTACHMENT 3
GROUNDWATER TECHNOLOGY, INCORPORATEDSTANDARD OPERATING PROCEDURES
TIM
AR30U56
E?GROUNDWATERTECHNOLOGY INC. Chakls Funl Wr.M. Rl. 1. Chadds Fim). IVnnsvlvania l<l.tl? I21SI .THS-Ufifi
STANDARD OPERATING PROCEDURES
FOR Rl RELATED FIELD INVESTIGATIONS
AT THE
KINMBERTON, PA SITE
JULY 1987
PREPARED BY:
GROUNDWATER TECHNOLOGY, INC.
Offic, ' "• •""•*•'•> «V»»«ia. Ohiii. CiiltffaJ". New V«rk. Calihimiii. Cimnccltcul.Vi. w. Texas. Pennsylvania. CanaJj »nd ChMc AR30 IUS7
INDEX
V^1.0 Well Drilling, Construction and Installation
A. Well Drilling Air Rotary Method - Equipment Cleaning
B. Well Construction and Installation
1. Well Construction for Monitoring Shallow WaterTable
2. Wall Construction for Monitoring Deep or SelectAquifer Zona(s)
3. Surveying and Locating of Newly InstalledMonitoring Wells
4. Well Development
W2.0 Equipment Cleaning Protocol
3.0 Sampling
A. Laboratory SchedulingB. Item CheckC. Sample Container Preparation
1. Preparation of Water Sample Containers forVolatile Organic Compound Analysis.
2. Preparation of Water sample containers for pH, TDSand chloride analysis.
3.1 Preparation for Monitoring Well Sampling
3.2 -Monitoring Well Sampling Procedures \_J
AR30U58
A. General Sampling Procedures for pH-TDS-ChloridesB. Sampling Procedures for Volatile Organic Compounds
Samples "
3.3 Labeling and Preservation Methods
A. LabelingB. Preservation Methods
3.4 Measures to Avoid Cross-Contamination of Samples
A. Well Sampling
4.0 Sampling Custody
4.1 Sampling Identification
4.2 Chain of Custody
5.0 Measurement of Various Field Parameters
6.0 Field Documents and Records
A. Field NotebooksB. Field Data Sheets
7.0 Generalized Health and Safety Plan
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1.0 WELL DRILLING, CONSTRUCTION AND INSTALLATION
A. Well Drilling Air Rotary Method - Equipment Cleaning
The drill rig and all drilling-related equipment willba steamed cleaned between borings to prelude thepossibility of equipment induced cross-contamination.Drilling wastes will be disposed of in an appropriatemanner.
B. Wall Construction and Installation
Monitor well construction and installation will be inaccordance with the described specifications for walldesign (shallow monitoring vs. deep aquifermonitoring).
1. Wall Construction for Monitoring Shallow WaterTable
Monitor wells designed to monitor the shallow watertable will be constructed of a clean and visuallyinspected 4" diameter threaded PVC casing and 4"diameter threaded PVC 0.020 slot wall screen. Noglua or cement will be used to connect PVCsegments. The PVC well screen will be capped atthe bottom with a threaded PVC cap. Tha sectionsof PVC will be assembled above ground and theninserted into an 8" - 10" diameter bore hole. Allbora holes will be drilled using air rotarymethods. To facilitate sampling and monitoring ofthe water table, well screens will generally extend20 - 30 feet below the water table and to within 5feet of the ground surface. The remaining wellwill be constructed of solid 4" flushjoint PVCcasing. A gravel pack (consisting of washed clasts
AR30U60
size 1/4 by 1/8 inch) will be installed from thebottom of the PVC well screen to a depth ofapproximately 3 feet below land surface.Wells will then be sealed from the surface by a 3foot annular seal comprised of cement/bentonitegrout. Wells will be finished with 6 or 8 inchsteel casing with a locking cap secured into thecement/bentonite grout (see Figure A-l).
The well utilized for aquifer pump testing will beconstructed in a similar manner to that describedabove, except that 8" diameter threaded PVC wellcasing and screen will be used. The well (#29)will extend approximately 50 to 60 feet below thewater table. The gravel pack and annular seal willbe as described above and the well will be finishedwith 10" steel casing (with a locking cap) securredinto the cement/bentonite grout.
2. Well Construction for Monitoring Deep or SelectAquifer Zohe(s).
Monitoring wells designed to monitor groundwater indeep or select zone(B) of aquifers will differ onlyslightly from those designed to monitor shallowwater-table systems. The installation will beexactly the same as the referred to in Section1.0.B.I except that 2" PVC casing will be used andwill extend into a select zone of interest. Theannular space between the casing and the bore holewall will be pressure grouted with cement/bentonitegrout along the entire length of the casing. A onefoot bentonite pellet seal will be incorporated atthe top of the gravel pack prior to cementing.Deep aquifer monitor wells will be screened fromthe bottom of casing to the bottom of the well,
AR30U6I
with a screened interval of no less than 20 feet.The annular space between the well screen and the \. Jwall of the bore hole will ba filled with gravelpack (see Figure A-l).
3. Surveying and Locating of Newly InstalledMonitoring Wells
OR'-''lr'£lVUi <_li»r>iNewly installed monitoirng walls will ba located (fcb)both horizontally and vertically by registeredsurvey crew. Well elevation will ba surveyed tonearest 0.01 foot and "tied" into the existingcoordinate system of tha USGS Datam (as surveyedduring previous wall installations).
4. Well Development
All newly installed monitoring walls will bedeveloped (pumping and purging of tha well bora)until water evacuated is clear.
2.0 EQUIPMENT CLEANING PROTOCOL
All well developement, in situ permeability, pump testingand sampling equipment will be cleaned and stored in anappropriate manner prior to use and subsequent to removalfrom the site.
Cleaning Protocol
1. Wash with alconox soap solution2. Rinse 3 times with tap water.3. Rinse with distilled watar.4. Allow for complete air drying.5. Wrap and store equipment in appropriate manner.
3.0 SAMPLING (SEE TABLE A-l FOR SUMMARY AND FLOW OF DATA)
A. Lab Scheduling
All sampling events to be conducted byGroundwater Technology, Inc. will be scheduled withthe analyzing laboratory to ensure that the lab canaccept the samples. The analyzing lab will be ORIGINALnotified at least two weeks prior to any sampling *'event. The laboratory will be informed of theapproximate number of samples to be collected, theparameters to be analyzed for, ad the anticipateddate and time of sample arrival.
B. Item Check
The following items will be checked prior to asampling trip:
1. Batteries of photoionization detector (PID) toassure that they are charged.
2. Any sampling equipment scheduled for use; to besure that the equipment is clean and in goodworking order.
3. Instrument calibration.
4. Any back-up systems; to be sure they are in goodworking order.
5. Sample bottle supply, to insure that an adequatesupply of clean sample bottles is available.Sample bottle preparation is discussed below.
6. a. Travel Blanks (one set for each set of samples
AR30U63
TABLE A - 1
SUMMARY OF SAMPLE AND DATA FLOW
GT contacts analyzing lab twoweeks prior to sampling to makearrangements for samples
GT collects watar and field data
Samples brought to GToffice to prepare themfor pick-up by theanalyzing laboratory
Samples collected byanalyzing laboratory
Laboratory analyzessamples
Analytical results sub-mitted to GT office
ORIGINAL(Red)
Fiald data submittedto GT offica
Data validated byQC officer
Data submitted toproject manager
Data submitted toclient & compiled forreport to RegulatoryAgency
AR30U61*
i^-^ o A waterproof pen
to be collected will be obtained from theanalyzing laboratory), to insure the integrityof the cleaning process, analysis andpreservation methods.
b. Field banks will be prepared on site at thetime the first samples are to be collected. ORIGINAL
(Red)Field sampling kits, to insure that all itemsnecessary to procure good, properly documentedsamples are present. A standard sampling kitwill contain the following items:
o Alconox soapo A jug of distilled water for rinsing hands and
sampling equipmento Disposable gloveso Paper towels
o Cloth labels for sample indentificationo A cooler with iceo Chain-of-custody formso Adequate supply of sample vials/containers
•*C. Sample Container Preparation
1. Preparation of water sample containers forVolatile Organic Compound Analysis:
Bottle type - 40 ml glass vials withteflon- lines septum caps (Pierce Catalog #13075or equivalent).
Cleaning procedure:
a. Wash caps, liner and vials with alconox
AR30U65
soap.b. Rinse liberally with tap water with a final
rinse of distilled watar.c. Dry caps and septa in oven at 105°C for
no more than 60 minutes. Dry vials in ovenat 105 C for a minimum of 60 minutes.
d. Cool in an inverted position in anorganic-frea atmosphere, and capimmediately. * C ''
2. Preparation of water sample containers for pH,TDS and chlorides.
Bottle type - 1 liter or largar narrow-neckedbottles with caps will be used to collect watersamples.
Detergent - Alconox soap to clean samplebottles.
Cleaning procedure:
a. Bottles and caps will ba washed in hot,soapy watar.
tb. Bottles and caps will ba rinsed five times
(or until soap suds and gone) with tapwatar.
c. Each bottle will ba given a final rinsewith distilled water. This means rinsingat least five times.
d. Bottles will ba drained and then cappeduntil used.
3.1 PREPARATION FOR MONITORING WELL SAMPLING
Prior to monitor well sampling, 3-5 volumes of water in
AR30U66
wells will be purged by either a Well Wizard purge system,an electric submersible Grundfos pump or a steel bailer.Stirring up of sediments in wells to be sampled will alwaysbe avoided. Once a well has been properly purged, samplecollection will follow the procedure outlined in Section 3.2
3.2 MONITORING WELL SAMPLING PROCEDURES
A. General Sampling Procedures - pH-TDS-Chloride Analysis
Wells will be sampled with a stainless steelbailer or Kemmerer sampler. Sample collection willproceed as follows:
1. Rinse a clean stainless steel bailer/Kemmerersampler at least five times with sample water.
2. Carefully pour/transfer sample water from thebailer/Kemmerer into a clean 1-liter sample bottleuntil full, then cap tightly.
3. Label the sample bottle with a cloth GTI label andwaterproof ink. Lables will include the followinginformation.
a. Sample identification numberb. Job identification numberc. Date and time of sample collectiond. Type of analysis requestede. Name of samplerf. Preservation, if any
4. Check to make sure the bottle cap is on tight,attach the chain of custody tags, then placelabeled sample bottle on ice immediatley.
AR30lli67
5. Fill out fiald data sheet.
6. The sample collected should be stored together withan unopened travel blank and fiald blank that hasaccompanied the sampler sine a the outset of thesampling avent. The sample sat and unopened blanksmust be stored together, under refrigeration.
7. Transport tha sample sat, on ica, back to thaoffica for pick-up by the anlysing laboratory.
B. Sample Procedure for VOC Samples (EPA Analytical Method624).
Tha sampling procedure for collecting VOC samples is asfollows:
1. Rinse a clean stainless steel bailar/Kremerarsampler at least fiva times with sample watar.
2. Carefully pour/transfer sample watar from thastainless steel bailer/Kemmerer into the samplevial, taking care to minimize turbulence, bubblingand time of exposure to air exposure to air. Filltha vial to overflowing. Watar should stand above .tha top of the vial (i.e., there should be a convexminiscus above the neck of the vial).
3. Carefully but quickly slip tha cap with septum ontotha vial with the teflon face of tha septum towardthe water. Tighten the cap securely, invert thevial, and tap the vial and tha cap against yourhand to asssura that there are no bubbles inside.If bubbles are present, open the vial, add a fewmore drops of sample water, and reseal.
4. Collect a duplicate sample.
5. Label the sample vials using cloth GroundwaterTechnology Inc. labels and water proof ink. Labelswill include the following information:
a. Sample indentification numberb. Job identification numberc. Date and time of sample collectiond. Type of analysis requestede. Name of samplerf. Preservation, if any
6. Check to make sure the vial caps are tight, attach....,,.C ft .'.:•••
the chain-of-custody tags, then place the labeled /p^Lsample and duplicate on ice immediately.
7. Fill out field data sheet.
8. The samples collected should be stored togetherwith an unopened travel and field blank that hasaccompanied the sampler since the outset of thesampling event. The sample set and unopened travelblanks must be stored together, underrefrigeration, in an area known to be free ofcontamination from solvents and other volatiles.
9. Transport the sample set, on ice, back to theoffice for pick-up by the analyzing laboratory.
U AR30U69
3.3 LABELING AND PRESERVATION METHODS
A. Labeling
Labels will be applied to sample vials at the time ofsample collection. The standard sample label used byGroundwater Technology, Inc. is a white cloth label.Information will ba written on labels with a blackwaterproof ballpoint pen, and will include tha sampleID number, the job ID number, tha data and time, thetype of analysis requested, the sampler's name andpreservation. Labels will ba positioned on samplevials so that they ara easily seen and so that they donot coma off if the vials ara wet for a prolongedpariod of tima. All sampling equipment that must bareused at later times will ba labeled after each usefor decontamination procedures. Information to bawritten on sampling equipment labels will include thadata used, tha sita and/or wall number, and thainitials of the sampler.
B. Preservative Methods
1. Watar Sample Preservation
•Samples will ba maintained on ica or refrigeratedat 4°C until they are analyzed.
3.4 MEASURES TO AVOID CROSS-CONTAMINATION OF SAMPLES
A. Well Sampling
All equipment will have been cleaned prior to arrivalon site. Measures taken to avoid cross-contaminationin well water samples will include the following:
AR30U70
complete all necessary information, using a blackwaterproof pen, as follows:
A. Tha Sample ID Number will be tha number assigned tothe particular sampling station.
B. Tha Sample Source will ba the name of the site.
C. The Analysis Required will ba indicated for eachsample.
D. Date taken will ba the data the sample was collectedusing tha format MM-DD-YY.
EXAMPLE: 08-15-86
E. Time will be the time the sample was collected.
EXAMPLE: 1430 or 2:30 p.m.
F. The sampler's name will be printed.
G. Preservation typa.
4.2 CHAIN OF CUSTODY
A. A chain-of-custody will be completed for each set ofsamples. Laboratory personnel preparing tha samplecontainers will initiate the chain-of-custody bysigning tha first "Relinquished By" line at the bottomof the chain-of-custody record indicating tha date andtime of transfer. Samples and/or sampling containerswill not leave the custody of the person receiving themuntil relinquished to another party. Custody is definedas:
flR30U72
1. In the actual physical possession oflaboratory/field personnel.
2. In the laboratory/field personnel's view afterbeing in physical possession.
3. In a locked area after being in physicalpossession.
4. In a designated, locked storage area.
Transfer of samples to the anlyzing laboratory willbe done by use of'common carrier. Carrierpersonnel will pereonnally secure samples andsample contianers in such a way that no containerscan be opened in transit. The person to whom v>custody is being transferred will sign on theappropriate "Received By" line of thechain-of-custody record, indicating that custody isbeing accepted by the carrier for all the sampleslisted in the sheet. For subsequent transfers ofcustody, the succeeding relinquish and receiptlines will be Used.
Upon arrival at the laboratory, the samplecustodian at the lab is responsible for maintainingpossession of the chain-of-custody samples and formaintaining all records, documenting thatpossession. Upon receipt of samples, the samplecustodian signs the shipping report accompanyingeach sample and records the date and time. All ofthe logging procedures are performed for eachsample by the custodian. The samples are thensecured under lock and key in refrigerated storage.
15 AR30U73
5.0 MEASUREMENT OF VARIOUS FIELD PARAMETERS
During select field activity (liquid level monitoring,permeability tasting, pump tasting, sampling), it willbe necessary to measure various parameters in tha fiald.
o pH will ba measured using a properly calibrated pHmeter.
o Temperature and specific conductivity will bemeasured using a YSI modal 33 S-C-T mater.
o Organic vapor levels will be measured using ahNu modal 101 photoionization analyzer, calibratedto Benzene using an 11.7 EV bulb (Factory ,,.,,.calibration at 100 ppm). ^ ,.- ,
' ' ' Sro Liquid levels will ba measured using an Oil
Recovery Systems' interface probe.
o All field values will ba recorded on appropriatefield sheets.
6.0 FIELD DOCUMENTS AND RECORDS
A. Field Notebooks
All field measurements will be recorded in boundfiald notebooks (Lietz brand transit fiald book no.8152-00 or equivalent). All pertinent calibrationdata for each day's work will ba assigned fieldnumbers which will ba recorded in tha fialdnotebook as well as on sample vial labels and on
field data sheets. Each page will be signed anddated.
B. Field Data Sheets
Data sheets will be compiled for field activities.The data will be recorded with a black waterproofpen. Information to be recorded on field sheetsincludes:
1. date(s)2. time(s)3. location4. project number5. type of field activity6. sample ID number (and type of sample)7. source of sample (well, pond, etc.)8. pertinent well data (pH, temperature, conductivity
flow rate, liquid level measurements).9. pumping method (for well samples)10. field parameters measured11. personell names (and signatures)
7.0 GENERALIZED HEALTH AND SAFETY PLAN
Groundwater Technology, Inc. general operating proceduresare based on EPA and OSHA cirteria. A site health andsafety plan is to include the use of latex or rubber workgloves, protective clothing, footware, and head gear.
Protective eye wear and organic vapor masks will beavilable if needed during site activities. Aphotoionization detector will be used for on-site screeningof ambient air conditions (i.e., around drilling rig shouldvolatile vapor levels require the use of organic vapormasks). Continuous screening of ambient air conditions
AR30U75
will ba conducted during the anticipated pump tastingprogram. All personnel within close proximity to tha watartreatment air stripping tower utilized for the pump tastingprogram will follow suitable on site health and safetymeasures (i.e, organic vapor masks).
A list of all emergency numbers including police, firedepartment, hospitals and key facility personnel will baon-site at all time.
AR30U76
LOCKING CAP ON 6-8"STEEL CASING -v A D ^^ LOCKING CAP ON 6-8" STEEL CASINGerr i torn IM rruFWT/ \ **____ ________^**^ SFTiiprn IM CFUPMT/nrMTnMiTrSECURED IN CEMENT/BENTONITE GROUT
6 MINIMUM OF-BENTONITEPELLETS
WELL SCREENSET TO WITHIN5' OF GROUNDSURFACE
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FIGURE A-lTYPICAL MONITORING WELL DESIGNSFOR MONITORING SHALLOW (A)AND DEEP (3) AQUIFER ZONES
19
ATTACHMENT 4
INSTRUCTION MANUALS FOR PH AMDCONDUCTIVITY METERS
O
AR30U78 ——_,
ANALYTICALBIG SCALE pH Meter
-Model 7O7-B
Operating Instructions
~l iiaujilcatI «Ui«« till 11. «•«!••«. Bit II t|| I (till
AR30U79
ANA. *'ICAL BIG SCALE pll HETKR. HOUEL 70 7- B
Operating Instructions
Set "Selector1* Switch to "0" position. Rotate"Calibrate1* knob clockwise and counterclockwise endobserve pointer lavement. Pointer should move freelyup and down scale as knob is rotated. Then seepointer to 7 pH with "Calibrate** knob.
Remove sample cup from Probe and rinse Probe indistilled or delonixed water. (If neither isavailable then rinse with Up water.)
•
Immerse Probe Unit in a beaker of 7 pR buffersolution. Turn Selector Switch to pH. RotateCalibrate knob until pointer reads 7 pll.
Rinse Probe Unit under tap water or in a* vessel ofclean water, snd immerse into s besker of 4 pH buffersolution. The meter should now read 4 pll. .
Rinse Probe Unit and instrument is now ready to teatrequired samples.
Turn Selector Switch to'o position and note reading. .This is important* (If Calibrate knob is inadvertentlyrotated during later testing, it would not be necessaryto to .through Steps 3 and 4 «gein.) Reset pointer bymeans of Calibrate knob to value noted above withSelector Switch in 0 position.
Turn Selector Switch to pll. Set Temperature dial totemperature of sample under test.
When finished with samples,, rinse Probe, replacesample cup end fill sample cup with water -to keepbulb moist.
Turn Selector Switch to "Off". •
To replace b'ttery, remove back of meter (4 cornerscrews). Remove old battery, snap on new battery,place in clip and replace, back. Use a standard9 volt Transistor Radio battery available locally.
AR30|l»80
.>,
ANALYTICAL pll PROBE UNIT
This Probe Unit is of a new type requiring no refillingwith KC1 solution. This ia accomplished with gel fillingand * ceramic junction. The Probe Unit must be ismrsedabove the top of the cup holder in order to make connectionwith the ceramic junction in the body of the electrode.
Clou P«Jy«ihrltnt
HomfltHolder
Coo.Cobl.BNC Conntctor
AR30U8I
N8TRUCT,ONS F ORVS, MOOltAND 33M 8-C-T METERS
AR30U82
TABLE OF CONTENTS
GENERAL DESCRIPTION . .... .. . . 2SPECIFICATIONS. ....... . . . ... 2OPERATION PROCEDURE .... . . . . 4
t Sltup . ............ .. 42 Ttnwtttift . ........ . 61 SMmuy ... 154 Conducunct .... . . . , ' SS itiot . . . . . 6
CIRCUIT DESCRIPTION MAINTENANCEA N D CALIBRATION . . . «t D««CIIC»«A . . . . . . 92 M«4lM«MftCt . . . . . . . . . 9
3 C«MM*HOA .... . 9PROBE ... . . 12
t OMCI<MIOA ol VSl 3300 ConduetwitT/Ttmptraiuf* P«obt 122 MttnicMAci . . t23 PlObt UM ' ; 14
• 4 Ctl C«bbut«n i Slind*id Solwtiont UYSI MODEL 33 AND 33M USED WITH YSt StA. S4 AND ST .OXYGEN METERS tft
WARRANTY ..... . .................... . . 21
AR30U8*
tiiifSi* IPs*•Hi IS B
AR30U85
»: ? 2 lit
AR30U86
13) SaluulvTh* salinity itadmos ara a function of tamptratuta andconductivity, thatalora tha accuracy « • function of both.The tamper atura tcafe and tamperMura control htv« btondmgnad to awwmit tht umpcfituti tnot contnbution tothe Mkraty enot. The *nof shown in f toura 3 it tht total ofth« ttmpttcttwt *ntf condwctwitY prob*. th« umpmtori»cait and the tatawty teal* ecior.
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AR30U88
CIRCUIT DESCRIPTION. MAINTENANCE AND CALIBRATIONt. Description ,•Tha circuit is composed of two parts, a multivibrator and switchingtransistors Tha multivibraior produces a square waveform voltage.Tha square wave is applied to two switching transistors They alter-nately apply two taiteries of opposite polarity to the probe thusproviding AC power which nurumaes poiantanon effects. The meteris in series with one battery and measures the current from it. Thecurrent from the battery is proportional to the conductance of the eel.Sakmfy is measured in a special range conductivity circuit which in*eludes a user-adjusted temperature compensator. In the temperature.fedbne and XI positions the multmbrator operates at 100 H* In thesalinity. XI00 and X10 positions the multivibrator operates at 600 H*and m these ranges pushng the CELL TEST button drops the frequen-cy 10 100 Hi atowmg the operator to judge the degree of probepolarisation2. MaintenanceThe only maintenance required is battery replacement Two "0" siteafcahne flashlight cent, such as Eveready EflS or equivalent. w«provide 200 hrs of operation Accuracy will not be mamtatfted if tine-carbon "0" cats ara used Battery replacement«indicated when theredbne adjustment cannot be accomplishedReplace batteries every s» months to reduce the danger of corrosiondue to leaky batteries To replace batteries, remove the su screwsfrom the rear plate The battery holders are color coded The PositiveIt button) end must go on red.J. Calibration of Model 33 (Model 33M date ere in parentheses.}It is possible for the temperature Inob to become loose or sk> fromMS normal position In an emergency the dial CM be re-positioned. Itmust be emphasited that this is an emergency procedure only, andthat the instrument should be returned to the factory tor properrecakbration at the earliest opportunity.
AR30U89
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AR30U9I
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AR30U93
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