Document x5G30XK4wJvBK1v6g5vpK5GGE
.. S4EH/ESC TCo. /Di v77TJept, A6ca t f on I
REPORT NO.: MSL-5738 ESC-UAG-86-46
J08/PR0JECT NO.: 6405 DATE: May 30, 1986
TITLE: ANALYSIS OF LULING SAMPLES AUTHORS: S. Gibson, S. Walker and R.W. Noble
ABSTRACT: Samples from Lullng were received for the analysis of PCOOs, PCOFs, 2,3,7,8*TCDO, metals, acid and base/ neutral extractables, pesticides and Aroclor formula tions. This report gives the results of these analyses.
rlrihennJ^X`" TECHNICAL APPROVAL:
Environmental Sciences Center Senior Research Group Leader APPROVED BY: Environmental Sciences Center Quality Assurance Specialist
APPROVAL DATE: ^ :3CJ
T lT t t : ANALYSIS OF LULING SAMPLES
rept n o e s c ^ A G - 8 6 -4 6 AUTMORS: S G ib s o n * S H a ,tte r and R w - M ob,e
copy no Q
r iobsiiv:
COMPANY CONFIDENTIAL
This documeni is the property of Monsanto Company and the recipient s responsible for its safekeeping and disposition. It contains CONFIDENTIAL INFORMATION which must not be reproduced, revealed to unauthomed persons or sent outside the Company without proper authontation
HONS 220937
D1ST RIBUTI O N
COPY NUMBER
]. L. Adams - 1560
2. S.D. Gibson - U4F
3. S.A. Walker - U1F 4. R.W. Noble - U1F 5. W.M. Mees - U4D 6. P.L . Sherman - LfLF 7-9 Reports Library - R2C 10. Chesterfield Information Center - AA3A
ABSTRACT ONLY
H.A. Woltemiann * U4E
COMPANY CONFIDENTIAL
This report hat been assigned to you. When it is no longer needed, vop are responsible for returning it to
i' vOu transfer it to anyone else, please let your librarian know, so the records can be changed.
* 1011X1 <*(v WIO!
HONS 220938
ANALYSIS REPORT
CATE: 22. May 1986 LOG NUMBER: U-86-03-14-01
PROJECTS NUMBER: 64 05 NOTEBOOK PAGE? 3353290
10:. L. Adams/ 1560
cc FILES/Mees P. Sherman
R. Noble
Title: Analysis of Luling Samples
Procedure: See attached report
Abstract: Samples from Luling wsre received for the analysis of PCDDs, PCDFs, 2,3,7,8-TCDD, metals, acid and base/neutral extractables, pesticides and Aroclor formulations. This report gives the results of these analyses.
Analysts: S. Gibson, S. Walker and R. w. Noble
ANALYST APPROVAL: RoykJ* Noble Senior Research Chemist
1 MONS 220939
ANALYSIS REPORT FOR LULING SAMPLES
INTRODUCTION
Nine eolla, two sediments and four wipe samples were received for
selected analyses of polychlorinated dibenzo-p-dioxins (PCDDe),
polychlorinated dibenzofurans (PCDFs),
2,3,7,8-tetrachloro
dibenzo-p-dioxin (2,3,7,8-TCDD), selected metals, acid and
base/neutral extractables, pesticides and Aroclor formulations.
The metals, acid and base/neutral extractables, pesticides and
Aroclor formulation analyses on samples 157 and f5 were performed
by Environmental Testing and Certification Corporation (ETC) of
Edison, NJ. The PCDD, PCDF and 2,3,7,8-TCDD analyses were
performed in our laboratories. For internal purposes the samples
were assigned Log number u-86-03-14-01. For quality assurance in
the analyses we performed MRC Method I07-QAQC-R3 was followed.
Briefly this method requires that for every set of samples of the
same matrix type a replicate sample, a low spiked sample, a high
spiked sample and a method blank must be analyzed. The reports
for the analyses performed by ETC are attached at the end of this
report.
PREPARATION AND ANALYSIS
Soil and sediment samples of 10 g were weighed and spiked with appropriate Internal standards. Wipes were spiked with carbon-13 labeled 2,3,7,8-TCDD prior to extraction. Then 15 mL of methanol (all solvents are Burdick and Jackson "distilled in glass" grade) and 150 mL of hexane are added. The samples are then shaken for 3 hours on a wrist action shaker and the hexane is decanted off. The hexane extracts were washed with 40 mL of concentrated sulfuric acid (untill clear), 30 mL of water and 40 mL of 1 M potassium hydroxide and 30 mL of water. The hexane was dried over sodium sulfate and concentrated to 3 mL.
The samples were then placed on the head of a mixed phase liquid chromatographic column consisting of (top to bottom) 2 g of silica, 4 g of silica plus 40% sulfuric acid, 1 g of silica, 2 g of silica plus 36% potassium hydroxide and 1 g of silica. The column was eluted with 50 mL of hexane which was subsequently concentrated to 3 mL. The hexane was then placed on the head of a column containing 2.5 g of Woelm basic alumina. This column was first eluted with 10 mL of 2% methylene chloride/hexane (v/v) mixture and this fraction discarded. An additional elution was made with 15 mL of a 50% methylene chloride/hexane (v/v) mixture to elute the pCDDs and PCDFs from the column.
For some of the samples it was necessary to conduct further cleanup using the EPA Option D technique in order to analyze for TCDDs. Option D involves placing the sample on top of a column containing 18% Carbopak C on Celite packed to a depth of 2 cm in
2
HONS 220940
a 1,0 cd ID pipet. The column was than aluted with 1 mL of hexane, 1 mL of 1:1 cyclohexane/methylene chloride, l mL of 75:20:5 methylene chloride/methanol/ben2ene and finally 2 mL of toluene. The toluene fraction was collected to be concentrated.
All samples had 50 uL of dodecane containing tribromobiphenyl as an internal standard added to the eluant as a keeper and were then concentrated to 50 uL under a gentle stream of purified
nitrogen and were submitted for GC/MS analysis. The GC/MS
analysis was conducted on a Hewlett/Packard 5987 instrument. The mass spectrometer was operated in' the selected ion monitoring mode analyzing for ions characteristic of the native (unlabeled) PCDDs, PCDFs and the internal standarde.
RESULTS
The results of the analyses are given in Tables 1-5.
Results
are not corrected for recovery for the PCDD and PCDF analyses in
Tables 1 and 3. Replicate analysis results for sample t 5 show a
large variability due to the presence of shells in the sample
causing homogeneity problems. Discussion with the customer
determined that these results met their needs.
MQNS 220941
Table 1. PCDD RESULTS FOR SOIL AND SEDIMENT (in ppb)
Sample
Cl-4
Cl-5
Cl-6
Cl-7
Cl-8
Background ND ND ND 0.4 1.2
Soil <5
600 0.7 3.3 1.5 3.1
Soil is R
7500
ND
2.2 5.3 6.9
Soil 113
0.9 ND
3.6 30 190
Soil 127
2.1 ND ND 0.4 1.5
Soil 135
0.7 ND
0.7 1.5 21
Soil #39
0.8 ND
0.8 1.6 16
Soil 51
ND ND 0.4 0.6 1.5
Soil *51 K % recovery spike level
10.1 107%
9.4
19.1
170% 11.4
11.6 103% 10.9
11.3 91%
11.8
11.9 109%
9.5
Soil |57
5.2 ND
1.4 0.8 1.4
Soil <59
4.8 ND
4.0 ND
0.2
Sediment #1
ND
ND
3.0 36 160
Sediment (1 L
1.1
1.2
3.5
29
104
% recovery
110%
100%
-a
-a
-a
spike level 1.0 1.2 1.1 1.2 1.0
Sediment #2
18
0.3 8.0 89 420
BLANK
ND ND ND ND ND
MDL
0.5 0.5 0.5 0.5 0.5 MDL method detection limit ND none detected at method detection limit ft replicate sample L,H low and high spiked samples a
spike recovery can not be calculated as sample is three times the spike level.
4 HONS 220942
Table 2. REPEATED RCDD RESULTS FOR SEDIMENT | 2 (in ppb)
Sample
Cl-4
Cl-5
Cl-6
Cl-7
Sediment # 2
15
ND
20 127
Sediment | 2 R 13 ND 22 156
BLANK
ND ND ND ND
MDL
0.5 0.5 0.5 0.5 MDL method detection limit
ND none detected at method detection limit
R replicate sample
Cl-8 1000 1500
ND 0.5
5 HONS 220943
Table 3. PCDF RESULTS FOR SOIL AND SEDIMENT (in ppb)
Sample
Cl-4
Cl-5
Cl-6
Cl-7
Background ND ND ND ND
Soil #5
3.9 1.4 3.8 0.9
Soil #5 R Soil 113 Soil #2?
4.9 3.5 5.4 1.2 0.2 2.6 4.2 0.9 ND ND ND ND
Soil 135
ND ND <0.9 0.4
Soil #39
ND ND <0.6 0.4
Soil #51
ND ND ND ND
Soil #51 H % recovery spike level
5.0 37% 13.6
25 84%
29.4
32 64%
49.7
8.1
76% 10.7
Soil #57
ND ND ND HD
Soil #59
ND ND ND ND
Sediment #1
0.2 <1.6
<1.9
0.6
Sediment #1 L
0.7
4.7
4.3
1.0
% recovery
46% 100% 82% 90%
spike level 1.0 1.2 1.1 1.2
Sediment #2
<0.6
<6.2
<22
1.9
BLANK
ND ND ND ND
MDL
0.5 0.5 0.5 0.5 MDL method detection limit HO none detected at method detection limit R replicate sample L,H low and high spiked samples
Cl ~8
ND
0.8
1.1 2.4 ND
0.9
1.0 ND
33 93%
35.3
ND
ND
2.4
5.3 81% 1.0 5.5 ND
0.5
6 MQNS 220944
Table 4 2378-TCDD RESULTS FOR SOIL AND SEDIMENT (in ppb)
Sample
2378-TCDD
gpb Added
Background
ND
Soil 15
510
Soil 15 R
7000
Soil #13
1.8
Soil #27
1.6
Soil #35
0.9
Soil #39
0.7
Soil #51
0.1
Soil #51 H
8.2 9.4
Soil #57
5.2
Soil #59
2.6
Sediment #1
ND
Sediment #1 L
1.0
1.0
Sediment #2
16.5
BLANK
ND
MDL
0.2
MDL method Hetection Unit
ND none detected at nethod detection limit
R replicate sample
L,H low and high spiked samples
?
HONS 220945
Table 5. 2378-TCDD RESULTS FOR WIPES (in ng)
Sample
2378-TCDD
ng Added
Auger 1 Bit
ND
Auger 1 Handle
ND
Auger 2 Bit
3.4
Auger 2 Handle
ND
High Spike Low Spike
Blank
44
4.3 ND
48 4.8
HDL
0.3
method Hetection limit
none detected at method detection limit
8 HONS 220946
[HVIHOHMtNiAL ZESTING <></ CEXriF'CAllUri
Technical Report for
MONSANTO COMPANY 800 N.LINDBERGH BLVD.
R3B ST.LOUIS, MO 63167
Cfla/n ar CviMy 0t( Htqtilttd r*t VC Dart
Aummtry Atoa/ta
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MONSANTO COMPANY 1 cwa^a/iy
MONCQftPCNQ 16*314 Ptalilty____ 4/tii/a Point can rim* ^HeurV*
Viea Praiftfarrc ft*farcfl a/>9 opi/w/an*
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HONS 220947
f NVItQHMf nr At.
C I s* Tf tTINQ tna CtfiTIFtCAr/QH
TABLE OF CONTENTS
Introduction Tibia t Raauita and Quality Atturanci Oita Tibia Mathod Pirtormanca Data Mathodotogy Qa Protocol Rapori Appandicaa
Appandlx A * Man Spactrai Data lor Quantilatad Compound! Appandlx Cl - QC/MS Subaldiary Data - Blank Chromatogram! Appandlx E - Chain of Cuatody Forma
MONS 220948
CNVIfiONMiNTAl | V Tf ST/N0 CiKUFlCATlOH
Introduction
This reoort contains the analytical results on your soil sample, 5 66/03/14 it is designed to include comprehensive data irom tne entire analytical process in order to satisfy the neeos of various levels of review The results obtained from your sample are presented in tabular format immediately following this introduction. Quality assurance date <s tabulated along with the appropriate eampie results for verification Depending on the analyses ordered, the duality assurance data may include results from blank, spiked Pienk. spiked sample (i.e matrix spike) end replicate sample as we as results from surrogate compound analyses Quality assurance data for verification of proper instrument performance is also Included where appropriate The report appendices include the chain of custody record for your sample and. whare appropriate the gas chromatograms and mass spectra The procedures used in the analyse of the sample ere described in this report $ methodology section Ail analytical procedures within our laooratory are performed within a strictly enforced Quality Assurance Protocol a description of ins Protocol la included in the report
Results
Semple results, and associated duality assurance date, are always tabulated in one or more of this report's Quantitative Results Tables The format of each table vanes with the class of analysis Priority Polluttnt* The priority pollutant compounds and elamants are listed with their NPDES (National Pollution Discharge elimination System) numbers, and the Method Detection Limit (MDL) published m the
Federal Register When e compound or element is present below its published MDL it is
reported as BMDL (Below Method Detection Limit). When e compound or element is not present at any detectable concentrations it is reported ss NO (Not Detected) mdl'i for non-aQueous matrices are based on USE pa published MDL's but are adjusted as per sample weight Matrix spike end replicate analyses, where included, were performed on samples randomly chosen within each quality assurance batch end are therefore not necessarily spikes end replicates of this report's sample Surrooata compound recovery date end instrument calibration date ere included in the Method Performance Date Tables
HONS 220949
ttHIMO tnt CtMine Alton
TABLE 1: QUANTITATIVE RESULTS and QUALITY ASSURANCE DATA Add Compounds - GC/MS Analysis Data (QR02)
apr i itte
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RONS 220950
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TABLE 1: QUANTITATIVE RESULTS and QUALITY ASSURANCE DATA BASE/NEUTRAL COMPOUNDS - QC/M$ ANALYSIS DATA (OR03)
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HONS 220951
ETC tMYlAOHktfHTAl Tiit WO CtAltnCAtrOH TABLE 1: OUANTtTATIVE RESULTS and OUAHTV ASSURANCE DATA
APR mt
BASE/NEUTRAL COMPOUNDS - GC/MS ANALYSIS DATA (OR03)
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HONS 220952
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TABLE 1: QUANTITATIVE RESULTS and QUALITY ASSURANCE DATA Priority Pollutant Matala - Analysis Data (QR05)
Ctato < 6wi*#t Pill **<** 4m |TC Nti
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HONS 220953
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_________ ,,.,,_ __ ,, ___-_-_-_---_-_-_--____
TABLE 2: METHOD PERFORMANCE DATA Surrogate Recovery Soli - GC/MSData (OR20)
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HONS 20954
II
TABLE 2i ttETHOO PERFORMANCE OATA (QR22>
GC-'flS Tuning Data - Dae* f luorot f tphany Iphoap in# (DFTPP) for Act da Anaiyai
m/'z
Ion Abundane* Cr I tar I#
* Ralatiua Abundane*
Baa#
Appropriate
Paah
Peak
Statue
51
68 69 70 127 197 196 199 2 75 365 441
442 443
30-60* of Mtl 198
Laaa than 2* of maaa 69
(r#f#r#nci on ly )
L#a* than 2* of maaa 69
40-60* of
198
Laaa than 1* of maaa 198
Baa# paah , 100* ra la 11 V* abundance
5-9* of maaa 198
10-30* of lMt 198
Greater tlnion 1* of maaa 198
0-100* of t 443
Greater than 40* Of <moot 198
17-23* of mo a 442
48 .32 .95
52 .22 .23
47 .25
0 . 00 100 .00
6 .94 20 .47
2 .33 9 . 10 55 . 89 10 .99
.48.32 1.81
52.22 .43
47.25
0. (JO
100.00 6.94
20.47 2.33
82.74 55.89 19,a7
Ok Uk Ok Clk Qk
Uk Ok Uk Uk
Uk Ok
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Run Nol Spactrun Not
03'31'86 141 59 > I >662 662
AnalyatI Proeeaaor t
QC Bateht Samp la* t
HONS 220955
*r *-ni>csis fte ST
19#
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TABLE 2i METHOD PERFORMANCE DATA (QR27)
C/HS m/*
Tuning
D#t - Dacafluorotriphanylphoapina tDFTPP) tor Basi/n#utrai
An#lya l a
5 Ralatiwa Abundance
Ion Abundance
Baaa
Appropr tat a
Cr 11# r i
Paak
Paak
Status
51 69 69 70 127 197 190 199 275 >65 441
442 447
70-605 of m## 190 L### tnn 25 of meae 69 (rafaranca only) Laaa than 25 of mama 69
40-605 of maaa 196 Laaa than 1% of maaa 190 Baaa peek, 1005 ra)aiivi abundance 5-95 of maaa 190
10-705 of maaa 190 Sraatar than 15 of maaa 190 0-1005 of maaa 447 Greeter than 405 of ma#a 190
17-275 of maaa 442
50.74 0.00
52.21 .26
40,40 0. 00
100.00 7.72
22.40 2.47
10.56 74.07
17.75
50.74 0 00
52.21 50
4B 60 0 . 00
100.00 7.72
22.40 2.67
74.75 74.07
IB.57
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04/01/94
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HONS 220956
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Methodology
tor
OC/MS Analysis of Priority Pollutant Compounds
The methods employed in the GC/MS analysis tor priority pollutants are astaoiisned Epa methods Rigid compliance with the instrument parameters and performance criteria o* the puoiished methods was achieved in some cases the precise amounts of sample used ana the sampie handling procedures vary with the complexity of the sample matrix Qualitative identification ot the priority pollutants was performad using the relative retention times the relative abundance of three characteristic ions end the abundance ratios The entire mass spectrum was reviewed to confirm each identification. Quantitative analysis of detected compounds was performed by using response factor generated by a major characteristic ion of the specific compound end an internal standard
Compounds, m addition to those on the priority pollutant list, were Identified through a computer-aided search of the NBS-EPA spectre library After review the identifications are included in a separate tabulation and labelled 'tentatively identified'
Adi Illl/Nli/irtl and P**tlcld* Priority Polluttnt Compovngt
For the analysis of tha Ac>d. Basa/Neulrai and Pesticide priority pollutants in a soil matrix a modification of EPA Method 625 was used The method can be summarized $ foi'ows A 30 gm semi-wet soil sampie is soxhiet extracted with U mixture of acetone end hexane The acetone is thermally stopped The remaining hexana axtract is diluted to 200 mi w<th methylene chloride end twice extracted with en eoueous NeOH solution followed by an extraction with deionized waiar. The methylene chloride extract is dried end concentrated io a t mi final voiuma This concentrate is injected inlo GC/MS instrument configured for the analysis of Base/Neutrai priority pollulant compounds The remaining aqueous extracts ere combined and the pH edjusleo to a value less than 2 Tha eoueous phase it serially extracted with 3 aiiQuots of methylene chloride The methylene chloride extracts ere dried concentrated to a 1 mi final volume The concentrate is mjecled into e GC/MS instrument configured for the eneiyeie of acid extractable priority poltuleni compounds
HONS 220957
VENTAL no CERTIFICATION
Methodology for
Analysis of Metals
AQUfOUS
The determination of metais in aqueous samples is performed according to the methods puonshed Dy pa m "Methods for Chemical Analysis of water end wastes" Epa-600/j-79-C30 March 1963 and the Federal Register, October 26 1983 Arjenic selenium and lhaiiium are determined by furnace aa, silver, aluminum tarium Deryiiium torom cadmium, caicium chromium cooper coba<1. iron, megnesiurn, manganese, moiyDdenum mpt-ei lead sodium, antimony tin, tiianium. vanadium, and line ara determined by icp emission speclrometry, eveebi where lower levels of detection ere reomred m these cases fag lead m groundwater monitoring samples) turnece aa is used ak furnace aa parameters are run cy method ot standard additions The determination o< mercury is performed Dy coio vapor aa EP tox/c/ty The determination o< metals m aqueous EP Toxicity leachates it performed according to me methods published by Epa <n "Test Methods 'or Evaluating sot'o wasta" EPa sw-sa6 revised April 1964 end the Federal Register. Oct 26 1963 1979 Silver, arsenic parium, cadmium chromium lead end selenium ere determined by iCP emission epectromelry Mercury is determined usmg coid vapor aa For leachates that ere organic in nature, the analyses are performed according 1o the methods described under oil/sluOoe below tOU/SEOlMENT The determination o< silver, beryllium, cadmium, chromium copper, nickel, eniimony, lead and line in sediment samples is performed according to methods published Dy EPa in "interim Melhods for tha Sampling end Analysis of Priority Pollutants in Sediments end Fish Tissue" EPA 600/4-81-055. October i960 Mercury is determined according io the sediment method published by EPA In "Method tor Chemical Aneiyets of water end Wastes', epa 600/4-79-020 March 1963 Arsenic, selenium end thallium are determined by furnace aa using mine add in a closed decomposition vessel for eampie digestion Ott/SLVCXiE The determination of silver, aluminum, boron, barium, beryllium, calcium cadmium coooer. chromium cobalt iron, magnesium, manganese, molybdenum, sodium, nicke< lead, antimony tm titanium, vanadium, end line in siudge/petrolsum-besad eamples le performed by icp amisson spectrometry using e magnesium nitrate dry ashing digestion technique Arsenic, seienium and thallium are determined by furnace aa using mtnc eod m a closed decomposition vessel <or sample digestion Mercury is determined by cold vapor aa using the same digestion tschn>Que
HONS 220958
CTA tNvmONUtNT al Civ Tf stina ntf ce^nncAHON
Summary of Quality Assurance/Quality Control Procedures (QA/QC)
Etc oases its quaiiiy assurance protocols on the following govammeni guidelines
'Handbook tor analytical Ouaiity Control m Water and Wastewater laboratories'. Epa-600/4-79-0i9. March 1979,
National Entorcemant investigation Center Policies, end Procedures manual. E PA-330/9/79/001-R October 1979,
the recommended guidelines for EPA Methods 624 end 62S (Federal Register December 3 1979 uboatao on Oclober 36.19841,
'Manual of Analytical Methods for the Analysis of Pesticides in Humans and Environmental Samples.' Epa 600/8-80-038, June 1980,
'Oelerrmnation ol 2,3 7.8-TCDO m Soil and Sediment' EPA, Region vii. Kansas City. September 1963.
Organic Analysis Multi-media. Mutti Concentretion-iFB WA64-A267. and
Dioxin Analysis Sod/Sedimeni Matrix. Muiti-Concenuation, Selecled ion Monitoring with jar Extretion Procedure-lFB WA64-A002
However, we have modified our protocols to provide a higher level of Oa/OC than the guidelines require For example, we analyze e higher than required number of duality conlroi samples and we pay especially careful attention to the certification of the `reference standard* compounds we use m analysis Below are listed the key QA/QC elements for me methods we used
Analysis ol Volatile Offisnic Coropounde by Gee Chromatography/Meat Spectrometry
- Each batch of 13 samples consists of 9 customer samples (at t maximum) one blank
sample, one spiked blank, one tpikad sample and one rapiicala sample This amounts to a 30% quality control lector
- Three surrogate compounds ere added to each sample in the batch of i3
- a bimd duality control sample is introduced to the laboratory tor analysis on a weekly bas<s
- Each GC/MS is checked andratuned. it necessary, at the beginning o< each day to ensure thet Ha performance on oromoiiuoroben2en (BFB) meeis me Epa criteria
- a ceubration curva for auantitalion is prepared using e mixture of volatile Organic
Pnonty Pollutant 'standards' ai a minimum of 3 different concentrations end using a mixture of 3 internal standards at a constant concentration
- The calibration curve is verified with a mixiure ol priority pollutant sianoaras every day if the response factors vary greaier man 25%, the instrument must be recalibrated
Analysis of Organic Compounds Extracted in Acid or Sese/Neutrat Solutions by Ges
Chrpmqtpqr jpn
PEtt^IY
- Each batch oi 20 samples consists oi 16 customer samples (at a maximum) one D'a^k sample one so*i-ed blink (lor water matrices! one sample spiked with the pr.oniy pollutant sienoaro mixture anq a duplicate customer sample This amounts to a 20%
Quality control factor
HONS 220959
CT/> *v'/AO/vvf<vr>u C (V teSTiNG r>4 C*TifiCATlON
- Tr.ree surrogate compounds are aoua to each sample m the oaten for Sese/he^'ra
anaiy^s
- ?r>ree surrogate compounds are aoaed to each sample in the oaten *or *c>o ara1 / S s
- a ebnd aua^ty control sample >s introduced to the laooralory for ana'ys'S on a wee- iy oas>s
- Each GC/MS is checked and retuneo i< necessary, at the oey.-n-ng of each aay o ensure mat its performance on decafiuorotriphenyiphospnine (OF tpp> meets me pa
criteria
* a caiipration curve for Quantitation is praoared using a mixture of standards con poseo of either the Organ.c Acid or Base'Neutral Extractable Comoounas at a m.nimum o* 3 concentrations and using five internal standards *or quantitation
Analysis of Metals
All $mpin
- New standards are prepared for eacn patch ot samples
- Normal caiipration is performed us "g a blank sampia and four standards that have been through the sample pr eparat>on procedure a regras$'on analysis <s used to construct the calibration curve
* ah EP Toxicity samptes and an samples determined by furnace atomic absorption are calculated by ti.e `method o' additions*
- For each sample analysis that reomres tna usa of the `method of additions' iechn.cue a three pomt calibration is performed using U S EPA `Methods for Chemical Ara ys s of water and wastes, <979* Results are obtained using imaar ragression analysis Any regression with a coefficient of correlation Deiow 0 990 t$ considered suspect necessitating review of calibration aete or eempie re-anaiysis
* in constructing the normal calibration curves the lowest concentration leve's we use are values greater than or equal to 5 times the instrumental Detection i>m<t (iDl)
- aii calibration standards art analyzed m duplicate, at e minimum
*'independent reference standards are used to check the accuracy of caiibraron standards
- a check standard >s analyzed every ten samples to validate the normal calibration
curve
- One customer sample out of every ten 1$ analyzed m triplicate
H^mpfnjput Smp/0t faxcaar fir u$fcury intlytit)
Samples are analyzed m batches of 30 or less For patches m which the sample mai-ces ere homogeneous. tr<e QC program is a minimum of 25% and consists of analyzing - 3 sets of triplicate analyses
- 2 Reoncate spikes * ' independentreference standard,
- ti Calibration sf noaros (processed using the sample preparation method' * 4 Cai'oration stanoaros ;w i1 cut sample preparation), and - 1 C-age-
HONS 220960
CTA tNVlKONMENTAt c I W TfSTINQ /ff CFAT/k/CAT/ON
4*mp/i (ttetpl for Mtrcuiy tntfjatt)
Samples are analyzed m batches oi 30 or less For eaiches m which the sample matrices are heterogeneous, the QC program is a minimum of 3S% ana consists of analyzing - 3 sets oi triplicate analyses - 2 Replicate spikes, - t Replicate independent reference Slenderds. - d Calibration standards (processed using the sample preparation mathod), - 1 Procedural Blank. - d calibration standards (without sample preparation), and * i Reageni Blank
Aniiyiti of Uorcuty
To analyze samples for mercury we group them py matrix in patches oi 30 or less Our OC program is a minimum ol 30% and consists of analyzing - aach of tn 30 customer samples in duplicate, - 3 sets of triplicate aneyisas. - 2 Replicate spikes. - 2 Replicate independent reference standards,
- to Calibration standards (processed using the sample preparation method), end
- 2 Procedural Blanks
Analysis of Pastlcides. H.erblcida_a_and PCB e by.Oas Chromaiogrephy
Pestic'de. herbicide and PCB samples era grouped m batches of 16 Customer eoncioi. > ,ess according to the type of analysis to be performed The OC program for each of these three types of analyses is a minimum of 20% and consists of analyzing
- i procedural blank aampiaCe reagent plank is analyzed m the case of non-water matrices).
- i spiked blank sample (the spiked blank is eliminated m the case of non-water matrices).
- i replicate sample. - t replicate spiked sample, and - t known rafemeca OC sample for at least each too samples analyzed The instrument is calibrated each run wiin three standards, ano checked every to samples
Analysis of Cyanidas. Phenols Fluoride Chloride Nitrate and Nitrite
- Aii parameters are analyzed using a Techmcon Autoanalyze' n GT - 3 calibration standards are analyzed at t-e beginning ana eno o< each oaten
MONS 220961
ETA* tNVt*OHUem*L
Civ T$iinq tn<t ce*rifiCATtoN
- Each batch (up to 80 samples) consists of analyzing one blank one sckea dank on* duplicate ana se><keo sam&ie every 20 samples, ana an EPA kno*n reference san-p.e
Analysis of Total Organic Carbon (TOC)
t OC samples are analyzed on a daily oass with the number o samples analyzed oer aay aeoenoent on me reouest for duplicate or auaaruoiicate analyses The Quality control program >s oesigneo to mamtam tne aporooriate amount of OC ana consists of the following elements
- Daily instrument calibration
One btann - Stanaara recaiipration every to samples - Spikeo samples at a low ana high level * E very sample is run in Qupiicete et e minimum
Analysis of Total Organic Heiide (TOX) - B'ank reagent water lor absolute carbon beckrouna must contain less than S ug/i of ha/ioe (as chionoe) - Using a trichloroohenol stanaara. the mean aasorotion efficiency must be within */15% of the stanaara value
- Calibration stanaaras are run every to samples.
- Every sample it run m duplicate at a minimum
AnalySia of.2,3,7,6^000 (Dfoxln) by OC/MS. (SIM)
- Each sample is dosed with e known auentity of ^Cjj-i.S.T.e-TCDD as internal stanaara end "Ci^-TCDD as surogata stanaara The action limns for surrogate standard results is +/- 4D% of the true vaiua Sampias showing surrogata stanaara resuite outside of these limits are reextracted and reanalyzed
Two laboratory 'metnod oienks' are run along with each sat of 24 or fewer samples The method blank is also dosed with the internal standard and surrrogete stanoaro
* At `east one per sat of 24 samples is run in duplicate to determine mtrateboratory precision
- Qualitative Requirements The following are met m order to confirm tne presence of netiva 2.3.7.8-TCOD a Isomer specificity must oe demonstrated Initially and verified once per ft-hou' work shift. The verification consists of injecting a mixture containing TCDD isomers which elute dose to 2 3.7.8-TCDD The 2,3.7.8-TCDO must be separated from mierfernng isomer, with no more than 25% vanay relative to the 2 3,7,8-TCOO peak 0 The 320/322 rat*o 'S within the range of 0 67 to 0 87 c ions 320. 322. and 257 are at orasant and maximize together the signal to ^anoise ratio must be 2 5 to t or better for an 3 ions d The retention time is eauai (witnm 3 seconas) the retention time lor me isotooicaiiy labeled 2.3.7,8-tcDD e At `east one of me positives can oe confirmed by obtaining partial scan soec'ra from mass 150 to mass 350 Tne oartia' scan gy'deunes are as to'iows
MOWS 220962
CT/* INVmONUtNTAL C lv TfsTtnQ *nc Cf Ar/F/CAfio/v
. the 320/324 ratio should be i 58 + /- 0 16
the 267/269 ratio should be 103 + /- 0 to
the 194/196 ratio should be t 54 +/- 0 IS
- One sample is spiked with native 2.3 7,6-TCDD at a level of tO PPB (for soil) tor each set of 24 or fewer samples
- in cases where no native 2 3 7,0-tcoO is detected, the actual detection limit is
estimated and reported based on a signal to noise ratio of 25 to 1 at ions 320 eno 322
* For each sample, the ihternei standard > present with at least a 10 to t signal to noise
ratio for boih mass 332 ana mess 334 Also, the internal standard 332/334 ratio musi
be within the range of 0 67 to 0 87
'
Subcontractor OA/QC
Each subcontrectoer is required lo mamtam an appropriate level of qualify control To insure this each subcontractor is required to submit to ETC the quality control data for an analyses it performs This dets is kept on file et ETc in general, the amount of quality convoi required is one duplicate sample with one spiked sample for every ten analyses
Chain -of -Custody
The cheln-of-custody procedure is part of our quality assurance protocol we believe our chein-of-cuslody record fully complies with the legal raqutraments of federal, stata and local government agencies and of the courts of law The record covers
- labeling of sample bottles, packing the Sample Shuttle and transferring the Shuttle under seal to the custody of s shipper,
- outgoing shipping manifests.
- the cheln-of*cu$tody form completed by the person(s) breaking the Shuttle seal takmQ the sample, reseeling the Shuttle and transferring custody to a snipper,
- 'nceming shipping manifests, - breaking the Shuttle's reseat, - storing each labeled temple bottle in a secured area, - disposition of aach sample to an analyst or technician, end
* the uee of the temple in each bottle m e testing procedure appropriate to the mienaed purpoet of the sample
The records Show for each imk in this process
- the person with custody, end
- the time and date each person accepted or relinquished custody
MOWS 220963
ETC ENVIRONMENTAL TESTING fU CERTIFICATION
Appendix A Mass Spectral Data
(or Quantitated Compounds
D a total ion chromatogram for each sample analyzed by a QC/viS instrument
2) a Quant report used by the analyst to determine Qualitative and Quantitative results of the compounds present
3) a mass soectrum end e reference spectrum for each priority podutent compound detected in the sample
HONS 220964
TOTAL ION ChSONOTOCMK
_
fr 1 i* MJttT 45,>'4$a, *u.~t#iS51 | T JC
TUIW -,BS474?,S ,3(( - Ju
it irt-r-T14^T u!'t"1tTo-1 r1itt't iri'i i4 'T-iit' t-1itr-i"*ai
Data filet >13667iiU7
Namei 660731 ACID
1
M t sc * L719AA ,UAA/'A/',S,30,ClVJl
Id File: I AC 1D >I US Title! PP/ACIO IDFILE
Last Calibration) 660331 1A:52
Operator ID: JH21B0 Quant Timai 660331 21i36 Injacted at: 660331 21:03
b i l 11
HONS 220965
QUANT REPQR)
Dp* r tor I U i Output Fi 1* i Oa ta F t 1 a i Namai 960331 rtllCI L7194A
JH2100
AI >667: l AQ
> I3667)> U7
ACID
I
^4747,5,30.09,1
Quant
Rav>
5 Quant Tima)
In jactad ati Dilution Factor)
0603)1 060331
BTL*12
2i:3t> 21:0)
1. u u
10 Ft la l IACIDMUS Ti t la i PP/HLlO luFILE Lot Calibration) 960331 14)*2
Compound
R.T. Scana Aria
Cone
Units
1> d4-1,4-DichIorobanzana
6.27 179
3 ) 2~F l uoropbanoI
f SL'P ft ) 4.19
62
9 ) Phano1-D5
(SURF?) 5.72
149
11 ) *d9-Naph tha t ana
9.30 354
12 ) 2,4-DiChlorophanoI
9.22 345
17) dlO-Acanaphtha tana
14.62 649
22) 2,4,6-Trichlorophanol
12.60 535
4 -- 2,4,4-T ah^Ta-r ap-harva 1 -- --- -------- 12.99- --65?
257---fr;5;*7-Tat r acMorophano 1
15.-00 -- -715
24) dlO-Phananthrana
19.07 899
25 ) 2,4 ,6-Tribromophano1
(SURR) 17.06 786
26) Pantachlorophanol
18.79 883
2B) dl2-Chry*ana
27.34 1362
12846
40.00 u&'-nL
21599
9u, 20 UG/ML
24474
96.32 ub^nL
29906
40. UO uS/riL,
1723
9.51 UG/ML
20642
40.00 UG/HL
115838 509.95 UG/tlL
------- 1797- _ ----- 7.91 QG/ML
--3555*-- 167,31
80950
40.00 UG'ML
22399
99,76 UG7ML
9b4
3.6 7 UG/ML
92208
40.00 U&7ML
q
9;
-v
9
4k
9 91 9 V' 9.
cv 1 Ul
Compound it I SI D
*0*3
MOMS 220966
reference rrowtflKt spectrum
Til*
N1S Rap, t tala laatPull apac.ra oF 1R* UfT $ Scan #J4I
pt Ab *
'*
tJ*I.AR am.
-4* 4R
;jv '
SAMPLE SPECTRUM rACKSR(K*HF SE`T*BCTEI>1
'f.Jr 'J3tf7 M3l ' SCIl ~I 171*TM ,0A4T4T,5,5*.M,i
Ipfc fib H*
** SU*
Sean 345 a.*i .in,
. () **
i.Cf4*
/
' Ii r * ^ i--t
* r-^i r f | '
( lM 1 i* ZRR
**a
/f Jl _ l irie sia
3SI
STS s 414
*a
/r /
1.4 .
3ta
SAMPLE SPECTRUM (UNAL TCRCt)
Fil* MJSST SttJJl ' SCTt ~
Ipk Ab 42R
`J
S3
4tS
"I . j / I
"L71*4# 7SS4747 ,'S ,5* ."f* ,T
Scan 345 *.*2 .in.
i`* **
**55/ 22 yS;* 4.4 4*
D* t F jIri >13667.:u?
Nainei 860331 ACID
1
Misei L719AA ,QA4747,S,30.09,1
Quant Time. 860331 21.36
Injectad Rti 860331 21.03
Compound No. 12
Compound Name. 2,4-DtehlorophRno1
Scan Numbari 345
Ratant ton Tima.
9,22 min.
Araai
1723
Concantrat ion.
8.51 UG/P1L
q-valua. 90
bin l
HONS 220967
Date F i I a < >136671s U7
Name! 060331 AC f0
]
died L719*h ,UA474?/S,30.U9/1
Quant Tima: 660331 21:36
Injected at: 060331 21i03
Compound No: 26 Compound Name! Panta eh 1orophano1
Scan Number: 603 Retention Tima! 10.79 min.
Areel
964
Concentrat ioni
3.67 UG/ML
q-ueluet 09
bi
MOWS 220968
BCrtREHCE STflNDQltD JPCCTRirn
__
r*i >iihi
i#v. c Cttt i4i.Tun (pt!.tp4_r thv hjs s'ic4n rni
p* ftp **
>J*
I4tlf.ll tin.
leee *e. \
*f7 lL it */ l1 >*3
e **
4 A. ,-ft* , . I - ^ , .-
( tw it*
*4* Vzid ' * iii
it*' " tie'
$OHp|_f 4tr-rirft r}orvftimit ytijiTftfirTEPi
71lr M'jffP ftpk ftp J4T(4
'T*C IP
I -L7T4fi ;#fllT47',S *5#.9* ,1* Scan *J?
>9M
If.4* 41 n.
HHt e
*T
(2 f l
I
\^Lx/r.J
ii* tit tie
ee
237 2(4
J2i
3*3 44J
/f
/
\/
N -e
' fie " fie jie <*i*'
SfiMTLC SftCCTftUn tUNftUT tftt D1
rfl >11(42 *3ir flCIJ - 1 121*4(5 *-,6(54247 ,t,J*.*,l * ~st^ 434
Ipk ftp 342(4
1*4
If.(I ain.
f***e
4
292244
>7*
441 46
321 * * \
-rX-T--,C`r-^-f *,-/ . .
j .--*2^6
26* 36* 3(6 4(6
Date File* >1*667)<U7
Name: 060731 ACID
1
Misei L?19ftH >QA4?ft7,S ,30.09,1
Quant Time) B60331 21*36
Injicted at) 060331 21*03
Compound No* 22
Compound Name* 2,4j6-TrichlorophsnoI
Scan Numberi 939
Retention Timei 12.60 min.
Area*
119B30
Concentration*
909.95 UG/hL
q-vi1ua * 9?
B1L6H
HONS 220969
f
TOTAL [DM CK*OMOTOS#OM____
f flV >f 6189 45. a-tse.a hu. 84*3Ji r ''(HPESTl711,S*4?47>$,3*,|
TIC
I
^.fit..
?i*..i. 1IH , lt*
2**1
21*8
i neeee
I
i i i
*
ii seeeee t i 7tiMe
*
(e*
4Mtt-
)
2IMM
IM*
j, t, jjfej
rr
('
> It It 2t 24 2* 32 H 4* 44
Data File >F6389lIU2 Name i 86 0731 #F B/NS.PE5T Mite: L?19mB,QB4747,5,30.09,1
Id Fi lei FBNPiiUS T [ i la: B/N*PEST ID FILE ____ .FOR F Lat Calibration! 860401 12i03
Operator ID) RA0157 Quant Tima) 060401 19:32 Injected at I 860401 1B<44
850326
HONS 220970
QUANT REPORT
Operator ID: RAO 157
Ou t pu t Fi lt *F6369)lAQ
Data File:
>F6389)U2
Hamai 860331 IF B/N6PEST
Miac) L7194B,QB4747,S,30.09,1
Quant Ravi 5
Quant Time:
Injected at)
Dt lutton Factor 1
860401 19:31 660401 16.44
1. 00
BTL*23
ID Pile! FBNPtiUS
Title: B/N*PEST ID FILE ....
FOR F
Lest Calibration) 660401 12:03
650326
Compound
R.T. Scan# Area
Cone
Unite
1) 2) 7)
8) 9) 12) 18 ) 19)
33) 39) 39) 41) 41) 45) 46) 54)
58) 59) 60) 61) 6T) 72) 04) 86) 90)
d4-l ,4-Dichlorobenzene
N-Nitrosodlmethylamtna
1,3-Diehlorobenzene
1,4-Dt chlorobenzene
1,2-Oichlorobenzene
Nit robenzene-D5
(SURR)
d6*Naphthalene
2-F1uorobiphany1
(SURR)
"dl0-Acanaphthalane Dimethyl phthelate
Dimethyl phthe lata
2t6*DinitrotO1u*nt
2,6-Din11roto Iuene
2,4-Dinitroto 1uene
Diethyl phthalata
dl0-Phenent hrene
Phenenthrene
Anthracene Dt-n-butyl phthelate
r luorenthene
Pyrene
dl2-Chry*ene
TerphenyI-D14
(SURR)
Butyl benzyl phthalata
bia(2-Ethy1 hexyl)phthe lata
6.50 249
19112
40.00 UG/ML
3-r57-
-----------5543 --
6tt56-------575-----------5875-------- Tv8? US/ML 6-r96----575---------- 5871 --------7 .--65 -UG/ML
6.96 7.92
275 329
5071 25944
7.98 ug/ml 37.90 UG/ML
9.76 433
84812
40.00 ug/ml
13.13
63515
31.10 ug/ml
15.08 l^T^fr------669
49813
40.00 UG/ML
. .r- .i^.
UG/*l
J5r06- ~?33 15.54----- 759
UG/ML -UG-'KL
UG-'ML
16.-92----- 831
UG/ML
19.59 987
UG-'ML
1Rt-66------- 991
UG4L
Vt-rM----- 951 25-r87-----14-t6-
UC-'ML
ucmL
23.36 1200
23r3A 5566
UG^ML -UC/ML
27.84 1452
UG-'ML
24.70 1275 56 r-45 --13 74
UG/ML
-UC^tL
28.52-1485
- UG-'ML
Q
97 100
9b 96 95 87
93 96
96 63
6b 6b
46 55 69
9t
96 93 95 5 95 100 91
68
99
Compound la 1STD
HOMS 209?1
t'CHCMCl tTAMBn^r JPCrTBUr _ H iT >fSiS2' I4i3it I'W C
<pka&- osm
?eeeeei y
. ?> ,/
< r
1 h CSl.STB. II
111 iv >*
Sc*P tit
i Bln, 41 41
- i'I'i . T ("I *e*t
,,,, t>)M,,., *,. r,
101 lii'
sanPLC spectrum (ibckcrouhd SutTpacTCoi
Tnr.'ftJe* 3483JT if t-S4i,PITuf|iBH,5N?4T,f
Ipk Ob 2lt
SU
ttet-
itte v
}' ..
t -4-...^,,,.f,., jiL.,./i. ,,
e 6
111
ii* r~
Mi r j i ' ' '12r*+
Sid"'*78
i .W Bin ,
ee -*
"M
SBMPLC SPECTRUM (UNALTEREDI
Pi l'">r$3eV 06*i3f F ~I''nIfCSTL7I*4||414P4?,J,3I.49,[ ` ' ------
Till
jeA 27( tXain.
/
lttt
5* / / *5
it
7
ji|l., 84 1 1^1 - '--[ T F T-,
It
Hi in r''
\L
{1+1.
t 2t
, r,-,
,, i *1
Data Fila! >F6J89:iU2 Manve: 860J51 *F B-'N&PEST n > c : L719*B,QB4747,S,30.09 , l Quant Timi: B60401 19:J2 Injected at: 860401 18:44
Compound Mol
9
Compound Name: 1,2-Dichlorobeniene
Scan Number: 275
Retention Timei
Araai
5071
6,96 min.
Concentration!
7.98 UG^ML
q-ualuti 95
BTlt,
MONS 220972
CTA fwvmowWT4i
C f V TST/WO <J
/C4T/0IV
Appendix Cl GC/MS Subsidiary Data
MONS 220973
Da ta Ft lei >[J663I1U?
Name: 860331 ACID
I
Mttci QC*?4?A ,QA4?4?,S,1,1
Id Fi lei IACIDiiUS Title! PP/ACID IDFlLE
C.a ibrar tom 660331 14:92
Operator ID) JH2160 Quant Timai 660331 16i52 Injected at: 860331 16*19
Bit#
MQNS 220974
QUANT REPORT
Operator IDs JH2160
Output Fi lai ''136631 lAQ
Data Fila s
>13663 tiU7
Nanas 660331 ACID
1
Til ac s QC47*7A (QAa?a7,S, 1,1
ID Filn I AC 10 m US T11 la s PP/aCID IDFJlE Lat Calibration! 660331 14t52
Quant Raut 5
Quant Tim*:
Injactad ati Dilution Factors
#61)33 1 16:52
660331 16>19 1,00
6tl 6
Compound
1)
in
17)
24)
28>
d4-l,4-Dichlorobeniene d8*Naphthalent dlO-Acanaphthalana dlO-Pbananthrana
*dl2-Chryaana
R.T. Scan#
6.17 9.26 14.46 16.92 27. 02
179 349
642 693 1349
Ar aa
39403 90499 34953 60065 16515
Cone
Un i t
40.00 40.00 40.00 40.00
40.00
ug/hl ug/ml UG/hL UG-'ITL
UG/TIL
* Compound la ISTD
HONS 220975
TOTm. tOM CMROMPTOCHON
rm >f*3#4
'u SiSJJi
. *f l^HiREST8C4T4T|, 4)*?4T,i. ]( ,
lt*t
248*
Data Fi La> >F4364i:<J2 Nani* t 660731 #F B/'N&PEST
flifc ! QC4747B,GB4747,S,30,1
Id Fi la : FBNPt :US
Tit l*: B-'N + PEST ID FILE
FOR F
Laat Calibration: 660401 02:06
Optrt tor ID: KUO786 Quant Tima 660401 09:56 lnjtctad a11 660401 09:06
650326
BTL#10
MONS 220976
QUANT REPORT
Operator ID; KUO706
Output Flits aF6304s:AQ
Oat* F: la :
>F6304s s U2
Names 060331 #F B^N&PEST
Mlc s QC4747B,084747,8,30,1
Quant Raui 5
Quant Times
Injected at >
Dilution Factors
060401 09!*!o
060401 09:00 1.00
btl#is
ID Filai FBNPtiUS
Titlai B/N*PEST ID FILE ....
FOR F
Last Calibrations 860401 02'06
050326
Compound
R. T. Scan# Araa
Cone
Units
1> *d4-l,4-Diehlorobeniana 2 > N-Nstroaodisnethylasnma 10 ) d8-Nephthelana 33 ) d10-Acanaphtha 1 ana 39 > Dimethyl phthalata
54) d10-Phenenthran* 60 > Di-n-butyl phthalata
?2) dl2-Chrysana 90 ) bia(2-Ethylhaxyl)phthalata
rv> ?cte fbund,
Compound It l$TO
6.53 249
24624
40.00 UG/ML
r-. `29 -------- H--
-UC--HL
9.77 432
09791
40.00 UG/ML
15.00 732
41534
40.00 UG/ttL
15-rfrS ------P3S--------ItH?-------- fri 39 -VKj.'KL
19.58 986
119392
40.00 UG/'tlL
21.09 1116
9574
3.24 UG/ML
27.02 1451
90321
40.00 UG/ML
20.41 1404
53616
25.56 UG^nL
9 10
9
9 10
9
< <.
MOMS 220977
ETC NVI/IOHMtNTAi TtSTlHQ I no C*TlftCATION
Appendix E Chaln-of Custody Forms
1) A field Chsm-of-Custody form (CCV la Included for all samples shipped by ETC shuttle
2) An in-house sample Chein-of Custody form Is included for alt samples not shipped by ETC shuttle
3) Any addttionel Chsm-of-Custody malarial providad by a client or
by a client's sampling agent is also included. 4) A subcontractor's Cham-of-Custody form la included for any
analytical work not performed within ETC's laboratory. 5) Analysis and Extraction Custody forms ara included for the
period the sample was in ETC's possession
HONS 220978
IHVtnOHUtHTAL Civ TtSTlHO fl* CtAVAlCATlQN
CHAIM Of CUSTODY
Companyijylo^nfCfoJob Mo. Addraaa____________ ________________..
_
Attantloni
Stmpla Daaeriptloni
CUSTOMER ID
DESCRIPTION
&0"r*tie * C~)
JL - &OH& <>J*A _______________ l
ETC *
limh
'
_ Llrts____
-- ------------------------------------- ------------ ------------------------------------ -------------------------- --------------- --------- -------- ---- - -
aaipla(a) Ralinquiahad by>
(lar* ZL<\ /c-z'o^ >0-n u (
**____ LUX___________ Pt*t____iJAih* .
Sampla(a) Racaivtd byi ^
______________________
Tima t } ' f ^_ Datat_ .?/i htt,
tM HAAllAH CtHJtA AAAKWA1 *W*ON. KJ m)T f**1) I*M*
HONS 220979
7
CHAIN Of CUSTODY ttCOtt)
MAC JO# NlMCt _
..
.
. CUSTtttt WPMStNTATIYI _
0 CONTRACT NUMBEt
(HC CONTRACT MANAGE*
PLANT NAME OR COM _
_ WC TEAM l [AMI _ <Cty ^
(Specific inform t Ion on soap)** It eMllebl* on etttthed *$*iplo IdentifierIon log*)
SI (no turn
Teto leeder Verlflcetf'sn of Collected Staple*:
XJ.'TKf'C
Dote
Tier
*/>/?< 'do*
teNrkl
telInqulthed bmtf&SU.Hii'i deceived by:
telInqulthed by: ^
deceived by:
*M/?i oivt ^'/n/u-Aur +4,^.^ h Ct~C
Lopped-In-by:
tecetved for AniTytlt by:
Method ef SMpaent: fi,r \' tr
Iheoher of Conti Inert: /
Spec 1^1 InjtrtKlIom {SonpTo priterrj tlon, lecurjtj, delivery to, etc.)
fr *S te AM
HONS 220980
HCWS 220981
ETC rltiriiC W
LABORATORY CHRONICLE- QC-MS 0prim*nt
OATE _*//</ . SHIFT--
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TUNE FILE____^yrk'ej
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ETC FOAM
MGNS 220982
ETC rifimC rt CMi'Ki'fl*
LABORATORY CHRONICLE: GC-MS Dtprtmnt (
DATE'^''^M/t
SHIFT,
FRACTION___vS/-*',
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INSTRUMENT _.
F.
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7 /V rjZztJ .
SEOUENCE File, KV2/ ____ __ method file , ib?F /*.< l2-\
ID FILE _
analyses) _
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=
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CURRENT CSOi STATUS
standards updated
STANDARD
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HONS 220983
CEYIVf*
fN*o**r*'*t a*i>'rC*i'Q*
LABORATORY CHRONICLE: GC MS Department
DATE _va;A1 /rt.
FRACTION____
SHIFT
r-------------------------
STANDARD
CONC
PAM
INSTRUMENT __
TUNE FILE-
SEQUENCE FILE _.
METHOD FILE __ .
ID FILE _ ANALYST(S)__
LOT NO*
SUPERVISOR, BATCH #'
St
7
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CURR(NT CMS STATU*
STANDARDS UPDATIO
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LOT VOL
MGNS 220984
PT/\ tHYIIIQHMtHTAL CIV/ TfsrwG *ntf cemiftcAiioN
LL 14166.
LABORATORY CHRONICLE: Metele Department Smplea_L'!i<W ; L.ll^
Hg Prep AA/ICAP Prep^^jia^
Chemist Wi'foJL
Date Ji/iiliL,
d/i [a.
Leb Supervisor.
ITC P9RW net
Date-i*/'H'
HONS 220985