Document qd8EKD405VVbKZy56z8DjVkZE
Study Title
T e n n e s s e e R iv e r V a lle y S a m p le s
Author
Mark E. Ellefson
Revised Report
September 12, 2003
Performing Laboratory
3M Environmental Laboratory Building 2-3E-09 935 Bush Avenue
St Paul, MN 55106
Project Identification
3M Environmental Laboratory Study # E02-0443
Total Number of Pages 276
Report E02-0443
Tenn. River Valley Samples
Table of Contents
List of Tables........................................................................................................................................... 3 Study Inform ation....................................................................................................................................4 Summary................................................................................................................................................. 5 Purpose................................................................................................................................................... 6 Test and Analytical Reference Substances...........................................................................................6 Test Systems........................................................................................................................................... 7 Method Summaries.................................................................................................................................8 Preparatory Methods.............................................................................................................................. 8 Sample Analysis......................................................................................................................................11 Analytical M ethod....................................................................................................................................12 Analytical Results....................................................................................................................................1 3 Data Sum m ary........................................................................................................................................ 20 Statistical M ethods................................................................................................................................. 2 5 Statement of Conclusion........................................................................................................................ 2 6 References.............................................................................................................................................. 2 6 List of Attachments..................................................................................................................................2 6 Signature Page........................................................................................................................................27 Attachment A: Analytical Method and SOP Deviations........................................................................28 Attachment B: Data Summary Tables................................................................................................... 40 Attachment C: Sample Chromatograms...............................................................................................67 Attachment D: Sample Prep Sheets, Test Substance, and Test System Inform ation...................... 230 Attachment E: Notes to File.......................................................................... ;.........................................270
3M Environmental Laboratory
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List of Tables
Table 1. Sample Location, Sample Type, and Analytical Data Summary.......................................... 5 Table 2: Characterization of the Test and Analytical Reference Substances.................................... 6 Table 3a. Description of Fish Tissue Analyzed in this Study.............................................................7 Table 3b. Description of River W ater Analyzed in this Study............................................................7 Table 3c. Description of River Sediments Analyzed in this Study.................................................... 7 Table 4a. Fish Tissue Sample Preparation Method.......................................................................... 8 Table 4b. Preparation of Extracted Calibration Curves for the Fish Tissue..................................... 9 Table 4c. Fish Tissue Analytical Data Quality Objectives..................................................................9 Table 4d. River W ater Sample Preparation M ethod......................................................................... 9 Table 4e. River W ater Sample Data Quality O bjectives................................................................... 1 0 Table 4f. River Sediment Sample Preparation Method.................................................................... 10 Table 4g. River Sediment Sample Data Quality O bjectives.............................................................. 11 Table 5. Sample Analysis Information...................................................................................................11 Table 6a. PFOS CalibrationStandard Reprocessing Sum mary........................................................ 14 Table 6b. FOSA CalibrationStandard Reprocessing Sum m ary........................................................ 15 Table 6c. PFOA CalibrationStandard Reprocessing Sum m ary........................................................ 16 Table 6d. PFHS CalibrationStandard Reprocessing Sum m ary........................................................ 17 Table 6e. PFBS CalibrationStandard Reprocessing Summary........................................................ 1 8 Table 7a. Catfish Analytical Data........................................................................................................ 21 Table 7b. Large mouth and Small mouth Bass Analytical Data........................................................ 22 Table 7c. River W ater Analytical Data................................................................................................ 2 3 Table 7d. River Sediment Analytical Data.......................................................................................... 2 4 Table 8. Sample Location, Sample Type, and Analytical Data Summary...........................................2 5
3M Environmental Laboratory
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Study Information
Requestor
Dale L. Bacon 3M Environmental Laboratory Bldg. 2-3E-09 935 Bush Avenue St. Paul, MN 55106 651-778-4736
Study Director Mark E. Ellefson 3M Environmental Laboratory Bldg. 2-3E-09 935 Bush Avenue St. Paul, MN 55106 651-778-5405
Study Location
Testing Facility 3M Environmental Laboratory Bldg. 2-3E-09 935 Bush Avenue St. Paul, MN 55106
William K. Reagen, Laboratory Manager Mark L. Anderson, Analytical Chemist Cindy M. Carlson, Analytical Chemist Ognjenka Krupljanin, Analytical Chemist
Experimental Dates
Sample Analysis Initiation: 26 June 2002 Sample Analysis Completion: 12 November 2002
Location of Archives
All original raw data and the report have been archived at the 3M Environmental Laboratory according to 3M Standard Operating Procedures. Remaining specimens pertaining to the analytical phase of this study will be archived at the 3M Environmental Laboratory for as long as the quality of the preparation affords evaluation.
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Summary
Fish, river water, and river sediment samples were collected from three locations in the Tennessee River near the 3M Decatur, Alabama facility. The samples were analyzed for perfluorobutane sulfonate (PFBS), perfluorohexane sulfonate (PFHS), perfluorooctanoate (PFOA).perfluorooctane sulfonylamide (FOSA), and perfluorooctane sulfonate (PFOS). The analyses were accomplished by extracting the samples using Solid Phase Extraction (SPE) and then analyzing them using HPLC-Electrospray/Mass Spectrometry (HPLC/ES/MS).
Sampling Location 1 (SL-1) was located downstream of the 3M facility near Fox Creek at river mile 296. Sampling Location 2 (SL-2) was across the river from the 3M facility at river mile 301. Sampling location 3 (SL-3) was upstream from the 3M facility at river mile 307.5.
Analytical results are presented in Table T.
Table 1. Sample Location, Sample Type, and Analytical Data Summary. Fish Tissue
Sampling Location & Species Sampled
PFBS (ng/g)
PFHS (ng/g)
PFOA (ng/g)
FOSA (ng/g)
PFOS (ng/g)
SL-1, C (n=6) SL-2, C (n=7) SL-3, C (n=6)
SL-1, LM (n=6) SL-2, LIVI (n=4) SL-3, LM (n=7) SL-3, SM (n=1)
<LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
<LLOQ
<LLOQ <LLOQ <LLOQ River W ater
<LLOQ1
<LLOQ <LLOQ <LLOQ
60.9 (6/ 6)2 <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ <LLOQ
113 (6/ 6)2 <LLOQ
15.2 (4/ 6)2
553 (6/6)2
169 (2/4)2 <LLOQ <LLOQ
SL-1, RW SL-2, RW SL-3, RW
PFBS
(pg/m L)
84 <LLOQ <LLOQ
PFHS
(pg/m L)
PFOA
(pg/m L)
196 550
<LLOQ
<LLOQ
<LLOQ
<LLOQ
River Sediments
FOSA (pg/m L)
25 <LLOQ <LLOQ
PFOS
(pg/m L)
491 <LLOQ <LLOQ
PFBS (pg/g)
PFHS (pg/g)
PFOA (pg/g)
FOSA (pg/g)
PFOS (pg/g)
SL-1, RS
577
130
732
1440
3130
SL-2, RS
437
<LLOQ
<LLOQ
141
457
SL-3, RS
452 <LLOQ 127
68 416
C = CatFish, LM * Larg mouth bass, SM = Small mouth bass, RW = River water, and RS = River Sediments. 'High triplicate value was statistically eliminated using Dixon's Q-Test. 2(Number of Fish > LLOQ / Number of Fish Analyzed). Only one River Water and one River Sediment sample were collected from each sampling location.
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Purpose
The purpose of this study is to perform quantitative screening for PFBS, PFHS, PFOA, FOSA, and PFOS in sport-caught fish, river water, and river sediments from three sampling locations of the Tennessee River near Decatur, Alabama.
T est and Analytical Reference Substances
Table 2: Characterization of the Test and Analytical Reference Substances.
T est and A nalytical Reference Substance
PFHS
FOSA
PFOA
Compound
Source
Storage Conditions 3M Laboratory Identification Number Physical Description Purity
PFHS, Perfluorohexanesulfonate
3M Specialty Materials, Bldg. 236-2B-11 Frozen
FOSA, Perfluorooctanesulfonamide
3M Specialty Materials, Bldg. 236-1B-10
Frozen
TCR-083
TCR-029
White Powder 98.6%
Light yellow waxy solid Undetermined
PFOA, Perfluorooctanoate Ammonium 3M Specialty Materials, Bldg. 236-1 B-10 Frozen
TCR-123
White Powder 95.0%
T est and A nalytical Reference Substance
PFBS
PFOS
Compound
Source
Storage Conditions 3M Laboratory Identification Number Physical Description Purity
PFBS, Potassium Perfluorobutane Sulfonate
Wildlife International
Frozen
TCR-359
White crystals 97.3%
PFOS, Potassium Perfluorooctanesulfonate 3M Specialty Materials, Bldg. 236-1 B-10 Frozen
TCR-129
White Powder Undetermined
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T est Systems
Table 3a. Description of Fish Tissue Analyzed in this Study
Source *Types Storage Conditions Location 1 Location 2 Location 3
F ish T issue
Tennessee River Catfish Large Mouth Bass Small Mouth Bass Frozen
Downstream from the 3M facility near Fox Creek (river mile 296) Across the river from the 3M facility (river mile 301) Upstream of the 3M facility (river mile 307.5)
a The fish were filleted and representative aliquots of the fillets were analyzed.
Table 3b. Description of River Water Analyzed in this Study
Source Storage Conditions Location 1
Location 2
Location 3
River W ater
Tennessee River
Chilled (approximately 4 C.) Downstream from the 3M facility near Fox Creek (river mile 296) Across the river from the 3M facility (river mile 301) Upstream of the 3M facility (river mile 307.5)
Table 3c. Description of River Sediments Analyzed in this Study
Source Storage Conditions Location 1
Location 2
Location 3
R iver S ediments
Tennessee River
Chilled (approximately 4 C.) Downstream from the 3M facility near Fox Creek (river mile 296) Across the river from the 3M facility (river mile 301) Upstream of the 3M facility (river mile 307.5)
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Method Summaries
The concentrations o f PFBS, PFHS, PFOA, FOSA, and PFOS in Fish Tissue, River Water, and River Sediments were determined by using Solid Phase Extraction (SPE) and High Performance Liquid Chromatography-Electrospray/Mass Spectrometry (HPLC/ES/MS).
Preparatory Methods
The following tables describe the sample preparation methods for the Fish Tissue, River W ater, and River Sediment samples. Data Quality Objectives (DQO) are also given for each sample preparation method.
Fish Tissue Sample Preparation Method
Table 4a. Fish Tissue Sample Preparation Method
Step
1 2 3 4
5 6 7
8
9 10
Fish T issue Sam ple Preparation M ethod
Approximately 2 g of Fish Tissue and 8 mL of ASTM Type 1Water were homogenized.
The homogenate was centrifuged to eliminate the foam and then shaken/vortexed to re suspend the homogenate.
Each homogenate was aliquoted into triplicate samples. This was accomplished by transferring 1.0 mL of homogenate to 3 separate 15 mL centrifuge tubes.
Matrix spikes (MS) were prepared for every other homogenate, in this case, an additional (4th) 1.0 mL of homogenate was transferred to another 15 mL centrifuge tube. The MS's were spiked with 100 uL of a 100 ug/mL spike solution containing each of the test substances.
5.0 mL of acetonitrile was then added to the centrifuge tubes. The tubes were capped and shaken for 20 min at 300 rpm.
After mixing, the samples were centrifuged at 3000 reffor 10 minutes to clarify the
supernatant.
The supernatantwas decanted into new 50 mL centrifuge tubes and diluted with 40 mL of water.
Waters C-18 Tri-functional, Sep-Pak 1g, 6cc SPE columns with attached 70 mL reservoirs were placed onto vacuum manifolds and pre-conditioned in the following manner. Approximately 10 mL of methanol was added to the columns and the vacuum was applied. Once most of the methanol had been pulled through, ASTM Type 1 Water was added (5-10 mL). When most of this was pulled through, more water was added (5-1OmL). When there was only a small amount of water left in the reservoir, the stopcock was turned to stop the vacuum to the column. The columns were not allowed to go dry.
The supemates from step 7 were passed through the pre-conditioned SPE columns. The aqueous eluent was not collected. The columns were allowed to dry for at least 3 minutes.
The analytes were eluted from the SPE columns with 2.0 mL of methanol into autovials.
See the preparation worksheets for other exact amounts, times, speeds, etc.
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Table 4b. Preparation of Extracted Calibration Curves for the Fish Tissue.
Step
1 2 3
P reparation of E xtracted C alibration C urves for the Fish T issue
There were two extracted Fish Tissue calibration curves: Large Mouth Bass and CatFish, Rangefinding experiments were done to determine which Fish Tissues had the lowest endogenous levels of the analytes. Then, one Large Mouth Bass and one CatFish sample containing the least amount of endogenous test substances were selected as the matrix to construct the calibration curves. The Small Mouth Bass was analyzed using the Large Mouth Bass calibration curve. The procedure for preparing the extracted calibration curves is the same as the Fish Tissue sample preparation, except the volumes were scaled-up to provide a homogeneous batch of fish tissue matrix. The differences are as follows:
Approximately 10 g of Fish Tissue and 40 mL of ASTM Type 1Water were combined and homogenized.
1.0 mL of homogenate was transferred to the appropriate number of tubes.
Each tube was spiked with the predetermined amount of spike solution.
Table 4c. Fish Tissue Analytical Data Quality Objectives.
Step
F ish Tissue Analytical D ata Q uality O bjectives
1 All samples were prepared in triplicate. The %RSD should be s 25%
Matrix spikes were performed on half of the fish of each type from each sampling location. 2 Recovery should be within 30% from expected values. A total of 18 matrix spikes were
prepared for the Fish Tissue samples.
Water blanks, consisting of an aliquot of water run through the entire sample preparation and
3
extraction process were prepared with samples from each sampling location. Water blanks containing < !4 LLOQ of each analyte for the data set in which they were run were
considered acceptable.
Extraction blanks, consisting of an aliquot of methanol run though a pre-conditioned SPE 4 cartridge, were prepared for each sampling location. Extraction blanks containing <
VxLLOQ of each analyte for the data set in which they were run were considered acceptable.
5 Mid-level calibration curve points were used as CCVs.
River Water Sample Preparation Method
Table 4d. River Water Sample Preparation Method
Step
1
2
R iver W ater Sam ple P reparation M ethod
Waters C-18 Tri-functional, Sep-Pak 1g, 6cc SPE columns with attached 70 mL reservoirs were placed onto vacuum manifolds and pre-conditioned in the following manner. Approximately 10 mL of methanol was added to the columns and the vacuum was applied. Once most of the methanol had been pulled through, ASTM Type 1 Water was added (5-10 mL). When most of this was pulled through, more water was added (5-1OmL). When there was only a small amount of water left in the reservoir, the stopcock was turned to stop the vacuum to the column. The columns were not allowed to go dry.
40 mL of the River Water was passed through a pre-conditioned SPE column. The columns were allowed to dry for at least 3 minutes.
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Table 4d. River Water Sample Preparation Method
Step
3
R iver W ater Sam ple P reparation M ethod
The analytes were eluted from the columns with 2.0 mL of methanol into autovials.
|
Table 4e. River Water Sample Data Quality Objectives
Step 1
2 3
R iver W ater Sam ple Data Q uality O bjectives
Water blanks, consisting of an aliquot of water run through the entire preparation and extraction process, were prepared with samples each day samples were extracted. Water blanks containing < 'A LLOQ of each analyte for the data set in which they were run were considered acceptable.
A non-extracted solvent calibration curve was used to quantitate the River Water samples. No extracted CCVs were prepared, a mid-level calibration curve point was used for this purpose.
No matrix spikes were preformed during the sample preparation of the River Water samples.
River Sediment Sample Preparation Method
Table 4f. River Sediment Sample Preparation Method
. Step
1 2 3 4 5
6
7 8
9
10 11 12
R iver S ediment Sam ple Preparation M ethod
There were 3 River Sediment samples, one from each sampling location. Triplicate samples plus a matrix spike were prepared for each location.
Initially, sediment was transferred to 50 mL centrifuge tubes and centrifuged at 6000 RCF for 20 min. The liquid was decanted off and the remaining sediment was used for the sample preparation
Approximately 20g of sediment and 35mL of 1% Acetic Acid (aqueous) were combined into 50mL centrifuge tubes.
Matrix spikes were prepared by adding 100 uL of 100 ug/mL spike solution to the predetermined MS tubes.
The tubes were capped, vortexed, and then shaken for 60 min at 300 RPM.
They were then centrifuged at 6000 RCF for 20 minutes.
Waters C-18 Tri-functional, Sep-Pak 1g, 6cc SPE columns with attached 70 mL reservoirs were placed onto vacuum manifolds and pre-conditioned in the following manner. Approximately 10 mL of methanol was added to the columns and the vacuum was applied. Once most of the methanol had been pulled through, ASTM Type 1 Waterwas added (5-10 mL). When most of this was pulled through, more water was added (5-1OmL). When there was only a small amount of water left in the reservoir, the stopcock was turned to stop the vacuum to the column. The columns were not allowed to go dry.
The aqueous solutions from step #5 were decanted from the samples and passed through pre-conditioned SPE cartridges. The aqueous eluates were discarded.
20 mL of methanol was then added to the sediment samples. The samples were vortexed, shaken for 30 min at 300 RPM, and then centrifuged at 6000 RCF for 20 minutes.
The methanol was decanted, passed through the SPE cartridge and collected. An additional 4 mL of methanol was used to wash the reservoir and the column.
The collected methanol was then added to approximately 200mL of ASTM Type 1Water.
This solution was then passed through a new pre-conditioned SPE cartridge. The aqueous eluate was discarded.
The analytes were eluted from the SPE cartridges with 2.0 mL of methanol into autovials.
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Table 4g. River Sediment Sample Data Quality Objectives
S tep
1 2
3
4 5
R iv e r Sedim ent Sam ple Data Q uality O bjectives
All samples were prepared in triplicate. The %RSD should be s 25%
Matrix spikes were performed on each sample. Recovery should be within 30% of expected values.
Two lab control samples, consisting of spiked water carried through the entire extraction process and analyzed with the samples, were prepared. However, the information was not used because the data suggested it was impossible to recover spiked analytes from acidified water when river sediment was not present
Water blanks, consisting of an aliquot of water run through the entire preparation and extraction process, were prepared. Acceptable values were < V i LLOQ tor the data set in which they were run.
The River Sediment samples were quantitated using a non-extracted solvent calibration curve. Mid-level calibration curve points were used as CCV's.
Sample Analysis
The samples were analyzed using HPLC/ES/MS. The analytical method was based on the 3M Environmental Laboratory Method ETS-8-155.1 "Analysis of Waste Stream, W ater Extracts or Other Systems Using HPLC-Electrospray/Mass Spectrometry".
The following table details sample run information, including the sequence and the run start date of each sample.
Table 5. Sample Analysis Information.
Sample
Location
1 Catfish
I
2 Large Mouth Bass 3 Small Mouth Bass 4 River Water
5 River Sediments
SL-1 SL-2 SL-3 SL-1 SL-2 SL-3 SL-3 SL-1 SL-2 SL-3 SL-1 SL-2 SL-3
Sequence
D020629 D020629 D020702 D020626 D020628 D020628 D020628 D020812 D020812 D020812 1021112 1021112 1021112
Date Sequence W as Started
29 Jun 02 29 Jun 02 02 Jul 02 26 Jun 02 28 Jun 02 28 Jun 02 28 Jun 02 12 Aug 02 12 Aug 02 12 Aug 02 12 Nov 02 12 Nov 02 12 Nov 02
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Analytical Method
Sample analysis was based on ETS-8-155.1 "Analysis of W aste Stream, W ater Extracts Or Other Systems Using HPLC-Electrospray/Mass Spectrometry". Methanol extracts were analyzed using HPLC/ES/MS in the negative ion mode. PFBS, PFHS, PFOA, FOSA and PFOS levels were evaluated versus calibration standards ranging in concentration from 1 1000 ng analyte/mL. The target ions were as follows: m/z = 299 (PFBS), m/z = 399 (PFHS), m/z = 413 (PFOA), m/z = 498 (FOSA), and m/z = 499 (PFOS). The analytical method used for analysis is presented below; modifications may be necessary to optimize the method for individual instruments.
Analytical Equipment
Liq uid C hrom atograph: Agilent/Hewlett-Packard Series 1100 Liquid Chromatograph system
Analytical column: Keystone BetasilTM C i82x50mm, 5pm particle size
Column temperature: 30 C
Cycle Time: 9.5 minutes
Flow rate: 300pL/min
Injection volume: 4 to 20pL
Mobile phase components:
'
Solvent A: 2.0 mM ammonium acetate in water
Solvent B: HPLC Grade Methanol
Solvent Gradient:
Tim e 0.00 0.50 0.80 3.50 5.50 6.50 9.50
%B 10 % 10 % 60 % 100% 100% 10 % 10 %
Mass S pectrom eter: Agilent/Hewlett-Packard Series 1100 APi/Mass Spectrometer Detector Software: Agilent ChemStationTM A.08.03 Fragmentar Voltage: m/z 299 = 100V
m/z 399 = 120V m/z 413 = 100V m/z 498 = 80V m/z 499= 140V
Capillary Voltage: 4000 V Gain = 1.0 EMV Mode: Electrospray Negative Gas Temperature: 350 C Drying Gas: 8.0 L /min. Nebulizer Pressure: 30 psig Analysis Type: Single Ion Monitoring (SIM)
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Analytical Results
Data quality objectives outlined in the Preparation Methods section were met.
Regressions. Quadratic curve fit was applied to calibration standards and sample data to improve quantitation over the concentration range appropriate to the data. All calibration curves had least-square fits of 0.990 or greater.
Calibration Standards. Standards ranging in concentration from approximately 1.0 to 1000 ng/mL were used for the calibration curves. The standard curve points had an injection volume of 10 uL. In some instances, the 1.0 ng/mL standard was injected at smaller volumes (1 ,2, and 5 uL), this was done to extend the low end of the calibration curve. Calibration curves were run before every analytical sequence. Percent deviations of each calibration standard were calculated. High-end curve points that were outside the 20% criteria of the target concentration were excluded from the curve calculations. Low-end curve points that were outside the 20% criteria were included in the curve calculations but excluded from the Lower Limit of Quantitation (LLOQ).
Continuing Calibration Verification (CCV)- For quantitative determinations, a mid-level matrix calibration check was analyzed at least every ten samples to monitor instrumental drift, with a lim it of 20% deviation of the target concentrations.
Lower Limit of Quantitation (LLOQ). The LLOQ was equal to the lowest standard in the calibration curve, with a level of accuracy within 20%, that demonstrated a response greater than two times the response of analyte in the blank samples.
System Suitability. Five system-suitability standards were analyzed before each initial calibration curve to measure the precision of the retention times and peak area. The precision criterion of 5% for the mean area recovery was achieved.
Lab Control Spikes (LCS). LCSs were performed for the River Sediments. However, the information was not used because the data suggested it was impossible to recover spiked analytes from acidified water when river sediment was not present.
Matrix Spikes (MS). Matrix spikes were performed for the Fish Tissue and the River Sediment samples. Desirable matrix spike recoveries are 30%. Not all matrix spikes met this criteria.
The Fish Tissue data was quantitated using an extracted calibration curve while the River Water and River Sediment samples were quantitated using unextracted calibration curves. The calibration curve range that was injected was from 1 ng/mL to 1000 ng/mL, but the range used differed. The tables that follow contain either the calibration standard or the sample preparation method Lower Limit of Quantitation (LLOQ) for the analytes for each sample at each location along with batch used and the analysis date. The sample preparation method LLOQs will be annotated in the tables.
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Table 6a. PFOS Calibration Standard Reprocessing Summary PFOS CONCENTRATION
Sample T ype and L o c a t io n
Batch and A nalysis Date
Catfish, SL-1
D020629,29 Jun 02
Catfish, SL-2
D020629,29 Jun 02
Catfish, SL-3
D020702,02 Jul 02
Large Mouth Bass, SL-1
D020626,26 Jun 02
Large Mouth Bass, SL-2
D020628,28 Jun 02
Large Mouth Bass, SL-3
D020628,28 Jun 02
Lower Lim ito f
Q uantitation (LLOQ)
2.5 ng/g 2.5 ng/g 1.0 ng/g 1.0 ng/g 2.5 ng/g 2.5 ng/g
Small Mouth Bass, SL-3
D020628,28 Jun 02
2.5 ng/g
River Water, SL-1 River Water, SL-2 River Water, SL-3
D020812A, 12 Aug 02 D020812A, 12 Aug 02 D020812A, 12 Aug 02
125 pg/mL* 125 pg/mL* 125 pg/mL*
RiverWater, SL-1
D020812B, 12 Aug 02
1.25ng/mL'
River Water, SL-2
D020812B, 12 Aug 02
1.25 ng/mL*
River Water, SL-3
D020812B, 12 Aug 02
1.25ng/mL*
River Sediment, SL-1 River Sediment SL-2 River Sediment SL-3
1021112,12 Nov 02 1021112,12 Nov 02 1021112,12 Nov 02
250pg/g* 250pg/g* 250 pg/g*
* Denotes sample preparation method LLOQ. Method LLOQ = Instrument LLOQ/Method Concentration Factor.
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Table 6b. FOSA Calibration Standard Reprocessing Summary FOSA CONCENTRATION
Sample T ype and L o c a t io n
Batch and A nalysis Date
Catfish, SL-1
D020629, 29 Jun 02
Catfish, SL-2 Catfish, SL-3
D020629, 29 Jun 02 D020702, 02 Jul 02
Large Mouth Bass, SL-1 Large Mouth Bass, SL-2 Large Mouth Bass, SL-3
D020626,26 Jun 02 D020628, 28 Jun 02 D020628,28 Jun 02
Small Mouth Bass, SL-3
D020628,28 Jun 02
River Water, SL-1 River Water, SL-2
D020812A, 12 Aug 02 D020812A, 12 Aug 02
River Water, SL-3
D020812A, 12 Aug 02
River Water, SL-1
D020812B, 12 Aug 02
River Water, SL-2
D020812B, 12 Aug 02
River Water, SL-3
D020812B, 12 Aug 02
River Sediment SL-1 River Sediment SL-2
1021112,12 Nov 02 1021112,12 Nov 02
River Sediment SL-3
1021112,12 Nov 02
Low er L imit of Q uantitation (LLO Q )
2.5 ng/g 2.5 ng/g 2.5 ng/g 5.0 ng/g 5.0 ng/g 5.0 ng/g 5.0 ng/g 25 pg/mL* 25 pg/mL* 25 pg/mL* 1.25 ng/mL* 1.25ng/mL* 1.25 ng/mL* 50pg/g* 50pg/g* 50pg/g*
* Denotes sample preparation method LLOQ. Method LLOQ = Instrument LLOQ/Method Concentration Factor.
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Table 6c. PFOA Calibration Standard Reprocessing Summary PFOA CONCENTRATION
Sample Type and L o c a t io n Catfish, SL-1 Catfish, SL-2 Catfish, SL-3
B atch and A nalysis Date
D020629,29 Jun 02 D020629,29 Jun 02 D020702,02 Jul 02
Low er Limit of
Q uantitatio n (LLOQ)
5.0ng/g
5.0 ng/g 5.0 ng/g
Large Mouth Bass, SL-1 Large Mouth Bass, SL-2 Large Mouth Bass, SL-3 Small Mouth Bass, SL-3
River Water, SL-1 River Water, SL-2 River Water, SL-3
D020626,26 Jun 02 D020628,28 Jun 02 D020628,28 Jun 02 D020628,28 Jun 02 D020812A, 12 Aug 02 D020812A, 12 Aug 02 D020812A, 12 Aug 02
2.5 ng/g 5.0 ng/g 5.0 ng/g 5.0 ng/g 50pg/mL* 50pg/mL* 50pg/mL*
River Water, SL-1 River Water, SL-2 River Water, SL-3 River Sediment, SL-1 River Sediment, SL-2 River Sediment SL-3
D020812B, 12 Aug 02 D020812B, 12 Aug 02 D020812B, 12 Aug 02
1021112,12 Nov 02 1021112,12 Nov 02 1021112,12 Nov 02
1.25ng/mL* 1.25ng/mL* 1.25 ng/mL* 250pg/g* 250pg/g* 250pg/g*
* Denotes sample preparation method LLOQ. Method LLOQ = Instrument LLOQ/Method Concentration Factor.
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Table 6d. PFHS Calibration Standard Reprocessing Summary
PFHS CONCENTRATION
Sample Type and L o c a t io n Catfish, SL-1 Catfish, SL-2 Catfish, SL-3
Batch and A nalysis Date
D020629,29 Jun 02 020629,29 Jun 02 D020702,02 Jul 02
Low er L imit of
Q uantitation (LLOQ)
2.5 ng/g
2.5 ng/g
2.5 ng/g
Large Mouth Bass, SL-1 Large Mouth Bass, SL-2 Large Mouth Bass, SL-3 Small Mouth Bass, SL-3
River Water, SL-1 River Water, SL-2 River Water, SL-3
D020626,26 Jun 02 D020628,28 Jun 02 D020628,28 Jun 02 D020628,28 Jun 02 D020812A, 12 Aug 02 D020812A, 12 Aug 02 D020812A, 12 Aug 02
1.0 ng/g 1.0 ng/g 1.0 ng/g 1.0 ng/g 25 pg/mL* 25 pg/mL* 25 pg/mL*
River Water, SL-1
D020812B, 12 Aug 02
1.25ng/mL*
River Water, SL-2
D020812B, 12 Aug 02
1.25ng/mL*
River Water, SL-3
D020812B, 12 Aug 02
1.25ng/mL*
River Sediment, SL-1 River Sediment, SL-2 River Sediment, SL-3
1021112,12 Nov 02 1021112,12 Nov 02 1021112,12 Nov 02
100 pg/g* 100 pg/g* 100 pg/g*
* Denotes sample preparation method LLOQ. Method LLOQ = Instrument LLOQ/Method Concentration Factor.
3M Environmental Laboratory
Page 17 of 276
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Tenn. River Valley Samples
Table 6e. PFBS Calibration Standard Reprocessing Summary PFBS CONCENTRATION
Sample T ype and Lo c a t io n
Catfish, SL-1
Batch and A nalysis Date D020629,29 Jun 02
Catfish, SL-2
D020629,29 Jun 02
Catfish, SL-3
D020702,02 Jul 02
Large Mouth Bass, SL-1
D020626,26 Jun 02
Large Mouth Bass, SL-2
D020628,28 Jun 02
Large Mouth Bass, SL-3
D020628,28 Jun 02
Small Mouth Bass, SL-3
D020628,28 Jun 02
River Water, SL-1
D020812A, 12 Aug 02
River Water, SL-2
D020812A, 12 Aug 02
River Water, SL-3
D020812A, 12 Aug 02
Low er Limit of Q uantitation (LLO Q )
5.0 ng/g 5.0 ng/g 5.0 ng/g 1.0 ng/g 2.5 ng/g 2.5 ng/g 2.5 ng/g 50 pg/mL* 50 pg/mL* 50 pg/mL*
River Water, SL-1 River Water, SL-2 River Water, SL-3 River Sediment SL-1 River Sediment SL-2 River Sediment SL-3
D020812B, 12 Aug 02 D020812B, 12 Aug 02 D020812B, 12 Aug 02
1021112,12 Nov 02 1021112,12 Nov 02 1021112,12 Nov 02
1.25ng/mL* 1.25ng/mL* 1.25ng/mL* 100pg/g*
100pg/g* 100 pg/g*
* Denotes sample preparation method LLOQ. Method LLOQ = Instrument LLOQ/Method Concentration Factor.
3M Environmental Laboratory
Page 18 of 276
Report E02-0443
Tenn. River Valley Samples
Blanks.
Method blanks, Milli-Q water taken through the solid phase extraction process, provided a measure of method background. In this experiment, they were labeled as "W B". One set was prepared for each location. In the Fish Tissue portion of the experiment, they were run with the Catfish samples. Acceptable values for the blanks were less than 50% of the Lower Lim it Of Quantitation (LLOQ). All method blanks in this study met this criterion.
The Fish Tissue segment of the experiment also contained method blanks for the SPE cartridges. These were labeled as "SB" and consisted of methanol that was used to extract pre-conditioned columns that did not have any sample added. All of these method blanks met the previous criterion.
Solvent blanks/Methanol blanks (methanol injections) provided a measure of instrument contamination. Acceptable solvent blanks must contain levels of target analyte less than 50% of the Lower Limit O f Quantitation (LLOQ). All of the solvent blanks in this study met this criterion except the following:
Note - Solvent Blanks that were before the System Suitability injections and did not pass the criteria are not recorded below.
D020626 extracted samples 0050 (PFBS, PFHS, and PFOA) and 0051 (PFHS). These were caused by carryover from higher level standard curve points. The solvent blanks that were run after these points showed minimal carryover.
D020628 sample 0051 (PFBS, PFHS, and PFOA), 0052 (PFHS), and 0053 (PFHS). This was caused by carryover from the high-level standard curve point. The solvent blanks that were run after showed minimal carryover.
D020629 samples 0059 (PFHS, PFOA, FOSA, and PFOS), 0060 (PFOS), and 0061 (PFHS, PFOA, and PFOS). This was caused by carryover from high-level standard curve points. The 0061 Methanol Blank had a significant level of analytes but this had no effect on the quality of the data. The next sample had trace amounts of analyte and was below the LLOQ for all analytes. Therefore, the 0061 Methanol Blank did not influence the sample. The next solvent blank (0067) had nominal analyte concentration.
D020702 samples 0042 (PFOS), 0059 (PFHS and PFOS), 0060 (PFOS), and 0061 (PFOS). This was caused by carryover from the high-level standard curve point. The solvent blanks that were run after showed minimal carryover.
D020812(A) samples 0016 (PFOA and FOSA) and 0031 (PFOA). These were caused by carryover from higher level standard curve points or system suitability points. The solvent blanks that were run after these points showed minimal carryover. Samples 0037 (PFOA) and 0039 (PFBS, PFHS, and PFOA) had carry-over from samples. Subsequent blanks showed minimal contamination.
1021112 samples 012 (PFBS, PFOA, and FOSA), 027 (PFBS, PFOA, and FOSA), 039(FOSA), 066, (PFOA and FOSA), 068 (FOSA), and 071 (FOSA). All of these can be attributed to carryover from high-level standards or samples.
3M Environmental Laboratory
Page 19 of 276
Report E02-0443
Tenn. River Valley Samples
Data Summary
Tables 7a, 7b, 7c, and 7d present the data for individual samples. Table 8 summarizes the average data for sample groups. Representative chromatograms are presented in Attachment C. Tables 7a, 7b, 7c, and 7d display the on-column and corrected concentrations for individual samples. Also included are the average concentrations for each set of samples standard deviation, and % Coefficient of Variation, when applicable. The final values reported are corrected for dilution/concentration factors introduced during sample preparation and by injection volume differences. The reported values were not adjusted for Matrix Spike Recoveries. When some of the samples within a group were < LLOQ, the average value for the group was calculated using the reported analytical value for samples > LLOQ and the LLOQ value for samples < LLOQ. The abbreviations are as follows: SL - Sample Location, C - Catfish, LM - Large mouth bass, SM - Small mouth bass, RW - River Water, and RS - River Sediment.
3M Environmental Laboratory*
Page 20 of 276
Report E02-0443
Tenn. River Valley Samples
Table 7a. Catfish Analytical Data.
LIMS #
Sample Name
PFBS (ng/g)
42777
42778 42779 42780 42781 42782 42783 42784 42785 42786 42789 42790 42791 42792 42793 42794 42795 42796 42797
SL-1; C-1-1 SL-1; C-1-2 SL-1. C-1-3
SL-1. C-2-1 SL-1. C-2-2 SL-1. C-2-3
SL-1. C-3-1 SL-1. C-3-2 SL-1. C-3-3
SL-1. C-4-1 SL-1. C-4-2 SL-1. C-4-3
SL-1. C-5-1 SL-1. C-5-2 SL-1. C-5-3
SL-1. C-6-1 SL-1. C-6-2 SL-1. C-6-3
SL-2; C-1-1 SL-2; C-1-2 SL-2. C-1-3
SL-2. C-2-1 SL-2. C-2-2 SL-2. C-2-3
SL-2. C-3-1 SL-2. C-3-2 SL-2. C-3-3
SL-2. C-4-1 SL-2. C-4-2 SL-2. C-4-3
SL-2. C-5-1 SL-2. C-5-2 SL-2. C-5-3
SL-2. C-6-1 SL-2. C-6-2 SL-2. C-6-3 SL-2. C-7-1 SL-2. C-7-2 SL-2. C-7-3
SL-3; C-1-1 SL-3; C-1-2 SL-3. C-1-3
SL-3. C-2-1 SL-3. C-2-2 SL-3. C-2-3
SL-3. C-3-1 SL-3. C-3-2 SL-3. C-3-3
SL-3. C-4-1 SL-3. C-4-2 SL-3. C-4-3
SL-3. C-5-1 SL-3. C-5-2 SL-3. C-5-3
SL-3. C-6-1 SL-3. C-6-2 SL-3. C-6-3
<LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
cLLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
<LLOQ cLLOQ <LLOQ <LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
cLLOQ cLLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
<LLOQ cLLOQ <LLOQ
cLLOQ <LLOQ <LLOQ
PFHS
(ng/g)
cLLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
<LLOQ cLLOQ <LLOQ
<LLOQ <l.LOQ cLLOQ
<LLOQ <LLOQ <LLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ <LLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
PFOA
(ng/g)
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ <LLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ CLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
FOSA
On-
column
(ng/g)
5.9 5.3 5.2
4.4 4.2 3.9
7.0 7.1 7.4
3.9 3.7 3.8
9.1 9.1 8.8
7.0 6.9 7.0
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
FOSA
Corr. for
Smpl Prep
(ng/g) 58.7 53.5 52.0
44.5 41.7 39.1
70.5 70.8 73.8
39.3 36.7 38.2
91.0 90.7 87.5
69.8 69.1 69.8
Ave,
Stnd. D
and
%C.V.
54.7 3.49 6.4%
41.8 2.67 6.4%
71.7 1.85 2.6%
38.1 1.30 3.4%
89.8 1.95 2.2%
69.5 0.41 0.6%
PFOS
On-
column
(ng/g)
11.2 10.5 10.0
9.8 9.2 8.6
16.1 17.9 19.2
17.1 16.2 16.6
8.1 8.0 7.8
5.9 6.0 5.9
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
1.9 1.9 1.4
1.2 1.1 1.2
cLLOQ cLLOQ cLLOQ
3.7 3.5 4.0
cLLOQ cLLOQ cLLOQ
cLLOQ 2.3 2.3
PFOS
Corr. for
Smpl Prep
(ng/g)
112.1 104.7 100.3
97.6 91.8 86.1
161.2 179.4 192.4
171.5 161.9 165.8
80.8 80.2 77.5
58.8 59.7 58.7
Ave.
Stnd. D
and
%c.v.
106 6.00 5.7%
91.8 5.77 6.3%
178 15.67 8.8%
166 4.82 2.9%
79.5 1.74 2.2%
59.1 0.57 1.0%
18.8 17 18.7 2.75 14.0 16.0% 11.5 11.7 11.5 0.44 12.2 3.7%
36.9 37.4 35.1 2.72 40.4 7.3%
23.3 23.5 23.2
3M Environmental Laboratory
Page 21 o f 276
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Tenn. River Valley Samples
Table 7b. Large mouth and Small mouth Bass Analytical Data.
LIMS#
Sample Name
PFBS (ng/g)
42798 42799 42800 42801
42802 42803 42804 42805 42806 42807 42808 42809 42810 42811 42812 42813 42814 42815
SL-1; LM-1-1 SL-1; LM-1-2 SL-1. LM-1-3
SL-1. LM-2-1 SL-1. LM-2-2 SL-1. LM-2-3
SL-1. LM-3-1 SL-1. LM-3-2 SL-1. LM-3-3
SL-1. LM-4-1 SL-1. LM-4-2
SL-1. LM-4-3
SL-1. LM-5-1 SL-1. LM-5-2 SL-1. LM-5-3
SL-1. LM-6-1 SL-1. LM-6-2 SL-1. LM-6-3
SL-2; LM-1-1 SL-2; LM-1-2 SL-2. LM-1-3
SL-2. LM-2-1 SL-2. LM-2-2 SL-2. LM-2-3
SL-2. LM-3-1 SL-2. LM-3-2 SL-2. LM-3-3
SL-2. LM-4-1 SL-2. LM-4-2 SL-2. LM-4-3
SL-3; LM-1-1 SL-3; LM-1-2 SL-3. LM-1-3 SL-3. LM-2-1 SL-3. LM-2-2 SL-3. LM-2-3
SL-3. LM-3-1 SL-3. LM-3-2 SL-3. LM-3-3
SL-3. LM-4-1 SL-3. LM-4-2 SL-3. LM-4-3
SL-3. LM-5-1 SL-3. LM-5-2 SL-3. LM-5-3
SL-3. LM-6-1 SL-3. LM-6-2 SL-3. LM-6-3
SL-3. LM-7-1 SL-3. LM-7-2 SL-3. LM-7-3
SL-3. SM-1-1 SL-3. SM-1-2 SL-3. SM-1-3
<LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ cLLOQ
<LLOQ <LLOQ
<LLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ CLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
PFHS (ng/g)
<LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ
cLLOQ cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ CLLOQ cLLOQ cLLOQ cLLOQ CLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
PFOA
(ng/g)
<LLOQ <LLOQ <LLOQ
<LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ cLLOQ
6.4
cLLOQ cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ CLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ CLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
PFOA Corrected for Smpl
Prep (ng/g)
64.3 (Eliminated via Q-Test)
FOSA Corrected
(ng/g)
<LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ cLLOQ cLLOQ
PFOS On-
column
(ng/g)
18.5 13.0 14.0 63.6 61.4 57.2 73.2 80.8 82.4 68.8 75.7
cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
CLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ CLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
65.3
46.6 41.5 38.9
69.3 59.9 66.0
cLLOQ cLLOQ cLLOQ
2.6 cLLOQ cLLOQ
9.7 11.8 8.5
53.1 54.1 56.9
cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ CLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
cLLOQ cLLOQ cLLOQ
PFOS Corrected for Smpl
Prep (ng/g) 185.5 130.0 139.7 635.5 614.0 571.7 732.1 807.7 824.4 688.4 757.0
653.3 465.5 415.0 388.7 693.2 599.1 660.2
25.6
96.7 117.6 84.7 530.8 540.9 569.4
152 29.61 19.5% 607 32.49 5.4% 788 49.18 6.2% 700 52.70
7.5% 423 39.03 9.2% 651 47.78 7.3%
100 16.68 16.7% 547 20.02 3.7%
3M Environmental Laboratory
Page 22 of 276
Report E02-0443
Tenn. River Valley Samples
Table 7c. River W ater Analytical Data.
LIMS #
38025 38026 38033 38034 38037 38038
LIM S#
38025 38026 38033 38034 38037 38038
LIM S#
38025 38026 38033 38034 38037 38038
LIM S#
38025 38026 38033 38034 38037 38038
LIMS #
38025 38026 38033 38034 38037 38038
Sample Name
SW01 SWOl-Dup
SW03 SW03-Dup
SW02 SW02-Dup
. PF,B (ng/mL)
3.0 3.7
<LLOQ <LLOQ
<LLOQ <LLOQ
Sample Name
SW01 SWOl-Dup
SW03 SW03-Dup
SW02 SW02-Dup
, PF,HS (ng/mL)
7.7 8.0
<LLOQ <LLOQ <LLOQ <LLOQ
Sample Name
SW01 SWOl-Dup
SW03 SW03-Dup
SW02 SW02-Dup
Sample Name
SW01 SWOl-Dup
SW03 SW03-Dup
SW02 SW02-Dup
Sample Name
SW01 SWOl-Dup
SW03 SW03-Dup
SW02 SW02-Dup
, PF,A
<n9 /mL) 21.3 22.7
<LLOQ <LLOQ <LLOQ <LLOQ
.
, F S/\ (ng,mL)
1.0 1.0 <LLOQ <LLOQ <LLOQ <LLOQ
PFOS /,
(ng/mL)
18.5 20.8 <LLOQ <LLOQ <LLOQ <LLOQ
Adjusted for Inj. Vol.
(ng/mL)
1.50 1.85
Adjusted for Sample Prep.
(Pg/mL)
75 93
Adjusted for Inj. Vol.
(ng/mL)
3.86 3.98
Adjusted for Sample Prep.
(pg/mL)
193 199
Adjusted for Inj. Vol.
(ng/mL) 10.66 11.33
Adjusted for Sample Prep.
(pg/mL) 533 566
Adjusted for Inj. Vol.
(ng/mL) 0.48 0.51
Adjusted for Sample Prep.
(pg/mL) 24 26
Adjusted for Inj. Vol.
(ng/mL)
9.25 10.40
Adjusted for Sample Prep.
(pg/mL)
462 520
. f ve,ra? (pg/mL)
84
<LLOQ
<LLOQ
. * ve,raga <Pg/mL)
196
<LLOQ
<LLOQ
.
<Pg/mL) 550
<LLOQ
<LLOQ
. ? ve,ra?? (pg/mL)
25
<LLOQ
<LLOQ
Avpraoe Average <Pg,mL)
491
<LLOQ
<LLOQ
The sample extracts were analyzed several times using different sized injection volumes in order to match the appropriate analytical ranges for extracted samples, matrix spikes, and calibration curves. Table 7c incorporates data using 20 uL extracted sample injection volumes, 2 uL matrix spike injection volumes, and 10 uL calibration curve injection volumes.
3M Environmental Laboratory
Page 23 of 276
Report E02-0443
Table 7d. River Sediment Analytical Data.
Tenn. River Valley Samples
Summaries for the average analyte concentration per sampling group and location are given below.
3M Environmental Laboratory
Page 24 of 276
Report E02-0443
Tenn. River Valley Samples
Table 8. Sample Location, Sample Type, and Analytical Data Summary. Fish Tissue
Sampling Location & Species Sampled
PFBS (ng/g)
PFHS (ng/g)
PFOA (ng/g)
FOSA (ng/g)
PFOS (ng/g)
SL-1, C (n=6) SL-2, C (n=7) SL-3, C (n=6 SL-1, LM (n=6) SL-2, LM (n=4) SL-3, LM (n=7) SL-3, SM (n=1)
<LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ
<LLOQ
<LLOQ
<LLOQ
<LLOQ
<LLOQ
<LLOQ
<LLOQ
<LLOQ1
<LLOQ
<LLOQ
<LLOQ
<LLOQ
<LLOQ
<LLOQ
River Water
60.9 (6/6)2 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ
113 (6/6)2 <LLOQ
15.2 (4/6)2 553 (6/6)2 169 2/4)2
<LLOQ <LLOQ
PFBS (pg/m L)
PFHS (pg/m L)
PFOA (pg/m L)
FOSA (pg/m L)
PFOS (pg/m L)
SL-1, RW SL-2, RW SL-3, RW
84 <LLOQ <LLOQ
196 550
<LLOQ
<LLOQ
<LLOQ
<LLOQ
River Sediments
25 <LLOQ <LLOQ
491 <LLOQ <LLOQ
PFBS
PFHS
PFOA
FOSA
PFOS
(pg/g)
(pg/g)
(pg/g)
(pg/g)
(pg/g)
SL-1, RS
I 577
130
732
1440
3130
SL-2, RS
437
<LLOQ
<LLOQ
141
457
SL-3, RS 452 <LLOQ 127 68 416
C = CatFish, LM *=Large mouth bass, SM = Small mouth bass, RW River water, and RS = River Sediments. ' High triplicate value was statistically eliminated using Dixon's Q-Test. 2(Number of Fish > LLO Q I Number of Fish Analyzed). Only one River W ater and one River Sediment sample were collected from each sampling location.
Attachment B contains additional data summary tables.
Statistical Methods
Statistical methods were limited to calculating averages, standard deviations, % coefficient of variation and statistical examination of outlying data points using Dixon's Q-Test.
3M Environmerttal Laboratory,
Page 25 of 276
Report E02-0443
Tenn. River Valley Samples
Statement of Conclusion
Fish Tissue:
Fish tissue obtained from Sample Location 1 contained quantifiable levels o f FOSA and PFOS. Fish tissue obtained from Sample Locations 2 and 3 contained quantifiable levels of PFOS only.
River Water:
W ater from Sampling Location 1 contained quantifiable levels of PFBS, PFHS, PFOA, FOSA, and PFOS. W ater obtained from sample Locations 2 and 3 did not contain quantifiable levels of analytes.
River Sediments:
River Sediment obtained at Sample Location 1 contained quantifiable levels of PFBS, PFHS, PFOA, FOSA, and PFOS. River Sediment obtained at sample Location 2 contained quantifiable levels of PFBS, FOSA, and PFOS. River Sediment obtained at sample Location 3 contained quantifiable levels of PFBS, PFOA, FOSA, and PFOS.
References
1. 3M Environmental Method ETS-8-155.1 "Analysis of Waste Stream, W ater Extracts Or Other Systems Using HPLC-Electrospray/Mass Spectrometry".
List of Attachments
Attachment A: Analytical Method and SOP Deviations Attachment B: Data Summary Tables Attachment C: Sample Chromatograms Attachment D: Sample Prep Sheets, Test Substance, and Test System Information Attachment E: Notes to File
Report Revisions
Typographical errors for the unit designators for Tables 1 ,6a-e, 7a, 7b, 7d, and 8 were corrected. The number o ffish sampled at each location was also added to Tables 1 and 8. The descriptions of the sampling locations were adjusted in the summary and in tables 3a, 3b, and 3c to reflect those reported In the Entrix report, July, 2003 (project #178401). Removed two values for PFHS in river water in tables 1 and 8 because they were <LLOQ. Re-calculated average values for PFOS in fish at sampling locations 2 and 3 and PFOA in sediment at sampling location 3 in tables 1 and 8 using LLOQ values for samples < LLOQ.
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Signature Page
We certify that this report is a true and complete representation of the data for this study:
William K. Reagen, Testing Facility Management
0 7 //Z ./0 3
Date
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A ttachment A: A nalytical Method and SOP Deviations
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3M Environmental Laboratory
Method Analysis of Waste Stream, Water Extracts or Other Systems Using
HPLC-Electrospray/Mass Spectrometry
Method Number: ETS-8-155.1
Author. Mark L. Anderson, Mark E. Ellefson Approved By:
Adoption Date: |/ / & I 00 Revision Date: C /3 0 ( *
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1.0 Scope and Application_____________________
1.1 Scope: This method describes the analysis of waste stream, water samples or other systems using HPLC-electrospray/mass spectrometry. 1.1.1 Specific analytes, ions, matrices, solvents, solutions, quality controls, internal standard(s) and other parameters will be defined in the protocol or the sample preparation worksheet(s).
1.2 Applicable Compounds: Electrospray ionizable compounds.
13 Matrices: 1.3.1 Waste Streams and other systems may consist o f aqueous and/or organic solvent systems or as designated in the protocol or sample preparation worksheet(s). 1.3.2 Water Samples include tap water, ground water, wastewater and other aqueous solutions. The matrix will be defined by the protocol or sample preparation worksheet(s).
2.0 Summary of Method__________________________________
2.1 This method describes the analysis of electrospray ionizable compounds, using HPLCelectrospray mass spectrometry (HPLC-ES/MS). The analysis is performed by the mass selection o f a single ion characteristic of a particular compound.
3.0 Definitions_____________________________________________________________
3.1 Atm ospheric Pressure Ionization (API): Commercially available HPLC-ES/MS single quadrupole systems allow for various methods o f ionization by utilizing a variety o f sources, probes, and interfaces. These include but are not limited to: Electrospray Ionization (ESI), Atmospheric Pressure chemical Ionization (APcI), Thermospray, etc. The ionization in these processes occurs at atmospheric pressure (i.e., not under a vacuum).
3.2 Electrospray Ionization (ES, ESI): A method o f ionization performed at atmospheric pressure, whereby ions in solution are transferred to the gas phase via tiny charged droplets. These droplets are produced by the application of a strong electrical field.
3 3 M ass Spectrom eter (MS): Commercially manufactured MS systems are equipped with single quadrupole mass selective detectors. Ions are selected on the basis of mass to charge ratio (m/z) and subsequently detected.
3.4 M icrom ass MassLynx / HP ChemStation Software: System software designed for the specific operation of an HPLC-ES/MS. Please refer to the manual for the specific instrument software.
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4.0 W arnings and Cautions
4.1 H ealth and Safety W arnings:
4.1.1 Use caution with the voltage cables for the electrospray probe. When engaged, the probe employs a voltage o f approximately 5000 Volts.
4.1.2 When handling samples or solvents wear appropriate protective clothing, gloves, and eyewear.
4.2 Cautions: 4.2.1 Operate solvent pumps below a backpressure o f 400 bar (5800 psi). If the backpressure exceeds 400 bar, the HP1100 will initiate automatic shutdown. 4.2.2 Do not run solvent pumps to dryness.
5.0 Interferences______ _________________________________
5.1 To minimize interferences when analyzing samples, Teflon should not be used for sample storage or any part o f instrumentation that comes in contact with the sample or extract.
6.0 EQUIPMENT______________________________________________ ___________ __ 6.1 Equipment listed below may be modified in order to optimize the system. Document any
modifications in the raw data as method deviations. 6.1.1 Micromass Platform LCZ Mass Spectrometer (or equivalent) equipped with an
electrospray ionization source. 6.1.2 HP 1100 low pulse solvent pump, solvent degasser, column compartment, and
autosampler of equivalent HPLC system.
7.0 S u p p l i e s a n d M a t e r i a l s ______________ ______________________________________________________ 7.1 Supplies
7.1.1 High purity grade nitrogen gas regulated to approximately 100 psi (or house air system.).
7.1.2 HPLC analytical column, such as a Betasil C l8 column (50x2mm, 5 pm particle size) or equivalent.
7.1.3 Capped autovials or capped 15 mL centrifuge tubes.
8.0 Reagents and Standards________________________________________________ 8.1 Reagents:
8.1.1 Methanol, HPLC grade or equivalent.
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8.1.2 Milli-QTM water (ASTM type I), all water used in this method should be Milli-QTM water or equivalent, and may be provided by a Milli-Q TOC Plus system or another vendor.
8.13 Ammonium acetate, reagent grade or equivalent.
8.1.3.1 When preparing different amounts than those listed, adjust accordingly.
8.1.3.2 2.0 mM ammonium acetate solution: Weigh approximately 0.300 g ammonium acetate. Pour into a 2000 L volumetric flask, add the appropriate volume o f Milli-Q water, mix until all solids are dissolved. Store at room temperature.
8.1.4 Other solvents and solutions may be used as stated in the protocol or the sample preparation worksheet.
8.2 Calibration Standards:
8.2.1 Typically two method blanks (Milli-Q water), two matrix blanks, and a minimum o f 5 solvent standards are analyzed with each group of samples.
9.0 Sample Handling______________________________________
9.1 Standards and prepared samples may be stored in capped autovials, capped 15 mL centrifuge tubes or other suitable containers until analysis.
9.2 If analysis will be delayed, standards and prepared samples may be refrigerated at approximately 4 C until analyses can be performed (refrigerator temperatures may have a detrimental affect on the solubility o f saturated solutions).
10.0 Q uality Control________________ ___________________
10.1 Blanks:
10.1.1 Solvent blanks, method blanks, and matrix blanks are prepared and analyzed with each sample set to determine contamination or carryover.
10.1.1.1
When the study matrices consist of highly purified solvents such as Type 1 water or HPLC grade organic solvents, the method and matrix blanks may be represented by a single solvent blank.
10.1.2 Solvent blanks should be analyzed prior to each calibration curve. Method blanks and matrix blanks should be analyzed after the initial calibration curve but prior to the study samples. If carryover is a problem, consecutive solvent blanks may be necessary.
10.2 M atrix Spikes:
103.1 Matrix spikes may be prepared for each set o f extracted samples (if applicable to the study) and analyzed to determine extraction efficiency.
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10.2.2 Matrix spike duplicates may be prepared periodically to measure the precision associated with the analysis.
10.23 Analyze the matrix spike and matrix spike duplicate (if prepared) in the same run as the original sample.
10.2.4 Matrix spike and matrix spike duplicate concentrations should fall in the mid range o f the initial calibration curve or should be prepared at 1.5-5 times the endogenous concentration of the analyte. Spike concentrations should fall in the low-range o f the initial calibration curve if extremely low levels are expected.
10.3 Continuing Calibration Verifications:
10.3.1 Continuing calibration verifications (CCV) are analyzed to verify the continued accuracy o f the calibration curve.
10.3.2 Analyze a mid-range calibration standard after every tenth sample, with a minimum o f one per sample set.
10.4 Internal Standard/Surrogate Standard:
10.4.1 An internal standard (IS) may be used to quantify the target analytes by establishing a relationship between the ratio o f analyte response to IS response and a known concentration o f the analyte o f interest. The IS should be spiked at an amount that will fall within the mid-range of the calibration curve. The IS should be added after the extraction process and before analysis.
10.4.2 A surrogate standard may be used for quality control. The surrogate is used to quantitatively evaluate the entire analytical procedure including sample preparation and analysis. The surrogate should be spiked at the beginning o f the sample preparation and should fall within the low to mid-range o f the calibration curve.
11.0 Calibration and Standardization_______________________________________
11.1 Analyze the standard curves prior to and following each set of samples. The average o f two standard curves may be plotted by linear regression (y = mx + b) weighted 1/x, or quadratic fit (y - ax2+ bx + c) using MassLynx or other suitable software. The calibration curves should not be forced through zero.
11.1.1 The closing calibration curve may be excluded if the CCV's meet acceptable criteria. If only the first curve is used, the calibration and standardization parameters are the same.
11.2 I f the initial calibration curve does not meet acceptance criteria perform routine maintenance or prepare a new standard curve (if necessary) and reanalyze.
11.3 For purposes of accuracy when quantitating low levels o f analyte, it may be necessary to use the low end o f the calibration curve rather than the full range. Example: when
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attempting to quantitate approximately 10 ppb o f analyte, generate a calibration curve consisting o f the standards from 5 ppb to 100 ppb rather than the full range of the curve (5 ppb to 1000 ppb). This will reduce inaccuracy attributed to linear regression weighting o f high concentration standards.
11.4 High and/or low points may be excluded from the calibration curves to provide a better fit over the linear range appropriate to the data or because they did not meet the pre determined acceptance criteria. Low-level curve points should also be excluded if their area counts are not at least twice that of the method blanks. Justification for exclusion o f calibration curve points will be noted in the raw data.
11.4.1 A minimum o f 5 points will be used to construct the calibration curve.
12.0 Procedures____________________________________________________________
12.1 Acquisition set-up - please reference the SOP that pertains to the specific instrument. Actual parameters will be recorded on the instrument printouts.
12.1.1 Set up the sample list.
12.1.1.1
Assign a sample list filename using the first letter of the name o f the instrument (T for Tucker), the year (00 for 2000), the month (04 for April), and the day (T001012 for October 12,2000 on Tucker). If more than one list is made on the same day, use increasing letters of the alphabet starting with A at the end of the list.
12.1.1.2 Assign a method (MS) file.
12.1.1.3 Assign an HPLC program (Inlet file).
12.1.1.4 Type in sample descriptions and vial position numbers.
12.1.2 To create a method, click on method in the Acquisition control panel then mass spectrometer headings and select SIR. Set ionization mode as appropriate and mass to 499 or other appropriate masses. A full scan is usually collected in addition to the SIRs. Save acquisition method. See the Micromass MassLynx GUIDE TO DATA ACQUISITION for additional information.
12.1.3 Typically the analytical batch run sequence begins and ends with a set o f solvent standards.
12.1.4 Samples are analyzed with a continuing calibration verification (CCV) injected after every tenth sample. Solvent blanks should be analyzed periodically to monitor for possible analyte carryover.
12.2 Using the Autosampler/Column Heater
12.2.1 Place sample vials into the sample tray according to the sample list prepared in Section 12.1.1.
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12.2.2 Attach the proper analytical column in the column heater compartment, fusing the switching valve, ensure that the tubing is runto the appropriate ports.
12.3 Using the Inlet E ditor
12.3.1 Set-up the HP 1100 using the following conditions or at conditions the analyst considers appropriate for optimal response. Record actual conditions in the instrument logbook:
123.1.1 Sample size = 10 jiL injection
1 2 3 .1 3 Flow rate = 300 pL/min.
1 2 3 .1 3 Cycle time = 10.0 minutes
123.1.4
Mobile phase components:
Solvent A: 2.0 mM Ammonium Acetate in Water
Solvent B: Methanol (MeOH)
Solvent Gradient: Time (min.)
%B
0.00 5.00 %
1.00 5.00%
4.50 95.0 %
8.00 95.0 %
8.50 5.00 %
10.0 Stop
12.4 Instrument Set-up
12.4.1 Refer to the Platform LCZ User's Guide, the MassLynx NT User's Guide, the ETS-9-36, "Operation and Maintenance o f the Micromass Platform LCZ Electrospray/Mass Spectrometer", or the SOP that pertains to the specific instrument
12.4.2 Check the solvent level in reservoirs and refill if necessary.
12.43 Check the tip o f the stainless steel capillary at the end of the probe with an eyepiece. The tip should be flat with no jagged edges. If the tip is found to be unsatisfactory, disassemble the probe and replace the stainless steel capillary.
12.4.4 Turn on the nebulizing gas.
12.4.5 Open the tune page. Click on `Operate' to initiate the desolvation heaters.
12.4.6 Open the Inlet Editor.
12.4.6.1 Set HPLC pump to "On".
12.4.6.2 Set the solvent flow to the desired flow rate.
12.4.6.3
Observe droplets coming out o f the tip of the probe. A fine mist should be expelled with no nebulizing gas leaking around the tip o f the probe. Readjust the tip of the probe if no mist is observed.
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12.4.6.4 Allow to equilibrate for at least 10 minutes.
12.4.7 The instrument uses these parameters at the following settings. These settings may change in order to optimize the response. Actual parameters will be recorded on the instrument printouts.
12.4.7.1 Drying gas 250-425 liters/hour
12.4.7.2 ESI nebulizing gas 10-15 liters/hour
12.4.7.3 HPLC constant flow mode, flow rate 10 - 500 pL/min
12.4.7.4 Pressure <400 bar (This parameter is not set, it is a guide to ensure the HPLC is operating correctly.)
12.4.7.5 Source Block temperature 150.
12.4.7.6 Desolvation temperature 250.
12.4.8 Print the tune page with its parameters, the Inlet page, sample list, mass spectrometer information, and all other applicable information and store it in the study binder with copies taped into the instrument run logbook.
12.4.8.1 All copies must be initialed and dated.
12.4.9 Click on start button on the MassLynx toolbar. Ensure beginning and ending sample numbers encompass all samples to be analyzed.
13.0 Data Analysis and Calculations___________________________________________ 13.1 Calculations (including, but not limited to):
13.1.1 Calculate matrix spike percent recoveries using the following equation:
% Recovery = Observed Result - Background Result x 100 Expected Result
13.1.2 Calculate percent difference using the following equation: % Difference *= Expected Cone. - Calculated Cone, x 100 Expected Cone.
13.1.3 Calculate actual concentration o f analyte in matrix (pg/mL): On-Column Concentration (pg/mL) x Dilution Factors = Calculated Concentration
14.0 Method Performance___________________________________________________
14.1 The Limit o f Quantitation (LOQ) is method, analyte, and matrix specific. For many analytes, the LOQ concentration is selected as the lowest acceptable non-zero standard in the calibration curve.
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14.2 Solvent and method blank area counts must be < Vi that of the lowest standard used in the calibration curve.
1 43 The coefficient o f determination (r2) value for the calibration curve must be greater than or equal to 0.980.
14.4 Continuing Calibration Verification (CCV) percent recoveries must be 30% o f the standard concentration.
14.5 Internal Standard recoveries should be within 50% of the spiked concentration.
14.6 If criteria listed in this method performance section are not met, maintenance may be performed on the system and samples reanalyzed or other actions as determined by the analyst. Document all actions in the raw data.
14.7 If data is to be reported when performance criteria have not been met, the data must be footnoted on tables and discussed in the text o f the report
15.0 Pollution Prevention and Waste Management
________ __
15.1 Sample extract waste and flammable solvent is disposed in high BTU containers, and glass pipette waste is disposed in broken glass containers located in the laboratory.
16.0 Recorps__________________________________________________________
16.1 Each page generated for a study must have the following information included either in the header or hand written on the page: study or project number, acquisition method, integration method, sample name, extraction date, dilution factor (if applicable), and analyst.
16.2 Print the tune page, sample list, acquisition method and all other applicable information to include in the appropriate study folder. Copy these pages and tape into the instrument run logbook.
163 Plot the calibrationcurve thenprintthese graphs and store in the study folder.
16.4 Print data integration summary, integration method, and chromatograms and file in the study binder.
16.5 Summarize data using suitable software and store in the study binder.
16.6 Back-up electronic data to appropriate medium. Record the file names and location o f backed-up electronic data in the study binder.
16.7 Documentation of analyte(s) and all reference substances will include trace numbers, lot # 's, purity, expiration, and storage conditions.
17.0 Attachments ________ _________________________________________________ 17.1 None
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18.0 References
18.1 Platform LCZ User's Guide, Micromass UK Limited, Tudor Road, Altrincham, W A14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom.
18.2 MassLynx NT User's Guide, Micromass UK Limited, Tudor Road, Altrincham, WA14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom.
18.3 MassLynx NT Guide To Data Acquisition, Micromass UK Limited, Tudor Road, Altrincham, WA14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom.
18.4 ETS-9-34.0, "Operation and Maintenance of Hewlett Packard HPLC 1100 System Equipped with a Mass Spectrometer Detector and/or a Photo Diode Array Detector".
18.5 ETS-9-36.0, "Operation and Maintenance of the Micromass Platform LCZ Electrospray/Mass Spectrometer".
19.0 Affected Documents___________________________________ 19.1 None
20.0 Revisions
Revision Number
Reason For Revision
Revision Date
1 Title Change
09 May 01
Section 1: Enlarged the scope of the method by including additional matrices. Also added
comments about specific parameters will be defined in the protocol or prep sheets.
Sections 1 and 2: Removed references to specific compounds.
Section 3: Removed paragraph on Conventional vs. Z-Spray probe interface.
Section 3: Changed to allow different systems and software.
Section 8: Added paragraph allowing fo r the use o f alternative solvents and solutions.
Section 9: Broadened the types of storage containers and conditions.
Section 10: Added comments to allow for flexibility in quality controls for different types of
studies and applicability.
Section 11: Added a paragraph allowing for die excluding of the second curve.
Section 11: Added a paragraph (11.4) allowing for the dropping of curve points and minimum
number of curve points needed.
Section 12: Added comments to reference the specific SOP's for set-up.
Section 12: Corrected numbering.
Section 16: Added paragraph on records of analytes and substances.
Section 18: Added reference to the method for the Hewlett-Packard LC/MS.
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Record of Deviation
I. Identification
Study/Project No.
Deviation Type:
(Check one)
TN River Valley E02-0443
SOP
^Method Equipment Procedure
Protocol Other:
Document Number: ETS-4-04.0
Date(s) of occurrence:
H Tu N* II. Description:
3 -- )kc,r j ,9ooX.
Required Procedure/process: ETS-4-04.0 section 4 states, "It is the responsibility of anyone handling samples to record the movement of those samples on the internal chain of custody form."........................................................................................................................................
Actual Procedure/process: The internal chain of custody forms were not generated or used in
the course of this study. ...
....
III. Actions Taken:
(such as amendment issued, SOP revision, etc.)
No additional action will be taken, as the information cannot be recalled so long after the fact.
Recorded By:
/i * w . - , 1 / U - ( i >; L Lk ~ )
IV. Impact on Study / Project
This deviation does not adversely affect the quality of the data.
Date:
J llu U lL
Authorized By: (Studyp ir c to r _ ,/P roject Lead)
"y "c p
/ , <T-L
Date: . /M
'rn ?
3M Environm ental Laboratory
/
_/Deviation No.
(assigned by Study D irector o r Project Lead at the end o f study o r project)
3M Environmental Laboratory
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Attachment B: Data Summary Tables
Tenn. River Valley Samples
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CTt 2*r*f * I K p**<,.
G)
2 m3< 3 3(D ST Q) O
(Q("DU> Ktk) O K3 O)
D020628 Largo Mouth, Extracted Curve
Sample Location 2 and 9
------------- p IBS(1M)
--------------W W S f lW
P fO A (411)
------------- F5A(4M)
P F 0 [4M ]
S am pT ype FUe S am ple Nam
Sample Info
Area
DUDEOOOl.O MaOH Blank
DUDE0002.D MaOH Blank
Sa m p l e OUOE0003.O MaOH Blank
s a m p l e DUDE0004.0 MaOH Blank
OUDE0O05.O MaOH Blank SAMPLE DUDE0006D 02003-50-07
SAMPLE OUDE0007.D 02003-504)7
DUOEOOOSO 02003-50437
DUDE0009D 02003-504)7
Sa m p l e DUD0010D 02003-504)7
SAMPLE DU OE001 I D MaOH Blank
SAMPLE DUDE0012D MaOH Blank
DUDE0013.D MaOH Blank SAMPLE DUDE00U.D 02003-50-01
DUOE001SD 02003-504)2
OUOE0016 D 02003-50433
SAMPLE 00060017 0 02003-504)4
SAMPLE DUDE0018D 02003-5005
SAMPLE DUOE00190 02003-50-06 SAMPLE DUDE0020.0 02003-5007
SAMPLE 00060021 D 02003-5008
s a m p l e DUDE022D 02003-5009 s a m p l e DUDE0023.D 02003-50-10
s a m p l e DUDE0024.D 02003-50-11
s a m p l e DUOE0025D MaOH Blank
SAMPLE DUOE0026 0 MaOH Blank
SAMPLE DUDE0027.D MaOH Blank
Sa m p l e DUDE0028D MaOH Blank
SAMPLE DM 0029. 02003-52-07
SAMPLE DUD60030.D 02003-5207
DUDE0031.0 02003-5207
SAMPLE DUD60032D 02003-5207
SAMPLE DUDE0033D 02003-5207
DUDE0O34. MaOH Blank
SAMPLE DUDE0035.D MaOH Blank
SAMPLE DUDE0O36.D MaOH Blank
SAMPLE DUDE0037.D MaOH Blank
DUDE0038.0 MaOH Blank
DDE039D 02003-52-12
CALIB.2 DUDE0040D 02003-5201
C B .3 0UDE0041.D 02003-5202 CALIB_4 DUDE0042 D 02003-524)3
CALIb 5
CALI8_6
CALJB.7 CALIB 6
DUDE0044 D 02003-5205 DUDE0045 0 02003-5206
DUDE0O46 0 0 2003-5207
CAL8 9 DUDE0047.D 02003-5209
C ALIBJO DUDE0048D 02003-5209
CALIBRI t
02003-52-10
C A L IB J 2 DUDE0050D 02003-52-11 SAMPLE OUDE0051 D MaOH Blank
SAMPLE DUDE0052.D MaOH Blank
SAMPLE DUDE0053 D MaOH Blank
SAMPLE D U 0 E 0054D MaOH Blank
SAMPLE OUDE0055.D SL-2; L M - i- i
SAMPLE DUDE0096.D SL-2; LM-1-1
SAMPLE DUOE0057.D SL-2. LM-1-3
SAMPLE DUOEOOS8.0 SL-2. LM-2-1
SAMPLE DU DE0059.D SL-2 LM-2-2
SAMPLE DUDE0060.D MaOH Blank
SAMPLE OU00061 D SL-2. LM-2-3
SAMPLE DUDE0042.D SL-2. LM-2-MS
MdOH Blank: TN-A-06115: OS Jun 0 2 (ip i); MLA/MEE
50959
MaOH Blank: T N -A 0 6 1 15; 0 5 J i * 02(fpa); MLA/MEE
8821
MaOH Blank: TN-A-06115; 0 5 Jun 02(rps); MLA/MEE
6577
MaOH Blank. TN-A-06115; 0 5 Jun 02(rps); MLA/MEE MaOH Blank
6406 7521
02003-5007; 100 Oppb Fish C uvas; CMC; 20 Jun 02
2097416
02003-5007; 100 Oppb Fish C urvai; CMC; 20 Jun 02
2113063
0 2 0 0 M 0 4 7 ; lOO.Oppb Flu Curvai. CMC: 20 Jun 02 02003-5007; 100 Oppb Fish C urvai; CMC: 20 Jun 02
2096675 2134643
02003-5007; lOO.Oppb Fish C urvai; CMC; 20 Jun 02
2192818
MaOH Blank: T N -A 0 6 1 15,05 Jun 02(rps); MLA/MEE MaOH Blank: TN -A 06115; 05 J u t 02{rp); MLA/MEE
12104 10360
MaOH Blank: T N -A 0 6 1 15; 05 Jun 02(rps); MLA/MEE
9357
02005-5001; 1 Oppb Fish Curves; CMC; 20 Jun 02
40598
02003-5002; 2.5ppb Fish Curvas; CMC; 20 Jun 02 0 2 0 0 3 -5 0 0 3 ,5.0ppt> Fish Curvas: CMC; 20 Jun 02
79832 147223
02003-50-04; lOOppb Fish Curvas; CMC; 20 Jun 02 0 2 0 0 3 -5 0 0 5 ,2 5 .Oppb Fish Curvas; CMC; 20 Jun 02 02003-5006; 50.0ppb Fish Curves; CMC; 2 0 Jun 02 02003-5007: to o oppb Fish Curvet; CMC. 20 Jun 02
278769 648125 1182803 2213027
02003-5008; 2S0.Gppb Fish Curvet; CMC; 20 Jun 02
4687263
02003 -5 0 0 9 :5 0 0 Oppb Fish C uvas; CMC; 20 Jun 02 02003-50-10,750 Oppb Fish Curves. CMC; 20 Jun 02
8112712 10964737
02003-50-11:1000 Oppb F ah Curvai: CMC: 2 0 Jun 02
13967277
MaOH Blank: T N -A 0 6 1 1 5 :05 Jun02(rps); MLA/MEE MaOH Blank: TN-A4J6115; 05 Jun02(rps); MLA/MEE MaOH Blank: TN-A-06115; 05 Jun 02(rps), MLA/MEE
54355 22742 15701
MaOH Blank
9258
Extractad LM Fish C im a . 02003-52-0?. lOOppb. MLA/CMC/MEE. 21 Jun 2136691 Extracted LM F a ft Curva. 02003-5247. lOOppb. MLA/CMC/MEE. 21 Jun 2150469 Extracted LM Fish C u va , 02003-52-07, lOOppb, MLA/CMC/MEE. 21 Jun 2166969
Extracted LM Fish Curve. 02003-524)7, lOOppb, MLA/CMC/MEE, 21 Jun 2173663
Extracted LM Fish Curve. 02003-524)7, lOOppb, MLA/CMC/MEE. 21 Jun 2169627
MaOH Blank: TN-A-06115.05 Jun02(rps); MLA/MEE
17369
MaOH Blank: TN-A-06115; 05 Jun Q2(rps); MLA/MEE
14649
MaOH Blank: TN-A-06115; 05 Jun02(rp$); MLA/MEE
10374
MaOH BlarA MaOH Blank
8462 8692
Extracted LM Fish Curve. 02003-52-12. Oppb, MLA/CMC/MEE. 21J
21067
Extracted LM Fish Curve. 02003-52-01.1ppb. MLA/CMC/MEE. 21J Extracted LM Fish Curve. 0203-52-2,2 Sppb, MLA/CMCWE. 2 Extracted LM Fish Curve. 02003-524)3. Sppb. MLA/CMCA4EE. 21J
60138 91267 167069
Extractad LM Fish Curva, 0 2 0 0 3 -5 2 ^ 4 .10ppb, MLA/CMC/MEE. 21
293200
Extractad LM Fish Curve. 02003-52-05. 25oob. MLA/CMC/MEE. 21 Extractad LM Fish C un. 02003-52-06, 50ppb. MLA/CMC/MEE. 21
658115 1090200
Extracted LM Fish Curva. 02003*524)7. lOOppb. MLA/CMC/MEE. 2 Extracted LM Fish Curve, 02003-52-06,250ppb, MLA/CMC/MEE. 2
2216763 3634649
Extracted LM Fish Curva. 02003-52-09.500oob. MLA/CMC/MEE. 2 Extracted LM Fish C im a . 02003-52-10,750ppb, MLA/CMC/MEE, 2
5724285 8377812
Extractad LM Fish Cuma. 02003-52-11, lOOOopb. MLA/CMC/MEE. MaOH Blank T N -A 8 1 5 .05 Jun 02(rps); MLA/MEE MaOH B la n k TN-A-06115; 05 Jun 02|rps); MLA/MEE
10572544 135270 40632
MaOH B la n k TNA-06115; 05 Jun 02{rps); MLA/MEE
21066
MaOH Blank Term. R iver Valley Fish. Prep-17 Jun 02. CMC/MLA 2'jun2
10067 21135
Tann. River Valley Fish. Prep-17 Jun 02. C MC/MLA 20 Jun 02
20629
Tenn. River Valley Fish. Prep-17 Am 02.CM CA4LA 20 Jun 02
19393
Tenn. River Valley Fish Prep-17 Jun 02. CMC/MLA 20 Jun 02
15144
Tenn. River Valley Fish. Prep-17 Jun 02. CM C/M LA 20 J u t 02
16562
MaOH Blame TN-A-06115:05 Ju n 02(ips)- MLA/MEE
12113
Tenn River Valley Fish. Prep. 17 Jun 02. CMC/MLA 20 Jun 02
15081
Tenn. R ive r Valley Fish. Prep-17 J u n 02. C M C /M LA 20 Ju n 02
1128038
Amount itO/mL
%
. __ *TM *
BLOQ
16058
BLOQ
2861
BLOQ
1148
BLOQ
1461
BLOQ
821
96.8
2466503
97.7
2524852
967
2488024
99.0
2519529
102.5
2611526
BLOQ
7369
BLOQ
3422
BLOQ
2233
BLOQ
36790
BLOQ
88911
4 7 170106
10.0
330293
25.2
781797
49.1
1448674
103.7
2681369
0.0 5544628 0.0 9691179
0.0 12472035 0.0 16323761
BLOQ
71782
BLOQ
27172
BLOQ
14497
BLOQ Ava: 6054
9 91 100.5 3299922
999 *5% 3297998
101.0 105.5 3299591
101.3
5% 3303476
101.1
95.5 3312131
BLOQ
16156
BLOQ
10401
BLOQ
4525
BLOQ
3295
BLOQ
2767
569.3
10699
1.3 133% 56215
2 5 102% 112619
5.5 111% 215548
10.6
106% 391865
257 448 103.9
103% 953911 90% 1737156 104% 3395491
246.1 0.0 0.0
99% 6538174* 0% 10427555 0% 13413127
0 0 0% 16208147
4 3 192927
BLOQ
61845
BLOQ
28251
BLOQ
5192
BLOQ
15514
BLOQ
14160
BLOQ
17841
BLOQ
10047
BLOQ
8084
BLOQ
6540
BLOQ
7449
4 M 1873683
Amount ng/m L.
%
aTM
BLOQ
94045
BLOQ
10393
BLOQ
7661
BLOQ
7526
BLOQ
5039
70.4
1089189
722
1122472
710
1115770
72.0
1118688
75.0
1165448
BLOQ
10027
BLOQ
9648
BLOQ
9309
BLOQ
21B88
BLOQ
43348
41 76384
8.4 143140
20 6
346389
39.4
641237
766
1224481
190.7
2662501
0.0 4595891
0.0 5988496
0.0 7595063
BLOQ
37974
BLOQ
19431
BLOQ
14944
BLOQ Ava: 8765
98.1 98.2 1693045
9 8 0 *5% 1663714
98.0
103.1 1665818
96.2
S% 1678355
9 8 5 93.2 1676355
BLOQ
15166
BLOQ
12972
BLOQ
10380
BLOQ
6851
BLOQ
6723
786.2
17661
1.1 111% 60008
2 6 104% 100860 5 3 106% 148026
10.0 100% 216321
25.4 101% 501075
479
96% 896792
101.4 101% 1709566
249.7 00 00
100% 3296780 0% 5372557 0% 6707917
0 0 0% 8094275
4.7 96235
BLOQ
39500
BLOQ
23914
BLOQ
6530
BLOQ
35273
BLOQ
41609
BLOQ
56954
BLOQ
25432
BLOQ
26800
BLOQ
11928
BLOQ
29311
43.1
86% 799701
ng/m L
%
,, Ana
BLOQ
12386
BLOQ
1862
BLOQ
0
BLOQ
0
BLOQ
0
601 2504397
622
2553024
61.8
2539110
620
2523163
649 2603526
BLOQ
8230
BLOQ
3811
BLOQ
2881
BLOQ
29094
BLOQ
68096
BLOQ
135045
BLOQ 165
267223 684935
33.2
68.7
178.5
0.0 10742575 0.0
0.0 18518442
BLOQ
73021
BLOQ
26674
BLOQ
17654
BLOQ A va : 15076
100.1
98.9 3057430
98.1 5% 2996627
9 8 2 103.8 2985961
9 9 1 -S% 2975217
98 9
93 9 2979648
BLOQ
14625
BLOQ
7774
BLOQ
4250
BLOQ
3749
BLOQ 815 7
3214
0.9 91% 120484
3.1 124% 167037 5 6 113% 232969 9.3 93%
25.2 48.3 101.3
101% 786600 97% 101% 3006870
249.6 100% 6431172
0 0 0% 10931270 0.0 0%
0 0 0%
BLOQ
BLOQ
36081
BLOQ
BLOQ . BL.Q "
24175
BLOQ
BLOQ
BLOQ
BLOQ
62964
BLOQ
5513
BLOQ
42.8 1 8 % 1431878
Amount nolm L
BLOQ BLOQ BLOQ BLOQ BLOQ 66.1 860 87.4 668 89 8 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ
6.4 208
%. 1809908 125681
2332782 2378213 2357322 2373987 110224 114843
190043
805138
487.1
0.0 BLOQ BLOQ BLOQ BLOQ 107.0 104.8 104.3 1039 1040 BLOQ BLOQ BLOQ BLOQ BLOQ
120883 A v a : 106711
+5% 1100
5% 996
4287052
99223
1 S 145% 3 0 121% 5 3 106% 1411190
24 3
97%
105 2 2478 500 5
105% 4366004 10Q% 11659265
00
BLOQ
BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 47.0
--
113317 94% 2749840
Amount no/m L
%
BLOQ
356 371 364 370 39 9 BLOQ BLOQ BLOQ BLOQ BLOQ
BLOQ BLOQ 1056
46
502 3 .0 %
B LO Q *' *
50.0
100%
t2M7/3003
P9Jof21
Tenn. River Valley Samples
7J *3<ooP-
m
CO
Report E02-0443
Tenn. River Valley Samples
9*3o<2l
3M Environmental Laboratorv
P a n 4? n f ? 7 fi
Report E02-0443
Tenn. River Valley Samples
D020629 Catfish, Extracted Curve
Sim pl Locations 1 and 2
3M Environmental Laboratory
Pane 44 of 276
Report E02-0443
Tenn. River Valley Samples
3M Environmental Laboratory
Pape 45 of 276
Report E02-0443
Tenn. River Valley Samples
>NNNNON J j {
<si:Ss "* "r *" e ; g i ia b oas 3 c i i 5 * 3Jj oo od e- o3 o29o:|^S8S|8o
^
<!? ?
|ljIIIlI=8lligiIiIlIi=Bi3iigs =i||!iii8 i B S I||SiH |i|i5SiS 5l|I|I|||||||s|:i||||
? I ? 2 I l I * " I I I | S l 3 f l l I I f | S= S i ! S S s f I I I 5 j
I*
88888**:9p S S * * - 00
sIllE
S
illS
I
s
S
iS
D020702 CatFish, Extracted Curve
Sample Location I
lII lIS a s l liS Is s IlliflS iiS is s s ilIlilS
SSI
I3I8 l88i
88? 8H?i.
ffi 0
Ili
^ 4 l i88888 S B I
8 8 8 8 8 11**1*
nm8s88;
uuou
SSB-SSsB I | |
BSSSSSSSS
S* *S*S!SSlS3SRS ssssill
41
88
10 A
U SS
M E-*s"I
444bi l i l l S
SSSloooSuoo
11f
r
u
Si gri
t 8f8l8f8t8
555'lllHJ}}; ":ss82l
II fi Hiliiii itlf if r iiiI H ms s s filli
iiiiisiiiiiiiiism iiiii 111iiillSHIIliilllliiii
liili! I l i l l l p l l l l lppoppoooo
23338333333333
o
8
ooQooooooooqoq
333333333833333
oapp n38S8S8i 3S3S3S8S
ouO>o5::QkoaQ oon>
W8 8LU:!t8UU8) L8U
5 :5 a o
331S333
*3!5!5322S2as!BS3aaaaasaa?: u n m m n n n m m u lh m i
.E!aISSa5::IaS5 Sa23aS
I W Vi
3M Environmental Laboratorv
o5);-KpSo;;p?So;;Sp>o:o o o o Do o:!
8188:8 8:8 l i i i i l i l i i i i i i SiS SiS Sis M aaisasB a as
23!:OE!3 S;;1Soegd;m:3 2JS>::3ui sja sis ilg 5i
t3uSuiIifSui i ij| <SS'il
Stugtu3tutgujiigitiji i I i li
5-5
P a n a Aft n f 0 7 K
SampTypa
PU
Swnpto N am t
SAMPLE SAMPLE
SAMPLE
SAMPLE
SAMPLE
SAMPLE SAMPLE
SAMPLE SAMPLE SAMPLE SAMPLE
SAMPLE SAMPLE SAMPLE
DUOEOOMD DUDE0070.0 O U 0E 0071.0 DUOEO072O
DUDBD73.D OUDE0074 o
DD007SO OUOEQ076.D OUOE0077O DUDE007I.D OUOE0079 0 Dpoeoo E o o e io OUOE0O82D DUOE 0 0 6 3 .0 OUOE0064O DUDEOOB5D DE086 DUOE0067D b E ci.o 0UOE 0069.O OUOEOOBOO OUOE0O91.D 0UDE0092 D DUDE0093 0
SL-3. C-2-MS SL-3. 0 3 -1 SL-3. 0 3 -2 SL-3.0 3 -3 02003-64-07 MaOH Blank S L -3 .0 4 -1 SL-3.0 4 -2 SL-3. C-4-3
SL-3.04-M S SL-3. OS-1 MaOH Blank SL-3 0 6 -2 SL-3. 0 5 -3 SL-3. OS-1 SL-3 0 6 -2 SL-3 0 6 -3 0200364-07
MaOH Blank SL-3. C4-MS
SL-3. WB-1 SL-3 W B2 SL-3. SB-1 SL-3. SB-2 02003-64-07
D020702 CatFIsh, Extracted Curve
Sampla Location 3
Sampia W o
Tann. R ivar Vallay Fish. Prap-17 Jun 02. CMCfMLA. 20 Ju n 02 Tann. Rivai Valay ran. Prap-17 Jun 02. CM C IM IA 20 Jun 02 Tann. Rivar VaBay Fiait Prap-17 Jun 02. CMC/MLA 20 Jun 02 Tann. Rime V a ia r Fnh. Prap-17 Jun 02. CMCIMLA. 20 J w i 02 02003-45-07; 100ppb CatFish curva; MLA/CMC/MEE; 21 Jun 02 MaOH Blank: TN-A-06115; 05 Jun 02(rpa): MLA/MEE ta n n . Rivr Vallay Puh. Prap-17 Jun 02. CMC/MLA. 20 Jun 02 T a n t. R im i V a ia r Flah. Prap-17 Jun 02. CUCIMtA. 20 Jun 02 Tann. Rivar Vallay FJah. Prap-17 Jim 02. CMC/MLA 20 Jen 02
Tann. R ivar V a lla r Flair. Prap-17 Jun 0 2 CUC/MLA. 20 Jun 02 Tarai. Rivar V afey F illi. Prap-17 Jun 02. CMC/MLA 20 Jun 02 MaOH Blank: TN-A4B115; 05 Jun Q2frpi); MLA/MEE Tann. Rivar V a ia r Frali. Prap-17 Jun 02. CMC/MLA. 20 Jun 02 Tann. Rivar Vakay Fish. Prap-17 Jun 02. CMC/MLA. 20 Jun 02 Tann. Rivar VaOay Fish. Prap-17 Jun 02. CMC/MLA. 20 Jun 02 Tann. Rivar VaOay Fish. Prap-17 Jun 02 CMC/MLA. 20 Jun 02 Tann. Rivar V alay Fish. Prap-17 Jun 02. CMC/MLA. 20 Jun 02
02003-45-07; lOOppb CalFish curva; MLA/CMC/MEE; 21 ju n 02 MaOH Blank: TN-A46115; 05 Jun 02(rps); MLA/MEE
Tann. R iv VaHay Fteh. Prap-17 Jun 02. CMCIMUL 20 Ju n 02 Tann. Rivar VaOay Fish. Prap-17 Jun 02. CMC/MLA. 20 Jun 02 Term. Rivar VaOay Fish Prap-17 Jun 02. CMC/MLA 20 Jim 02 Tann. Rivar VaOay Fish. Prap-17 Jun 02. CMC/MLA. 20 Jun 03 Tann River VaOay Fish. Prap-17 Jun 02. CMC/MLA 20 Jun 02 0203*45-o: io p p b CioFkih curva; MLMC/MEE; 21 Jun 2
"FFBS (44)
Aras
Amount
%
1511507 24320 16540 24807
2333052 16062 17195 21375 16443
1510215 10806 11100 16001 15727 0 13227 12338
2300088 18148
1587590 25327 20971 16148 17484
2317083
Hl
BLOQ BLOQ BLOQ 99.4 BLOQ BLOQ BLOQ BLOQ 1.4 BLOQ BLOQ BLOQ BLOQ BLOQ 8LOQ BLOQ 97.8 BLOQ S4J BLOQ BLOQ BLOQ BLOQ 96.7
129% 99% 123%
98% 129% 99%
2262593 6020 5270 3605
4563714 12313 5789 3965 3417
2210130 7747 3871 3303 3630 0 2199 2077
4413612 11187
2023286 7877 3347 3074 1442
4430280
PFH51J M i
Amount ng /m L
47.0 BLOQ BLOQ BLOQ 101.3 BLOQ BLOQ BLOQ BLOQ 46.4 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 97.4 BLOQ 41.4 BLOQ BLOQ BLOQ BLOQ 97.8
%
4% 101% 1%
97% 3% 98%
1084739 21977 14365 13566 2255277 15890 11833 9130 9515 1006147 12540 10666 19136 11772
0 21296 12192 2239179 15766 1111957 14443 15176 14720 17869 2267607
Amount ng/mL
-- BLOQ BLOQ BLOQ 100.0 BLOQ BLOQ BLOQ BLOQ 40.8 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 99.2 BLOQ 45.4 BLOQ BLOQ BLOQ BLOQ 100.7
POSA U M ) Amount
PFS {4M ) Amount
17% 100% 62%
69% 91% 101%
1795365 " 26327 22632 20526 3638935 10892 26647 20987 26620 2019128 18677 5463 12319 11964
0 22050 19076 3532761 9243 1852522 5535 4520 5445 6879 360S386
in -- BLOQ BLOQ BLOQ 104.0 BLOQ BLOQ BLOQ BLOQ 56.6 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 100.9 BLOQ 51.9
BLOQ BLOQ BLOQ 1030
100% 104%
2301120 164262 165052 159839 4758709 93159
113%
101% 104%
307947 333760 2405599 133232 81061 136306 137529
0 251766 250469 r 4644253 83526 2223094
BLOQ BLOQ
BLOQ BLOQ BLOQ BLOQ
BLOQ 44.4
-- --
103%
75775 76590 4694062
BLOQ 1016
102%
Tenn. River Valley Samples
1X174001
P a n 4P o f P7E
3M Environments! Laboratorv
E02-O443
Tenn. R ivar Valley W ater Samptec
D020812A River Water Samples
Semple Location 1, 2, end 3. Low end o f cuive.
_
Tenn. River Valley Samples
Report E02-0443
02-0443 Tann. R iver Valley W ater Samples
HIS a m p T y p e
Sample Name
SAMPLE SAMPLE
SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE
DUDE0071.D DUDE0072 D DUDE0073D DUDE0074.0 DUDE0075D
DDE0076D DO0E0077O
DU0E0078.D DUOE0O78D UOE0080.D OUOE0081 0 OUOEOOB2.0
DUOEO83.0 0UDEQ084.D DUOE0O85D OUOEOOWO DU OE0 0 8 7 .0
PUOE0O66.O DUDEOO09.D D U O E 0 0 9 0 .0 DUOE0 0 9 1 0
DU0E0092O DUOE0093 0 DUOE00940 0ODE009S0 OUOE0O96.O
38027 MaOH Blank
38029 02003-50-05 MaOH Blank
3803?
MaOH Blank
38033 MaOH Blank
38034 MaOH Blank
w t<
MaOH Blank 38037
MaOH Blank 38038
MaOH Blank 38039
MaOH Blank 38041
MaOH Blank 38043
MaOH B a r*
38047 02003-50-05 MeOH Blank
Sam pla In f
E02-0443-M027; Water Sample: porvGLP: 7/17/02. OK MaH Blanlc TN-A-06115 .0 5 Jun 02(rps): MLA/MEE
E02-044M 8029: W atar Sample: notvG LR 00/02: OK 02003-50^05; 25 Oppb FW i C uivet; CMC; 20 Jun 92 MeOH Blank THA-08115; 09 Jun 02(rp): MLA/MEE
024443*30032: Water Sample: norvGLP; 972002 OK MaOH Blank: TN-A-06115; 05 Jun Q2(mt): MUUMEE
E02^0443-38033; W aler Samplet; non-GLP; 6/20/02; OK MeOH Blenk TN-A-061 IS; 05 Jun 02(rpt>: MLA/MEE
E02-044>-38034. W eier Samplet; non-GLP; 8/20/02; OK MeOH Blenk: TN-A-0611S. 05 Jun Q2(rps): MLA/MEE
E02-0443-38035; Water Samplet: non-GLP; 6/20*02; OK MeOH Blenk: TN-A-06115; OS Jun 02(ipt); MLA/MEE
E02-0443-38037; W aler Samplet; non-GLP; 6/20/02, OK MeOH Blenk; TN-A-06115; 05 Jun 02(fDt): MLA/MEE
E02-0443-38038; W aler Samplet; norvGLP; 6/20/02; OK MeOH Blank. TN-A-061 IS; OS Jun 02(rpt>; MLA/MEE
02-0443-38039; W ila r Samplat; non-GLP; 6/20/02; OK MaOH Blank: TN-A-06115.05 Jun 02(rpt); MLA/MEE
E02-O443-38041; Water Samplet; norvGLP; 6/20/02; OK MaOH Blank: TN-A-06115; 05 Jun 02(rp>): MLA/MEE
E02-0443-38043; Water Samplet; norvGLP; 6/20/02, OK MeOH Blank TN-A-06115; 05 Jun 02(rpt); MUUMEE
E02-0443-36047: W aler Samplat; norvGLP; 6/20/02: OK 02003 50-05; 25 Opp Fh Curvet; CMC; 20 Jun 02 MeOH Blank TN-A-06115; 05 Jun 02(rpt); MUUMEE
D020812A
River Water Samples
Sample Locations 1,2, a n d ). Low and o f curva.
__________ PH35 (299)
PFHSff)
inj. voL (u l)
Amt
Amount ng/niL
% A rta
Amount ng/m L
20 102829
3.1
10
13008
BLOQ
20 89092
2.7
10 724200
26.3
10
13620
BLOQ
20 19361 BLOQ
10 11442 BLOQ
20 26800 BLOQ
10
12025
BLOQ
20 , 28016
BLOQ
10 15199 BLOQ
20 28791 BLOQ
10 12265 BLOQ
20 32546 BLOQ
10 12779 BLOQ
20 34896 BLOQ
10 12019 BLOQ
20 38973 BLOQ
10 12360 BLOQ
20 41348 BLOQ
10
12372
BLOQ
20 32848 BLOQ
10
13840
BLOQ
20 35842 BLOQ
10 721194
26.2
10
15210
BLOQ
1051k 105%
405593 2733
252177 612476
3194 157296
0 5685
666 8673
0 168441
1155 12978
0 8214
0 160575
0 183987
0 16543
0 6361 806664 2279
12.6 BLOQ
7.9 26.6 BLOQ 4.9 BLOQ BLOQ BLOQ BLOQ BLOQ 5.2 BLOQ BLOQ BLOQ BLOQ BLOQ 5.0 BLOQ 5.1 BLOQ BLOQ BLOQ BLOQ 28.4 BLOQ
% 108%
108%
Amt
412129 11372 328881 413005 11620 64190 10679 11537 10246 17031 10432 93950 10273 14081 9659 15139 9665 88104 1045 90881 1Q293 9481 10282 10590 413655 10747
Amount ng /m L
25.0 BLOQ 21.8 260 BLOQ
4.8 BLOQ BLOQ BLOQ BLOQ BLOQ
5.6 BLOQ BLOQ BLOQ BLOQ BLOQ
5.1 BLOQ
5.4 BLOQ BLOQ BLOQ BLOQ 28.1 BLOQ
S am plet wer injtetad I two different inject)on volumet: 10 and 20 u L Ony tha 20 uL Injaction* wre usad for reporting.
% 112%
112%
FOSA (491}
A ra *
Amount ng/m L
%
121332 2566 34000 760492 3670 136473 2582 5487 2219 6747 2137 108416 1871 6547 1764 3452 2043 146553 2297 147415 2080 6471 1671 5664 602001 3062
4.0
BLOQ 1.1 282
BLOQ 4.8
BLOQ BLOQ BLOQ BLOQ BLOQ
3.1 BLOQ BLOQ BLOQ BLOQ BLOQ
4.6 BLOQ
4. BLOQ BLOQ BLOQ BLOQ 289 BLOQ
105% 108%
TTOSW
Amt
Amount ng/m L
%
808339
31385 831568 813299 30284 190157 28784 35066 26273 51049 29174 152206 28491
43851 28142 44198 28231 170640 28058 198423 28951 30951 28000 33414 826526 29397
26.6 BLOQ 202 266 BLOQ
8.2 BLOQ BLOQ BLOQ BLOQ
BLOQ 4.9
BLOQ BLOQ BLOQ BLOQ BLOQ
4.6 BLOQ
5.5 BLOQ BLOQ BLOQ BLOQ 272 BLOQ
107% 109%
7DJ TO33-
rmoo g W
Tenn. River Valley Samples
\mtnaa
ppeel
Report E02-0443
Tenn. River Valley Samples
1021112 River Sediments
Sample Location 1 ,2 , and 3.
Report E02-0443
Tenn. River Valley Samples
1021112
River Sediments
S im p l L o c a tio n s 1, 2, and 3.
---------------- p i T 5 5 T J
SampType
Fife
ki). Vol (UL) Sem ple Name
Sample Info
Area
Amount ng/m L
SAMPLE IT CHY068 0 10
MeOH Ba n k M eOH Blank; TN-A-06264; 12 Sept 02irp>: MLA/MEE
18871
ITC H Y069D 20
0443-36045-4 E02-0443-38045-4; SL-3; MeOH Extract 21 O d02; M U
330170
10 SAMPLE fTCHY071.0 10
02005-50-06 MeOH Blank
0 2 0 03-5006; 50.0ppb Fish Curve; 20Jun02; CMC M eOH Blank: TN-A-06264; 12 Sept 02(rps); MLA/MEE
1617080 21377
i 0443-38045-MS(4) E02-0443-38045-MS(4); SL-3; MeOH E xtra ct 21 O ct 02; M U
456655
SAMPLE ITCHY073D 10
MeOH Blank MeOH Blank: T N -A 0 6 2 4 :12 Sept 02(m s): MLA/MEE
18285
SAMPLE
1
0443-WM Q2-0443-WB-4; W ater B la r * MeOH E xtra ct 21 Oct 02; M U
1603660
SAMPLE ITCHY075.O 10
MeOH Blank MeOH Blank: TN-A-06264; 12 Sept 0 2 fip t): MLAAIEE
20645
SAMPLE ITCHY076.D 10
0443-LCS-4 E02-0443-LCS-4; Lab Control Spike; MeOH Exfcact 21 O ct 02; 4 22710
SAMPLE ITCHY077D 10
MeOH Blank MeOH Blank: T N -A -06264.12 Sept 02(rpl: MLA/MEE
17405
ITCHY078.0 20
4 3 -3 8 0 4 4 -5 E02-0443-36044-5, SL-1; MeOH E xtract 21 Oct 02; M U
497463
SAMPLE ITC H Y 079.0 10
MeOH Blank M eOH Blank; TN-A-06264; 12 Sept 02(rps); MLA/MEE
20039
20 SAMPLE IT C H Y 0 8 1 0 10
0443-38045-5 02-0443^3XM5-5; SL-3: MeOH E xtract 21 Oct 02; M U MeOH Blank M eOH Blank: TN-A-06264; 12 Sapt02(m *1: MLA/MEE
369663 16740
20 0443-38048-5 E 02-0443-38048-5, SL-2; MeOH E xtract 21 Oct 02; M U
436046
SAMPLE ITCHY0B3.D 10
MeOH Blank MeOH Blank.' TN-A-06264; 12 Sept 02(rpa): MLA/MEE
19499
ITCHY64.D 10 M43-38046-MS(5> E02-0443-38046-MS/5); SL-2: MeOH Extract; 21 Oct 02; M U
1606166
10 02003-5006 02003-50-06; 50 Qppb Fish Curve; 20Jun02; CMC
1590860
SAMPLE 1TCHY066D 10
MeOH Blank M eOH B la n k TN-A-06264; 12 Sept 02(rpa); MLA/MEE
24560
SAMPLE TCHY087.D 10 SAMPLE r r c H Y o e s D 10
MeOH Blank MeOH Blank
MeOH B la n k TN-A-06264; 12 Sept 02(rp$); MLA/MEE MeOH Blank; TN-A-06264; 12 Sept 02(rpe); MLA/MEE
19986 22823
BLOQ 90 48.4
BLOQ 12.7 BLOQ 47.9 BLOQ BLOQ BLOQ 13.9 BLOQ 102 BLOQ 12.1 BLOQ 48.0 47.5 BLOQ BLOQ BLOQ
PFHS (5 H |
PFOA (413|
% a ,..
* ng/m L
%
Ana
*nmg /mu*L
97% 25% 96%
2077 31122 2126881 9759 1845453 2720 2143465 9652 25972 1925 105333
BLOQ BLOQ 47.9 BLOQ 41.3 BLOQ 46.3 BLOQ BLOQ BLOQ
2.3
96% 83% 97%
24249 46537 675275 27571 796892 25291 815469 25074 24197 22877 247938
BLOQ BLOQ 62.1 BLOQ 47.6 BLOQ 35 5 BLOQ BLOQ BLOQ 13.4
2395 29644 1796 16686
BLOQ BLOQ BLOQ BLOQ
22062 51340 22796 51651
BLOQ BLOQ BLOQ BLOQ
96% 95%
1830 1578870 2095232
2366 3882 2217
BLOQ 35.1 47.1 BLOQ BLOQ BLOQ
70% 94%
21824 672354 862750 22523 . 21381 23535
BLOQ 39.1 51.3 BLOQ BLOQ BLOQ
a r t not reported, they ere for method development only.
% 104% 94% 71%
78% 103%
ra s rp n r"
----------------- P F G { t t t l --
**"
Amount ng/m L
%
. A r"
Amount ng /m L
%
15965 36022 1911480 12534
886709 451
1234862 539
356694 624
1307614 796
56609 0
135750 0
1100535 1927507
392 0 0
BLOQ 1.0 45.8
BLOQ 210 BLOQ 29.3 BLOQ 8.4 BLOQ 31.1 BLOQ 1.4 BLOQ 3.3 BLOQ 261 46.2 BLOQ BLOQ BLOQ
92% 42%
" *
52% 92%
427165 41842 38769 39305 35140 41633 36038
1949205 36534 34087
93 47 2 BLOQ 43 7 BLOQ " 37.3 " BLOQ
87% " 75% .. .......
BLOQ --
BLOQ
BLOQ
BLOQ 463 47.1 BLOQ
93%
BLOQ
TaXO(D5
m
o
I
g
Tenn. River Valley Samples
Itf CMMwtlil
12/17/3002
Pee# 12721
Report E02-0443
Tenn. River Valley Samples
1021112
River Sediments Sample Locations 1,2, and 3.
PFBS (299)
In). On-Column On-Column Corrected Corrected fo r Average,
Vol Sample Name
Sample Info
Area
Amount
%cvAvarage fo r inj. Vol Sample Prap. Stnd 0 and
(uL)
(ng/mL) (ng/mL) (ng/mL)
(pg/mL)
(pgrmL)
20 0443-30044*1 E02-0443-38044-1; SL-1; 4 383859
10.6
11.6
5.3
529 677
20 0443-36044-2 E02-0443-38044-2: SL-1; 4 383608
10.6
5.3 529 83
20 0443-38044-3 E02-0443-38044-3; SL-1; 4 482034
9.120 0453-38045-1 E02-0443-36045-1 ; SL-3; 4 325254
13.5 6.9
6.7 4.4
673 14% 443 452
20 0453-38045-2 E02-0443-3#05-2; SL-3; 4 305101
8.3
4.1 413 44
20 0453-36045-3 E02-O443-38CM5-3: SL-3; 4 364688
10.0
5.0 500 10%
20 0463-36046-1 E02-0443-38046-1; SL-2; 4 327380
8.9
8.9
4.5
43B 437
20 0463-36046-2 E02-M43-M046-2; SL-2; 4 232749
6.2
3.1 302 134
20 0463-38046-3 E02-0443-36046-3; SL-2; 4 420079
11.7
5.8 571 31%
PFHS (399)
20 0443-38044-1 E02-0443-36044-1; SL-1; 4 122635 20 0443-38044-2 E02-0443-38044-2; SL-1; 4 116901 20 0443-38044-3 E02-0443-38044-3; SL-1; 111724 20 0453-36045-1 E02-0443-38045-1; SL-3; 13341 20 0453-36045-2 02-0443-38045*2; SL-3; 4 11469 20 0453-38045-3 E02-0443-36045-3; SL-3; 12125 20 0463-36046-1 E02-0443-38046-1; SL-2; 17353
2.7 2.6 2.5 BLOQ BLOQ BLOQ BLOQ
2.6 BLOQ BLOQ
1.4 1.3 1.2 BLOQ BLOQ BLOQ BLOQ
136 132 124 BLOQ BLOQ BLOQ BLOQ
130 6 5% BLOQ BLOQ BLOQ BLOQ
20 0463-38046-2 E02-0443-38046-2; SL-2; 18434 20 0463-36046-3 E02-0443-38046-3; SL-2; 25494
BLOQ BLOQ
BLOQ BLOQ
BLOQ BLOQ
BLOQ BLOQ
PFOA (413)
Sample W t (g)
38044 38044-MS
20.0 20 01
38045
20.1
38045-MS 38046
38046-MS
20.30 20.4 19.98
Regular sample are averge* of tna ftwee weights.
=>Average of tripticales
Corrected fo r fnl. Vol. = On-Cot Amount * 0.5
Corrected fo r Sample Preo 9 On-Cot Amount 0.5 2 * 1000
Sample Weight (Ave)
"2" is the Final Vo! of the Extract (mL)
3M Environmental Laboratory
Peg*
Page 53 of 276
Report E02-0443
Tenn. River Valley Samples
E02-0443
Combined Large Mouth Bass Data Table
UMS# 42798 42799 42800 42801 42802 42803 42804 42805 42806 42807 42808 42609
42810
42811 42812 42613 42814 42815
PFBS (299) PFHS (399)
PFOA (413)
Corrected
Sample Amount Amount Amount tor Smpl
Name
ng/mL ng/mL ng/mL
Prep
__________ (ng/mL)
SL-1; LM-1-1 BLOQ BLOQ BLOQ
SL-1; LM-1-2 BLOQ BLOQ BLOQ
SL-1. LM-1-3 BLOQ BLOQ BLOQ
SL-1. LM-2-1 BLOQ BLOQ BLOQ
SL-1. LM-2-2 BLOQ BLOQ BLOQ
SL-1. LM-2-3 BLOQ BLOQ BLOQ
SL-1. LM-3-1 BLOQ SL-1. LM-3-2 BLOQ
BLOQ BLOQ
BLOQ BLOQ
SL-1. LM-3-3 BLOQ BLOQ BLOQ
SL-1. LM-4-1 BLOQ BLOQ BLOQ
SL-1. LM-4-2 BLOQ BLOQ
6.4
64.3
SL-1. LM-4-3 BLOQ BLOQ BLOQ
SL-1. LM-5-1 BLOQ BLOQ BLOQ
SL-1. LM-5-2 BLOQ BLOQ BLOQ
SL-1. LM-5-3 BLOQ BLOQ BLOQ
SL-1. LM-6-1 BLOQ BLOQ BLOQ
SL-1. LM-6-2 BLOQ BLOQ BLOQ
SL-1. LM-6-3 BLOQ BLOQ BLOQ
SL-2; LM-1-1 BLOQ BLOQ BLOQ
SL-2; LM-1-2 BLOQ BLOQ BLOQ
SL-2. LM-1-3 BLOQ BLOQ BLOQ
SL-2. LM-2-1 BLOQ BLOQ BLOQ
SL-2. LM-2-2 BLOQ BLOQ Bl OQ
SL-2. LM-2-3 BLOQ BLOQ BLOQ
SL-2. LM-3-1 BLOQ BLOQ BLOQ
SL-2. LM-3-2 BLOQ BLOQ BLOQ
SL-2. LM-3-3 BLOQ BLOQ BLOQ
SL-2. LM-4-1 BLOQ BLOQ BLOQ
SL-2. LM-4-2 BLOQ BLOQ BLOQ
SL-2. LM-4-3 BLOQ BLOQ BLOQ
SL-3; LM-1-1 BLOQ BLOQ BLOQ
SL-3; LM-1-2 BLOQ BLOQ BLOQ
SL-3. LM-1-3 BLOQ BLOQ BLOQ
SL-3. LM-2-1 BLOQ BLOQ BLOQ
SL-3. LM-2-2 BLOQ BLOQ BLOQ
SL-3. LM-2-3 BLOQ BLOQ BLOQ
SL-3. LM-3-1 BLOQ
BLOQ
BLOQ
SL-3. LM-3-2 BLOQ
BLOQ
BLOQ
SL-3. LM-3-3 BLOQ BLOQ BLOQ
SL-3. LM-4-1 BLOQ BLOQ BLOQ
SL-3. LM-4-2 BLOQ BLOQ BLOQ
SL-3. LM-4-3 BLOQ BLOQ BLOQ
SL-3. LM-5-1 BLOQ BLOQ BLOQ
SL-3. LM-5-2 BLOQ BLOQ BLOQ
SL-3. LM-5-3 BLOQ BLOQ BLOQ
SL-3. LM-6-1 BLOQ BLOQ BLOQ
SL-3. LM-6-2 BLOQ BLOQ BLOQ
SL-3. LM-6-3 BLOQ BLOQ BLOQ
SL-3. LM-7-1 BLOQ BLOQ BLOQ
SL-3. LM-7-2 BLOQ BLOQ BLOQ
SL-3. LM-7-3 BLOQ BLOQ BLOQ
SL-3. SM-1- BLOQ BLOQ BLOQ
SL-3. SM-1-2 BLOQ BLOQ BLOQ
SL-3. SM-1-3 BLOQ BLOQ BLOQ
FOSA (49B)
Amount ng/mL
BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOa BLOQ BLOQ
BLOQ
BLOQ
BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ
Amount ng/mL
18.5 13.0 14.0 63.6 61.4 57.2 73.2 80.8 82.4
68.8 75.7 65.3 46.6 41.5 38.9 69.3 59.9 66.0
BLOQ BLOQ BLOQ
2.6 BLOQ BLOQ
9.7 11.8 8.5 53.1 54.1 56.9 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ
BLOQ
BLOQ
BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ
PFOS (499) Corrected tor Smpl Prep (ng/mL) 185.5 130.0 139.7 635.5 614.0 571.7 732.1 807.7 824.4 688.4 757.0 653.3 465.5 415.0 388.7 693.2 599.1 660.2
25.6
96.7 117.6 84.7 530.8 540.9 569.4
Ave, Stnd Dev, and
%CV
152 29.61 19.5% 607 32.49 5.4% 788 49.1B 6 .2% 700 52.70 7.5% 423 39.03 9.2% 651 47.78 7.3%
100 16.68 16.7% 547 20.02 3.7%
Corrected for sample prep. Amount (ng/mL) * 10
3M Confidential
___________ SL-1, LM________
____________ PFOA
PFOS
Average (ppb) : 64.3
553.4
Stnd. D.: NA
220
12/17/2002
SL-2, LM _____________ PFOS Average (ppb) : 280.8
Stnd. D.: 251
Pag* 14 0/21
3M Environmental Laboratory
Page 54 of 276
Report E02-0443
Tenn. River Valley Samples
E02-0443
Combined CatFish Data Table
PFBS (299) PFHS (399) PFOA (413)
UM S#
Sample Name
Amount ng/m L
Am ount ng/m L
Amount ng/m L
42777 42778 42779 42760 42781 42782 42763 42784 42785 42786 42789 42790 42791 42792 42793 42794
42795 42796 42797
SL-1; C-1-1 SL-1; C-1-2 SL-1. C-1-3 SL-1.C-2-1 SL-1. C-2-2 SL-1. C-2-3 SL-1. C-3-1 SL-1. C-3-2 SL-1. C-3-3 SL-1. C-4-1 SL-1. C-4-2 SL-1. C-4-3 SL-1. C-5-1 SL-1. C-5-2 SL-1. C-5-3 SL-1. C-6-1 SL-1. C-6-2 SL-1. C-6-3 SL-2; C-1-1
SL-2; C-1-2 SL-2. C-1-3 SL-2. C-2-1
SL-2. C-2-2 SL-2. C-2-3 SL-2. C-3-1 SL-2. C-3-2 SL-2. C-3-3 SL-2. C-4-1 SL-2. C-4-2 SL-2. C-4-3 SL-2. C-5-1 SL-2. C-5-2 SL-2. C-5-3 SL-2. C-6-1 SL-2. C-6-2 SL-2. C-6-3 SL-2. C-7-1 SL-2. C-7-2 SL-2. C-7-3
SL-3; C-1-1 SL-3; C-1-2 SL-3. C-1-3 SL-3. C-2-1 SL-3. C-2-2 SL-3. C-2-3 SL-3. C-3-1 SL-3. C-3-2 SL-3. C-3-3 SL-3. C-4-1 SL-3. C-4-2 SL-3. C-4-3 SL-3. C-5-1 SL-3. C-5-2 SL-3. C-5-3 SL-3. C-6-1 SL-3. C-6-2 SL-3. C-6-3
BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ
BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ
BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ
BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ
BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ
BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ
Amount ng/m L
5.9 5.3 5.2 4.4 4.2 3.9 7.0 7.1 7.4 3.9 3.7 3.8 9.1 9.1 8.8 7.0 6.9 7.0 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ
FOSA (498)
Corrected fo r Smpl
Prep (ng/m L)
58.7 53.5 52.0 44.5 41.7 39.1 70.5 70.8 73.8 39.3 36.7 38.2 91.0 90.7 87.5 69.8 69.1 69.8
Ave, Stnd Dev, and
%CV
54.7 349 6.4% 41.8 2.67 6.4% 71.7 1.85 2.6% 38.1 1.30 3.4% 89.8 1.95 2.2% 69.5 0.41 0.6%
Amount ng/m L
11.2 10.5 10.0 9.8 9.2 8.6 16.1 17.9 19.2 17.1 16.2 16.6 8.1 8.0 7.8 5.9 6.0 5.9 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ
1.9 1.9 1.4 1.2 1.1 1.2 BLOQ BLOQ BLOQ 3.7 3.5 4.0 BLOQ BLOQ BLOQ BLOQ 2.3 2.3
PFOS (499)
Corrected for Smpl
Prep (n g /m L )
112.1 104.7 100.3 97.6 91.6 66.1 161.2 179.4 192.4 171.5 161.9 165.8 80.6 80.2 77.5 56.8 59.7 58.7
Ave, Stnd Dev, and
%CV
106 6.00 5.7% 91.8 5.77 6.3% 178 15.67 8.6% 166 4.82 2.9% 79.5 1.74 2.2% 59.1 0.57 1.0%
18.6 18.7 14.0 11.5 11.5 12.2
17.21 2.75 16.0% 11.73 0.44 3.7%
36.9 35.1 40.4
37.45 2.72 7.3%
23.5 232
23.32 0.19 0.6%
C orrected foramtedtd.
* Am ount (ng/mL) * 10
________________SL-1, C____________
FOSA
PFOS
Average (ppb) :
60.9
113.4
Stnd. D.:
16.6
46.6
_________ SL-3, C ________________ PFOS
Average (ppb) ; Stnd. D.:
22.3 10.6
M Eflwrw im nM laboratory
12/17/2003
Rege 1Sof21
3M Environmental Laboratory
Page 55 of 276
Report E02-0443
E02-0443 Fish Tissu* Matrix Splk* % R*cov*ri*s
-Column Amount Ino/mL) Triedcalt Aw n a a tno/m 50 nQftnL Final C one Spika
Tenn. River Valley Samples
Report E02-0443
1021112
Condensed River Sediments Data Table
On- On-Col. Corrected Cone. Corrected fo r Cone. Corrected fo r Spike or MS - Endogenous
Sample Name ln|. Description Column fo r In je c t Vol.
In). Vot. And
In). Vol., Dilution, and M S% C orrected MS %
Vol
(ng/mL)*
(ng/mL)
Dilution (ng/mL) Sample W t (pg/mL) Recovery
Recovery
PFBS (299)
0443-WB 0443-38044 0443-38044-MS(3) 0453-38045 0453-38045-MS(3) 0453-38046 0463-38046>MS(3)
10 20 10 20 10 20 10
Water Blank Site #1
Site 1 MS Site #3
Site #3 MS Site #2
Site 2 MS
BLOQ 11.6 40.6 9.1 45.9 8 .9 39.2
5.8 40.6 4.5 4S.9 4.5 39.2
PFHS (399)
0443-WB 0443-38044 0443-38044-MS(3) 0453-38045 0453-38045-MSO) 0463-38046 0453-38046-MS(3)
10 20 10 20 10 20 10
Water Blank Site#1
Site 1 MS Site #3
Site #3 MS Site #2
Site #2 MS
BLOQ 2.6 30.7
BLOQ 37.8 BLOQ 38.7
BLOQ 1.3 30.7
BLOQ 37.8 BLOQ 36.7
PFOA (413)
0443-WB 0443-38044 0443-38044-MS(3) 0453-36045 0453-38045-MS(3) 0463-38046 0483-38046-MS(3)
10
20 10
20
10
20 10
Water Blank Site #1
Site IM S Site 3
Site 3 MS Site 2
Site 2 MS
BLOQ 14.7 38.4 2.6 40.3
BLOQ 41.1
BLOQ 7.3 38.4 1.3 40.3
BLOQ 41.1
FOSA (498)
0443-WB 0443-38044 0443-38044-MS(3) 0453-38045 0453-38046-MS(3) 0463-38046 0463-38046-MS(3)
10
20
10
20
10
20
10
Water Blank Site #1
Site 1 MS Site 3
Site 3 MS Site 2
Site 2 MS
BLOQ 26.8 32.0 1.4 26.9 2.0 28.8
BLOQ 14.4 32.0 0.7 25.9 1.4 28.6
PFOS (499)
0443-WB 0443-38044
10 Water Blank 20 Site #1
1.1 62.8
043-3044-MS(3) 0453-38045
04S3-38046-MSP) 0463-38046
1C 20 10 20
Site 1 MS Site 3
Site 3 MS Site 2
51.9 8.3 29.9 9.3
0463-38046-MS(3) 10
Site 2 MS
30.9
* Are averages except for the MS unless noted.
BLOQ * Below Limit of Quantitation
0453*38045, PFOA is a single point
1.1 31.4
51.9 4.2 29.9 4.7 30.9
11.8 81.3 9.1 91.9 6.9 78.3
BLOQ 2.6 61.4
BLOQ 75.6 BLOQ 73.4
BLOQ 14.7 76.7
2.6
80.6 BLOQ 62.1
BLOQ 28.8 63.9 1.4 51.8 2.9 57.3
2.2 62.8 103.9 6.3 59.8 9.3 61.8
577 4062 452 4591 437 3913
BLOQ 130 3068
BLOQ 3779 BLOQ 3667
BLOQ 732 3834 131 4026
BLOQ 4103
BLOQ 1439 3194
68 2587 141 2863
2182 3132 5193 416 2990 457 3086
81% 92% 78%
70% 63% 69%
61% 76% 73%
59%
77% 61% 62%
62% 78%
64% 52% 57%
35% 50% 54%
104% 60% 62%
41% 51% 52%
Sampla W t ( a )
Final Extract Volum (mL)
38044
20.0
38044-MS
20.01
38045
20.1
38045-MS 38046
20.30 20.4
38046-MS
19.98
Regular amples are avergas of the three weights.
On-Col. Corrected fo r In le c t Vol. (ng/m L)
* On-Column * 0.5 The inject Voi factor is oniy for the regular samples. 0.5 is the InJ. Voi factor.
Cone. Corrected fo r Ini, Vol. And D ilutio n (no/m U
On-Column * 0.5 * Final Extract Vol.
Cone. C orrected fo r In i. Vol.. OHutton, and Sam ple W t (p flfm U
On-Column * 0.5 * Final Extract Vol. * 1000 Sample W t
Solke or MS % Recovery
On-Column MS 50
MS - Endooeous Corrected MS % Recovery
a OrvCoiumn MS - On-Col Corrected for Inject Vol. Smut 50
Full Hat o f sam ple w t (g)
38044-1
20.04
38044-2 38044-3 38044-MS
20.06 20.00 20.01
38045-1
20.08
38046-2
20.04
38045-3
2007
38045-MS
2030
38046-1
20 13
38045-2 38046-3 38046-MS
20.98 20.21 19.96
Average fa) 20.0 20.1 20.4
- - Tenn. River Valley Samples
SMConfidenti!
12/17/2002
Page 17 of 21
E02-0443
River Sediment* Matrix Spike % Recoveries
P F B S (299)
PFHS (399)
PFOA (413)
FOSA (499)
PFOS (499)
Sam ple Nam e
Sam ple In fo
A m ount (ng/m L)
T rip lic a te A ve ra g e (ng/m L)
0443*38044 Sample Location 1. River Sediments Average
0 443-36044-M S O )
S am ple Location 1, R iver Sedim ents
0453*38045 Sam ple Location 3, River Sediments Average
0 4 S 3 -39045-M S (3)
Sample Location 3. River Sediments
0463*36046 Sample Location 2, River Sediments Average
0463-38046*M S (3 )
Sample Location 2, River Sediments
40.6 45.9 39.2
5.6 4.5 4.5
C orrected MS%
R e c o v e ry
70%
83%
69%
Amount (ng/m L)
T rip lic a te Average (ng/m L)
30.7 37.8 36.7
1.3 BLOQ BLOQ
C orrected MS %
R e c o v e ry
59%
76% 73%
Am ount (ng/m L)
T rip lc e te A verage (ng/m L)
38.4 40.3 41.1
7.3 13 BLOQ
C orrected MS%
R e c o v e ry
Am ount (ng/m L)
T riplicate A v e ra g e (ng/m L)
62% 78% 82%
32.0 25.9 28.6
14.4 0.7 1.4
C orrected US%
R e c o v e ry
A m ount (ng/m L)
T riplicate Average (ng/m L)
35% 50% 54%
51.9 29 9 309
31.4 42 4.7
C orrected MS %
R ecovery
41%
51% 52%
Calculated fin a l concentrations o f M Ss targeted to 50 n g /m L Triplicate everages are from the Condensed River Sediments Data Tables.
C o rre cte d MS R ecoveries I f th e T rip lic a te A verage Is B LO Q , then A m o u il fno/m u
50 ng/m L Final Cone. Spike e ls e : * Am ount fn o /m U - Triplicate Average (ng/mL)
50 ng/m L Final C o n e Spike
A m ount (ng/m L) h a s b e e n co rre c te d fo r th e in jection volum e. These calculations are found on the C ondensed River Sedim ents D ate Table.
* oa<o9.
otmo
j c.u*>
I
Tenn. River Valley Samples
3M Confidnti*l
12/17/2002
Pag I I of 21
Sequence
File
0020812 0020112 D020812 D020S12 D020812 0020812 D020812 0020812 D020812 D020812 D020812 0020812 0020812 D020812
0020012 D020812 0020812 D020812 D020612
DUDE0067.D DUDE00S8.D DUDE0071.D DUDE0073.D DUDE0076D DUDE0076.D DUDE0080.D DUDE0082.D DUOE0084.D DUDE0086.D DUOE0068.D DUDE0090.D DUDE0092D DUDE0094.D
DUDE0127.0 DUOE0130.D DUDE0133.D DUDE0136 D DUDE0139.D
LIM S *
38025 38028 38027 38029 38032 38033 38034 38035 38037 38038 38039 38041 38043 38047
38028 38030 38036 38040 38042
D e s c rip tio n
SW01 S W O i-O u p S W O l-Low FCSOI-Low
FB02 SW03 SW03-DUP SW03-LOW SW02 SW02-Dup SW02-LOW FSC02-LOW Trip Blank #1 Trip Blank #2
SW01-Med FSC01-Med SW03-Med SW02-Med FSC02-Med
E02-0443
Combined River Water Data Table
fnj. Voi. (uL) 20 20 20 20 20. 20 20 20 20 20 20 20 20 20
p m--------------
(299)--------------
PFHS (399)
Am ount On-
Amount On-
C o lu m n ng/mL
A djusted for InJ. V oi. ng/m L
C o lum n ng/m L
A djusted fo r Inj. Voi. ng/m L
3.0 3.7 3.1 2.7 BLOQ BLOQ
1.50 1.85 1.57 1.33
7.7 8.0 12.8 7.9 4.9 BLOQ
3.86 3.98 6.40 3.93 2.43
BLOQ BLOQ BLOQ BLOQ BLOQ
0.3 0.13 5.2 2.60 0.4 0.20 0.2 0.12 5.0 2.46
BLOQ BLOQ BLOQ
5.1 BLOQ BLOQ
2.53
PFO A (413)
Am ount OnAdjusted fo r
Colum n Inj. Voi. ng/mL
ng/m L
21.3 22.7 28.0 21.B 4.9 BLOQ BLOQ 5.8 BLOQ BLOQ 5.1 5.4 BLOQ BLOQ
10.66 11.33 13.98 10.92 2.47
2.80
2.54 2.69
F O (498)
Am ount OnC o lu m n
ng/m L
1.0
Adjusted fo r Inj. Voi. ng/m L
0.48
1.0 0.51 4.0 2.00
1.1 4.6 BLOQ
0.56 2.28
BLOQ
3.6 BLOQ BLOQ
1.79
4.8 2 4 2 4.9 2.43
BLOQ
BLOQ
2 BLOQ 2 BLOQ 2 BLOQ 2 BLOQ 2 BLOQ
392.6 424.9 404.9 415.9 413.1
1963 2124 2024 2079 2066
388.4 427.9 398.5 407.6 416.9
1942 2139 1992 2038 2085
302.1 300.2 324.5 299.2 303.3
1511 1501 1623 1496 1542
PFOS (499)
Am ount OnAdjusted for
Colum n Inj. Voi. ng/m L
ng/m L
18.5 20.8 26.6 20.2 52 BLOQ BLOQ 4.9 BLOQ BLOQ 46 5.5 BLOQ BLOQ
9.25 10.40 13.29 10.09 2.59
2.47
2~23 2.73
361.8 423.7 365.3 358.0 426.8
1809 2118 1626 1790 2134
g
l
Tenn. River Valley Samples
3M Confidential
12/17/2002
Page 19
Report E02-0443
Term. River Valley Samples
E02-0443
Condensed River Water Data Table
LlM S #
38025 38028 38033 38034 38037 38038 38028 38030 38036 38040 38042
38025 38026 38033 38034 38037 38038 38028 38030 38036 58040 38042
38025 38026 38033 36034 38037 38038 38028 38030 38036 38040 38042
38025 38026 38033 38034 38037 38038 38028 38030 38036 36040 38042
38025 38026 36033 38034 38037 38038 38028 38030 38036 38040 38042
Sampl* Nnw
SW01 SW01-Dup
SW03 SW03-Dup
SW02 SW02-Dup SW01-Med FSC01*Med SW03-Med SW02-Med FSC02-Med
SW01 SWOl-Dup
SW03 SW03-Dup
SW02 SW02-Dup SWOl-Med FSC01-Med SW03-Med SW02-Med FSC02-Med
SW01 SWOl-Dup
SW03 SW03-Dup
SW02 SW02-DUP SWOl-Med FSC01-Med SW03-Med SW02-Med FSC02-Med
SW01 S W O l- D u p
SW03 SW03-DUP
SW02 SW02-DUP SW01-Med FSC01-Med SW03-Med SW02-Med FSC02-Med
SW01 SWOl-Dup
SW03 SW03-Dup
SW02 SWD2-Dup SW01-Med FSCOI-Med SW03Med SW02-Med FSC02-Med
PFBS (299)
InJ. Voi. (uL)
20 20 20 . 20 20 20 2 2 2 2 2
Am. ou, nt On- A. .d.just.e.d.fo r
(n q /m U
Vol. (ng/mL)
3.0 3.7 <LOQ <100 <LOQ <LOQ
<LOQ <10Q <LOQ <LOQ <OQ
PFHS (399)
1.50 1.85
Adjusted for Sample Prep.
(p q /m U 75 93
20 7.7
3.86
20 8.0
3.98
20 <LOQ
20 0.3
0.13
20 0.4
0.20
20 0.2
0.12
2 392.6
1963
2 424.9
2124
2 404.9
2024
2 415.9
2079
2 413.1
2066
PFOA (413)
193 199
6.5 9.0 6.2
20 21.3
10.66
20 22.7 20 <10Q 20 <100
11.33
20 <LOQ 20 <LOQ
2 386.4 2 427.9
1942 2139
2 398.5
1992
2 407.6 2 416.9
2036 2065
FOSA (498)
533 566
20 1.0 20 1.0 20 <LOQ
0.48 0.51
20 <LOQ
20 <LOQ
20 <LOQ
2 302.1
1511
2 300.2
1501
2 324.5
1623
2 299.2
1496
2 308.3
1542
PFOS (499)
24 26
20 18.5 20 20.8 20 <LOQ 20 < 1 0 0 20 <LOQ 20 <LOO
2 361.8 2 423.7 2 365.3 2 358.0 2 426.8
9.25 10.40
1809 2118 1826 1790 2134
462 520
84 <LOQ <LOQ
196 6.5 6.0
550 <LOQ <LOQ
25 <LOQ <LOQ
491 <LOQ <LOQ
I sI ci
Adjusted fo r Int. Vol Inoim U For 20 uL injections A m ount/2 For 2 uL injections Amount *5
Adjusted for Sample Prao fpq/mLI - (Adjusted for In). Vol. / 20) * 1000 20 is the factor of original concentration 1000 is the conversion from op to pg.
3M ConSds n ia l
12/17/2002
P9* 2 0 o r21
3M Environmental Laboratory
Pane 60 of ?7fi
Report E02-0443
Tenn. River Valley Samples
E02-0443
Tenn. River Valley Samples
Summary Table
Catfish, Sample Location 1
Catfish, Sample Location 2
Catfish, Sample Location 3
Large Mouth, Sample Location 1
Large Mouth, Sample Location 2
Large Mouth, Sample Location 3
Small Mouth, Sample Location 1
River Water, Sample Location 1
River Water, Sample Location 2
River Water, Sample Location 3
River Sediments, Sample Location 1 River Sediments, Sample Location 2 River Sediments, Sample Location 3
PFBS (ng/mL)
<LOQ
Location Averages
PFHS (n g /m L )
PFOA (ng/mL)
FOSA (ng/mL)
<LOQ
<LOQ
60.9
<LOQ
<LOQ
<LOQ
<LOQ
<LOQ
<LOQ
<LOQ
<LOQ
<LOQ
<LOQ
64.3
<LOQ
<LOQ
<LOQ
<LOQ
<LOQ
<LOQ
<LOQ
<LOQ
<LOQ
<LOQ
<LOQ
PFBS
PFHS
(p g /m L )-, (pg/mL)
84 196
<LOQ
PFOA (pg/mL)
550
<LOQ
FOSA (Pg/mL)
25
<LOQ
8
<LOQ
<LOQ
<LOQ
7
PFBS . . PFHS
(ng/mL)
(n g /m L )
576.9
130.5
<LOQ
<LOQ
PF0A
FOSA
(ng/mL) ; .' (ng/mL)
732.4
1439.0
436.9
<LOQ
<LOQ
141,4
452.0
<LOQ
130.5
68.0
PFOS (ng/mL)
113
<LOQ
22.3
553
281
<LOQ
<LOQ PFOS (pg/mL)
491
<LOQ
<LOQ PFOS (ng/mL) 3132.3
457.3
416.2
The Fish Tissue results are calculated by taking the average of the averages. Please refer to Combined Large Mouth and Catfish Data Tables for averages of samples.
3M Confidential 3M Environmental Laboratory
12/17/2002
Page 21 of 21 Page 61 of 276
Report E02-0443
Tenn. River Valley Samples
m o
05 Cl
D020626Extracted CCV Calculation PFBS ..........
Solvent Curve: 02003-50 Sequence: D020626Extracted......................................................................
la t m -1
K
t` e V
Of
d
Od
O
d
o
d
Od
dd
-fio
b
d
dOj
' dd
iHBglB^
ft
a
a
in
do
in
d
0.
CTOtdo
E
C* m<<oam
in cm*
miCCnMOaCoMCccMMbo" MoiC1n--Oicnq
a<o
1
isflOcC<TOo0" CCC<OOO0 ssCCOOcnactooo
N(0CM0OI Si s
NatacCo0oOo
o
*
MBB cmin
g
d
ooiCnMoooda
go
do
oooidCnMooooidn
ooo
d
86
1 *- o
r f
V
T"
-
-
-
-
-
-
-
I sa 020
cVeCCCoMMOoCCCtoOOOCsChcOOo- tcaacooo
CO0
sco I
a
taacorc-ooo*o*
I-V" r" - - - - - - -
ffa * aCMin o iCnMoin Too- CmoMmoo
i
2
o 3a3
m
so3
COr COa oLoUoLoUoUoJ UJ O3 O3 a3 o3
OQa Q
oo3CUoooMJ TCOD3OLoMU- COUO3COMMJ to3COUOooMJ
3M Environmental Laboratory
1 101% I [ 99% I
- 1 .6 5 |
o o
Ooo Oo oo
Oo o Oo o
I
|
D U D E 0 0 6 5 I 2 4 8 3 3 5 8 I| 1 0 1 . 1 1 |
S g A jj
a cq
in cq
a cq
a cq
a cq
a cq
9 9 .4 4
9 9 .7 0
I 2 4 4 5 6 3 4 I|
I 2 4 5 1 6 2 2 |I
f
it *
oo V"
h o
CoO
oo
UJ UJ
Q
33
Q
Page 62 of 276
3n
Report E02-0443
Tenn. River Valley Samples
Page 2 ot 5
12/12/2002
D020626Extracted CCV Calculation PFHS
_____________________ ____ _______0 0 : 1
".
B oo
t?O' O O O d d
K a o p- 0 p d d d 0
60 dd
V.
c> t v co cm CM < <
? 10 s d
*-> d
B ss an? r
8 to 8 *CM"
"IT
T*
CO cn M to
0
s 2?CM
to (O
0 S to
CO to T --
[ip*
H *
I sCM CN p* hO a> cn s
CCMO CM
CM 8
tCoO CM
0 8
CO 0 > CO
0) O
0 CM s
O
0
O d
! I H i -
no
m
0
8 O0
n
to
6 T-
to CM 8
O O O d 0
d 08 0O dd to 0
O O O d
00 0 d
CM in
*- O
| | r p- T- - -
* - T" -
ig o HI+
8 CM to
M LU MV r --
CM 3
n to
r f CM h -
1 CO ' f
IP 11
P <9 .0 d
i f f lv
BH H tNt
CM
o>
I* CM O
K CO
8 CM
CM
to CM
0 CCOO
i s0
he'
Oo>
en o>
CO 8 o> S0
f jj^ B ^ T" T " - V T
p* T" -
to 0
to O (M to
0 0 -
O0
to CM
0 to
i 's
l g k <0 * to CO r*. co o> O
CM CO
CM CM CM CM
0 0S
0
8
0
0 0
0 0
0 0
OO Oa
O OO
s Ul s UlS a l 8 iu tu
U l LU LU LU
O Oi l t O Q O O O
gkW 3
H n :.. 0
3 0
3 Q
3 O
3
3 O
3 a
3
O
3
O
3
O
3M Environmental Laboratory
1 103% 1
I D U D E 0 0 7 8 1 I 3 0 4 5 7 4 9 |1 1 0 3 . 3 3 |I_______1 2 5 ______ 11 1 0 3 % |
| 102% |
- 1 .5 6 | - 1 .5 6 |
0 0 0 O0 0 0
! 3 0 0 8 9 3 2 |1 1 0 1 . 9 5 1
1_____ 2 L i : _____ !
O O
iV CN CO O
8 CtoO CtoO
tCoO tCoO
1 3043366 j
i
PtKfc-
to 0CO 0 IU O 3
Q
C0O 0 UJ a 3 0
Page 63 of 276
3M Confidential
Solvent Curve: 02003-50 Sequence: D020626Extractetl
paoe g4 0f 275
3M Environmental Laboratory
Solvent Curve: 02003-50 Sequence: D020626Extracted
DUDE0013 DUDE0014 DUDE0015
DUDE0016 DUDE0017 OUDE0018 DUOEO019 DUDE0020 DUDE0021 DUDE0022 DUDE0023
1 2.5 5 10 25 50 100 250 500
1 1 1 1 1 1 1 1 1 1 1
D020626Extracted
CCV Calculation
PFOA
25542 51665 94999 182546 422134 765880 1368745 2938643 4830576
" -1 1.000 ?
25542
1
2.500 .?
51665
* 1 ' v 5.000 > 94999 .
' ,1 ' 10.000
182546
1
25.000
422134
1 50.000 : 765880
1 . 100.000 1368745
1
250.000
2938643
1
500.000
4830576
1
0.000
: 0 : >
1 0.000
0
-0 39 1.47 4.57 -8.6 10.87 . 8.7 28.38 13.5 J 54.23 8.5' 10192 1.9 245.43 -1;8 501.83 0.4 -2.21 -2.21
Ol 0*1
0.0- . O.O.-
0.0'
. .0.0 o.o 0.0 < 0.0 .
. - 0.0- v,. . 0.0
000
-8 90E+00 biSiM- 1403L9727
31085.7902
"file.*!. * DUDE0065 DUDE0078 DUOE0081
; rpna*ji> cis&iroin;**?* 1459295 109.37 1486918 111.66 1477410 110.87
-2.21 -2.21 -2.21
-2.21 -2.21 -2.21 -2.21
100 100 100
109% 112% 111%.:
0. 0. 0 .0 0 0 0
3M Confidential
12/12/2002
Page 3 of 5
Tenn. River Valley Samples
Report E02-0443
Page 65 of 276
3M Environmental Laboratory
Solvent Curve: 02003-50 Sequence: D020626Extracted
DUDE0013 OUOEQ014 UDE0015 DUOE001S DUDE0017 DUDE0018 DUDE0019 OUDE0020 DUDE0021 DUDE0022 DUDE0023
1 2.5 5 10 25 50 100 250 500
1 1 1 1 1 1 1 1 1 1 1
D020626Extracted
C C V Calculation
FOSA
29611 71308 136118 275178 693598 1376588 2665321 6144958 11083740
:...1 :
1.000 ;
.-29611
1 . ! ..
2.50 . - ; 71308
5.000
136118
-'.'-I" 10.000;
275178 ....
1 25.000 ; 693598
1
50.000
1376588
1 100.000 2665321
1
250.000
6144958
1 500.000 11083740
1 0.000
0
1 0.000
0
1
0
0.73 0.0 1
2.26 -9.4
0.0
4.65 -7.0
0.0'
9.79 ?Z1 ... 0.0 .
25.36 : 1.4
0.0
51.19 2.4- - o.o o y
101.39 . 1.4 .:o.O" .
248.44 -0.6 ' 0.0 ;-
500.40. 0.1
o.ov -
-0.36
0.0 -
-0.36
t m
. 0.00
Saas -i.o2E*oi 272231456 9701.53073
I
DUDE0065 2677359 DUDE0078 2644901 DUDE0081 2687949
101.87 100.58 102.29 -0.36 -0.36 -0.36 -0.36 -0.36 -0.36 -0.36
100 102% 100 101% 100 102%
0 0 o ..
0 0 0 0
3M Confidential
12/12/2002
Page 4 of 5
Tenn. River Valley Samples
Report E02-0443
D020626Extracted
CC V Calculation
Solvent Curve: 02003-50
PFOS
Sequence: P020626Extracted______________________________________________________ _
DUDE0013 DUDE0014 DUDE0015
DUDE0016 DUDE0017 DUDE0018 DUDE0019 DUDE0020 DUDE0021 DUDE0022 DUDE0023
1 2.5
5 10 25 50 100 250 500 750
1
284722 .
1 , .-, : i.ooo * " ^ 7 2 2 ' -2.13
T T vo T r
1 326649
1 2.500. ... 326649.,. . 0.32
' , 0.0 -, :
1 407979 .. , / T : v : V 5:000 407979. ' ^ :3.56<-
- " 0.0 ,
1 578578
1 . 10.000 ; 578578
10.37, 3.7 .. ^ - o .a 1.,,.
1 1046115
1 . 25.000
1046115
29.25 17.0 . 0.0 -
1 1748100 -1
50.000
1748100 - 58.22 16.4 t * 0.0 '
1 2980202
1 ; 100,000 : 2980202
111.03 11.0.
o.o" '.
1
6053335
. y 250.000
6053335
256.37 2.5 .. .'O'.'V.i
1 9834704
1
500.000
9834704
477.48 -4.5 - ' 0.0 ..
1 13136147
1
750.000
13136147
764.72 2.0
0.0 -
1
1 0.000
0 -1257
0.0 i;.
1
0 .0.001
r n m r n -I .10E+01 25197.8029
e g S g s 318501.997
DUDE0065 3038328 DUDE0078 3004248 UOE0081 2998564
113.59 112.09 111.84 -1257 -12.57 -12.57 -12.57 -12.57 -12.57 -12.57
100 114% 100 112% 100 112%
0 0 0 0. 0. 0 0
3M Confidential
12/12/2002
Page 5 of 5
- _ Tenn. River Valley Samples
Report E02-0443
Report E02-0443
Attachment C: Sample Chromatograms
Tenn. River Valley Samples
3M Environmental Laboratory
Page 67 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: DUDE0056.D Report Date: 27-Aug-2002 13:27
Page 1
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file \\Etstarget\target\chem\dudejr.i\D020626Extracted.b\DUDE0056.D
Lab Smp Id SL -1. LM-1-3
Inj Date
26- JUN-2002 23:16
Operator
mla
Inst ID: dudejr.i
Smp Info
Tenn. Ri ve r Va l l e y Fish. Prep-17 Ju n 02. CMC/MLA. 20 Ju n 02
Mise Info
Comment
Method Meth Date Cal Date Als bottle
\ \ E t s t a r g e t \ t a r g e t \ c h e m \ d u d e j r .i\D02062 6E xt rac te d. b\ D02 0 6 2 6extra 27- Aug-200213:22 dudejr.i Quant Type: ESTD
26-JUN-2002 22:00
Cal File: DUDE0049.D
43
Dil Factor 1.00000
Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds IB FPBS (299)
20 PPHS (399)
21 PPOA (413 ) 22 POSA (499) 23 PPOS (499)
QUANT SIG NASS
299 299 299 399 399 399 413 413 49B 498 499 499
CONCENTRATIONS
ON-COLUMN PINAL
RT EXP RT OLT RT R85P0NSB
(ng/mL)
(ng/mL)
3.388 3.17 3.723 3.805 3.401 3.976 4.003 3.873 4.755 4.441 4.174 4.605
3.381 3.381 3.381 3.792 3.792 3.792 3.990 3.990 4.762 4.762 4.174 4.174
0.007 **0.205
0.342 0.013 -0.391 0.184 0.013 -0.117 -0.007 -0.321 0.000 0.431
11884 2064 1527 9981 4708 4267
15342 5385
85375 984
1903432 19079
553.334 553.695 553.714 809.355 809.488 809.499 837.253 837.750 0.11598 1917.31 13.9702 1680.28
553 5S4 554 809 809 809 837 838 0.116 1920 14.0 1680
Exact C c;ycf Original
JJ i l ol
Initiai
Data
3M Environmental Laboratory
Page 68 of 276
Report E02-0443
Tenn. River Valley Samples
Data Fil*; VsEtstarget\targetSchem\dudejr,iSD020626Extracted,bSDUDE0056.D
Page 2
3M Environmental Laboratorv
Exact Copy nf Original
11 IA/n!n->~
InitiaJ Date
Report E02-0443
Tenn. River Valley Samples
Bata File; SSEtstargetStargetSchemSdudejriSD020626Extracted*bSDUDE0056*D
22 FOSA <498) 23 PFOS <499>
3M Environmental Laboratory
Exact Cep f-j
Initial
Page 70 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: DUDE0058.D Report Date-. 27-Aug-2002 13:27
Page 1
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file \\ Et st ar get\target\chem\dudej r .i\ D0 20 62 6E xt rac te d.b \ D U D E 0 0 5 8 .D
Lab Smp Id S L -1. LM-2-2
Inj Date Operator
26- JUN-2002 23:38 mla
Inst ID: dudejr.i
Smp Info
Tenn. River Va ll ey Fish. Prep-17 J u n 02. CMC/MLA. 20 J u n 02
Mise Info
Comment
Method Meth Date
Cal Date Als bottle
\\Etstarget\target\chem\dudejr.i\D020626Extracted.b\D020626extra 27- Aug-2002 13:22 dudejr.i Quant Type: ESTD
2 6 -JUN-2002 22:00
Cal File: DUDE0049.D
45
Dil Factor 1.00000 Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
.
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
IKi
Coopounds IS PFBS 1299)
20 PFHS (399) 21 PPOA (413) 22 POSA (498) 23 PFOS (499)
QUANT SIG NASS
299 299 299 299 399 399 413 413 49S 499 499
CONCBNTRATIONS
ON-COLUMN PINAL
RT EXP RT DLT RT RBSPONSB
(ng/mL)
(ng/aL)
3.388 3.190 3.304 3.723 3.805 3.545 3.867 4.229 4.762 4.174 4.605
3 .381 3.381 3.381 3.381 3.792 3.792 3.990 3.990 4.762 4.174 4.174
0.007 -0.191 -0.07S
0.342 0.013 -0.247 -0.123 0.239 0.000 0.000 0.431
11577 4980 5158 2027 13422 2338 47254 2413
142853 3385486
16466
553.345 553.588 553.581 553.696 809.269 809.548 0.65557 837.894 1.96576 61.4006 1680.36
553 554 554 554 809 810 0.656 838 1.96 1.4 16BO
Exact Ccpy of Original
Ci'nt >3/10
Initial
Data
3M Environmental Laboratory
Page 71 of 276
Report E02-0443
Tenn. River Valley Samples
Data Fila: S\EtstaretStarat\chan\dudejr.i\D020626Extracted.b\IXJDE0058.D
Paga 2
4.5- :
4.2 3.9-; 3.6- ^ 3.3-: ? 3.0-: S 2.7-
1.8;
1.5-;
1.2;
3.00 3.20 3.40 ' 3.60 3.80
___________Hin____________
20 PFHS <399>
3M Environmental Laboratory
Exact Copy ni Origina!
-C W
Initial
> X / '/ a / 5 > -
Date
Page 72 of 276
Report E02-0443
Tenn. River Valley Samples
Fil* SSEtstart\tarj#t\che\dudejr*i\D20626Extractd.b\DUDE0058.D 21 PFOA <413>
Pag 3
22 FSA <496>
23 PFOS <499>
3M Environmental Laboratory
Exact Copy of Origina! ,Ctn( i q / i j / x.
InitiaJ Date
Page 73 of 276
Report E02-0443
Tenn. River Valley Samples
Dettaci File : DUDE0063 .D Report Date: 27-Aug-2002 13:27
Page 1
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
D a ta file \\Etst ar ge t\ tar ge t\ ch em \d udej r .i \ D 0 2 0 6 2 6 E x t r a c t e d .b\DUDE0063 D
Lab Smp Id SL-1. LM-3-2
'
Inj Date
27-JUN-2002 00:33
Operator
mla
Inst ID: dudejr.i
Smp Info
Tenn. River Va ll ey Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02
Misc Info
Comment
Method Meth Date
\\Etstarget\target\chem\dudejr.i\D020626Extracted.b\D020626extra 27-Aug-2002 13:22 dudejr.i Quant Type: ESTD
Cal Date
26-JUN-2002 22:00
Cal File: DUDE0049.D
Als bottle 49
Dil Factor 1.00000
Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds 18 PFBS (259)
20 PPHS (399)
21 PPQA (413) 22 POSA (499) 23 PPOS (499)
QUANT SI6 HASS
299 299 299 299 399 399 399 413 413 498 498 499 499
CONCENTRATIONS
ON-COLUMN PINAL
RT EXP RT DLT RT RESPONSB
(ng/mL)
(ng/mL)
3.388 3.176 3.723 3.812 3.798 3.545 3.976 3.997 3.853 4.762 4.414 4.174 4.605
3.381 3.381 3.381 3.381 3.792 3.792 3.792 3.990 3.990 4.762 4.762 4.174 4.174
0.007 -0.205
0.342 0.431 0.006 -0.247 0.184 0.007 -0.137 0.000 -0.348 0.000 0.431
11469 2575 1432 378 9750 3036 4357
15533 5478
236312 970
3964776 26340
553.349 553.676 553.718 553.756 809.361 809.530 809.497 837.243 837.745 4.98115 1917.31
80.7677 1680.07
553 554 554 554 809 810 809 837 838 4.98 1920 80.8 1680
Exact Copy of Origina!
- & y y i i / z/ oj-
Initial Date
3M Environmental Laboratory
Page 74 of 276
Report E02-0443
Tenn. River Valley Samples
Data File; \\Etstarget\target\chen\duciejr*i\D020626Extracted,b\DUDE0063.D
I
Page 2
i
3M Environmental Laboratory
Exact Copy of Origins
ii'if y -- 10-h o t n i--
initial
Data
Pane 75 nf 7 7
Report E02-0443
Tenn. River Valley Samples
Data Fila: S\Etstargat\target\chem\dudeJr.i\D020626Extracted*b\DUDE0063.D 21 PFA (413)
22 FOSP <498)
23 PFOS (499)
3M Environmental Laboratory
Ecact C opy o f O r i g l i
City
Initiai
Page 76 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: DUDE0068.D Report Date: 27-Aug-2002 13:27
Page l
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file \ \ E t st ar ge t\ tar ge t\ ch em \d ude jr.i\D02062GExtracted.b\DUDE0068.D
Lab Smp Id SL-1. LM-4-2
Inj Date
27-JUN-2002 01:28
Operator
mla
Inst ID: dudejr.i
Smp Info
Tenn. River Va ll ey Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02
Mise Info
Comment
Method Meth Date
\\ Et st ar g e t \ t a r g e t \ c h e m \ d u d e j r .i\D020626Extracted.b\D020626extra 27-Aug-2002 13:22 dudejr.i Quant Type: ESTD
Cal Date
26-JUN-2002 22:00
Cal File: DUDE0049.D
Als bottle 52
Dil Factor 1.00000
Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds 16 PPBS (S9)
20 PPHS (399)
21 PFOA (913) 22 POSA (498) 23 PPOS (499)
QUANT SZG HASS
299 299 299 399 399 399 413 496 499 499 499
CONCENTRATIONS
ON-COLUMN FINAL
RT EXP RT DLT RT RBSPONSE
(ng/mL)
(ng/aL)
3.388 3.183 3.723 3.798 3.354 3 . 5S9 3.997 4.762 4.174 3.867 4.605
3.381 3.391 3.381 3.792 3.792 3.792 3.990 4.762 4.174 4.174 4.174
0.007 -0.198
0.342 0.006 -0.438 -0.233 0.007 0.000 0.000 -0.307 0.431
51072 2350 1509
491S4 415
3064 161661
97875 . 3814537
1524 16518
0.83331 553.684 553.715 0.63726 809.596 809.529 6.42649 0.51796 75.6964 icao.7 1680.35
0.833 554 SS4
0.637 810 810
6.43 0.518
75.7 1480 1680
Exact Copy cf Original /JL//C. / A 2--
Initial Date
3M Environmental Laboratory
Page 77 of 276
Report E02-0443
Tenn. River Valley Samples
Data Fi la: \SEt*targ*t\target\ch*wSdudejr,iSD020626Extract#d,b\DUDE0068D
Page 2
3M Environmental Laboratory
ExactCopy Or~!n=<
L -m L .. / M o j ^
nitiai oste
Page 78 of 276
Report E02-0443
Tenn. River Valley Samples
Data File; SSEtstargetstarget\chem\dudejr,i\D020626Extractei*b\DUDE068.B 21 PFOA (413)
22 FOSA (498)
23 PFQS (499)
3M Environmental Laboratory
Exact Copy of Origina!
L L lio jfa -x .
Initial Date
Page 79 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: \ \ E t s t ar ge t\ tar ge t\ ch em \d udej r .i\D020628.b\DUDE0058.D Page 1 Report Date: 09-Dec-2002 13:07
3M Environmental Laboratory
E02-0443 Tenn. River Valley Samples
Data file : \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0058.D
Lab Smp Id: SL-2. LM-2-1
Inj Date : 29-JUN-2002 02:15
Operator : mla
Inst ID: dudejr.i
Smp Info : Tenn. River Va ll ey Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02
Mise Info :
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020628.b\D020628.m
Meth Date : 09-Dec-200213:01 dudejr.i Quant Type: ESTD
Cal Date : 29-JUN-2002 00:48
Cal File: DUDE0050.D
Als bottle: 28
Dil Factor: 1.00000
Integrator : Falcon
Compound Sublist: a 11.sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds
16 PFBS (2991
20 PFHS (399)
f 21 PFQA (413) ! 22 FOSA (498) 4 23 PFOS (499) |,:i
QUANT SIG MASS
299 299 299 399 399 413 496 499 499
CONCENTRATIONS
ON-COLUMN
FINAL
RT EXP RT DLT RT RESPONSE
(ng/mL)
(ng/mL)
3.386 3.183 3.757 3.005 3.545 4.004 4.776 4.1B1 4.60S
3.388 3.366 3.388 3.798 3.798 3.997 4.769 4.174 4.174
0.000 -0.205
0.369 0.007 -0.253 0.007 0.007 0.007 0.431
15144 2946 2208
10047 540
25432 65904 1346329 20726
569.524 569.996 570.025 786.229 786.477 815.277 1885.85 2.56372 1659.69
570 570 570 786 766 815(H) 1880 2.56 1660
QC Flag Legend M - Compound response manually integrated.
Exact Copy of Original
3M Environmental Laboratory
Page 80 of 276
Report E02-0443 Data Fi!: SSEtstarfetStaret\chew\dud*jr.iSB')20628,b\DUDE0058.D
Tenn. River Valley Samples
Page 2
20 PFHS <399)
3M Environmental Laboratory
Exact Copy of Origina! rx / / j/ rru
Initial Date
Page 81 of 276
Report E02-0443
Data Fila: \SEtstarietStart*t\chw<\dudeJr.i\D020623.b\DUDE0058.D 21 PFOA <413)
Tenn. River Valley Samples
22 FOSA <49B) 23 PFOS <499)
3M Environmental Laboratory
Exact Copy Oats
Paae 82 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\Etst arget\target\chem\dudejr.i\D020628.b \ D U D E 0 0 6 4 .D Page 1 Report Date: 09-Dec-2002 13:07
3M Environmental Laboratory
E02-0443 Tenn. River Valley Samples
Data file \\Etstar ge t\ tar ge t\ ch em \d ude jr.i\ D 0 2 0 6 2 8 .b\DUDE0064.D
Lab Smp Id SL-2. LM-3-2
Inj Date
29-JUN-2002 03:21
Operator
mla
Inst ID: dudejr.i
Smp Info
Tenn. River Va ll ey Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02
Mise Info
Comment
Method Meth Date
\\Etstarget\target\chem\dudejr.i\D020S28,b\D020628.m 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD
Cal Date
29-JUN-2002 00:48
Cal File: DUDE0050.D
Als bottle 33
Dil Factor 1.00000
Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds
18 PFBS (299)
20 PFHS (399) 21 PFA (413) 22 POSA (498) 23 PFOS (499)
QUANT SIG MASS
299 299 299 399 413 498 499 499
CONCENTRATIONS
ON-COLUMN
FINAL
RT EXP RT DLT RT RESPONSE
(ng/mL)
(ng/mL)
3.401 3.210 3.771 3.818 4.017 4.789 4.194 4.625
3.388 3.38B 3.388 3.798 3.997 4.769 4.174 4.174
0.013 -0.178
0.383 0.020 0.020 0.020 0.020 0.451
22037 3476 3793
17063 36939 98985 1627015
1774
569.257 569.916 569.964 0.08850 814.559 0.72476 11.7650 1660.28
569 570 570 0.08 8 5 (M) 814 <M) 0.725 11.8 1660
QC Flag Legend M - Compound response manually integrated.
YacfCo-
(2C__ initial
3M Environmental Laboratory
Page 83 of 276
Report E02-0443 Data File: SSEtstarget\target\che\dudejriSD020628*b\DUDE064.D
Tenn. River Valley Samples
Page 2
3M Environmental Laboratory
: CopyofOriginal
initial
/ .I f / a Ja >
Oats
Page 84 of 276
Report E02-0443
Data Fi les WEtataratStarget'schew'sdudajr, 1\D*>20628.b\DUDE0064,D
Tenn. River Valley Samples
22 FOSA <498) 23 PFOS <499>
3M Environmental Laboratory
Exact Copy of Origin*;
L l -- 12 h o /n ^
initial
D a te
Page 85 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0070 D Paqe 1 Report Date: 09-Dec-2002 13:07
3M Environmental Laboratory
E02-0443 Tenn. River Valley Samples
Data file : \\Etstarget\target\chem\dudejr.i\D020628,b\DUDE0070 D Lab Smp Id: SL-2. LM-4-3
Inj Date : 29-JUN-2002 04:26
Operator : mla
Inst ID: dudejr.i
Smp Info : Tenn. River Va ll ey Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Misc Info :
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020628.b\D020628.m
Meth Date : 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD
Cal Date : 29-JUN-2002 00:48
Cal File: DUDE0050.D
Als bottle: 37 Dil Factor: 1.00000
Integrator: Falcon Target Version: 4.12
Compound Sublist: all.sub
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds
IB PFBS (299)
20 PFH5 (399 2 1 PFQA (4 1 3 ) 2 2 POSA (4 9 8 ) 23 PPOS (499)
QUANT SZG MASS
299 299 299 399 413 496 499 499 499
CONCENTRATIONS
ON-COLUMN
PINAL
RT EXP RT DIiT RT RESPONSE
(ng/mL)
(ng/mL)
3.3 8 8 3.1 8 3 3.7 5 7 3.8 0 5 4.0 0 3 4.7 7 6 4.1 7 4 3.6 0 5 4 .6 0 5
3.3 8 8 3.3 8 8 3.3 8 8 3.7 9 8 3.9 9 7 4 .7 6 9 4 .1 7 4 4.1 7 4 4.1 7 4
0 .0 0 0 > 0.205
0 .3 6 9 0 .0 0 7 0 .0 0 6 0 .0 0 7 0 .0 0 0 -0 .3 6 9 0 .4 3 1
13695 1232 1592
10665 23745 120542 2949014
2773 32944
5 6 9 .5 8 0 5 7 0 .0 6 2 5 7 0 .0 4 9 7 8 6 .2 1 3 8 1 5 .3 6 6 1 .4 5 5 8 3 5 6 .9 4 3 2 1 6 6 0 .2 5 1 6 5 9 .3 1
570 570 570 7 8 6 (M) 8 1 5 (M) 1 .4 6 5 6 .9 1660 1660
QC Flag Legend M - Compound response manually integrated.
Sract Copy of Origina!
initia)
Data
3M Environmental Laboratory
Page 86 of 276
Report E02-0443 Dat* Fil: S\Etstaret\taret\ch*\dudejr.iM>020628.bSDUDE007'>*D
Tenn. River Valley Samples
Pace 2
3M Environmental Laboratory
ExactCopy of Originai
,3 / t / A x.
initial
Oats
Page 87 of 276
Report E02-0443
Data Fil: \\Etstar{etStaret\chem\duciejr*i\D020628,bSDUDE0070,D 21 PFOA C413>
Tenn. River Valley Samples
2 3 PFOS ( 4 9 9 )
3M Environmental Laboratory
Exact Copy r.f ^ -VfrKJL. 3-./// o i _
initial Qa;r.
Page 88 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\ Et st ar get\target\chem\dudej r .i\ D 0 2 0 6 2 8 .b \ D U D E 0 0 7 6 .D Page l Report Date : 09-Dec-2002 13:08
3M Environmental Laboratory
E02-0443 Tenn. River Valley Samples
Data file : \\ Et st ar ge t\target\chem\dudejr.i\ D 0 2 0 6 2 8 .b\DUDE0076.D
Lab Smp Id: SL-3. LM-1-3
Inj Date : 29 -JUN-2002 05:32
Operator : mla
Inst ID: dudejr.i
Smp Info : Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun
Misc Info :
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020628.b\D020628.m
Meth Date : 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD
Cal Date : 29-JUN-2002 00:48
Cal File: DUDE0050.D
Als bottle: 42
Dil Factor: 1.00000
Integrator: Falcon Target Version: 4.12
Compound Sublist: all.sub
02
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds 18 PFBS (299)
20 PFHS (399) 21 PFOA 1413) 22 FOSA (498) 23 PFOS (499)
QUANT 5IG MASS
299 299 299 399 399 413 498 499 499
CONCENTRATIONS
ON-COLUMN
RT EXP RT DLT RT RESPONSE
(ng/mL)
PINAL (ng/mL)
3.388 3.189 3.764 3.80S 3.559 3.996 4.899 4.174 4.611
3.388 3.388 3.3B8 3.798 3.798 3.997 4.769 4.174 4.174
0.000 -0.199
0.376 0.007 -0.239 -0.001 0.130 0.000 0.437
17998 3724 1B36
16875 3229
60835 78316 716542 12921
569.414 569.966 570.039 0.08359 786.407 0.95299 0.02433 1637.71 1659.94
569 570 570 0.0636 786 0 . 9 5 3 IM) 0 . 0 2 4 3 (M) 1640 1660
QC Flag Legend M - Compound response manually integrated.
ExactCopyofOriginal initial Data
3M Environmental Laboratory
Page 89 of 276
Report E02-0443 Oats Filtj \NEtstaret\taretSch#mSdudejr*iMW20628bSDUDE0076*D
Tenn. River Valley Samples
Page 2
18 PFBS <299> 20 PFHS <399>
3M Environmental Laboratory
Exact Copy f Origina!
i ?/.\/&L.
initial
Dau
Page 90 of 276
Report E02-0443 Bat F il*s W E titarg* tStarget\chem\dudeJ r . 1\D'J20628. b\DUDE0076. D
Tenn. River Valley Samples
Page 3
22 FOSA <498> 23 PFOS (499)
3M Environmental Laboratory
Exact Co,;\' r.' i<r._ i2
'nitial
Page 91 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: \ \ E t st ar ge t\ tar ge t\ ch em \d ude jr.i\ D 0 2 0 6 2 8 .b \ D U D E 0 0 8 9 .D Page 1 Report Date: 09-Dec-2002 13:08
3M Environmental Laboratory
E02-0443 Tenn. River Valley Samples
Data file \\Etstarget\target\chem\dudejr.i\ D0 20 62 8. b\ DUD E0 08 9.D
Lab Smp Id S L - 3 . LM-4-3
Inj Date
29-JUN-2002 07:55
Operator
mla
Inst ID: dudejr.i
Smp Info
Tenn. River Va ll ey Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun
Mise Info
Comment
Method
\\Etstarget\target\chem\dudejr.i\D020628.b\D020628.m
Meth Date 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD
Cal Date
29-JUN-2002 00:48
Cal File: DUDE0050.D
Als bottle 52
Dil Factor 1.00000
Integrator Falcon Target Version: 4.12
Compound Sublist: all.sub
02
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds
18 PFBS (299)
20 PFHS (399) 21 PPOA (413) 22 FOSA (498) 23 PFOS (499)
QUANT SIG HASS
299 299 299 399 399 413 498 499 499
CONCENTRATIONS
ON-COLUMN
RT EXP RT DLT RT RESPONSE
(ng/mL)
FINAL (ng/mL)
3.395 3.190 3.751 3.805 3.552 4.003 4.769 4.174 4.605
3.388 3.38B 3.388 3.798 3.798 3.997 4.769 4.174 4.174
0.007 >0.19B
0.369 0.007 -0.246 0.006 0.000 0.000 0.431
12936 3732 1991 7393 2451
24746 64726 1029081 18761
569.610 569.966 570.033 786.298 786.427 815.313 1885.89 1627.64 1659.75
570 570 570 786 786 8 1 5 (M) 1380 1630 1660
QC Flag Legend M - Compound response manually integrated.
ExactCopy nf Oriciw
U -IlqJ o.
initial Oat-'
3M Environmental Laboratory
Page 92 of 276
Report E02-0443 Data Fi le: \\Ettarg#t\iargat\chaeiSdule,jr*iSD,>20629*b\DUDE0089#D
Tenn. River Valley Samples
Page 2
18 PFBS <289)
3M Environmental Laboratory
Exact Copy of Origins!
Initial Date
Page 93 of 276
Report E02-0443
Dit File: S\EtstartetStare*tSeh*nSdudeJr.iM20628.b\DUDE0089.D 21 P R M <413)
Tenn. River Valley Samples
22 FOSA (498) Ion 498.00
4.0^
~ 3.5-'
I
4.40 4.60 4.'80 5.00
___________ in
23 PFOS <499)
2*7-
2*4: 2.1-; 1.8-|
f 1*B:
S i *8-:
0.9
rIon 499.00
0.6
L0.3- _____ __/_________L -ff
3.80 4.00 4.20 4.40 4.60 Hin
3M Environmental Laboratory
'-xzct Copy of Original C)4X__ Wtia!
Page 94 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\Etstarget\target\c he m\ du de jr . i \ D 0 20 62 8. b\D UD E0 10 2.D Page 1 Report Date: 09-Dec-2002 13:08
3M Environmental Laboratory
E02-0443 Tenn. River Valley Samples
Data file \\ Et st ar ge t\target \c he m\ du dej r .i \ D 0 20 62 8. b\ DUD E0 10 2.D
Lab Smp Id SL-3. LM-7-2
Inj Date
29-JUN-2002 10:18
Operator
mla
Inst ID: dudejr.i
Smp Info
Tenn. River Va ll ey Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02
Misc Info
Comment
Method
\\Etstarget\target\chem\dudejr.i\D020628.b\D020628.m
Meth Date 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD
Cal Date
29-JUN-2002 00:48
Cal File: DUDE0050.D
Al s bottle 62
Dil Factor 1.00000
Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds 18 PFSS (299)
20 PFHS (399) 21 PFOA 1413) 22 FOSA (498)
23 PFOS (499)
QUANT SIG MASS
299 299 299 399 413 498 498 499 499
CONCENTRATIONS
ON-COLUMN
FINAL
RT EXP RT DLT RT RESPONSE
(ng/mL)
(ng/mL)
3.388 3.176 3.757 3.799 3.997 4.769 4.441 4.175 4.598
3.388 3.388 3.398 3.798 3.997 4.769 4.769 4.174 4.174
0 .0 0 0
-0.212 0.369
0 .001 0 .000 0 .000
-0.328
0 .001
0.424
24706 1376 1023 9487
62864 23637
779 906705
29289
569.154 570.057 570.071 786.244 1.06124 1887.28 1888.05 1631.60 1659.43
o10 H
569 570 570 786 (M)
1890 1890 1630 1660
QC Flag Legend M - Compound response manually integrated.
&act Co.oy g 0r:r'int:; U n i tz/sc/e-^
3M Environmental Laboratory
Page 95 of 276
Report E02-0443 Bata File: Y\EtstaretNtar{etSchenSdudejr,iSD020628,b\DUDEC>102*D
Tenn. River Valley Samples
18 PFBS C299)
3M Environmental Laboratory
Exact Copy of Original
< t D / / * / O*--
Initial Date
Page 96 of 276
Report E02-0443
Data File: S\Etstar^et\taret\chem\cJudejr,iSD02628.bSDUDE0102*D
Tenn. River Valley Samples
22 POSA <498)
3M Environmental Laboratory
Exact Copy of Origin-,'
/ g / t o / ax.
Initial
Date
Page 97 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\ Et st ar ge t\ tar ge t\ ch em \d ude jr.i\D020628.b\DUDE0104.D Page 1 Report Date: 09-Dec-2002 13:08
3M Environmental Laboratory
E02-0443 Tenn. River Valley Samples
Data file \\Etstarget\target\chem\dudejr.i\D020628,b\DUDE0104.D
Lab Smp Id SL-3. SM-1-1
Inj Date
29-JUN-2002 10:40
Operator
mla
Inst ID: dudejr.i
Smp Info
Tenn. River Va ll ey Fish. Prep-17 Jun 02. CMC/MLA. 20 Ju n 02
Mise Info
Comment
Method
\\Et st ar ge t\ tar ge t\ ch em \d ude jr.i\D020628.b\D020628.m
Meth Date 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD
Cal Date
29-JUN-2002 00:48
Cal File: DUDE0050.D
Als bottle 65
Dil Factor 1.00000
Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds 18 PFBS (299)
20 PFHS (399)
21 PFOA (413) 22 FOSA 149) 23 PPOS (499)
QUANT SIG MASS
299 299 299 399 399 399 413 498 499 499
CONCENTRATIONS
ON-COLUMN
ET EXP ET BUT ET RESPONSE
(ng/mL)
FINAL (ng/mL)
3.388 3.190 3.757 3.812 3.566 4.174 3.996 4.769 4.174 4.605
3.388 3.388 3.386 3.798 3.79B 3.798 3.997 4.769 4.174 4.174
0.000 -0.198
0.369 0.014 -0.232 0.376 -0.001 0.000 0.000 0.431
10955 2138 1256
11252 5688 975
55673 41082 429027 15813
S69.686 570.027 570.062 786.197 786.343 786.466 0.67774 1886.69 1646.86 1659.85
5-70 570 570 786 786 786 0 . 6 7 8 (M) 1 8 9 0 (M) 1650 1660
QC Flag Legend M - Compound response manually integrated.
Exact Copy of Original
inifiaJ
Data
3M Environmental Laboratory
Page 98 o f 276
Report E02-0443
Data Fila: SSEtstargatStarg*tXchnSdudeJp.iM20S28.bSDUIIE104.S
Tenn. River Valley Samples
P a je 2
18 PFBS <299)
3M Environmental Laboratory
Exact Copy of On.jfn&:
L lo i / z A*/<)2^
?nitia!
ate
Page 99 of 276
Report E02-0443
Data File VsEtstargetStargetSchem\dudejr.i\D020628b\DUDE0104*D
Tenn. River Valley Samples
Page 3
2 2 FOSA ( 4 9 8 ) 23 PFOS <499>
3M Environmental Laboratory
Exact Copy of Origins! -tez-- `J J ta J ji2-
'nitiai Ogio
Page 100 o f 276
Report E02-0443
Tenn. River Valley Samples
D a ta File: \\Etstarge t\ tar ge t\ ch em \d udej r .i \ D 0 2 0 6 2 8 .b \ D U D E 0 1 0 5 .D Page 1 Report Date: 09-Dec-2002 13:08
3M Environmental Laboratory
E02-0443 Tenn. River Valley Samples
Data file : \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0105.D Lab Smp Id: S L - 3 . SM-1-2
Inj Date : 29-JUN-2002 10:51
Operator : mla
Inst ID: dudejr.i
Smp Info : Tenn. River V a l l e y Fish. Pr ep -17 Jun 02. CMC/MLA. 20 Jun
Mise Info :
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020S28,b\D020628.m
Meth Date : 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD
Cal Date : 29-JUN-2002 00:48
Cal File: DUDE0050.D
Al s bottle: 66
Dii Factor: 1.00000
Integrator : Falcon
Compound S u b l i s t :a l l .sub
Target Version: 4.12
02
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds ia PFBS (299)
20 PFHS (399)
21 PFOA M13) 22 FOSA (498) 23 PPS (499)
QUANT SIG MASS
299 299 299 399 399 399 413 498 499 499
CONCENTRATIONS
ON-COLUMN
FINAL
HT EXP RT DLT RT RESPONSE
(ng/mL)
(ng/mL)
3.366 3.162 3.764 3.825 3 .552 4.194 3.996 4.769 4.174 4.605
3.388 3.388 3.388 3.798 3.798 3.798 3.997 4.769 4.174 4.174
0.000 0.206
0.376 0.027 -0.246 0.396 -0.0Q1 0.000 0.0QO 0.431
11225 1896 1126
12780 6122 930
52802 40143 469574 14246
569.676 570.037 570.067 786.158 786.331 786.467 0.52474 1886.72 1645.58 1659.89
570 570 570 786 786 786 0.525 (M) 1 8 9 0 (M) 1640 1660
QC Flag Legend M - Compound response manually integrated.
Exact Co?j ot Crininal
Cik7L U l t o / Pi--
initial
Date
3M Environmental Laboratory
Page 101 of 276
Report E02-0443
Tenn. River Valley Samples
iDt F 1e : SSEtstarge tStargetSchwiSdud*j r .SD-J20628. bSDUDE0105 .D
\\Ets t-artStr etSchemSdudej r *iSD020&28 ,b\DUI0i05 *0
Page Z
20 PFHS <399)
3M Environmental Laboratory
Cu'v or Origina! CktLLL r g / / c / aj_
Pitia! Date
Paae 102 of 276
Report E02-0443
Data File: NSEtstargetStargetSch*mSdudejr.iSI262a.bSDUDEi05.D 21 PFOA (413)
Tenn. River Valley Samples
Pae 3
22 FOSfl (498)
II
3M Environmental Laboratory
Exact Copy of Origina!
iniiiat Doto
Page 103 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\ Et st ar ge t\target\chem\dudejr.i\D02062 8. b\ DUD E0 10 8.D Page 1 Report Date: 09-Dec-2002 13:08
3M Environmental Laboratory
E02-0443 Tenn. River Valley Samples
D a t a file : \ \ E t s t a r ge t\ tar ge t\ ch em \d ude jr.i\D020628.b\DUDE0108.D Lab Smp Id: SL-3. SM-1-3
Inj Date : 29-JUN-2002 11:25
Operator : mla
Inst ID: dudejr.i
Smp Info : Tenn. Ri ve r Va ll ey Fish. Prep-17 Jun 02. CMC/MLA. 20 Ju n 02
Mise Info :
Comment :
Method
: \ \ E t s t a r ge t\ tar ge t\ ch em \d ude jr.i\D020628,b\D020628.m
Meth Date : 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD
Cal Date : 29-JUN-2002 00:48
Cal File: DUDE0050.D
Al s bottle: 67
Dil Factor: 1.00000
Integrator: Falcon
Compound Sublist: all.sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds
18 PFBS {299)
20 PFHS (399) 21 PFOA 1413) 22 POSA (49B) 23 PFOS 1499)
QUANT SIO MASS
299 299 299 399 413 498 499 499
CONCENTRATIONS
ON-COLUMN
PINAL
RT EXP RT DLT RT RESPONSE
(ng/mXi)
(ng/mL)
3.386 3.183 3.764 3.798 3.996 4.762 4.174 4.S98
3.388 3.388 3.388 3.798 3.997 4.769 4.174 4.174
0.000 -0.205
0.376 0.000 -0.001 -0.007 0.000 0.424
16091 2727 1568
13195 54265 44388 458983 1S684
569.468 570.005 570.049 786.147 0.60270 1886.57 1645.91 1659.85
569 570 570 7 8 6 (M) 0 . 6 0 3 (M) 1 8 9 0 (M) 1640 1660
QC Flag Legend M - Compound response manually integrated.
Exact Copy of Origina!
-l / / m h o 1
initial Date
3M Environmental Laboratory
Page 104 o f 276
Report E02-0443
Hat Filai SSEtstarjetStarjetSchenSdudejr.i\I20628.bM)UDE0108.D
Tenn. River Valley Samples
Paje 2
20 PFHS <399) 3M Environmental Laboratory
Exact Co;jyof Orpirui
initia!
o,v r
Page 105 o f 276
Report E02-0443
Data File; \SEtstargetNtarget\cheeSdudejr.ISD020628.tADUDE0108.D 21 PFOA <413>
Tenn. River Valley Samples
22 FOSft 498>
3M Environmental Laboratory
Exact Copy of Originai
S - * ? r i h o / c i .
Infilai Date *
Page 106 o f 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\ Et s t a r g e t \ t a r g e t \ c h e m \ d u d e j r .i\D020629.b\DUDE0089 D Page 1 Report Date: 27-Aug-2002 10:06
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file : \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0089.D
Lab Smp Id: SL-1. WB-1
Inj Date : 01-JUL-2002 04:25
Operator : mla
Inst ID: dudejr.i
Smp Info : Tenn. River Va ll ey Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun
Misc Info :
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020629.b\D020629.m
Meth Date 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD
Cal Date : 30-JUN-2002 22:46
Cal File: DUDE0058.D
Als bottle: 47
Dil Factor: 1.00000
Integrator: Falcon
Comp ou nd S u b l i s t : a l l .sub
Target Version: 4.12
02
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds
18 PPBS (299)
20 PFHS (399) 21 PFOA (913) 22 FOSA (499) 23 PFOS (499)
QUANT SI MASS
299 299 299 399 413 498 499 499
CONCENTRATIONS
ON-COLUMN
PINAL
RT BXP RT DLT RT RBSPONS8
(ng/taL)
(ng/mL)
3.313 2.944 3.163 3.798 4.004 4.776 4.188 4.60S
3.381 3.381 3.381 3.792 3.990 4.756 4.168 4.168
-0.068 -0.437 -0.218
0.006 0.014 0.020 0.020 0.437
33577 478
2981 8170 10932 7649 96922 22825
1223.22 1224.54 1224.39 0.16435 819.144 2744.00 1274.91 1277.09
1220 1220 1220 0.164
819 2740 1270 1280
Exact Co,: initiai
(02-- 0*1,"
3M Environmental Laboratory
Page 107 of 276
Report E02-0443
Tenn. River Valley Samples
Sata File: SNEtstarget\targetSchem\dudejr.i\D020629*bMUDE089,D SSEtstarget\target\chemSdudejr .i\D020629 .bSDUDEC089.B
Page 2
18 PFBS <299)
20 PFHS <399) 3M Environmental Laboratory
Exact Copy ;
C J jn r
initial
(,0 2Oat-
Page 108 of 276
Report E02-0443
Data File: \\Etitar{et\tarset\che*\dudejr.l\D020629.b\DUBE0089.D 21 PFOfl <4131
Tenn. River Valley Samples
Page 3
22 FOSA <498>
3M Environmental Laboratory
Exact Copy or Origina!
L2 ,//o /( >J--
!nitia(
Date
O 4 r\r\ ,, r
Report E02-0443
Tenn. River Valley Samples
D a t a File: \\ Et starget\t a r g e t \ c h e m \ d u d e j r .i\ D02Q629.b\DUDE0127.D Page 1 Report Date: 27-Aug-2002 10:07
3M Environmental Laboratory
E02-0443/ Tenn. River Valley Samples
D a t a file : \\Etstar ge t\ tar ge t\ ch em \d u d e j r .i\D020629.b\DUDE0127.D
Lab Smp Id: SL-2. WB-1
Inj Date : 01-JUL-2002 11:23
Operator : mla
Inst ID: dudejr.i
Smp Info : Tenn. Rive r V a l l e y Fish. Prep-17 Ju n 02. CMC/MLA. 20 Jun 03
Mise Info :
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020629.b\D020629.m
Meth Date : 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD
Cal Date : 30-JUN-2002 22:46
Cal File: DUDE0058.D
Als bottle: 76
Dil Factor: 1.00000 Integrator: Falcon
Compound Sublist: all.sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds
ia PPBS (29)
30 PFKS (3SJ)
31 PPOA (413) 33 POSA (49) 33 PFOS (499)
QUANT SIO HASS
399 399 399 399 413 49S 499 499
CONCENTRATIONS
ON-COLUMN
PINAL
RT SXP RT DLT RT RBSPONSB
(ng/rtL)
(ng/mL)
3.319 3.176 3.791 3.983 3.996 4.776 4.1B6 4.598
3.301 3.381 3.792 3.793 3.990 4.756 4.168 4.168
-0.062 -0.205 -0.001
0.190 0.006 0.020 Q.02 0.430
21873 37B4 3614 1921
12881 3433
86874 12403
1223.32 1224.35 0.03478 797.168 819.035 2744.18 1275.20 1277.40
1220 1220 0.0348
797 819 3740 1280 1280
O W Cop1 '> Original
O n/
`nitfaJ
Date
3M Environmental laboratorv
r*-~-
Report E02-0443
Data Files \SEtstargetStarget\chenSdudejr,i\D020629.b\DUDE0127.D
Tenn. River Valley Samples
Pae 2
18 PFBS (299> 3M Environmental Laboratory
_/
initial
5T
4 <1 4
07P
Report E02-0443
Bata File* \\EtstargetstargetSchefnSdudejr. iSD020629 .bSDUBECrl^.D 21 PFOA <413)
Tenn. River Valley Samples
23 PFOS <499) C n \'irA n rv )o n f*il I U ^ ra trin
fe n Oo.:.'v Origin
-CjJOC,, .i X / t o / i-
fiifia! Data
Report E02-0443
Tenn. River Valley Samples
Data File: DUDE0089.D Report Date: 27-Aug-2002 11:06
Page 1
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file : \\Etstarget\target\chem\dudejr.i\D020702(D20702),b\DUDE0089.D
Lab Smp Id: S L - 3 . WB-1
Inj Date : 03-JUL-2002 07:02
Operator : mla
Inst ID: dudejr.i
Smp Info : Tenn. River Va ll ey Fish. Prep-17 J u n 02. CMC/MLA. 20 Jun 02
Mise Info :
Comment
Method Meth Date Cal Date
:
: \\Etstarget\target\chem\dudejr.i\D020702(D20702).b\D020702.m
: 27-Aug-2002 11:01 dudejr.i Quant Type: ESTD
: 03-JUL-2002 01:21
Cal File: DUDE0058.D
Als bottle: 72
Dil Factor: 1.00000 Integrator : Falcon
Compound Sublist: all.sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds
1 PFBS (299)
20 PPHS (399) 21 PPOA (913) 22 POSA (499) 23 PPOS (499)
QUANT S16 MASS
299 299 299 399 399 413 498 499 499
CONCENTRATIONS
ON-COLUMN
PINAL
RT EXP RT DLT RT RESPONSE
(ng/L)
(ng/L)
3.326 3.1*3 3.777 3.B25 3.545 4.010 4.803 4.194 4.591
3.387 3.387 3.387 3.791 3.791 3.949 4.749 4.167 4.167
>0.061 >0.204
0.390 0.034 -0.246 0.021 0.05S 0.027 0.424
2S327 3226 498 7477 937 14443 S53S 42445
32937
1219.58 1220.47 1220.58 0.25845 0.12420 795.103 2854.35 1323.02 1324.34
1220 1220 1220 0.258 0.124
7SS(H) 2850(H) 1320 1320
QC Flag Legend M - Compound response manually integrated.
Exact CopyofGrig:r,.v initiai Dato
3M Environmental Laboratory
Paae 113 of 276
Report E02-0443
Tenn. River Valley Samples
Sata File: S\EtltargetStarjet\che*\dudejr.iSD020702<D20702).bSDUDE0089.D
Page 2
18 PFBS <299) 20 PFHS <399)
Exact Copy of Original
dittai
nato
Report E02-0443
Tenn. River Valley Samples
Data File* \\Etst*ret\t*ret\ch*\dudejr.i\D020702<I)207C>2>,b\DUDE0089.D 21 PFOA <413)
22 FDSA <498>
23 PFOS <499>
3M Environmental Laborston'
-;ciCf Copy ur Original C hjt_m /
Report E02-0443
Tenn. River Valley Samples
D a ta File: \ \ E t s t a r g e t \ t a r g e t \ c h e m \ d u d e j r .i\D020629.b\DUDE0064.D Page 1 Report Date: 27-Aug-2002 10:05
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file : \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0064.D
La b Smp Id: SL-1. C-l-3
Inj Date : 30-JUN-2002 23:51
Operator : mla
Inst ID: dudejr.i
Smp Info : Tenn. Ri ve r Va ll ey Fish. Prep-17 Ju n 02. CMC/MLA. 20 Ju n 02
Mise Info :
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020629.b\D020629.m
Meth Date : 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD
Cal Date : 30-JUN-2002 22:46
Cal File: DUDE0058.D
Als bottle: 2 8
Dil Factor: 1.00000
Integrator: Falcon
Comp ou nd S u b l i s t : a l l .sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds
18 PPBS <299)
30 PPHS (399) 31 PPOA (413) 22 POSA (49) 23 EPOS <499)
QUANT S26 NASS
299 299 299 399 413 498 499 499 499
CONCENTRATIONS
ON-COLUMN
PINAL
RT BXP RT DLT RT RBSPONSB
(ng/ntL)
(ng/mL)
3.388 3.178 3.751 3.798 3.997 4.758 4.ITS 4.434 4.805
3.381 3.381 3.381 3.792 3.990 4.758 4.188 4.188 4.188
0.007 -0.205
0.370 0.006 0.007 0.000 0.007 L .2 6 0.437
12710 3939 2555 7182
23937 140625 480884
5778 16925
1223.84 1224.34 1224.42 0.13625 0.38259 5.20388 10.0262 1277.60 1277.27
1220 1220 1220 0 . 1 3 6 (N) 0.382 (N) 5 . 2 0 (N) 10.0 1280 1280
QC Flag Legend M - Compound response manually integrated.
Exact Copy of Origin;.
( - k flC . i. 2 h s / o t -
inaia?
>n.
3M Environmental Laboratory
Paae 116 of 276
Report E02-0443
Tenn. River Valley Samples
Bata File: \SEttartetStaptetSchenSdudejr.iU)020629.bSDUDE0064.D
Pas 2
7.2-
SSEts tar **t\t*r jt\chew\dud*j r iSD020629* b\DUDE0064 O
6.9-J
6. 6
6 .3
6. 0
5 .7 ;
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5.1-1
4.8-; 4.5;
4 ,2 :'
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3.6-;
3.3- ;
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0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 Hin
18 PFBS <299)
20 PFHS (399) Pn\/rnnrnon^a! I ahat-alnn*
-fac Copy y/-.
t-ljip /o x -
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j ;\\
Report E02-0443
Itata File: S\Etst*ret'starj;et'schenSduclej r ,iSD020629,bSDUDE0064,D
Tenn. River Valley Samples
23 PFOS <499> 3M Environmental Laboratory
Qct Co? C ki!L_ l2 .(io [ o i
o ~t
Report E02-0443
Tenn. River Valley Samples
D a ta File: \ \ E t s t a r g e t \ t a r g e t \ c h e m \ d u d e j r .i\D020629.b\DUDE0065.D Page 1
Report Date: 27-Aug-2002 10:05
.
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file \\Etstarget\target\chem\dudejr,i\D020629.b\DUDE0065.D
Lab Smp Id S L - 1 . C-2-1
Inj Date
01-JUL-2002 00:02
Operator
mla
Inst ID: dudejr.i
Smp Info
Tenn. Ri ve r V a l l e y Fish. Prep-17 J u n 02. CMC/MLA. 20 Ju n
Mise Info
Comment
Method Metti Date Cal Date
\\Etstarget\target\chem\dudejr.i\D020629.b\D020629.m
27-Aug-2002 09:59 dudejr.i Quant Type: ESTD
30-JUN-2002 22:46
Cal File: DUDE0058.D
Als bottle 29
Dil Factor 1.00000 Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
02
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds
IB PFBS (399) J ! ' 30 PPHS (399) ; j
21 PFOA (413) 5 33 POSA (498) i 33 pros (499) i i
QUANT SIG HASS
299 299 299 399 399 3 99 413 49ft 499 499 499
CONCENTRATIONS
ON-COLUMN
FINAL
RT BXP RT DLT RT RBSPONSB
(svg/mL)
(ng/mL)
3.388 3.169 3 .751 3.79ft 3.402 3.539 3.997 4.763 4.175 3.792 4.605
3.381 3.361 3.361 3.792 3.792 3.792 3.990 4.756 4.16ft 4.16ft 4.16ft
0.007 0.212
0.370 0.006 0.390 0.253 0.007 0.007 0.007 -0 .376 0.437
13624
1223.79
2606
1224.40
1621
1224.47
10531
0.23151
1006
797.194
2533
0.00404
26775 . 0.54153
122304
4.44736
472057 2335
9.76111 1277.70
21371
1277.14
1220 1220 1220 0.232
797 0.00404
0 . 5 4 2 <M) 4.45 9.76 1280 1280
QC Flag Legend M - Compound response manually integrated.
`ixaci Co;; :
7iiia' nati)
3M Environmental Laboratory
P u n o 110 o f 07R
Report E02-0443
Tenn. River Valley Samples
Data Fil** SSEtstart*tStart\chm\dudjr-,i\D020629.b\DUDE0065.r
Pat* 2
W E t l t a r tatStar t*t\chm\dud*jr .1\D02029.b\DUDE0065 .D
S.Z-I
5.0- ;
4.8- :
4.6^
4.4-
4.Z-;
4.0- j
3.8- ;
3.6^
3.4- :
3.2-i
3.0- *
2.8- ; z.6-1 2.4-: 2.2-j
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1.8-: 1.6-;
1.4- j
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0.4-;
0.2-i U___ L U iLl___________________________ I I -
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0.5 1.0 1.S Z.O 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7,0 7.5 8.0 8.5 9.0 Hin
18 PFBS (299)
3M Environmental Laboratorv
iact Copy oi Original
tiLL_ 2-!/ o f
initia) Date
p ? n o 1 r>t
Report E02-0443
Data Fil; SSEtstart*tStaritSehen\dudejr.i\D020629.b\DUDE0065.D 21 PFOA <413)
Tenn. River Valley Samples
23 PFOS (499)
9 ^^ C n iiirr.n n n o rt5 l I
CO^V . ( d L - (M ie le .Z.
initiai Date
n 4 0 4 ,,./ o -* r
Report E02-0443
Tenn. River Valley Samples
Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDEQ071.D Page 1 Report Date: 27-Aug-2002 10:05
3M Environmental Laboratory
E02-0443, Tenn. R i v e r V a l l e y Samples
Data file : \\Etstarget\target\chem\dudejr.i\D020629,b\DUDE0071.D
Lab Smp Id: SL-1. C-3-2
Inj Date : 01-JUL-2002 01:08
Operator : mla
Inst ID: dudejr.i
Smp Info : Tenn. River Va ll ey Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02
Misc Info :
Comment Method
: %4 : \\Etstarget\target\chem\dudejr.r\D020629.b\D020629.m
Meth Date : 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD
Cal Date : 30-JUN-2002 22:46
Cal File: DUDE0058.D
Als bottle: 34
Dil Factor: 1.00000 Integrator: Falcon
Compound Sublist: all.sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds
IS m a (299)
1 ! 30 PPHS U M )
21 PPOA (413) ai POSA (49) I J 23 PPOS (499)
QUANT SXG HASS
299 299 299 399 413 498 498 499 499
CONCENTRATIONS
ON-COLUMN
PINAL
RT BXP RT DLT RT RESPONSE
(ng/mL)
(ng/mL)
3.388 3.176 3.750 3.798 3.997 4.762 5.009 4.174 4.505
3.381 3.3S1 3.381 3.792 3.990 4.756 4.756 4.168 4.166
0.007 -0,205
0.36 0.006 0.007 0.006 0.253 0.006 0.437
15305 2054 1430
12488 20288 185959
9781 742237
20176
1223.69 1224.45 1224.48 0.28719 0.17034 7.07763 2743.92 17.9441 1277.17
1220 1220 1220 0.287(H) 0.178(H) 7.08 2740 17.9 1280
QC Flag Legend M - Compound response manually integrated.
faciCopro: c.r,ir.;
a-- < L u d o lf
initias Date
3M Environmental Laboratory
Page 122 of 276
Report E02-0443 Data Fil#$ SNEtstaretStarsetSchemSdudajr,iSD020629*b\DUDE007i*D
Tenn. River Valley Samples
Pa 2
3M Environmental Laboratory
Exact Coi-'y '
Page 123 of 276
Report E02-0443
Fil; S\Etstar#t\taret\chw\dud#jr.i\D0229*b\DUDE0071*D 21 PFOA <413>
Tenn. River Valley Samples
Pe 3
23 PFOS <499>
ixxac C o p y Ci .'ici
a it 1 Data
Report E02-0443
Tenn. River Valley Samples
D a ta File: \ \ E t s t a r g e t \ t a r g e t \ c h e m \ d u d e j r .i\D020629,b\DUDE0076.D Page 1 Report Date: 27-Aug-2002 10:06
3M Environmental Laboratory
E02-0443, Term. River Valley Samples
Data file \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0076.D
Lab Smp Id SL-1. C-4-2
Inj Date
01-JUL-2002 02:03
Operator
mla
Inst ID . dudej r .i
Smp Info
Tenn. Ri ve r Va l l e y Fish. P r e p - 17 Ju n 02. C M C / M L A . 20 J u n 02
Misc Info
Comment Method Meth Date
\\Etstarget\target\chem\dudejr.i\D020629.b\D020629.m 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD
Cal Date
30-JUN-2002 22:46
Cal File: DUDE0058.D
Als bottle 37
Dil Factor 1.00000
Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compound
1 PPBS (299)
20 PFHS (399) 21 PPOA (413) 22 POSA (498) 23 PPOS (499)
QUANT SIG HASS
299 299 299 399 413 498 499 499 499
499
CONCENTRATIOMS
ON-COLUMN
PINAL
RT EXP RT DLT RT RBSPONSB
(ng/mL)
(ng/L)
3.381 3.224 3.750 3.792 3.997 4.789 4.174 3.785 4.434 4 . COS
3.381 3.381 3.381 3.792 3.990 4.756 4.168 4.168 4.168
4 .1CB
0.000 -0.1S7
0.369 0.000 0.007 0.013 0.006 -0.383 0.266
0 .4 9 7
13243 2813 629 5712
11767 103527 684549
516 11460
00929
1223.81 1224.40 1224.53 0.09444 819.097 3.67245 16.1878 1277.75 1277.43
1 2 7 7 .1 5
1220 1220 1220 0 . 0 9 4 4 (M)
819 (M) 3.67 16.2 1280 1280
1200
QC Flag Legend M - Compound response manually integrated.
C-lriC L3- ( i/ ~l--
initia! D' :
3M Environmental Laboratory
Page 125 of 276
Report E02-O443
Data F e : VsEtstar*t;etStartet\cbew\dudejr*i\D2629*b\DUDE0076*D
Tenn. River Valley Samples
18 PFBS (299)
Ion 299*.00w
3*02*7-
3M Environmental Laboratory
act Ci :y
Paae 126 of 276
Report E02-0443
Fil: S\Et*targtStartet\chiSdudjr.iM)020629.b\DUDE0076.D 21 PF0A (413)
Tenn. River Valley Samples
23 PFOS <499) 3M Environmental Laboratory
SGCI Copy
-J "!.
Page 127 o f 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0097 D Paae 3
Report Date: 27-Aug-2002 10:06
1
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file Lab Smp Id
S\L\ E-t2s.tCa~r1g-e3t\ tar ge t\ ch em \d ude jr .i \D 02 06 29.b\DUDE0097.D
Inj Date
01-JUL-2002 05:53
Operator Smp Info
ttla
Inst ID: dudejr i
Tenn. Rive r Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Ju n 02
Mise Info
Comment
Method Meth Date
\\Etstarget\target\chem\dudejr.i\D0 2 0 6 2 9 .b\D020629 m 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD
Cal Date
30-iJUN-2002 22:46
Cal File: DUDE0058.D
Als bottle 54
'
Dil Factor 1.00000
Integrator Falcon Target Version: 4.12
Comp ou nd Sublist: a l l .sub
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds 18 PPBS (399)
20 PFHS (399)
21 PFOA (413) 22 POSA (494) 2 3 PPOS (4 )
QUANT SXQ NASS
299 299 299 399 399 399 399 413 498
499
499
CONCENTRATIONS
ON-COLUMN PINAL
RT EXP RT DLT RT RBSPONSB
(ng/mL)
(ng/wL)
3.387 3.189 3.750 3.798 3.394 3.558 3.982 3.998 4.762
4 .180
4.611
3.381 3.381 3.381 3.792 3.792 3.792 3.792 3.990 4.756
4 . ICO
4.168
0.006 - 0.212
0.369 0.006 -0.398 -0.234 0.190 0.006 0.006
0.012
0.443
11345 2189 1134 3692 1197 8611 1879
12700 14954
126853
11361
1223.92 1224.44 1224.50 0.03700 797.188 0.17689 797.169 819.045 0.02301
1 2 7 4 .0 2
1277.43
1220 1220 1220 0.0370
797 0.177
797 8 1 9 (N) 0.0230(H)
1270
1280
QC Flag Legend M - Compound response manually integrated.
fciiSCt Cop's l'.: J l " '
3M Environmental Laboratory
Page 128 of 276
Report E02-0443 Dita Fila: SSEtstaretStaretSchem\dud*jr.iSD020629.b\DUDE0097.D
Tenn. River Valley Samples
Pa* 2
1 8 PFBS <299> 2 0 PFHS <399>
3M Environmental Laboratory
fc-Vici- Co-;.
p C .... ( / / j - i.
` P /')
-
Page 129 of 276
Report E02-0443
Data Fila; S\Etstarj#tStar,tSchwSciudejr,i\IK>20629.b\DUDE09?* 21 PFOA (413)
Tenn. River Valley Samples
Pas 3
23 PFOS <499)
3M Environmental Laboratory
ExactCopy of Original
Date
Page 130 o f 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\Etstarget\target\chem\dudejr.i\D020629,b\DUDE0105.D Page l Report Date-. 2 7 -Aug-2002 10:06
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
D a t a file : \\Etstarge t\ tar ge t\ ch em \d ude jr .i \D 02 06 29 .b\ DU DE Ql 05.D Lab Smp Id: SL-2. C-3-2
Inj Date : 01-JUL-2002 07:21
Operator : mla
Inst ID: dudejr.i
Smp Info : Tenn. River Va ll ey Fish. Prep-17 Ju n 02. CMC/MLA. 20 J u n 02
Misc Info : Comment :
Method
: \ \ E t s t a r g e t \ t a r g e t \ c h e m \ d u d e j r .i\D020629.b\D020629 .m
Meth Date : 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD
Cal Date : 30-JUN-2002 22:46
Cal File: DUDE0058.D
Al s bottle: 60 Dil Factor: 1.00000
Integrator: Falcon
Compound Sublist: all.sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compound 18 PFBS 1395)
20 PPKS 1399)
21 PPOA (413) 22 POSA (499) 23 PFOS (499)
QUANT SI6 NASS
299 299 299 399 399 399 413 498 498 499 499 499
CONCENTRATIONS
ON-COLUMN
FINAL
RT BXP RT DLT RT RBSPONSB
(ng/L)
(ng/m.)
3.388 3.142 3.750 3.798 3.S4S 3.975 3.995 4.789 4.427 4.174 4.434 4.505
3.381 3.381 3.381 3.792 3.792 3.792 3.990 4.756 4.756
4 .169
4.168 4.168
0.007 0.219
0.369 0.006 -0.247 0.184 0.006 0.013 0.329 0.006 0.266 0.437
9238 1696 2638 3298 4903 3370 8771 20521 14(6
176402
85700 19533
1224.04 1224.47 1224.41 0.02579 0.07143 0.02784 819.264 0.25210 2744.26 0.98663 1275.24 1277.19
1220 1220 1220 0.0256 0.0714 0.0278
15(H) 0.252
2740 0.997
1280 1280
QC Flag Legend M - Compound response manually integrated.
ExactCopy
3MI Environmental Laboratory
Page 131 o f 276
Report E02-0443
lut* Fil*; S\Etst%reeiAtrt*t\chn\ckKlejr*iSD020629*b\DUDE0105*D
Tenn. River Valley Samples
Pt* 2
18 PFBS <299)
20 PFHS <399) 3M Environmental Laboratory
(Exact Cl,/,
-_
/ y ai-- Osu
Pan 13? o f ?7F
Report E02-0443
Data Fil; \\Et*tartt\tar'tet\chet.\dud*jr.iMW20629.b\DUDE0105.D 21 PFOft (413)
Tenn. River Valley Samples
Pat 3
22 FOSA (498) 23 PFOS <499)
3M Environmental Laboratory
Exact C c/jy
.t7C__ fe/SaT*
Page 133 of 276
Report E02-0443
Tenn. River Valley Samples
D a ta File: \\Etstarget\ta rg et \ c h e m \ d u d e j r .i\D020629.b\DUDE0117.D Page l Report Date: 27-Aug-2002 10:07
3M Environmental Laboratory
E02-0443, Term. River Valley Samples
Data file : \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0117.D
Lab Smp Id: SL-2. C-6-1
Inj Date : 01-JUL-2002 09:33
Operator : mla
Inst ID: dudejr.i
Smp Info : Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun
Misc Info :
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020629,b\D020629.m
Meth Date : 27-Aug-200209:59 dudejr.i Quant Type: ESTD
Cal Date : 3 0 -JUN-2002 22:46
Cal File: DUDE0058.D
Als bottle: 69
Dil Factor: 1.00000
Integrator: Falcon
Compound Sublist: all.sub
Target Version: 4.12
02
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds
1 m s (J99)
20 PPHS (399) 21 PPOA (913) 22 POSA (999) 22 PPOS (999)
QUANT SIG MASS
299 299 299 399 413 4M 499 499
CONCENTRATIONS
ON-COLUMN
RT EXP RT DLT RT RESPONSE
fng/L)
PINAL (ng/mL)
3.398 3.176 3.750 3.798 3.996 4.769 4.181 4.605
3.381 3.381 3.381 3.792 3.990 4.756 4.168 4.168
0.007 -0.205
0.369 0.006 0.006 0.013 0.013 0.437
9473
1224.02
1418
1224.48
545 1224.53
2433
0.00120
8100
819.302
22417
0.33013
221283
2.26035
22665 1277.10
1220 1220 1220 0 . 0 0 1 2 0 (M)
8 1 9 (M) 0.330
2.26 1280
QC Flag Legend M - Compound response manually integrated.
Exact Copy of Or'r M : initia'
3M Environmental Laboratory
Page 134 of 276
Report E02-0443 Data Fil$ SSEtstarjatStarjatScheas*dudejr*iSD020629.bSDl/DE0il7.D
Tenn. River Valley Samples page 2
18 PFBS <299)
3M Environmental Laboratory
Exact Copy of Origina!
C u iC ^ /jJ ja J jT -
S 'fa '
oat.
Page 135 of 276
Report E02-0443
Data File: \SEtstareetStareetSche\dudejr.iSD02029.bSDUDE0117.D 21 PFOfl <4131
Tenn. River Valley Samples
Pace 3
23 PFOS <499)
3M Environmental Laboratory
i;xaci Copy Ciig;n-il i~'*' ' Dztr
Page 136 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: DUDE0066.D Report Date-, 27-Aug-20O2 11:05
Page 1
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file \\Etstarget\target\chem\dudejr.i\D020702(D20702).b\DUDE00S6.D
Lab Smp Id SL-3. C-2-2
'
Inj Date
03-JUL-2002 02:49
Operator
mla
Inst ID: dudejr.i
Smp Info
Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 J u n 02
Misc Info
Comment
Method
\\Etstarget\target\chem\dudejr.i\D020702(D20702).b\D020702 m
M e t h Date 27-Aug-2002 11:01 dudejr.i Quant Type: ESTD
Cal Date
03-JL-2002 01:21
Cal File: DUDE0058 D
Als bottle 55
'
Dil Factor 1.00000
Integrator Falcon Target Version: 4.12
Compound Sublist:all.sub
Co nc en tr at io n Formula-. Amt * D F * CpndVariable
Cpnd Variable
Local Compound Variable
Corapound 18 PFBS (299)
20 PFHS 2 1 PPOA 22 POSA 23 PPOS
(399) (413) (498) (499)
QUANT S1G HASS
299 299 299 399 413 498 499 499
CONCENTRATIONS
ON-COLUMN
PINAL
RT RXP RT DLT RT RBSPON58
(n g /ra L )
(ng/m L)
3 .3 9 5 3 .1 8 3 3 .7 5 7 3.8 1 9 4 .0 0 3 4 .8 0 3 4 .1 8 1 4.5 9 1
3 .3 8 7 3 .3 8 7 3 .3 8 7 3.7 9 1 3 .9 8 9 4 .7 4 8 4 .1 5 7 4 .1 6 7
O.OOB -0 .2 0 4
0.3 7 0 0.0 2 8 0.0 1 4 0.0S 5 0.0 1 4 0 .4 2 4
14872 3040 2236 S059
22949 23838 193614 239S4
1 2 2 0 .0 0 1 2 2 0 .4 8 1 2 2 0 .5 1 0 .2 0 3 9 4 0 .2 7 0 7 4 0 .4 3 1 0 8 1 .1 4 5 3 7 1 3 2 4 .2 2
1220 1220 1220 0 . 2 0 4 (N) 0 . 2 7 1 (M) 0 .4 3 1 1 .1 4 1320
QC Flag Legend M - Compound response manually integrated.
TM ct Copy of Origina,
Date
3M Environmental Laboratory
Page 137 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\Etstaret\tartt\cbe*\dudejr*i\D020702<D2702)*b\DUDE0066.D
Pace 2
18 PFBS <299>
$..i
2 0 PFHS < 3 9 9 )
3M Environmental Laboratory
Exact Copy of Origina!
(1L_ /,1 / / o / i -
Lnitia!
Oatp
Pace 138 of 278
Report E02-0443
Tenn. River Valley Samples
Data Fil: VsEtstar(tSfcartSchnSdudjr,.iMI620702<D20702),bvJ)UDE0066,D 21 PFOA <413)
Pas 3
23 PFOS <499)
3M Environmental Laboratory
Exact Copy of Original W M onto
Paae 139 of 276
Report E02-0443
Tenn. River Valley Samples
D a t a File : DUDE0076 .D Report Date: 27-Aug-2002 11:06
Page 1
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file \\Etstarget\target\chem\dudejr.i\D020702(D20702).b\DUDE0076.D
Lab Smp Id SL-3. C-4-2
Inj Date
03-JUL-2002 04:39
Operator
mla
Inst ID: dudejr.i
Smp Info
Tenn. River Va ll ey Fish. Prep-17 Jun 02. CMC/MLA. 20 Ju n 02
Mise Info
Comment
Method
\\ Et starget\target\chem\dudej r .i\D020702(D20702) .b\D020702.m
Meth Date 27-Aug-2002 11:01 dudejr.i Quant Type: ESTD
Cal Date
03-JUL-2002 01:21
Cal File: DUDE0058.D
Als bottle 62
Dil Factor 1.00000
Integrator Falcon
Compound Sublist: a l l .sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds I t PPBS (29)
20 p r u a (399)
21 PPOA (433) 22 POSA (499) 23 PROS (499)
QUANT SIO NASS
299 299 299 299 299 399 422 498 499 49 499
CONCBWTRATIONS
ON-COLUMN
RT BXP RT DLT RT R8SPONSS
(ng/mL)
PINAL (ng/mL)
2.394 3.182 3.770 3.825 3.S72 4.010 4.010 4.749 4.187
3 .8 1 1
4.591
2.387 3.387 3.387 3.791 3.791 3.791 3.989 4.748 4.167
4 .167
4.167
0.007 -0.205
0.383 0.034 -0.219 0.219 0.021 0.021 0.020
-0.3S 6
0.424
21375 2087 1284 3965 3286 3291 9130
20987 307947
13 67
20381
1219.74 1220.52 1220.55 0.18277 0.16964 0.16973 795.310 0.35235 3.50667
1334.68
1324.29
1220 1220 1220 0 .183 0.170 0.170
795 1M) 0.352
3.51
1330
1320
QC Flag Legend M - Compound response manually integrated.
Exact Copy of Origina!
3M Environmental Laboratory
Page 140 of 276
Report E02-0443
Tenn. River Valley Samples
Data File; SSEttargetStarget'\che*Sdu<iejr.iSD020702<I>20702).b\DUDE0076,B
Page 2
18 PFBS <299) 3M Environmental Laboratory
Exact Copy of Origina!
.C i * 19-1( ) i~
Initia.!
oa'-:
Pone
n f 97C
Report E02-0443
Tenn. River Valley Samples
D a ta F i l a ; W E t lt a r ja t \t a r ^ * t S o h a m \ d u d a jr . i\B 02Q 702<B 20702) . b\DUDE0076. D 21 PFOA <4135
2 2 FOSft <49B> 2 3 PFOS <499>
3M Environmental Laboratory
i Copyof Original
C J M .. l ^ / j f L'* Date
P a n o 1 4 7 rsf 7 7 R
Report E02-0443
Tenn. River Valley Samples
Data File : DUDE0083.D Report Date: 27-Aug-2002 11:06
Page 1
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file \\Etstarget\target\chem\dudejr.i\D020702(D20702).b\DUDE0083 D
Lab Smp Id: SL-3. C-6-1
Inj Date : 03-JUL-2002 05:56
Operator : mla
Inst ID: dudejr.i
Smp Info : Tenn. Ri ve r Va ll ey Fish. Prep-17 Ju n 02. CMC/MLA. 20 Jun 02
Mise Info :
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020702(D20702).b\D020702.m
M e t h Date .* 27-Aug-2002 11:01 dudejr.i Quant Type: ESTD
Cal Date : 03-JUL-2002 01:21
Cal File: DUDE0058.D
Als bottle: 68
Di i Factor*. 1.00000
Integrator: Falcon
Compound Sublist : a l l .sub
Target Version: 4.12
Concentration Formula: Amt * DF * CpndVariable
Cpnd Variable
Local Compound Variable
Compounds
18 FFBS (299) 20 PPHS (399) 21 PPOA (4X3) 22 FOSA (490) 23 FPOS (499)
3
\
QOANT SIS MASS
299 299 413 498 499
CONCENTRATIONS
ON-COLUNN FINAL
RT BXP RT DLT RT RESPONSE
(ng/mL)
(ng/mL)
Compound Not Detected. Compound Not Detected. Compound Not Detected. Compound Not Detected. Compound Not Detected.
3M Environmental Laboratory
!-:.vact Copy oi Original
one
Date
Page 143 of 276
Report E02-0443
Tenn. River Valley Samples
Data Filet S\EtstargitStareet\cheSdudJr.l\D020702(D20702).bSDUDE0083.I)
Page 2
18 PFBS (299) (UnetetaotacD 20 PFHS <399> JndataetaeD 3M Environmental Laboratory
Exact Copy of Original
cm... is-IjLoj^
1 Ai* ** nyet
Report E02-0443
Tenn. River Valley Samples
iuta Files \SEtstargetStareetSche\dudejr.iSD020702(D2702).bM>UI>E0083.D 21 PFOA (413) (Undetected)
Page 3
22 FOSA (498) (Undetected) 23 PFOS (499) (Undetected)
3M Environmental Laboratory
-.'.'c i Copy of Original
C k L - L 3 d iU s> 9 -
:nitia!
Data
Page 145 of 276
Report E02-0443
Tenn. River Valley Samples
D a ta File: \\ Et s t a r g e t \ t a r g e t \ c h e m \ d u d e j r .i\ D0 20 8 2A .b \DU DE 00 65.D Page 1 Report Date: 27-Aug-2002 14:11
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0065.D
Lab Smp Id Water Blank-1
Inj Date
12-AUG-2002 23:11
Operator
mla
Inst ID: dudejr.i
Smp Info
E02-0443 Water Blank Water Samples; non-GLP; 6/20/02; OK
Mise Info
Comment
Method
\\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m
Meth Date 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD
Cal Date
12-AUG-2002 16:13
Cal File: DUDEQ027,D
Als bottle 20
Dil Factor 1.00000
Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
Compound 1 PPBS U9)
2 PFHS 1399) 2 PPOX 1913) 4 POSA (49B) S PPOS (499)
QUANT SIG NASS
299 299 299 399 399 413 49# 499
goncbotrxxions
ON-COLUMN PINAli
RT EXP RT DLT RT RBSPONSB
(ng/mL)
(ng/L>
3.353 3.209 4.201 3.804 3.565 4. Ql 4.809 4.201
3.394 3.394 3.394 3.791 3.791 3.982 4.76# 4.160
'0.041 '0.105
0.807 0.013 '0.226 0.034 0.041 0.041
29174 5546 1904 5192 1012 9179 3390
34010
0.54141 503.660 503.788 0.15468 0.02703 0.04921 0.10549 0.16998
0.541 504 504
0.155 0.0270 0.0492
0.105 0.170
3M Environmental Laboratory
i^CQCi QOgt*/ 0T 'ji'iCj'ii.'!:
CdJii. __ U / / o f
Initial Date
Page 146 of 276
Report E02-0443 Data Fila: S\Et*tarit^tarttSch*Sdud*jr.iSD<>2<>B12A.bSDUBE<>065.D
Tenn. River Valley Samples
Pa*a 2
i PFBS <299) 2 PFHS <399) 3M Environmental Laboratory
Exact Copy o: Or;;-:
A * i i is J jjiL X -
initia!
Date
Page 147 of 276
Report E02-0443
D U File: SSEtltrc*t\trsetSchenSdudejr.SD020812A.b\DUEE0065.D
3 PFOA <413)
Tenn. River Valley Samples
4 FOSA <498) B PFOS <499)
3M Environmental Laboratory
Exact Copy of Crien-
Initial a Dater .a -
Page 148 o f 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\Etstarget\target\chem\dudejr.i\D02082A.b\DUDE0066 D Paqe l Report Date: 27-Aug-2002 14:11
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file : \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0066.D La b Smp Id: Wa t e r B l a n k - 2
Inj Date : 12-AUG-2002 23:22
Operator : mla
Inst ID: dudejr.i
Smp Info : E02-0443 Water Blank Water Samples; non-GLP; 7/17/02; OK
Misc Info :
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m
Meth Date : 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD
Cal Date : 12-AUG-2002 16:13
Cal File: DUDE0027.D
Als bottle: 21
Dil Factor: 1.00000
Integrator: Falcon Target Version: 4.12
Compound Sublist: all.sub
Cowpounda 1 PFBS (299)
2 PPHS (399) 3 PPQA (413) 4 POSA (498) 5 PFOS (499)
QUANT SIG MASS
299 299 299 299 399 413 413 498 499
CONCENTRATIONS
ON-COLUMN
PINAL
RT BXP RT DLT RT RESPONSE
(ng/oL)
(ng/aL)
3.354 3.210 3.743 4.195 3.805 4.010 4.359 4.810 4.201
3.394 3.394 3 .394 3.394 3 .791 3.982 3.982 4.768 4.160
-0.040 0.184
0.349 0.801 0.014 0.028 0.377 0.042 0.041
54510 10619
1176 3650 4219 11746 1069 3371 33507
1.43376 503.482 503.813 503.727 0.12496 0.21476 401.976 0.10487 0.15720
1.43 503 504 504
0.125 0.215
402 0.105 0.157
ExactCcipy of Cfe;;.-.
3M Environmental Laboratory
Page 149 of 276
Report E02-0443 Data Fila: \\EttarttStarttSch\dud*jr.l\K>20812A.b\DUDE00.6.D
Tenn. River Valley Samples
Pag Z
3M Environmental Laboratory
fccaciCov J S /^ Z Date
Page 150 of 276
Report E02-0443
nata File* SSEtitarjetStar|;etScheSdudejr.iM)020812Pl.b\BUDE006.D 3 PFOfi <413)
Tenn. River Valley Samples
Pace 3
4 FOSA <49 0)
S PFOS <499)
3M Environmental Laboratory
bactCopy
X itiL fnWai "
17
Page 151 o f 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\ Et st ar g e t \ t a r g e t \ c h e m \ d u d e j r .i\D02082A.b\DUDE0076 D Pace 1
Report Date: 27-Aug-2002 14:11
'a
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file Lab Smp Id
3\8\0E3t2starget\target\chem\dudejr.i\D020812A.b\DUDE0076 'D
Inj Date
13-AUG-2002 01:12
Operator
mla
Inst ID: dudejr.i
Smp Info
E02-0443-38032; Water Samples; non-GLP; 6/20/02; OK
Mise Info
Comment
Method
\\Etstarget\target\chem\dudejr.i\D02 08 l2A.b\D02 0 8 l2A m
Meth Date 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD
Cal Date
12-AUG-2002 16:13
Cal File: D U D E 0 0 2 7 .D
Al s bottle 26
Dil Factor 1.00000
Integrator Falcon Target Version: 4.12
Compound Sublist: all.sub
Compound 1 PPB3 (a s s )
2 PPHS (a ss) 3 PPOA (413) 4 POSA (4SS) S PPOS (4SS)
QUANT SIQ NASS
299 299 299 299 299 299 399 413 499 499
CONCBNTRATIONS
ON-COLUMN
PINAL
RT BXP RT DLT RT RESPONSE
(ng/nL)
(ng/mL)
3.401 2.540 3.203 3.91 4.044 4.215 3.90S 4.003 4.799 4.1B1
3.394 3.394 3.394 3.394 3.394 3.394 3.791 3.992 4.7(8 4.1(0
0.007 **0.854 -0.191
0.424 0.(50 0.821 0.014 0.021 0.021 0.02
193(1 147211
19(( 29(2
759 777 15729S 84190 138473 190157
0.19(64 4.72(22 503.795 503.751 503.929 503.927 4.95809 4.94452 4.5(920 5.18991
0.197 4.73 504 504 504 504 4.86 4.94 4.57 5.19
3M Environmental Laboratory
Exact Copi
Cri ( Ul U L '
initial
Difir.
Page 152 of 276
Report E02-0443
Bata Fil; SSEt5trtNt^gt\chmNdudJr.i\D02812A.bSDUDE007.D
Tenn. River Valley Samples Pae 2
3M Environmental Laboratory
Exact Copyof Origina!
(J y C w lt o I o L ^
initia! Date
Page 153 of 276
Report E02-0443
Data Til: SVtstargatStargetSchmSdudjr.iM)020812A.bMUDE0076.I> 3 PFOft <413)
Tenn. River Valley Samples
4 FOSA <498) 8 PFOS <499)
3M Environmental Laboratory
'c Copy <;/ Onr~;l:A} t i n c tilc fo -L .
Paae 154 of 276
Report E02-0443
Tenn. River Valley Samples
D a ta File: \ \ E t s t a r g e t \ t a r g e t \ c h e m \ d u d e j r .i\ D0 20 8 2 A . b \ D U D E 0 0 7 3 .D Page l Report Date: 27-Aug-2002 14:11
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
D a t a file \\Etst ar ge t\ tar ge t\ ch em \d udej r .i\D020812A.b\DUDE0073.D
Lab Smp Id 38029
Inj Date Operator
Snip Info
13-AUG-2002 00:39 m l a Inst ID: dudejr.i E02-0443-38029; Water Samples; non-GLP; 6/20/02; OK
Misc Info
Comment Method
Meth Date
Cal Date
\\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m
27-Aug-2002 14:06 dudejr.i Quant Type: ESTD
12-AUG-2002 16:13
Cal File: DUDE0027.D
Als bottle 25
Dil Factor 1.00000 Integrator Falcon
Compound Sublist : a l l .sub
Target Version: 4.12
Coiapounda
l PPBS <29) 2 PPHS (99) 3 PPOA 4 POSA (49#) 5 PPOS (499)
ri
QUANT SIG NASS
39 39 413 49 49 499
RT sx? m
DLT RT RBSPONSB
CONCENTRATIONS
ON*COLUMN
FINAL
(ng/*L)
(ng/mL)
3 .408 3 . 11 4.009 4.796 4.167 4.467
3.394 3.791 3.962 4.768 4.160 4.160
0.014 0.020 0.027 0.028 0.027 0.307
9092 252177 328861
34000 631586 131570
2.65691 7.85210 21.8421 1.31439 20.1641 3.2904
2.64(H) 7.8S 21.8 1.11(H) 20.2 3.29
QC Flag Legend M - Compound response manually integrated.
Exact Copy' o f Orini:r
Lh}C__ l3 . h p / o i-
Wsf
Of:!:
3M Environmental Laboratory
Page 155 o f 276
Report E02-0443 Data Fila: S\Etstarget\target\chSdud,jr.i\DCi20812A.bSDtJDE0073.D
Tenn. River Valley Samples
Paga 2
1 PFSS <29 9)
3M Environmental Laboratory
Exact Copy
.
RitiriI
Paas 15R of 27R
Report E02-0443
Data Fila; SSEtstarjetStartetSchenSdudejr. i\D020812A.b\DUDE0073.D 3 PFOA <413>
Tenn. River Valley Samples
4 FOSA <490)
3M Environmental Laboratory
Exact Copy of Origin: 1
M LL. I'llfo/a z -
Initia!
Date
Page 157 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\Etstarget\target\chem\dudejr.i\D02082B.b\DUDE0130 D Paqe 1 Report Date: 29-Aug-2002 07:12
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
D L
a a
t b
a
fi Smp
leId::
3\8\0E3t0starget\target\chem\dudejr.i\D020812B.b\DUDE0130.D
Inj Date : 13-AUG-2002 11:08
Operator : mla
Inst ID: dudejr.i
Smp Info : E02-0443-38030; Water Samples; non-GLP; 7/17/02; OK
Mise Info :
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020812B.b\D020812B.m
Meth Date : 29-Aug-2002 07:08 dudejr.i Quant Type: ESTD
Cal Date : 13-AUG-2002 06:44
Cal File: DUDE0106.D
Als bottle: 42
Dil Factor: 1.00000
Integrator: Falcon
Compound Sublist: all.sub
Target Version: 4.12
Compounds 1 PPBS (99)
a PFHS (399) 3 PFOA <411) 4 FOSA (49) 5 PFOS (499)
QUANT S IO MASS
299 299 299 299 399 413 498 499
CONCENTRATIONS
ON-COLUMN PINAL
RT 8XP RT DLT RT RESPONSB
(ng/mL)
(ng/mL)
3.387 2.498 3.203 3.777 3.777 3.988 4.741 4.139
3.394 3.394 3.394 3.394 3.791 3.982 4.768 4.160
-0.007 -0.896 -0.191
0.3 83 -0.014 -0.014 -0.027 -0.021
197441 1231 2246
11268 8387299 4152125 7980357 8914428
2926.50 2935.66 2935.62 2935.20 424.865 427.860 300.226 423.673
2930 2940 2940 2940
425 428 300 424
teact Copy a : O ri: L2h
3M Environmental Laboratory
Pane 158 or 776
Report E02-0443
Data Fil: S\Etstarct\target\chem\dudJr.i\D020612BbM)UD0130,D
Tenn. River Valley Samples
Pag 2
2 PFHS <J99>
3M Environmental Laboratory
u V ,t/a .
initia-
r-z-,-.
CO * * 0-7C?
Report E02-0443
Data File; S\Etitarjt\tareet\ch*\tiudejr.i\ D020812B.b\DUDE0130.D 3 PFOA <413)
Tenn. River Valley Samples
4 FOSA <498)
5 PFOS <499)
3M Environmental Laboratory
Exact Copy;,; jC l \x I j o/ d ~>-
Page 160 o f 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\ Et st ar get\target\chem\dudej r .i\D02082A.b\DUDE0092.D Page 1 Report Date: 27-Aug-2002 14:12
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file : \\Etstarget\target\chem\dudej r.i\D020812A.b\DUDE0092.D
Lab Smp Id: 38043
Inj Date : 13-AUG-2002 04:09
Operator : mla
Inst ID-. dudejr.i
Smp Info : E02-0443-38043; Water Samples; non-GLP; 6/20/02; OK
Mise Info :
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m
Meth Date : 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD
Cal Date : 12-AUG-2002 16:13
Cal File: DUDE0027.D
Als bottle: 34
Dil Factor: 1.00000
Integrator: Falcon
Compound Sublist: all.sub
Target Version: 4.12
Coapounda 1 PFBS (1991
2 PFHS (399) 3 PPOA (113) 4 POSA (9) 5 PPOS (499)
QUANT SIG NASS
399 299 299 299 299 399 413 49ft 499
CONCENTRATIONS
ON-COLUMN
PINAL
RT RXP RT DLT RT RBSPON3B
(ng/aL)
(ng/mL)
3.354 2.451 3.210 3 . aia 4.037 3.942 4.010 4.794 4.195
3.394 3.394 3.394 3.394 3.394 3.791 3.982 4.76ft 4.140
-0.040 -0.943 -0.184
0.424 0.443 0.171 0.02ft 0.02ft 0.035
3284ft 739
4284 1244 1953 14543 9481 4471 30951
0.47061 503.829 503.434 503.811 503.786 0.50173 0.06868 0.2069ft 0.07297
0.671 504 504 504 504
0.502 0.0667
0.207 0.0730
3M Environmental Laboratory
&<3Ct Copy nf Q frh!
Page 161 of 276
Report E02-0443 D*t Fil; SSEt*t*r*t\tarf;tSchm\dudejr1SD020812A*bSDUDE0092,D
Tenn. River Valley Samples
Pa* 2
2 PFHS <399>
3M Environmental Laboratory
r i !. fiinl x h o l o x -
nira! Daia
P an ir o o* 07R
Report E02-0443
Data Files SSEtstar*et\tartet\ehenSdudejr.iSD020812A.IAmJDE0092.1) 3 PFOA <413)
Tenn. River Valley Samples
4 FOSA <498) B PFOS <499)
h i e r wm
n . -------
Report E02-0443
Term. River Valley Samples
D a ta File: \\E t starget\target\c he m\ du de jr .i\D020 81 2A .b \DU DE 00 67.D Page Report Date: 27-Aug-2002 14:11
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
D a ta file : \\ Et st ar ge t\target\chem\dudejr .i\D020812A.b\DUDE0067.D
Lab Smp Id: 38025
Inj Date : 12-AUG-2002 23:33
Operator : mla
Inst ID: dudejr.i
Smp Info : E02-0443-38025; Water Samples; non-GLP; 6/20/02; OK
Misc Info :
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m
Meth Date : 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD
Cal Date : 12-AUG-2002 16:13
Cal File: DUDE0027.D
Als bottle: 22
Dil Factor: 1.00000
Integrator: Falcon
Compound Sublist: all.sub
Target Version: 4.12
Compounds
1 PPBS 2 PFHS 3 PPOA 4 POSA 5 PPOS
(299) (399) (413) (498) (499)
quant sig
MASS
299 399 413 49B 499 499
EXP RT
DLT RT RESPONSE
CONCENTRATIONS
ON-COLUMN
PINAL
(ng/mL)
(ng/mL)
3.401 3.812 4.003 4.796 4.181 4.468
3.394 3.791 3.982 4.76B 4.160 4.160
0.007 0.021 0.021 0.028 0.021 0.308
98538 247750 321649
29388 583658 135043
2.99206 7.71134 21.3198 0.96228 18.4924 3.40254
2 . 9 9 () 7.71 21.3 0.962 IH) 18.5 3.40
QC Flag Legend M - Compound response manually integrated.
i
13Ct Co; C l L . U /[ > ja i---
3M Environmental Laboratory
Page 164 of 276
Report E02-0443
Sata File: SSEttarjetStarjet\cheS<iudjr.iSD020812n.b\BUBE0067.B
Tenn. River Valley Samples
Page 2
1 PFBS <299>
3M Environmental Laboratory
Paoe 165 of 276
Report E02-0443
Data Fila: S\Etstarat\taret\cha\ciudejr*iM)020912A*bMUJDE0067*D 3 PFOA ( 4 1 3 )
Tenn. River Valley Samples
Pag* 3
4 FOSA < 4 9 8 ) 5 PFOS < 4 9 9 )
3M Environmental Laboratory
* pp ~ *7r
Report E02-0443
Tenn. River Valley Samples
D a t a File: \ \ E t s t a r g e t \ t a r g e t \ c h e m \ d u d e j r .i\D02082A.b\DUDE0069.D Page 1 Report Date: 27-Aug-2002 14:11
3M Environmental Laboratory-
E02-0443, Tenn. River Valley Samples
Data file \\Etstarget\target\chem\dudejr.i\D0208l2A.b\DUDE0069.D
Lab Smp Id 38026
Inj Date Operator
Smp Info
12-A U G - 2002 23-.55 ml a Inst ID: dudejr.i E02-0443-38026; Water Samples; non-GLP; 7/17/02; OK
Mise Info
Comment Method Meth Date Cal Date
\\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m
27-Aug-2002 14:06 dudejr.i Quant Type: ESTD
12-AUG-2002 16:13
Cal File: DUDE0027.D
Als bottle 23
Dil Factor 1.00000
Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
Compound*
1 PPBS (199) 2 PPHS (399) 3 PPOA (413) 4 POSA (499) S PPOS (499)
QUANT SIO MASS
299 399 413 499 499 499
CONCENTRATIONS
ON-COLUMN PINAL
RT EXP RT DLT RT R8SPONSB
(ng/*L)
(ng/aL)
3.401 3.811 4.003 4.789 4.180 4.447
3.394 3.791 3.982 4.768 4.160 4.160
0.007 0.020 0.021 0.021 0.020 0.307
118567 255866 340061
31162 648655 140168
3.70420 7.96948 22.6524 1.02079 20.7906 3.56801
3.70(H) 7.97 22.6 1 . 01(H) 20.8 3 .S7
QC Flag Legend M - Compound response manually integrated.
3M Environmental Laboratory
C t t l t / / / / O'*-
Page 167 of 276
Report E02-0443 Sata Fila: \\Etstarcat\tarcet\chem\dudajr .iSD020812B.b\DUDE009,D
Tenn. River Valley Samples
Pa 2
Z.4 z'.B _________
M3O2_-__3_U____I_o
2 PFHS (399)
3M Environmental Laboratory
eT c,* * 0 n . C7V_
Oats
P a n 1RB o f 97P;
Report E02-0443
Bata F U * S SSEtstargetStargttScheiiiSdud*ji~.i\IK>20812A.bSDlJDE069.B 3 PFOA <413)
Tenn. River Valley Samples
4 FOSA <498) B PFOS <499)
3M Environmental Laboratory
h a d Capy -c<v;:;r.--(H C
Page 169 of 276
Report EQ2-0443
Tenn. River Valley Samples
D a t a File: \\ Et st ar g e t \ t a r g e t \ c h e m \ d u d e j r . i\ D0 20 8 2A .b \DU DE 00 71.D Page 1 Report Date: 27-Aug-2002 14:11
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
D a ta file : \ \ E t s t a r g e t \ t a r g e t \ c h e m \ d u d e j r .i\D020812A.b\DUDE0071.D
Lab Smp Id: 38027
Inj Date : 1 3 -AUG-2002 00:17
Operator : mla
Inst ID: dudejr.i
Smp Info : E02-0443-38027; Water Samples; non-GLP; 7/17/02; OK
Misc Info
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m
Meth Date : 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD
Cal Date : 12-AUG-2002 16:13
Cal File: DUDE0027.D
Als bottle: 24
Dil Factor: 1.00000
Integrator: Falcon
Compound Sublist: all.sub
Target Version: 4.12
Conpound*
1 PPBS (199) 2 PFHS (399) 3 PPOA (413) 4 POSA (491) S PPOS (499)
QUANT SIO NASS
29 399 413 49 499 499 499
CONCENTRATIONS
ON-COLUMN
PINAL
RT RXP RT DLT RT RBSFONSB
(ng/ttL)
(ng/L)
3.401 3.811 4.002 4.794 4.180 3.864 4.447
3.394 3.791 3.982 4.748 4.140 4.140 4.140
0.007 0.020 0.020 0.028 0.020 -0.294 0.307
102829 405593 412129 121332 808339
4108 85093
3.14444 12.7977 27.9472 4.00115 24.5743 379.787 1.79743
3.14(H) 12.8 28.0 4.00 26.4
380 1.80
QC Flag Legend M - Compound response manually integrated.
' CY.
3M Environmental Laboratory
Page 170 of 276
Report E02-0443
Bata Fila: SSEtstar atStaratSchenSdudej r .iSD020812AbSBUDE071*D
Tenn. River Valley Samples
Paca 2
i PFBS <299) 2 PFHS <399)
3M Environmental Laboratory
C i,w t / t / c
Page 171 of 276
Report E02-0443
Data Fila: S\Etstarat\taretSchew\duc*ajr*iND20812A*b\DUDE0071*D 3 PFOA <413)
Tenn. River Valley Samples
4 F OSA <498)
3M Environmental Laboratory
c fc /w o i-
Dano 17? nf ?7C
Report E02-0443
Tenn. River Valley Samples
Data File: \\Etstarget\target\chem\dudejr.i\D02082A.b\DUDE0078 D Page 1 Report Date: 27-Aug-2002 14:11
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
D a ta file : \\ Et st arget\target\chem\dudejr .i\D020812A.b\DUDE0078.D
Lab Smp Id: 38033
Inj Date : 13-AUG-2002 01:34
Operator : mla
Inst ID: dudejr.i
Smp Info : E02-0443-38033; Water Samples; non-GLP; 6/20/02; OK
Mise Info :
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m
Meth Date : 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD
Cal Date : 12-AUG-2002 16:13
Cal File: DUDE0027.D
Als bottle: 27
Dil Factor: 1.00000
Integrator: Falcon
Compound Sublist: all.sub
Target Version: 4.12
Compounds 1 PPBS (
2 PPHS (399) 3 PFQA <*13> 4 POSA (49 5 PFOS (199)
QUANT SIO MASS
299 299 299 299 299 299 413 494 499
CONCENTRATIONS
RT EXP RT
DLT RT RBSPONSB
ON-COLUMN (ng/sL)
FINAL (ng/ttL)
3.340 3.210 3.818 4.058 3.812 3.949 4.010 4.796 4.194
3.394 3.394 3.394 3.394 3.791 3.791 3.982 4.768 4.140
-0.034 -0.184
0.424 0.464 0.021 0.178 0.028 0.028 0.034
26600 4235 1671 634 5685 5436
11537 5497
35066
0.45093 S03.706 503.796 503.832 0.16974 0.16313 0.20129 0.17456 0.20349
0.451 504 504 504
0.170 0.162 0.201 0.174 0.203
3M Environmental Laboratory
Page 173 o f 276
Report E02-0443 Dita File: \\Etstarset\tarsetSchea\dudejr.i\D020812fi.bSDUDE0078.D
Tenn. River Valley Samples
Pase 2
2 PFHS <399>
3M Environmental Laboratory
: .'.a uo j , c M . l l n l o K.
P i i *"7 /* * 9 0 7 C
Report E02-0443 Data Fi Ir; SSEtstargetStargetSchewSdudejr.iSD0208i2A.b\DUDE0078.D
Tenn. River Valley Samples
Page 3
4 FOSA <49S>
3M Environmental Laboratorv
''CiL}.- rt-...
Psno 17: of 97R
Report E02-0443
Tenn. River Valley Samples
D a t a File: \\ Et st ar ge t\ tar ge t\ ch em \d ude jr .i\D02082A.b\DUDE0080.D Page 1 Report Date: 27-Aug-2002 14:11
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0080.D
Lab Smp Id 38034
Inj Date
13-AUG-2002 01:57
Operator
mla
Inst ID: dudejr.i
Smp Info
E02 - 0 4 4 3 - 3 8 0 3 4 Water Samples; non-GLP; 6/20/02; OK
Mise Info
Comment
Method Meth Date
\\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD
Cal Date Als bottle
12-AUG-2002 16:13 23
Cal File: DUDE0027.D
Dil Factor 1.00000
Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
Copounds
1 PPBS 2 PPHS 3 PPOA 4 POSA
(299) (399) (413) (496)
5 PFOS (4 9 9 )
quant s is
MASS
299 399 413 498 498 499
BXP RT
DLT RT RESPONSE
CONCENTRATIONS
ON-COLUMN
PINAL
(ng/m L)
(ng/m L)
3.4 0 1 3.8 1 2 4.0 1 0 4.7 9 6 5 .0 9 0 4.1 9 4
3.3 9 4 3 .7 9 1 3.9 8 2 4.7 6 8 4.7 6 8 4 .1 6 0
0.0 0 7 0.0 2 1 0.0 2 8 0.0 2 8 0.3 2 2 0.0 3 4
28016 8673
17031 6747 276
51049
0 .5 0 0 7 0 0 .2 6 1 0 4 0 .5 5 6 0 3 0 .2 1 6 0 7 0 .0 0 2 9 4 0 .7 1 1 2 7
0.501(H ) 0 .2 6 1 0 .5 5 6 0.2 1 6 0 .0 0 2 9 4 0 .7 1 1
QC Flag Legend M - Compound response manually integrated.
3M Environmental Laboratory
Car
ok
Page 176 of 276
Report E02-0443 Data Fil: WEtstarjetStarftSch*Sdudjr .i\I0208i2fi.bSDUDE0080.D
Tenn. River Valley Samples
Paee 2
2 PFHS < 39 9)
3M Environmental Laboratory
P 3 0 0 1 7 7 <> 9 7 C
Report E02-0443
Data Fila: S\EtstaretStartet\chenSdud#jr.i\D0208i2A.b\DUDE0080.D 3 PFOft (413)
Tenn. River Valley Samples
4 FOSA <498> S PFOS (499)
1 shr>rotr>rv
o: Original
fet'j
Date
170
Report E02-0443
Tenn. River Valley Samples
D a ta File: \\ Et starget\ t ar ge t\ ch em \du de jr .i\ D0 20 8 2 A . b \ D U D E 0 0 8 4 .D Page 1 Report Date: 27-Aug-2002 14:11
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file : \\Etstarget\target\chem\dudej r .i\D020812A.b\DUDE0084.D
Lab Smp Id: 38037
Inj D a te : 13-AUG-2002 02:41
Operator : mla
Inst ID: dudejr.i
Smp Info : E 0 2 - 0 4 4 3 -38037; Wa te r Samples,- non-GLP; 6/20/02; OK
Mise Info :
Comment
Method
: \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m
Meth Date : 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD
Cal Date : 12-AUG-2002 16:13
Cal File: DUDE0027.D
Als bottle: 30
Dil Factor: 1.00000
Integrator: Falcon
Compound Sublist: all.sub
Target Version: 4.12
Compounds
1 PFBS ( 2 9 9) 2 PPHS ( 399) 3 PPOA (13) 4 POSA, (9) 5 p p o a (99)
QUANT SIS MASS
299 399 413 498 499
COHCBNTRATIONS
ON-COLUMN PINAL
RT RXP RT DLT RT R8SPONSB
(ng/ttL)
(ng/mL)
3.353 3.805 4.010 4.798 4.188
3.394 3.791 3.982 4.788 4.180
>0.041 0.014 0.028 0.028 0.028
32546 1297B 14081
8547 43651
0.6S999 0.39267 0.36547 0.20948 0.47606
0.660(H) 0.393 0.365 0.209 0.476
QC Flag Legend M - Compound response manually integrated.
Of. (j-j.
."Slj
a. . .
3M Environmental Laboratory
Page 179 of 276
Report E02-0443
Data Fil: \ \ E t t ^ e t S t ^ c t \ c W \ d u d * j r . i \ D 0 2 < > 8 i 2 A . b \ D U D E 0084.1!
Tenn. River Valley Samples
Pae 2
2 PFHS <399>
3M Environmental Laboratory
'*xaciCoyo; Orfgij53
L> ^ g x
Dao 100 **
Report E02-0443
Data Fi Its S\EtstargttStarcttSchtnSdudtjr.iSD020812A.bM)UDE0084>D 3 PFOft <4135
Tenn. River Valley Samples
4 FOSA (498) B PFOS (499)
3M Environmental Laboratory
i / W cJ--
Ppoo 1S1 of 97R
Report E02-0443
Tenn. River Valley Samples
Data File; \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0086 D Paqe 1 Report Date: 27-Aug-2002 14:12
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file : Lab Smp Id:
\38\0E3t8starget\target\chem\dudejr.i\D020812A.b\DUDE0086
D
Inj Date : 1 3 -AUG-2002 03:03
Operator : mla
Inst ID: dudejr.i
Smp Info : E02-0443-38038; Water Samples; non-GLP; 6/20/02; OK
Misc Info :
Comment :
Method
: \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m
Meth Date : 27-Aug-2002 14:06
r .i Quant Type : ESTD
Cal Date : 12-AUG-2002 16:13 Als bottle: 31
Cal File: DUDE0027.D
Dil Factor: 1.00000
Integrator: Falcon Target Version: 4.12
Compound Sublist: all.sub
;| Coapounda
1 FFBS 3 PFHS 3 PPQA 4 POSA 5 PFOS
(399) (399) <413) (490 (499)
QUANT SIS MASS
399 399 413 499 499
CONCENTRATIONS
ON-COLUMN
PINAL
RT 8XP RT DLT RT RESPONSE
(ng/L)
<ng/*L)
3.353 3.812 4.003 4.798 4.188
3.394 3.791 3.9B2 4.768 4.140
>0.041 0.021 0.021 0.028 0.028
34B96 8214
1S135 3452
44194
0.74264 0.24701 0.43379 0.107S4 0.49338
0.743(H) 0.247 0.434 0.108 0.493
; QC Flag Legend i
. M - Compound response manually integrated.
i
t
.i
Exact Copyof Origina;
JniSaJ
Dato
3M Environmental Laboratory
Page 182 of 276
Report E02-0443 Data Fila: SSEtstartetStartetSchenSdiKiejr. lSD020812n.bSDUDE0086.D
Tenn. River Valley Samples
Pate 2
2 PFHS ( 3 9 9 )
3M Environmental Laboratory
tVCtCopy of Originai iU o /rrx -
D fm 1 01
9TP
Report E02-0443
Data Filai SSEtstaratStargatSchemSudajr .iSDO2O012A.b\IHJD0086.D 3 PFOA <413>
Tenn. River Valley Samples
4 FOSA <498> S PFOS <499>
3M Environmental Laboratory
'rxnctCopyofOriginai
C- r ~ l Dite
Pane 184 of ? 76
Report E02-0443
Tenn. River Valley Samples
Data File: \\Etstarget\target\chem\dudejr.i\D02082B.b\DUDE0127.D Paqe 1 Report Date: 29-Aug-2002 07:12
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
Data file \\Etstarget\target\chem\dudejr.i\D020812B.b\DUDE0127 D Lab Smp Id 38028
Inj Date
13-AUG-2002 10:35
Operator
emc
Inst ID: dudejr.i
Smp Info
E 0 2 - 0443-38028; Wa te r Samples,- non-GLP; 7/17/02; OK
Mise Info
Comment
Method
\\Etstarget\target\chem\dudejr.i\D020812B.b\D020812B.m
Meth Date 29-Aug-2002 07:08 dudejr.i Quant Type: ESTD
Cal Date
13-AUG-2002 06:44
Al s bottle 41
Cal File: DUDE0106.D
Dii Factor 1.00000
Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
Conpounda 1 PPBS (299)
2 PFHS (299) 3 PFOA (413) 4 FOSA (498) S PFOS (499)
QUANT SZG MASS
399 399 399 399 399 399 399 413 498 499
CONCENTRATIONS
ON-COLUMN
PXNAL
RT BXP RT DLT RT RESPONSE
(ng/itL)
(ng/mL)
3.388 2.697 3.073 3.777 4.085 4.349 3.777 3.962 4.741 4.140
3.394 3.394 3.394 3.394 3.394 3.394 3.791 3.982 4.768 4.160
-0.006 -0.697 -0.321
0.383 0.691 0.8SS -0.014 -0.020 -0.027 -0.020
195308 963
9274 8460
602 439 7874701 3848302 802S349 7827644
2926.60 2935.68 2935.29 2935.33 2935.69 2935.70 392.569 388.428 302.105 361.783
2930 2940 2940 2940 2940 2940
392 388 302 362
'*'<^1 j ; v `jVir/'uhi
i ' . V .
3M Environmental Laboratory
Paoe 185 of 276
Report E02-0443
Data File: S\Etstar{et\tirct\chenSdudejr.iM)020812B.b\DUDE0127.D
Tenn. River Valley Samples
Pate 2
1 PFBS <299) 3M Environmental Laboratory
-,;uoi C o// of Origina! Iz fo t T-
tnttia! Dais
Pape 186 of 276
Report E02-0443
Data File: SStstarj;etStar|:etNcheSdudejr*iSD020812B*bM)UDC>t27,D 3 PFOA (413)
Tenn. River Valley Samples
Page 3
4 FOSA <498>
6 PFOS <499)
3M Environmental Laboratory
xrct Copy o; OriclriT'
riit/aj
l n if;
Pane 187 of 276
Report E02-0443
Tenn. River Valley Samples
D a ta File: \ \ Et st ar ge t\ta r g e t \ c h e m \ d u d e j r .i \ D 0 2 0 81 2B .b \DU DE 01 33.D Page 1 Report Date: 29-Aug-2002 07:12
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
D a t a file \\Etstarget\target\chem\dudejr.i\D020812B.b\DUDE0133.D
Lab Smp Id 38036
Inj Date
13-AUG-2002 11:41
Operator
mla
Inst ID: dudejr.i
Smp Info
E02-0443-38036; Water Samples; non-GLP; 6/20/02; OK
Mise Info
Comment
Method
\\Etstarget\target\chem\dudejr.i\D020812B.b\D020812B.m
Meth Date 29-Aug-2002 07:08 dudejr.i Quant Type: ESTD
Cal Date
13-AUG-2002 06:44
Cal File: DUDE0106.D
Als bottle 43
Dil Factor 1.00000
Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
Com pound* 1 VFBS [2 9 9 )
2 PPHS (3S S ) 3 FPOA (4 1 3 ) 4 POSA (4 9 8 ) 5 PPOS (4 9 9 )
QUANT S IG MASS
299 299 299 299 299 399 413 498 499 499
C O N C ENTRATIONS
ON-COLUM N
F IN A L
RT BXP RT D LT RT RBSFONSB
(iv g /m L }
< n g /i L )
3 *3 8 8 3 .0 7 3 3 .7 7 7 4 .0 8 5 4 .2 4 2 3 .7 7 1 3 .9 8 2 4 .7 3 5 4 .1 3 3 3 .8 3 2
3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .7 9 1 3 .9 8 2 4 .7 6 8 4 .1 6 0 4 .1 6 0
> 0 .0 0 6 -0 .3 2 1
0 .3 8 3 0 .6 9 1 0 .8 4 8 -0 .0 2 0 -0 .0 2 0 -0 .0 3 3 -0 .0 2 7 -0 .3 2 8
2020S3 1800S 9508 820 817
8071912 3927038 8558553 7890357
906
2 9 2 6 .2 9 2 9 3 4 .8 8 2 9 3 5 .2 8 2 9 3 5 .6 8 2 9 3 5 .6 8 4 0 4 .8 7 0 3 9 8 .4 8 7 3 2 4 .5 3 5 3 6 5 .2 6 5 3 0 7 1 .2 5
2930 2930 2940 2940 2940
405 398 324 365 3070
3M Environmental Laboratory
Exact Copy f,;<yg,,-
M O I u Ij p / ^
initiai ->(<
Paoe 188 of 27
Report E02-0443
Data File: \\EtstarsetStarSetSchem\dudejr.i\D02081ZB.b\DUDE0133.D
Tenn. River Valley Samples
Pace 2
1 PFBS <299) 2 PFHS (399)
3M Environmental Laboratory
IzX&ciCopy fif Orb?n-
C JH jL LOz/ j d I s l ^ inijip' y , l:.
m eD 3 r,o -ta o a r
Report E02-0443
Data File SSEtstarjit\targetScb*nSdudajr.iSD020812B.b\DUDE0133.D 3 PFOA (413>
Tenn. River Valley Samples
4 FOSA (498)
3M Environmental Laboratory
4JJ2C n /fd / l-
D o n o 1Qn
Report E02-0443
Tenn. River Valley Samples
D a ta Pile: \\Etstarge t\ tar ge t\ ch em \d ude jr .i \ D 0 2 0 8 2 B .b\DUDE0136.D Page 1 Report Date: 29-Aug-2002 07:12
3M Environmental Laboratory
E02-0443, Tenn. River Valley Samples
D a t a file : \\Etstarge t\ tar ge t\ ch em \d ude jr .i \D 02 08 12 B.b \D UD E0 13 6.D Lab Smp Id: 38040
Inj Date : 1 3 -AUG-2002 12:14
Operator : mla
Inst ID: dudejr.i
Smp Info : E02-0443-38040; Water Samples; non-GLP; 6/20/02; OK
Misc Info :
Comment Method
: : \\Etstarget\target\chem\dudejr.i\D020812B.b\D020812B.m
M e t h Date : 29-Aug-2002 07:08 dudejr.i Quant Type.- ESTD
Cal Date : 13-AUG-2002 06:44
Cal File: DUDE0106.D
Als bottle: 44
Dil Factor: 1.00000 Integrator: Falcon
Compound Sublist: a l l .sub
Target Version: 4.12
Com pounds 1 PFBS (2 9 9 )
2 PPHS (3 9 9 ) 3 PFOA {4 1 3 ) 4 POSA (*98) 5 PP09 (4 9 9 )
QUANT S IG HASS
299 299 299 299 299 399 413 498 499
C O N C E N T R A T IO N S
O N -C O LU M N
P IN A L
RT EXP RT D LT RT RESPONSE
(n g /m L )
(n g /n L )
3 .3 0 7 2 .9 3 6 3 .0 7 3 3 .9 3 2 4 .0 2 3 3 .7 7 7 3 .9 0 1 4 .7 4 1 4 .1 3 2
3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .7 9 1 3 .9 9 2 4 .7 6 8 4 .1 6 0
*0 .0 0 7 - .4 S 8 *0 .3 2 1
0 .4 3 9 0 .6 2 9 -0 .0 1 4 -0 .0 2 1 -0 .0 2 7 -0 .0 2 8
200230 5425
13185 10649
485 8246279 3997548 7955892 7760025
2 9 2 6 .3 7 2 9 3 5 .4 7 2 9 3 5 .1 1 2 9 3 5 .2 3 2 9 3 5 .7 0 4 1 5 .9 7 5 4 0 7 .5 9 9 2 9 9 .2 0 5 3 5 8 .0 4 0
2930 2940 2940 2940 2940
416 409 299 358
3M Environmental Laboratory
Page 191 of 276
Report E02-0443 Data F i l e S\Etstargt\targetSchai*\du<Jejr,iSD020812B.b\DUDE0136.D
Tenn. River Valley Samples
Page 2
1 PFBS < 2 9 3 )
3M Environmental Laboratory
iyi20iCl/pi 'Jl'.'iii'lj.-;
2 C ..
L o fd i' jgt-:
Paae 192 o<276
Report E02-0443
Data F U * : SSEt*tars*tStar{etSeh*nSdudejr.iSD020812B.bSDUDE0136.D 3 PfOA <413)
Tenn. River Valley Samples
4 POSA <490)
S PFOS <499)
3M Environmental Laboratory
B sci Copv C ia L r / j. / / / i x .
Paae 193 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\Etstarget\target\chem\itchy.i\I021112.b\lTCHY034.D Page 1 Report Date: 19-Nov-2002 14:49
3M Environmental Laboratory-
Data file \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY034.D
Lab Smp Id 0443-WB-l
Inj D a te Operator
Smp Info
12-NOV-2002 13:40 m l a Inst ID: itchy.i E 0 2 -0443-WB-l; Wa te r Blank; M e O H Extract; 21 Oct 02; M L A
Mise Info
Comment
Method Meth Date Cal Date
\\ Et st ar ge t\target\chem\itchy .i\ I0 21112.b\1021112 .m
13-Nov-2002 09:16 itchy.i
Quant Type : ESTD
12-NOV-2002 12:14
Cal File: ITCHY026.D
Als bottle 21
Dii Factor 1.00000
Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
Compounds 1 p r o s (299)
a FFH3 (399) 3 PFOA (413) 4 POSA (499) S PPOS (499)
QUANT SIG MASS
299
299 299 399 413 413 498 499
CONCENTRATIONS
ON-COLUMN PINAL
RT EXP RT DLT RT RESPONSE
(ng/mli)
(ng/mL)
3.421 3.252 4.129 3.840 4.039 4.348 4.867 4.209
3.422 3.422 3.422 3.830 4.020 4.020 4.867 4.199
-0 . 0 0 1 -0.170
0.707
0.0 10
0.019 0.328
0 .0 0 0
0.0 10
37874 7026 7366 2541
13412 10274
1927 78922
0.55035 933.500 933.490 0.13306 744.874 745.050 0.17216 1.09119
0.550 933 933
0.133 745 745
0.172 1.09
3M Environmental Laboratory
Exact Copv 1 ;...
rC M L inla)
.`pi;:
Page 194 of 276
Report E02-0443 Bat* File: SSEtstarget\target\chem\itcha*i\1021112*b\ITCHY034*D
Tenn. River Valley Samples
Page 2
1 PFBS (299)
2 PFHS <399) 3M Environmental Laboratory
Paoe 195 of 276
Report E02-0443
Dat Fil*: SSEt*tare*fcStarEet\oh*nMtoha.l\I021112.bMTCHY034.D
3 PFOA <413)
'
Tenn. River Valley Samples
4 FOSA <498) O PFOS <499>
3M Environmental Laboratory
Pane 196 of ?76
Report E02-0443
Tenn. River Valley Samples
Data File: \ \ E t st ar ge t\ tar ge t\ ch em \i tch y.i\l021112.b\lTCHY035 D Paoe l
Report Date: 19-Nov-2002 14:49
.
'a
3M Environmental Laboratory-
Data file Lab Smp Id
\\Etstarget\target\chem\itchy.i\l021112.b\ITCHY035 D
0 4 4 3 -WB-2
Inj Date
12- NOV-2002 13:51
Operator
mla
Inst ID: itchy.i
Smp Info Mise Info
E 0 2 - 0 4 4 3 - W B - 2 ; Wa te r Blank; M e OH Extract; 21 Oct 02; M L A
Comment
Method
\\ Et st ar ge t\ tar ge t\ ch em \i tch y.i \ 1 0 2 1 1 1 2 .b\I0 2 1 1 1 2 .m
Meth Date 13- NOV-2002 09:IS itchy.i
Quant Type: ESTD
Cal Date
12-NOV-2002 12:14
Cal File: ITCHY026.D
Als bottle 22
Dil Factor 1.00000
Integrator Falcon Target Version: 4.12
Compound Sublist: all.sub
Compound 1 PPBS (299)
2 PPHS (399)
3 PFOA (413)
4 POSA 5 PFOS
(49ft) (499)
QUANT BIG MASS
299 299 299 399 399 413 413 49ft 499
CONCENTRATIONS
ON-COLUMN
RT RXP RT DLT RT RESPONSE
(ng/nlt)
FINAL (ng/mL)
3.411 3.252 4.119 3.S30 3.491 4.029 4.34ft 4.B67 4.219
3.422 3.422 3.422 3.830 3.830 4.020 4.020 4. 867 4.199
-0 . 0 1 1 -0.170
0.697
0.000
-0.339 0.009 0.320
0 .0 0 0
0 .0 2 0
32544 5958 3285 3628 1344
14592 12065
2453 42341
0.39726 933.530 933.607 0.15642 0.10734 0.04324 744.949 0.18434 0.23630
0.397 934 934
0.156 0.107 0.0432
745 0.184 0.236
3M Environmental Laboratory
Exact CityyofCrkk.-.
Page 197 o f 276
Report E02-0443 Data Filai SSEtstarjetStarjetSchemM tchy.1S 1021112.bSITCHY035.D
Tenn. River Valley Samples Paja 2
i PFBS <299)
2 PFHS <399) 3M Environmental Laboratory
faaci Copy a: Orlq:
ia. (i& isi
'
Paoe 193 of27R
Report E02-0443
Sata File: S'^EtsterjetStarjetSchenS itehy.iS 1021112.b S ITCHY035.D 3 PFOA <413)
Tenn. River Valley Samples
Page 3
4 FOSA <498) B PFOS <499)
3M Environmental Laboratory
^ c Copy OfOrigins!
Page 199 of 276
Report E02-0443
Tenn. River Valley Samples
D a ta File: \ \ E t s t a r g e t \ t a r g e t \ c h e m \ i t c h y .i\I021112.b\lTCHY038.D Page 1 Report Date: 19-Nov-2002 14:49
3M Environmental Laboratory
D a ta file \ \ E t s t a r g e t \ t a r g e t \ c h e m \ i t c h y .i\I021112.b\ITCHY038.D
Lab Smp Id 0443-38044-1
Inj Date
12-NOV-2002 14:23
Operator
mla
Inst ID: itchy.i
Smp Info
E 0 2 -0443-38044-1; SL-1; Me O H Extract; 21 Oct 02; ML A
Mise Info
Comment
Method
\\ Et st ar ge t\ t a r g e t \ c h e m \ i t c h y . i \ I 0 2 1 1 1 2 .b\I021112 .m
Meth Date Cal Date
13-NOV-2002 09:16 itchy.i 12-NOV-2002 12:14
Quant Type: ESTD Cal File: ITCHY026.D
Als bottle 25
Dil Factor 1.00000
Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
Com pounds
1 PFBS ( 2 9 9 )
2 PPHS (2 9 9 )
3 PPOA (4 1 2 ) 4 POSA (499) 5 PPOS (4 9 9 )
QUANT S IG HASS
299 299 299 399 399 413 413 498 499
CONCENTRATIONS
O N -C O LU M N
P IN A L
RT RXP RT D L T RT RBSPONS8
(n g /m L )
(n g /m L )
3 .5 1 1 3 .9 7 0 4 .3 0 9 3 .8 4 0 3 .4 3 2 4 .0 4 0 3 .7 0 1 4 .8 8 7 4 .2 1 9
3 .4 2 2 3 .4 2 2 3 .4 2 2 3 .8 3 0 3 .8 3 0 4 .0 2 0 4 .0 2 0 4 .8 6 7 4 .1 9 9
0 .0 8 9 0 .5 4 8 0 .8 8 7 0 .0 1 0 -0 .3 9 8 0 .0 2 0 -0 .3 1 9 0 .0 2 0 0 .0 2 0
363859 2593 4148
122635 18909
295590 8211
1250415 2785277
1 0 .5 9 7 8 9 3 3 .6 2 7 9 3 3 .5 8 2 2 .7 1 9 9 9 0 .4 8 4 9 2 1 6 .1 9 4 9 7 4 5 .1 6 6 2 9 .6 7 1 1 6 7 .6 5 6 2
1 0 .6 934 934
2 .7 2 0 .4 8 5
1 6 .2 74S
2 9 . 7 (H ) 6 7 . 6 (H )
QC Flag Legend M - Compound response manually integrated.
Exact Copy u: Originai
3M Environmental Laboratory
Paae 200 of 276
Report E02-0443
Data File: SSEtstargetStargetScheiMtchy.iM021il2.bMTCHY038.D
Tenn. River Valley Samples
Page 2
1 PFBS <299> 2 PFHS <399)
3M Environmental Laboratory
Pane
r\f
Report E02-0443
Data Filas \SEt*trjetNtrtetSchwSitchy.iM021112.b'sITCHY038.D 3 PFOA <413)
Tenn. River Valley Samples
Pa* 3
4 FOSA <498) 5 PFOS <499)
3M Environmental Laboratory
CC-i'/ nT OnQTisi C i) t- l f u lf r - '
P n n = ? 0 ? nf ?7 F
Report E02-0443
Tenn. River Valley Samples
D a ta File: \ \ E t s t a r g e t \ t a r g e t \ c h e m \ i t c h y .i \ I 0 2 1 H 2 ,b\ITCHY040 .D Page l Report Date: 19-Nov-2002 14:49
3M Environmental Laboratory
Data file : \\Etstarget\target\chem\itchy.i\l021112.b\ITCHY040.D
Lab Smp Id: 0443-38044-2
Inj Date : 12-NOV-2002 14:45
Operator : mla
Inst ID: itchy.i
Smp Info : E02-0443-38044-2; SL-1; M e O H Extract; 21 Oct 02; M L A
Mise Info :
Comment :
Method
: \ \ E t s t a r g e t \ t a r g e t \ c h e m \ i t c h y .i\I021112.b\I021112.m
Meth Date : 13-NOV-2002 09:16 itchy.i
Quant Type: ESTD
Cal Date : 12-NOV-2002 12:14
Cal File: ITCHY026.D
AlS bottle: 26
Dil Factor: 1.00000 Integrator : Falcon
Compound Sublist: all.sub
Target Version: 4.12
Compound 1 PPBS (399)
2 PFHS (39) 3 PFO (413) 4 POSA (49) 5 PPOS (499)
QUANT SXG MASS
399 399 399 399 399 413 413 498 499
CONCENTRATIONS
ON-COLUMN
PINAL
RT BXP RT DLT RT RRSPONSB
(ng/aL)
(ng/aL)
3.433 3.970 4.309 3.840 3.433 4.040 3.711 4.887 4.319
3.423 3.432 3.422 3.630 3.830 4.020 4.030 4.867 4.199
0 .0 10
.S48 0.887
0.0 10
-0.398
0.0 20
-0.309
0.0 20 0 .0 2 0
383608 1970
62861 118901
13878 260003
9S04 1361450 2885124
10.5904 933.645 1.26871 2.63937 0.37675 14.1091 745.093 32.3550 70.2517
10 .6
934 1.27 2.64 0.377 14.1
74S 32.4 70.2(H)
QC Flag Legend M - Compound response manually integrated.
U h l
3M Environmental Laboratory
Pace 203 of 276
Report E02-0443 Data File: S\Etstare*tStarjt\ch*Sitchy.iM021112.b\ITCHY040.D
Tenn. River Valley Samples
Page 2
3M Environmental Laboratory
Braci Copy o Origini;
Page 204 of 276
Report E02-0443
Dt Fi.lt: S\EttT5ttStarttt\eht1Sltcha.iSI021112.bMTCHY040.D 3 PFOfl <413>
Tenn. River Valley Samples
6 PFOS <499>
3M Environmental Laboratory
ctc o-iinUi-,
Page 205 of 276
Report E02-0443
Tenn. River Valley Samples
D a ta File: \ \ E t s t a r g e t \ t a r g e t \ c h e m \ i t c h y .i\l021112.b\ITCHY042.D Page l Report Date: 19-Nov-2002 14:49
3M Environmental Laboratory
D a ta file : \\ Et sta rg et\ t kr ge t\ ch em \i t c h y .i \ I0 2 1 1 1 2 .b\lTCHY042.D
Lab Smp Id: 0443-38044-3
Inj Date : 12-NOV-2002 15:07
Operator : mla
Inst ID: it ch y.i
Smp Info : E 0 2-0443-38044-3; SL-1; M e O H Extract; 21 Oct 02; M L A
Mise Info :
Comment :
Method
: \\Etstarget\target\chem\itchy.i\I021112.b\I021112.m
Meth Date : 13-Nov-2002 09:16 itchy.i
Quant Type: ESTD
Cal Date : 12-NOV-2002 12:14
Cal File: ITCHY026.D
Als bottle: 27
Dil Factor: 1.00000
Integrator: Falcon
Compound Sublist: all.sub
Target Version: 4.12
Compounds 1 PPB3 (299)
2 PPHS (999) 3 PPOA (913) 4 POSA (998 ) 5 PPOS (999)
QUANT SIG MASS
299 299 399 399 413 413 498 499
CONCENTRATIONS
ON-COLUMN
FINAL
RT RXP RT DLT RT RESPONSE
(ng/*L)
(ng/mL)
3.531 4.299 3.840 3 .432 4.040 3.701 4.887 4.219
3.422 3.422 3.830 3.830 4.020 4.020 4.867 4.199
0.109 0.877
0 .0 10
-0.398
0 .0 2 0
-0.319
0.0 20
0.0 20
482034 50026
111724 19590
2S3343 8515
1033771 2109105
13.4894 0.89957 2.48445 0.49957 13.7201 745.149 24.4638 50.3621
13.5 0.900
2.48 0.500
13.7 745
24.5(H) 50.4
QC Flag Legend M - Compound response manually integrated.
fr.act;V/:;;/ (- I Z / j D
3M Environmental Laboratory
Page 206 of 276
Report E02-0443 Data FiltS vAEtst*ret\t*ret\che*\itchyi'\I021112*b\ITCHY043..D
Tenn. River Valley Samples p* 2
i PFBS <299>
3M Environmental Laboratory
, s/h^iu-m
.' '
y-fit
Pape 207 of 276
Report E02-0443
Data Filas S\tst*rjetStarjet\ehen\itcha.1M 021112.bSITCHY042.D 3 PFOA <413)
Ion 413.00
Tenn. River Valley Samples
Paja 3
Hin
4 FOSft <498)
B PFOS <499)
3M Environmental Laboratorv
Pane ?08 of ?7F
Report E02-0443
Tenn. River Valley Samples
Data File: \\Etstarget\target\chem\itchy.i\I021112.b\lTCHY046 D Pace i
Report Date: 19-Nov-2002 14:49
'a
3M Environmental Laboratory
D a t a file : \ \ E t s t a r g e t \ t a r g e t \ c h e m \ i t c h y .i\l021112.b\lTCHY046 D
Lab Smp Id: 0453-38045-1
`
Inj Date : 12-NOV-2002 15:50
Operator : mla
Inst ID: itchy i
Smp Info : E 0 2 -0443-38045-1; SL-3; M e O H Extract; 21 Oct 02- M L A
Mise Info :
'
Comment :
Method
: \ \ E t s t a r g e t \ t a r g e t \ c h e m \ i t c h y .i\l0 2 1 1 1 2 .b\l021ll2.m
Meth Date : 13-Nov-2002 09:16 itchy.i
Quant Type- ESTD
Cal Date : 12-NOV-2002 12:14 AlS bottle: 31
Cal File: ITCHY026 D '
Dil Factor: 1.00000
Integrator: Falcon Target Version: 4.12
Compound Sublist: all.sub
Compound* l PPBS
2 FPHfl (399) 3 PFOA (413)
4 POSA (49S) 5 PPOS (499)
QUANT SXO NASS
399 399 399 399 399 413 413 413 498 498 499 499
CONCENTRATIONS
ON-COLUMN
FINAL
RT 8XP RT DLT RT RESPONSE
<ng/L)
(ng/aL)
3.413 3.9S0 4.309 3.840 3.442 4.040 3.711 4.379 4.887 4.598 4.219 4.568
3.422 3.422 3.422 3.830 3.830 4.020 4.020 4.020 4.867 4.867 4.199 4.199
-0 . 0 1 0 0.528 0.887
0.0 10
-0.388
0.0 20
-0.309 0.359
0 .0 2 0
-0.269
0.0 20
0.369
325254 2272
17131 13341
8750 48048
9113 7941 48310 5183 418454 11802
8.88037 933.636 933.210 0.36520 0.26651 1.92935 745.115 745.181 1.24672 0.24754 9.07817 1354.25
8 .8 8
934 933 0.365 0.266 1.93 745 745 1.25 0.248 9.08 1350
> Origina!
C in e . L k l i L ,
'. ;.j|
1)3 * 9
3M Environmental Laboratory
Page 209 of 276
Report E02-0443 Data Fila: SSEt*tartatStarf*t\ehai\itchy.iSI02112.b\ITCHY046.D
Tenn. River Valley Samples
Pac 2
1 PFBS <299)
3M Environmental Laboratory
e in
OrpinsI
iji lfc -' )
Paae 210 of 276
Report E02-0443
Data File; SSEtstaritStartetSeh*Sitcha.iSI021112.bSITCHY046.D 3 PFOA (413)
Tenn. River Valley Samples
4 FOSA <498) 5 PFOS <499)
Gl);'"
3M Environmental Laboratory
Page 211 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: \ \ E t s t a r g e t \ t a r g e t \ c h e m \ i t c h y .i\I021112.b\lTCHY048.D Page 1 Report Date: 19-NOV-2002 14:49
3M Environmental Laboratory-
Data file : \\Etstarget\target\chem\itchy.i\l021112.b\ITCHY048.D
Lab Smp Id: 0453-38045-2
Inj Date : 12- NOV-2002 16:12
Operator : mla
Inst ID: itchy.i
Smp Info : E 0 2-0443-38045-2; SL-3; M e O H Extract; 21 Oct 02; ML A
Mise Info :
Comment :
Method
: \\Etstarget\target\chem\itchy.i\I021112.b\I021112.m
Meth Date : 13-Nov-2002 09:16 itchy.i
Quant Type: ESTD
Cal Date : 12-NOV-2002 1 2 :1 4
Cal File: I T C H Y 0 2 6 .D
Als bottle: 32
Dii Factor: 1.00000
Integrator: Falcon
Compound Sublist: all.sub
Target Version: 4.12
Compounds 1 PPBS (29)
2 PFHS <39)
3 PFOA M13) 4 POSA U9B) 5 PP03 (*9)
QUANT SIO HASS
299 299 299 399 399 399 413 413 494 498 499 499
CONCENTRATIONS
ON-COLUMN
RT BXP RT DLT RT RBSPONSB
(ng/aL)
PINAL {ng/mLi
3.421 3.940 4.318 3.840 3.441 4.029 4.049 3.710 4.886 4.617 4.229 4.568
3.422 3.422 3.422 3.830 3.830 3.83 0 4.020 4.020 4.867 4.867 4.199 4.199
-0 . 0 0 1 0.538 0.896
0.0 10
-0.389 0.199 0.029
-0.310 0.019
-0.250 0.030 0.369
305101 7189
12829 11469 18109 10665 60231
8754 46172
4067 323943
6825
8.29128 933.495 933.333 0.32496 0.46772 0.30767 2.61856 745.135 1.19716 0.22171 6.84536 1354.37
8.29 933 933
0.325 0.468 0.308
2.62 745
1.2 0
0 .2 2 2
6.84 1350
3M Environmental Laboratory
Page 212 of 276
Report E02-0443
Data Fll*: S\EtstarstStartet\ohan\itcha.iSI021112.b\ITCHV048.B
Tenn. River Valley Samples
Paje 2
2 PFHS <399>
3M Environmental Laboratory
l-'ii'-tU,
Vinim i
J Z i'j
Page 213 of 276
Report E02-0443
Dt Fil; S\EtstarsetStrj*tSeheSitchy.iM02H12,b\ITCHY048,D 3 PFOA <413>
Tenn. River Valley Samples
pe* 3
B PFOS <499
3M Environmental Laboratory
Paae 214 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: \ \ E t s t a r g e t \ t a r g e t \ c h e m \ i t c h y .i\I021li2.b\ITCHYORi D Report Date: 19-Nov-2002 14:49
Page 1
3M Environmental Laboratory
Data file Lab Smp Id
\ \ E t s t a r g e t\ tar ge t\ ch em \i tch y. i\ I0 21 11 2,b\ITCHY051 D
0453-38045-3
'
Inj Date
12-NOV-2002 16:44
Operator Smp Info Mise Info
m ^-a Inst ID: itchy.i E 0 2 - 0 4 4 3 - 3 8 0 4 5 - 3 ; SL-3; M e O H Extract; 21 Oct 02; M L A
Comment
Method
\ \ E t s t a r g e t \ t a r g e t \ c h e m \ i t c h y .i\l021ll2 . b \ l 0 2 1 H 2 .m
Meth Date 13-Nov-2002 09:16 itchy.i
Quant Type: ESTD
Cal Date
12-NOV-2002 12:14
Als bottle 33
~Ca`l Fil'e: ITCHY026.D
Dil Factor 1.00000
Integrator Falcon Target Version.- 4.12
Compound Sublist: all.sub
:>oun<U 1 PPBS (2 J9 )
2 PFHS (39 9 )
3 PFQA (4 1 3 ) 4 POSA (4 9 8 ) 5 PPOS (49 9 )
QUANT S IQ NASS
299 299 299 399 399 399 413 413 413 498 498 499 499
CONCENTRATIONS
ON-COLUMN
FINAL
RT EXP RT DLT RT RESPONSE
(ng/aL )
(n g /aL )
3.4 0 2 3 .950 4.3 0 9 3.7 2 0 3.4 3 1 4.0 3 9 4.0 4 9 3.7 1 1 4.3 8 8 4.8 9 7 4 .S 88 4 .2 2 9 3.9 3 0
3.4 2 2 3.4 2 2 3.4 2 2 3 .8 3 0 3.8 3 0 3 .8 3 0 4.0 2 0 4.0 2 0 4 .0 2 0 4.8 5 7 4.8 6 7 4.1 9 9 4.1 9 9
> 0.020 0.5 2 8 0.8 8 7
-o.iio -0 .3 9 9
0 .2 0 9 0 .0 2 9 -0 .3 0 9 0 .3 6 8 0 .0 3 0 -0 .2 7 9 0.0 3 0 -0 .2 6 9
364686 2069
18856 1212S
2424 11470 54999 12405 12668 65768
4044 420485
4504
1 0 .0 3 5 3 9 3 3 .6 4 2 0 .0 0 4 3 4 0 .3 3 9 0 6 0 .1 3 0 5 5 0 .3 2 4 9 8 2 .3 2 2 4 2 7 4 4 .9 3 0 7 4 4 .9 1 5 1 .6 5 1 5 8 0 .2 2 1 1 7 9 .1 2 6 2 3 1 3 5 4 .4 3
1 0 .0 934
0.0 0 4 3 4 0 .3 3 9 0.1 3 0 0.3 2 5 2 .3 2 745 745 1 .6 5 0.2 2 1 9 .1 3 1350
f-'-vu'{J,
3M Environmental Laboratory
Page 215 of 276
Report E02-0443
Data Fil: SSEtstar{;tStare*tSch*r>i\itchy.iSI021112.b\ITCHY051.D
Tenn. River Valley Samples
Pag 2
1 PFBS <299> 2 PFHS <399> 3M Environmental Laboratory
Pano
r\f 07R
Report E02-0443
Data F U ; \SEtstarttStarstSch*MtehaUM02i.il2.bMTCHY051.D 3 PFOA <413)
Tenn. River Valley Samples
P** 3
4 FOSA <498) S PFOS <499)
"f li/io/ts
3M Environmental Laboratory
Page 217 of 276
Report E02-0443
Tenn. River Valley Samples
Data File: \\Etstarget\target\chem\itchy.i\I021112,b\ITCHY053 D Paqe 1 Report Date: 19-Nov-2002 14:49
3M Environmental Laboratory
Data file \\Etstarget\target\chem\itchy.i\I021112.b\lTCHY053.D
Lab Smp id 04 53 -3 80 45- M S (3)
Inj Date
12-NOV-2002 17:06
Operator
mla
Inst I D : i t c h y .i
Smp Info Misc Info
E 0 2 - 0 4 4 3 - 3 8 0 4 5 - M S (3); SL-3; M e O H Extract; 21 Oct 02; M L A
Comment
Method
\ \ E t st ar ge t\ tar ge t\ ch em \i tch y. i\ I0 21 11 2-b\l0 2 1 1 1 2 .m
Meth Date 13-NOV-2002 09:16 itchy.i
Quant Type: ESTD
Cal Date
12-NOV-2002 12:14
Cal File: ITCHY026.D
Als bottle 34
Dil Factor 1.00000
Integrator Falcon
Compound Sublist: all.sub
Target Version: 4.12
Compounds
1 P7BS <SS)
2 PPHS (399) 3 PPOA Ul3> 4 POSA US) 5 PPOS U9)
QUANT SIO MASS
29 299 299 299 413 413 498 499 499
CONCENTRATIONS
ON-COLUMN
PINAL
RT BXP RT DLT RT RHSPONS8
(ng/mL)
(ng/mL)
3.422 3.940 4.289 3.820 4.020 3.491 4.84? 4.199 3.920
3.422 3.422 3.422 3.830 4.020 4.020 4.84? 4.199 4.199
0.000
0.518 0.857 -0 . 0 1 0
0 .0 0 0
-0.329
0.000
0.000
-0.279
1540798 4713
118794 1495558
C9139C 6714
1092819 1285345
2917
45.9348 933.509 2.88083 37.8097 40.2752 745.250 25.8793 29.9181 1354.46
45.9 934
2 .8 8
37.8 40.3
745 25.9 29.9 1350
3M Environmental Laboratory
Page 218 of 276
Report E02-0443
Dt Fil: SSEfc*tareetStartfcNchSltcha.lS1021112.bMTCHV053.I)
Tenn. River Valley Samples
Pte 2
2 PFHS (399>
3M Environmental Laboratory
' W .. /./bfis
Ir'*-;r 11
V
-4E)
Paoe 219 of 279
Report E02-0443
Data Fila: S\Ettir*t\tarttSchSitchy.iSI021112.bSITCHY053.D 3 PFOft <413)
Tenn. River Valley Samples
Pace 3
4 FOSft < 4 9 8 )
3M Environmental Laboratory
Car Ui Cp x '
Bst*)
Page 220 of 276
Report E02-0443
Tenn. RiverValley Samples
D a t a File: \ \ E t s t a r g e t \ t a r g e t \ c h e m \ i t c h y .i \ I 0 2 1 H 2 , b \ I T C H Y 0 5 5 . D Page 1 Report Date: 19-Nov-2002 14:50
3M Environmental Laboratory-
D a t a file \\ Et st ar ge t\ tar ge t\ ch em \i t c h y .i\I021112.b\lTCHY055.D
Lab Smp Id 0463-38046-1
Inj Date
12-NOV-2002 17:28
Operator
mla
Inst ID: itchy.i
Smp Info
E 0 2 -0443-38046-1; SL-2; M e O H Extract; 21 Oct 02; ML A
Mise Info
Comment
Method
\ \ E t s t a r ge t\ tar ge t\ ch em \i tch y.i\I021112.b\I021112 .m
Meth Date 13-NOV-2002 09:16 itchy.i
Quant Type: ESTD
Cal Date
12-NOV-2002 12:14
Cal File: ITCHY026.D
Als bottle 41
Dil Factor 1.00000
Integrator Falcon
Comp ou nd Sublist : a l l .sub
Target Version: 4.12
Compounds 1 PFB3 (299)
2 PFKS (39) 3 PPOA (413) 4 POSA (499) S PFOS (493)
QUANT SI6 HASS
299 299 299 399 399 413 413 49B 499 499
CONCENTRATIONS
ON-COLUMN
FINAL
RT BXP RT DLT RT RBSPONSB
(ng/*L>
(ng/mL)
3.531 4.099 4.319 3.840 3.422 4.040 3.711 4.887 4.219 3.930
3.422 3.422 3.422 3.830 3.830 4.020 4.020 4.887 4.199 4.199
0.109 0.567 0.897
0.0 10
-0.408
0 .0 2 0
-0.309
0 .0 2 0 0 .0 2 0
-0.269
327380 SOOC 8043
17353 14192 53375
7259 120467 417236
11862
8.94256 933.558 933.471 0.45146 0.38350 2.23055 745.219 2.92155 9.04935 1354.25
8.94 934 933
0.4SI 0.383
2.23 745
2.92 9.05 1350
'"Cu tt
3M Environmental Laboratory
Pano
o f 07R
Report E02-0443 Sata F ile : S\E t& trtet\tr (jeVscheinSitchy. i \ I 021112.b \ITCHY0S5. D
Tenn. River Valley Samples
Paje 2
1 PFBS <2991
3M Environmental Laboratory
P a n o 9 0 0 a f n-7f:
Report E02-0443
Dafca Fil: S\Etst4rgetStarctSohnSitchy.iM021112.bSlTCHY05S.l) 3 PFOA <413)
Tenn. River Valley Samples Pe 3
4 FOSfi <498>
3M Environmental Laboratory
'aCl
Page 223 of 276
Report E02-0443
Tenn. River Valley Samples
D a t a File: \ \ E t s t a r g e t \ t a r g e t \ c h e m \ i t c h y .i\l021112.b\ITCHY057.D Page 1 Report Date: 19-Nov-2002 14:50
3M Environmental Laboratory
Data file \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY057.D
Lab Smp Id 0463-38046-2
Inj Date
12-NOV-2002 17:50
Operator
mla
Inst ID: itchy.i
Smp Info
E 0 2 -0443-38046-2; SL-2; M e O H Extract; 21 Oct 02; M L A
Mise Info
Comment
Method Meth Date Cal Date
\\Etstarget\target\chem\itchy.i\I0211l2,b\I02lll2.m
13-NOV-2002 09:16 itchy.i
Quant Type: ESTD
12-NOV-2002 12:14
Cal File: ITCHY026.D
Al s bottle 42
Dil Factor 1.00000
Integrator Falcon
C o mp ou nd Sublist : a l l .sub
Target Version: 4.12
Coapounda a FPBS 119)
2 FPHS (399) 3 PPOA (413)
4 POSA (498) S FPOS (499)
QUANT SIG NASS
399 299 299 299 399 399 413 413 413 498 499 499
CONCENTRATIONS
ON-COLOMN
FINAL
RT BXP RT DLT RT RESPONSE
(ng/ttL)
(ng/mL)
3.511 3.940 4.089 4.319 3.840 3.432 4.040 3.711 4.349 4.887 4.229 3.930
3.422 3.422 3.422 3.422 3.830 3.830 4.020 4.020 4.020 4.847 4.199 4.199
0.089
0.538
0.647
0.897
0.010
0.398
0.020
0.309
0.349
0.020
0.030
0.269
232749 2658 5270 7437
18434 10544 3 5197
7629 12091 103503 393650 12978
6.18256 933.625 933.550 933.488 0.47471 0.30507 1.20373 745.199 744.948 2.52745 8.49146 1354.23
6.18 934 934 933
0.475 0.305
1.20
745 745 2.S3 (N) 8.49 1350
QC Flag Legend M - Compound response manually integrated.
r.-.T
3M Environmental Laboratory
Page 224 of 276
Report E02-0443
Data Filet WEtstargetStarcetScheuSitchy,i M 021112.b\ITCHY057.D
Tenn. River Valley Samples
Pae 2
1 PFBS <299> 2 PFHS <399>
3M Environmental Laboratory
Page 225 of 276
Report E02-0443
Data File; SSEt*tartet\tar*etSchew\itoha.iSI021112.b\ITCHY057.D
3 PFOA <413)
Tenn. River Valley Samples
Page 3
4 FOSA <498)
8 PFOS <499)
3M Environmental Laboratory
D 3/4 O O ff A *V7C
Report E02-0443
Term. River Valley Samples
Data File: \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY059.D Page 1 Report Date: 19-Nov-2002 14:50
3M Environmental Laboratory
Data file \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY059.D
Lab Smp Id 0463-38046-3
Inj Date
12- NOV-2002 18:12
Operator
mla
Inst ID: itchy.i
Smp Info
E 0 2 -0443-38046-3; SL-2; M e O H Extract; 21 Oct 02; MLA
Mise Info
Comment
Method
\\Etstarget\target\chem\itchy.i\I021112.b\I021112.m
Meth Date Cal Date
13- Nov-2002 09:16 itchy.i
Quant Type: ESTD
12-NOV-2002 12:14
Cal- Fi-le: ITCHY026.D
Als bottle 43
4t
Dii Factor 1.00000 Integrator Falcon
Target Version: 4.12
Co m p o u n d Sublist : a l l .sub
Compounds 1 PFBS (39)
2 pros (399) 3 PFOA (413)
4 POSA (491) 5 PROS (499)
sI
QUANT SIG MASS
299 299 299 399 399 413 413 413 49 499 499
CONCENTRATIONS
ON-COLUKN PINAL
RT BXP RT DLT RT RESPONSE
(ng/mL)
(ng/mL)
3.S41 4.090 4.319 3.850 3.432 4.040 3.711 4.369 4.087 4.229 3.930
3.422 3.422 3.422 3.830 3.830 4.020 4.020 4.020 4.867 4.199 4.199
0.119 0.668 0.897 0.020 -0.398 0.020 -0.309 0.349 0.020 0.030 -0.269
420079 6904
11582 25494 17014 40917
8SB0 11804 133252 478587 14760
11.6624 933.503 933.369 0.62654 0.44417 1.52653 745.145 744.964 3.21870 10.5027 1354.19
11.7 934 933
0.626 0.444
1.53 745 745
3.22 10.5 1350
Ritaci; Ctjyv
.
m L . } ife l L '
3M Environmental Laboratorv
Pace 227 of 276
Report E02-0443
juta Fil: N\Etjtarget\tirset\ch*i\itchy.i\l021112.b\lTCHYO9.D
Tenn. River Valley Samples
Pace 2
1 PFBS <299) 2 PFHS <399) 3M Environmental Laboratory
CnS a//*/67--
o 'io *.t
Report E02-0443
Tenn. River Valley Samples
Data Filai \\Et*taret\tartet\chet>Mtchy.l\I021112.b\lTCHV059,D 3 PfOA <4131
Paje 3
6 PFOS <4991
3M Environmental Laboratory
'''i
rO.i--imn.y
Page 229 of 276
Report E02-0443
Tenn. River Valley Samples
Attachment D: Sample Prep Sheets, Test Substance, and Test System Information
3M Environmental Laboratory
Page 230 of 276
Report E02-0443
Tenn. River Valley Samples
Csntrifuga ID:. T z .
RCF/PRM Readout: 3 COO Minute.
-- Temp *C 1
Col8 TIDfl^.'&Ann [g / |Y i t i U M . Col7 Spiking Standard ID* (?3p<3-3 Approximate Cone. I f ^ Amount added 1 0 0 * L
T/D/l M-OC.Aen
< 0 / t t /(ft- (1 ^
Co\ $ T A J fi ^ Ji/irvi
3M Environmental Laboratory
C/nC w
3M Environmental Laboratorv
c o i n T7D/I
I p h 'i I D V LW \C -
Col 12 TfD/l If.g.V
(a l l X I h i ( A vC
Water ID H ilt. -ElIC iT >1S
Col 13 TIDfl IdWriiV. Li I k'f
<1Col 14 T/DIKuAT/W.
I i Q l ("!~ X C * ^ L
MeOH ID: TM-A * ^ 5 3 C)_____\_f`O_t_I _0_)t,' *i*?L, ipf/.P-artwi1,)
f i t l n <vfre %,k* fuf
n^r l^
( ) J c n 'lllj r " `"fh > ( ^ V "( : . r t r ^ t r j v r M S^ Y * ( v * ~ t
DP,,,S.,.'0'6a 5xv'w H.7i,n,si-,nhf-o^(*i*y/fn * ')s ' 1 0
Pane 231 of 276
Report E02-0443
Tenn. River Valley Samples
U b Request:
- ( D H '/ >
I t j tu iiix-, di
Tennessee River Valley Samples
Sample Location 1, Catfish
9 J
1
;
1
SL-1, C-1-1 SL-1, C-1-2 SL-1, C-1-3 SL-1.C-2-1 SL-1. C-2-2
SL-1, C-2-3
i m I
1
2 2*
s
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--
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--
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& C DR C F /P R M Readout:.
d l_Temp C.
c o m T/pq IQ y ^ rx Li / ('S s a c r r C Col T/Dq\.> W D p,w L> / i r / g l
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water ID i M U i -Q l T ( Y V^U\
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MeOH ID: TN-A.
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3M Environmental Laboratory
Page 232 of 276
Report E02-0443
Tenn. River Valley Samples
Lab Request:
Tennessee River Valley Samples
Sample Location 2- Large Mouth & Location 3-Small Mouth
0*
g aa 0E
1a. 0E
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SL-2, LM-3-1 J'CLc-llo 7
SL-2. LM-3-7J SL-2, LM-3-/J --
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Centrifuge ID: I f l Z . ______________
coi 5 Tmn 7 3 3 > * ~ t o t if C n U c /v \( Centrifuge ID: | C i ^ ___________
R C F /^R M R eadout:
M in u te s | Q __________ T e m p * C 3 t f t /
com T/D/t j's'SfW'i L>/ IK,k\XrhrC
RCF/PRM Readout:
Minutes O?.________ Temp c n
c o is T/D/i 9 ,'3 lW> L > i I Y > ~ y a * (
Col 7 Spiking Standard ID* 0 3 3 - 2 - ~71
Approximate Cone. Vfyv^ Amount added! cm3 lA-L-
T/D/l U .<tW > L / l i r / f) L -f Ik T
@ G *-iC L / n / o i
C I &: T w f l - W i ( t / t X io j- c*ry<-
* 3M Environm ental Laboratory
Col 12 T/D/l
______ L j M -- I L # \ A
Water ID H < \V > - & T f T ^ lv x S>
Col T/D/l
fc / I e! I mi.) r .-1/ A) tA
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Page 3
i/o.7--- *
3M Environmental Laboratory
Paae 233 of 276
Report E02-0443
Tenn. River Valley Samples
Tennessee River Valley Samples
Lab F
1 *
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9a
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--
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W a te r ID
\ \ \ - Q -T C ( , ^ U -S
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ip tiii-n-au
coi io T/D/i 11iSjvrx y n f; <n i rLw(_
C o l T/Q /i j ' O ^ Y I I d / f l i C k i T Q L d /, ,in o ( j
Cantrjfugo IP: \ f \ * Z -- ___________
co ts tom
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? O P S )___ \t7RCF/PRM R eadout
M in m a a
Tamp *C
^ R C ^ RM Raadout:* ^ C C O Minutes \ C
Tnrrm c_t2d~*
C o in T /D /lf . l ^ P v W t i I K i ^ C m C
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Col 7 Spiking Standard 10 * Q p Q ^ 3 - 7 7
ApproximateConc.J^J_vrt_Amountadded ICO Lit--
Col 13 T/D/l y . l t - | 9 / X , I I f i y? U
Col 14 T/D/l
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Page 4 of 6
W v -?<.CrT t ~
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3M Environmental Laboratory
Pano ??d of ?7fi
Report E02-0443 Lab Request a-
Tenn. River Valley Samples
Tennessee River Valley Samples
Sample Location 3, Large Mouth
i f , A c CorTft J / t i - /" M - U P*< 0<
W v " ^ J */?V
Col 2 t i u i
I p / | 7 1 0 L C U C
Balance ID O D
___ Tube type/sizej)k
coi 3von IP.HDpr^ (t til /
Water ID M l 111
CCT f r l u S
C o l 4 T/D/i T puH m i i i n f I 0 3 _ ^ p M d /s e ttin o f a
Coi s t/d/i
( a 1 1 It i 2 n TM c
Cantrtuga ID:. ' T c , ^
RCF/PRM Readout:, 3 c l x j _Minute*_
Tenui *C / * ?
C o l T / D / I % - V t . f lj . j S '/ C o l 7 S p ikin g S tandard ID # Aooroxim ate Cone. L ^ 0 ,*v* Am ount adrim t I O O ^ l L
T/D/I
lit / l ! i ../ A X l > L _
fa/TTvm-^S' Q 3 D v b/i'i/cn-
3M Environment laboratory
C o l 9 S haker ID O a s i ,
Equil Start T/O/l i l . J / i n ^ ( , H \ ! f t
EquilStop T/D /ll t < b iV v ( l /
1 1C o l 10 T/D/I M S f v n Ij i I K c X c r v iC .
Centrifuge ID: j ( \ ~ 2 - ____________ ^ R C ^/PRM Readout. ^ X \P | Minutee
P 3_Temp*C.
C o l l i T/D/I i : ^ n u / II? / 0 9 - C lv iC
Col 1 2 T/D /I/ ? / $
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C o l 13 T/D/1 i 5 $ 0
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Peg Sot 6
3M Environmental Laboratory
Page 235 of 276
Report E02-0443
Tenn. River Valley Samples
Tennessee River Valley Samples
Lab Request:
.
Sample Location 3, Catfish
9 !
1
SL-3,C-1-1 SL-3,C-1-2
S01m i1
2
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4
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11 12 13
14
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SL-3,C-1-3 --
SL-3.C-2-1
SL-3,C-2-2
SL-3.C-2-3 --
SL-3,C-2-MS --
\d
SL-3,C-3-1 /.m /f r \
SL-3,C-3-1 SL-3.C-3-1 SL-3. C-4 SL-3.C-4 SL-3,C-4 SL-3,C-4-MS SL-3.C-5-1 SL-3,C-5-2
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fC ol 3 T/D /l / 7 7 p n / [1> ( H -- C t V - * -
Water ID Mili'.-e. TftCHrlS
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Centrifuge ID:. T c i - z -
c o m T /p /iiJ 'C y w
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T e n *C
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Approximate Cono.. I f f i h C L _Amount added. K % i l
Col 14 TIDII ( D ? C ) i & l X '. I W L A fM
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3M Environmental laboratory
MeOH ID: T N -A _ Q S 0 J v o l O w
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Page 6 of 6 5c,,/y "./fs ,, vy /M W y.
- l i P c t iee n
l-M -n o **-
3M Environmental Laboratorv
Paoe 236 of 276
Tenn. River Valley Samples
3M Environmental Laboratori
Date Started: Study Number:
15-O ct-02
E02-0443
Soil Extraction Worksheet
Type of Column Used: Water c-18 trlfunct, Sep-Ptk, Ig, ce
Cap and M ix V n i Precondition Extraction C o lu m n Cap and M l* V > u ^
c
i X
D .I
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12
02*0443-38044-1 T. R. V. Sediment
02*0443*38044-2 T. R. V. Sediment
02-0443-38044-3 T. R. V. Sediment
E02-0443-38044-3M. T. R. V. Sediment MS
E02-0443-38045-1 T. R. V. Sediment
02-0443-36048*2 T. R. V. Sediment
E02-0443*38045-3 T. R. V. Sediment
E02-0443-38045-3M: T. R. V. Sediment MS
E02*O443*38046*1 T. R. V. Sediment
E02-0443-38046-2 T. R. V. Sediment
02-0443*38046*3 T. R. V. Sediment
E02-0443-36046-3M! T. R. V. Sediment MS
E02-0443-WB-1
Water Blank, no aed.
E02-0443-WB-2
Water Blank, no sed.
E02-O443-LCS-1
Lab Control Spike
E02-0443-LCS-2 Lab Control Spike
02-0443-38044-4 T. R. V. Sediment
E02-0443-38045-4-. T. R. V. Sediment
E02-0443-3804#Mt: T. R. V. Sediment MS
E02-0443-WB-3
Water Blank, no sed.
E02-0443-LCS-3 Lab Control Spike
2-0443-38044-5 T. R. V. Sediment
E02-0443-38045-5 T. R. V. Sediment
E02-0443-38046-5 T. R. V. Sediment
E02-0443-38046-5M: T. R. V. Sediment MS
E02-0443-WB-4
Water Blank, no sed.
E02-0443-LCS-4 Lab Control Spike
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1
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H 1 17
StrataX, 8B-S100-FCH. lOOOmgmL StrataX, 8B-S100-FCH. 1000m/6mL / - 7 ) StrataX. 8B-S100-FCH, lOOOmgmL L S StrataX. 8B-S100-FCH. 1000mg/6mL StrataX. 8B-S100-FCH. 1000mg/6mL r J . Strata C1B-E, 8B-S004-JCH-S. 1000ma/6mL Strata C18-E, 8B-S004-JCH-S. 1000mg/6mL Strata C18-E. 8B-S004-JCH-S. 1000mg/6mL Strata C18-E. 8B-S004-JCH-S. 1000mg/6mL Strata C16-E, 8B-S004-JCH-S. 1000mg/6mL Strata CUPE. 8B-S004-JCH-S. 1000mg/6mL
Col 3: Baiane ID >7 V T/D/l I d O ~ 3 ( '/ / ? , O i T t i J / r l 1+
C o l 4: Standard ID
.
Standard Concentration: !
Amount Standard Added: ' ' 1
T/O/l I Y C / 3 / /.- T L -1 /
fffji- f >* iv i t s
<-
C ol 6: Standard ID: d i O ' W - r t T . 0 Volume Added: 1 5 e t, -</ i u l 1* 1} t? . f f r l / y T/D/l Il'.O C / l l r ^ r ! / 'J / W > t
Col S: T/D/l_ S r l J
T r j / , ^ kft
Col 7: Centrifuge ID: Speed: ,'j C ' j -- / ! Duration:
T/D/l l i n o / . i t n ,
? Afcpm
T / -,) / ' L l
C o l8 : 1/Ofl / . ^ V ? / .1 / r t / r < V
5C ol 9: T/04 / , W / J / f?. ? Col 10: MsOH ID: TA/'-A- Q W
Volume added: J r t a m A
T/D/i <?g<5/ z r S n x i / r T W
` ,1 ^ -* * * rj.
Col 11: T/D/l OE l O f A O c f i .
C ol 12: Centrifuge ID:
Speed: ($09 (P g
Duration: O m * n
T/D/l
are ,/ 3 3 r v / -
__________ rft$?rpm
V %-
Col 15:D iuterlD :_______
Volume of sample added:. Volume o f Diluent Added:, Oiluent ID
Final Dilution Factor_____ T/D/l__________________
} <*><: T/P/l IQ G < z / 1 l1 c* T W I / M l A -
Col 16:Jnternal Standard ID_
Internal standard Cone._____
"
Col 14: T/D/l.
l i Q / i l Q -TQU/bu Amount Added: _______
Volume of sample:_________
IS Concentration__________
T/D/l_______
Samole Extract Storaae
/?"VSamDles stored in refrioerator/fieezer ID
at S.
dearma C una analviia
N * - : `/A,W - r -J>' tV ' i r - ^ n . / t c . g j
_______________<,?.;&
T/D/i 15 35 / oUO t'jh f)]/ s u a -
^ " / 77
mW
B ' ic
Initial __ Data_
i i Simjt \ <i< r i j / f f i.j/i-r.' i
/ V , ' ' r f o ' i.,
*--- nr-rcr".^'ic *( 1 ",e(T t.I
. . T ' o n - / / 7 J f - 7 7 / 5 3 , 1 7 ' j . -
s . :s * > * * ' V i J / V j . .
rij /r
^ . , ,, ^ 4 7 i *> Q /f.4 i -j/A / f ;
. 'r
J
'<
' Lot#: S300-18, Production Lot: P300080902 StrataX, 8B-S001-JCH-S: C18-E Sorbent, Phenomena*
Lot#: S201-13. Production lo t: P201061202 Peg* 1 of 2
ille s i
ZJ ToI3
3.
m oM <b
CJ
Report E02-0443
3M Environmental Laboratory
Date Started: 15-Oct-Q2 Study Number E02-0443 Method Used:________________
Soil Extraction Worksheet Study Title: Tenn. River Valley Sediments.
N o te s :___________ Removed Bottles 2 of 4 tor each location from the refrigerator. Placed them on a shaker 1 ambient temperature at 200 rpm. Caps were taped before placed on shaker. - *7 1 / - / % Lf
---- A d J f V flS tta f e y y
f< td C f H & t v h t Ar/c)et) ..& ( ( 3 a ^
,,riJ T a e a c 4
fu irr. strJrjl,)
JS 6 1 . 0 6 Ir/
T'a p a l A r + * f .
3 Z u b e r Z o r J tZ jA __ {occ/Z/o^ ___________________________________
-- C a lm S /f' Q_/00 ftCFt Z a r
u / ^ T ^ . - U O O -0 J . / 0?)o--> H o M U
----- - m t r * l o f a i - f a r e ack /o ro '/tn . V s v t.r * /
-----Cir>7n'ftp`'() (?.6-000 RCF' /o r
UC/*,
3<?p / V - O , 3 KP i i ~Z T 9. So 3 X n V i - 9 0 . 0 . - u n Z /rJ /fi) T f f t j f = 3C f o r a / / re*?t,u^)________________
----- Canti
Zittii/) / fo 5f,pPraZ> j l a h l / f r ) Stm i . C-f><T', Zvbt. ~~-y<* 7 # - 16 iSZZZ-i
---- />/'
Cifs. lit r/lOti)
J a r >J ,,'fc t(- Zr, -/?- V t,,s i/oy** /, , / 7 c'( f t;jL & ua
0 T lf (L ) .*110. /K O;/ U__________________________ __________________________________________________
----R - Y >7 / l ' h Z !d /> >& O S / S ,
jT o
J* R 7 -
< F h J lfU _______________
T h e W p u j k r * r ) r t . j T s a m p /t ?i c-'/ ''>, t ^ / J h - e i ~n, 7 / / n * / f i t e \ w//p p , i T ~ //* /?- V Y i: .' ____________
._y__Xvfe li'p't t )
___ The Vsitebf r) Oi>f'
..y-* T r j --t '
> ' A T*>* *t/*r> p-.'t/>,, --
--///ic 1
( 5j .JJ j . `{iL- OZ
j Z i * t e f ery/or* n **) fF co/o>*> - .TA Z-A -
T)eJ~/TkiX_______________
I U - > n C ij( e
t * / - teocr-O - 7 ^ g S l O r t i cro~, -A e say J \as&s 5P U `PJ CJ&A /O -/3 )
------------ Cf/ul----- {lJe.tf'eZ r-- The*__ lL__W-a i__g J J e
L /l'./h -Q Tcfi/tti
. X I - -fhr S*?*- _
-------- Z-C is " > P c < ? / w n f -- ^ r r c T iir n ta r t ) __ 7S> co^rp^Tk^Z* -fh * / u Z/* C & x? p T ~Z o s i-Xe 57>*7S? C~! I Sa*/* ~)
T i t -- Colun* 1-- Uy-v.ee. ^ H \*n -e.(u frr) L ,/ u L o / S le O H C T A /- J ' Q 6 U \ - S i Uh- 5 3 'J'/toJL
r \ , Th e t c CjO/Crtn-- 7^2v_c ^AL Ife siu /zf^ J -S 1 M -- xTTk__________________ __________
\ j / vter ^ZSjp.--U. i i ' p-tn (L--2 L2
j? & , r yrrot ~f~
g r / r - T ^ r Z i t k 'f- //*t p ,
TZf, ,7 (^.V A'~> /) -/b y/e pou;k/t /fi g/ y?,. 6'V //7y^^7^'r. c,,,,
~!t\r
'jZ /o y / s ( h ' Z f r 1*7* ~- & v '-s
1
____ ________________________
t
"Exact Cu^jy ufOiiginal
ZEUGM I Initial Date
Tenn. River Valley Samples
Page 238 of 276
p0* ? of 2
Report E02-0443
Tenn. River Valley Samples
Lab Request:
_______ III),<&
56
a *
s E h
iM
i V)
0 2a
at
5I
If
1 23
b L - i ' C A - 0 / 7. f ry?
-yiA----------------
* ii. r e i ----------------
.'/ (A
Tennessee River Valley Samples
Extracted Curve Information
_____ _____
j
i c
E
5
?
5 e
a 3
S? . gu
I 3 / is S il
? ?
1 {S of i tl 5
5S 1a
s1
H 1*
I;-
s 2a ?
5 e
M U
li
Is
nIo It o
3
i
an a
J L
O !1
1? l ||l
48
8
1 9 10 11
S Jt / t / \S
2
11
s1
"0S
e
1c
12 iA
S a
i
li E 0c 9 <0 TS 3 I _ 2 5
13 t-'
5 1 a. il s !!
14
t/
s
c E
15
O i r J \jfjl / 0
\p -P tk / h i A c
L D L - )) \
U /l.D tH H Lt 0 ~ i
y
t/ /
i / i/
l/ '
^ Is .H o . -/V H
V
*
\( 3 > X:
1
\
\
Cot2 T/D/I ( D H J 0
c l) f d j i ! t a A H
C ol 9 S haker ID ./^ M l i n i - ii4 W
Batanee ID 9 0 0 __________Tube tvee/size
Col 3 T/Dfl K T O .0
I l7 . in i 0 i M h
Water ID /!//'> U T0( PU-, Col4 T/Dfl f l y j 5 ;)/ a . . , I U>1
if
Speed/ettingX2_
qil S ta rt T /D /l f i 1 0
i h l iM S tW .
qtiil Slop T/D/l
J l /7 W /0 t ^ ^/
Colio T/D/l. h ' W 3 1 1 X - / m / / 7-
Centrifuga 10:._ & ______________
c o l 5 T /D fl I O O P 3 / 1 3 - / #<?
(fjC > P R M R e a d o u t:^ 0 8 0 M inute
K)
T e n C 3 )
Centrifuga ID:
I / VT ^ ~ ^
RCF/RM^Readout:f i 7 ' T Minutes i . * 0 \ i Uv_'
Col 6 T/Dfl //flO -)/ ) X W ^ / *
Temp ` C j J ' u ' / l ' C K i )
C o l 11 T /D fl / 5 V 3 7 / / X - / } _ / ! * 4
C o l 12 T/D/l V a tfllrV i
3/ /X 1*/
Water ID . M J h - Q TOO P h i
C o l 7 S p lk ln o S ta n d a rd ID * g J 0 ) 7 ~ O 7 f r f ? > O i J t l / J
A p p ro xim a te Cone. V i * ' P**1* A m ount added____________
1; /''- ^5 f 0 > Y " OSS>
T/D/l ! k'O
31 7 n t g - 1' 11
d /
o' 7 / 0 / 7 / l i L _
4 i,u jo . tv.4
3M Emironmantal laboratory
2i L / / i!
_H T~
H H 6 ^ > -- ..
COM3 T/D/l H > > 9 Parfit it &) Cot 14 T/D/l SC> 3 / J -1 / V
MeOH ID: TN-A / ) A O / ^ V > l I}><> J " ^ jttiCtn
P a g a te li
3M Environmental Laboratory
Page 239 of 276
Report E02-0443
Tenn. River Valley Samples
Prep Date: Analysts initials:
Non GLP SPE Columns Extraction Worksheet
6/20/2002 OK
Method Revision: Study Number:
Q
no
ETS 8 154 .0 -
E02-0443
i . - J . u to c t'i
Volume ot
Sample Number sample
or description
filtered
water blank E02-0443-38025
40 ml 40 ml
E02-0443-38026 E02-0443-38027 E02-0443-38028 E02-0443-38029 E02-0443-38030 E02-0443-38032 E02-0443-38033 E02-0443-38034 E 0 2 -0 4 4 3 -3 8 0 3 5 E02-0443-38036 E 0 2 -0 4 4 3 -3 8 0 3 7 E02-0443-38038 E02-0443-38039 E02-0443-38040 E02-0443-38041 E02-0443-38042 E 0 2 -0 4 4 3 -3 8 0 4 3 E 0 2 -0 4 4 3 -3 8 0 4 7
40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml
Type of column
used
1g, 6ml, C18 lot 2057B2
1g, 6ml, C18 lot 2057B2
1g, 6ml, C1B lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 2057B2
1g. 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 20S7B2 1g. 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, CIS lot 20S7B2 1g, 6ml, C18 lot 20S7B2 1g, 6ml, C18 lot 20S7B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml. C18 lot 2057B2 1g, 6ml, C16 lot 2057B2
Amount and spike mix used
NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA
Elution solvent and
volume
MeOHTN-A-6116 2ml
MeOHTN-A-6116 2ml
MeOHTN-A-6116 2ml
MeOHTN-A-6116 2ml
MeOH TN-A-6116 2ml
MeOHTN-A-6116 2ml
MeOH TN-A- 6116 2ml
MeOHTN-A-6116 2ml
MeOH TN-A-6116 2ml
MeOH TN-A- 6116 2ml
MeOH TN-A-6116 2ml
MeOHTN-A-6116 2ml
MeOH TN-A- 6116 2ml
MeOHTN-A-6116 2m!
MeOH TN-A-6116 2ml
MeOHTN-A-6116 2ml
MeOH TN-A- 6116 2ml
MeOHTN-A-6116 2ml
MeOH TN-A-6116
2ml MeOH TN-A- 6116
2ml
Comments
>( *V/- 0 . J
Extraction Steps (initial when/if done):
C * ii condition column with MeOH;
wash with milliq; O t 4^ filter sample;
o K_ vacuum dry the column; c K elute column with solvent; _ o K tra n s fe r extract into an autovial
Additional comments:
^XXu_i i'r^
.
/Utr? ' J2.o .u^f
,
.
C~ff O'f mE T
if* ^ Lrt> 0t,/y
6 ^ ' S* ^
ExactCopv -
Utiai
3M Environmental Laboratory
Pano TdO nf 07R
Report E02-0443
Tenn. River Valley Samples
Non GLP SPE Columns Extraction W orksheet
Prep Date:
7/17/2002
Analysts initials: OK
Volume ot
Sample Number sample
or description
filtered
water blank E02-0443-38026 E02-0443-38027 E02-0443-38028 E02-0443-38030
40 ml 40 ml 40 ml 40 ml 40 ml
Type of column
used
1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 20S7B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 2057B2
V
Method Revision: g f & f r l S t t P ' O C' [ l ' ' n ' t ,
Study Number E02-0443
'
Amount and spike mix used
NA NA
NA NA NA
Elution solvent and
volume
MeOH TN-A-AHetcl 2ml
MeOH TN-A-W-W 2ml
MeOH TN-A- 6M6 2ml
MeOH TN-A-.&H 2ml
MeOH TN-A- 6146. 2ml V/
Comments
^V
X
\u
\
Extraction Steps (initial when/if done):
flK c ondition column with MeOH; < M wash with milliq; ^ f ilter sample;
DK_jvacuum dry the column; /P ^ alute column with solvent; p K . transfer extract into an autovial
Additional comments:
( T X 'S eT)
>t<
Exact Copy c: or.;
Initial ^
- > G > c h c C ~ f ) 'c t l a
*? .
w-tfvg ) l i t r o *
k l r J o 4f o f *
L f 1 w * i o J > / u i * J i o
3M Environmental Laboratory
P p n a - > `1 n * 0 7 G
Tenn. River Valley Samples
r,
Description: Ei/trecf-fJ La Fiih Cufjc.
Date Prepared: ^ I
f f h __________
.
Storage Location: _ _ _ 3 r ~ Expiration Date:
MULTI-LEVEL PREPARATION LOG
Book No. 02 003
Page No.
52
Solvent: A le O H __________
Standard ID #
Description (ppO>
I Component Standards
Expiration
Description /Y/V________ __
ID# Cone ' V k
. Ipf**
Date UhVox
lOOppn, fllce H iX
3?W --
100Fp*__ "A>/oi ------
02 003-52-1 02003-52-2 02 003-52-3 02 003-52-4 02 003-52-5 02 003-52-5 02 003-52-7 02 003-52-8 1
J 3 .S s 1 0 S se> 1 0 0 >se J
Amount of Component Standard Added
Std 1 3ul -- --
Std 2 vL
--
--
Std 3 l& v i --
--
Std 4 ~Z0ul
--
--
Std 5
--
--
Std 6 l-O O u i
--
--
Std 7 .....
--
Std 8
---
Sj L
Final Volume G O
a
a
*
a
__ _FInal Concentration (pp^
I 3 .S S 1 0 >5 So t o o Z S I
Description
[ lOOpn*, :
M l/
---
Standard ID #
Description Component Standards
ID # Cone
- crrti
Expiration Date
bkoi>-oy> --
--"
loo
-- --
uA V o x -- --
oFinal Volume - ( *
Final Concentration
02003-52-0 02003-52-10 02003-52-11 02 003-52-12 02003-52-13 02 003-52-14 02 003-52-15 02 003-52-16
S0 0
7-SO }0><2>0
0
--
--
----
Amount of Component Standard Added
Std 9 l( M -- -----
:> 5 00
Std 10 1 5 v /C
--
--
Std 11 ^ Q>u L
-- --
0* /COO
Std 12 ui
Std 13 -- --
Std 14 --
--
-- --- /. **
3 ~3*
0
Std 15 --
-- --
--
Std 16 ---- .
-- 1 ----- 1 --. J
--1
L ^ c ^ + r v . -Ti*A'(ptrri>,c t it it h -
tact Copyoforig/nai Raviewed
ffi
JDate
x TOC3D
m
oN>
Report E02-0443
3M Environmental Laboratory
Description: Date Prepared:
C a tT ish ( * * * 3t T u *
Storage Location:
,
MULTI-LEVEL PREPARATION LOG
Book No. 02 003
Page No.
54
Solvent: S ^ p D A / ______________
Standard ID # Description
( ffb)
Componesnt Standards
Description
ID #
Cone
Expiration Date
lr r fa b v , Me N OOen* o'.ks M ilfllO H
i 7f f *
'*/>/> 4
-o lOOfin^ V i } / oa
--
Finai Volume (n O Final Concentration L f*>v
02 003-54-1
I
Std 1
/L
----
I
02003-54-2
s
Std 2
SoL
--
--
a .s
02 003-54-3
5
02 003-54-4
)0
02 003-54-5
5
02 003-54-0
So
Amount of Component Standard Added
Std 3
0U
--
Std 4
o)fcl/C --
Std 5
S0uL
--
Std 6
/ M l
--
-- ---- _
*
s to as
-- a
SO
02 003-54-7
too
Std 7
--
L>
-- *
/D
02 003-54-0
aso
Std 8 --
o L
--
3 J f 1
Standard ID #
Description Component Standards
Description
lOO^tn f'h f t If I n A O f/
ID # Cone OQj*I
Expiration Date
02 003-54-9 02 003-54-10 02 003-54-11 02 003-54-12 02 003-S4-13 02 003-54-14 02 003-54-15 02 003-54-16
S00
75o W OO
(2>
--
----
Amount of Component Standard Added
Std 9 Ifo L
Std 10 I9 u L
Std 11 }0 u L
Std 12 O
Std 13
Std 14
Std 15
Std 16
Tenn. River Valley Samples
Page 243 of 276
t3> L c^c
Final Volume i.m L ) Final Concentration\ % l )
TKlIft-LU.S" .(**<_
3
/O o o
py of Original
Initial Data
Reviewed
Signature,
F f u - c , 71--
Ze
Tenn. River Valley Samples 3M Environmental Laboratory
ft I
Description: ~R sL
_________
Date Prepared: T u n c n x _________
Prepared B y : _______________
MULTI-LEVEL PREPARATION LOG
Book No. 02 003 Page No. ___ 50
Storage Location:
______________________ Solvent: M e o H ________________
Expiration Date: i i /
3M Trace # : T N f t - ^ 5 3 o ___________
Standard ID #
02 003-50-1 02 003-50-2 02 003-50-3 02003-50-4 02003-50-5 02 003-50-6 02003-50-7 02 003-50-8
Description I Component Standards
Description
ID # Cone
\p o ~ K H W _________________ r>io3*-~IR
1
IQOfp~-> M>v_____________ QJooS - l i Igft/jQ"
1 -------- -------------- X
_____________
Expiration Date
I I / P 3 / oi-
I-0<ifrj .A E & tc
Std 1 l< W -
Std 2 P 5 > xL
S-Opta Amount of Component Standard Added
Std 3
5 0 j iL
Std 4 lOOjuL
Std 5
qsqm L
Std 6 5ccyU
3 _ IC *W ,
Std 7 u \ *P
asouk
Std 8 --
h /a 3 l o i . -- -- -- -- -- -- lO ^ L . a s > .L
Finai Volume Final Concentration, onV^
IOmC ' 1 0 __a-sr
so
1o a s s o IO O
1 Standard ID # H Description
02 003-50-9 02 003-50-10 02003-50-11 02 003-50-12 02 003-50-13 02 003-50-14 02 003-50-15 02 003-50-16
--- A------ -- SO O *,,\, TSoot ICOOooW
1 Component Standards
Amount of Cc mponent Standard Added
Expiration
H Description
ID #
Cone
Date
Std 9 Std 10 Std 11 St 112 ^ ^ 1 3
Std 14 Std 15 Std 161
1 lpp^-% M i*
0 * 0 3 3 - i 9 -. liV.r~__ \ \ / * V u y . --
--- --
fc
I
llofppp-> M i V_______________ 0 3 OOJ-3S l? P f rr. U / J 3 / c2u S fV 1-
iOO^uL
a,,
--
" / fl
t(o9
Final Volume
lI-n L ,
->
MAA O--reo
Final Concentration , p p to 5 0 O
150
lOGO
O)
Exact Copy of Original
Reviewed
T v /d ? )
Signature,
Date
/1 4
Initial Date
AjOJBJuqe i|tqUuiUOJ|/\U3 VVE
Exact concentration of every point of every analyte
Prep date:
"T u rv-Q_____________
Analyst: C/VA-C__________________ _
Solvent & TN-A #: iM M H , T T ^ A - I j . y g r>____________ Final Volume of each point: ^ t_ _____________________
Target analytes: > F tA S , FCiSft ,
, Pr&S.
___________________________
Standard mix used for preparing the curve:
Curve point number
Amount of mix used
02 003-50-1 02 003-50-2 02 003-50-3
See fifu e rs e
I- 0
5 -S D
S
'V p
fC&IPr V>FCA
IC O
lo o
a.so 3 . S<
5 .O D
Analyte concentration in every point , ^ ^
PF&S* 1.0 0
v' Fos, l-o
3 A [
4 .q l
i
r" i
r\
Book No: 02003 Page No: 50
------- -r
X
*aoo. 0rm1o
Ag
CO
02 003-50-4 02 003-50-5 02 003-50-6
lb . c o
I0 .O i . cA q . q s 5 5 .0 0 a s .io 0 4 M SO 5 ^ 3 .0
q q -i 2 4 .i< \
4 4 .8 a
t i
\ \ \
-- --
02 003-50-7 02 003-50-8
`H ' S JOO tYs c o .^ q ^ . 7 5 q q .7 < i c3.Si'..C 5 5 1 :0 ... <P4|.<\ 0 4 4 4
1
\ \
02 003-50-9
/ `tT S L B L 5 D D . S 0 3 . 0
4 4 %. 1
02 003-50-10 02 003-50-11 02 003-50-12 02 003-50-13
Ak
N/
.n S k C L 1 1 5 3 ,0 .... 7 4 8 . 1 M - O . IM .c s ^ T S
7 ^ 8 .1 q ci7 .q
1t I
----
Tenn. River Valley Samples
02 003-50-14
..
J
02 003-50-15 02 003-50-16
L ._ ._ -
-------------- 1
[__________________
-- rr 1 1
Exact Copy of Original
M P u ig tamal Data
Reviewed by: Signature,
Date
Report E02-0443
Tenn. River Valley Samples
r~
i
SINGLE COMPONENT PREPARATION LOG
Date: * 1 Oc. t
Analyst:
/ v} j , ' i _____________
Book No. 02 D5D Page No. 34
Description: I
` jilk t * / ^ ! \ f in
B i \ f 0>l FFV ?Co A r-PfS
Stock Nrnberg
Weight or Volume Used:
Concentration or
_
Purity:_______
Corrected Weight:
Final Volume:
Storage Location:______ 3 f~h~
Balance ID:
A/
Other Correction Factors:
Solvent and TN-A Number
7v/v 7 W t i r -
( r i U r 7C f U i )
Final Concentration:
Expiration Date: A / t j 0 J
Boct Copy of Origina)
/ l l B lk S Initia) Cato
3M Environmental Laboratory
Page 246 of 276
Report E02-0443
Tenn. River Valley Samples
Description: V i T .k
Date Prepared: (p / Iff i CO--
Prepared By:_ CMC________
Storage Location:_
Expiration Date:
i l / ,3 .3 ) CQ--^
MULTI-COMPONENT PREPARATION LOG Book N o . 02 002 Page No. ___ 33
Solvent: H - f 'O , V4~ 3M Trace #: TN-A- ( n i f i n
J Description
F o 5 p> P F dp-
P rS S ,
1 Standard ID #
02 002-33
I
Component Standard
Cone, or ID# Purity
CCCi - IT
3 n :F
o acot-i^
Expiration Weight or Date Volume
V'/t>/3 T S IjJ L
t/<c,|t>3 5 3 ^ <-
Corrected Weight
Final Concentration
Balance ID
to ft
n r t - J g ^ 73V
I0 . OppyV%
03LC.D -X35T5' a \ w
W Sjjl L
aM bl
if p m
tv
p p **
lo tta i--
0 o o i ~ q 3 3 0 -1
\c > V *-
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vy
i 0 0 ^ p|3vV\
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/>prvA
ti 1 1 ^ '" ^ ...
C ....... - ...........
N
Final Volume
Approximate Concentration of the mix ) p p ,V A
ExactCopyofOriginal
z_ <B
Initiai Data
Reviewed by:--^
Signature,
I / Ju 0 ^
Date
3M Environmental Laboratory
Page 247 of 276
Report E02-0443
Tenn. River Valley Samples
Date:
SINGLE COMPONENT PREPARATION LOG h / \ Z I Q~ ~
Analyst______ r k \ L
Description:
Sfti I6t_ M f X .
Book No. 02 022 Page No. 77
Stock Number
~ ____________
Weight orVolume Used:
aso^L
rX iorf
ce ID:
Concentration or Purity:
K'",,*V ' ) s 9
** ID O p p ro ,
( '| ' / .
,.i l/^
Corrected Weight
Solvent amnd TN-A
v.
NumberJ ^ l L L i d O L l l U A .
Final Volume: Storage Location:
Final Concentration: Lp p m .
Expiration Date: U / A ? I O i^
Exact Copy of Original A lA -
Reviewed by:
Signatura,
Data
3M Environmental Laboratory
Page 248 of 276
Report E02-0443
Tenn. River Valley Samples
A SINGLE COMPONENT PREPARATION LOG
HDate:
$ fp ~ f 0 3
A
Book No. 02 040 Paga No. 80
Analyst:^ / 1 I
Description:i: / % A r & f / c A n J ih / l ' / l h -
Stock Number.
- I t fr,W J
Weight orVolume Used:
Balance ID:
A/A
Concentration or Purity:_
Corrected Weight: _
MA
Other Correction Factors:
A.
SolventatnndaTicNw-Av sS I Number i l h - T O C P / u
Final Volume:
21
Final Concentration:
/%
Storage Location:
T 1* F i r f f t p
Expiration Date: A / * , M
Reviewed by:
3M Environmental Laboratory
Paoe 249 of 276
Report E02-0443
Tenn. River Valley Samples
SINGLE COMPONENT PREPARATION LOG
Date:
| rf> O H __________
CKJAnalyst:_______ ____________
Book No. 02 001 Page No. 17
Description:______ *7T " f t S
Stock Number.
'- ` E
Weight orVolume Used:
Concentration or Purity:
_ to
1$. G Jc
Corrected Weight
Balance ID:________
Other Correction Factors:
fJA
Solvent and TN-A ,,
/,
Number H(?OW
_
3
Final Volume:
eo u d
Storage Location:
Final Concentration; 2> I I `O
Expiration Date:_______ j - I O - O 3>
3M Environmental Laboratory
Pane 250 of 276
Report E02-0443
Tenn. River Valley Samples
SINGLE COMPONENT PREPARATION LOG Date:_____I I O O S _________
Analyst_______ O K * ___________
Book No. 02 001 Page No. 19
Description:__
Stock Number
/ / ? ?WeightorVolume Used:
0?.
",
"O
Concentration or Purity:
iiPOik.
Corrected Weight:
M_
Balance ID:
Other Correction Factors:
.AM
Solventand TN-A Number
1H iO t I f N ' h - Z z s S - ' S
Final Volume:
oI'o AmU
Storage Location:
Final Concentration:
f f --------------
Expiration Date:
lo o 's
3M Environmental Laboratory
Page 251 of 276
Report E02-0443
Tenn. River Valley Samples
0 1Date: 1 r , F f b
SINGLE COMPONENT PREPARATION LOG
Analyst: f l ) / / p _______________
fC KDescription^ ?FOS>
Book No. 02 001 Page No. 84
Stock Numben_
Weight orVolume Used:
n ro V
(p .J p A b j
Concentration or Purity:
Corrected Weight:
Balance ID:
m.
Other Correction Factors:
T M 'A -C & ? Solvent and TN-A
Number:1A i'pfnnr'i -R /'r f - r) 3 L/ l `e?
yi H Zfre*>0i
Final Volume: Storage Location:
Final Concentration:
0 ^ o p>i
Expiration Date: ~ % ]~ e b (2 )
Exact Copyof Original
Initial Oats
Reviewed by ( \ w L l ( L s J t f r U ,
Signature, P
^
f1 i l l L~i. Data
3M Environmental Laboratory
Page 252 of 276
Report E02-0443
Tenn. River Valley Samples
SINGLE COMPONENT PREPARATION LOG Date: ^ K T * b Q Q
Analyst: a \A______
r c - mDescription: PTDA
Book No. 02 001 Page No. 85
Stock Numbor._
-C o ~ }0
Weight or Volume Used:
0 .5750* /
Concentration or Purity:
Corrected Weight:
_______
Balance ID:
m
Other Correction Factors:
Solvent and TN-A
Number f o O U / l A Z - A - k M ?
Final Volume: .2.5 1L
Storage Location:
J
21
T ^ )r-
Final Concentration: Expirallon Date:
Exact Copy of Origina!
/ i M - J&fec. y * * * -
initial Date
Reviewed t
1 1 4 "'
3M Environmental Laboratory
Page 253 of 276
Report E02-0443
Tenn. River Valley Samples
Date:
SINGLE COMPONENT PREPARATION LOG
f lO
Analyst A H A ____________
Book No. 02 022 No. 66
Description: P t - R S / 1 - T Q i t . u r s C c ^ ,, 5 o , n )
StockNumber- T C .R - m e > n - 0 ? l / TCR -iS ? Q l / m > )
Weight orVolume Used:
._
0,5 M 5 a
Concentration or Purity:
^n - jn. 5 o/0/
Corrected Weight
0 -W f,
0
Final Volume: M
lei
Storage Location: lA F /r
a
fl
*
Balance ID:
Other Correction Factors:
m.
Solventand TN-A Number / p O f - / , T A / " f o / J / ^
Final Concentration:
v2 t .
Expiration Date: ^ A ' f i n / 0 3
Reviewed by: t D
ls
3M Environmental Laboratory
Page 254 of 276
Report E02-0443
Tenn. River Valley Samples
SINGLE COMPONENT PREPARATION LOG
Date: J o T u n i C~
Ana|yst:__CRC_______
Description: P C . tvV *-
kv\
Book No. 02 022 Page No. 79
Stock Number
( ) " D M
Weight or Volume Used:
IO ^ia L
Balance ID: W P>
Concentration or Purity:
lQ|0pkvx
Corrected Weight
Other Correction Factors:
Solvent and TN-A Number W \ e o H , TJVjfl ~
D
Final Volume:
1 1 } r W |__
Storage Location:
Final Concentration: Expiration Date: w j a - s l 7L,
Reviewed
S ignatura,
Date
3M Environmental Laboratory
Page 255 of 276
Report E02-0443
Tenn. River Valley Samples
TCR# Substance trade name or reference #: Substance/chemical name:
Lot/batch #: Location of synthesis, Fabrication, or derivation records: Molecular Formula: Condition: Expiration date:
Purity:
3M# Entered by (Initials) LAC Std Location/Storage F19, Frozen Amount of Retain 0.3610 g
TCR-83
anat
TCR Receipt & General Information
TCR Substance #
SE036
Perfluorohexanesulfonate Primary std
Received from:
George Moore
Date Received:
09/03/1999
Amount received (wt. or vol): 154 g, 277.38 g
gross wt
C6F13S03-K+ white powder 10/18/2006 96.6% LAC 01/17/01
NB120067-69 Date Entered 09/03/1999 Initials
Number/size of containers: Shipper: MSDS (y/n)
Records received:
1/150 mL glass container Courier Y (J N
MSDS, NMR Characterization
Request #59085
'
Interim final report from Centre and
Certificate of Analysis. LAC 04/26/01
Checked By
Date
Date Checked by (Initial/Date)
Initials
ate 10/19/1999
Checked by (Initial/Date)
Comments
Standard has been moved to Freezer 19 in room 347 KJD 06/06/00 Sent to Centre Analytical for Certificate of Analysis Analysis on 07/08/00 LAC 07/31/00 Standard was stored at room temperature prior to 06/06/00. LAC 12/19/00 Shipping Codes: 41-2600-9459-8. LAC 06/14/01 Original label - 8/4/99 RWW-11/2/01
Initials
Shipping comments: NOT REGULATED, 3M shipping ID: 1-2700-4647-3. LAC 01/10/02 Attachments
Date
Checked By Date
se036msds.pdf se036nmrreq59085.pd
EOO-1878-COA-SE036-PFHS-R O Archived/Substnce Not Available |
3M Environmental Laboratory
Page 256 of 276
Report E02-0443
Tenn. River Valley Samples
TCR# Substance trade name or reference #: Substance/chemical name:
Lot/batch #: Location of synthesis, Fabrication, or derivation records: Molecular Formula: Condition: Expiration date:
Purity:
3M# Entered by (Initials) LAC Std Location/Storage F19, Frozen Amount of Retain 0.2233g
TCR-29 PFOSA
TCR Receipt & General Information
TCR Substance #
Perfluorooctane sulfonyl amide or Perfluorooctanesulfonamide AC KJO 7/24/00 L-15709
Building 236
Received from:
R. Buckanin
Date Received:
04/20/1999
Amount received (wL orvol): 124.98g
gross w t
C8F17S02NH2
Number/size of containers:
light yellow waxy solid MCH 0 7 /2 2 /9 9 Shipper
10/31/2006
MSDS (y/n)
TBD, KJD 05/05/00
Records received:
NA Date Entered
Checked By
1/100 mLglass container Road Runner Y < >N MSDS, summary page of FID analysis #57915
Date
Initiais
Date Checked by (Initial/Date)
Initials
Date 10/18/1999
Checked by (Initial/Date)
Comments
Initials
Gross weight difference due to removal of parafilm LAC 04/28/99 Standard has been moved to Freezer 19 In room 347 KJD 06/06/00 Standard was stored at room temperature prior to 06/06/00. LAC 12/19/00 The expiration date was assigned based on hydrolysis study EL-1132 and photolysis study W2783 which showed this compound to be stable, LAC 10/31/01 Original label dated 3/18/97 - RWW 10/26/01 Shipping Comments: NOT REGULATED, shipping code
- LB-1000-1570-9, L-15709. LAC 01/08/02
Attachments
Date
Checked By Date
sd029msds.pd sd029fid57915.p
C 'A rchlved/Substance Not Available ;
/
3M Environmental Laboratory
Page 257 of 276
Report E02-0443
Tenn. River Valley Samples
TCR# Substance trade name or reference #: Substance/chemical name:
Lot/batch #: Location of synthesis, fabrication, or derivation records: Molecular Formula: Condition: Expiration date:
Purity:
3M # Entered by (Initials) KJD Std Location/Storage F19, Frozen Amount of Retain 0.2737 g
TCR Receipt & General Information
TCR-123 PFOA (POAA)
TCR Substance #
tcr-So3-033
FC-143 Ammonium Perfluorooctanoate (Primary Std) 332
3M
Received from:
N/A
Date Received:
02/02/2000
Amount received (wt. or vol): 278.20 g gross w t
C7F15COO-NH4+ White powder KJD-2/2/00 10/31/2006 95.0% LAC 01/17/01
N/A Date Entered
Initials
Initials
Number/size of containers: Shipper MSDS (y/n)
Records received:
1/ -200 mL glass bottle Unknown Y ( )N
MSDS Interim final report from Centra and Certificate of Analysis. LAC 04/26/01
Checked By
Date
Date Checked by (Initial/Date)
Date 02/17/2000
Checked by (Initial/Date)
Comments
Initials
Was originally TN-A-2143, KJD 2/21/00 Standard has been moved to Freezer 19 In room 347 KJD 6/8/00
standard was weighed on 9/28/00. Standard was stored frozen at -20C+/-10C until shipment on
10/03/00.LAC 10/03/00 Shipping Codes: 98-0211-0891-9/FC-SOOO-0192-0(<30 g on dry ice) LAC 06/14/01 Standard stored at room temperature prior to 6/6/00 LAC-12/26/00 Label - rocorded-10/98 RWW-11/6/01
Shipping comments: REGULATED-TOXIC Dangerous goods In excepted quantity of Class 6, UN2811. 3M Shipping ID: 98-0211-7394-7, (4 lb. carton) fully
regulated. LAC 01/09/02_______________________
Attachments
Date
Checked By Date
tcr99030-30msds.pdf 'A
E00-1763-COA-99030-30-PFOA-R
Archived/SubstanceNotAvailable I
V.
3M Environmental Laboratory
Page 258 of 276
Report E02-0443
Tenn. River Valley Samples
TCR# Substance trade name or reference #: Substance/chemical name:
Lot/batch #. Location of synthesis, Fabrication, or derivation records: Molecular Formula: Condition: Expiration date:
Purity: 3M #
Entered by (Initials) KJD
Std Location/Storage F19, Frozen
Amount of Retain 0.1867 g
TCR Receipt & General Information
TCR-129 PFOS
TCR Substance # .
TCRjSu3-03l
FC-9S
Received from:
Potassium perfluorooctanesulfonate
N/A
AC KJD 7/24/00
215
Date Received:
02/02/2000
N/A Amount received (wt or vol): 40.1441 g gross w t
CSF17S03-K+ white powder 12/01/2010 TBD, KJD 5/5/00 N/A
Date Entered
Initials
Initials
Number/size of containers: Shipper MSDS (y/n)
Records received:
1/ 60ml naigene bottle N/A Y F.) N
MSDS
Checked By
Date
Date
Checked by (Initlat/Date)
Date 02/17/2000
Checked by (Initial/Date)
Comments
Initials
Was originally TN-A-2144, KJD 2/21/00 Standard has been moved to Freezer 19 in room 347 KJD 6/6/00 Shipping Codes: FC-S000-0185-6(<30 g on dry ice) LAC 06/14/01 Standard was stored at room temperature prior to 6/6/00 LAC 12/26/00
Received 5/96 RWW11/6/01 Shipping Comments: Dangerous goods in excepted quantity of Class 6, UN2811. REGULATED-TOXIC 98-0211-0888-5 (>30 g (1 oz
sample)) Not on dry Ice. LAC 01/08/02
Attachments
Date
Checked By Date
tcr99030-36msds.pdf A rch iv ed /S ub sta nc eNot Available ]
3M Environmental Laboratory
Page 259 of 276
Report E02-0443
Tenn. River Valley Samples
TCR# Substance trade name or
reference #:
Substance/chemical name:
Lot/batch #: Location of synthesis, Fabrication, or derivation records: Molecular Formula: Condition: Expiration date:
Purity:
3M# Entered by (Initials) KJD Std Location/Storage Freezer F-19, frozen Amount of Retain 0.2826 g
TCR Receipt & General information
TCR-ia
TCR Substance #
TCR-00017-071
PFBS
Potassium perfluorobutane sulfonate 2
Wildlife
Received from:
Wildlife
Date Received:
06/30/2000
Amount received (wt. or vol): -100 g, 121.5285 g gross w t
C4F9S03-K+ good/ fluffy white crystals 01/17/2007 97.3% LAC 04/26/01
L-7038 LAC 01/03/01 Date Entered
Initials
Initials
Numberfsize of containers: Shipper MSDS (y/n)
Records received:
1/ -100 mL plastic container unknown Y( iN
MSDS Interim final report from Centre and Certificate of Analysis. LAC 04/26/01
Checked By
Date
Date Checked by (Initial/Date)
Date 06/30/2000
Checked by (Initial/Date)
Comments
Wildlife International Number 5292 KJD 6/30/00 Standard Is being stored in Freezer F-19 at -20C KJD 7/17/00 Formula added on 07/24/00 by KJD Sent to Centre Analytical for Certificate of Analysis Analysis on 07/05/00 LAC 07/31/00 By F-11926 process LAC 01/03/01
Shipping comments: NOT REGULATED, (based on shipping code of LB-1000-0703-8). LAC 01/10/02
Attachments
Initials
Date
Checked By Date
tcr00017-71 msds.pdf tcr000^71 lotinfo.
& E00-1877-COA-00017-71-PFBS-R
: O rchived/Substance Not Available 1
L^
3M Environmental Laboratory
Pnno ?pn or ?7fi
Report E02-0443
3M Environmental Laboratory
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CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD
Page _1_
Tenn. River Valley Samples
Page 261 of 276
FORM ENT-131
[
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0 2 - 0 4 -V i
Report E02-0443
3M Environmental Laboratory
Atlanta Goleta Wilminton
Boston Houston ______
Dallas Okemos Walnut Creek
Dearborn Olympia
. East Greenwich Sacramento
Edmond Tacoma
Gig Harbor Ventura
CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD
Page _ A _ o t J L
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Dearborn Olympia
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Report E02-0443
Tenn. River Valley Samples
FOFM ENT-131
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Report E02-0443
3M Environmental Laboratory
Atlanta Goleta Wilminton
Boston
Houston
__
Dallas Okemos Walnut Creek
Dearborn Olympia
East Greenwich Sacramento
Edmond Tacoma
Gig Harbor Ventura
CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD
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Tenn. River Valley Samples
Pa9e 264 of 276
Report E02-0443
3M Environmental Laboratory
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Atlanta Goleta Wilminton
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Boston Houston
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Dallas Okemos Walnut Creek
Dearborn Olympia
East Greenwich Sacramento
Edmond Tacoma
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Ventura
CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD
Page 3 of 3
Tenn. River Valley Samples
Pa9e 265 of 276
FORM ENT-131
Tenn. River Valley Samples 3M Pm/ironmental Laboratory
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Boston Houston ______
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Dearborn Olympia
East Greenwich Sacramento
Edmond Tacoma
Gig Harbor Ventura
CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD
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Tenn. River Valley Samples
page 2e7 of 276
FORM ENT-131
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Page 268 of 276
3M Environmental Laboratory
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Report E02-0443
3M Environmental Laboratory
O Atlanta Goleta Wilminton
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(S O Z -O J U
Boston Houston
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Dallas Okemos 0 Walnut Creek
Dearborn Olympia
D East Greenwich
Sacramento
Edmond Tacoma
Gig Harbor Ventura
CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD
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Tenn. River Valley Samples
Page 269 of 276
FORM f ENT-131
Report E02-0443
A t t a c h m e n t E: N o te s to F ile
Tenn. River Valley Samples
3M Environmental Laboratory
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Report E02-0443
Term. River Valley Samples
3M ENVIRONMENTAL LABORATORY
Note to File
Project o r Study N um ber: E02-0443
LIM S Number: NA
Affected D ata: D020626Extracted, D020628, D020629, and D020702 (Fish Tissue)
1. The follow ing sam ples w ere m islabeled in their respective sequences. They were all labeled as "-1-1" w hen they should have been labeled as "-1-2". The list is as follows: D020626Extracted: DUDE0055, D020628: DUDE0056 and DUDE0075, D020629: DUDE0063 and DUDE0096, and D020702: DUDE0062.
2. All o f the fish tissue sample preparation was done at the same time; therefore, W ater Blanks (WB) and Solvent Blanks (SB) were done with each Sample Location, not with each different type o f fish from each location. This was done since the W Bs and SBs are for examining the sample preparation process and are independent o f the species o f fish being analyzed. The WBs and SBs were analyzed with the Catfish samples. For this reason, there are not any WB or SB data contained within the Large Mouth or Small M outh analytical sequences.
3. The fish tissue samples w ere analyzed in triplicate. Each fish tissue parent sample was first weighed out into a container (Colum n 2), had w ater added (Column 3), and then hom ogenized (Column 4) before it w as separated into triplicates. The w eight are recorded in the "-1" rows o f the Fish Tissue prep sheets. It is not until Column 6 that the triplicates are generated from the homogenate (M Ss are also generated at this time). The samples that were labeled w ith "-M S" w ere spiked w ith the spike solution in Colum n 7.
4. The fish tissue that w as used in the extracted fish curves was from the fish tissue sample with the lowest am ount of endogenous analyte concentration. This was determined during a prelim inary range-finding experim ent.
5. The extracted fish tissue standard curves had a 0 ppb curve point. This point was part o f the calibration curve and was "Enabled" in the quantitation software, but it was not calculated as part o f the curve.
6. The 10 ng/m L standard curve point in the Extracted Large M outh Standard Curve had 21% and 22% deviations, exceeding the criteria by 1% and 2%. These points were not excluded from the curves and their inclusion had no negative effect on the data quality due to the point being surrounded by at least two passing calibration points on both sides.
3M Environmental Laboratory
Page 271 of 276
Report E02-0443
Tenn. River Valley Samples
3M ENVIRONMENTAL LABORATORY
Note to File
Project o r Study N um ber: E02-0443
LIM S Number: NA
Affected D ata: 1021112/River Sedim ents
1. Lab Control Samples (LCS) were perform ed for the River Sediments. However, the information was not used because the data suggested it was impossible to recover spiked analytes from acidified water when river sediment was not present.
2. The injection files from the sequence 1021112 that are after file Itchy062 are not part o f the reportable analyses. These samples were m ethod development only.
Recorded
Date:
3M Environmental Laboratory
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Page 272 of 276
Report E02-0443
Tenn. River Volley Samples
3M ENVIRONMENTAL LABORATORY
Note to File
Project o r Study N um ber: E02-0443
LIM S Number: NA Affected D ata: D020812A and D020812B.
1. A ll data that is in D020812A and D020812B are from one original sequence: D020812. The D 020812 parent sequence is m ade up o f 161 injections/files. Files D U D E0001 to D U D E0096 are found in the sub-sequence D 020812A . Files D U D E 0097 to D U D E 0161 are in sub-sequence D 020812B. The parent sequence w as broken up into tw o separate sub-sequences after LC/MS analysis to sim plify data analysis. Low concentration sam ples that fall in the bottom end o f the standard calibration curve (0.1 ng/m L to 50 ng/m L) are in sub-sequence D020812A. V ery high concentration samples that required small injection volum es that fall in the top end o f the curve (5 ng/m L to 1000 ng/m L) are in sub-sequence D020812B. There are not any files that are contained in both sub-sequences.
2 T here are tw o different extraction dates for the sam ples: 20 Jun 02 and 17 Jul 02. This is due to a re-extraction o f 5 samples whose results were questionable.
3.
The following are the LIM S numbers and the sample names o f the samples and their associated duplicates and
matrix spikes: 38025 SW01
SW=Sample W ater(Sample Location)
38026 SW 01-Dup
FSC=Field Sample Control
38027 38028 38029
SW O l-L ow SW 01-Med F S C O l-L o w
FB= Field Blank Low=Low Field Spike M ed=M edium Field Spike
38030 FSC01-Med 38032 FB02
38033 SW03
38034 SW03-Dup
38035 SW03-Low
38036 SW03-Med
38037 SW02
38038 SW 02-Dup
38039 SW02-LOW
38340 SW 02-Med
38041 FCS02-LOW
38042 FCS02-Med
38043 T rip B lank #1
and
38047 Trip Blank #2
Date:
3M Environmental Laboratory
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Report E02-0443
Tenn. River Valley Samples
3M ENVIRONMENTAL LABORATORY
Note to File
Project o r Study N um ber: E02-0443
LIM S Number: NA
Affected D ata: D020626Extracted
1. In the D 020626E xtracted sequence there w ere not any Extracted CCV curve points run. AH subsequent Fish Tissue sequences had extracted CCVs included. The unextracted CCVs were quantitated against the unextracted fish curve, 02003-050, using an Excel spreadsheet. All o f the unextracted CCVs passed and the results are found in Appendix B: D ata Summary Tables.
Recorded By:.
Date:
3M Environmental Laboratory
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Report E02-0443
Tenn. River Valley Samples
3M ENVIRONMENTAL LABORATORY
Note to File
Project o r Study Num ber: E02-0443
LIM S Number: NA
Affected D ata: All D ata
Note: This is to explain how the quantitation was performed on the data. 1. The entire calibration curve was entered into the quantitation software and the curve was then analyzed. In many cases, high level curve points were "Disabled" in the software and w ere rem oved from the curve calculation. In all instances in which this w as done, the disabled curve points show a recovery o f 0%. Low end curve points that had % Recoveries that exceeded the criteria or were <2X the solvent blanks levels were not used. These points were still included in the calibration curve calculations, however, they were not used in the determination o f the LOQ.
2. In the raw data that com es from the Target software, concentrations that would normally be quantitated as a very low or a negative value are assigned an extreme positive value. These values are easily noticed due to their abnorm ally large values along with very small area counts. These values, along with values that are below the limit o f quantitation, are changed to "BLOQ" to eliminate any possible confusion.
Recorded By:
Date:
3M Environmental Laboratory
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Page 275 of 276
Report E02-0443
Tenn. River Valley Samples
3M ENVIRONMENTAL LABORATORY
Note to File
Project or Study N um ber: E02-0443
LIM S Number: NA
Affected D ata: Fish Tissue
1. In the sam ple preparation process o f the fish tissue, after the hom ogenization process (Step 4), the hom ogenate is centrifuged for a short tim e and then shaken (Step 5). The centrifugation w as done to eliminate the foam that developed during the homogenization process. The homogenate was then shaken/vortexed to make the solution hom ogenous again.
3M Environmental Laboratory
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