Document MMeoZYD5q13O0GYGZa54E7BwL
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
Final Report
A n a ly s is o f P F O A , P F B S , P F H S , a n d P F O S in G r o u n d W a t e r S a m p le s C o lle c te d a t th e F o rm e r S lu d g e In c o rp o ra tio n A re a (F S IA ) fro m D e c a tu r, A L 4 th Q u a r t e r 2 0 1 3
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Report Date - Date of Final Signature
T e s tin g L a b o ra to ry 3 M E n v iro n m e n ta l H e a lth a n d S a fe ty O p e ra tio n s
E n v iro n m e n ta l L a b o ra to ry 3 M C e n te r, B ld g 2 6 0 -0 5 -N -1 7
S t. P a u l, M N 5 5 1 4 4
Requester
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The testing reported herein meet the requirements of ANSI/ISO/IEC 17025:2005 "General Requirements for the Competence of Testing and Calibration Laboratories", in accordance with A2LA Certificate # 2052.01. Additionally, the laboratory's quality system has been audited and was determined to be in conformance with the EPA GLPs (40 CFR 792) by an independent assessment.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
3M Environmental Laboratory
3M Environmental Laboratory Technical Director: William K. Reagen, Ph.D. 3M Principal Analytical Investigator: Susan Wolf Report Author: Kevin Eich
Analytical Report ISO13-05-05
Analysis of PFOA, PFBS, PFHS, and PFOS in Ground Water Samples Collected at the Former Sludge Incorporation Area (FSIA) from Decatur, AL 4th Quarter 2013
Report Date: Date of Final Signature
1 Introduction/Summary
The 3M Environmental Laboratory prepared and analyzed water samples collected by Weston Solutions personnel from Decatur, AL. Samples were collected on November 19, November 20, and November 21 and returned to the 3M Environmental Laboratory on November 25, 2013 at ambient conditions. All samples were analyzed for perfluorooctanoic acid (PFOA), perfluorobutane sulfonate (PFBS), perfluorohexane sulfonate (PFHS) and perfluorooctane sulfonate (PFOS) under laboratory project number ISO13-05-05.
The 3M Environmental Laboratory prepared sample containers for thirty-one groundwater well locations. Each empty container was marked with a "fill to here" line that corresponded to a final volume of 200 mL. Sample bottle sets for each groundwater sampling location included a field sample and field sample duplicate. Select locations also included one field spike sample. Containers designated for field matrix samples were fortified with an appropriate matrix spike solution containing PFOA, PFBS, PFHS, and PFOS prior to being sent to the field for sample collection. Sampling locations DAL-GW-136R, DAL-GW-137R, DAL-GW-137S, DAL-GW-138R, and DAL-GW-143R were not collected due to the well being dry.
Samples were analyzed for PFOA, PFBS, PFHS, and PFOS by ETS-8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis".
Table 1 summarizes the sample results using the analytical method identified above. All results for quality control samples prepared and analyzed with the samples will be reported and discussed elsewhere in this report.
The testing reported herein meet the requirements of ANSI/ISO/IEC 17025:2005 "General Requirements for the Competence of Testing and Calibration Laboratories", in accordance with A2LA Certificate # 2052.01. Additionally, the laboratory's quality system has been audited and was determined to be in conformance with the EPA GLPs (40 CFR 792) by an independent assessment.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
Table 1. Sample Results Summary (1)
3M LIMS ID ISO13-05-05-001 ISO13-05-05-002
ISO13-05-05-003 ISO13-05-05-004
ISO13-05-05-005 ISO13-05-05-006
ISO13-05-05-007 ISO13-05-05-008
ISO13-05-05-010 ISO13-05-05-011
ISO13-05-05-012 ISO13-05-05-013
ISO13-05-05-014 ISO13-05-05-015
ISO13-05-05-017 ISO13-05-05-018
Sample Description
DAL-GW-130R-0-131121 DAL-GW-130R-DB-131121
Average %RPD Sample/Sample Dup DAL-GW-130S-0-131121 DAL-GW-130S-DB-131121
Average %RPD Sample/Sample Dup DAL-GW-130L-0-131121 DAL-GW-130L-DB-131121
Average %RPD Sample/Sample Dup DAL-GW-131R-0-131121 DAL-GW-131R-DB-131121
Average %RPD Sample/Sample Dup DAL-GW-131S-0-131121 DAL-GW-131S-DB-131121
Average %RPD Sample/Sample Dup DAL-GW-131L-0-131121 DAL-GW-131L-DB-131121
Average %RPD Sample/Sample Dup DAL-GW-133R-0-131120 DAL-GW-133R-DB-131120
Average %RPD Sample/Sample Dup DAL-GW-133S-0-131120 DAL-GW-133S-DB-131120
Average %RPD Sample/Sample Dup
PFOA Concentration
(ng/mL)
955 962 959 0.73 195 187 191 4.2 62.7 59.5 61.1 5.2 2300 2530 2420 9.5 33.1 33.2 33.2 (2) 0.30 104 108 106 (2) 3.8 51.7 52.1 51.9 (2) 0.77 393 399 396 1.5
PFBS Concentration
(ng/mL)
17.6 17.9 17.8 1.7 3.84 3.71 3.78 3.4 1.47 1.39 1.43 5.6 54.8 58.9 56.9 7.2 1.08 1.05 1.07 (2) 2.8 3.73 3.96 3.85 (2) 6.0 2.80 2.90 2.85 (2) 3.5 9.68 10.2 9.94 5.2
PFHS Concentration
(ng/mL)
132 132 132 0.0 33.4 32.8 33.1 1.8 11.6 10.8 11.2 7.1 303 326 315 7.3 5.81 6.08 5.95 (2) 4.5 22.6 27.1 24.9 (2) 18 17.9 16.1 17.0 (2) 11 70.5 70.8 70.7 0.42
PFOS Concentration
(ng/mL)
571 585 578 2.4 147 140 144 4.9 72.7 68.5 70.6 5.9 1210 1300 1260 7.2 7.08 6.58 6.83 (2) 7.3 45.6 47.2 46.4 (2) 3.4 35.9 31.7 33.8 (2) 12 251 256 254 2.0
NA = Not Applicable (1) All samples associated with the reported sampling location were diluted and analyzed by external standard calibration unless
noted otherwise. The analytical method uncertainties for the reported results using method ETS-8-044.1 by direct injection are as follows: PFOA 17%, PFBS 17%, PFHS 16%, and PFOS 19%. (2) All samples associated with the reported sampling location were analyzed by internal standard calibration. The analytical method uncertainties for the reported results using method ETS-8-044.1 by direct injection are as follows: PFOA 12%, PFBS 14%, PFHS 22%, and PFOS 14%. (3) The RPD value did not meet method acceptance criteria of <20%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
Table 1 continued. Sample Results Summary (1)
3M LIMS ID ISO13-05-05-020 ISO13-05-05-021
ISO13-05-05-022 ISO13-05-05-023
ISO13-05-05-024 ISO13-05-05-025
ISO13-05-05-027 ISO13-05-05-028
ISO13-05-05-030 ISO13-05-05-031
ISO13-05-05-033 ISO13-05-05-034
ISO13-05-05-035 ISO13-05-05-036
ISO13-05-05-039 ISO13-05-05-040
Sample Description
DAL-GW-133L-0-131120 DAL-GW-133L-DB-131120
Average %RPD Sample/Sample Dup DAL-GW-134R-0-131120 DAL-GW-134R-DB-131120
Average %RPD Sample/Sample Dup DAL-GW-134S-0-131120 DAL-GW-134S-DB-131120
Average %RPD Sample/Sample Dup DAL-GW-134L-0-131120 DAL-GW-134L-DB-131120
Average %RPD Sample/Sample Dup DAL-GW-135R-0-131119 DAL-GW-135R-DB-131119
Average %RPD Sample/Sample Dup DAL-GW-135S-0-131119 DAL-GW-135S-DB-131119
Average %RPD Sample/Sample Dup DAL-GW-135L-0-131119 DAL-GW-135L-DB-131119
Average %RPD Sample/Sample Dup DAL-GW-136S-0-131120 DAL-GW-136S-DB-131120
Average %RPD Sample/Sample Dup
PFOA Concentration
(ng/mL)
367 369 368 0.54 1720 1820 1770 5.6 25.8 25.9 25.9 (2) 0.39 536 535 536 0.19 4060 4020 4040 0.99 59.0 60.0 59.5 (2) 1.7 595 605 600 1.7 120 119 120 0.84
PFBS Concentration
(ng/mL)
8.29 8.67 8.48 4.5 43.9 45.6 44.8 3.8 0.688 0.628 0.658 (2) 9.1 9.93 10.6 10.3 6.5 71.8 72.3 72.1 0.69 2.33 2.32 2.33 (2) 0.43 15.7 16.8 16.3 6.8 2.98 2.96 2.97 0.67
PFHS Concentration
(ng/mL)
59.2 59.4 59.3 0.34 390 405 398 3.8 7.49 7.53 7.51 (2) 0.53 100 97.4 98.7 2.6 812 787 800 3.1 20.2 21.6 20.9 (2) 6.7 124 124 124 0.0 20.6 20.3 20.5 1.5
PFOS Concentration
(ng/mL)
310 325 318 4.7 1240 1280 1260 3.2 27.8 29.1 28.5 (2) 4.6 515 498 507 3.4 1180 1210 1200 2.5 16.0 15.8 15.9 (2) 1.3 183 186 185 1.6 126 125 126 0.80
NA = Not Applicable (1) All samples associated with the reported sampling location were diluted and analyzed by external standard calibration unless
noted otherwise. The analytical method uncertainties for the reported results using method ETS-8-044.1 by direct injection are as follows: PFOA 17%, PFBS 17%, PFHS 16%, and PFOS 19%. (2) All samples associated with the reported sampling location were analyzed by internal standard calibration. The analytical method uncertainties for the reported results using method ETS-8-044.1 by direct injection are as follows: PFOA 12%, PFBS 14%, PFHS 22%, and PFOS 14%. (3) The RPD value did not meet method acceptance criteria of <20%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
Table 1 continued. Sample Results Summary (1)
3M LIMS ID ISO13-05-05-041 ISO13-05-05-042
ISO13-05-05-049 ISO13-05-05-050
ISO13-05-05-053 ISO13-05-05-054
ISO13-05-05-055 ISO13-05-05-056
ISO13-05-05-057 ISO13-05-05-058
ISO13-05-05-060 ISO13-05-05-061
ISO13-05-05-063 ISO13-05-05-064
ISO13-05-05-065 ISO13-05-05-066
Sample Description
DAL-GW-136L-0-131120 DAL-GW-136L-DB-131120
Average %RPD Sample/Sample Dup DAL-GW-137L-0-131119 DAL-GW-137L-DB-131119
Average %RPD Sample/Sample Dup DAL-GW-138S-0-131119 DAL-GW-138S-DB-131119
Average %RPD Sample/Sample Dup DAL-GW-138L-0-131119 DAL-GW-138L-DB-131119
Average %RPD Sample/Sample Dup DAL-GW-CW26C-0-131121 DAL-GW-CW26C-DB-131121
Average %RPD Sample/Sample Dup DAL-GW-CW26L-0-131121 DAL-GW-CW26L-DB-131121
Average %RPD Sample/Sample Dup DAL-GW-140R-0-131120 DAL-GW-140R-DB-131120
Average %RPD Sample/Sample Dup DAL-GW-141R-0-131119 DAL-GW-141R-DB-131119
Average %RPD Sample/Sample Dup
PFOA Concentration
(ng/mL)
96.5 96.7 96.6 0.21 0.477 0.450 0.464 (2) 5.8 178 184 181 3.3 0.613 0.664 0.639 (2) 8.0 443 460 452 3.8 897 871 884 2.9 110 113 112 2.7 2.56 2.59 2.58 (2) 1.2
PFBS Concentration
(ng/mL)
2.51 2.52 2.52 0.40 0.0920 0.0903 0.0912 (2) 1.9 5.64 5.45 5.55 3.4 <0.0250 <0.0250 <0.0250 (2) NA 8.14 8.73 8.44 7.0 14.1 14.6 14.4 3.5 1.10 1.06 1.08 3.7 0.0731 0.0491 0.0611 (2) 39 (3)
PFHS Concentration
(ng/mL)
16.1 16.0 16.1 0.62 0.115 0.0956 0.105 (2) 18 24.3 25.4 24.9 4.4 0.0568 0.0618 0.0593 (2) 8.4 63.3 64.6 64.0 2.0 118 113 116 4.3 13.8 13.3 13.6 3.7 0.418 0.459 0.439 (2) 9.4
PFOS Concentration
(ng/mL)
97.1 97.2 97.2 0.10 1.84 1.64 1.74 (2) 11 247 254 251 2.8 0.486 0.404 0.445 (2) 18 448 462 455 3.1 1400 1350 1380 3.6 118 119 119 0.84 7.41 6.93 7.17 (2) 6.7
NA = Not Applicable (1) All samples associated with the reported sampling location were diluted and analyzed by external standard calibration unless
noted otherwise. The analytical method uncertainties for the reported results using method ETS-8-044.1 by direct injection are as follows: PFOA 17%, PFBS 17%, PFHS 16%, and PFOS 19%. (2) All samples associated with the reported sampling location were analyzed by internal standard calibration. The analytical method uncertainties for the reported results using method ETS-8-044.1 by direct injection are as follows: PFOA 12%, PFBS 14%, PFHS 22%, and PFOS 14%. (3) The RPD value did not meet method acceptance criteria of <20%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
Table 1 continued. Sample Results Summary (1)
3M LIMS ID ISO13-05-05-067 ISO13-05-05-068
ISO13-05-05-071 ISO13-05-05-072
Sample Description
DAL-GW-142R-0-131121 DAL-GW-142R-DB-131121
Average %RPD Sample/Sample Dup DAL-GW-145R-CM31122 DAL-GW-145R-DB-131122
Average %RPD Sample/Sample Dup
PFOA Concentration
(ng/mL)
65.4 68.1 66.8 4.0 83.0 85.3 84.2 2.7
PFBS Concentration
(ng/mL)
2.32 2.30 2.31 0.87 2.24 2.32 2.28 3.5
PFHS Concentration
(ng/mL)
12.6 13.3 13.0 5.4 9.57 10.0 9.79 4.4
PFOS Concentration
(ng/mL)
163 166 165 1.8 177 181 179 2.2
NA = Not Applicable (1) All samples associated with the reported sampling location were diluted and analyzed by external standard calibration unless
noted otherwise. The analytical method uncertainties for the reported results using method ETS-8-044.1 by direct injection are as follows: PFOA 17%, PFBS 17%, PFHS 16%, and PFOS 19%. (2) All samples associated with the reported sampling location were analyzed by internal standard calibration. The analytical method uncertainties for the reported results using method ETS-8-044.1 by direct injection are as follows: PFOA 12%, PFBS 14%, PFHS 22%, and PFOS 14%. (3) The RPD value did not meet method acceptance criteria of <20%.
2 Methods - Analytical and Preparatory
2.1 Methods
Analysis was completed using 3M Environmental Laboratory Method ETS-8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis".
Table 2. Target Analytes
Target Analytes Perfluorobutanoic Acid (C4 Acid) Perfluorooctanoic Acid (C8 Acid) Perfluorobutanesulfonate (C4 Sulfonate ) Perfluorooctanesulfonate (C8 Sulfonate)
Acronym PFOA PFBS PFHS PFOS
Reference Material Structure
Linear and Branched Linear Linear
Linear and Branched
2.2 Sample Collection
All samples were collected in 250 mL NalgeneTM (high-density polyethylene) bottles prepared at the 3M Environmental Laboratory. Samples were collected on November 19, November 20, and November 21 and returned to the 3M Environmental Laboratory on November 25, 2013 at ambient conditions. Prior to sample collection, bottles designated for field matrix spikes were spiked in the laboratory with a known volume of an appropriate matrix spiking solution containing PFOA, PFBS, PFHS, and PFOS.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
Table 3. Sample Description Key Code.
String Number 1 2 3 4
String Descriptor Sample Location Sample Type Well Identifier Well Level
5 Sample Type
6 Sampling Date
Example: DAL-GW-130R-DB-131121
DAL= Decatur, Alabama GW= Ground Water Example: 130 R = Residuum shallow water-bearing zone L = Bedrock water-bearing zone S = Epikarst middle water-bearing zone 0 =primary sample DB =duplicate sample FMS = Field Matrix Spike LS = Low field matrix spike HS = High field matrix spike 131121 - November 21,2013
2.3 Sample Preparation
12/5/13: Solvent dilution / external standard analysis. All samples and laboratory control spikes were diluted with methanol prior to sample analysis. Samples requiring a 1:10 dilution were prepared by removing a 1.0 mL aliquot of the well mixed sample and diluting it with 9.0 mL of methanol. Samples requiring a 1:20 dilution were prepared by removing a 0.5 mL aliquot of the well mixed sample and diluting it with 9.5 mL of methanol. Samples requiring a 1:50 dilution were prepared by removing a 0.2 mL aliquot of the well mixed sample and diluting it with 9.8 mL of methanol. Samples requiring a 1:100 dilution were prepared by removing a 0.1 mL aliquot of the well mixed sample and diluting it with 9.9 mL of methanol.
12/10/13: All samples were prepared by removing a 0.4 mL aliquot of the well mixed sample and diluting it with 0.4 mL of methanol (dilution factor of 2). During the preparation of the laboratory control samples, an aliquot of a separate internal standard spiking solution was added to the laboratory control samples (nominal concentration of 1 ng/mL). The sample bottles were spiked with an internal standard mix at a nominal concentration of 1 ng/mL prior to being sent to the field for sample collection. The laboratory control samples were then diluted with methanol in the same manner as the samples.
2.4 Analysis
All samples and quality control samples were analyzed for the four target analytes using high performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). Pertinent instrument parameters, the liquid chromatography gradient program, and the specific mass transitions analyzed are described in the tables below. The following analytical runs were processed and reported herein:
12/5/13: Solvent dilution / external standard analysis for PFOA, PFBS, PFHS, PFOS (samples extracted 12/5/13); locations 130R, 130S, 130L, 131R, 133S, 133L, 134R, 134L, 135R, 135L, 136S, 136L, 138S, CW26C, CW26L, 140R, 142R, 145R, Trip Blank mid and high FMS.
12/10/13: Solvent dilution / internal standard analysis for PFOA, PFBS, PFHS, PFOS (samples extracted 12/10/13); locations 131S, 131L, 133R, 134S, 135S, 137L, 138L, 141R, rinseate blanks, trip blank and trip blank low FMS.
Due to the nature of the sample, the wide range of concentrations found in the sample, and the environmental occurrence of multiple isomers of the laboratory's analytes of interest, the software used for processing the analytical results is not able to consistently integrate the analytical peak, manual integration of the analytical peak is necessary. All manual integrations are performed following the procedures outlined in method ETS-12-010. The consistency of the laboratory's integration is ensured
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
through the training of laboratory personnel, the peer review process required for all manual integrations, the review of manual integrations by the QAU, and where necessary the review of manual integrations by laboratory management.
Table 4. Instrument Parameters
Instrument Name Analysis Dates Analytical Method Liquid Chromatograph Guard column Analytical column Injection Volume Mass Spectrometer Ion Source Polarity Software
ETS Buster 12/5/13, 12/10/13
ETS-8-044.1 Agilent 1100 Betasil C18 (4.6 mm X 100 mm), 5 x Betasil C18 (4.6 mm X 100 mm), 5 x 5, 10, 20, 25, uL Applied Biosystems API 4000 Turbo Spray
Negative Analyst 1.6.1
Table 5. Liquid Chromatography Gradient Program
Step
0 1 2 3 4 5 6 7 8 9
Total Time (min)
0 0.5 4.0 6.0 11.0 13.0 13.5 16.0 16.5 19.0
Flow Rate (uL/min)
2 mM Ammonium Acetate
ETS Buster 12/5/13 and 12/10/13
750 90.0
750 90.0
750 70.0
750 70.0
750 20.0
750 20.0
750 10.0
750 10.0
750 90.0
750 90.0
Methanol
10.0 10.0 30.0 30.0 80.0 80.0 90.0 90.0 10.0 10.0
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
Table 6. Mass Transitions
Analyte
Mass Transition Q1/Q3
Internal Standard
Mass Transition Q1/Q3
Reference Material Structure
413/369
PFOA
413/219
[13C8]PFOA (1)
421/376
Linear and Branched
413/169
PFBS
299/80 299/99
[18O2]PFBS (1)
303/84
Linear
PFHS
399/99 399/80
[13Cs]PFHS (1)
402/99
Linear
499/99
PFOS
499/80
[13C8]-PFOS (1)
507/80
Linear and Branched
499/130
Dwell time was 50 msec for each transition. The individual transitions were summed to produce a "total ion chromatogram" (TIC), which was used for quantitation.
(1) Internal standard was used for the analysis on 12/10/13.
3 Data Analysis
3.1 Calibration
12/5/13: Solvent dilution / external standard calibration. Diluted samples were analyzed against an external standard calibration curve for PFOA, PFBS, PFHS, and PFOS. Calibration standards were prepared by spiking known amounts of stock solutions containing the analytes of interest into 50 mL of 90:10 methanol: laboratory Milli-QTM water. A total of eleven calibration standards ranging from 0.1 ng/mL to 150 ng/mL (nominal) were analyzed. A quadratic, 1/x weighted, calibration curve was used to fit the data for each analyte. The data were not forced through zero during the fitting process. Calculating the standard concentration using the peak area counts and the resultant calibration curve confirmed accuracy of each curve point. The reference standards of PFOA and PFOS used to prepare the calibration standards consisted of both linear and branched isomers.
12/10/13: Direct Injection / internal standard calibration. Samples were analyzed against a matrix-matched stable isotope internal standard calibration curve. Calibration standards were prepared by spiking known amounts of the stock solution into laboratoryprepared reagent water. The calibration standards contained an internal standard mix at a nominal concentration of 0.5 ng/mL. A total of fourteen curve points were analyzed with the samples ranging from 0.0125 ng/mL to 100 ng/mL. A quadratic, 1/x weighted, calibration curve of the ratio of the standard peak area counts over the internal standard peak area counts was used to fit the data for each analyte. The data were not forced through zero during the fitting process.
For all analyses, each curve point was quantitated using the overall calibration curve and reviewed for accuracy. Method calibration accuracy requirements of 10025% (10030% for the lowest curve point) were met for all analytes. The correlation coefficient (r) was greater than 0.995 for all analytes.
3.2 System Suitability
A calibration standard was analyzed four times at the beginning of the analytical sequence to demonstrate overall system suitability. The acceptance criteria for system suitability samples is less than or equal to 5% relative standard deviation (RSD) for peak area or peak area ratio and retention time criteria of less than or equal to 2% RSD. These criteria were met for all analytes with the following exceptions:
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
12/10/13 Analysis: The system suitability for area counts was greater than five percent for PFHS (8.9%).
A method deviation is included in the raw data.
3.3 Limit of Quantitation (LOQ)
The LOQ as defined in method ETS-8-044.1 is the lowest non-zero calibration standard in the curve that meets linearity and accuracy requirements and for which the peak area ratio (or peak area) is at least two times the average peak area ratio (or peak area) of the method blanks. The LOQs associated with the sample analysis are listed in the table below.
Table 7. LOQ
Analysis Date
Calibration
12/5/13
External standard
12/10/13
Internal standard
Dilution Factor
2 5 10 20 50 100 2
PFOA LOQ, ng/mL
0.192 0.479 0.958 1.92 4.79 9.58 0.0480
PFBS LOQ, ng/mL
0.200 0.500 1.00 2.00 5.00 10.0 0.0250
PFHS LOQ, ng/mL
0.200 0.500 1.00 2.00 5.00 10.0 0.0250
PFOS LOQ, ng/mL
0.185 0.464 0.927 1.85 4.64 9.27 0.0232
3.4 Continuing Calibration
During the course of the analytical sequence, several continuing calibration verification samples (CCVs) were analyzed to confirm that the instrument response and the initial calibration curve were still in control. The method acceptance criteria of 100% 25% was met for all analytes for all analyses.
3.5 Blanks
Three types of blanks were prepared and analyzed with the samples: method/procedural blanks, a field/trip blank, and a single equipment rinseate blank. Method blank results were reviewed and used to evaluate method performance to determine the LOQ for each analyte.
3.6 Lab Control Spikes (LCSs)
Low, mid, and high lab control spikes were prepared with each sample preparation batch for the target analytes and analyzed in triplicate. LCSs were prepared by spiking known amounts of the analytes into synthetic groundwater or laboratory Milli Q water to produce the desired concentration. The LCS samples were then diluted in a similar manner as the samples (if diluted) prior to sample analysis. The method acceptance criteria, average of each level of LCS should be within 100% 20% with an RSD <20%, was met for all LCSs with the following exceptions:
12/10/13 analysis: The acceptance criteria for accuracy were met with the exception of the high set of LCS for PFHS (122%).
A method deviation is filed in the raw data. All batch LCS recovery results were used in the evaluation of the analytical method uncertainty in section 3.7 of the report.
The following calculations were used to generate data in Table 8.
Calculated Concentration LCS Percent Recovery
Spike Concentration
%
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
LCS% RSD = standard deviation LCS replicates * 1QQ% average LCS recovery
Table 8. Lab Control Spike Results
ETS-8-044.1 Analyzed 12/5/13 External Standard Calibration
Lab ID LCS-131204-1 LCS-131204-2 LCS-131204-3 Average %RSD LCS-131204-4 LCS-131204-5 LCS-131204-6 Average %RSD LCS-131204-7 LCS-131204-8 LCS-131204-9 Average %RSD
PFOA (Linear and Branched)
Spiked Concentration
(ng/mL)
Calculated Concentration
(ng/mL)
%Recovery
0.477 0.477 0.477
4.77 4.77 4.77
38.2 38.2 38.2
0.496 0.370 0.457 92.4% 15% 5.58 5.20 4.45 106% 11% 38.3 38.3 41.0 102% 3.9%
104 77.6 95.7
117 109 93.2
100 100 107
Spiked Concentration
(ng/mL) 0.498 0.498 0.498
4.98 4.98 4.98
39.8 39.8 39.8
PFBS Calculated Concentration
(ng/mL)
0.490 0.402 0.473 91.4% 10% 6.02 5.53 4.62 108% 13% 41.1 40.5 42.8 104% 2.5%
%Recovery 98.5 80.8 95.0
121 111 92.8
103 102 107
ETS-8-044.1 Analyzed 12/5/13 External Standard Calibration
Lab ID LCS-131204-1 LCS-131204-2 LCS-131204-3 Average %RSD LCS-131204-4 LCS-131204-5 LCS-131204-6 Average %RSD LCS-131204-7 LCS-131204-8 LCS-131204-9 Average %RSD
Spiked Concentration
(ng/mL) 0.498 0.498 0.498
4.98 4.98 4.98
39.8 39.8 39.8
PFHS Calculated Concentration
(ng/mL)
0.482 0.377 0.511 91.8% 16% 5.96 5.53 4.62 108% 13% 39.8 40.2 42.9 103% 4.2%
%Recovery 96.8 75.7 103
120 111 92.8
100 101 108
PFOS (Linear and Branched)
Spiked Concentration
(ng/mL)
Calculated Concentration
(ng/mL)
%Recovery
0.461 0.461 0.461
4.61 4.61 4.61
36.9 36.9 36.9
0.481 0.346 0.437 91.3% 16% 5.46 4.85 4.33 106% 11% 37.4 36.7 40.3 103% 5.0%
104 75.1 94.7
118 105 93.9
101 99.4 109
PAGE 11 OF 20
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
Table 8 continued. Lab Control Spike Results
ETS-8-044.1 Analyzed 12/10/13 Internal Standard Calibration
Lab ID
LCS-131210-1 LCS-131210-2 LCS-131210-3 Average %RSD LCS-131210-4 LCS-131210-5 LCS-131210-6 Average %RSD LCS-131210-7 LCS-131210-8 LCS-131210-9 Average %RSD
PFOA (Linear and Branched)
Spiked Concentration
(ng/mL)
Calculated Concentration
(ng/mL)
%Recovery
0.190 0.190 0.190
9.52 9.52 9.52
38.0 38.0 38.0
0.197 0.194 0.203 104% 2.4% 10.8 10.2 10.6 111% 3.2% 41.7 44.4 42.3 113% 3.4%
104 102 107
114 107 111
110 117 111
Spiked Concentration
(ng/mL) 0.199 0.199 0.199
9.94 9.94 9.94
39.6 39.6 39.6
PFBS Calculated Concentration
(ng/mL)
0.203 0.251 0.232 115% 11% 11.6 10.3 10.8 110% 6.0% 42.8 44.9 44.9 111% 2.6%
%Recovery 102 126 116
117 104 109
108 113 113
ETS-8-044.1 Analyzed 12/10/13 Internal Standard Calibration
Lab ID
LCS-131210-1 LCS-131210-2 LCS-131210-3 Average %RSD LCS-131210-4 LCS-131210-5 LCS-131210-6 Average %RSD LCS-131210-7 LCS-131210-8 LCS-131210-9 Average %RSD
Spiked Concentration
(ng/mL)
PFHS
Calculated Concentration
(ng/mL)
0.199 0.199 0.199
9.94 9.94 9.94
39.6 39.6 39.6
0.196 0.218 0.221 106% 6.2% 10.7 10.7 11.5 111% 4.2% 51.7 44.9 49.0 122% 7.0%(1)
%Recovery 98.7 109 111
108 108 116
130 113 124
PFOS (Linear and Branched)
Spiked Concentration
(ng/mL)
Calculated Concentration
(ng/mL)
%Recovery
0.184 0.184 0.184
9.21 9.21 9.21
36.7 36.7 36.7
0.204 0.188 0.205 108% 5.1% 10.4 10.3 9.91 111% 2.4% 39.4 42.2 41.2 111% 3.6%
111 102 112
113 112 108
107 115 112
(1) The average LCS recovery did not meet method acceptance criteria of 100% 20%.
PAGE 12 OF 20
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
3.7 Analytical Method Uncertainty
Analytical method uncertainty is based on historical QC data that is control charted and used to evaluate method accuracy and precision. The method uncertainty is calculated following ETS-12012.2. The standard deviation is calculated for the set of accuracy results (in %) obtained for the QC samples. The expanded uncertainty is calculated by multiplying the standard deviation by a factor of 2, which corresponds to a confidence level of 95%.
The analytical method uncertainty as calculated by ETS-12-012.2 for PFHS by internal standard calibration was 15%. However, the recovery of the high set of LCS analyzed on 12/10/13 was 122% for PFHS by internal standard calibration for the samples analyzed on this date. Therefore, the analytical method uncertainty was expanded for samples analyzed by internal standard calibration for PFHS to 22%.
Table 9. Analytical Method Uncertainty
Analyte PFOA PFBS PFHS PFOS PFOA PFBS PFHS PFOS
Calibration External External External External Internal Internal Internal Internal
Standard Deviation (%) 8.26 8.67 7.81 9.34 5.98 7.07 NA 7.19
Method Uncertainty 17% 17% 16% 19% 12% 14% 22% 14%
NA = Not Applicable
3.8 Field Matrix Spikes (FMS) and Laboratory Matrix Spikes (LMS)
Field matrix spike sample containers were prepared for all locations to verify that the analytical method is applicable to the collected matrix. Field matrix spikes are generated by adding a measured volume of field sample to a container spiked by the laboratory with the target analytes prior to shipping sample containers to the field for sample collection. Field matrix spikes must be at least 0.5 times the analyte concentration to be considered an appropriate spike level. Field matrix spike recoveries within method acceptance criteria of 10030% confirm that "unknown" components in the sample matrix do not significantly interfere with the extraction and analysis of the analytes of interest. The reference standards for PFOA and PFOS in the field matrix spiking solution consisted of linear and branched isomers. The locations for which FMS sample containers were prepared are listed in Table 10.
Field matrix spikes are presented in section 4 of this report.
FMS ,,Recovery = 4(-S--a-m--p- -le---C--o--n--c-e--n-t-r-a--t-i-o-n---o--f-F--M---S------A--v-e--r-a-g2-e---C--o--n--c--e-n--t-r-a--t-i-o-n--:-F--i-e-l-d--S--a--m--pL-le---&---F--ie--ld---S--a--m- pL-le---D--u-p*.1)0 0 % Spike Concentraton
PAGE 13 OF 20
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
Table 10. Field Matrix Spike (FMS) Concentrations
Sampling location 137S 134S 133R, 136L 133S, CW26C 134L, CW26L 131R, 135R
Trip Blank
Spike Level FMS FMS FMS FMS FMS FMS FMS Low FMS Mid FMS High
PFOA ng/mL 0.992
9.92 49.6 198 496 1980 9.92 49.6 1980
PFBS ng/mL
1.00 10.0 50.0 200 500 2000 10.0 50.0 2000
PFHS ng/mL
1.00 10.0 50.0 200 501 2000 10.0 50.0 2000
PFOS ng/mL 0.998
9.98 49.9 200 499 2000 9.98 49.9 2000
4 Data Summary and Discussion
Tables 11-21 below summarize the sample results and target analyte field matrix spike recoveries for the sampling locations as well as the Trip Blank. Each table provides the average concentration and the relative percent difference (%RPD) of the sample and sample duplicate. Results and average values are rounded to three significant figures. Percent relative difference (%RPD) values are rounded to two significant figures. Because of rounding, values may vary slightly from those listed in the raw data. Field matrix spikes meeting the method acceptance criteria of 30%, demonstrate that the method is appropriate for the given matrix. All target analyte field matrix spikes met method acceptance criteria.
Table 11. DAL-GW-131R
3M LIMS ID
Description
ISO13-05-05-007
DAL-GW-131R-0-131121
ISO13-05-05-008 ISO13-05-05-009
DAL-GW-131R-DB-131121 DAL-GW-131R-FMS-131121
Average Concentration (ng/mL) %RPD
PFOA
Concentration (ng/mL)
%Recovery
2300
NA
2530
NA
4510
106
2420 ng/mL 9.5%
PFBS
Concentration (ng/mL)
%Recovery
54.8 NA
58.9 NA
2070
101
56.9 ng/mL 7.2%
PFHS
3M LIMS ID
Description
ISO13-05-05-007 ISO13-05-05-008 ISO13-05-05-009
DAL-GW-131R-0-131121 DAL-GW-131R-DB-131121 DAL-GW-131R-FMS-131121
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
303 NA
326 NA
2380
103
315 ng/mL 7.3%
NA = Not Applicable Samples were diluted 1:100 and analyzed using external standard quantitation.
PFOS
Concentration (ng/mL)
%Recovery
1210
NA
1300
NA
3250
99.8
1260 ng/mL 7.2%
PAGE 14 OF 20
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
Table 12. DAL-GW-133R
3M LIMS ID
Description
ISO13-05-05-014 ISO13-05-05-015 ISO13-05-05-016
DAL-GW-133R-0-131120 DAL-GW-133R-DB-131120 DAL-GW-133R-FMS-131120
Average Concentration (ng/mL) %RPD
PFOA
Concentration (ng/mL)
%Recovery
51.7 NA 52.1 NA 100 97.0
51.9 ng/mL 0.77%
PFBS
Concentration (ng/mL)
%Recovery
2.80 NA 2.90 NA 61.9 118
2.85 ng/mL 3.5%
PFHS
3M LIMS ID
Description
ISO13-05-05-014 ISO13-05-05-015 ISO13-05-05-016
DAL-GW-133R-0-131120 DAL-GW-133R-DB-131120 DAL-GW-133R-FMS-131120
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
17.9 NA 16.1 NA 66.2 98.4
17.0 ng/mL 11%
NA = Not Applicable Samples were diluted 1:2 and analyzed using internal standard quantitation.
PFOS
Concentration (ng/mL)
%Recovery
35.9 NA 31.7 NA 85.9 104
33.8 ng/mL 12%
Table 13. DAL-GW-133S
3M LIMS ID
Description
ISO13-05-05-017
DAL-GW-133S-0-131120
ISO13-05-05-018 ISO13-05-05-019
DAL-GW-133S-DB-131120 DAL-GW-133S-FMS-131120
Average Concentration (ng/mL) %RPD
PFOA
Concentration (ng/mL)
%Recovery
393 NA 399 NA 570 87.7
396 ng/mL 1.5%
PFBS
Concentration (ng/mL)
%Recovery
9.68 NA 10.2 NA 234 112
9.94 ng/mL 5.2%
PFHS
3M LIMS ID
Description
ISO13-05-05-017
DAL-GW-133S-0-131120
ISO13-05-05-018
DAL-GW-133S-DB-131120
ISO13-05-05-019
DAL-GW-133S-FMS-131120
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
70.5 NA 70.8 NA 288 108
70.7 ng/mL 0.42%
NA = Not Applicable Samples were diluted 1:10 and analyzed using external standard quantitation.
PFOS
Concentration (ng/mL)
%Recovery
251 NA 256 NA 471 109
254 ng/mL 2.0%
PAGE 15 OF 20
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
Table 14. DAL-GW-134S
3M LIMS ID
Description
ISO13-05-05-024
DAL-GW-134S-0-131120
ISO13-05-05-025
DAL-GW-134S-DB-131120
ISO13-05-05-026
DAL-GW-134S-FMS-131120
Average Concentration (ng/mL) %RPD
PFOA
Concentration (ng/mL)
%Recovery
25.8 NA 25.9 NA 35.7 NC
25.9 ng/mL 0.39%
PFBS
Concentration (ng/mL)
%Recovery
0.688
NA
0.628
NA
11.5 108
0.658 ng/mL 9.1%
PFHS
3M LIMS ID
Description
ISO13-05-05-024
DAL-GW-134S-0-131120
ISO13-05-05-025 ISO13-05-05-026
DAL-GW-134S-DB-131120 DAL-GW-134S-FMS-131120
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
7.49 NA 7.53 NA 18.3 108
7.41 ng/mL 0.53%
NA = Not Applicable NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration. Samples were diluted 1:2 and analyzed using internal standard quantitation.
PFOS
Concentration (ng/mL)
%Recovery
27.8 NA 29.1 NA 38.0 NC
28.5 ng/mL 4.6%
Table 15. DAL-GW-134L
3M LIMS ID
Description
ISO13-05-05-027
DAL-GW-134L-0-131120
ISO13-05-05-028
DAL-GW-134L-DB-131120
ISO13-05-05-029
DAL-GW-134L-FMS-131120
Average Concentration (ng/mL) %RPD
PFOA
Concentration (ng/mL)
%Recovery
536 NA
535 NA
1000
93.6
536 ng/mL 0.19%
PFBS
Concentration (ng/mL)
%Recovery
9.93 NA 10.6 NA 536 105
10.3 ng/mL 6.5%
PFHS
PFOS
3M LIMS ID
Description
ISO13-05-05-027
DAL-GW-134L-0-131120
ISO13-05-05-028
DAL-GW-134L-DB-131120
ISO13-05-05-029
DAL-GW-134L-FMS-131120
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
100 NA 97.4 NA 644 109
98.7 ng/mL 2.6%
Concentration (ng/mL)
%Recovery
515 NA
498 NA
1080
115
507 ng/mL 3.4%
NA = Not Applicable Samples were diluted 1:10 and analyzed using external standard quantitation.
PAGE 16 OF 20
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
Table 16. DAL-GW-135R
3M LIMS ID
Description
ISO13-05-05-030
DAL-GW-135R-0-131119
ISO13-05-05-031
DAL-GW-135R-DB-131119
ISO13-05-05-032
DAL-GW-135R-FMS-131119
Average Concentration (ng/mL) %RPD
PFOA
Concentration (ng/mL)
%Recovery
4060
NA
4020
NA
5530
NC
4040 ng/mL 0.99%
PFBS
Concentration (ng/mL)
%Recovery
71.8 NA
72.3 NA
2080
100
72.1 ng/mL 0.69%
PFHS
3M LIMS ID
Description
ISO13-05-05-030
DAL-GW-135R-0-131119
ISO13-05-05-031 ISO13-05-05-032
DAL-GW-135R-DB-131119 DAL-GW-135R-FMS-131119
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
812 NA
787 NA
2750
97.5
800 ng/mL 3.1%
NA = Not Applicable NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration. Samples were diluted 1:50 and analyzed using external standard quantitation.
PFOS
Concentration (ng/mL)
%Recovery
1180
NA
1210
NA
3040
92.3
1200 ng/mL 2.5%
Table 17. DAL-GW-136L
3M LIMS ID
Description
ISO13-05-05-041
DAL-GW-136L-0-131120
ISO13-05-05-042
DAL-GW-136L-DB-131120
ISO13-05-05-043
DAL-GW-136L-FMS-131120
Average Concentration (ng/mL) %RPD
PFOA
Concentration (ng/mL)
%Recovery
96.5 NA 96.7 NA 153 114
96.6 ng/mL 0.21%
PFBS
Concentration (ng/mL)
%Recovery
2.51 NA 2.52 NA 60.5 116
2.52 ng/mL 0.40%
PFHS
PFOS
3M LIMS ID
Description
ISO13-05-05-041
DAL-GW-136L-0-131120
ISO13-05-05-042
DAL-GW-136L-DB-131120
ISO13-05-05-043
DAL-GW-136L-FMS-131120
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
16.1 NA 16.0 NA 74.7 117
16.1 ng/mL 0.62%
Concentration (ng/mL)
%Recovery
97.1 NA 97.2 NA 153 112
97.2 ng/mL 0.10%
NA = Not Applicable Samples were diluted 1:10 with a larger injection volume to achieve a dilution factor o f 2 and analyzed using external standard quantitation.
PAGE 17 OF 20
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
Table 18. DAL-GW-CW26C
PFOA
3M LIMS ID
Description
ISO13-05-05-057
DAL-GW-CW26C-0-131121
ISO13-05-05-058
DAL-GW-CW26C-DB-131121
ISO13-05-05-059
DAL-GW-CW26C-FMS-131121
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
443 NA 460 NA 617 NC
452 ng/mL 3.8%
PFBS
Concentration (ng/mL)
%Recovery
8.14 NA 8.73 NA 236 114
8.44 ng/mL 7.0%
PFHS
3M LIMS ID
Description
ISO13-05-05-057 ISO13-05-05-058 ISO13-05-05-059
DAL-GW-CW26C-0-131121 DAL-GW-CW26C-DB-131121 DAL-GW-CW26C-FMS-131121
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
63.3 NA 64.6 NA 284 110
64.0 ng/mL 2.0%
PFOS
Concentration (ng/mL)
%Recovery
448 NA 462 NA 680 NC
455 ng/mL 3.1%
NA = Not Applicable NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration. Samples were diluted 1:10 and analyzed using external standard quantitation.
Table 19. DAL-GW-CW26L
3M LIMS ID
Description
ISO13-05-05-060
DAL-GW-CW26L-0-131121
ISO13-05-05-061 ISO13-05-05-062
DAL-GW-CW26L-DB-131121 DAL-GW-CW26L-FMS-131121
Average Concentration (ng/mL) %RPD
PFOA
Concentration (ng/mL)
%Recovery
897 NA
871 NA
1330
89.9
884 ng/mL 2.9%
PFBS
Concentration (ng/mL)
%Recovery
14.1 NA 14.6 NA 524 102
14.4 ng/mL 3.5%
3M LIMS ID
Description
ISO13-05-05-060
DAL-GW-CW26L-0-131121
ISO13-05-05-061
DAL-GW-CW26L-DB-131121
ISO13-05-05-062
DAL-GW-CW26L-FMS-131121
Average Concentration (ng/mL) %RPD
PFHS
Concentration (ng/mL)
%Recovery
118 NA 113 NA 622 101
116 ng/mL 4.3%
PFOS
Concentration (ng/mL)
%Recovery
1400
NA
1350
NA
2030
NC
1380 ng/mL 3.6%
NA = Not Applicable NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration. Samples were diluted 1:20 and analyzed using internal standard quantitation.
PAGE 18 OF 20
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-05
Table 20. Trip Blank
3M LIMS ID ISO13-05-05-075 ISO13-05-05-076 ISO13-05-05-077 ISO13-05-05-078
Description
DAL-GW-TRI P-0-131121 DAL-GW-TRIP-LS-131121 DAL-GW-TRIP-MS-131121 DAL-GW-TRIP-HS-131121
PFOA
Concentration (ng/mL)
<0.0480 (1) 11.1 (1) 55.0 (2) 2010 (3)
%Recovery
NA 112 111 102
PFBS
Concentration (ng/mL)
<0.0250 (1) 11.7 (1) 57.1 (2) 2200 (3)
%Recovery
NA 117 114 110
PFHS
3M LIMS ID ISO13-05-05-075 ISO13-05-05-076 ISO13-05-05-077 ISO13-05-05-078
Description
DAL-GW-TRI P-0-131121 DAL-GW-TRI P-LS-131121 DAL-GW-TRIP-MS-131121 DAL-GW-TRIP-HS-131121
Concentration (ng/mL)
<0.0250 (1) 10.9 (1) 56.4 (2) 2140 (3)
%Recovery
NA 109 113 107
NA = Not Applicable (1) Samples were diluted 1:2 and analyzed using internal standard quantitation. (2) Samples were diluted 1:10 and analyzed using external standard quantitation. (3) Samples were diluted 1:50 and analyzed using external standard quantitation.
PFOS
Concentration (ng/mL)
<0.0232 (1) 10.7 (1) 56.5 (2) 2100 (3)
%Recovery
NA 107 113 105
Table 21. Rinseate Blank
PFOA
PFBS
PFHS
PFOS
3M LIMS ID ISO13-05-05-073 ISO13-05-05-074
Description DAL-GW-145R-RB01 -131122 DAL-GW-135R-RB02131119
Concentration (ng/mL)
<0.0480 <0.0480
Concentration (ng/mL)
<0.0250 <0.0250
Concentration (ng/mL)
<0.0250 <0.0250
Concentration (ng/mL)
<0.0232 <0.0232
Samples were diluted 1:2 and analyzed using internal standard quantitation.
5 Conclusion
Laboratory control spikes were used to determine the analytical method accuracy and precision for all analytes. The accuracy and precision were then used to estimate the method uncertainty for the results. Field and laboratory matrix spike recoveries demonstrated that the analytical method was appropriate for the given sample matrix. Method ETS-8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis" was used for analysis. Analytical results are reported in Table 1 and 11-21 of this report.
PAGE 19 OF 20
3M ENVIRONMENTAL LABORATORY REPORT NO. IS013-05-05
6 Data / Sample Retention
All remaining sample and associated project data (hardcopy and electronic) will be archived according to 3M Environmental Laboratory standard operating procedures.
7 Signatures
Susan T. Wolf, 3M Principal Analytical Investigator
Date
William K. Reagen, Ph.D., 3M Environmental Technical Director
J fy tA /
Date
The 3M Environmental Laboratory's Quality Assurance Unit has audited the data and report for this project.
Quality Assurance Representative
' Date
This test report shall not be reproduced except in full, without written approval of the 3M Environmental Laboratory.
PAGE 20 OF 20
