Document M4oeGqMBed2LDqBdp68B7eRdz
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
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 2 nd Q u a r t e r 2 0 1 3
L a b o ra to ry R e q u e s t N u m b e r: IS O 1 3 -0 5 -0 2 M e th o d R e q u ire m e n t: 3 M M e th o d E T S -8 -0 4 4 .1
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
G a ry H o h e n s te in 3 M B u ild in g 2 2 4 -5 W -0 3 S a in t P a u l, M N 5 5 1 4 4 -1 0 0 0 P ho ne : (6 5 1 ) 7 3 7 -3 5 7 0
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 the A2LA Testing 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.
PAGE 1 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
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 ISO13-05-02
Analysis of PFOA, PFBS, PFHS, and PFOS in Ground Water Samples Collected at the Former Sludge Incorporation Area (FSIA) from Decatur, AL 2nd 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 June 21, June 26, June 27, June 28, July 1, July 2, and July 3, 2013 and returned to the 3M Environmental Laboratory on July 11,2013 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 ISO13-05-02.
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-138R, and DAL-GW-140R were not collected due to the well being dry or it could not be accessed.
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.
Testing Cert. # 2052.01
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 the A2LA Testing 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.
PAGE 2 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
Table 1. Sample Results Summary (1)
3M LIMS ID ISO13-05-02-001 ISO13-05-02-002
ISO13-05-02-004 ISO13-05-02-005
ISO13-05-02-007 ISO13-05-02-008
ISO13-05-02-009 ISO13-05-02-010
ISO13-05-02-011 ISO13-05-02-012
ISO13-05-02-013 ISO13-05-02-014
ISO13-05-02-015 ISO13-05-02-016
ISO13-05-02-017 ISO13-05-02-018
Sample Description
DAL-GW-130R-0-130626 DAL-GW-130R-DB-130626
Average %RPD Sample/Sample Dup DAL-GW-130S-0-130626 DAL-GW-130S-DB-130626
Average %RPD Sample/Sample Dup DAL-GW-130L-0-130626 DAL-GW-130L-DB-130626
Average %RPD Sample/Sample Dup DAL-GW-131R-0-130703 DAL-GW-131R-DB-130703
Average %RPD Sample/Sample Dup DAL-GW-131S-0-130703 DAL-GW-131S-DB-130703
Average %RPD Sample/Sample Dup DAL-GW-131L-0-130703 DAL-GW-131L-DB-130703
Average %RPD Sample/Sample Dup DAL-GW-133R-0-130703 DAL-GW-133R-DB-130703
Average %RPD Sample/Sample Dup DAL-GW-133S-0-130703 DAL-GW-133S-DB-130703
Average %RPD Sample/Sample Dup
PFOA Concentration
(ng/mL)
881 1000 941 (2)
13 190 186 188 2.1 63.0 61.9 62.5 1.8 2460 2290 2380 7.2 27.0 24.2 25.6 (3) 11 105 106 106 0.95 52.6 53.2 52.9 1.1 379 379 379 0.0
PFBS Concentration
(ng/mL)
15.0 17.6 16.3 16 3.55 3.37 3.46 5.2 1.43 1.37 1.40 4.3 57.1 53.4 55.3 6.7 0.957 0.765 0.861 (3) 22 (4) 3.22 3.37 3.30 4.6 2.63 2.61 2.62 0.76 9.11 9.40 9.26 3.1
PFHS Concentration
(ng/mL)
122 141 132 14 31.3 30.6 31.0 2.3 11.6 11.7 11.7 0.86 330 317 324 4.0 5.70 4.75 5.23 (3) 18 22.4 22.2 22.3 0.90 15.5 15.6 15.6 0.64 70.8 72.6 71.7 2.5
PFOS Concentration
(ng/mL)
524 600 562 14 142 143 143 0.70 70.9 69.8 70.4 1.6 1440 1360 1400 5.7 5.88 5.39 5.64 (3) 8.7 42.3 44.6 43.5 5.3 29.0 29.0 29.0 0.0 307 306 307 0.33
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 21 %, PFBS 13%, PFHS 14%, and PFOS 16%. (2) The analytical method uncertainty has been expanded to 32% for PFOA. See section 4 for further discussion. (3) 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 11%, PFBS 12%, PFHS 12%, and PFOS 12%. (4) The RPD value did not meet method acceptance criteria of <20%. (5) The analytical method uncertainty has been expanded to 39% for PFOA. See section 4 for further discussion. (6) The analytical method uncertainty has been expanded to 31 % for PFHS. See section 4 for further discussion.
PAGE 3 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
Table 1 continued. Sample Results Summary (1)
3M LIMS ID ISO13-05-02-019 ISO13-05-02-020
ISO13-05-02-021 ISO13-05-02-022
ISO13-05-02-024 ISO13-05-02-025
ISO13-05-02-027 ISO13-05-02-028
ISO13-05-02-029 ISO13-05-02-030
ISO13-05-02-031 ISO13-05-02-032
ISO13-05-02-034 ISO13-05-02-035
ISO13-05-02-039 ISO13-05-02-040
Sample Description
DAL-GW-133L-0-130703 DAL-GW-133L-DB-130703
Average %RPD Sample/Sample Dup DAL-GW-134R-0-130626 DAL-GW-134R-DB-130626
Average %RPD Sample/Sample Dup DAL-GW-134S-0-130626 DAL-GW-134S-DB-130626
Average %RPD Sample/Sample Dup DAL-GW-134L-0-130626 DAL-GW-134L-DB-130626
Average %RPD Sample/Sample Dup DAL-GW-135R-0-130703 DAL-GW-135R-DB-130703
Average %RPD Sample/Sample Dup DAL-GW-135S-0-130703 DAL-GW-135S-DB-130703
Average %RPD Sample/Sample Dup DAL-GW-135L-0-130703 DAL-GW-135L-DB-130703
Average %RPD Sample/Sample Dup DAL-GW-136S-0-130628 DAL-GW-136S-DB-130628
Average %RPD Sample/Sample Dup
PFOA Concentration
(ng/mL)
694 658 676 5.3 1920 1920 1920 0.0 15.8 15.3 15.6 (3,5) 3.2 507 502 505 0.99 3510 3420 3470 2.6 40.5 40.2 40.4 0.74 574 592 583 3.1 103 105 104 1.9
PFBS Concentration
(ng/mL)
13.2 12.9 13.1 2.3 49.7 49.7 49.7 0.0 0.384 0.395 0.390 (3) 2.8 9.86 9.84 9.85 0.20 62.1 59.5 60.8 4.3 1.79 1.65 1.72 (3) 8.1 15.1 14.9 15.0 1.3 2.59 2.78 2.69 7.1
PFHS Concentration
(ng/mL)
110 108 109 1.8 480 483 482 0.62 4.41 4.56 4.49 (3) 3.3 97.0 97.3 97.2 0.31 746 727 737 2.6 16.0 14.3 15.2 ft6) 11 130 128 129 1.6 19.0 19.4 19.2 2.1
PFOS Concentration
(ng/mL)
746 730 738 2.2 1280 1270 1280 0.78 17.5 17.5 17.5 (3) 0.0 521 522 522 0.19 1180 1120 1150 5.2 12.8 10.7 11.8 (3) 18 147 156 152 5.9 118 122 120 3.3
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 21 %, PFBS 13%, PFHS 14%, and PFOS 16%. (2) The analytical method uncertainty has been expanded to 32% for PFOA. See section 4 for further discussion. (3) 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 11%, PFBS 12%, PFHS 12%, and PFOS 12%. (4) The RPD value did not meet method acceptance criteria of <20%. (5) The analytical method uncertainty has been expanded to 39% for PFOA. See section 4 for further discussion. (6) The analytical method uncertainty has been expanded to 31 % for PFHS. See section 4 for further discussion.
PAGE 4 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
Table 1 continued. Sample Results Summary (1)
3M LIMS ID ISO13-05-02-041 ISO13-05-02-042
ISO13-05-02-045 ISO13-05-02-046
ISO13-05-02-047 ISO13-05-02-048
ISO13-05-02-052 ISO13-05-02-053
ISO13-05-02-054 ISO13-05-02-055
ISO13-05-02-057 ISO13-05-02-058
ISO13-05-02-059 ISO13-05-02-060
ISO13-05-02-064 ISO13-05-02-065
Sample Description
DAL-GW-136L-0-130628 DAL-GW-136L-DB-130628
Average %RPD Sample/Sample Dup DAL-GW-137S-0-130627 DAL-GW-137S-DB-130627
Average %RPD Sample/Sample Dup DAL-GW-137L-0-130626 DAL-GW-137L-DB-130626
Average %RPD Sample/Sample Dup DAL-GW-138S-0-130628 DAL-GW-138S-DB-130628
Average %RPD Sample/Sample Dup DAL-GW-138L-0-130628 DAL-GW-138L-DB-130628
Average %RPD Sample/Sample Dup DAL-GW-CW26C-0-130628 DAL-GW-CW26C-DB-130628
Average %RPD Sample/Sample Dup DAL-GW-CW26L-0-130628 DAL-GW-CW26L-DB-130628
Average %RPD Sample/Sample Dup DAL-GW-141R-0-130702 DAL-GW-141R-DB-130702
Average %RPD Sample/Sample Dup
PFOA Concentration
(ng/mL)
90.0 90.4 90.2 0.44 0.346 0.346 0.346 (3) 0.0 0.355 0.384 0.370 (3) 7.8 174 175 175 0.57 1.21 1.10 1.16 (3) 9.5 411 407 409 0.98 665 642 654 3.5 1.88 2.16 2.02 (3) 14
PFBS Concentration
(ng/mL)
2.27 2.27 2.27 0.0 0.115 0.107 0.111 (3) 7.2 0.0775 0.0725 0.0750 (3) 6.7 4.86 4.90 4.88 0.82 0.0529 0.0433 0.0481 (3) 20 7.39 7.60 7.50 2.8 13.0 12.1 12.6 7.2 0.0519 0.0499 0.0509 (3) 3.9
PFHS Concentration
(ng/mL)
15.6 16.2 15.9 3.8 0.0865 0.0983 0.0924 (3) 13 0.0906 0.0871 0.0889 (3) 3.9 23.6 23.7 23.7 0.42 0.139 0.159 0.149 (3) 13 59.9 61.5 60.7 2.6 99.3 97.0 98.2 2.3 0.334 0.321 0.328 (3) 4.0
PFOS Concentration
(ng/mL)
95.4 92.3 93.9 3.3 0.523 0.530 0.527 (3) 1.3 1.17 1.21 1.19 (3) 3.4 236 237 237 0.42 0.638 0.687 0.663 (3) 7.4 408 428 418 4.8 969 924 947 4.8 5.42 5.11 5.27 (3) 5.9
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 21 %, PFBS 13%, PFHS 14%, and PFOS 16%. (2) The analytical method uncertainty has been expanded to 32% for PFOA. See section 4 for further discussion. (3) 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 11%, PFBS 12%, PFHS 12%, and PFOS 12%. (4) The RPD value did not meet method acceptance criteria of <20%. (5) The analytical method uncertainty has been expanded to 39% for PFOA. See section 4 for further discussion. (6) The analytical method uncertainty has been expanded to 31 % for PFHS. See section 4 for further discussion.
PAGE 5 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
Table 1 continued. Sample Results Summary (1)
3M LIMS ID ISO13-05-02-066 ISO13-05-02-067
ISO13-05-02-068 ISO13-05-02-069
ISO13-05-02-070 ISO13-05-02-071
Sample Description
DAL-GW-142R-0-130628 DAL-GW-142R-DB-130628
Average %RPD Sample/Sample Dup DAL-GW-143R-0-130621 DAL-GW-143R-DB-130621
Average %RPD Sample/Sample Dup DAL-GW-145R-0-130701 DAL-GW-145R-DB-130701
Average %RPD Sample/Sample Dup
PFOA Concentration
(ng/mL)
68.3 67.0 67.7 1.9 35.3 36.0 35.7 2.0 74.3 75.3 74.8 1.3
PFBS Concentration
(ng/mL)
2.27 2.29 2.28 0.88 1.73 1.61 1.67 7.2 1.98 1.98 1.98 0.0
PFHS Concentration
(ng/mL)
13.6 12.9 13.3 5.3 6.93 6.53 6.73 5.9 9.45 9.65 9.55 2.1
PFOS Concentration
(ng/mL)
162 170 166 4.8 24.3 26.0 25.2 6.8 135 141 138 4.3
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 21 %, PFBS 13%, PFHS 14%, and PFOS 16%. (2) The analytical method uncertainty has been expanded to 32% for PFOA. See section 4 for further discussion. (3) 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 11%, PFBS 12%, PFHS 12%, and PFOS 12%. (4) The RPD value did not meet method acceptance criteria of <20%. (5) The analytical method uncertainty has been expanded to 39% for PFOA. See section 4 for further discussion. (6) The analytical method uncertainty has been expanded to 31 % for PFHS. See section 4 for further discussion.
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 June 21, June 26, June 27, June 28, July 1, July 2, and July 3, 2013 and returned to the 3M Environmental Laboratory on July 11,2013 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.
PAGE 6 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
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-130626
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 130626 - June 26, 2013
2.3 Sample Preparation
7/15/13 and 8/20/13: 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.
7/19/13: All samples were prepared by removing a 0.75 mL aliquot of the well mixed sample and diluting it with 0.75 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:
7/16/13: Solvent dilution / external standard analysis for PFOA, PFBS, PFHS, PFOS (samples extracted 7/15/13); locations 130R, 130S, 130L, 131R, 131L, 133R, 133S, 133L, 134R, 134L, 135R, 135L, 136S, 136L, 138S, CW26C, CW26L, 142R, 143R, 145R, Trip Blank mid and high FMS.
7/19/13: Direct injection / internal standard analysis for PFOA, PFBS, PFHS, PFOS (samples extracted 7/19/13); locations 131S, 134S, 135S, 137S, 137L, 138L, 141R, rinseate blanks, trip blank and trip blank low FMS.
7/20/13: Solvent dilution / external standard analysis for PFHS (samples prepared on 7/15/13); Trip Blank high FMS.
8/21/13: Solvent dilution/external standard analysis for PFOA (samples prepared on 8/20/13); locations 135S and 135L.
PAGE 7 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
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 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 7/16/13, 7/19/13, 7/20/13, 8/21/13
ETS-8-044.1 Agilent 1100 Betasil C18 (4.6 mm X 100 mm), 5 g Betasil C18 (4.6 mm X 100 mm), 5 g 2, 5, 10, 20, 25, ijL 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 (pL/min)
750 750 750 750 750 750 750 750 750 750
2 mM Ammonium Acetate 90.0 90.0 70.0 70.0 20.0 20.0 10.0 10.0 90.0 90.0
Methanol 10.0 10.0 30.0 30.0 80.0 80.0 90.0 90.0 10.0 10.0
PAGE 8 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
Table 6. Mass Transitions
Analyte
Mass Transition Q1/Q3
Internal Standard
Mass Transition Q1/Q3
Reference Material Structure
PFOA
413/369 413/219
[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
[13Cb]PFHS (1)
402/99
Linear
PFOS
499/99 499/80
[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 7/19/13.
3 Data Analysis
3.1 Calibration
7/16/13, 7/20/13, and 8/21/13: 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.
7/19/13: 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 thirteen curve points were analyzed with the samples ranging from 0.0125 ng/mL to 50 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.
PAGE 9 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
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
7/16/13
External standard
7/19/13 7/20/13
8/21/13
Internal standard External standard
External standard
Dilution Factor
2 5 10 20 50 2 25 10 50
PFOA LOQ, ng/mL
0.192 0.479 0.958 1.92 4.79 0.0240
NA 0.958 4.79
PFBS LOQ, ng/mL
0.200 0.500 1.00 2.00 5.00 0.0250
NA NA NA
PFHS LOQ, ng/mL
0.500 1.25 2.50 5.00 12.5 0.0250 2.50 NA NA
PFOS LOQ, ng/mL
0.464 1.16 2.32 4.64 11.6 0.0232 NA NA NA
NA=Not Applicable
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:
7/16/13 analysis: The acceptance criteria for accuracy were met with the exception of the mid set of LCS for PFOA (121%).
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
%
PAGE 10 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
,LCS% ,,R,,S,,D = -s--ta--n--d--a--r-d--d--e--v-i-a--t-i-o-n---L--C--S---r-e- p- -li-c--a--te--s- **100% average LCS recovery
Table 8. Lab Control Spike Results
ETS-8-044.1 Analyzed 7/16/13 External Standard Calibration
Lab ID LCS-130715-1 LCS-130715-2 LCS-130715-3 Average %RSD LCS-130715-4 LCS-130715-5 LCS-130715-6 Average %RSD LCS-130715-7 LCS-130715-8 LCS-130715-9 Average %RSD
PFOA (Linear and Branched)
Spiked Concentration
(ng/mL)
Calculated Concentration
(ng/mL)
%Recovery
0.958 0.958 0.958
9.58 9.58 9.58
38.2 38.2 38.2
1.05 1.04 1.00 107% 2.7% 11.4 11.7 11.8 121% 1.7% (1) 37.2 41.4 41.0 104% 5.6%
109 109 104
119 122 123
97.5 108 107
Spiked Concentration
(ng/mL) 1.00 1.00 1.00
10.0 10.0 10.0
39.8 39.8 39.8
PFBS Calculated Concentration
(ng/mL)
1.06 1.07 1.03 105% 2.0% 11.2 11.6 11.3 114% 1.8% 37.3 41.0 41.3 100% 5.7%
%Recovery 106 107 103
112 116 113
93.7 103 104
ETS-8-044.1 Analyzed 7/16/13 External Standard Calibration
Lab ID LCS-130715-1 LCS-130715-2 LCS-130715-3 Average %RSD LCS-130715-4 LCS-130715-5 LCS-130715-6 Average %RSD LCS-130715-7 LCS-130715-8 LCS-130715-9 Average %RSD
Spiked Concentration
(ng/mL) 1.00 1.00 1.00
10.0 10.0 10.0
39.8 39.8 39.8
PFHS Calculated Concentration
(ng/mL)
1.03 1.00 1.04 102% 2.0% 11.6 11.9 11.8 118% 1.3% 38.2 40.8 42.2 102% 5.1%
%Recovery 103 100 104
116 119 118
95.9 103 106
PFOS (Linear and Branched)
Spiked Concentration
(ng/mL)
Calculated Concentration
(ng/mL)
%Recovery
0.927 0.927 0.927
9.27 9.27 9.27
36.9 36.9 36.9
0.932 0.980 0.929 102% 3.1% 10.7 11.0 10.6 116% 1.5% 35.2 39.2 40.2 103% 7.0%
101 106 100
115 118 115
95.3 106 109
(1) Average LCS recovery did not meet method acceptance criteria of 100 20%.
PAGE 11 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
Table 8 continued. Lab Control Spike Results
ETS-8-044.1 Analyzed 7/19/13 Internal Standard Calibration
Lab ID
LCS-130719-1 LCS-130719-2 LCS-130719-3 Average %RSD LCS-130719-4 LCS-130719-5 LCS-130719-6 Average %RSD LCS-130719-7 LCS-130719-8 LCS-130719-9 Average %RSD
PFOA (Linear and Branched)
Spiked Concentration
(ng/mL)
Calculated Concentration
(ng/mL)
%Recovery
0.190 0.190 0.190
1.90 1.90 1.90
19.0 19.0 19.0
0.172 0.168 0.162 88.1% 2.7% 1.84 1.72 1.64 91.3% 5.8% 15.4 15.9 16.1 83.2% 2.2%
90.3 88.4 85.5
97.0 90.5 86.5
81.1 83.9 84.5
Spiked Concentration
(ng/mL) 0.199 0.199 0.199
1.99 1.99 1.99
19.9 19.9 19.9
PFBS Calculated Concentration
(ng/mL)
0.178 0.168 0.184 88.6% 4.4% 1.93 2.02 1.80 96.2% 5.5% 16.1 16.5 16.4 82.1% 1.3%
%Recovery 89.2 84.5 92.2
97.0 101 90.6
80.9 82.9 82.6
ETS-8-044.1 Analyzed 7/19/13 Internal Standard Calibration
Lab ID
LCS-130719-1 LCS-130719-2 LCS-130719-3 Average %RSD LCS-130719-4 LCS-130719-5 LCS-130719-6 Average %RSD LCS-130719-7 LCS-130719-8 LCS-130719-9 Average %RSD
Spiked Concentration
(ng/mL) 0.199 0.199 0.199
1.99 1.99 1.99
19.9 19.9 19.9
PFHS Calculated Concentration
(ng/mL)
0.188 0.184 0.166 90.1% 6.6% 1.95 2.10 1.90 99.5% 4.9% 16.1 16.4 17.1 83.1% 3.2%
%Recovery 94.3 92.6 83.3
98.0 105 95.5
81.0 82.3 86.1
PFOS (Linear and Branched)
Spiked Concentration
(ng/mL)
Calculated Concentration
(ng/mL)
%Recovery
0.184 0.184 0.184
1.84 1.84 1.84
18.4 18.4 18.4
0.176 0.171 0.180 95.5% 2.4% 1.76 1.82 1.78 97.2% 1.5% 15.4 16.3 15.7 85.7% 2.7%
95.7 93.1 97.6
95.9 98.8 96.8
83.6 88.4 85.1
PAGE 12 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
Table 8 continued. Lab Control Spike Results
ETS-8-044.1 Analyzed 8/21/13 External Standard Calibration
Lab ID LCS-130820-1 LCS-130820-2 LCS-130820-3 Average %RSD LCS-130820-4 LCS-130820-5 LCS-130820-6 Average %RSD LCS-130820-7 LCS-130820-8 LCS-130820-9 Average %RSD
PFOA (Linear and Branched)
Spiked Concentration
(ng/mL)
Calculated Concentration
(ng/mL)
%Recovery
0.958 0.958 0.958
9.58 9.58 9.58
38.2 38.2 38.2
0.830 0.917 0.900 92.1% 5.3% 10.0 10.1 10.3 105% 1.5% 39.3 39.8 40.9 105% 2.0%
86.6 95.7 94.0
104 105 107
103 104 107
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 PFOA by external standard calibration was 15%. However, the recovery of the mid set of LCS analyzed on 7/16/13 was 121% for PFOA by external standard calibration for the samples analyzed on this date. Therefore, the analytical method uncertainty was expanded for samples analyzed by external standard calibration for PFOA to 21%.
Table 9. Analytical Method Uncertainty
Analyte PFOA PFBS PFHS PFOS PFOA PFBS PFHS PFOS
Calibration External External External External Internal Internal Internal Internal
NA = Not Applicable
Standard Deviation (%) NA 6.42 7.13 8.24 5.28 6.08 5.98 6.16
Method Uncertainty 21% 13% 14% 16% 11% 12% 12% 12%
PAGE 13 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
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.
An appropriate field matrix spike was not available for PFOA for sampling locations 135S and 135L; therefore, a laboratory matrix spike was prepared on the primary sample to verify that the method was appropriate for these two locations.
Field matrix spikes are presented in section 4 of this report.
FMS Recovery - (Sample Concentration of FMS - Average Concentration: Field Sample & Field Sample Dup.) * 1 qq% Spike Concentraton
Table 10. Field Matrix Spike (FMS) and Lab Matrix Spike (LMS) Concentrations
Sampling location 137L and 138L 134S and 135S 130S, 135L, and 140R 130R 134R
Trip Blank
ISO13-05-02-031 (135S) ISO13-05-02-034 (135L)
Spike Level FMS FMS FMS FMS FMS FMS Low FMS Mid FMS High LMS LMS
PFOA ng/mL
1.00 20.0 100 501 1002 1.00 100 1002 99.0 1000
PFBS ng/mL
1.00 20.1 100 502 1004 1.00 100 1004 NA NA
PFHS ng/mL 0.999
20.0 99.8 499 998 0.999 99.8 998 NA NA
PFOS ng/mL
1.00 19.9 99.4 497 994 1.00 99.4 994 NA NA
4 Data Summary and Discussion
Tables 11-20 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.
PAGE 14 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
All target analyte field matrix spikes met method acceptance criteria with the following exceptions:
DAL-GW-130R; The FMS recovery for PFOA was 67.8%. The analytical uncertainty for this location was expanded to 32%.
DAL-GW-134S; The FMS recovery for PFOA was 60.6%. The analytical uncertainty for this location was expanded to 39%.
DAL-GW-135S; The FMS recovery for PFHS was 69.4%. The analytical uncertainty for this location was expanded to 31%.
An appropriate field matrix spike was not available for PFOA for sampling locations DAL GW 135S and DAL GW 135L; therefore, a laboratory matrix spike was prepared on the primary sample to verify that the method was appropriate for these two locations. The laboratory matrix spike recoveries met method acceptance criteria.
Table 11. DAL-GW-130R
3M LIMS ID
Description
ISO13-05-02-001
DAL-GW-130R-0-130626
ISO13-05-02-002
DAL-GW-130R-DB-130626
ISO13-05-02-003
DAL-GW-130R-FMS-130626
Average Concentration (ng/mL) %RPD
PFOA
Concentration (ng/mL)
%Recovery
881 NA
1000
NA
1280
67.8 (1)
941 ng/mL 13% (1)
PFBS
Concentration (ng/mL)
%Recovery
15.0 NA 17.6 NA 527 102
16.3 ng/mL 16%
PFHS
PFOS
3M LIMS ID
Description
ISO13-05-02-001
DAL-GW-130R-0-130626
ISO13-05-02-002
DAL-GW-130R-DB-130626
ISO13-05-02-003
DAL-GW-130R-FMS-130626
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
122 NA 141 NA 661 106
132 ng/mL 14%
Concentration (ng/mL)
%Recovery
524 NA
600 NA
1090
106
562 ng/mL 14%
NA = Not Applicable Samples were diluted 1:20 and analyzed using external standard quantitation. (1) FMS did not meet method acceptance criteria of 30. The analytical uncertainty was expanded to 32%.
PAGE 15 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
Table 12. DAL-GW-130S
3M LIMS ID
Description
ISO13-05-02-004
DAL-GW-130S-0-130626
ISO13-05-02-005
DAL-GW-130S-DB-130626
ISO13-05-02-006
DAL-GW-130S-FMS-130626
Average Concentration (ng/mL) %RPD
PFOA
Concentration (ng/mL)
%Recovery
190 NA 186 NA 273 84.8
188 ng/mL 2.1%
PFBS
Concentration (ng/mL)
%Recovery
3.55 NA 3.37 NA 103 99.1
3.46 ng/mL 5.2%
PFHS
3M LIMS ID
Description
ISO13-05-02-004
DAL-GW-130S-0-130626
ISO13-05-02-005
DAL-GW-130S-DB-130626
ISO13-05-02-006
DAL-GW-130S-FMS-130626
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
31.3 NA 30.6 NA 136 105
31.0 ng/mL 2.3%
NA = Not Applicable Samples were diluted 1:10 and analyzed using external standard quantitation.
PFOS
Concentration (ng/mL)
%Recovery
142 NA 143 NA 248 106
143 ng/mL 0.70%
Table 13. DAL-GW-134R
3M LIMS ID
Description
ISO13-05-02-021
DAL-GW-134R-0-130626
ISO13-05-02-022
DAL-GW-134R-DB-130626
ISO13-05-02-023
DAL-GW-134R-FMS-130626
Average Concentration (ng/mL) %RPD
PFOA
Concentration (ng/mL)
%Recovery
1920
NA
1920
NA
2620
69.9
1920 ng/mL 0.0%
PFBS
Concentration (ng/mL)
%Recovery
49.7 NA 49.7 NA 825 77.2
49.7 ng/mL 0.0%
PFHS
3M LIMS ID
Description
ISO13-05-02-021
DAL-GW-134R-0-130626
ISO13-05-02-022
DAL-GW-134R-DB-130626
ISO13-05-02-023
DAL-GW-134R-FMS-130626
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
480 NA
483 NA
1320
84.0
482 ng/mL 0.62%
NA = Not Applicable Samples were diluted 1:20 and analyzed using external standard quantitation.
PFOS
Concentration (ng/mL)
%Recovery
1280
NA
1270
NA
2210
94.1
1280 ng/mL 0.78%
PAGE 16 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
Table 14. DAL-GW-134S
3M LIMS ID
Description
ISO13-05-02-024
DAL-GW-134S-0-130626
ISO13-05-02-025
DAL-GW-134S-DB-130626
ISO13-05-02-026
DAL-GW-134S-FMS-130626
Average Concentration (ng/mL) %RPD
PFOA
Concentration (ng/mL)
%Recovery
15.8 NA 15.3 NA 27.7 60.6 (1) 15.6 ng/mL 3.2% (1)
PFBS
Concentration (ng/mL)
%Recovery
0.384
NA
0.395
NA
15.4 74.8
0.390 ng/mL 2.8%
PFHS
PFOS
3M LIMS ID
Description
ISO13-05-02-024
DAL-GW-134S-0-130626
ISO13-05-02-025 ISO13-05-02-026
DAL-GW-134S-DB-130626 DAL-GW-134S-FMS-130626
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
4.41 NA 4.56 NA 19.5 75.2
4.49 ng/mL 3.3%
Concentration (ng/mL)
%Recovery
17.5 NA 17.5 NA 33.2 79.0
17.5 ng/mL 0.0%
NA = Not Applicable Samples were diluted 1:2 and analyzed using internal standard quantitation. (1) FMS did not meet method acceptance criteria of 30. The analytical uncertainty was expanded to 39%.
Table 15. DAL-GW-135S
3M LIMS ID
Description
ISO13-05-02-031
DAL-GW-135S-0-130703
ISO13-05-02-032
DAL-GW-135S-DB-130703
ISO13-05-02-033
DAL-GW-135S-FMS-130703
ISO13-05-02-031 LMS
DAL-GW-135S-0-130703 LMS
Average Concentration (ng/mL) %RPD
PFOA (1)
Concentration (ng/mL)
%Recovery
40.5 NA 40.2 NA NA NA 137 97.6
40.4 ng/mL 0.74%
PFBS (2)
Concentration (ng/mL)
%Recovery
1.79 NA 1.65 NA 16.5 73.6 NA NA
1.72 ng/mL 8.1%
PFHS (2)
PFOS (2)
3M LIMS ID
Description
ISO13-05-02-031
DAL-GW-135S-0-130703
ISO13-05-02-032
DAL-GW-135S-DB-130703
ISO13-05-02-033
DAL-GW-135S-FMS-130703
ISO13-05-02-031 LMS
DAL-GW-135S-0-130703 LMS
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
16.0 NA 14.3 NA 29.0 69.4 (3) NA NA 15.2 ng/mL 11% (3)
Concentration (ng/mL)
%Recovery
12.8 NA 10.7 NA 26.5 74.2 NA NA
11.8 ng/mL 18%
NA = Not Applicable (1) Samples were diluted 1:10 and analyzed using external standard quantitation. (2) Samples were diluted 1:2 and analyzed using internal standard quantitation. (3) FMS did not meet method acceptance criteria of 30. The analytical uncertainty was expanded to 31%.
PAGE 17 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
Table 16. DAL-GW-135L
3M LIMS ID
Description
ISO13-05-02-034
DAL-GW-135L-0-130703
ISO13-05-02-035
DAL-GW-135L-DB-130703
ISO13-05-02-036
DAL-GW-135L-FMS-130703
ISO13-05-02-034 LMS
DAL-GW-135L-0-130703 LMS
Average Concentration (ng/mL) %RPD
PFOA (1)
Concentration (ng/mL)
%Recovery
574 NA
592 NA
NA NA
1510
92.7
583 ng/mL 3.1%
PFBS (2)
Concentration (ng/mL)
%Recovery
15.1 NA 14.9 NA 114 98.6 NA NA
15.0 ng/mL 1.3%
PFHS (2)
3M LIMS ID
Description
ISO13-05-02-034
DAL-GW-135L-0-130703
ISO13-05-02-035
DAL-GW-135L-DB-130703
ISO13-05-02-036
DAL-GW-135L-FMS-130703
ISO13-05-02-034 LMS
DAL-GW-135L-0-130703 LMS
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
130 NA 128 NA 229 100 NA NA
129 ng/mL 1.6%
NA = Not Applicable NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration. (1) Samples were diluted 1:50 and analyzed using external standard quantitation. (2) Samples were diluted 1:10 and analyzed using external standard quantitation.
PFOS (2)
Concentration (ng/mL)
%Recovery
147 NA 156 NA 250 99.1 NA NA
152 ng/mL 5.9%
Table 17. DAL-GW-137L
3M LIMS ID
Description
ISO13-05-02-047
DAL-GW-137L-0-130626
ISO13-05-02-048
DAL-GW-137L-DB-130626
ISO13-05-02-049
DAL-GW-137L-FMS-130626
Average Concentration (ng/mL) %RPD
PFOA
Concentration (ng/mL)
%Recovery
0.355
NA
0.384
NA
1.13 76.1
0.370 ng/mL 7.8%
PFBS
Concentration (ng/mL)
%Recovery
0.0775
NA
0.0725
NA
0.897
82.2
0.0750 ng/mL 6.7%
PFHS
3M LIMS ID
Description
ISO13-05-02-047
DAL-GW-137L-0-130626
ISO13-05-02-048
DAL-GW-137L-DB-130626
ISO13-05-02-049
DAL-GW-137L-FMS-130626
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
0.0906
NA
0.0671
NA
0.982
89.4
0.0889 ng/mL 3.9%
NA = Not Applicable Samples were diluted 1:2 and analyzed using internal standard quantitation.
PFOS
Concentration (ng/mL)
%Recovery
1.17 NA 1.21 NA 2.06 87.0
1.19 ng/mL 3.4%
PAGE 18 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
Table 18. DAL-GW-138L
3M LIMS ID
Description
ISO13-05-02-054
DAL-GW-138L-0-130628
ISO13-05-02-055
DAL-GW-138L-DB-130628
ISO13-05-02-056
DAL-GW-138L-FMS-130628
Average Concentration (ng/mL) %RPD
PFOA
Concentration (ng/mL)
%Recovery
1.21 NA 1.10 NA 1.89 73.5
1.16 ng/mL 9.5%
PFBS
Concentration (ng/mL)
%Recovery
0.0529
NA
0.0433
NA
0.872
82.4
0.0481 ng/mL 20%
PFHS
3M LIMS ID
Description
ISO13-05-02-054
DAL-GW-138L-0-130628
ISO13-05-02-055
DAL-GW-138L-DB-130628
ISO13-05-02-056
DAL-GW-138L-FMS-130628
Average Concentration (ng/mL) %RPD
Concentration (ng/mL)
%Recovery
0.139
NA
0.159
NA
1.01 86.2
0.149 ng/mL 13%
NA = Not Applicable Samples were diluted 1:2 and analyzed using internal standard quantitation.
PFOS
Concentration (ng/mL)
%Recovery
0.638
NA
0.687
NA
1.51 84.8
0.663 ng/mL 7.4%
Table 19. Trip Blank
3M LIMS ID
ISO13-05-02-074 ISO13-05-02-075 ISO13-05-02-076 ISO13-05-02-077
Description
DAL-GW-TRIP-0DAL-GW-TRIP-LSDAL-GW-TRIP-MSDAL-GW-TRIP-HS-
PFOA
Concentration (ng/mL)
<0.0240 (1) 0.757 (1) 92.4 (2) 774 (2)
%Recovery
NA 75.7 92.2 77.2
PFBS
Concentration (ng/mL)
<0.0250 (1) 0.819 (1) 109 (2) 931 (2)
%Recovery
NA 81.9 109 92.7
PFHS
3M LIMS ID
ISO13-05-02-074 ISO13-05-02-075 ISO13-05-02-076 ISO13-05-02-077
Description
DAL-GW-TRIP-0DAL-GW-TRIP-LSDAL-GW-TRIP-MSDAL-GW-TRIP-HS-
Concentration (ng/mL)
<0.0250 (1) 0.877 (1) 105 (2) 976 (2)
%Recovery
NA 87.8 105 97.8
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.
PFOS
Concentration (ng/mL)
<0.0232 (1) 0.745 (1) 101 (2) 1000 (2)
%Recovery
NA 74.5 102 101
PAGE 19 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-05-02
Table 20. Rinseate Blank
PFOA
PFBS
PFHS
PFOS
3M LIMS ID ISO13-05-02-072 ISO13-05-02-073
Description DAL-GW-141R-RB-130702 DAL-GW-130S-RB-130626
Concentration (ng/mL)
<0.0240
<0.0240
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 11-20 of this report.
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.
PAGE 20 OF 21
7 Signatures
3M ENVIRONMENTAL LABORATORY REPORT NO. IS013-05-02
The 3M Environmental Laboratory's Quality Assurance Unit has audited the data and report for this project.
Quality Assurarjpe Representative
Date
This test report shall not be reproduced except in full, without written approval of the 3M Environmental Laboratory.
PAGE 21 OF 21
