Document G66oJYyRoGDzKgGD31qkED5yn
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Final Report
Analysis of PFOA, PFBS, PFHS, and PFOS in Aqueous Samples from 3M Decatur, Alabama: Groundwater Treatment Plant GAC System December 2013
Laboratory Request Number: ISO13-07-11 Method Requirement: 3M Method ETS-8-044.1
Report Date - Date of Last Signature
Testing Laboratory 3M EHS&S Operations 3M Environmental Laboratory
Building 260-5N-17 Maplewood, MN 55144-1000
Requester Gary Hohenstein 3M Building 224-5W-03 Saint Paul, MN 55144-1000 Phone: (651) 737-3570
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 A2LA assessment.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
3M Environmental Laboratory
3M Environmental Laboratory Technical Director: William K. Reagen, Ph.D. 3M Principal Analytical Investigator: Susan Wolf Report Author: Chelsie Grochow
Analytical Report ISO13-07-11
3M Decatur Groundwater Treatment Plant System; December 2013 Sampling
Report Date: Date of Last Signature
1 Introduction/Summary
The 3M Environmental Laboratory analyzed water samples from the groundwater treatment plant GAC system at the 3M Decatur, AL facility. Water samples were collected by Weston Solutions personnel on December 13, 2013. Samples were returned to the 3M Environmental Laboratory for analysis of Perfluorooctanoate (PFOA), Perfluorobutane sulfonate (PFBS), Perfluorohexane sulfonate (PFHS), Perfluorooctane sulfonate (PFOS) under laboratory project number ISO13-07-11. Analysis of the samples was completed as specified under 3M Environmental Laboratory General Project Outline (GPO) number GPO11-1006.
The 3M Environmental Laboratory provided sample containers for seven sampling locations; ACI, ACM2, ACE, WW8R, WW9R, WW10R, and WW11R. The sample set consisted of a field sample, field sample duplicate and a field matrix spike. Each empty container was marked with a "fill to here" line that corresponded to a final volume of 200 mL. Containers reserved for field matrix spikes were fortified with an appropriate matrix spike solution containing all analytes prior to being sent to the field for sample collection. Sample bottles for sampling locations ACM2 and ACE, along with the Trip Blank sample and low spike, were fortified with internal standards and surrogates prior to being sent to the field for sample collection. Due to an error during the bottle prep, internal standard was not added to the ACE FMS sample prior to analysis.
Samples were prepared and analyzed by method ETS-8-044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis". Select internal standards were used to aid in the data quality objectives.
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 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 A2LA assessment.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Table 1. Sample Results Summary
3M LIMS ID
Sample Description
ISO13-07-11-001 ISO13-07-11-002
ISO13-07-11-004 ISO13-07-11-005
ISO13-07-11-007 ISO13-07-11-008
ISO13-07-11-010 ISO13-07-11-011
ISO13-07-11-013 ISO13-07-11-014
ISO13-07-11-019 ISO13-07-11-020
ISO13-07-11-022 ISO13-07-11-023
DAL-GW-ACI; Sample DAL-GW-ACI; Sample Dup
Average %RPD Sample/Sample Dup DAL-GW-ACM2; Sample DAL-GW-ACM2; Sample Dup
Average %RPD Sample/Sample Dup DAL-GW-ACE; Sample DAL-GW-ACE; Sample Dup
Average %RPD Sample/Sample Dup DAL-GW-WW8R; Sample DAL-GW-WW8R; Sample Dup
Average %RPD Sample/Sample Dup DAL-GW-WW9R; Sample DAL-GW-WW9R; Sample Dup
Average %RPD Sample/Sample Dup DAL-GW-WW10R; Sample DAL-GW-WW10R; Sample Dup
Average %RPD Sample/Sample Dup DAL-GW-WW11R; Sample DAL-GW-WW11R; Sample Dup
Average %RPD Sample/Sample Dup
PFOA Concentration
(ng/mL)
1840 1820 1830 (1) 1.1 0.0729 0.0775 0.0752 (2) 6.1 0.0728 0.0868 0.0798 (2) 18 2700 2730 2720 (1) 1.1 2670 2700 2690 (1) 1.1 1910 1870 1890 (1) 2.1 1050 1060 1060 (1) 0.94
PFBS Concentration
(ng/mL)
1330 1360 1350 (1) 2.2 1430 1440 1440 (1) 0.69 0.0725 0.0806 0.0766 (2)
11 316 316 316 (1) 0.0 264 253 259 (1) 4.2 239 238 239 (1) 0.42 200 195 198 (1) 2.5
PFHS Concentration
(ng/mL)
687 703 695 (1) 2.3 0.0587 0.0829 0.0708 (2) 34 (3) <0.0500 0.0648 0.0648 (2) NA 1260 1270 1270 (1) 0.79 1170 1160 1170 (1) 0.85 889 880 885 (1) 1.0 515 508 512 (1) 1.4
PFOS Concentration
(ng/mL)
1960 1980 1970 (1) 1.0 0.531 0.606 0.569 (2) 13 0.0276 0.0330 0.0303 (2) 18 4070 4050 4060 (1) 0.49 4160 4210 4190 (1) 1.2 2950 2890 2920 (1) 2.1 1570 1560 1570 (1) 0.64
NA = Not Applicable (1) Reported results were prepared and analyzed by ETS-8-044.1 using external standard calibration. The analytical method
uncertainties associated with the reported results are as follows: PFOA 17%, PFBS 17%, PFHS 16%, and PFOS 21 %. (2) Reported results were prepared and analyzed by ETS-8-044.1 using internal standard calibration. The analytical method
uncertainties associated with the reported results are as follows: PFOA 17%, PFBS 14%, PFHS 23%, and PFOS 21 %. (3) Sample/sample duplicate RPD did not meet acceptance criteria of <20%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
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 Perfluorooctanoic Acid (C8 Acid) Perfluorobutanesulfonate (C4 Sulfonate ) Perfluorohexanesulfonate (C6 Sulfonate) Perfluorooctanesulfonate (C8 Sulfonate)
Acronym PFOA PFBS PFHS PFOS
Reference Material Structure
Linear + Branched Linear Linear
Linear + Branched
2.2 Sample Collection
Samples were collected on December 13, 2013 in NalgeneTM (high-density polyethylene) bottles prepared at the 3M Environmental Laboratory. 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. Sample bottles for sampling locations ACM2 and ACE, along with the Trip Blank sample and low spike, were fortified with a mixture of mass-labeled internal standards at a nominal concentration of 1 ng/mL and a mixture of surrogate recovery standards at a nominal concentration of 0.1 ng/mL. Collected sample bottles were received by the laboratory at ambient conditions on December 18, 2013.
2.3 Sample Preparation
All samples were diluted with methanol and analyzed for all analytes. Samples diluted 1:10 were prepared by removing a 1 mL aliquot of the well mixed sample and adding 8.9 mL of methanol and 0.1 mL of a surrogate spiking solution. The 1:100 dilutions were prepared by removing a 0.1 mL aliquot of the well mixed sample and adding 9.8 mL of methanol and 0.1 mL of a surrogate spiking solution. Prepared samples were analyzed by external standard calibration. Further dilution may have been applied by using a lower injection volume on the instrument.
The ACE and ACM2 sample sets and the Trip Blank sample were prepared and analyzed for all analytes by transferring an aliquot of the well mixed sample into an autovial. Prepared samples were analyzed by internal standard calibration. Following sample analysis, it was discovered that the ACE FMS sample was not fortified with internal standard. Therefore, internal standard was added to an aliquot of the ACE FMS sample, and the ACE sample set was re-analyzed by internal standard calibration.
During the preparation of the laboratory control samples for internal standard calibration, 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 for ACE, ACM2, and Trip Blank 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 analyzed in the same manner as the samples.
2.4 Analysis
All samples and quality control samples were analyzed for 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.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
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 3. Instrument Parameters.
Instrument Name
Analysis Dates
Analytical Method Liquid Chromatograph Guard column Analytical column Injection Volume Mass Spectrometer Ion Source Polarity Software
ETS Buster 1/8/14 - external standard calibration 1/9/14 and 1/10/14 - internal standard calibration
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 or 20 xL Applied Biosystems API 4000
Turbo Spray Negative
Analyst 1.6.1
Table 4. Liquid Chromatography Gradient Program.
Step Number
0 1 2 3 4 5 6 7 8 9
Total Time (min)
0.00 0.50 4.00 6.00 11.0 13.0 13.5 16.0 16.5 19.0
Flow Rate (uL/min)
750 750 750 750 750 750 750 750 750 750
Percent A (2 mM ammonium acetate)
90.0 90.0 70.0 70.0 20.0 20.0 10.0 10.0 90.0 90.0
Percent B (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. ISO13-07-11
Table 5. Mass Transitions.
Analyte
Mass Transition Q1/Q3
Internal Standard (1)
Mass Transition Q1/Q3
413/369
PFOA
413/219
[13C8]PFOA
421/376
413/169
PFBS
299/80 299/99
[18O2]PFBS
303/84
PFHS
399/99 399/80
[13Cs]PFHS
402/80
499/99
PFOS
499/80
[13C8]PFOS
507/80
499/130
[13C4]PFOA surrogate
417/372
[13C8]PFOA
421/376
[13C4]PFOS surrogate
503/80
[13C8]PFOS
507/80
Dwell time was 20 msec for each transition. The individual transitions were summed to produce a "total ion chromatogram" (TIC), which was used for quantitation.
(1) Internal standards were used for the analysis on 1/9/14 and 1/10/14.
3 Data Analysis
3.1 Calibration
External Standard Calibration Analysis on 1/8/14: Samples were analyzed against an external standard calibration curve. Calibration standards were prepared by spiking known amounts of the stock solution containing the target analytes into 90:10 methanol: Milli-Q laboratory water. A total of eleven spiked standards ranging from 0.02 ng/mL to 50 ng/mL (nominal) were analyzed. The standards also contained the surrogates at concentrations ranging from 0.02 ng/mL to 25 ng/mL nominal. A quadratic, 1/x weighted, calibration curve of the standard peak area counts was used to fit the data for each analyte. The data were not forced through zero during the fitting process. Calculating the standard concentrations using the peak area counts and the resultant calibration curve confirmed accuracy of each curve point.
Internal Standard Calibration Analysis on 1/9/14 and 1/10/14: Samples were analyzed against a matrix-matched stable isotope internal standard calibration curve. Calibration standards were prepared by spiking known amounts of stock solutions into laboratory prepared reagent water. The calibration standards contained an internal standard mix at a nominal concentration of 1 ng/mL. A total of thirteen calibration standards ranging from 0.025 ng/mL to 25 ng/mL (nominal) were analyzed with the prepared samples. O f these thirteen calibration standards, eleven contained the surrogates at concentrations ranging from 0.025 ng/mL to 10 ng/mL nominal. 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. Calculating the standard concentrations using the peak area ratios and the resultant calibration curve confirmed accuracy of each curve point.
For each calibration curve, the reference standards of PFOA and PFOS used to prepare the calibration standards consisted of both linear and branched isomers. 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.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
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/ratio and retention time criteria of less than or equal to 2% RSD. These criteria were met for all analytes.
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 area counts are at least twice those of the appropriate blanks. The LOQs associated with the sample analysis are listed in Table 6.
Table 6. LOQ
Analyte
LOQ, ng/mL 1/8/14 Analysis
LOQ, ng/mL 1/9/14 Analysis
PFOA
0.0192 (1)
0.0240
PFBS
0.0200 (1)
0.0250
PFHS
0.0200 (1)
0.0500
PFOS
0.0185 (1)
0.0232
(1) The dilution factor was not applied to the LOQ.
LOQ, ng/mL 1/10/14 Analysis
0.0287 0.0250 0.0500 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.
3.5 Blanks
Two types of blanks were prepared and analyzed with the samples: method blanks/solvent blanks and field/trip blanks. Each blank result was 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 for the target analytes and analyzed in triplicate, while only low and high lab control spikes were prepared for the surrogates. LCSs were prepared by spiking known amounts of the analytes into either 10 mL of laboratory-prepared matrix matched water or 1 mL of Milli-Q water to produce the desired concentration. When applicable, the LCSs were then diluted with methanol in the same manner as the samples. Method ETS-8-044.1 states that the average recovery of LCSs at each spiking level be within 80%-120% with a RSD <20%. All LCS samples met method accuracy criteria except for the mid level LCSs for PFHS (123%) on 1/9/14 and PFOS (121%) on 1/10/14. A method deviation is included with the raw data.
All LCSs were used in the determination of the analytical method uncertainty in section 3.7.
The following calculations were used to generate data in Table 7.
Calculated Concentration * . LCS Percent Recovery -------------------------------------* 100%
Spike Concentration
LC S% RSD = standard deviation LC S replicates *ioo% average LC S recovery
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Table 7. Lab Control Spike Results.
ETS-8-044.1 External Standard Calibration Analyzed 1/8/14
Lab ID
PFOA (Linear + Branched)
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
LCS-140108-1 LCS-140108-2 LCS-140108-3
Average %RSD
LCS-140108-4 LCS-140108-5 LCS-140108-6
Average %RSD
0.191 0.191 0.191
4.74 4.74 4.74
0.180 0.174 0.176 92.5% 1.7%
4.86 4.82 4.79 102% 0.57%
94.2 91.1 92.1
102 102 101
LCS-140108-7 LCS-140108-8 LCS-140108-9
Average %RSD
38.2 38.2 38.2
38.0 36.3 35.9 96.2% 3.1%
99.6 95.1 94.0
Spiked Concentration
(ng/mL)
PFOA surrogate
Calculated Concentration
(ng/mL)
0.199 0.199 0.199
0.222 0.219 0.217 110% 1.4%
4.94 5.16 4.94 5.07 4.94 5.07
104% 1.1%
%Recovery 112 110 109
105 103 103
ETS-8-044.1 External Standard Calibration Analyzed 1/8/14
Lab ID
Spiked Concentration
(ng/mL)
PFBS
Calculated Concentration
(ng/mL)
LCS-140108-1 LCS-140108-2 LCS-140108-3
Average %RSD LCS-140108-4 LCS-140108-5 LCS-140108-6
Average %RSD LCS-140108-7 LCS-140108-8 LCS-140108-9
Average %RSD
0.199 0.199 0.199
4.95 4.95 4.95
39.8 39.8 39.8
0.204 0.201 0.195 100% 2.1%
5.04 5.03 4.94 101% 1.2%
41.9 41.3 40.1 103% 2.0%
%Recovery 102 101 97.9
102 102 99.9
105 104 101
Spiked Concentration
(ng/mL) 0.199 0.199 0.199
4.95 4.95 4.95
39.8 39.8 39.8
PFHS Calculated Concentration
(ng/mL)
0.194 0.211 0.198 101% 4.3%
4.89 4.83 4.82 97.9% 0.72%
>ULOQ >ULOQ >ULOQ
NA
%Recovery 97.7 106 99.4
98.7 97.6 97.4
NA NA NA
>ULOQ = analyte concentration exceeded upper limit of quantitation NA = Not Applicable (1) LCS recovery did not meet acceptance criteria of 100 20%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Table 7 continued. Lab Control Spike Results.
ETS-8-044.1 External Standard Calibration Analyzed 1/8/14
Lab ID
PFOS (Linear + Branched)
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
LCS-140108-1 LCS-140108-2 LCS-140108-3
Average %RSD
LCS-140108-4 LCS-140108-5 LCS-140108-6
Average %RSD
0.185 0.185 0.185
4.59 4.59 4.59
0.178 0.185 0.179 97.6% 2.0%
4.79 4.71 4.76 104% 0.56%
96.2 99.8 96.7
104 103 104
LCS-140108-7 LCS-140108-8 LCS-140108-9
Average %RSD
36.9 36.9 36.9
37.4 36.0 35.9 98.6% 2.1%
101 97.6 97.2
Spiked Concentration
(ng/mL)
PFOS surrogate
Calculated Concentration
(ng/mL)
0.190 0.190 0.190
0.226 0.220 0.236 120% 3.4%
4.73 5.38 4.73 5.40 4.73 5.35
114% 0.51%
%Recovery 119 116 124
114 114 113
ETS-8-044.1 Internal Standard Calibration Analyzed 1/9/14
Lab ID
PFOA (Linear + Branched)
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
LCS-140109-1 LCS-140109-2 LCS-140109-3
Average %RSD
LCS-140109-4 LCS-140109-5 LCS-140109-6
Average %RSD
0.190 0.190 0.190
1.90 1.90 1.90
0.201 0.202 0.208 107% 2.2%
2.20 2.12 2.20 115% 2.0%
106 106 110
116 112 116
LCS-140109-7 LCS-140109-8 LCS-140109-9
Average %RSD
19.0 19.0 19.0
20.7 21.6 22.1 113% 3.2%
109 114 116
Spiked Concentration
(ng/mL)
PFOA surrogate
Calculated Concentration
(ng/mL)
0.198 0.198 0.198
0.230 0.244 0.235 119% 3.0%
1.98 2.40 1.98 2.31 1.98 2.35
119% 1.7%
%Recovery 116 123 119
121 117 119
>ULOQ = analyte concentration exceeded upper limit of quantitation NA = Not Applicable (1) LCS recovery did not meet acceptance criteria of 100 20%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Table 7 continued. Lab Control Spike Results.
ETS-8-044.1 Internal Standard Calibration Analyzed 1/9/14
Lab ID
Spiked Concentration
(ng/mL)
PFBS
Calculated Concentration
(ng/mL)
LCS-140109-1 LCS-140109-2 LCS-140109-3
Average %RSD
LCS-140109-4 LCS-140109-5 LCS-140109-6
Average %RSD
0.198 0.198 0.198
1.98 1.98 1.98
0.210 0.212 0.229 110% 5.0%
2.15 2.08 2.08 106% 2.2%
LCS-140109-7 LCS-140109-8 LCS-140109-9
Average %RSD
19.9 19.9 19.9
20.3 21.1 22.0 106% 4.3%
%Recovery 106 107 116
109 105 105
102 106 111
Spiked Concentration
(ng/mL) 0.198 0.198 0.198
1.98 1.98 1.98
19.9 19.9 19.9
PFHS Calculated Concentration
(ng/mL)
0.179 0.235 0.211 105% 14%
2.47 2.40 2.41 123% 1.7% (1)
21.5 21.9 22.6 111% 2.8%
%Recovery 90.4 119 106
125 121 122
108 110 114
ETS-8-044.1 Internal Standard Calibration Analyzed 1/9/14
Lab ID
PFOS (Linear + Branched)
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
LCS-140109-1 LCS-140109-2 LCS-140109-3
Average %RSD
LCS-140109-4 LCS-140109-5 LCS-140109-6
Average %RSD
0.184 0.184 0.184
1.84 1.84 1.84
0.224 0.216 0.219 119% 2.1%
2.11 2.09 2.18 116% 2.6%
122 117 119
115 113 119
LCS-140109-7 LCS-140109-8 LCS-140109-9
Average %RSD
18.4 18.4 18.4
20.6 20.5 21.1 113% 1.5%
112 112 115
Spiked Concentration
(ng/mL)
PFOS surrogate
Calculated Concentration
(ng/mL)
0.189 0.189 0.189
0.199 0.207 0.257 117% 14%
1.89 2.01 1.89 1.95 1.89 2.05
106% 2.4%
%Recovery 105 109 136
106 103 108
>ULOQ = analyte concentration exceeded upper limit of quantitation NA = Not Applicable (1) LCS recovery did not meet acceptance criteria of 100 20%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Table 7 continued. Lab Control Spike Results.
ETS-8-044.1 Internal Standard Calibration Analyzed 1/10/14
Lab ID
PFOA (Linear + Branched)
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
LCS-140110-1 LCS-140110-2 LCS-140110-3
Average %RSD
LCS-140110-4 LCS-140110-5 LCS-140110-6
Average %RSD
0.190 0.190 0.190
1.90 1.90 1.90
0.196 0.194 0.202 104% 2.0%
2.18 2.08 2.26 115% 3.9%
103 102 106
115 110 119
LCS-140110-7 LCS-140110-8 LCS-140110-9
Average %RSD
19.0 19.0 19.0
21.3 21.2 20.7 111% 1.6%
112 112 109
Spiked Concentration
(ng/mL)
PFOA surrogate
Calculated Concentration
(ng/mL)
0.198 0.198 0.198
0.237 0.217 0.249 118% 7.3%
1.98 2.35 1.98 2.23 1.98 2.27
115% 3.1%
%Recovery 120 109 126
119 112 115
ETS-8-044.1 Internal Standard Calibration Analyzed 1/10/14
Lab ID
Spiked Concentration
(ng/mL)
PFBS
Calculated Concentration
(ng/mL)
LCS-140110-1 LCS-140110-2 LCS-140110-3
Average %RSD
LCS-140110-4 LCS-140110-5 LCS-140110-6
Average %RSD
0.198 0.198 0.198
1.98 1.98 1.98
0.201 0.212 0.204 104% 2.9%
2.12 2.20 2.25 111% 3.2%
LCS-140110-7 LCS-140110-8 LCS-140110-9
Average %RSD
19.9 19.9 19.9
20.8 20.6 20.1 103% 1.5%
%Recovery 101 107 103
107 111 114
104 103 101
Spiked Concentration
(ng/mL) 0.198 0.198 0.198
1.98 1.98 1.98
19.9 19.9 19.9
PFHS Calculated Concentration
(ng/mL)
0.208 0.213 0.245 112% 9.3%
2.21 2.28 2.18 112% 2.2%
22.9 22.1 21.2 111% 3.6%
%Recovery 105 107 124
112 115 110
115 111 107
>ULOQ = analyte concentration exceeded upper limit of quantitation NA = Not Applicable (1) LCS recovery did not meet acceptance criteria of 100 20%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Table 7 continued. Lab Control Spike Results.
ETS-8-044.1 Internal Standard Calibration Analyzed 1/10/14
Lab ID
PFOS (Linear + Branched)
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
LCS-140110-1 LCS-140110-2 LCS-140110-3
Average %RSD
LCS-140110-4 LCS-140110-5 LCS-140110-6
Average %RSD
0.184 0.184 0.184
1.84 1.84 1.84
0.208 0.222 0.198 114% 6.2%
2.26 2.12 2.28 121% 4.1% (1)
113 121 107
123 115 124
LCS-140110-7 LCS-140110-8 LCS-140110-9
Average %RSD
18.4 18.4 18.4
21.1 20.8 19.1 110% 5.0%
114 113 104
Spiked Concentration
(ng/mL)
PFOS surrogate
Calculated Concentration
(ng/mL)
0.189 0.189 0.189
0.204 0.218 0.197 109% 5.1%
1.89 2.35 1.89 2.18 1.89 2.26
120% 4.2%
%Recovery 108 115 104
125 115 120
>ULOQ = analyte concentration exceeded upper limit of quantitation NA = Not Applicable (1) LCS recovery did not meet acceptance criteria of 100 20%.
3.7 Analytical Method Uncertainty
Analytical 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-12-012.2. 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 method uncertainty determined by ETS-12-012.2 was 21% for PFHS and 18% for PFOS, but the method uncertainty has been expanded based on the %bias of the non-compliant mid-level LCSs.
Table 8. Analytical Method Uncertainty.
Analyte PFOA PFBS PFHS PFOS PFOA PFBS PFHS PFOS
Calibration Method External Standard External Standard External Standard External Standard Internal Standard Internal Standard Internal Standard Internal Standard
Standard Deviation (%) 8.56 8.70 7.92 10.7 8.50 6.80 10.7 9.12
Method Uncertainty 17% 17% 16% 21% 17% 14% 23% 21%
PAGE 12 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
3.8 Field Matrix Spikes (FMS)
A field matrix spike was collected at each sampling point 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 for sample collection. 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 standards used for the preparation of the field matrix spiking solutions contained reference materials comprised of both linear and branched isomers for PFOA and PFOS. 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 0 0 % Spike Concentraton
Table 9. Field Matrix Spike Concentrations.
Location ACI ACM2 ACE WW8R, WW9R, WW10R, WW11R
Trip Blank
Description Field Matrix Spike Field Matrix Spike Field Matrix Spike Field Matrix Spike Low Field Matrix Spike High Field Matrix Spike
Firial Concentr.tion (ng/mL
PFOA
PFBS
PFHS
PFOS
2480 4.96 4.96
2500 5.00 5.00
2510 5.00 5.00
2500 4.99 4.99
2480
2500
2510
2500
4.96 2480
5.00 2500
5.00 2510
4.99 2500
4 Data Summary and Discussion
The tables below summarize the sample results and field matrix spike recoveries for the seven 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. Relative percent 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 field matrix spike samples and surrogate recovery standards met method acceptance criteria except where noted below.
DAL-GW-ACM2; the FMS sample (5 ng/mL) was not appropriate for PFBS; however, the surrogate recovery standard 13C4-PFOS met method acceptance criteria. No additional QC samples were prepared.
PAGE 13 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Table 10. DAL GW ACI 131213 (1)
3M LIMS ID
Description
ISO13-07-11-001
DAL-GW-ACI-0-131213
ISO13-07-11-002
DAL-GW-ACI-DB-131213
ISO13-07-11-003
DAL-GW-ACI-FMS-131213
Average Concentration (ng/mL) %RPD
PFOA
PFBS
Concentration
(ng/mL)
%Recovery
1840
NA
1820
NA
4200
95.6
1830 ng/mL 1.1%
Concentration
(ng/mL)
%Recovery
1330
NA
1360
NA
3690
93.6
1350 ng/mL 2.2%
3M LIMS ID
Description
ISO13-07-11-001
DAL-GW-ACI-0-131213
ISO13-07-11-002
DAL-GW-ACI-DB-131213
ISO13-07-11-003
DAL-GW-ACI-FMS-131213
Average Concentration (ng/mL) %RPD
PFHS
PFOS
Concentration
(ng/mL)
%Recovery
687 NA
703 NA
3210
100
695 ng/mL 2.3%
Concentration
(ng/mL)
%Recovery
1960
NA
1980
NA
4780
112
1970 ng/mL 1.0%
13C4-PFOA
13C4-PFOS
3M LIMS ID
Description
ISO13-07-11-001
DAL-GW-ACI-0-131213
ISO13-07-11-002
DAL-GW-ACI-DB-131213
ISO13-07-11-003
DAL-GW-ACI-FMS-131213
Average Concentration (ng/mL) %RSD
%Recovery
94.2 93.1 89.7 92.3% 2.5%
%Recovery
110 115 110 112% 2.6%
NA = Not Applicable (1) Samples were analyzed by external standard calibration. The surrogate recovery standards 13C4-PFOA and 13C4-PFOS were
added to the samples during sample preparation.
PAGE 14 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Table 11. DAL GW ACM2 131213
3M LIMS ID
Description
ISO13-07-11-004
DAL-GW-ACM2-0-131213
ISO13-07-11-005
DAL-GW-ACM2-DB-131213
ISO13-07-11-006
DAL-GW-ACM2-FMS-131213
Average Concentration (ng/mL) %RPD
3M LIMS ID
Description
ISO13-07-11-004
DAL-GW-ACM2-0-131213
ISO13-07-11-005
DAL-GW-ACM2-DB-131213
ISO13-07-11-006
DAL-GW-ACM2-FMS-131213
Average Concentration (ng/mL) %RPD
PFOA (1)
PFBS (2)
Concentration
(ng/mL)
%Recovery
0.0729
NA
0.0775
NA
5.51 110
0.0752 ng/mL 6.1%
Concentration
(ng/mL)
%Recovery
1430
NA
1440
NA
1460
NC
1440 ng/mL 0.69%
PFHS (1)
PFOS (1)
Concentration
(ng/mL)
%Recovery
0.0587
NA
0.0829
NA
5.47 108
0.0708 ng/mL 34% (3)
Concentration
(ng/mL)
%Recovery
0.531
NA
0.606
NA
6.00 109
0.569 ng/mL 13%
13C4-PFOA (1) 13C4-PFOS (1)
3M LIMS ID
Description
ISO13-07-11-004
DAL-GW-ACM2-0-131213
ISO13-07-11-005
DAL-GW-ACM2-DB-131213
ISO13-07-11-006
DAL-GW-ACM2-FMS-131213
Average Concentration (ng/mL) %RSD
%Recovery
110 105 108 108% 2.3%
%Recovery
102 93.6 88.3 94.6% 7.3%
NA = Not Applicable NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration. (1) Samples were analyzed by internal standard calibration. (2) Samples were analyzed by external standard calibration. (3) Sample/sample duplicate RPD did not meet acceptance criteria of <20%.
PAGE 15 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Table 12. DAL GW ACE 131213 (1)
3M LIMS ID
Description
ISO13-07-11-007
DAL-GW-ACE-0-131213
ISO13-07-11-008
DAL-GW-ACE-DB-131213
ISO13-07-11-009
DAL-GW-ACE-FMS-131213
Average Concentration (ng/mL) %RPD
3M LIMS ID
Description
ISO13-07-11-007
DAL-GW-ACE-0-131213
ISO13-07-11-008
DAL-GW-ACE-DB-131213
ISO13-07-11-009
DAL-GW-ACE-FMS-131213
Average Concentration (ng/mL) %RPD
PFOA
PFBS
Concentration
(ng/mL)
%Recovery
0.0728
NA
0.0868
NA
5.22 104
0.0798 ng/mL 18%
Concentration
(ng/mL)
%Recovery
0.0725
NA
0.0806
NA
4.65 91.5
0.0766 ng/mL 11%
PFHS
PFOS
Concentration
(ng/mL)
%Recovery
<0.0500
NA
0.0648
NA
4.72 93.1
0.0648 ng/mL
Concentration
(ng/mL)
%Recovery
0.0276
NA
0.0330
NA
4.75 94.6
0.0303 ng/mL 18%
13C4-PFOA
13C4-PFOS
3M LIMS ID
Description
ISO13-07-11-007
DAL-GW-ACE-0-131213
ISO13-07-11-008
DAL-GW-ACE-DB-131213
ISO13-07-11-009
DAL-GW-ACE-FMS-131213
Average Concentration (ng/mL) %RSD
%Recovery
98.5 102 104 100% 2.8%
%Recovery
112 91.7 94.1 102% 11%
NA = Not Applicable (1) Samples were analyzed by internal standard calibration.
PAGE 16 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Table 13. DAL GW WW8R 131213 (1)
3M LIMS ID
Description
ISO13-07-11-010
DAL-GW-WW8R-0-131213
ISO13-07-11-011
DAL-GW-WW8R-DB-131213
ISO13-07-11-012
DAL-GW-WW8R-FMS-131213
Average Concentration (ng/mL) %RPD
3M LIMS ID
Description
ISO13-07-11-010
DAL-GW-WW8R-0-131213
ISO13-07-11 -011
DAL-GW-WW8R-DB-131213
ISO13-07-11-012
DAL-GW-WW8R-FMS-131213
Average Concentration (ng/mL) %RPD
PFOA
PFBS
Concentration
(ng/mL)
%Recovery
2700
NA
2730
NA
4930
89.1
2720 ng/mL 1.1%
Concentration
(ng/mL)
%Recovery
316 NA
316 NA
2640
93.0
316 ng/mL 0.0%
PFHS
PFOS
Concentration
(ng/mL)
%Recovery
1260
NA
1270
NA
3610
93.2
1270 ng/mL 0.79%
Concentration
(ng/mL)
%Recovery
4070
NA
4050
NA
6490
97.2
4060 ng/mL 0.49%
13C4-PFOA
13C4-PFOS
3M LIMS ID
Description
ISO13-07-11-010
DAL-GW-WW8R-0-131213
ISO13-07-11 -011
DAL-GW-WW8R-DB-131213
ISO13-07-11-012
DAL-GW-WW8R-FMS-131213
Average Concentration (ng/mL) %RSD
%Recovery
90.6 86.5 82.7 86.6% 4.6%
%Recovery
108 107 101 105% 3.6%
NA = Not Applicable (1) Samples were analyzed by external standard calibration. The surrogate recovery standards 13C4-PFOA and 13C4-PFOS were
added to the samples during sample preparation.
PAGE 17 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Table 14. DAL GW WW9R 131213 (1)
3M LIMS ID
Description
ISO13-07-11-013
DAL-GW-WW9R-0-131213
ISO13-07-11-014
DAL-GW-WW9R-DB-131213
ISO13-07-11-015
DAL-GW-WW9R-FMS-131213
Average Concentration (ng/mL) %RPD
3M LIMS ID
Description
ISO13-07-11-013
DAL-GW-WW9R-0-131213
ISO13-07-11-014
DAL-GW-WW9R-DB-131213
ISO13-07-11-015
DAL-GW-WW9R-FMS-131213
Average Concentration (ng/mL) %RPD
PFOA
PFBS
Concentration
(ng/mL)
%Recovery
2670
NA
2700
NA
4820
85.9
2690 ng/mL 1.1%
Concentration
(ng/mL)
%Recovery
264 NA
253 NA
2590
93.2
259 ng/mL 4.2%
PFHS
PFOS
Concentration
(ng/mL)
%Recovery
1170
NA
1160
NA
3460
91.2
1170 ng/mL 0.85%
Concentration
(ng/mL)
%Recovery
4160
NA
4210
NA
6640
98.0
4190 ng/mL 1.2%
13C4-PFOA
13C4-PFOS
3M LIMS ID
Description
ISO13-07-11-013
DAL-GW-WW9R-0-131213
ISO13-07-11-014
DAL-GW-WW9R-DB-131213
ISO13-07-11-015
DAL-GW-WW9R-FMS-131213
Average Concentration (ng/mL) %RSD
%Recovery
88.3 89.6 85.5 87.8% 2.4%
%Recovery
111 105 106 107% 3.0%
NA = Not Applicable (1) Samples were analyzed by external standard calibration. The surrogate recovery standards 13C4-PFOA and 13C4-PFOS were
added to the samples during sample preparation.
PAGE 18 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Table 15. DAL GW WW10R 131213 (1)
3M LIMS ID
Description
ISO13-07-11-016
DAL-GW-WW10R-0-131213
ISO13-07-11-017
DAL-GW-WW10R-DB-131213
ISO13-07-11-018
DAL-GW-WW10R-FMS-131213
Average Concentration (ng/mL) %RPD
3M LIMS ID
Description
ISO13-07-11-016
DAL-GW-WW10R-0-131213
ISO13-07-11-017
DAL-GW-WW10R-DB-131213
ISO13-07-11-018
DAL-GW-WW10R-FMS-131213
Average Concentration (ng/mL) %RPD
PFOA
PFBS
Concentration
(ng/mL)
%Recovery
1910
NA
1870
NA
3940
82.7
1890 ng/mL 2.1%
Concentration
(ng/mL)
%Recovery
239 NA
238 NA
2460
88.8
239 ng/mL 0.42%
PFHS
PFOS
Concentration
(ng/mL)
%Recovery
889 NA
880 NA
3110
88.6
885 ng/mL 1.0%
Concentration
(ng/mL)
%Recovery
2950
NA
2890
NA
5110
87.6
2920 ng/mL 2.1%
13C4-PFOA
13C4-PFOS
3M LIMS ID
Description
ISO13-07-11-016
DAL-GW-WW10R-0-131213
ISO13-07-11-017
DAL-GW-WW10R-DB-131213
ISO13-07-11-018
DAL-GW-WW10R-FMS-131213
Average Concentration (ng/mL) %RSD
%Recovery
90.3 86.8 84.2 87.1% 3.5%
%Recovery
109 102 111 107% 4.4%
NA = Not Applicable (1) Samples were analyzed by external standard calibration. The surrogate recovery standards 13C4-PFOA and 13C4-PFOS were
added to the samples during sample preparation.
PAGE 19 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Table 16. DAL GW WW11R 131213 (1)
3M LIMS ID
Description
ISO13-07-11-019
DAL-GW-WW11R-0-131213
ISO13-07-11-020
DAL-GW-WW11R-DB-131213
ISO13-07-11-021
DAL-GW-WW11R-FMS-131213
Average Concentration (ng/mL) %RPD
3M LIMS ID
Description
ISO13-07-11-019
DAL-GW-WW11 R-0-131213
ISO13-07-11-020
DAL-GW-WW11 R-DB-131213
ISO13-07-11-021
DAL-GW-WW11 R-FMS-131213
Average Concentration (ng/mL) %RPD
PFOA
PFBS
Concentration
(ng/mL)
%Recovery
1050
NA
1060
NA
3260
88.7
1060 ng/mL 0.94%
Concentration
(ng/mL)
%Recovery
200 NA
195 NA
2420
88.9
198 ng/mL 2.5%
PFHS
PFOS
Concentration
(ng/mL)
%Recovery
515 NA
508 NA
2730
88.4
512 ng/mL 1.4%
Concentration
(ng/mL)
%Recovery
1570
NA
1560
NA
3940
94.8
1570 ng/mL 0.64%
13C4-PFOA
13C4-PFOS
3M LIMS ID
Description
ISO13-07-11-019
DAL-GW-WW11 R-0-131213
ISO13-07-11-020
DAL-GW-WW11 R-DB-131213
ISO13-07-11-021
DAL-GW-WW11 R-FMS-131213
Average Concentration (ng/mL) %RSD
%Recovery
91.7 90.0 84.7 88.8% 4.1%
%Recovery
108 110 104 107% 2.9%
NA = Not Applicable (1) Samples were analyzed by external standard calibration. The surrogate recovery standards 13C4-PFOA and 13C4-PFOS were
added to the samples during sample preparation.
PAGE 20 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Table 17. Trip Blank Results
3M LIMS ID
ISO13-07-11-022 ISO13-07-11-023 ISO13-07-11-024
Description
DAL-GW-TRI P-0-131213 DAL-GW-TRIP-LS-131213 DAL-GW-TRI P-HS-131213
3M LIMS ID
ISO13-07-11-022 ISO13-07-11-023 ISO13-07-11-024
Description
DAL-GW-TRI P-0-131213 DAL-GW-TRI P-LS-131213 DAL-GW-TRI P-HS-131213
PFOA
PFBS
Concentration (ng/mL)
<0.0240 (1) 4.37 (2) 2200 (2)
%Recovery
NA 88.1 88.7
Concentration (ng/mL)
<0.0250 (1) 4.74 (2) 2110 (2)
%Recovery
NA 94.8 84.4
PFHS
PFOS
Concentration (ng/mL)
<0.0500 (1) 4.45 (2) 2160 (2)
%Recovery
NA 89.0 86.1
Concentration (ng/mL)
<0.0232 (1) 4.54 (2) 2420 (2)
%Recovery
NA 91.0 96.8
13C4-PFOA
13C4-PFOS
3M LIMS ID
ISO13-07-11-022 ISO13-07-11-023 ISO13-07-11-024
Description
DAL-GW-TRI P-0-131213 DAL-GW-TRI P-LS-131213 DAL-GW-TRI P-HS-131213
%Recovery
115 (1) 100 (2) 94.0 (2)
%Recovery
92.0 (1) 114 (2) 115 (2)
NA = Not Applicable (1) Samples were analyzed by internal standard calibration. (2) Samples were analyzed by external standard calibration. The surrogate recovery standards 13C4-PFOA and 13C4-PFOS were
added to the samples during sample preparation.
PAGE 21 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
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 matrix spike recoveries demonstrated that the analytical method was appropriate for the given sample matrix. Analysis was completed using 3M Environmental Laboratory Method ETS-8044.1 "Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis". Analytical results are reported in Table 1 and 10-17 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.
7 Attachments
Attachment A: Analyte T rend Data for select sampling points at the Decatur Ground Water T reatment Plant (GWTP) GAC System.
8 Signatures
Digitally signed by Susan T. Wolf DN: c=US, st=MN, l=St. Paul, ou=3M Environmental Laboratory - authenticated by LRA, email=stwolf@mmm.com, o=3M, cn=Susan T. Wolf Reason: I am the author of this document Date: 2014.01.27 11:22:30 ~06'00'
Susan T. Wolf, 3M Principal Analytical Investigator
Digitally signed by Wiliam K. Reagen DN: c=US, st=MN, l=St. Paul, ou=Laboratory Director, ou=3M Environmental Laboratory - authenticated by LRA, email=wkreagen@mmm.com, o=3M, cn=Wlliam K. Reagen Reason: I am approving this document Date: 2014.01.27 12:03:47-06'00'
William K. Reagen, Ph.D., 3M Environmental Laboratory Technical Director
Date Date
The 3M Environmental Laboratory's Quality Assurance Unit has audited the data and report for this project.
Digitally signed by Daryl K. Peterson DN: c=US, st=MN, l=St. Paul, ou=3M Environmental Laboratory - authenticated by LRA, email=dpeterson2@mmm.com, o=3M, cn=Daryl K. Peterson Date: 2014.01.28 08:54:12 -06'00'
Quality Assurance Representative
Date
This test report shall not be reproduced except in full, without written approval o f the 3M Environmental Laboratory.
PAGE 22 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Attachment A: Analyte Trend Data for select sampling points at the Decatur Ground Water Treatment Plant (GWTP) GAC System ACI (Activated Carbon Influent) - Sample Results in ng/mL
ACI PFOA PFBS PFHS PFOS
1/17/13 1910 588 895 1810
2/13/13 2300 830 1580 2940
3/27/13 2220 1060 1090 2490
4/29/13 1480 1360 777 1670
5/31/13 1860 1040 940 2150
6/27/13 1480 708 942 1590
7/23/13 1630 1230 749 1680
9/30/13 2320 356 1400 3240
10/28/13 1880 1590 866 2100
11/18/13 2190 1100 1330 2240
12/13/13 1830 1350 695 1970
ACE (Activated Carbon Effluent) - Sample Results in ng/mL
ACE PFOA PFBS PFHS PFOS
1/17/13 <0.0240 <0.0250 <0.0250 <0.0232
2/13/13 0.124
0.0360 0.178
0.0329
3/27/13 0.0380
<0.0250 0.0477
<0.0232
4/29/13 0.0422 0.392 0.0570
<0.0232
5/31/13 0.0725 24.8 0.105
<0.0232
6/27/13 0.0717 111 0.118
<0.0232
7/23/13 0.0641 1960 0.0778 0.0277
9/30/13 0.115 1950 0.156
0.0452
10/28/13 0.231 0.379 0.180
0.0785
11/18/13 0.478 0.592 0.366
0.0726
12/13/13 0.0798 0.0766 0.0648 0.0303
PAGE 23 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Attachment A: Analyte Trend Data for select sampling points at the Decatur Ground Water Treatment Plant (GWTP) GAC System WW8R - Sample Results in ng/mL
W W 8R PFOA PFBS PFHS PFOS
1/17/13 4350 410 1930 5710
2/13/13 3250 354 1900 4850
3/27/13 3640 385 1760 5120
4/29/13 3190 364 1610 4830
5/31/13 2760 289 1330 4180
6/27/13 2760 282 1340 4110
7/23/13 2640 263 1260 3910
9/30/13 2890 303 1370 4100
10/28/13 2830 312 1300 4410
11/18/13 3040 362 1440 4750
12/13/13 2720 316 1270 4060
WW9R - Sample Results in ng/mL
FC Charting to r DAL WW9R 500OH------------------------------------------------------------------------------------
PFOA------- -------PFOS------- --------
PFBS------- --------
PFHS-------
W W 9R PFOA PFBS PFHS PFOS
1/17/13 2710 184 954 3690
2/13/13 2850 236 1400 4100
3/27/13 3330 278 1440 4660
4/29/13 2650 244 1200 4340
5/31/13 2660 226 1120 4210
6/27/13 2630 225 1140 4150
7/23/13 2410 212 1030 3670
9/30/13 2730 249 1220 4200
10/28/13 2820 286 1280 4380
11/18/13 2950 305 1340 4540
12/13/13 2690 259 1170 4190
PAGE 24 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO13-07-11
Attachment A: Analyte Trend Data for select sampling points at the Decatur Ground Water Treatment Plant (GWTP) GAC System WW10R - Sample Results in ng/mL
W W 10R PFOA PFBS PFHS PFOS
9/30/2013 2070 247 1030 2770
10/28/2013 2150 264 1030 3160
11/18/2013 2400 303 1120 3890
12/13/2013 1890 239 885 2920
WW11R - Sample Results in ng/mL
W W 11R PFOA PFBS PFHS PFOS
9/30/2013 1720 299 1000 2200
10/28/2013 1100 240 511 1670
11/18/2013 1320 287 680 1850
12/13/2013 1060 198 512 1570
PAGE 25 OF 25
