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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
Final Report
Analysis of PFOA, PFBS, PFHS, and PFOS in Aqueous Samples from 3M Decatur, Alabama: Groundwater Treatment Plant GAC System March 2014
Laboratory Request Number: ISO14-07-03 Method Requirement: 3M Method ETS-8-044.1
Report Date - Date of Last Signature
Testing Laboratory 3M EHS 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. ISO14-07-03
3M Environmental Laboratory 3M Environmental Laboratory Technical Director: William K. Reagen, Ph.D. 3M Principal Analytical Investigator: Susan Wolf Report Author: Susanna Emond
Analytical Report ISO14-07-03
3M Decatur Groundwater Treatment Plant System; March 2014 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 March 31, 2014. 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 ISO14-07-03. Analysis of the samples was completed as specified under 3M Environmental Laboratory General Project Outline (GPO) number GPO13-1289. 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 surrogate recovery standards prior to being sent to the field for sample collection. 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". Internal standards were used for select samples 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.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
Table 1. Sample Results Summary (1)
3M LIMS ID
Sample Description
PFOA Concentration
(ng/mL)
ISO14-07-03-001 ISO14-07-03-002
ISO14-07-03-004 ISO14-07-03-005
ISO14-07-03-007 ISO14-07-03-008
ISO14-07-03-010 ISO14-07-03-011
ISO14-07-03-013 ISO14-07-03-014
ISO14-07-03-016 ISO14-07-03-017
ISO14-07-03-019 ISO14-07-03-020
DAL-GW-ACI-0 - 140331 DAL-GW-ACI-DB - 140331
Average %RPD Sample/Sample Dup DAL-GW-ACM2-0 - 140331 DAL-GW-ACM2-DB - 140331
Average %RPD Sample/Sample Dup DAL-GW-ACE-0 - 140331 DAL-GW-ACE-DB - 140331
Average %RPD Sample/Sample Dup DAL-GW-WW8R-0 - 140331 DAL-GW-WW8R-DB - 140331
Average %RPD Sample/Sample Dup DAL-GW-WW9R-0 - 140331 DAL-GW-WW9R-DB - 140331
Average %RPD Sample/Sample Dup DAL-GW-WW10R-0 - 140331 DAL-GW-WW10R - 140331
Average %RPD Sample/Sample Dup DAL-GW-WW11R-0 - 140331 DAL-GW-WW11R-DB - 140331
Average %RPD Sample/Sample Dup
2350 2470 2410 5.0 2.15 1.91 2.03 1(2)
12 0.257 0.266 0.262 (2)
3.4 3330 3240 3290 2.7 3580 3180 3380
12 2110 2170 2140 2.8 1190 1180 1190 0.84
PFBS Concentration
(ng/mL)
536 546 541 1.8 3240 3230 3240 0.31 0.224 0.223 0.224 (2) 0.45 344 370 357 7.3 356 325 341 9.1 278 277 278 0.36 257 250 254 2.8
PFHS Concentration
(ng/mL)
1090 1120 1110 2.7 0.927 0.808 0.868 (2)
14 0.105 0.111 0.108 (2)
5.6 1430 1510 1470 5.4 1630 1460 1550
11 1030 1030 1030 0.00 544 554 549 1.8
PFOS Concentration
(ng/mL)
3430 3760 3600 9.2 3.60 3.28 3.44 (2) 9.3 0.131 0.146 0.139 (2)
11 5980 5600 5790 6.6 4920 5920 5420
18 3760 3210 3490
16 1870 1910 1890 2.1
(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 14%, PFBS 18%, PFHS 10%, and PFOS 8.0%.
(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 11 %, PFBS 21 %, PFHS 17%, and PFOS 10%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
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 March 31,2014 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 prior to being sent to the field for sample collection. Collected sample bottles were received by the laboratory at ambient conditions on April 4, 2014.
2.3 Sample Preparation
All samples were initially prepared by diluting with methanol (dilution factor of 100) and analyzing for all target analytes. 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 (nominal concentration of 1 ng/mL). Prepared samples were analyzed by external standard calibration.
The ACE and ACM2 sample sets and the Trip Blank sample and low spike were subsequently 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). Prepared samples were 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 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.
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-12-010.1 The consistency of the laboratory's integration is
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
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.1
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 DaVinci 4/15/14 - external standard calibration 5/1/14 - internal standard calibration
ETS-8-044.1 Agilent 1290 Prism RP (2.1 mm X 50 mm), 5 x Betasil C18 (2.1 mm X 100 mm), 5 x
5 xL Applied Biosystems API 6500
Turbo Spray Negative
Analyst 1.6
ETS McCoy
4/30/14- external standard calibration
ETS-8-044.1 Agilent 1290 Betasil C18 (4.6 mm X 100 mm), 5 u Betasil C18 (4.6 mm X 100 mm), 5 u 10 or 5 uL Applied Biosystems API 5500 Turbo Spray
Negative Analyst 1.6.1
Table 4. Liquid Chromatography Gradient Program (1)
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
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
(1) The flow rate was 300 |jl_/min for ETS DaVinci analyses on 4/15/14 and 5/1/14, and 750 |jl_/min for McCoy analysis on 4/30/14.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
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 5/1/14.
3 Data Analysis
3.1 Calibration
External Standard Calibration Analysis on 4/15/14 and 4/30/14: 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 ten spiked standards ranging from 0.1 ng/mL to 100 ng/mL (nominal) were analyzed. O f these ten calibration standards, eight contained the surrogates at concentrations ranging from 0.1 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 5/1/14: 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 50 mL of 50:50 methanol:laboratory reagent water. The calibration standards contained an internal standard mix at a nominal concentration of 0.5 ng/mL. A total of thirteen calibration standards ranging from 0.0125 ng/mL to 50 ng/mL (nominal) were analyzed with the prepared samples. O f these thirteen calibration standards, ten contained the surrogates at concentrations ranging from 0.0125 ng/mL to 10 ng/mL (nominal). Low or high points may have been disabled to meet method criteria. 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. ISO14-07-03
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 with the exception of the peak area count RSD for 13C4-PFOS analyzed on 4/15/14 (6.1%). A method deviation is included with 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 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 4/15/14 and 4/30/14 Analysis 111
LOQ, ng/mL 5/1/14 Analysis (2)
PFOA
9.58
0.0240
PFBS
10.0
0.0250
PFHS
10.0
0.0250
PFOS
9.27
0.0232
(1) The dilution factor of 100 was applied to the LOQ.
(2) The dilution factor of 2 was applied to the LOQ.
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 with the following exception:
5/1/14 Analysis: The mid level LCSs for PFBS had an average recovery of 78.9%. 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
______ ,, ,, ,, standard deviation LCS replicates LCS% RSD = ------------------------------------- - --------- * 100%
average LCS recovery
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
Table 7. Lab Control Spike Results.
ETS-8-044.1 External Standard Calibration Analyzed 4/15/14
Lab ID
Spiked Concentration
(ng/mL)
PFBS
Calculated Concentration
(ng/mL)
LCS-140408-1 LCS-140408-2 LCS-140408-3 Average %RSD
1.00 1.12 1.00 1.08 1.00 1.06
109% 2.8%
LCS-140408-4 LCS-140408-5 LCS-140408-6 Average %RSD LCS-140408-7 LCS-140408-8 LCS-140408-9 Average %RSD
10.0 10.8 10.0 10.4 10.0 10.3
105% 2.5%
79.4 83.6 79.4 86.5 79.4 84.6
107% 1.9%
%Recovery
Spiked Concentration
(ng/mL)
PFHS
Calculated Concentration
(ng/mL)
112 1.00
1.10
108 1.00
1.08
106 1.00
1.07
108% 1.4%
108 10.0
10.8
104 10.0
10.5
103 10.0
10.4
106% 2.0%
105 79.4
83.5
109 79.4
86.3
107 79.4
83.5
106% 2.2%
%Recovery 110 108 107
108 105 104
105 109 105
ETS-8-044.1 External Standard Calibration Analyzed 4/15/14
Lab ID
PFOA (Linear + Branched)
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
13C4-PFOA surrogate
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
LCS-140408-1 LCS-140408-2 LCS-140408-3 Average %RSD
0.958 0.958 0.958
1.09 1.06 1.07 112% 1.5%
114 111 111
0.998 0.998 0.998
1.10 1.07 1.10 109% 1.1%
110 108 110
LCS-140408-4 LCS-140408-5 LCS-140408-6 Average %RSD
9.58 10.3 9.58 9.88 9.58 10.3
106% 2.2%
107 103 107
9.98 11.1 9.98 11.2 9.98 11.7
114% 3.3%
111 112 118
LCS-140408-7 LCS-140408-8 LCS-140408-9 Average %RSD
76.0 84.8 76.0 83.7 76.0 84.4
111% 0.90%
112 110 111
(1) LCS recovery did not meet acceptance criteria of 100 20%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
Table 7 continued. Lab Control Spike Results.
ETS-8-044.1 External Standard Calibration Analyzed 4/15/14
Lab ID
PFOS (Linear + Branched)
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
13C4-PFOS surrogate
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
LCS-140408-1 LCS-140408-2 LCS-140408-3 Average %RSD
0.927 0.927 0.927
1.02 1.03 1.04 111% 0.90%
110 111 112
0.956 0.956 0.956
1.03 1.04 1.02 108% 1.4%
108 109 106
LCS-140408-4 LCS-140408-5 LCS-140408-6 Average %RSD LCS-140408-7 LCS-140408-8 LCS-140408-9 Average %RSD
9.27 9.87 9.27 9.81 9.27 10.1
107% 1.6%
73.6 78.7 73.6 81.1 73.6 81.4
109% 1.9%
106 106 109
107 110 111
9.56 10.7 9.56 10.6 9.56 10.6
111% 0.52%
112 111 111
ETS-8-044.1 External Standard Calibration Re-analysis 4/30/14
Lab ID
PFOS (Linear + Branched)
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
13C4-PFOS surrogate
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
LCS-140430-1 LCS-140430-2 LCS-140430-3 Average %RSD LCS-140430-4 LCS-140430-5 LCS-140430-6 Average %RSD
0.927 0.927 0.927
9.27 9.27 9.27
0.989 0.981 0.975 106% 0.94%
9.47 10.0 9.79 105% 2.9%
107 106 105
102 108 106
0.956 0.956 0.956
9.56 9.56 9.56
1.05 1.06 1.05 110% 0.91%
10.6 11.0 10.9 113% 2.3%
109 111 110
110 115 114
LCS-140430-7 LCS-140430-8 LCS-140430-9 Average %RSD
36.9 38.9 36.9 40.2 36.9 40.8
108% 2.4%
105 109 110
(1) LCS recovery did not meet acceptance criteria of 100 20%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
Table 7 continued. Lab Control Spike Results.
ETS-8-044.1 Internal Standard Calibration Analyzed 5/1/14
Lab ID LCS-140429-1 LCS-140429-2 LCS-140429-3 Average %RSD LCS-140429-4 LCS-140429-5 LCS-140429-6 Average %RSD LCS-140429-7 LCS-140429-8 LCS-140429-9 Average %RSD
PFOA (Linear + Branched)
Spiked Concentration
(ng/mL)
Calculated Concentration
(ng/mL)
%Recovery
13C4-PFOA surrogate
Spiked Concentration
(ng/mL)
Calculated Concentration
(ng/mL)
%Recovery
0.190 0.190 0.190
0.151 0.154 0.179 85.0% 9.5%
79.5 81.2 94.2
0.198 0.198 0.198
0.162 0.190 0.190 91.3% 9.1%
81.7 96.2 96.0
9.50 7.58 9.50 8.47 9.50 8.19
85.0% 5.6%
79.8 89.1 86.2
1.98 1.61 1.98 1.81 1.98 1.76
87.1% 5.9%
81.4 91.3 88.7
38.0 35.5 38.0 33.8 38.0 33.2
89.9% 3.5%
93.5 88.9 87.4
ETS-8-044.1 Internal Standard Calibration Analyzed 5/1/14
Lab ID LCS-140429-1 LCS-140429-2 LCS-140429-3 Average %RSD LCS-140429-4 LCS-140429-5 LCS-140429-6 Average %RSD LCS-140429-7 LCS-140429-8 LCS-140429-9 Average %RSD
Spiked Concentration
(ng/mL)
PFBS
Calculated Concentration
(ng/mL)
0.198 0.198 0.198
0.166 0.181 0.176 88.0% 4.5%
9.92 7.38 9.92 7.95 9.92 8.14
78.9% 5.0% (1)
39.6 33.3 39.6 32.5 39.6 29.7
80.4% 5.8%
%Recovery
Spiked Concentration
(ng/mL)
PFHS
Calculated Concentration
(ng/mL)
83.8 0.198
0.169
91.6 0.198
0.190
88.7 0.198
0.186
91.8% 6.1%
74.4 9.92
8.21
80.2 9.92
8.54
82.0 9.92
8.43
84.6% 2.0%
84.0 39.6
36.1
82.0 39.6
36.5
75.1 39.6
36.1
91.6% 0.50%
%Recovery 85.4 95.9 94.1
82.8 86.1 85.0
91.3 92.1 91.3
(1) LCS recovery did not meet acceptance criteria of 100 20%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
Table 7 continued. Lab Control Spike Results.
ETS-8-044.1 Internal Standard Calibration Analyzed 5/1/14
Lab ID LCS-140429-1 LCS-140429-2 LCS-140429-3 Average %RSD LCS-140429-4 LCS-140429-5 LCS-140429-6 Average %RSD LCS-140429-7 LCS-140429-8 LCS-140429-9 Average %RSD
PFOS (Linear + Branched)
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
13C4-PFOS surrogate
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
0.184 0.184 0.184
0.173 0.153 0.167 89.2% 6.5%
94.2 82.9 90.6
0.189 0.189 0.189
0.170 0.164 0.183 91.2% 5.6%
90.0 86.9 96.8
9.20 7.56 9.20 8.11 9.20 8.09
86.1% 4.0%
82.1 88.2 88.0
1.90 1.62 1.90 1.75 1.90 1.75
89.9% 4.3%
85.4 92.0 92.3
36.7 32.4 36.7 32.7 36.7 34.0
90.0% 2.5%
88.3 89.1 92.6
(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 analytical method uncertainty as calculated by ETS-12-012.2 for PFBS by internal standard calibration was 11%. The recovery of the mid set of LCS analyzed on 5/1/14 was 78.9% for PFBS by internal standard calibration for the samples analyzed on this date. The analytical uncertainty was expanded to 21 %.
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 (%) 7.04 9.03 5.05 4.02 5.38 NA 8.55 5.21
NA = Not Applicable
Method Uncertainty 14% 18% 10% 8.0% 11% 21% 17% 10%
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
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. Table 9 lists the concentrations of the field matrix spikes used for this sampling round. 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 spike recoveries and associated results for each sample set 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
1980 4.94 2470 1980 4.94
1980 4.95 2480 1980 4.95
1980 4.95 2480 1980 4.95
1980 4.95 2480 1980 4.95
2470
2480
2480
2480
In addition to target analyte field matrix spikes, sample bottles for locations ACM2 and ACE, along with the Trip Blank sample and low spike, contained stable isotope surrogate recovery standards 13C4PFOA and 13C4-PFOS, which were added at a nominal concentration of 0.1 ng/mL prior to sample collection. The 13C4-labeled PFOA were selected to represent PFOA. The 13C4-labeled PFOS was selected to represent the C4, C6, and C8 perfluorosulfonic acids. Surrogate recoveries within method acceptance criteria of 10030% confirm that "unknown" components in the sample matrix do not significantly interfere with the preparation and analysis of the analytes of interest. The surrogate spike recoveries are presented in section 4 of this report.
Calculated Concentration,,.,.,.... SRS Recovery = ---------------------------------------- *100%
Spike Concentration
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.
PAGE 12 OF 24
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
For those analytes where the field matrix spike level was not appropriate as compared to the sample concentration, the surrogate recovery standards were used to assess method accuracy. For all sampling locations, surrogate recovery standards where applicable and field matrix spike recoveries met method acceptance criteria (where applicable).
Table 10. DAL GW ACI 140331 (1)
3M LIMS ID
Sample Description
ISO14-07-03-001
DAL-GW-ACI-0 - 140331
ISO14-07-03-002
DAL-GW-ACI-DB - 140331
ISO14-07-03-003
DAL-GW-ACI-FMS - 140331
Average Concentration (ng/mL) %RPD
PFOA
PFBS
Concentration
(ng/mL)
%Recovery
2350
NA
2470
NA
4680
115
2140 ng/mL 5.0%
Concentration
(ng/mL)
%Recovery
536 NA
546 NA
2540
101
541 ng/mL 1.8%
3M LIMS ID
Sample Description
ISO14-07-03-001
DAL-GW-ACI-0 - 140331
ISO14-07-03-002
DAL-GW-ACI-DB - 140331
ISO14-07-03-003
DAL-GW-ACI-FMS - 140331
Average Concentration (ng/mL) %RPD
PFHS
PFOS
Concentration
(ng/mL)
%Recovery
1090
NA
1120
NA
3330
112
1110 ng/mL 2.7%
Concentration
(ng/mL)
%Recovery
3430
NA
3760
NA
6110
127
3600 ng/mL 9.2%
13C4-PFOA
13C4-PFOS
3M LIMS ID
Sample Description
ISO14-07-03-001
DAL-GW-ACI-0 - 140331
ISO14-07-03-002
DAL-GW-ACI-DB - 140331
ISO14-07-03-003
DAL-GW-ACI-FMS - 140331
Average Concentration (ng/mL) %RSD
%Recovery
104 104 94.9 101% 5.3%
%Recovery
101 98.0 94.8 98.0% 3.4%
NA = Not Applicable (1) Samples were analyzed by external standard calibration on 4/15/14. The surrogate recovery standards 13C4-PFOA and 13C4-
PFOS were added to the samples during sample preparation.
PAGE 13 OF 24
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
Table 11. DAL GW ACM2 140331
3M LIMS ID
Sample Description
ISO14-07-03-004
DAL-GW-ACM2-0 - 140331
ISO14-07-03-005
DAL-GW-ACM2-DB - 140331
ISO14-07-03-006
DAL-GW-ACM2-FMS - 140331
Average Concentration (ng/mL) %RPD
3M LIMS ID
Sample Description
ISO14-07-03-004
DAL-GW-ACM2-0 - 140331
ISO14-07-03-005
DAL-GW-ACM2-DB - 140331
ISO14-07-03-006
DAL-GW-ACM2-FMS - 140331
Average Concentration (ng/mL) %RPD
PFOA (1)
PFBS (2)
Concentration
(ng/mL)
%Recovery
2.15 NA 1.91 NA 7.02 101 2.03 ng/mL 12%
Concentration
(ng/mL)
%Recovery
3240
NA
3230
NA
3220
NC
3240 ng/mL 0.31%
PFHS (1)
PFOS (1)
Concentration
(ng/mL)
%Recovery
0.927
NA
0.808
NA
5.67 97.0
0.868 ng/mL 14%
Concentration
(ng/mL)
%Recovery
3.60 NA 3.28 NA 8.27 97.6 3.44 ng/mL 9.3%
13C4-PFOA (1) 13C4-PFOS (1) 13C4-PFOS (2)
3M LIMS ID
Sample Description
ISO14-07-03-004
DAL-GW-ACM2-0 - 140331
ISO14-07-03-005
DAL-GW-ACM2-DB - 140331
ISO14-07-03-006
DAL-GW-ACM2-FMS - 140331
Average Concentration (ng/mL) %RSD
%Recovery
101 103 98.8 101% 2.1%
%Recovery
97.4 92.1 108 99.1% 8.1%
%Recovery
107 108 114 109% 3.6%
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 on 5/1/14. (2) Samples were analyzed by external standard calibration on 4/15/14. The surrogate recovery standard 13C4-PFOS was added
to the samples during sample preparation.
PAGE 14 OF 24
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
Table 12. DAL GW ACE 140331 (1)
3M LIMS ID
Sample Description
ISO14-07-03-007
DAL-GW-ACE-0 - 140331
ISO14-07-03-008
DAL-GW-ACE-DB - 140331
ISO14-07-03-009
DAL-GW-ACE-FMS - 140331
Average Concentration (ng/mL) %RPD
3M LIMS ID
Sample Description
ISO14-07-03-007
DAL-GW-ACE-0 - 140331
ISO14-07-03-008
DAL-GW-ACE-DB - 140331
ISO14-07-03-009
DAL-GW-ACE-FMS - 140331
Average Concentration (ng/mL) %RPD
PFOA
PFBS
Concentration
(ng/mL)
%Recovery
0.257
NA
0.266
NA
4.95 94.9
0.262 ng/mL 3.4%
Concentration
(ng/mL)
%Recovery
0.224
NA
0.223
NA
5.21 101
0.224 ng/mL 0.45%
PFHS
PFOS
Concentration
(ng/mL)
%Recovery
0.105
NA
0.111
NA
4.90 96.8
0.108 ng/mL 5.6%
Concentration
(ng/mL)
%Recovery
0.131
NA
0.146
NA
4.90 96.2
0.139 ng/mL 11%
13C4-PFOA
13C4-PFOS
3M LIMS ID
Sample Description
ISO14-07-03-007
DAL-GW-ACE-0 - 140331
ISO14-07-03-008
DAL-GW-ACE-DB - 140331
ISO14-07-03-009
DAL-GW-ACE-FMS - 140331
Average Concentration (ng/mL) %RSD
%Recovery
98.3 107 94.5 99.8% 6.2%
%Recovery
91.2 107 96.4 98.2% 8.1%
NA = Not Applicable (1) Samples were analyzed by internal standard calibration on 5/1/14.
PAGE 15 OF 24
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
Table 13. DAL GW WW8R 140331 (1)
3M LIMS ID
Sample Description
ISO14-07-03-010
DAL-GW-WW8R-0 - 140331
ISO14-07-03-011
DAL-GW-WW8R-DB - 140331
ISO14-07-03-012
DAL-GW-WW8R-FMS - 140331
Average Concentration (ng/mL) %RPD
3M LIMS ID
Sample Description
ISO14-07-03-010
DAL-GW-WW8R-0 - 140331
ISO14-07-03-011
DAL-GW-WW8R-DB - 140331
ISO14-07-03-012
DAL-GW-WW8R-FMS - 140331
Average Concentration (ng/mL) %RPD
PFOA
PFBS
Concentration
(ng/mL)
%Recovery
3330
NA
3240
NA
6200
118
3290 ng/mL 2.7%
Concentration
(ng/mL)
%Recovery
344 NA
370 NA
3310
119
357 ng/mL 7.3%
PFHS
PFOS
Concentration
(ng/mL)
%Recovery
1430
NA
1510
NA
4420
119
1470 ng/mL 5.4%
Concentration
(ng/mL)
%Recovery
5980
NA
5600
NA
8730
119
5790 ng/mL 6.6%
13C4-PFOA
13C4-PFOS
3M LIMS ID
Sample Description
ISO14-07-03-010
DAL-GW-WW8R-0 - 140331
ISO14-07-03-011
DAL-GW-WW8R-DB - 140331
ISO14-07-03-012
DAL-GW-WW8R-FMS - 140331
Average Concentration (ng/mL) %RSD
%Recovery
103 104 91.4 99.6% 7.2%
%Recovery
92.8 98.2 90.2 93.7% 4.4%
NA = Not Applicable (1) Samples were analyzed by external standard calibration on 4/15/14. The surrogate recovery standards 13C4-PFOA and 13C4-
PFOS were added to the samples during sample preparation.
PAGE 16 OF 24
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
Table 14. DAL GW WW9R 140331
3M LIMS ID
Sample Description
ISO14-07-03-013
DAL-GW-WW9R-0 - 140331
ISO14-07-03-014
DAL-GW-WW9R-DB - 140331
ISO14-07-03-015
DAL-GW-WW9R-FMS - 140331
Average Concentration (ng/mL) %RPD
3M LIMS ID
Sample Description
ISO14-07-03-013
DAL-GW-WW9R-0 - 140331
ISO14-07-03-014
DAL-GW-WW9R-DB - 140331
ISO14-07-03-015
DAL-GW-WW9R-FMS - 140331
Average Concentration (ng/mL) %RPD
PFOA (1)
PFBS (1)
Concentration
(ng/mL)
%Recovery
3580
NA
3180
NA
5850
100
3380 ng/mL 12%
Concentration
(ng/mL)
%Recovery
356 NA
325 NA
3020
108
341 ng/mL 9.1%
PFHS (1)
PFOS (2)
Concentration
(ng/mL)
%Recovery
1630
NA
1460
NA
4130
104
1550 ng/mL 11%
Concentration
(ng/mL)
%Recovery
4920
NA
5920
NA
7390
79.6
5420 ng/mL 18%
13C4-PFOA (1) 13C4-PFOS (1) 13C4-PFOS (2)
3M LIMS ID
Sample Description
ISO14-07-03-013
DAL-GW-WW9R-0 - 140331
ISO14-07-03-014
DAL-GW-WW9R-DB - 140331
ISO14-07-03-015
DAL-GW-WW9R-FMS - 140331
Average Concentration (ng/mL) %RSD
%Recovery
101 103 90.2 98.2% 7.1%
%Recovery
85.4 89.7 88.6 87.9% 2.6%
%Recovery
109 105 106 107% 1.8%
NA = Not Applicable (1) Samples were analyzed by external standard calibration on 4/15/14. The surrogate recovery standards 13C4-PFOA and 13C4-
PFOS were added to the samples during sample preparation. (2) Samples were analyzed by external standard calibration on 4/30/14. The surrogate recovery standard 13C4-PFOS was added
to the samples during sample preparation.
PAGE 17 OF 24
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
Table 15. DAL GW WW10R 140331 (1)
3M LIMS ID
Sample Description
ISO14-07-03-016
DAL-GW-WW10R-0 - 140331
ISO14-07-03-017
DAL-GW-WW10R-DB - 140331
ISO14-07-03-018
DAL-GW-WW10R-FMS - 140331
Average Concentration (ng/mL) %RPD
PFOA
PFBS
Concentration
(ng/mL)
%Recovery
2110
NA
2170
NA
4070
97.7
2140 ng/mL 2.8%
Concentration
(ng/mL)
%Recovery
278 NA
277 NA
2260
100
278 ng/mL 0.36%
3M LIMS ID
Sample Description
ISO14-07-03-016
DAL-GW-WW10R-0 - 140331
ISO14-07-03-017
DAL-GW-WW10R-DB - 140331
ISO14-07-03-018
DAL-GW-WW10R-FMS - 140331
Average Concentration (ng/mL) %RPD
PFHS
PFOS
Concentration
(ng/mL)
%Recovery
1030
NA
1030
NA
3030
101
1030 ng/mL 0.0%
Concentration
(ng/mL)
%Recovery
3760
NA
3210
NA
5980
126
3490 ng/mL 16%
13C4-PFOA
13C4-PFOS
3M LIMS ID
Sample Description
ISO14-07-03-016
DAL-GW-WW10R-0 - 140331
ISO14-07-03-017
DAL-GW-WW10R-DB - 140331
ISO14-07-03-018
DAL-GW-WW10R-FMS - 140331
Average Concentration (ng/mL) %RSD
%Recovery
106 109 94.0 103% 7.8%
%Recovery
99.0 98.6 91.5 96.4% 4.4%
NA = Not Applicable (1) Samples were analyzed by external standard calibration on 4/15/14. The surrogate recovery standards 13C4-PFOA and 13C4-
PFOS were added to the samples during sample preparation.
PAGE 18 OF 24
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
Table 16. DAL GW WW11R 140331
3M LIMS ID
Sample Description
ISO14-07-03-019
DAL-GW-WW11R-0 - 140331
ISO14-07-03-020
DAL-GW-WW11R-DB - 140331
ISO14-07-03-021
DAL-GW-WW11R-FMS - 140331
Average Concentration (ng/mL) %RPD
PFOA (1)
PFBS (1)
Concentration
(ng/mL)
%Recovery
1190
NA
1180
NA
3450
115
1190 ng/mL 0.84%
Concentration
(ng/mL)
%Recovery
257 NA
250 NA
2350
106
254 ng/mL 2.8%
3M LIMS ID
Sample Description
ISO14-07-03-019
DAL-GW-WW11 R-0 - 140331
ISO14-07-03-020
DAL-GW-WW11 R-DB - 140331
ISO14-07-03-021
DAL-GW-WW11 R-FMS - 140331
Average Concentration (ng/mL) %RPD
PFHS (1)
PFOS (2)
Concentration
(ng/mL)
%Recovery
544 NA
554 NA
2590
103
549 ng/mL 1.8%
Concentration
(ng/mL)
%Recovery
1870
NA
1910
NA
3850
99.0
1890 ng/mL 2.1%
13C4-PFOA (1) 13C4-PFOS (1) 13C4-PFOS (2)
3M LIMS ID
Sample Description
ISO14-07-03-019
DAL-GW-WW11 R-0 - 140331
ISO14-07-03-020
DAL-GW-WW11 R-DB - 140331
ISO14-07-03-021
DAL-GW-WW11 R-FMS - 140331
Average Concentration (ng/mL) %RSD
%Recovery
108 108 98.7 105% 5.2%
%Recovery
102 102 98.2 101% 2.0%
%Recovery
107 106 101 104% 2.8%
NA = Not Applicable (1) Samples were analyzed by external standard calibration on 4/15/14. The surrogate recovery standards 13C4-PFOA and 13C4-
PFOS were added to the samples during sample preparation. (2) Samples were analyzed by external standard calibration on 4/30/14. The surrogate recovery standard 13C4-PFOS was added
to the samples during sample preparation.
PAGE 19 OF 24
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
Table 17. Trip Blank Results
3M LIMS ID
ISO14-07-03-022 ISO14-07-03-023 ISO14-07-03-024
Sample Description
DAL-GW-TRIP-0 - 140331 DAL-GW-TRIP-LS - 140331 DAL-GW-TRIP-HS - 140331
3M LIMS ID
ISO14-07-03-022 ISO14-07-03-023 ISO14-07-03-024
Sample Description
DAL-GW-TRIP-0 - 140331 DAL-GW-TRIP-LS - 140331 DAL-GW-TRIP-HS - 140331
PFOA
PFBS
Concentration (ng/mL)
<0.0240 (1) 4.89 (1) 2840 (2)
%Recovery
NA 99.0 115
Concentration (ng/mL)
<0.0250 (1) 4.74 (1) 2490 (2)
%Recovery
NA 95.8 101
PFHS
PFOS
Concentration (ng/mL)
<0.0250 (1) 4.61 (1) 2690 (2)
%Recovery
NA 93.1 109
Concentration (ng/mL)
<0.0232 (1) 4.90 (1) 2910 (2)
%Recovery
NA 92.9 118
13C4-PFOA (1) 13C4-PFOS (1) 13C4-PFOA (2) 13C4-PFOS (2)
3M LIMS ID ISO14-07-03-022 ISO14-07-03-023 ISO14-07-03-024
Sample Description DAL-GW-TRIP-0 - 140331 DAL-GW-TRIP-LS - 140331 DAL-GW-TRIP-HS - 140331
%Recovery 98.9 106 NA
%Recovery 106 95.4 NA
%Recovery 101 103 100
%Recovery 94.7 98.5 100
NA = Not Applicable (1) Samples were analyzed by internal standard calibration on 5/1/14. (2) Samples were analyzed by external standard calibration on 4/15/14. The surrogate recovery standards 13C4-PFOA and 13C4-
PFOS were added to the samples during sample preparation
PAGE 20 OF 24
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
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 Trend Data for the Decatur Ground Water Treatment Plant (GWTP) GAC System.
8 Signatures
cJj
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 have reviewed this document Date: 2014.05.19 15:50:44 -05*00*
Susan T. Wolf, 3M Principal Analytical Investigator
Digitally signed by William K. Reagen DN: c=US. st=MIN. l=St. Paul. ou=Laboratory Director. ou=3M Environmental Laboratory -
Reason: I am approving this document Date: 2014.05.20 14:35:21 -05'00'
William K. Reagen, Ph.D., 3M Environmental Laboratory Technical Director
The 3M Environmental Laboratory's Quality Assurance Unit has audited the data and report for this project.
Digitally signed by Tanya K. Rude DN: c=US, st=MN, l=St. Paul, ou=3M Environmental Laboratory - authenticated by LRA, email=trude@mmm.com, o=3M, cn=Tanya K.
placement o f m y signature on this document Date: 2014.05.20 06:41:39 -05'00'
Quality Assurance Representative
This test report shall not be reproduced except in full, without written approval o f the 3M Environmental Laboratory.
PAGE 21 OF 24
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
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
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
1/30/14 1580 202 845 2700
2/27/14 1870 1470 737 1800
3/31/14 2410 541 1110 3600
ACE (Activated Carbon Effluent) - Sample Results in ng/mL
FC Charting for DAL GWTP ACE
PFOA------- -------PFOS------- --------
PFBS------- --------
PFHS-------
ACE PFOA PFBS PFHS PFOS
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
1/30/14 0.490 0.257 0.219 0.209
2/27/14 0.138
0.0360 0.0706 0.0966
3/31/14 0.262 0.224 0.108 0.139
PAGE 22 OF 24
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
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
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
WW9R - Sample Results in ng/mL
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
1/30/14 2660 326 1460 3990
2/27/14 2560 331 1370 4170
3/31/14 3290 357 1470 5790
W W 9R PFOA PFBS PFHS PFOS
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
1/30/14 2900 317 1460 4800
2/27/14 2630 270 1370 4660
3/31/14 3380 341 1550 5420
PAGE 23 OF 24
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-03
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
9/30/13 2070 247 1030 2770
10/28/13 2150 264 1030 3160
11/18/13 2400 303 1120 3890
12/13/13 1890 239 885 2920
1/30/14 1330 250 757 1570
2/27/14 1780 260 935 2860
3/31/14 2140 278 1030 3490
WW11R - Sample Results in ng/mL
W W 11R PFOA PFBS PFHS PFOS
9/30/13 1720 299 1000 2200
10/28/13 1100 240 511 1670
11/18/13 1320 287 680 1850
12/13/13 1060 198 512 1570
1/30/14 814 168 362
1540
2/27/14 1300 262 696 2100
3/31/14 1190 254 549 1890
PAGE 24 OF 24
