Document KGaV44nYZXeB12DZLBedx3Oq6
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
Final Report
Analysis of PFOA, PFBS, PFHS, and PFOS in Aqueous Samples from 3M Decatur, Alabama: Groundwater Treatment Plant GAC System April 2014
Laboratory Request Number: ISO14-07-04 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. ISO14-07-04
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 ISO14-07-04
3M Decatur Groundwater Treatment Plant System; April 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 April 23, 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 ISO14-07-04. 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. ISO14-07-04
Table 1. Sample Results Summary (1)
3M LIMS ID
Sample Description
PFOA Concentration
(ng/mL)
ISO14-07-04-001 ISO14-07-04-002
ISO14-07-04-004 ISO14-07-04-005
ISO14-07-04-007 ISO14-07-04-008
ISO14-07-04-010 ISO14-07-04-011
ISO14-07-04-013 ISO14-07-04-014
ISO14-07-04-016 ISO14-07-04-017
ISO14-07-04-019 ISO14-07-04-020
DAL-GW-ACI-0-140423 DAL-GW-ACI-DB-140423
Average %RPD Sample/Sample Dup DAL-GW-ACM2-0-140423 DAL-GW-ACM2-DB-140423
Average %RPD Sample/Sample Dup DAL-GW-ACE-0-140423 DAL-GW-ACE-DB-140423
Average %RPD Sample/Sample Dup DAL-GW-WW8R-0-140423 DAL-GW-WW8R-DB-140423
Average %RPD Sample/Sample Dup DAL-GW-WW9R-0-140423 DAL-GW-WW9R-DB-140423
Average %RPD Sample/Sample Dup DAL-GW-WW10R-0-140423 DAL-GW-WW10R-140423
Average %RPD Sample/Sample Dup DAL-GW-WW11R-0-140423 DAL-GW-WW11R-DB-140423
Average %RPD Sample/Sample Dup
2080 2070 2080 0.48 0.128 0.108 0.118 1(2)
17 0.175 0.168 0.172 (2) 4.1 2690 2760 2730
2.6 2770 2860 2820 3.2 1850 1850 1850 0.00 1110 1130 1120 1.8
PFBS Concentration
(ng/mL)
1230 1260 1250 2.4 2610 2590 2600 0.77 67.4 71.9 69.7 4.3 280 285 283 1.8 256 257 257 0.39 240 246 243 2.5 207 216 212 4.3
PFHS Concentration
(ng/mL)
785 794 790 1.1 0.154 0.153 0.154 (2) 0.65 0.0742 0.0881 0.0812 (2) 17 1180 1170 1180 0.85 1090 1140 1120 4.5 888 882 885 0.68 526 527 527 0.19
PFOS Concentration
(ng/mL)
1440 1520 1480 5.4 0.310 0.309 0.310 (2) 0.32 0.0566 0.0567 0.0567 (2) 0.18 3770 3910 3840 3.6 3580 4060 3820 (3) 13 2190 2060 2130 (3) 6.1 1480 1770 1630 18
(1) Reported results from samples prepared and analyzed by ETS-8-044.1 using external standard calibration except where otherwise noted. The analytical method uncertainties associated with the reported results are as follows: PFOA 11 %, PFBS 11%, PFHS 11%, and PFOS 10%.
(2) Sample set 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 14%, PFBS 22%, PFHS 11 %, and PFOS 16%.
(3) Results obtained without concurrent preparation and analysis of LCSs as a quality control measure. See section 3.6 and 4 for details.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
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 April 23, 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 May 1,2014.
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). On-column sample dilution was utilized for dilution levels of 200-fold. 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
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
procedures outlined in SOP ETS-12-010.1 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 McCoy 5/06/14- external standard calibration 5/12/14 - internal standard calibration 5/29/14 - 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
Step Number
0 1 2 3 4 5 6 7 8 9
Total Time (min)
0.0 0.50 4.00 6.00 11.00 13.00 13.50 16.00 16.50 19.00
Flow Rate (uL/min)
Percent A (2 mM ammonium acetate)
ETS-8-044.1 Analysis 750 750 750 750 750 750 750 750 750 750
90 90 70 70 20 20 10 10 90 90
Percent B (Methanol)
10 10 30 30 80 80 90 90 10 10
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
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 5/12/14.
3 Data Analysis
3.1 Calibration
External Standard Calibration Analysis on 5/6/14 and 5/29/14: 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 twelve spiked standards ranging from 0.02 ng/mL to 100 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 5/12/14: Samples were analyzed for all analytes 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 (0.0125 ng/mL to 10 ng/mL (nominal) for the SRSs). 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 the analysis on 5/12/14, there was a period near the middle of the internal standard calibration curve where the instrument failed to provide reliable chromatography. This resulted in an either a highly inaccurate calibration standard concentration or decreased confidence in the ability of the chromatogram to represent the analyte of interest. A single mid-level standard for PFOA, PFBS, and PFHS was disabled to give the best and most reliable curve. This is a deviation from the method, but was required for proper quantitation.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
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.
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 PFBS analyzed on 5/6/14 (7.7%). A method deviation is filed 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
PFOA PFBS PFHS PFOS
LOQ, ng/mL 5/6/14 Analysis (1)
1.92 5.00 2.00 1.85
LOQ, ng/mL 5/6/14 Analysis (2)
3.84 10.0 4.00 3.70
LOQ, ng/mL 5/12/14 Analysis (3)
0.0480 0.0500 0.0250 0.0232
LOQ, ng/mL 5/29/14 Analysis (4)
NA NA NA 18.5
NA = Not Applicable (1) The dilution factor of 100 was applied to the LOQ. Analysis for the Trip Blank HS and locations ACM2 and ACE for PFBS. (2) The dilution factor of 200 was applied to the LOQ. Analysis for locations ACI, WW8R, WW9R, WW10R, and WW11R. (3) The dilution factor of 2 was applied to the LOQ. Analysis for the Trip Blank sample and low spike, and locations ACM2 and
ACE for PFOA, PFHS, and PFOS. (4) The dilution factor of 200 was applied to the LOQ. Analysis for location WW11R for PFOS.
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. 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:
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
5/12/14 Analysis: The mid level LCSs for PFBS had an average recovery of 77.8%. A method deviation is included with the raw data and the analytical method uncertainty has been expanded for sample results for PFBS obtained via internal standard calibration.
According to ETS-8-044.1, low lab control spikes should be prepared at a concentration in the range of approximately four to ten times higher than the targeted lower LOQ , the mid LCS should be prepared near the midpoint of the calibration curve and the high lab control spikes at approximately 80% of the upper LOQ (ULOQ). For the analysis on 5/6/14, the low LCS concentrations (nominal 1 ng/mL) were greater than ten times the LLOQ and the high LCS concentrations (nominal 40 ng/mL) were less than 80% of the ULOQ. The high level LCSs were spiked at a lower concentration to represent the majority of the analytes based on the expected sample concentrations. While the high LCS concentrations were not within 80% of the ULOQ, all sample concentrations were within the concentration range of the three spiked LCS levels. In the future, LCSs will be prepared that cover a wider range of the calibration curve and the expected values. A method deviation has been included with the raw data.
5/29/14 analysis: Samples associated with locations WW9R and WW10R were re-prepared and analyzed for PFOS to confirm the FMS recoveries from initial sample analysis on 5/6/14. No LCSs were included in the analytical batch. A method deviation is filed with the raw data. See section 4 for discussion.
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. ISO14-07-04
Table 7. Lab Control Spike Results.
ETS-8-044.1 External Standard Calibration Analyzed 5/6/14
Lab ID
Spiked Concentration
(ng/mL)
PFBS
Calculated Concentration
(ng/mL)
LCS-140506-1 LCS-140506-2 LCS-140506-3 Average %RSD
1.00 0.972 1.00 1.01 1.00 0.986
98.9% 1.9%
LCS-140506-4 LCS-140506-5 LCS-140506-6 Average %RSD LCS-140506-7 LCS-140506-8 LCS-140506-9 Average %RSD
10.0 10.4 10.0 10.4 10.0 10.9
106% 2.7%
39.8 46.3 39.8 45.4 39.8 47.3
116% 2.2%
%Recovery
Spiked Concentration
(ng/mL)
PFHS
Calculated Concentration
(ng/mL)
97.2 1.00
1.01
101 1.00
1.02
98.6 1.00
1.00
101% 1.1%
104 10.0
10.7
104 10.0
10.9
109 10.0
11.1
109% 1.8%
116 39.8
45.5
114 39.8
43.5
119 39.8
44.7
112% 2.3%
%Recovery 101 102 99.7
107 109 111
114 109 112
ETS-8-044.1 External Standard Calibration Analyzed 5/6/14
Lab ID
PFOA (Linear + Branched)
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
PFOS (Linear + Branched)
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
LCS-140506-1 LCS-140506-2 LCS-140506-3 Average %RSD LCS-140506-4 LCS-140506-5 LCS-140506-6 Average %RSD
0.958 0.958 0.958
9.58 9.58 9.58
0.952 0.987 0.966 101% 1.8%
10.4 10.3 10.6 109% 1.8%
99.4 103 101
109 107 111
0.927 0.927 0.927
9.27 9.27 9.27
0.966 1.00 0.990 106% 2.0%
10.4 10.3 10.5 112% 0.89%
104 108 107
112 111 113
LCS-140506-7 LCS-140506-8 LCS-140506-9 Average %RSD
38.2 44.0 38.2 41.9 38.2 42.5
112% 2.4%
115 110 111
36.9 42.3 36.9 40.4 36.9 41.3
112% 2.7%
115 109 112
(1) LCS average recovery did not meet method acceptance criteria of 100 20%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
Table 7 continued. Lab Control Spike Results.
ETS-8-044.1 External Standard Calibration Analyzed 5/6/14
Lab ID
13C4 -PFOA surrogate
Spiked Concentration
(ng/mL)
Calculated Concentration
(ng/mL)
%Recovery
13C4 -PFOS surrogate
Spiked Concentration
(ng/mL)
Calculated Concentration
(ng/mL)
%Recovery
LCS-140506-1 LCS-140506-2 LCS-140506-3 Average %RSD
0.998 0.998 0.998
1.07 1.08 1.13 110% 2.6%
108 108 113
0.956 0.956 0.956
1.02 1.04 1.05 108% 1.6%
106 109 109
LCS-140506-4 LCS-140506-5 LCS-140506-6 Average %RSD
9.98 11.7 9.98 11.9 9.98 12.0
119% 1.3%
117 119 120
9.56 11.2 9.56 11.4 9.56 11.4
119% 0.49%
118 119 119
ETS-8-044.1 Internal Standard Calibration Analyzed 5/12/14
Lab ID LCS-140512-1 LCS-140512-2 LCS-140512-3 Average %RSD LCS-140512-4 LCS-140512-5 LCS-140512-6 Average %RSD LCS-140512-7 LCS-140512-8 LCS-140512-9 Average %RSD
Spiked Concentration
(ng/mL)
PFBS
Calculated Concentration
(ng/mL)
0.198 0.198 0.198
0.200 0.201 0.193 100% 2.2%
9.92 7.42 9.92 7.71 9.92 8.04
77.8% 4.0% (1)
39.6 35.2 39.6 34.1 39.6 35.3
88.1% 1.9%
%Recovery
Spiked Concentration
(ng/mL)
PFHS
Calculated Concentration
(ng/mL)
101 0.198 0.216
102 0.198
0.203
97.7 0.198
0.199
104% 4.2%
74.8 9.92
9.74
77.7 9.92
9.56
81.0 9.92
8.59
93.7% 6.7%
89.0 39.6
42.3
86.2 39.6
38.5
89.2 39.6
40.4
102% 4.8%
%Recovery 109 102 101
98.2 96.4 86.6
107 97.3 102
(1) LCS average recovery did not meet method acceptance criteria of 100 20%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
Table 7 continued. Lab Control Spike Results.
ETS-8-044.1 Internal Standard Calibration Analyzed 5/12/14
Lab ID LCS-140512-1 LCS-140512-2 LCS-140512-3 Average %RSD LCS-140512-4 LCS-140512-5 LCS-140512-6 Average %RSD LCS-140512-7 LCS-140512-8 LCS-140512-9 Average %RSD
PFOA (Linear + Branched)
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
PFOS (Linear + Branched)
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
0.190 0.190 0.190
0.205 0.201 0.225 111% 6.3%
108 106 119
0.184 0.184 0.184
0.196 0.208 0.204 110% 3.3%
106 113 111
9.50 8.64 9.50 8.65 9.50 8.92
91.9% 1.9%
90.9 91.0 93.9
9.20 8.14 9.20 8.22 9.20 8.52
90.2% 2.4%
88.5 89.4 92.6
38.0 36.2 38.0 35.1 38.0 38.6
96.5% 5.1%
95.2 92.4 102
36.7 38.1 36.7 37.8 36.7 37.1
103% 1.5%
104 103 101
ETS-8-044.1 Internal Standard Calibration Analyzed 5/12/14
Lab ID LCS-140512-1 LCS-140512-2 LCS-140512-3 Average %RSD LCS-140512-4 LCS-140512-5 LCS-140512-6 Average %RSD
13C4 -PFOA surrogate
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
13C4-PFOS surrogate
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
0.198 0.198 0.198
0.186 0.188 0.212 98.6% 7.4%
93.9 95.0 107
0.189 0.189 0.189
0.177 0.209 0.200 103% 8.8%
93.4 111 106
1.98 1.92 1.98 2.12 1.98 2.00
102% 5.0%
96.9 107 101
1.90 1.85 1.90 2.00 1.90 1.89
101% 3.9%
97.4 105 99.7
(1) LCS average recovery did not meet method acceptance criteria of 100 20%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
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 13%. The recovery of the mid set of LCSs for PFBS analyzed on 5/12/14 was 77.8%; therefore, the analytical method uncertainty was expanded to 22% based on the LCS recovery %bias.
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 (%) 5.56 5.74 5.34 5.12 7.01 NA 5.60 8.24
Method Uncertainty 11% 11% 11% 10% 14% 22% 11% 16%
NA = Not Applicable
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 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.
The following calculation was used to generate data in section 4.
FMS Recovery - (Sample Concentration of FMS - Average Concentration: Field Sample & Field Sample Dup.) *100% Spike Concentraton
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3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
Table 9. Field Matrix Spike Concentrations.
Final Concentration (ng/mL
Location ACI ACM2 A C E (1) WW8R, WW9R WW10R, WW11R
Trip Blank
Description
Field Matrix Spike Field Matrix Spike Field Matrix Spike Field Matrix Spike Field Matrix Spike Low Field Matrix Spike High Field Matrix Spike
PFOA
1980 4.94 4.47 2470 1980 4.94 2470
PFBS
1980 4.95 4.48 2480 1980 4.95 2480
PFHS
1980 4.95 4.48 2480 1980 4.95 2480
PFOS
1980 4.95 4.48 2480 1980 4.95 2480
(1) Sample bottle was overfilled by more than 10%. The FMS spike levels were adjusted accordingly.
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 was 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. Surrogate spike recoveries are presented in section 4 of this report.
The following calculation was used to generate data in section 4.
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.
All field samples met method acceptance criteria with the following exception:
The FMS spike level at 5 ng/mL was not appropriate for PFBS for sampling locations ACM2 and ACE. However, the surrogate recovery standard l3C4-PFOS met method acceptance criteria and therefore; no additional QC samples were prepared.
During the initial sample analysis on 5/6/14, the FMS recoveries for PFOS for sampling locations WW9R and WW10R did not meet acceptance criteria of 30%. The samples were re-prepared and analyzed against an external standard calibration curve to verify the FMS results on 5/29/14. Re analysis of these samples produced FMS recoveries that met method acceptance criteria; however, LCSs were not prepared and included with the re-analysis. This is a deviation from the method. The
PAGE 13 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
presence of other compliant QC measures; system suitability, curve accuracy and fit, surrogate recoveries, CCVs, and FMS recovery, support the reporting of this data. Data is reported and flagged in Tables 1, 14, and 15.
Table 10. DAL GW ACI 140423 (1)
3M LIMS ID
Sample Description
ISO14-07-04-001
DAL-GW-ACI-0-140423
ISO14-07-04-002
DAL-GW-ACI-DB-140423
ISO14-07-04-003
DAL-GW-ACI-FMS-140423
Average Concentration (ng/mL) %RPD
PFOA
PFBS
Concentration
(ng/mL)
%Recovery
2080
NA
2070
NA
3840
89.3
2080 ng/mL 0.48%
Concentration
(ng/mL)
%Recovery
1230
NA
1260
NA
3180
97.7
1250 ng/mL 2.4%
3M LIMS ID
Sample Description
ISO14-07-04-001
DAL-GW-ACI-0-140423
ISO14-07-04-002
DAL-GW-ACI-DB-140423
ISO14-07-04-003
DAL-GW-ACI-FMS-140423
Average Concentration (ng/mL) %RPD
PFHS
PFOS
Concentration
(ng/mL)
%Recovery
785 NA
794 NA
2730
98.0
790 ng/mL 1.1%
Concentration
(ng/mL)
%Recovery
1440
NA
1520
NA
3010
77.3
1480 ng/mL 5.4%
13C4-PFOA
13C4-PFOS
3M LIMS ID
Sample Description
ISO14-07-04-001
DAL-GW-ACI-0-140423
ISO14-07-04-002
DAL-GW-ACI-DB-140423
ISO14-07-04-003
DAL-GW-ACI-FMS-140423
Average Concentration (ng/mL) %RSD
%Recovery
112 111 107 110% 2.7%
%Recovery
105 106 103 105% 1.3%
NA = Not Applicable (1) Samples were analyzed by external standard calibration on 5/6/14. 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. ISO14-07-04
Table 11. DAL GW ACM2 140423 (1)
3M LIMS ID
Sample Description
ISO14-07-04-004
DAL-GW-ACM2-0-140423
ISO14-07-04-005
DAL-GW-ACM2-DB-140423
ISO14-07-04-006
DAL-GW-ACM2-FMS-140423
Average Concentration (ng/mL) %RPD
3M LIMS ID
Sample Description
ISO14-07-04-004
DAL-GW-ACM2-0-140423
ISO14-07-04-005
DAL-GW-ACM2-DB-140423
ISO14-07-04-006
DAL-GW-ACM2-FMS-140423
Average Concentration (ng/mL) %RPD
PFOA
PFBS (2)
Concentration
(ng/mL)
%Recovery
0.128
NA
0.108
NA
4.31 84.9
0.118 ng/mL 17%
Concentration
(ng/mL)
%Recovery
2610
NA
2590
NA
2720
NC
2600 ng/mL 0.77%
PFHS
PFOS
Concentration
(ng/mL)
%Recovery
0.154
NA
0.153
NA
4.68 91.4
0.154 ng/mL 0.65%
Concentration
(ng/mL)
%Recovery
0.310
NA
0.309
NA
4.83 91.3
0.310 ng/mL 0.32%
13C4-PFOA
13C4-PFOS 13C4-PFOS (2)
3M LIMS ID
Sample Description
ISO14-07-04-004
DAL-GW-ACM2-0-140423
ISO14-07-04-005
DAL-GW-ACM2-DB-140423
ISO14-07-04-006
DAL-GW-ACM2-FMS-140423
Average Concentration (ng/mL) %RSD
%Recovery
108 106 104 106% 1.9%
%Recovery
95.7 102 93.0 96.9% 4.7%
%Recovery
107 111 110 109% 2.0%
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 5/12/14 except where otherwise noted. (2) Samples were analyzed by external standard calibration on 5/6/14. The surrogate recovery standard 13C4-PFOS was added
to the samples during sample preparation.
PAGE 15 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
Table 12. DAL GW ACE 140423 (1)
3M LIMS ID
Sample Description
ISO14-07-04-007
DAL-GW-ACE-0- 140423
ISO14-07-04-008
DAL-GW-ACE-DB-140423
ISO14-07-04-009
DAL-GW-ACE-FMS-140423
Average Concentration (ng/mL) %RPD
3M LIMS ID
Sample Description
ISO14-07-04-007
DAL-GW-ACE-0-140423
ISO14-07-04-008
DAL-GW-ACE-DB -140423
ISO14-07-04-009
DAL-GW-ACE-FMS -140423
Average Concentration (ng/mL) %RPD
PFOA
PFBS (2)
Concentration
(ng/mL)
%Recovery
0.175
NA
0.168
NA
3.76 80.3
0.172 ng/mL 4.1%
Concentration
(ng/mL)
%Recovery
67.4 NA 71.9 NA 74.9 NC 69.7 ng/mL 4.3%
PFHS
PFOS
Concentration
(ng/mL)
%Recovery
0.0742
NA
0.0881
NA
4.25 93.1
0.0812 ng/mL 17%
Concentration
(ng/mL)
%Recovery
0.0566
NA
0.0567
NA
3.86 84.9
0.0567 ng/mL 0.18%
13C4-PFOA
13C4-PFOS 13C4-PFOS (2)
3M LIMS ID
Sample Description
ISO14-07-04-007
DAL-GW-ACE-0- 140423
ISO14-07-04-008
DAL-GW-ACE-DB-140423
ISO14-07-04-009
DAL-GW-ACE-FMS-140423
Average Concentration (ng/mL) %RSD
%Recovery
107 96.3 89.4 97.6% 9.1%
%Recovery %Recovery
108 103 102 104% 3.2%
109 110 111 110% 0.95%
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 5/12/14 except where otherwise noted. (2) Samples were analyzed by external standard calibration on 5/6/14. The surrogate recovery standard 13C4-PFOS was added
to the samples during sample preparation.
PAGE 16 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
Table 13. DAL GW WW8R 140423 (1)
3M LIMS ID
Sample Description
ISO14-07-04-010
DAL-GW-WW8R-0-140423
ISO14-07-04-011
DAL-GW-WW8R-DB-140423
ISO14-07-04-012
DAL-GW-WW8R-FMS-140423
Average Concentration (ng/mL) %RPD
3M LIMS ID
Sample Description
ISO14-07-04-010
DAL-GW-WW8R-0-140423
ISO14-07-04-011
DAL-GW-WW8R-DB-140423
ISO14-07-04-012
DAL-GW-WW8R-FMS-140423
Average Concentration (ng/mL) %RPD
PFOA
PFBS
Concentration
(ng/mL)
%Recovery
2690
NA
2760
NA
5120
97.0
2730 ng/mL 2.6%
Concentration
(ng/mL)
%Recovery
280 NA
285 NA
2560
92.0
283 ng/mL 1.8%
PFHS
PFOS
Concentration
(ng/mL)
%Recovery
1180
NA
1170
NA
3490
93.5
1180 ng/mL 0.85%
Concentration
(ng/mL)
%Recovery
3770
NA
3910
NA
6600
112
3840 ng/mL 3.6%
13C4-PFOA
13C4-PFOS
3M LIMS ID
Sample Description
ISO14-07-04-010
DAL-GW-WW8R-0-140423
ISO14-07-04-011
DAL-GW-WW8R-DB-140423
ISO14-07-04-012
DAL-GW-WW8R-FMS-140423
Average Concentration (ng/mL) %RSD
%Recovery
101 110 108 107% 4.3%
%Recovery
98.1 110 102 104% 6.1%
NA = Not Applicable (1) Samples were analyzed by external standard calibration on 5/6/14. 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. ISO14-07-04
Table 14. DAL GW WW9R 140423 (1)
3M LIMS ID
Sample Description
ISO14-07-04-013
DAL-GW-WW9R-0-140423
ISO14-07-04-014
DAL-GW-WW9R-DB-140423
ISO14-07-04-015
DAL-GW-WW9R-FMS-140423
Average Concentration (ng/mL) %RPD
3M LIMS ID
Sample Description
ISO14-07-04-013
DAL-GW-WW9R-0-140423
ISO14-07-04-014
DAL-GW-WW9R-DB-140423
ISO14-07-04-015
DAL-GW-WW9R-FMS-140423
Average Concentration (ng/mL) %RPD
PFOA
PFBS
Concentration
(ng/mL)
%Recovery
2770
NA
2860
NA
5370
103
2820 ng/mL 3.2%
Concentration
(ng/mL)
%Recovery
256 NA
257 NA
2760
101
257 ng/mL 0.39%
PFHS
PFOS (2)
Concentration
(ng/mL)
%Recovery
1090
NA
1140
NA
3790
108
1120 ng/mL 4.5%
Concentration
(ng/mL)
%Recovery
3580
NA
4060
NA
6860
123
3820 ng/mL 13%
13C4-PFOA
13C4-PFOS 13C4-PFOS (2)
3M LIMS ID
Sample Description
ISO14-07-04-013
DAL-GW-WW9R-0-140423
ISO14-07-04-014
DAL-GW-WW9R-DB-140423
ISO14-07-04-015
DAL-GW-WW9R-FMS-140423
Average Concentration (ng/mL) %RSD
%Recovery
106 112 107 109% 2.8%
%Recovery
104 106 103 104% 1.5%
%Recovery
88.9 97.5 97.1 94.5% 5.1%
NA = Not Applicable (1) Samples were analyzed by external standard calibration on 5/6/14 except where noted. The surrogate recovery standards
13C4-PFOA and 13C4-PFOS were added to the samples during sample preparation. (2) Results obtained on 5/29/14 without concurrent preparation and analysis of LCSs as a quality control measure.
PAGE 18 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
Table 15. DAL GW WW10R 140423 (1)
3M LIMS ID
Sample Description
ISO14-07-04-016
DAL-GW-WW10R-0-140423
ISO14-07-04-017
DAL-GW-WW10R-DB-140423
ISO14-07-04-018
DAL-GW-WW10R-FMS-140423
Average Concentration (ng/mL) %RPD
3M LIMS ID
Sample Description
ISO14-07-04-016
DAL-GW-WW10R-0-140423
ISO14-07-04-017
DAL-GW-WW10R-DB-140423
ISO14-07-04-018
DAL-GW-WW10R-FMS-140423
Average Concentration (ng/mL) %RPD
PFOA
PFBS
Concentration
(ng/mL)
%Recovery
1850
NA
1850
NA
4060
112
1850 ng/mL 0.00%
Concentration
(ng/mL)
%Recovery
240 NA
246 NA
2140
95.8
243 ng/mL 2.5%
PFHS
PFOS (2)
Concentration
(ng/mL)
%Recovery
888 NA
882 NA
2820
97.7
885 ng/mL 0.68%
Concentration
(ng/mL)
%Recovery
2190
NA
2060
NA
4410
115
2130 ng/mL 6.1%
13C4-PFOA
13C4-PFOS 13C4-PFOS (2)
3M LIMS ID
Sample Description
ISO14-07-04-016
DAL-GW-WW10R-0-140423
ISO14-07-04-017
DAL-GW-WW10R-DB-140423
ISO14-07-04-018
DAL-GW-WW10R-FMS-140423
Average Concentration (ng/mL) %RSD
%Recovery
109 108 106 108% 1.2%
%Recovery
104 103 100 103% 2.0%
%Recovery
99.2 94.6 101 98.1% 3.2%
NA = Not Applicable (1) Samples were analyzed by external standard calibration on 5/6/14 except where noted. The surrogate recovery standards
13C4-PFOA and 13C4-PFOS were added to the samples during sample preparation. (2) Results obtained on 5/29/14 without concurrent preparation and analysis of LCSs as a quality control measure.
PAGE 19 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
Table 16. DAL GW WW11R 140423 (1)
3M LIMS ID
Sample Description
ISO14-07-04-019
DAL-GW-WW11R-0-140423
ISO14-07-04-020
DAL-GW-WW11R-DB-140423
ISO14-07-04-021
DAL-GW-WW11R-FMS-140423
Average Concentration (ng/mL) %RPD
3M LIMS ID
Sample Description
ISO14-07-04-019
DAL-GW-WW11 R-0-140423
ISO14-07-04-020
DAL-GW-WW11 R-DB-140423
ISO14-07-04-021
DAL-GW-WW11 R-FMS-140423
Average Concentration (ng/mL) %RPD
PFOA
PFBS
Concentration
(ng/mL)
%Recovery
1110
NA
1130
NA
3110
101
1120 ng/mL 1.8%
Concentration
(ng/mL)
%Recovery
207 NA
216 NA
2350
108
212 ng/mL 4.3%
PFHS
PFOS
Concentration
(ng/mL)
%Recovery
526 NA
527 NA
2480
98.7
527 ng/mL 0.19%
Concentration
(ng/mL)
%Recovery
1480
NA
1770
NA
3990
119
1630 ng/mL 18%
13C4-PFOA
13C4-PFOS
3M LIMS ID
Sample Description
ISO14-07-04-019
DAL-GW-WW11 R-0-140423
ISO14-07-04-020
DAL-GW-WW11 R-DB-140423
ISO14-07-04-021
DAL-GW-WW11 R-FMS-140423
Average Concentration (ng/mL) %RSD
%Recovery
103 101 104 103% 1.7%
%Recovery
97.5 99.0 98.7 98.4% 0.80%
NA = Not Applicable (1) Samples were analyzed by external standard calibration 5/6/14. 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. ISO14-07-04
Table 17. Trip Blank Results
3M LIMS ID
ISO14-07-04-022 ISO14-07-04-023 ISO14-07-04-024
Sample Description
DAL-GW-TRI P-0-140423 DAL-GW-TRIP-LS-140423 DAL-GW-TRI P-HS-140423
3M LIMS ID
ISO14-07-04-022 ISO14-07-04-023 ISO14-07-04-024
Sample Description
DAL-GW-TRI P-0-140423 DAL-GW-TRI P-LS-140423 DAL-GW-TRI P-HS-140423
PFOA
PFBS
Concentration (ng/mL)
<0.0480 (1) 4.41 (1) 2510 (2)
%Recovery
NA 89.3 102
Concentration (ng/mL)
<0.0500 (1) 4.19 (1) 2480 (2)
%Recovery
NA 84.6 100
PFHS
PFOS
Concentration (ng/mL)
<0.0250 (1) 5.12 (1) 2510 (2)
%Recovery
NA 103 101
Concentration (ng/mL)
<0.0232 (1) 4.73 (1) 2620 (2)
%Recovery
NA 95.6 106
13C4-PFOA (1) 13C4-PFOS (1) 13C4-PFOA (2) 13C4-PFOS (2)
3M LIMS ID ISO14-07-04-022 ISO14-07-04-023 ISO14-07-04-024
Sample Description DAL-GW-TRI P-0-140423 DAL-GW-TRI P-LS-140423 DAL-GW-TRI P-HS-140423
%Recovery 104 103 NA
%Recovery 104 88.3 NA
%Recovery 112 109 113
%Recovery 111 110 105
NA = Not Applicable (1) Samples were analyzed by internal standard calibration on 5/12/14. (2) Samples were analyzed by external standard calibration on 5/6/14. 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. ISO14-07-04
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
Digitally signed by Susan T. W olf
Date: 2014.06.09 07:54:13 -05*00*
Susan T. Wolf, 3M Principal Analytical Investigator
Digitally signed by William K. Reagen DN: c=US, st=MN, l=St. Paul, ou=Laboratory Director, ou=3M Environmental Laboratoryauthenticated by LRA, email=wkreagen@mmm.com, o=3M, cn=William K. Reagen Reason: i am approving this document Date: 2014.06.09 08:13:14 -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.
(/it
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. Rude Reason: I agree to the terms defined by the placement o f m y signature on this document Date: 2014.06.09 08:00:37 -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 22 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
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
5/31/13 I8 6 0 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
4/23/14 2080 1250 790 1480
ACE (Activated Carbon Effluent) - Sample Results in ng/mL
ACE PFOA PFBS PFHS PFOS
5/31/13 0 .0 7 2 5 24.8 0 .1 0 5
< 0 .0 2 3 2
6/27/13 0 .0 7 1 7 111 0.118
<0.0232
7/23/13 0.0641 1960 0.0778 0 .0 2 7 7
9/30/13 0 .1 1 5 1950 0 .1 5 6
0 .0 4 5 2
10/28/13 0 .2 3 1 0 .3 7 9 0 .1 8 0
0 .0 7 8 5
11/18/13 0 .4 7 8 0 .5 9 2 0 .3 6 6
0 .0 7 2 6
12/13/13 0.0798 0 .0 7 6 6 0.0648 0.0303
1/30/14 0 .4 9 0 0 .2 5 7 0 .2 1 9 0 .2 0 9
2/27/14 0.138
0 .0 3 6 0 0 .0 7 0 6 0 .0 9 6 6
3/31/14 0.262 0 .2 2 4 0.108 0.139
4/23/14 0.172 69.7
0.0812 0 .0 5 6 7
PAGE 23 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
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
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
1/30/14 2660 326 1460 3990
2/27/14 2560 331 1370 4170
3/31/14 3290 357 1470 5790
4/23/14 2730 283 1180 3840
FC Charting fb r DAL_WW9R
PFOA------- -------PFOS------- --------
PFBS------- --------
PFHS-------
W W 9R PFOA PFBS PFHS PFOS
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
4/23/14 2820 257 1120 3820
PAGE 24 OF 25
3M ENVIRONMENTAL LABORATORY REPORT NO. ISO14-07-04
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
4/23/14 1850 243 885 2130
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
4/23/14 1120 212 527 1630
PAGE 25 OF 25
