Document 91V8Nx0D03bQZXeZDa8DmJ1oe

3M ENVIRONMENTAL LABORATORY REPORT NO. IS013-07-07 Final Report Analysis o f PFOA, PFBS, PFHS, and PFOS in Aqueous Samples from 3M Decatur, Alabama: Groundwater Treatment Plant GAC System - July 2013 Laboratory Request Number: 1S013-07-07 Method Requirement 3M Method ETS-8-044.1 Report Date - D ate erf 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 th e testing reported herein meet the requirements o f ANSi/lSO/lEC 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 PAGE 1 OF 21 3M ENVIRONMENTAL LABORATORY REPORT NO. IS013-07-07 3M Environmental Laboratory 3M Environmental Laboratory Technical Director: W illiam K. Reagen, Ph.D. 3M Principal Analytical Investigator Susan W olf Report Author: Chelsie Grochow Analytical Report IS 0 1 3-07-07 3M Decatur Groundwater Treatm ent Plant System; July 2013 Sampling Report Date: Date o f Last Signature 1 Introduction/Summary The 3M Environmental Laboratory analyzed w ater samples from the groundwater treatm ent p la it GAC system a t the 3M Decatur, AL facility. W ater samples w ere collected by Weston Solutions personnel on July 23, 2013. Samples w ere returned to the 3M Environmental Laboratory for analysis of Perfluorooctanoate (PFO A), Perfluorobutane sulfonate (PFBS), Perfiuorohexane sulfonate (PFH S), Perfluorooctane sulfonate (P FO S ), and the surrogate recovery standards 13C4-P FO A and 13C4-P FO S under laboratory project number IS 0 1 3-07-07. Analysis o f the sam ples w as com pleted as specified under 3 M Environm ental Laboratory G eneral Project O utline (G P O ) num ber G P O l 1-1006. The 3M Environmental Laboratory provided sample containers for five sampling locations; A C I, ACM 2, ACE, W W 8R , and W W 9R . 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 spBce solution containing all analytes prior to being sent to the field for sam ple collection. Sam ple bottles for sampling locations ACM 2 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. Samples w ere prepared and analyzed by method ETS-8-Q44.1 "Method of Analysis for the Determination of Perfiuorinated Compounds in W ater 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 o f ANSI/lSOflEC 17025:2005 "General Requirements for the Competence o f 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 assessm ent PAGE 2 OF 21 3M ENVIRONMENTAL LABORATORY REPORT NO. 5013-07-07 T a b le 1. S am p le R esu lts S um m ary 3M U M S 10 Sample Description tS O I3-07-07-001 fS O I3-07-07-002 DAL-GW-ACI; Sample DAL-GW-ACt; Sample Dup Average %RPD Sample/Sample Dup (SO I3-07-07-004 IS O I307-07-005 DAL-GW-ACM2; Sample DAL-GW-ACM2; Sample Dup Average %RPD Sample/Sample Dup IS O I307-07-007 IS O I307-07-008 IS 013 0 7 0 7 0 1 0 IS O I3 0 7 0 7 0 1 1 IS O I3 0 7 0 7 0 1 3 (S O I3 0 7 0 7 0 1 4 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 PFOA Concentration ing/m L) 1650 1610 1630 2 .6 875 844 860 3 .6 0.0663 0.0619 0.0641 6.9 2530 2750 2640 8.3 2370 2440 2410 2.9 PFBS Concentration (ng/mL) 1230 1230 1230 0.0 1210 1210 1 2 1 0 <1) 0.0 1970 1950 1960 1.0 2 2m 263 3 .8 210 214 212 1.9 PFHS Concentration (ng/mL) 757 741 749 2.1 601 585 693 2.7 0.0784 0.0771 0.0778 1.7 1210 1300 1260 7 .2 1020 1040 1030 1.9 PFOS Concentration (ng/m L) 170) 1660 1680 2 .4 1.35 1.27 1 .3 1 6.1 0.0267 0.0287 0 .0 2 7 7 7.2 3850 3970 3910 3.1 3600 3740 3670 3 .8 N A =N ot Applicable (1) Reported resutis were prepared and analyzed by ETS-8-044.1 using external standard calibration. The analytical method uncertainties associated with the reported results are as folows: PFOA 14%, PFBS 12%, PFLB 13%, and PFOS 15%. (2) Reported results were prepared and analyzed by ETS-8-044.1 using internal standard cafibratKxi. The analytical method uncertainties associated with the reported results are as folows: PFOA 10%, PFHS 14%, and PFOS 15%. 2 Methods - Analytical and Preparatory 2.1 Methods Analysis was completed using 3M Environmental Laboratory Method ETS-8-044.1 "Method of Analysis far the Determination of Perfluorinated Compounds in W ater by LC/M S/M S; Direct Injection Analysis". Table 2. Target Analytes T a rg e t A n alytes PeffluofoodanacAad (C8 Arid) Perfluoroutanesulfonate (C4 Sulfonate ) Perfluorohexanestifonate (C6 Sulfonate) Perfluoroodanesrifonate (C8 SrJfonate) A cronym PFOA PFBS PFHS PFOS R eference M ate ria l S tru ctu re Linear + Branched Linea" Linea- Linear+ Branched PAGE 3 O F 21 3M ENVIRONMENTAL LABORATORY REPORT NO. IS013-07-07 2.2 Sam ple Collection Samples w ere collected on July 2 3 ,2 0 1 3 in NalgeneTM (high-density polyethylene) bottles prepared at f ie 3M Environmental Laboratory. Prior to sam ple collection, bottles designated for field matrix spikes were spiked in the laboratory with a knows volume o f an appropriate matrix spiking solution containing PFOA, PFBS, PFHS, and PFO S. Sam ple bottles for sampling locations A CM 2 and ACE, along with the Trip Blank sample and tow spke, w ere fortified with a mixture of mass-labeled internal standards at a nominal concentration of 1 ng/mL and a mixture o f surrogate recovery standards at a nominal concentration of 0.1 ng/mL. Collected sam ple bottles w ere received by the laboratory at ambient conditions on July 2 5 ,2 0 1 3 . 2.3 Sam ple Preparation All samples were diluted with methanol and analyzed for all a n a ly te . 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 o f a surrogate spiking solution. The 1:100 dilutions w ere prepared by removing a 0.1 mL aliquot of the well mixed sample and adding 9.8 mL erf methanol and 0.1 mL of a surrogate spiking solution. Prepared samples were analyzed by external standard calibration. T h e A CE and ACM 2 sam ple sete and the Trip Blank sample w ere prepared and analyzed for all analytes by transferring an aliquot of the well mixed sample into an autovial. Prepared samples w ere 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, ACM 2, and Trip Blank were spiked with an internal standard mix at a nominal concentration of 1 ng/m L prior to being sent to the field for sample collection. The laboratory control samples were analyzed mthe sam e m anner as the samples. 2.4 Analysis All sam ples and quality control samples were analyzed for four target analytes using high performance liquid chromatography/tandem mass spectrometry (H PLC /M S/M S). 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. 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. PAGE 4 OF 21