Document 65OR4ezqrJv7zwx8B0EzovXME

L P h o n e : (814) 231-8032 BACK TO MAIN Fax: (814) 231-1253 or (814) 231-1580 Analytical Report FIuorochemical Characterizationof DrinIking Water Samples Columbus, GA (W2336) Centre Analytical Laboratory Report No. 023-007F (Revision 2) (Revision Date 3/21/01) Testing Laboratory Centre Analytical Laboratory, Inc. 3048 Research Drive State College, PA 1680'1 3M Environmental Laboratory Contact Kent R. Lindstrom Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 55133-3331 Phone: (651) 778-5352! Requester Kris J. Hansen, Ph.D. 3M EnvironmentalTechnology & Safety Services Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 55133-3331 PAGE 1 OF5 BACK TO MAIN 1 introduction Results are reported for the analysis of a series of drinking water samples received by Centre Analytical Laboratories, Inc. (Centre) from the 3M Environmental Laboratory. The samples were collected from Columbus, GA. The Centre study number assigned to the project is 023-007. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS)was requestedfor all samples. A total of 16 samples were received for analysis. The samples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals: 0 Table 1:Target Analysis ComDound Name Perfluorooctane Sulfonate Perfluorooctane Sulfonvlamide Perfluorooctanoate The analytical method used was validated by Centre. The ?validationprotocol and results are on file with Centre. Data presented here is the highest quality data available at this time. 2 Sample Receipt The samples were submitted in individual plastic containers and were not preserved. Sixteen individual sample containers were received. Samples were received on 02/15/00. The sample collection dates were not supplied. Chain-of-custodyinforrriationis presented in Attachment C. 3 Holding Times The analytical method used was validated against a maximum holding time of 14 days. The stability of the analytes of interest for longer periods has; not been determined. However, it should be noted that field fortifications in water and other matrices have shown acceptable recoveries at 100 and 1000 ng/L for periods longer than 14 days. PAGEZOF5 BACK TO MAIN 4 Methods -Analytical and Preparatory 4.1 LCIMSIMS 4.1.1 Sample Preparation for LC/MS/MS Analysis Samples were initially treated with 200 ULof 250 mgR sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (SPE) was used to prepare the samples for LC/MS/MS analysis. A forty-milliliter portion of sample was transferred to a C18SPE cartridge. The cartridge was first eluted with 5 mL of 40% methanol in water solution. The eluate was discarded and the SPE column was then eluted with 100% methanol. A 5 ml portion of methanol was collected for analysis by LC/MS/MS. This treatment resulted in an eight-fold concentration of the samples prior to analysis. 4.1.2 Sample Analysis by LC/MS/MS In HPLC, an aliquot of extract is injected and passed through a liquid-phase chromatographic column. Based on the affinity of the analyte for the stationary phase in the column relative to the liquid mobile phase, the analyte is retained for a characteristic amount of time. Following HPLC separation, ES/MS provides a rapid and accurate means for analyzing a wide range of organic compounds, including fluorochemicals. Electrospray is generally operated at relatively mild temperatures; molecules are ionized, fragmented, and detected. Ions characteristic of known fluorochemicals are observed and quantitated against standards. A Hewlett-PackardHP1100 HPLC system coupled to a Nlicromass Ultima MS/MS was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples were extracted on 2/24/00 and analyzed by MS/MS between 2/26/00 and 2/27/00. The HPLC and MS/MS methods used for analysis and instrument parameters can be found in attachment D. 5 Analysis 5.1 Calibration A 7-point calibration curve was analyzed at the beginning and end of the analytical sequence for the compounds of interest. The calibration points were prepared at 0, 25, 50, 100, 250, 500, and 1000 ng/L (ppt) The response of the quantiltation ion versus the concentration was plotted for each point. Using linear regression with `I/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determinztion (P) were determined. A calibration curve is acceptable if r 10.985 (?2 0.970). Calibration standards are prepared using the same SF'E procedure used for samples. Calibration check standards were analyzed periodically (every three to five sample injections) throughout the analysis sequence. Compliance is obtained if the standard analyte concentrations are within +/-20% of the actual value. For the results reported here, calibration criteria were met. PAGE 3OF5 BACK TO MAIN 5.2 Blanks Extraction blanks were prepared and analyzed with every extraction batch of samples. The extraction blanks should not have any target analytes present at or above the concentration of the low-level calibration standard. For these samples, the extraction blanks were compliant. Instrument blanks in the form of clean methanol solvent were also analyzed after every highlevel calibration standard, and after known high-level samples. Again, the blanks should not have any target analytes present at or above the low-level calibration standard. For the samples presented here the instrument blanks are compliant. 5.3 Surrogates Surrogate spikes are not a component of the LC/MS/MS analytical method. 5.4 Matrix Spikes Matrix spikes were prepared for every sample at a concentration of 100 ngL using all compounds of interest. Matrix spike recoveries are given in Attachment B. Field spikes were also prepared on several samples at ia concentration of 100 ng/L using all compounds of interest. Field spike recoveries are also given in Attachment B. The field spike results for sample MC-529H gave recoveries for all compounds of approximately 1000 %, indicating that this sample was possibly spiked at 1000 ppt instead of 100 ppt. 5.5 Duplicates All samples were analyzed in duplicate. Results are given along with the sample results in Attachment A. 5.6 LaboratoryControl Samples Milliq water was spiked with all compound of interest at 25 and 250 ngL. All recoveries for all compounds were between 70-130% in each LCS. 5.7 Sample Related Comments Field blank samples consisted of empty containers. Forty milliliters of type I water filtered through a hypercarb cartridge was added to the empty container and analyzed in the same manner as the other samples. 6 Datasummary Please see Attachment A for a detailed listing of the analytical results. 7 DatdSample Retention Samples are disposed of one month after the report is issued unless otherwise specified. All electronic data is archived on retrievable media and hard copy reports are stored in data folders maintained by Centre. PAGE 4 OF5 BACK TO MAIN 8 Attachments 8.1 Attachment A: Resutts 8.2 Attachment B: MatrixSpike Recoveries(Fieldand LaboratorjSpikes) 8.3 Attachment C: Chain of Custody 8.4 Attachment D: LC/MS/MS Raw Analytical Data 9 Signatures Kevin J Lloyd, Vice President Date 27WwQCH 2041 Date Other Lab Members Contributing to Data Enaksha Wickremesinhe Karen Smith PAGE 5 OF5 (a\Centre Analytical Laboratories,,Inc. 30418 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 BACK TO MAIN Analytical Results W2336 Columbus, GA 3M Sample Identification MC-515H MC-517H MC-520H MC-521H MC-523H MC-526H MC-528H MC-531H NA MC-532H NA IMC-533H Sample Description Intake-P/N Intake-P/N duplicate Intake-FieldBlank Empty OUtflOW-P/N Outflow-P/N duplicate Site 1 P/N Site 1 P/N duplicate Site 2 P/N Site 2 P/N duplicate Site 3 P/N Site 3 P/N duplicate Field Blank-P/N Empty PFOS (ngl/L) 61.2 53.3 ND 61.5 62.5 57.5 55.7 57.4 55.4 61.7 57.8 ND PFOSA (ng/L) NQ NQ ND NQ NQ NQ NQ NQ NQ NQ NQ ND POAA (ng/L) 25.5 NQ ND 28.8 25.3 26.0 NQ 26.3 NQ 25.4 NQ ND ILimit of Detection (LOD) for the procedure is appoximately 2.5 ng/L for PFOS and PFOSA and 7.5 ng/L for POAA ILimit of Quantitation (LOQ) for the procedure is 25 ng/L for all compounds IYD - Compound not detected IVQ - Compound detected at a level between the LOD and LOQ. Result is not quantifiable. IVD < LOD < NQ < LOQ 43 Please refer to the reverse side for our standard terms and conditions. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Samde ID: I MC-519H I Spiked Amount (ng/L): I 100 I PFOS PFOSA POAA Sample Concentration 61.2 11.7 25.5 Matrix Spike Result (ng/L) 166 125 129 Matrix Spike Result (% Recovery) 104.8 113.3 103.5 I Criteria (Pass / Fail) PASS PASS PASS A Upper Recovery Limit: I 130 I Note: Sample results less than 25 ng/L are reported as NQ in the results se'ctionas they are below the limit of quantitation. Results are given in this table for recovery calculations only. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I MC-525H Spiked Amount (ng/L): I 100 I PFOS PFOSA POAA L Sample Concentration (n!m 61.5 14.9 28.8 Matrix Spike Result (ng/L) 172 125 139 Matrix Spike Result (% Recovery) 110.5 110.1 1 10.2 Criteria (Pass / Fail) PASS PASS PASS Lower Recovery Limit: I Upper Recovery Limit: I 70 J 130 1 Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I Spiked Amount (ng/L): [ MC-530H 100 PFOS PFOSA ,POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 57.5 14.9 26.0 Matrix Spike Result 185 130 148 I 70 I 130 I Matrix Spike Result (% Recovery) 127.5 115.1 122.0 Criteria (Pass / Fail) PASS PASS PASS Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: L MC-531H I Spiked Amount (ng/L): I 100 1 PFOS PFOSA POAA Sample Concentration 57.4 12.6 26.3 Matrix Spike Result (ng/L) 176 132 132 Matrix Spike Result (% Recovery) 118.6 119.4 105.7 Criteria (Pass / Fail) PASS PASS PASS Upper Recovery Limit: I 130 Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculationsonly. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: 1 MC-532H I Spiked Amount (ng/L): I 100 I PFOS PFOSA POAA Sample Concentration (ng/L) 61.7 14.8 25.4 Matrix Spike Result (ng/L) 168 121 128 Matrix Spike Result (% Recovery) 106.3 106.2 102.6 Criteria (Pass / Fail) PASS PASS PASS Lower Recovery Limit: I 70 Upper Recovery Limit: r 130 Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: [ MC-518H I Spiked Amount (ng/L): I 100 I PFOS PFOSA POAA Sample Concentration (ng/L) 61.2 11.7 25.5 Matrix Spike Result (ng/L) 185 137 144 Matrix Spike Result ("A Recovery) 123.8 125.3 118.5 Criteria (Pass / Fail) PASS PASS PASS Lower Recovery Limit: [ Upper Recovery Limit: r 70 1 130 1 Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I Spiked Amount (ng/L): MC-524H 1 100 I PFOS PFOSA POAA Sample Concentration (ng/L) 61.5 14.9 28.8 Lower Recovery Limit: I 70 Upper Recovery Limit: I 130 Matrix Spike Result (ng/L) 167 128 138 Matrix Spike Result (% Recovery) 105.5 113.1 109.2 Criteria (Pass / Fail) PASS PASS PASS Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I MC-529H 1 Spiked Amount (ng/L): I ~~ ~~ 100 IPFOS I~PPFFOOSSAA POAA I I I Sample Concentration (ng/L) Matrix Spike Result (ng/L) I I 57.5 1410 I I 14.9 I 1551 I 26.0 1293 Lower Recovery Limit: I 70 I Upper Recovery Limit: I ~~ 130 Matrix Spike Result ("/. Recovery) 1352.5 1536.1 1267.0 I I Criteria (Pass / Fail) I I FAIL I FAIL I FAIL Note: Sample results less than 25 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. Matrix spike recoveries indicate that this sample was spiked at 1000 ng/L instead of the 100 ng/L level indicated by the samplers Shipping Addrera: 3M Bkig 2 - E 0 9 935 Bush Avenue S I Paul.MN 55106 lalaphone: Sample Recelvlng: (6Sl)778-4948 Allamale: (661)7764761 FAX: (661)no4m BACK TO MAIN Projedl~l~rqectm-m d.+.,/., Y Template # Project Lead $,& &*C/A ' Internal Due Date Dept. # (main) by/) - Y ]Telephone # Epecld InrtrucUonr and/or ~pacitic~AegulalorRyaquiremenle: m e w . lunl01 d a l e d m . reponbymila.elc ) FAX# (.f q -- 1 1)&~- b17(o Analysis Requested: Complele below. Attach any asroclaled Inlomallon. 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