Document 6weEwrrMeE6XpXQJ2rKXaM7Q3

BACK TO MAIN CEntrE Analytical Laboratories, Inc. 3048 Research Drive State Ca?ge,PA 16801 www.centrelab.com (814) 231-8032 Fax: (814) 231-1253 or (814) 231-1580 Analytical Report Fluorochemical Characterization of Drinking Water Samples Decatur, Alabama (Wl979) Centre Analytical Laboratory Report No. 023-007B (Revision 1) Revision Date 3/'20/01 Testing Laboratory Centre Analytical Laboratory, Inc. 3048 Research Drive State College, PA 16801 3M Environmental Laboratory Contact Kent R. Lindstrorri Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 55133-3331 Phone: (651) 778-5:352 Requester Kris J. Hansen, Ph.D. 3M Environmental Technology & Saifety Services Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 551334331 PAGE 1 OF 5 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 EnvironmentalLaboratory. The samples were collectedfrom Decatur, Alabama. The Centre study number assignedto the project is 023-007. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LCIMSRVIS)was requestedfor all samples. A total of 14 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 Perfluorooctane Sulfonate Perfluorooctanoate The analytical method used was validated by Centre. The validation protocol and results are on file with Centre. Data presented here is the highest quality data available,atthis time. 2 Sample Receipt The samples were submitted in individual plastic containers and were not preserved. Fourteen individual sample containers were received. Samples were received on 02/15/00. The sample collection dates were not supplied. Chain-of-custody information is 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 hiaS 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/Lfor periods longer than 14 days. PAGE 2 GF5 BACK TO MAIN 4 Methods - Analytical and Preparatory 4.1 4.1.1 4.1.2 LC/MS/MS Sample Preparationfor LC/MS/MS Analysis Samples were initially treated with 200 UL of 250 mc& sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (SPE) was used to prepare the samples for LC/MS/MS analysis. A forty-milliliterportion of sample was transferredto a CIS SPE cartridge. The cartridge was first eluted with 5 m i 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. Sample Analysis by LC/MS/MS In HPLC, an aliquot of extract is injected and passed through a liquid-phasechromatographic column. Based on the affinity of the analyte for the stationary phase in the column relative to the liquidmobile phase, the analyte is retained for a ch(aracteristicamount of time. Following HPLC separation, EWMS 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 quantitatedagainst standards. A Hewlett-PackardHP1100 HPLC system coupledto a Micromass Ultima MS/MS was usedto analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples were extracted on 2/18/00 and analyzed by MS/MS between 2/16/00 and 2/19/00. The HPLC and MS/MS methods usedfor analysis and instrument parameterscan 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 quantitation ion versus the concentration was plotted for each point. Using linear regression with l/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (P) were determined. A calibration curve is acceptable if r ~ 0 . 9 8 5(?2 0.970). Calibration standards are preparedusing the same SPEZ procedureusedfor samples. Calibration check standards were analyzed periodically (every three to five sample injections) throughout the analysis sequence. Compliance i:j obtained if the standard analyte concentrations are within +/-20% of the actual value. For the results reportedhere, calibration criteria were met. PAGE 3 OF 5 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 calibrationstandard. 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 analyticalmethod. 5.4 Matrix Spikes Matrix spikes were prepared for every sample at a concentration of 100 ngR using all compounds of interest. Matrix spike recoveries are giver1in Attachment 8. Field spikes were also prepared on several samples at a concentration of 100 ngR using all compounds of interest. Field spike recoveries are also given in Attachment B. 5.5 Duplicates All samples were analyzed in duplicate. Results are given along with the sample results in Attachment A. 5.6 Laboratory Control Samples Milliq water was spiked with all compound of interest at 25 and 250 ngR. Initial analysis of the 25 ng/L LCS showed low recovery for PFOS. The standard was reinjected and was found to have acceptable recovery (70-130%). All other recoveries for all compounds were between 70130% 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 Data Summary Please see Attachment A for a detailed listing of the anailytical results. 7 DatdSample Retention Samples are disposed of one month after the report is issued unless othetwise specified. All electronic data is archived on retrievable media and hard copy reports are stored in data folders maintained by Centre. PAGE4OF5 BACK TO MAIN 8 Attachments 8.1 Attachment A: Results 8.2 Attachment 6:Matnx Spike Recoveries (Fieldand Laboratory Spikes) 8.3 Attachment C: Chain of Custody 8.4 Attachment D: LC/MS/MS Raw Analytical Data 9 Signatures Kevin J Lloyd, Vice President - 3/74 Date - $?fldeccl -0 1 Date Other Lab Members Contributing to Data Enaksha Wickremesinhe Karen Smith 4w\ Inc. Centre Analytical Laboratories. 3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 BACK TO MAIN Analytical Results W1979 Decatur, Alabama 3M Sample Identification Sample Description PFOS (nghL) PFOSA (ng/L) POAA (ng/L) MC-215H MC-217H MC-220H MC-221H MC-223H MC-226H MC-228H MC-233H Intake-PIN ND ND ND Intake-P/N duplicate ND ND ND Intake-FieldBlank Empty ND ND ND Outflo~-P/N ND NO ND Outflow-PIN duplicate ND ND ND Site 1 P/N ND NO ND Site 1 PIN duplicate ND NO ND Field Blank PIN Empty ND ND ND Limit of Detection (LOD) for the procedure is appoximately 2.5 ng/L for PFOS and PFOSA and 7.5 ng/L for P O W Limit of Quantitation (LOQ) for the procedure is 25 ngIL for all compounds ND - Compound not detected NQ - Compound detected at a level between the LOD and LOQ. Result is not quantifiable. ND e LOD e NQ c LOQ - - Please refer to the reverse side for our standard terms and conditions. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery !Sample ID: I !SpikedAmount (ng/L): 1 MC-219H 100 POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 99.4 115 107 I 70 1 130 I -Matrix Spike - Result ("/. Recovery) 99.4 - 115.01 107.O Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: I Spiked Amount (ng/L): I MC-225H I ~ ~ 100 PFOS PFOSA POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (m-) 0 0 0 Matrix Spike Result (ng/L) 105 113 109 70 1 1 130 1 - Matrix Spike - Result (% Recovery) 105.0 - 113.0 109.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Flecovery Sample ID: I MC-230H I Spiked Amount (ng/L): I 100 I PFOS PFOSA POAA Lower Recovery Limit: Upper Recovery Limit: L Sample Concentration (ng/L) 0 0 0 I 70 I 130 Matrix Spike Result (ng/L) 97.9 108 102 > I Matrix Spike -- Result (% Recovery) 97.9 108.0 102.0 I Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sarnule ID: I MC-218H 1 I I Spiked Amount (ng/L): I 100 I PFOS PFOSA POAA Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 100 78.4 115 - Matrix Spike Result -(% Recovery) 100.0 - 78.4 115.0 Upper Recovery Limit: I 130 I Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I MC-224H 1 Spiked Amount (nglL): [ 100 PFOS PFOSA POAA Sample Concentration 0 0 0 Matrix Spike Result (ng/L) 102 83.9 110 Lower Recovery Limit: I Upper Recovery Limit: I 70 130 I -Matrix Spike Result -(Oh Recovery) 102.0 83.9 - 110.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample CD: c MC-229H I Spiked Amount (nglL): I 100 ILEA Sample Concentration (n!m 0 0 0 Matrix Spike Result 113 83.8 118 - Matrix Spike - Result (% Recovery) 1 13.0 - 83.8 118.0 Criteria (Pass / Fail) PASS PASS PASS i h V h .lliCntal Laboratory FG7, %??e - P'AC Shlpplng Addrasr: 3.4 Bldy 2 - 3 0 9 935 Bush Avsnua Telaphonr: Sample Racalvlng: (651) 7784948 Allarnala: (651) 77a-5753 Chain of Custody /Reque: BACK TO MAIN Jr'Laboratory Analytical 1 71 22 3M Env. * For !n!nr!:! ' Project # , use Q"!y . .. 1(method. tun1101 ddlectm. tepoiimg - units. eIc ) - . I I Analysis Requested: Complsla below. Attach any arsoclalrd Inlomallon. . 2. 3. 4. 8. 9. 10. Zollected by (print). n/lA Itern # Relinquished by/Affdiation U - I Sample Condilion Upon Receipt: Temperalure: 'C Acceptable 0 Other: 0 Received on Ice Collector's signature: n / / p , - FddW V Time ' I , Dale Shlpped Via: , -~ Y J L D I I I I Coinmenls. -- Time Date I I BACK TO MAIN a h v i l .mental Laboratory Form 30770. PWO Sliipplnp AJdrara: 3M BMp 2-3E09 lalaphone: Sarnpla Racalvlnp: (151) 771-4940 Chain of Custody /Reque Project IDlProject Name cp3-Q37 I Template # U I Final ReDOd Due &le U I Spaclal lnrtrucllonr andlor Spacins RaoulaloN Rasulremanlr: .. .. . e. C . ... Client Sample Identification 3M LIMS# Date Time Sampled Sampled Matrix/ Media Conlract Lab Analysis Requested: Cornplsla below- Attach any asroclalad Informalon. :ollecled by (print): ,lJ Item # I' I & Relinquished bylAMliation Collector's signature: I Date Shipped Via: L 2.h vlw Receiv-ed bylAffiliation Time- - Date