Document M45Jo2x42RyDx5vbdq3Q53p77

BACK TO MAIN CEntrE Analud tica-l Laboratories. Inc. :allege, PA 16801 www.centrelab.com L P h o n e : (814)231-8032 Fax: (814)231-1253or (814)231-1580 Analytical Report Fluorochemical Characterizationof Drin,kingWater Samples Cleveland, Tennessee (W1973) Centre Analytical Laboratory Report No. 023-007A (Revision 1) Revision Date 3,1191/01 Testing Laboratory Centre Analytical Laboratory, Inc. 3048 Research Drive State College, PA 168011 3M Environmental Laboratory Contact Kent R. Lindstroni Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 55133-3331 Phone: (651) 778-5352 Requester Kris J. Hansen, Ph.D. 3M Environmental Technology & Safety Services Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 55133-3331 PAGE 1 OF5 BACK TO MAIN 7 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 collected from Cleveland, Tennessee. The Centre study number assigned to the project is 023007. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requestedfor all samples. A total of 17 samples were receivedfor analysis. The samples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals: Table 1: Target Analysis I ComDound Name PerfluorooctaneSulfonate Perfluorooctane Sulfonvlamide I p l cronvm I The analytical method used was validated by Centre. The validation protocol and results are on file with Centre. Data presentedhere is the highest quality di3ta available at this time. 2 Sample Receipt The samples were submitted in individual plastic co'ntainers and were not preserved. Seventeen 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. Samples MC-127H and MC-134H were not analyzed as per client request. (Telephone call to Kris Hansen on 2/16/00). 3 Holding Times The analytical method used was validated against a rnaximum 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. PAGE2OF5 BACK TO MAIN 4 Methods - Analytical and Preparatory 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/MS/MS Analysis Samples were initially treated with 200 ULof 250 m g L 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 C18SPE cartridge. The cartridge was first eluted with 5 mL of 40% metlian,olin 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-phasechromatographic 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 8cha.racteristicamount 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 coupledto a Micromass Ultima MS/MS was usedto analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples were extracted on 2/17/00 and analyzed by MS/MS between 2/17/00 and 2/18/00. The HPLC and MS/MS methods used for analyisis 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 point$; 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 10.985 (?2 0.970). Calibration standards are prepared using the same SPE iprocedure used for samples. Calibration check standards were analyzed periodically i: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 melt. PAGE3 OF5 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-levelcalibrationstandard. For these samples, the extractionblanks were compliant. Instrument blanks in the form of clean methanol solvlent 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 lowlevel calibration standard. For the samples presentedhere the instrument blanks are compliant. 5.3 Surrogates Surrogate spikes are not a component of the LC/MS/I\AS,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 given in Attachment B. Field spikes were also prepared on several samples at a concentration of 100 ng/L 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 iIt 25 and 250 ngR. Initialanalysis 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 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 maintainedby Centre. PAGE4OF5 BACK TO MAIN 8 Attachments 8.1 Attachment A: Results 8.2 Attachment B: Matrix Spike Recoveries (Field and 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 Date - $7 f n a w 2001 Date Other Lab Members Contributing to Data Enaksha Wickremesinhe Karen Smith PAGE 5 0 F 5 \ 4 CLEabntorEraAtonraklsy.itiIcnacl. 3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 BACK TO MAIN Analytical Results W1973 Cleveland, Tennesse 3M Sample Identification MC-115H MC-117H MC-120H MC-121H MC-123H MC-126H MC-128H MC-131H NA MC-132H NA MC-133H Sample Description Intake-PIN Intake-P/N duplicate Intake-Field Blank Outflo~-P/N Outflow-PIN duplicate Site 1 PIN 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 (ngk) ND ND ND ND ND ND ND ND ND ND ND ND PFOSA (ng/L) ND ND ND ND ND ND ND ND ND ND ND ND POAA (ng/L) ND ND ND ND ND ND ND ND ND 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 POAA Limit of Quantitation(LOQ) for the procedure is 25 ng/L for all compounds ND - Compound not detected NQ - Compound detected at a level between the LOD and LOQ. Result is not quantiiiable. ND < LOD < NQ < LOQ Please refer to the reverse side for our standard terms and conditions. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Lower Recovery Limit: lJDDer Recoverv Limit: Sample Concentration 0-m) 0 0 0 Matrix Spike Result (ng/L) 88.5 114 103 I 70 I I 130 -Matrix Spike - Result (% Recovery) 88.5 - 114.0 103.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: Spiked Amount (ng/L): [ MC-125H 100 I Sample Concentration (ng/L) 0 0 0 Lower Recovery Limit: I 70 Upper Recovery Limit: I 130 Matrix Spike Result (ng/L) 81.8 106 91.7 -Matrix Spike - Result (% Recovery) 81.8 - 106.0 91.7 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN .AttachmentB: LC/MS/MS Laboratory Spike Recovery !Sample ID: I MC-130H I Spiked Amount (ng/L): I 100 I IPFOS [E? Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 0 0 0 1 70 I 130 Matrix Spike Result (ng/L) 88.4 106 105 -Matrix Spike - Result (% Recovery) 88.4 - 106.0 105.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Rrecovery Sample ID: MC-131H I Spiked Amount (ng/L): 1 100 lF%A POAA Sample Concentration 0 0 0 Matrix Spike Result (ng/L) 80.9 107 102 Lower Recovery Limit: I 70 Upper Recovery Limit: 1 130 1 Matrix Spike Result (% Recovery) I I Criteria (Pass / Fail) 107.0 102.0 PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery !Sample ID: I MC-132H !Spiked Amount (ng/L): I 100 1 'Lower Recovery Limit: Upper Recovery Limit: Sample Concentration OWL) 0 0 0 Matrix Spike Result (ng/L) 97.5 106 103 [ 70 1 1 130 1 -Matrix Spike -- Result (% Recovery) 97.5 - 106.0 103.0 Criteria (Pass / Fail) PASS PASS PASS L BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Samde ID: I MC-118H I Spiked Amount (ng/L): I 100 1 PEA POAA Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 96.9 64.7 113 I Umer Recoverv Limit: I 130 I -Matrix Spike -- Result (% Recovery) 96.9 - 64.7 113.0 Criteria (Pass / Fail) PASS FAIL PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: !SpikedAmount (ng/L): MC-124H 1 100 Sample Concentration Matrix Spike Result Lower Recovery Limit: I Upper Recovery Limit: I 0 134 0 123 70 1 130 1 .- Matrix Spike -.- Result (% Recovery) 110.0 134.0 .- 123.0 Criteria (Pass / Fail) PASS FAIL PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery !Sample ID: I MC-129H !Spiked Amount (ng/L): I 100 1 k?IPFOS Sample Concentration (ngU 0 0 0 Matrix Spike Result (ng/L) 105 125 114 -Matrix Spike Result -(% Recovery) 105.0 - 125.0 1 14.0 Upper Recovery Limit: I 130 Criteria (Pass / Fail) PASS PASS PASS h v i i mental Laboratory Form 38776 - PWO Shipping Address: 3M Bldg 2-3509 935 Bush Avenue SI Paul, t.4N 55106 Telephone: Sample Receiving: (651) 778-4948 Alternate: (651) 778-6753 FAX: (651) 778-6176 nethod. limil of detedion. reportingunits, etc ) BACK TO MAIN Chain of Custody /Reque. Project IDlProject Name 0 ~ - - ~ Template # ht,3 n Project Lead &I~V Deot # (main) 434 I Jr Laboratory Analytical ~m-L-,\7 Internal Due Date Class/Job/Proiect # f r I 17120 ~~ kHA ` v e 3M Env. Project # For Inteil,d Use Only d &= I 6Analysis Requested: Complete below. Anach any associated infomalion. 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