Document NGboQ0yv8qvM8w0p09pw0p2zy

BACK TO MAIN Centre Analytical Laboratorks, Inc. 3048 Research Drive State C%?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 Mobile, Alabama (W2151) Centre Analytical Laboratory Report No. 0123-007C(Revision 1) Revision Date 3L201'01 Testing Laboratory Centre Analytical Laboratory, Inc. 3048 Research Drive State College, PA 16130'1 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 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 Environmental Laboratory. The samples were collectedfrom Mobile, Alabama. The Centre study number assignedto 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 receivedfor analysis. The samples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals: 1 0 Table 1:Target Analysis Comoound Name Perfluorooctane Sulfonate Perfluorooctane Sulfonvlamide Perfluorooctanoate 1 4 h;Tm PFOSA POAA 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 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-custodyinformationis presented in Attachment C. 3 Holding Times The analytical method used was validated against a niaximum 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. PAGE 2 OF5 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 uL of 250 mSlR 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 CI8 SPE cartridge. The cartridge was first eluted with 5 mL of 40% methariol in water solution. The eluate was discarded and the SPE column was then eluted with 100/o 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-PackardHPl 100 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 2/23/00 and analyzed by MS/MS between 2/23/00 and 2/24/00. 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 begirlning 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 (?) 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 (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. 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 lowlevel 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/FAS analytical method. 5.4 Matrix Spikes Matrix spikes were prepared for every sample at a concentration of 100 ng/L using all compounds of interest. Matrix spike recoveries are given in Attachrnent 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 6. 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 2 5 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 cornpounds were between 70- 130% in each LCS. 5.7 Sample Related Comments Field blank samples consisted of empty containers. Forty millililers 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 ai?alyticalresults. 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: Results 8.2 Attachment 6:Matrix Spike Recoveries (Fieldand Laboratory Spikes) 8.3 Attachment C: Chain of Custody 8.4 Attachment D: LC/MS/MS Raw Analytical Data 9 Signatures ager, Operations Manager - I Kevin J Lloyd, Vice President Date 3 7 M+&U 200 I Date Other Lab Members Contributing to Data Enaksha Wickremesinhe Karen Smith PAGE5OF5 (-A\ CEntrE Analyitical Laboratories. Inc. 30.48 Research Drive, State College PA 16801 814-231-8032 814-231-1253 BACK TO MAIN Analytical Results W2151 Mobile, Alabama 3M Sample Identification MC-415H MC-417H MC-420H MC-421H MC-423H MC-426H MC-428H MC-431H NA MC-432H NA MC-433H Sample Description Intake-P/N Intake-P/N duplicate Intake-Field Blank 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 (ng/L) ND ND ND ND ND ND ND ND ND ND ND ND PFOSA (nglL) ND ND ND ND ND ND ND ND ND ND ND ND POAA (nglL) 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 anci 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 quantiliable. ND < LOD e NQ < LOQ - - Please refer to the reverse side for our standard teirms and conditions. BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery !Sample ID: MC-419H I !Spiked Amount (ng/L): I 100 Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 97.4 104 102 Matrix Spike Result ( O h Recovery) I Criteria (Pass / Fail) 104.0 102.0 PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery !Sample ID: I MC-425H I !Spiked Amount (ng/L): 1 100 I Lower Recovery Limit: IJpper Recovery Limit: I Sample Concentration 0 0 I 70 I 130 Matrix Spike Result (n!m 90.6 112 104 I Matrix Spi;ke Result .- 1(% Recovery) 90.6 112.0 104.0 Criteria (Pass / Fail) PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery !Sample ID: I MC-430H I !Spiked Amount (ng/L): 100 1 Lower Recovery Limit: IJpper Recovery Limit: Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 96.8 121 105 I 70 I 130 I -Matrix Spike - Result 1(% Recovery) 96.8 - 121.o 105.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery !Sample ID: 1 MC-431H I :SpikedAmount (ng/L): I 100 1 Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 95.0 124 104 -Matrix Spike - Result (% Recovery) 95.0 - 124.0 104.0 Upper Recovery Limit: I 130 I Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery !Sample ID: I !SpikedAmount (ng/L): I MC-432H 100 POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 0 0 0 I 70 I 130 Matrix Spike Result (ng/L) 87.0 110 92.1 -Matrix Spike - Result (% Recovery) 87.0 1 10.0 92.1 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: MC-418H [%EA POAA Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 114 109 111 Lower Recovery Limit: I 70 Upper Recovery Limit: I 130 1 -Matrix Spike - Result ( O h Recovery) 1 14.0 109.0 111.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: I MC-424H Spiked Amount (ng/L): I 100 J POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 96.6 106 98.0 1 70 1 130 1 .- Matrix Spike Result (% Recoven4 96.6 106.0 .- 98.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery !Sample ID: I MC-429H I !Spiked Amount (ng/L): I 100 I 1IPFOS IPFOSA IPOAA Sample Concentration (ng/L) 0 0 0 Matrix Spike Result (ng/L) 104 118 108 -Matrix Spike - Result (% Recovery) 104.0 - 1 18.0 108.0 IJpper Recovery Limit: I 130 I Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN 31111 Envii .mental Laboratory Form 38778 ~ PWO iue. Jr Laboratorv Analvtical 1 7 128 3M Env. I Project # For lnter8,di Use Only Shipping Address: 3M BidQ 2-3E-09 Telephone: Sample Receiving: (651) 778-4948 Template # 'I a b d 935 Bush Avenue SI Paul.MN 55106 Allernate: (651) 778-6753 FAX: (651) 7784176 ,Dept. # (main) I Internal Due Date ClasslJoblProjed# 0 0 1 ~ S I J ~ T kr';3 - Contact Name s;m 2 Company a- = Po i Mailing Address Hk,.,gfi & J ; & ~ Q 2 -3f.-lgLf 5 - > Q City. State, Zip , %L![, SS 133 Telephone# hs) 772s-la Olb 1 Date Available Y &. - Date Due FAX# (lo5]377&-b1710 Contract Lab Specialinstructionsand/or Specific ReaulaloryRequlrements: [method. limit of deledion. repodingunits. elc.) I I Analysis Requested: Complete below. Anach any associated information. Envii &mentaLl aboratory F o n 30770 - PWO Shipping Address: 3M BMg 2-3E-09 935 Bush Avenue SI Pau1,MN 55106 Telephone: Sample Recelvlng:(651) 778-4940 Alternate: (651) 778-6751 FAX: (651) 778-6176 BACK TO MAIN Chain of Custody /Reque. Project IDlProject Name m3 Template # Project Lead +#, k f l wA Dept. # (main) u 4/ 3r Laboratory Analytical 17129 Y IInternal Due Date IClasslJoblProject# 00 1 0 ~ 3 w F 3M Env ) Project # For triteilldl Use Only Preservatives: L 05 I Analysis Requested: Complslebelow. Anach any asaoclatedInformation. rIrrTITiI irI \ Collected by (print): A/ I >r U v- 0 Item # +A Relinquished bylAffiliation 0 I Samole Condition Uoon Receiot: 0 Acceotable 0 Other: Orlginal -Accompanying Sampler +. Date Collectots signature: A/\A Shipped Via: I I Comments: ? Last Page -Originator See Reverse Side for Inslnidtnnr ~- Time Date / c 3 3 L-IS%Z I