Document NNKb5NYB4nkjrnazoR8rr7kxw

BACK TO MAIN Centre Analytical Laboratories, Inc. 3048 Research Drive ^ Phone: (814) 231-8032 State College, PA 16801 www.centrelab.com Fax: (814) 231-1253 or (814) 231-1580 Analytical Report Fluorochemical Characterization of Drinking Water Samples Decatur, Alabama (W1979) 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. 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 Environmental Technology & Safety Services Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 55133-3331 PAGE 10F 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 collected from Decatur, Alabama. The Centre study number assigned to the project is 023-007. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requested for 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: Table 1: Target Analysis Compound Name Perfluorooctane Sulfonate Perfluorooctane Sulfonvlamide Perfluorooctanoate Acronym PFOS 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. 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 H o ld in g Tim es 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. PAGE2 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 mg/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-milliliter portion of sample was transferred to a C i8 SPE 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-Packard HP1100 HPLC system coupled to a Micromass Ultima MS/MS was used to 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 2/18/00 and 2/19/00. 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 quantitation ion versus the concentration was plotted for each point. Using linear regression with 1/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (r2) were determined. A calibration curve is acceptable if r >.0.985 (r2 > 0.970). Calibration standards are prepared using the same SPE 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. 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-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 ng/L using all compounds of interest. Matrix spike recoveries are gsven 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 at 25 and 250 ng/L. 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 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 Data Summary Please see Attachment A for a detailed listing of the analytical results. 7 Data/Sample 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. PAGE4 OF5 BACK TO MAIN 8 Attachments ::v''' . ::' . ;' : 8.1 Attachment A; Results 8.2 Attachment B: Matrix Spike Recoveries (Reid and Laboratory Spikes) 8.3 Attachment C: Chain of Custody 8.4 Attachment D: LC/MS/MS Raw Analytical Data 9 Signatures Other Lab Members Contributing to Data Enaksha Wickremesinhe Karen Smith PACE 5 OF5 BACK TO MAIN ANALYTICAL REPORT Centre Analytical Laboratories. Inc. 3048 Research Drive, State College PA 16801 814-231-8032 PAX 814-231-1253 Analytical Results W1979 Decatur, Alabama 3M Sample Identification Sample Description PFOS (ng^L) PF( (ng/L) POAA (ng/L) MC-215H MC-217H MC-220H MC-221H MC-223H MC-226H MC-228H MC-233H Intake-P/N ND ND ND Intake-P/N duplicate ND ND ND Intake-Field Blank Empty ND ND ND Outflow-P/N ND ND ND Outflow-P/N duplicate ND ND ND Site 1 P/N ND ND ND Site 1 P/N duplicate ND ND ND Field Blank P/N 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 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 quantifiable. 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 Sample ID: Spiked Amount (ng/L): MC-219H 100 PFOS PFOSA POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 0 0 0 70 130 Matrix Spike Result (ng/L) 99.4 115 107 Matrix Spike Result (% Recovery) 99.4 115.0 107.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: Spiked Amount (ng/L): MC-225H 100 PFOS PFOSA POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 0 0 0 70 130 Matrix Spike Result (ng/L) 105 113 109 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 Recovery Sample ID: Spiked Amount (ng/L): MC-230H 100 PFOS PFOSA POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 0 0 0 70 130 Matrix Spike Result (ng/L) 97.9 108 102 Matrix Spike Result (% Recovery) 97.9 108.0 102.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: Spiked Amount (ng/L): MC-218H 100 PFOS PFOSA POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 0 0 0 70 130 Matrix Spike Result (ng/L) 100 78.4 115 Matrix Spike Result (% Recovery) 100.0 78.4 115.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN Attachment B: LC/MS/MS Field Spike Recovery Sample ID: Spiked Amount (ng/L): MC-224H 100 PFOS PFOSA POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 0 0 0 70 130 Matrix Spike Result (ng/L) 102 83.9 110 Matrix Spike Result (% 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 fO: Spiked Amount (ng/L): MC-229H 100 PFOS PFOSA POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 0 0 0 70 130 Matrix Spike Result (ng/L) 113 83.8 118 Matrix Spike Result (% Recovery) 113.0 83.8 118.0 Criteria (Pass / Fail) PASS PASS PASS BACK TO MAIN 3 M E n^10v770i i oum. m e n t a l L a b o r a t o r y Chain of Custody/Requet. j r Laboratory Analytical 1T122 3* MF nEr nInvt.an .^ i I (ParoHjenclut # Shipping Address: 3M Bldg 2-3E-09 935 Bush Avenue St Paul, MN 5106 Telephone; Semple Receiving: (651)778-4948 Alemete: (651) 778-6753 FAX: (651) 778-6178 Project 1P ro je c t Name nfl/S -C P '7 ffl,,|-E -CHvf * Y n U ^ O u M v f A u , L ^ S Template # . -J^inal Report Due Da(3" <J Project Lead , . . Internal Due Date - Dept, it (main) O ^X^l 1 Class/Job/Project # Q f ) Contact Name ^ f3Wfl Company 3 ^ y ) Date Available *t ~C oao oc Mailing Address City, state. Zip Telephone f t , y ) . - Z i - Q * )____f t P nua. rs g /3 3 -7 f t . ( , r U f t - Specie! Instructions end/or Specific Regulatory Requirements: (method, limil of detection, reporting units, etc ) fry 3 3 3 3 J f a x # ibs-nn%-teinu> Date Due Contract Lab cz T i t Analysis Requested: O A J -o r u s im i D c c ^ u `t A L Item # Client Sample Identification 3M LIMS# 1. m e - \ S \ \ - 3 X A - U - P j / J . tA jf t - f t 2. jL ~ ) ]l ~F C A I [^aJ o - D u c p P 3. . m L ^ I & t i - J ^ A a U - = F w ; U l y im - P ) i > 4. 5. M L - a m t i -U h S p iU -P i./v 6. m c - ^ i - l ^ r k l u - t c l A 6 \a y ) K J l A J - t o f t k i M C 'Z & M -O iM h * u -P A ) ' 7. i \ C - a t t -<X> \ I d u j - V i A A / U h - C U ) - P 8. 9. M L 2 2 1 \ - O i A ^ i o u ) ' T n / l A S o i L l - P i A J m C -3 P .T i 1- a A l t v u j 'l A J o ^ n i h - P Ia ) 10. m c - a * ( g t f - s ) h l f l / O ________________________ \/ Date Sampled hJl A V Time Matrix/ Sampled Media f O \ A . 1a )a U Preservatives: o2 X o if) atft o> 4 oC 2 Enter lha number of containers of each / O nS --2 OC HXo3 o i 1 Complete below. Attach any associated Information. / \ \i \< / ,,o i 7 bX Ay 7 / /z i 1 -- -- 1 1 \ 1 \ 1 Collected by (print): k j ( { \ Collector's signature: . i i / v . Item # Relinquished by/Affiliation Time : . Date Shipped Via: . Received by/Affiliation Time Date \-lO \ I m J L a P i l u f r J l c m l r Y ] _______________ d iJ ih -IC o /d JL > Z -l9 -< iZ > Chain of Custody Sample Condition Upon Receipt: flf Acceptable O Other: Temperature: 'C e Received on Ice O llier Associated CoC |"J \ 3 0 , O t S - t t \~) )^3,nPS| (7lV) CoP'8S l0: n ia fe ,n ta 5 l r>i3>t, ni2>3. ni3>-j 1-3 L A L ,^ ^ Com menls BACK TO MAIN 3M Envil menial Laboratory Form 38778 - PWO S h ip p in g Address: 3M BJdg 2-3E-09 935 Bush Avenue SI Paul. M N 55106 Telephone: Sample Receiving: (651) 778-4948 Altemele: (651)7784753 FAX: (651) 776 6178 Contact Name n S Company jrChain of Custody/Reque. Laboratory Analytical 17123 Project ID/Project Name Template# g ^ -C e T l H it -)l4 V 6 'K / O' "E lO FinA ReOporritnDiuie/ iSaUte J L f Project Lead Internal Due Date Dept. # (main) Class/Job/Project # e>Oi O ^ . Date Available O 3M Env i Project # For intuI.di Lise Only' Report Results to: Add,. s, z t-0 7 fo M Dale Due Ctly. Stale. Z.p (Smpeetchioadl,InluTsnetirtuleoclptdiohentoesnctaeionnd#,/orerpSoptteincgifiucnRitse,geutcla.)tory Requiremse_n_ts_:__________,____________FAX * I b & l l _______________________ Contract Lab G `i , V - C V - \ ................................................ ...... ..... . . Preservatives: c _ U T Q_ Analysis Requested: Complete below. Attach any associatedInformation. Other Total Number of Containers ' ic W / D lcaA w , A L " oXzn OCXO OO>VI z0co) Item # Client Sample Identification 1. m e - S i h V f r t \ ( L l \ j * \ n io p P 2. 3. 4. 5. m tr & M I-T i 'M L S p 'iU -P jA J_____________ ( h L - 2 li ^ 1r r l h f U ~ P lM ______________ . -". fn . /iia.yih~ P lA )-Ji.iy i'nOh i 3M UMS# Date Sampled i______ VY Time Sampled a j \A \/ 6. 7. ______________________________________________________________ \s P > - 8. . , < 9 ^ 9. 10. ;1 V y y- Matrix/ Media UAW \1/ Enter thenumberof containers of each / n7 F -- ^7' 7V ? r ~ \ / /f y ......V l \ l 1 (Enter an'X' intheboxbelowtoindicaterequest) Collecled by (print): a J Item # : Relinquished by/Affillation l-M [ ^ [ \ n / j J z / ! i r f e r V Time Date ;> Collector's Shipped signa Via: ure: . A i . M ? ; Received by/Affillation : i /- ^ ______--Czr --=?^ 2M hIo o /H, y ; Time : Date / o 1 - IV-0T Chain of Custody Sample Condition Upon Receipt: Temperature: c Acceptable 0 Other: e Received on Ice Other Associated CoCs n i d o , n u i . n t j a , 1- 7 c j s , n i z n , Copies to: m a s , n P 'i , 0)50,1-71^1, n i3 3 , n i 3 H C TV /tc ,:rr / / /-i Comments