Document ZJYaL1nRKv21dpqVO2vpx21ZY

iPhone: (814)231-8032 BACK TO MAIN Fax:(814)231-1253 or (814)231-1 580 Analytical Report Fluorochemical Characterization of Slurface Water Samples Pensacola, FI (W2176) Centre Analytical Laboratory Report No. 023-014C (Revision 1) Revision Data 3/21/01 Testing Laboratory Centre Analytical Laboratory, Inc. 3048 Research Drive State College, PA 16801 3M Environmental Laborafiery Contact Kent R. Lindstrorni Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 551333331 Phone: (651) 778-3352? Requester Kris J. Hansen, Ph.D. 3M Environmental Technology & Safety Services Bldg. 2-3E-09 P.O. Box 33331 St. Paul, MN 55133-33311 PAGE 1 OF 5 BACK TO MAIN 1 Introduction Results are reported for the analysis of a series of surface water samples received by Centre Analytical Laboratories, Inc. (Centre) from the 3M Environrnental Laboratory. The samples were collected from Pensacola, FI. The Centre study number assigned to the project is 023-014. Specific fluorochemical characterization by liquid chrornatcqraphy / tandem mass spectrometry (LC/MS/MS) was requestedfor all samples. A total of 8 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 ComDoundName Perfluorooctane Sulfonate Perfluorooctane Sulfonvlamide Perfluorooctanoate 1 ;zjd 1 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 05/03/00. The sample collection dates were not supplied. Chain-of-custody inlorniation is presented in Attachment C. 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 4.1.1 4.1.2 LC/MS/MS Sample Preparationfor 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 WiaS transferred to a Cle 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. Sample Analysis by LC/MS/MS In HPLC, an aliquot of extract is injected and passed thrlough 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 aga.inststandards. 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 5/17/00 and analyzed by MS/MS on 5/19/00. 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 l/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (?) were determined. A calibration curve is acceptable if r 20.985 (?2 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. PAGE3OF5 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 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 LCIMSAAS (analyticalmethod. 5.4 Matrix Spikes Matrix spikes were prepared for every field sample (excluding blanks) at a concentration of 100 ng/L using all compounds of interest. Matrix spike recoveries are given in Attachment B. All laboratory matrix spikes showed recoveries of all compounds between 70-130%. Field spikes were prepared on sample MC-301H at a concentration of 100 ng/L using all compounds of interest. The field spike is identitied as sample MC-304H. Field spike recoveries are also given in Attachment B. All field spikes showed recoveries of all compounds between 70-130%. 5.5 Duplicates All field samples (excluding blanks) 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. All recoveries for all compounds were between 70-130% in each LCS. Recoveries are given with the raw data in Attachment D. 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: Results 8.2 Attachment8:Matrix Spike Recoveries (Fieldand LaboratorySpikes) 8.3 Attachment C: Chain of Custody 8.4 Attachment D: LC/MS/MS Raw Analytical Data 9 Signatures Kevin J Lloyd, Vic; President Date J?MdEcUomi Date Other Lab Members Contributing to Data Enaksha Wickremesinhe Karen Smith David Bell PAGE 5 OF5 \ 4 LaboratoriEk,.Inc. Centre Analytical 3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 BACK TO MAIN Analytical Results W2176 Pensacola, FI 3M Sample identification MC-301H MC-303H MC-306H NA MC-307H NA MC-308H MC-384H NA Sample Description Site 1 PIN Surface Water Site 1 P/N Surface Water Duplicate Site 2 P/N Surface Water Site 2 PIN Surface Water Duplicate Site 3 P/N Surface Water Site 3 PIN Surface Water Duplciate Field Blank-P/N Empty Quiet Surface Water Quiet Surface Water Duplicate PFOS (ngll.) NQ NQ 28.5 NQ NQ NQ ND NQ NQ PFOSA (ng/L) 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 quantifiatlle. ND e LOD < NQ < LOQ POAA (nglL) ND ND ND ND ND ND ND ND ND - - 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: MC-305H !Spiked Amount (ng/L): [ 100 I Sample Concentration 20.8 0 0 =-Matrix (;I;) l1o151 Lower Recovery Limit: I 70 I IJpper Recovery Limit: I 130 I I Spike Result ([%Recovery) 81.2 I 105.0 111.0 Criteria (Pass / 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. Also note that sample MC-305H is a laboratory spike of sample MC-30'1H BACK TO MAIN Attachment 6: LC/MS/MS Laboratory Spike Recovery !Sample ID: I MC-306H 1 !Spiked Amount (ng/L): 1 100 1 Lower Recovery Limit: lJpper Recovery Limit: Sample Concentration (ngN 28.5 0 0 I 70 I 130 --Matrix );;;( 1 1 Spike Result (%Recovery) 95.5 - 98.5 101.0 i Criteria (Pass / Fail) PASS PASS PASS - BACK TO MAIN Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: Spiked Amount (ng/L): I MC-307H 100 J POAA Lower Recovery Limit: Upper Recovery Limit: Sample Concentration 20.9 0 0 Matrix Spike Result (ng/L) 109 98.2 102 I 70 I 130 1 -Matrix Spike Result -(% Recovery) 88.1 - 98.2 102.0 Criteria (Pass / Fail) PASS PASS PASS Note: Sample results less than 25 ng/L are reported as NQ in the rtisults 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 :Samde ID: MC-384H I !SpikedAmount (ng/L): I 100 I-ower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 15.7 0 0 Matrix Spike Result (ng/L) 107 88.2 94.0 I 70 I I 130 I -Matrix Spike - Result (% Recovery) 91.3 - 88.2 94.0 Criteria (Pass / Fail) PASS PASS PASS IVote: Sample results less than 25 ng/L are reported as NQ in the resullts section as they are Ibelow 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: Spiked Amount (ng/L): MC-304H 1 100 Lower Recovery Limit: Upper Recovery Limit: Sample Concentration (ng/L) 20.8 0 0 r~~ 70 I 130 Matrix Spike Result (ng/L) 93.6 80.2 96.9 I -Matrix Spike - Result (% Recovery) 72.8 - 80.2 96.9 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. Also note that sample MC-304H is a field spike of sample MC-301ti a Environmental Laboratory Form 38770 - PWO Shipping Address: 3M 8Mg. 2-3E49 935 Bush Avenue SL Paul. MN 55106 Telephone: Sample Recelvlng: (651) 7784946 Alternate: (651) 778-6753 FAX:1651) 778-6176 I Lv',<U-n c, f,, Contact Name I I# I , 1 I IW I I I-I 1 7~ I3 Company 1 4 BACK TO MAIN Chain of Custody /Request for Laboratory Analytical 2 6 8 Project IDlProject N a m e & m 0 \ 1 Iw&,,&ta\leM & L$-n Template # Project Lead I [ Dept. # (main) 4aq \ Final Report Due Date Internal Due Date I Class/Job/Project # 0010535[ IDate Available ~~ I .--- 3M Env. Lab Project# =r-u* Ii- iiiiuriiaIi Iu,s--e u--nI_ i y. L 8 si EJ City, State. zip w,Y) ' - pc (lo511-7It-Cn17CO Telephone # & , ~ J \ T % 01 ipec1.l Inatructionsendlor Specific Regulatory Requlrementa: I method. limit of detection. reporling unils. etc.) 35133 FAX# Date Due Contract Lab Analysis Requested: Complete below. Attach any assodated information. I Client Sample Identification I. r I un . - Collected by (print): 60 Y I I I 1 Relinauished bv/Affiliation - L c m 0 SarnDle Condition UDon Receiot: remperature: 'C d c c e D t a b l e 0 Other: d c e i v e d on Ice II ' I I I Daie -I.ime Matrix/ I I I I I Sampled Sampled Int\pt I Date Collector's signature: Shipped Via: I Received by/Affiliation ~ Comments I I Time I Date