Document 2j7M0GGGNNjxQy8doxzROqOn7

AR.JSl>-0673> Centre Analytical Laboratories, Inc. 3048 Research Drive Phone: (814) 231-8032 State College, PA 16801 Fax: (814) 231-1253 or (814) 231-1580 Analytical R eport Fluorochemical Characterization of Surface Water Samples Mobile, Alabama (W2151) Centre Analytical Laboratory Report No. 023-014D r- 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 1 0 F 5 000970 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 Environmental Laboratory. The samples were collected from Mobile, Alabama. The Centre study number assigned to the project is 023-014. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requested for all samples. A total of 8 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 Perfiuorooctane 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. Eight individual sample containers were received. Samples were received on 05/03/00. The sample collection dates were not supplied. Chain-of-custody information is presented in Attachment A. 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 has not been determined. PAGE 2 OF5 000971 4 Methods - Analytical and Prepara tory 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 C18SPE 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 5/17/00 and analyzed by MS/MS on 5/20/00. 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. PAGE 3 OF 5 O ff0 9 7 Z 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 field sample (excluding blanks) at a concentration of 100 ng/L using all compounds of interest. Matrix spike recoveries are given in Attachment C. POAA showed low matrix spike recoveries in samples MC-407H and MC-484H. All other compounds showed matrix^spikes recoveries between 70-130% in all samples. Field spikes were prepared on sample MC-401H at a condentration of 100 ng/L using all compounds of interest. Field spike recoveries are also given in Attachment C. All compounds showed recoveries 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 B. 5.6 Laboratory Control Samples Milliq water was spiked with all compound of interest at 25 and 250 ng/L. 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 Data Summary Please see Attachment B 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. PAGE 4 OFS 000973 8 Attachments 8.1 Attachment A: Chain-of-Custody 82 Attachment B: Results. 8.3 Attachment C: Matrix Spike Recoveries (Field and Laboratory Spikes) 8.4 Attachment D: LC/MS/MS Raw Analytical Data 9 Signatures Kevin J Lloyd, Vice President Other Lab Members Contributing to Data Enaksha Wickremesinhe Karen Smith David Bell Date PAGE 5 OFS 000974 3048 Research Drive, State College PA 16801 814-231-8032 FAX 814-231-1253 A nalytical Results W 2151 M obile, Alabam a 3M Sam ple Identification Sam ple D escription PFO S (ng /L) PFOSA (ng/L) M C -401H M C -403H M C-406H NA M C -407H NA M C -408H M C -484H NA Site 1-P/N Surface W ater Site 1-P/N Surface W ater Duplicata Site 2-P/N Surface W ater Site 2-P/N Surface W ater Duplicate Site 3-P/N Surface W ater Site 3-P/N Surface W ater Duplicate Field Blank-P/N Empty Q uiet Surface W ater Q uiet Surface W aterpu p licate 23.9 J 22.0 J 3 9 .6 4 2 .8 3 4 .7 3 6 .3 <25 3 3 .3 3 1 .5 6.6 J 6.2 J 12.9 J 13.3 J 8.6 J 9.8 J. <25 7.9 J 7.6 J J Compound is present, but below the reporting lim it of 25 ng/L. The result is an estim ated value. Method Detection Limits are approximately 2.5 ng/L for PFO S and PFO SA and 7 .5 ng/L for POAA. POAA (ng/L) 25.5 27 53.9 59.8 82.6 82.8 <25 27 . 24.9 J Please re fer to th e reverse sid e fo r o u r stan d ard term s a n d conditions. 000975 BEST CO PY AVAILABLE Adsdhitoiwonnaol nsawmepsltinmgaspites Environmental Sampling Sites and Supply Chain Facilities for Mobile, AL 000976 BEST COPY AVAI LAB -- r if s ..J 0\ 1090 Map/ QuocLoonv i R?ad Ljindfjjl__ Ino.;OIOOOQOT.IfKxX p | | . Additional sampling sites shown on cast map Environmental Sampling Sites West of Mobile, AL 00097?