Document 85qpz35arQMp8qJeq7yRbv0gZ

AR226-3650 Attachment A 000003 " > r4,~ V ANALYTICAL REPORT ST LT R E N T STL Denver 4 9 5 5 Yarrow Street Arvada, CO 8 0 0 0 2 Tel: 30 3 7 3 6 0 1 0 0 Fax: 3 0 3 4 3 1 7171 w w w .stl-inc.com PFOA Analysis Lot#: D6A270318 Dale VanDeVelde GE Plastics State Route 892 DuPont Road PO Box 68 Washington, WV 26181 Severn Trent Laboratories, Inc./STL Denver Project Manager February 13,2006 Leaders in Environmental Testing Severn Trent Uiuratories, !nc. 000003a Table Of Contents Standard Deliverables Report Contents Standard Deliverables The CoverLetter and the Report Coverpage are considered integral parts o fthis StandardDeliverablepackage. This report is incomplete unless allpages indicated in this Table o fContents are included. Table o f Contents Case N arrative Executive Summary - Detection H ighlights M ethods Summary M ethod/A nalyst Summary L ot Sam ple Summary A nalytical Results QC D ata Association Summary Chain-of-Custody Total Number of Pages 000004 Case Narrative D6A270318 The results included in this report have been reviewed for compliance with the Laboratory Quality Manual. All results have been found to meet all requirements ofNELAC and any exceptions are noted below. This report shall not be reproduced except in full, without the written approval o f the laboratory or sponsor. Dilution factors and footnotes have been provided on each datasheet to assist in the interpretation of the results. Sample Arrival and Receipt The two solid samples presented in this report were received at the STL Denver laboratory at a temperature o f 18.8C on January 27,2006. The sample containers were received in an acceptable condition. Standards Analytical standards were prepared using the acid form of the compound perfluorooctanoic acid (PFOA). A di-carbon-13 labeled perfluorooctanoic acid, [l,2-di-l3C] was introduced at the extraction step and was used as an internal standard for quantitation of PFOA. Results are reported as PFOA and as ammonium perfluorooctanoate (APFO) for QC samples. A multiplier of 1.0406 is applied to PFOA results to correct for the molecular weight differences between PFOA and APFO. Sample Extraction and Analysis The samples presented in this report were originally analyzed for the target analyte by STL Denver's SOP DEN-LC-0012A. For solid samples ten grams o f sample are extracted in 50 mL of basified methanol in a sonication bath for three hours, followed by shaking for 24 hours. Each sample was spiked with the internal standard, prior to extraction. After the sample is extracted, centrifuged, and filtered, it is analyzed by LC/MS/MS. Because of limited sample sent, only 1 gram of sample was extracted for CC3YFG RESIN and RD 9112 RESIN. Method OC Samples The Method Blank is reagent sand spiked with internal standard and prepared with each batch of 20 samples of the same matrix. The method blanks were non-detect at the reporting limit. Each batch is prepared with a Laboratory Control Sample (LCS). The recoveries of two concentration levels of Laboratory Control Samples were within control limits for both analytical batches. Due to limited sample volume, MS/MSD samples could not be performed for QC batches 6031073 and 6039144. Two LCS samples were analyzed for each batch to demonstrate that the analytical system was operating in control. 000005 Analytical Comments The sample results were not corrected for moisture content. Internal standard recoveries were in control. Both samples were analyzed at a dilution to obtain the target analyte within the calibration range of the instrument. The reporting limit is adjusted according to the dilution required. The two solid samples for this project were originally analyzed using our soil extraction procedure because it was the most appropriate technique our laboratory has validated for solid matrices. These original analyses were successful, however, the analytical chemist performing the analyses noted that a precipitate had formed in the sample extract when he went to analyze them. This observation indicates there may be a loss of analyte from the solution to the solid form and therefore a low-biased result may be obtained. The results obtained in the original analyses were: CC3YFG RESIN RD 9112 RESIN 78.000 ug/kg 130.000 ug/kg We recommended an alternate preparation method be performed to verify these results. Hie alternative method was solvent dilution. A weighed amount o f each sample was diluted with methanol and analyzed. These samples were not completely soluble in methanol, however, any potential PFOA residue would be soluble. Precipitates did not form in the solvent diluted samples and the results obtained are shown below. CC3YFG RESIN RD 9112 RESIN 110.000 ug/kg 160.000 ug/kg The confirmation analyses (second preparation technique) indicate that there may be a significant low bias in the original results. The results of the second analyses are approximately 25% higher than the original analyses. It is the reviewer's opinion that the second analysis results are the better representation of the samples' PFOA content. 000006 EXECUTIVE SUMMARY - Detection Highlights D6A270318 PARAMETER CC3YFG RESIN SAMPLE 12/18/05 001 Perfluorooctanoic Acid Perfluorooctanoic Acid ED 9112 RESIN SAMPLE 12/18/05 002 Perfluorooctanoic Acid Perfluorooctanoic Acid RESULT 78000 110000 130000 160000 REPORTING LIMIT UNITS 2500 250 ug/kg ug/kg 25000 250 ug/kg ug/kg ANALYTICAL METHOD DEN -LC-0012 DEN -LC-0012 DEN -LC-0012 DEN -LC-0012 000007 METHODS SUMMARY D6A270318 ANALYTICAL PARAMETER_________________________________________ METHOD______ LC/MS/MS, PFOA DEN -LC-0012 References: DEN Severn Trent Laboratores, Denver, Facility Standard Operating Procedure. PREPARATION METHOD 000008 METHOD / ANALYST SUMMARY D6A270318 ANALYTICAL METHOD _________________ _ ANALYST______ DEN -LC-0012 Steve Cowling References: DEN Severn Trent Laboratores, Denver, Facility Standard Operating Procedure. ANALYST ID_____ 008738 000009 SAMPLE SUMMARY D6A270318 SAMPLED SAMP WO # SAMPLE# CLIENT SAMPLE ID________________________________________________ DATE TIME HWFOE 001 CC3YFG RESIN SAMPLE HWFOF 002 RD 9112 RESIN SAMPLE 12/18/05 12/18/05 NOTE(S) ;_________________________________________ - The analytical results of the samples listed above are presented on the following pages. - All calculations are performed before rounding to avoid round-off errors in calculated results. - Results noted as "ND" were not detected at or above the stated limit. - This report must not be reproduced, except in full, without the written approval of the laboratory. - Results for the following parameters are never reported on a dry weight basis: color, corrosivity, density, flashpoint, ignitability, layers, odor, paint filter test, pH, porosity pressure, reactivity, redox potential, specific gravity, spot tests, solids, solubility, temperature, viscosity, and weight. ooooio GE Plastics Client Sample ID: CC3YFG RESIN SAMPLE HPLC Lot-Sample #... Date Sampled__ Prep Date..... Prep Batch #... Dilution Factor D6A270318-001 12/18/05 01/31/06 6031073 1000 Work Order #...: HWF0E1AA Date Received..: 01/27/06 Analysis Date..: 02/02/06 Analysis Time..: 12:43 Method........ : DEN -LC-0012 Matrix PARAMETER_____________________ RESULT________ Perfluorooctahoic Acid 78000 REPORTING LIMIT UNITS 2500 ug/kg PERCENT SURROGATE_____________________ RECOVERY______ 13C2 92 RECOVERY LIMITS (50 - 200) : SOLID O O O O ll GE Plastics Client Sample ID: HD 9112 RESIN SAMPLE HPLC Lot-Sample#...: D6A270318-002 Date Sampled...: 12/18/05 Prep Date..... : 01/31/06 Prep Batch #...: 6031073 Dilution Factor: 10000 Work Order #...: HWF0F1AA Date Received..: 01/27/06 Analysis Date..: 02/02/06 Analysis Time..: 12:57 Method........ : DEN -LC-0012 Matrix........ : SOLID REPORTING PARAMETER_____________________ RESULT_________ LIMIT UNITS____ Perfluorooctanoic Acid 130000 25000 ug/kxj PERCENT RECOVERY SURROGATE_____________________ RECOVERY_______ LIMITS 13C2 96 (50 - 200) 000013 GE Plastics Client Sample ID: BD 9112 BESIN SAMPLE HPLC Lot-Sample Date Sampled... Prep Date..... Prep Batch #... Dilution Factor D6A270318-002 12/18/05 02/08/06 6039144 100 Work Order #. Date Received. Analysis Date. Analysis Time. HWF0F1AE 01/27/06 02/08/06 11:04 Method........ : DEN -LC-0012 Matrix. PARAMETER Perfluorooctanoic Acid RESULT 160000 REPORTING LIMIT UNITS 250 ug/kg SURROGATE 13C2 PERCENT RECOVERY 94 RECOVERY LIMITS (50 - 200) : SOLID 000014 QC DATA ASSOCIATION SUMMARY D6A270318 SAMPLE# 001 002 Sample Preparation and Analysis Control Numbers MATRIX SOLID SOLID SOLID SOLID ANALYTICAL METHOD DEN -LC-0012 DEN -LC-0012 DEN -LC-0012 DEN -LC-0012 LEACH BATCH # PREP BATCH # 6031073 6039144 6031073 6039144 MS RUN# 6031053 6031053 >00015 METHOD BLANK REPORT HPLC Client Lot #...: D6A270318 MB Lot-Sample #: R6A310000-073 Analysis Date..: 02/02/06 Dilution Factor: 1 Work Order # __ : HWJ7J1AA Prep Date..... : 01/31/06 Prep Batch # __ : 6031073 Matrix........ : SOLID Analysis Time..: 12:29 PARAMETER_____________ Perfluorooctanoic Acid REPORTING RESULT________ LIMIT UNITS ND 2.5 ug/kg METHOD_______ DEN -LC-0012 SURROGATE 13C2 PERCENT RECOVERY 97 RECOVERY LIMITS (50 - 200} NOTE (S) :____________________________________ Calculations are performed before rounding to avoid round-off errors in calculated results. 000016 METHOD BLANK REPORT HPLC Client Lot #...: D6A270318 MB Lot-Sample #: R6B080000-144 Analysis Date..: 02/08/06 Dilution Factor: 1 Work Order #...: HW2L81AA Prep Date..... : 02/08/06 Prep Batch #...: 6039144 Matrix...... .. : SOLID Analysis Time..: 10:51 PARAMETER_____________ Perfluorooctanoic Acid REPORTING RESULT________ LIMIT UNITS______ METHOD______ ND 2.5 ug/kg DEN -LC-0012 SURROGATE 13C2 PERCENT RECOVERY 103 RECOVERY LIMITS {50 - 200) NOTE(S) :____________________________________ Calculations are performed before rounding to avoid round-off errors in calculated results. 000017 LABORATORY CONTROL SAMPLE EVALUATION REPORT HPLC Client Lot #... LCS Lot-Sample# Prep Date..... Prep Batch #... Dilution Factor D6A270318 Work Order #... : HWJ7J1AC R6A310000-073 01/31/06 Analysis Date..: 02/02/06 6031073 Analysis Time..: 12:34 1 Matrix PARAMETER Perfluorooctanoic Acid Ammonium Perfluorooctanoate (APFO) PERCENT RECOVERY 102 102 RECOVERY LIMITS (70 - 130) (70 - 130) METHOD DEN -LC-0012 DEN -LC-0012 SURROGATE 13C2 PERCENT RECOVERY 89 RECOVERY LIMITS (50 - 200) NOTE (S) :____________________________________ Calculations are performed before rounding to avoid round-off errors in calculated results. Bold print denotes control parameters : SOLID 000018 LABORATORY CONTROL SAMPLE DATA REPORT HPLC Client Lot #...: D6A270318 Work Order #...: HWJ7J1AC LCS Lot-Sample#: R6A310000-073 Prep Date..... : 01/31/06 Analysis Date..: 02/02/06 Prep Batch #...: 6031073 Analysis Time..: 12:34 Dilution Factor: 1 Matrix..... . : SOLID PARAMETER Perfluorooctanoic Acid Ammonium Perfluorooctanoate (APFO) SPIKE AMOUNT 49.5 51.5 MEASURED AMOUNT 50.6 52.7 UNITS ug/kg ug/kg PERCENT RECOVERY 102 102 METHOD DEN -LC-0012 DEN -LC-0012 SURROGATE 13C2 PERCENT RECOVERY 89 RECOVERY LIMITS (50 - 200) NOTE (S) : Calculations are performed before rounding to avoid round-off errors in calculated results. Bold print denotes control parameters 000019 LABORATORY CONTROL SAMPLE EVALUATION REPORT HPLC Client Lot #...: D6A270318 Work Order #...: HWJ7J1AD LCS Lot-Sanale#: RSA310000-073 Prep Date..... : 01/31/06 Analysis Date-.: 02/02/06 Prep Batch #...: 6031073 Analysis Time..: 12:38 Dilution Factor: 1 Matrix........ : SOLID PARAMETER Perfluorooctanoic Acid Ammonium Perfluorooctanoate (APFO) PERCENT RECOVERY 98 98 RECOVERY LIMITS (70 - 130) (70 - 130) METHOD DEN -LC-0012 DEN -LC-0012 SURROGATE 13C2 PERCENT RECOVERY 90 RECOVERY LIMITS (50 - 200) NOTE(S) :____________________________________ Calculations are performed before rounding to avoid round-off errors in calculated results. Bold print denotes control parameters 000020 LABORATORY CONTROL SAMPLE DATA REPORT HPLC Client Lot # -- : D6A270318 Work Order #...: HWJ7J1AD LCS Lot-Sarople#: R6A310000-073 Prep Date..... : 01/31/06 Analysis Date..: 02/02/06 Prep Batch. : 6031073 Analysis Time..: 12:38 Dilation Factor: 1 Matrix....... .: SOLID PARAMETER Perfluorooctanoic Acid Ammonium Perfluorooctanoate (APFO) SPIKE AMOUNT 4.95 5.15 MEASURED AMOUNT 4.86 5.06 UNITS ug/kg ug/kg PERCENT RECOVERY 98 98 METHOD DEN -LC-0012 DEN -LC-0012 SURROGATE 13C2 PERCENT RECOVERY 90 RECOVERY LIMITS (50 200) MOTE (S) ____________________________________ Calculations are performed before rounding to avoid round-off errors in calculated results. Bold print denotes control parameters 000021 LABORATORY CONTROL SAMPLE DATA REPORT HPLC Client Lot #..- : D6A270318 Work Order #...: HW2L81AC LCS Lot-Sample#: R6B080000-144 Prep Date..... : 02/08/06 Analysis Date..: 02/08/06 Prep Batch : 6039144 Analysis Time..: 10:55 Dilution Factor-: 1 Matrix....... .: SOLID PARAMETER Pexfluorooctanoic Acid Ammonium Perfluorooctanoate (APPO) SPIKE AMOUNT 2.00 2.08 MEASURED AMOUNT 2.07 2.16 UNITS ug/kg ug/kg PERCENT RECOVERY 104 104 METHOD DEN -LC-0012 DEN -LC-0012 SURROGATE 13C2 PERCENT RECOVERY 96 RECOVERY LIMITS (50 - 200) NOTE (S) :_________________________________ - Calculations are performed before rounding to avoid round-off errors in calculated results. Bold print denotes control parameters 00023 STL Denver 4955 YarrowStreet Arvada, CO 80002 phone303-726-0100 fax 303-421-7171 Client Contact GE Plastics PO Box 68 State Routs 692 Washington. WV 26181 304/863-7737 304/663-7825 ABS Resin C-8 analysis Washington, WV 26181 PO BOX68 Sample Identification CC3YFG resa smote RD9112 resinsample Chain of Custody Record A/*MW t / \ 0 ft V**f* Project Manager Tel/Fax: AnalysisTurnaround Time Calendar(C 1er WorkDavafW l. TATIfdifferent tamRetM Site Contact: Lab Contact: IT 1,1 3 li!a Wk t , t f \ Mi a i * A S A P 1--* 2days H a i___ S _______ __________________B 1Sample Sample Sample sr Date Time T7pc Matrix C M . i M ' m Resinsolid X 12/18/05 Resinsolk X Date: Carrier: ! STLS li V li R N TRENT ievent Trent Laboratories, Inc. COC No: oC COCs Job No. SDG No. SanoleSpedite Notes: AnalvseibrC-8 PF0A1 insotid matrix Anaiyse for C-8 (PFO) te solidmairi: --i --J n .j j n! (preservation Used: 1- Ice. 2=*HCU 3- H2S04: 4-HN03: 5NaOH: 6- Other HonorIdentification Non-Hazard Flammable a SkinIrritant CD PoisonB Spedili tosiructioni/QC Requirements & Comments! 1 Sample D isposal ( A fee ma\ tbe assessed if sam ples ere retained longer than 1month) Vnhmn Return To Client / P Disposal By Lab ^ Archive For________________ Months JcuQCi i J M Sfmqnishedby: ReBnqmshetfby: Company: Company: tete/Tteie:, 1/XL9& D^oTime: Reeeteedbyr'"'^ DatefTime; Received by: f (CSomapawny: Company: Dste/Timc Date/Time: A M *' \)(A J 00024