Document jyGdvDn6oOJgD4LVkZYy5wrRR

RECYCLED CO cn AR226-2646 05/09 '02 13:51 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3735 PAGE 2 AR226-2646 REPORT N O . t STT-91-1 DATE ISSUED} 01/16/92 COPY NUMBER} RICHMOND, VIRGINIA FIBERS DEPARTMENT SPRUANCE "TEFLON" TECHNICAL E. I. DU PONT DE NEMOURS & CO., INC. COMPANY CONFIDENTIAL TECHNICAL REPORT PERFLUORO OCTANOIC ACID CONCENTRATION (C8) IN WASTE WATER J. C. Moore REPORT WRITTEN BY: WORK SUPERVISED BY; PREVIOUS RELATED REPORTS: PROJECT CODE: PERIOD COVERED: NOTEBOOKS COVERED: J. C. Moore___________________ JAMES L. SIBLEY_______ ________ SPAR 79-3, SPAR 82-1, TR 82-1 N/A___________________________ 9/91 - 12/91__________________ N/A ABSTRACT The company has set a CEG (Community Exposure Guideline) of 1 ppb in water for ammonium pefluoro octanoate (C8), a surfactant in the Teflon* dispersion used to produce Teflon* Fiber. A conservative position of assuming all C8 ends up in the James River would produce an average concentration of 0.1 ppb. The only time the CEG could be exceeded would be during periods of extreme low flows in the river. 05/09 '02 13:51 ID:DUPONT ENV AFFAIRS FAX1-804-383-3785 PAGE 5 STT-91-1 TABLE OF CONTENTS m. 1. INTRODUCTION 1-4 2. DISCUSSION 1-4 A. EARLIER ISSUES 8. TEFLON* DISPERSIONS C- PREVIOUS CONCERNS D. PRESENT ENVIRONMENTAL CONCERNS 3. REFERENCES .5 4. TABLES o JC'H-1 THE EFFECT OF HEAT ON EXTRACTABILITY OF C8 FROM YARN 5. FIGURES 6 1. MASS BALANCE OF C8 IN TEFLON* SPINNING 7 2 . HASS BALANCE OF C8 IN SPRUANCE WASTE WATER SYSTEM 8 3. PROPOSED MASS BALANCE OF C8 IN TEFLON* SPINNING 9 4. PROPOSED MASS BALANCE AROUND WASTE WATER SYSTEM 6- APPENDIX 10 I. SPRUANCE C8 ASSESSMENT II II. SPRUANCE C8 ANALYSIS 12 III. ANALYTICAL DATA FOR LMG LABORATORY NO. 20152 13-28 05/09 '02 13:52 ID:DUPONT ENV AFFAIRS FAH:1-804-383-3785 PAGE 6 STT-91-1 1. 1. INTRODUCTION Teflon* colloidal dispersion is mixed with viscose in the manufacture of Teflon* fiber. The cellulose contained in the viscose is regenerated in the coagulation/acid bath in spinning. The regenerated cellulose acts as a matrix to bind Teflon* particles prior to sintering. Surfactants are used in the manufacture of colloidal Teflon* dispersions to prevent conglomeration of particles. One of the surfactants used is F-143, ammonium perfluoro octanoate (commonly referred to as C8). 2, DISCUSSION A. EARLIER ISSUES In 1978, the 3M Company notified DuPont that C8 used in Teflon* polymerization may be teratogenic. Airborne dust or vapors were felt to be the source of the exposure. Several technical projects(Reports SpAR 79-3, SpAR 82-1 & TR 82-1) were initiated to study the potential exposure to C8 by DuPont employees. C8 was not detected in the work place air environment. The handling of coated packing yarns or direct contact with Teflon* dispersion were the only potential areas that personnel can be exposed to significant levels of C8 (Ref. 4). Tests at Haskell Lab shoved no transfer of C8 from yarns to rabbit skin and suggested C8 exposure of persons handling dry yarn is minimal (Ref. 5). C8 was later determined not to be teratogenic by 3H and DuPont's Haskell Labs. B. TEFLON* DISPERSION Teflon* dispersion is produced in a batch operation at Washington Berks. C8 which, is the ammonium salt of perfluoro octanoic acid is used as a wetting agent to prevent conglomeration of the Teflon* particles. A batch of dispersion is initially about 7000 lbs which contains 3000 lbs of Teflon* monomer. A total of 4060 grams of C8 is added to the batch in the precharge and injection steps. After polymerisation is completed, the dispersion is decanted to obtain BOX solids. Washington Works estimates that 50% of the C8 is removed with the decanted superannuate and the other 50% goes with the concentrated dispersion. On a Teflon* solids basis, the C8 concentration would be 1490 ppm, and 900 ppm on a dispersion basis. The Teflon* dispersion (T 3311) used for fiber production is pH adjusted with sodium hydroxide which changes the C8 from an ammonium salt to a sodium salt- In the coagulating/acid bath used in Teflon* fiber spinning, the C8 will convert to the acid form, perfluoro octanoic acid. 05/09 '02 13=52 IDDUPONT ENV AFFAIRS FAX1-804-383-3785 PAGE 7 $TT-9l-l. 2. DISCUSSION CONT'D C, PREVIOUS CONCERNS Previous research examined employee potential exposure to C8 through handling of yarn. Sintered Teflon* yarn had non-detectable levels of C8 (Ref. 4). The Teflon* fiber sintering temperature is 325 C. The boiling point of perfluoro octanoic acid is 188 C. Yarns with a Teflon* coating, which are not exposed to high temperatures did contain detectable levels of C8. Thermal treatment of these yarns was effective in removing the C8, The research showed that the C8 removal was a function of time and temperature (Table l),(Sef, 2). IR scans of off gas from the heated yarn samples provided the basis for the conclusion that the C8 decarboxylates into C02 and perfluoro monohydride and does not evaporate as it is heated up to 200 C- (Ref- 4). The data follows the kinetic "rule of thumb" that increasing the temperature 10 C produces a doubling of the rate- Extrapolating this relationship up to the sintering temperature of Teflon* predicts that all the C8 is removed from the fiber, D- PRESENT ENVIRONMENTAL CONCERNS The present environmental concerns with C8 are with ground water contamination. A CEG (Community Exposure Guidelines) of 1 ppb in water has been established by Haskell Labs. Samples of effluent from different spots in the Teflon* spinning process were taken to estimate the concentration of C8 in the site's waste . streams. Sample locations are listed in Appendix I. CH2M Hill was contracted to analyze the samples. A summary of their results are in Appendix I. A complete report from CK2M Hill is contained in Appendix II. The sample results do not allow for a complete mass balance. The measured concentrations in the effluent streams only accounts for about 5Q> of the C8,(Pig. 1 & 2 ). There are several possible explanations, the initial C8 concentration is 750 ppm on a dry Teflon* basis, the C8 , chemically reacts, it is encased in the yarn, it decomposes, evaporates or the reported levels are in error low. The lower initial C8 concentration is not likely because of independent analysis done by Washington Work and Spruance have measured the concentration, at about 1000 ppm on a dispersion basis. The C8 will change to perfluoro octanoic acid in the bath which should not react with the normal contents of the Teflon* spinning acid bath. There is no reasonable way to prove the idea of C8 being encased in the yarn. 05/09 '02 13:52 IDDUPONT ENV AFFAIRS FAX=1-804-383-3785 PAGE 8 STT-91-1 2. DISCUSSION CONT'D D. PRESENT ENVIRONMENTAL CONCERNS CONT'D Previous work measured C8 on unsinterred Teflon* yarn at 60 ppm (Ref. 4). The concentration would need to be 700 ppm to account for the Missing C8. The previous work concluded that the C8 carried with the unsinterred Teflon* yarn would decompose during the sinterring process. This is in contradiction to Washington Works process of recovering C8 from their "fine powder" exhaust stream. "Fine powder" Teflon* has been tested and found to contain little or no C8- The "fine powders" are dried at 190 C. Washington Works recovery of C8 from the "fine powders" exhaust contradicts the previous conclusion about decarboxylation versus evaporation. If C8 evaporates off the yarn in the fiber spinning process, it should condensed in the spinning exhaust system. To reduce the potential for a duct fire, water is sprayed in the exhaust hood to reduce the temperature down below 65 C, The exhaust gas then passes through a wet scrubber and the final gas temperature is basically reduced to ambient conditions. The water drained from the exhaust hood and the scrubber go into the Teflon* basement east floor trench. If all of the C$ eventually ends up in the sewer, this would lead to the conclusion that the analysis from CH2M . Hill are low. CH2H Hill ran surrogates on three samples. Surrogate recoveries were not determined on the high concentrated samples due to the large dilution required for analysis. Surrogates were run on the discharge from the exhaust scrubber and two distilled water samples, one sent by Spruance and one from CH2H Hill's lab- The exhaust scrubber effluent was analyzed to have 1.8 ppb of C8, and the detection of known amounts of surrogate material added was less than 50%. The explanation for the low surrogate recovery was due to the noise created by a large non-target chromatographic peak coupled with a large dilution factor. Decomposition products of cellulose that are scrubbed out of the exhaust gas are the mostly likely cause of the non-target chromatographic peak. . The surrogate recoveries on the distilled water samples ran from 52% to 86%. The possibility of the analysis being low is real. There is alot of contradicting material on the fate of C8 in the Teflon* spinning process. The belief that CH2M Hill's results are low by a factor of ~2X would tie together the majority of the material. The 60 ppm measured concentration of C8 on the yarn only accounts for `5% of the total material. The other 95% exits the process in the wet portion of the spinning process, the washing step since the acid bath is 100% recycled. The 5% on the yarn evaporates and then condenses in the exhaust hood similar to Washington Works recovery process. Only trace amounts of C8 should reach the scrubber. The amount found in the exhaust scrubber was less than 0.02% of the total amount. 05/09 '02 13:53 IDDUPONT ENV AFFAIRS FAK:1-804-383-3785 PAGE 9 STT-91-1 4. 2. DISCUSSION CQNT'P D. PRESENT ENVIRONMENTAL CONCERNS CQNT'P If 95% of the C8 exits the process with the wash water, the concentration of SK #2 sample should have been 4600 ppb, CH2H Hill's measured amount of 2400 ppb is 52% of that level. This percentage is in the range of report surrogate recoveries on distilled water. The most conservative position in estimating the potential environmental Impact is to assume that all of the C8 ends up in the plant's waste effluent. This would about double all of CH2H Hill's measured concentrations (Fig 3 & 4), During the sampling period 11/13 & 11/14/91 and estimated 1194 grams/day of C8 were discharge to the James River. The long terra average(1937 to 1987) flow for the James River is 5104 HHgpd- This would make the C8 concentration in the James River an estimated 0.06 ppb. The average annual production Tate for Teflon fibers is 1 MM lb. This would discharge 1490 lb- of C8 to the James River annually. The estimated 08 concentration in the river would be 0,10 ppb. The maximum production rate for Teflon fibers is 4200 lb./day. This could add 6.3 lbs C8/day to the James River and produce an estimated C8 concentration, of 0.15 ppb in the river. The low flow in a 10 year repeating cycle (as defined by 7Q10) for the James River is 408 HHgpd. An average production rate during this period would produce an estimated C8 concentration in the James River of 1.20 ppb and maximum production rates would increase the concentration to L.84 ppb. During the low flow periods, which should happen once every 10 years, production may need to be curtailed to 2300 lb./day of Teflon* fiber to stay below the CEG of 1 ppb. 05/09 '02 13=53 ID=DUPONT ENV AFFAIRS FAX=1-804-383-3785 STT-91-1 REFERENCES 1. Forte, H.A. <*. SpAR 79-3 2. Forte, H . A . , Hokhtar, A.M. - PCD Monthly, June, 1981 3. Shelburne, S-S- - PCD Monthly, December, 1981 4. Shelburne, S.S., Forte, H.A., Hokhtar, A.H. - SpAR 82-1 5- Burks, P.P., - TR 82-1 05/09 '02 13:53 IDDUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 8TT-91-1 TABLE 1 THE EFFECT OF HEAT OH EXTRACTABILITY OF C8 FROM YARM (Ref. 2) Initial C8 concentration on 9450 I & T yarn ~ 600 ppm % C8 Remaining on Yarn Time of Heat(minutes) 150 C 175 C 200 C ' 10 75 41 N/D 20 72 12 N/D 30 72 N/D N/D 40 47 N/D N/D N/d Not detectable, < 5 ppm Least Square Fit for proposed 1st Order Decarboxylation 15Q*C A - A 0 * e~-0155c (t-minutes) 175C A - A0 * +10-C -> (0.106/0.0155) - 2.16 (close to "rule of thumb" for temperature dependency of kinetic reactions, +10C roughly doubles reaction rate) aExtrapolation to 200*0 using power of 2.16 per 10"C @ 2 0 0 'C A . A 0 * e `" .ast t - 10 min, A,, * 600 ppm A * 0.4 ppm which is <5 ppm minimum detectable limit 05/09 '02 13:53 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 12 STT-91-1 FIGURE 1 MASS BALANCE OF C8 USING CHgM HILL TEST RESULTS TEFLON* SPINNING NOVEMBER 13* 1991 A7M SSft*& es 5ui kc<jeMUTi0iy-rt* * E 0 ,n 3 * 1 0 0 / Co.54-1 1 9<o7 O' ^r- ni-J 6 - <1 Q u N. 00 * n d ? tr j s A 3 n o i u A A t IS 05/09 '02 13:53 IDDUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 13 STT-91-1 FIGURE 2 MASS BALANCE OF C USING CHgM HILL TEST RESULTS SPRUANCE WASTE'.HATER'TREATMENT SYSTEM NOVEMBER 13, 1991 is s u x u s 8, AvtiitAt. s.54 UM.<yam. Rueis <p dKtrt Uh a ,touu's t e^riWAlt potlift -J O.Q^ppJ, 05/09 '02 13:53 IDDUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 14 STT-91-1 FIGURE 3 . PROPOSED MASS BALANCE OF C8 IN TEFLON* SPINNING NOVEMBER 13, 1991 I1HI v r* &w q 15 05/09 '02 13=54 IDDUPONT ENV AFFAIRS FAK:1-804-383-3785 PAGE 15 STT-91-1 . FIGURE 4 PROPOSED MASS BALANCE AROUND WASTE WATER SYSTEM NOVEMBER 13, 1991 10. scuxer, I 05/09 '02 13:54 IDDUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 16 STT-91-11 APPENDIX I SPRAHCE C8 ASSESSMENT e . I. d u p a r r d e N e m o u r s & co., i n c , Fibers Business cc: G. L. Kennedy - Haskell G. A. Hapka - Legal R. A. Reich- Engr, - Louviers J. D. Chidley R. L. Dunn C. P. flihal r . c. Xeatts D. M. Schwartz G, R- Sisson j, s. Tschritter SPRUANCE FIBERS PLANT Richmond, Virginia December 4, 1991 5TOt / . C. MOORE - TEFION TECHNICAL FROM: T. V. ROBERTSON - ENVIRONMENTAL AFFAIRS SPRUANCE C8 ASSESSMENT A s a result of our discussions of 11/1/91, Environmental Affairs has sampled various points in the Spruance Teflon process as well as the site wastewater treatment system for ammonium perfluorooctanate (CB). The results are contained in the attached table C8 is used as a dispersant to make PTFE at Parkersburg PTFE is used at Spruance to make Teflon^ fiber* CB is an impurity in PTFE and, thus, is introduced into the process at Spruance- The sampling scheme employed evaluated the C8 content at the wash water discharge in the spinning operation, in the air emissions control scrubber effluent, in - the area process sewer, in the site composite process sewer (inlet to wastewater treatment system), and at the discharge of the WWTS which combines with the non-contact streams discharging to the James River. C8 content in these samples appear in line with your earlier estimates. Assuming Outfall 002 flow of 10 MMGD, a total site effluent of 14.4 MMGD (winter time), and a James River low flow 7Q1Q of 408 MMGD, a river concentration of 0.4 ppb is calculated as a worst case. I would appreciate your comments on these sample results. TVR:mcp 29:1.30 05/09 '02 13:54 IDDUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 17 STT-91-1 APPENDIX II SPRUANCE C8 ASSESSMENT SPRUANE C8 ANALYSIS 12. SAMPLE NO. 1 2 3 4 5 6 SAMPLE TYPE LOCATION C8 CONC. (a/q /L ) Composite* Composite* SM#2 wash Water Discharge Scrubber Effluent Discharge 2400 1.8 . 24 Hour Composite East Trench (Process Sewer) 950 24 Hour Composite influent to WWTS (Outfall 006) 22 24 Hour Composite Effluent from WWTS (Outfall 002) Blank-DI Water _ 18 <MDL * 4 grabs collected over 8 hours and combined as one sample. MDL - detection limit 0,1 /og/L 29:1.30 05/09 '02 13:54 IDDUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 18 STT-91-1 APPENDIX III ANALYTICAL DATA FOR LMG LABORATORY NO. 20152 November 27, itv. LMG-27317 .XX 13. Mr Tom Roberteon El DuPont de Nemours Co., Inc. Spruance Plant - East Office Bldg. p.O. Box 27001, Jefferson Davis Hwy. Richmond, Virginia 23261 RE; Analytical Data for l m g Laboratory No. 20152 Dear Mr. Robertson: On November IS, 1991, the CH2M HILL Montgomery Laboratory received six samples With a request for analysis of selected organic parameters. The analytical results and associated quality control data are enclosed. Any unusual difficulties encountered during the analysis of these samples are discussed in the case narrative. If you should have any questions concerning the data, please inquire. The CH2H HILL policy is to store samples for up to 30 days after reporting. - if you desire, our laboratory will maintain your samples for a longer period at a cost of $5.00 per sample per month. Samples determined to be hazardous can either be returned to you or disposed of at a cost of $2 5 . 0 0 per sample. Sincerely, i/ J c u J b ^ o A - ^ a JU - wanda L. Hall Data Package Supervisor Enclosures . CH2MHIU Quality Aii'ihflirntt ?56? FS'tlane Drive P Q 80x23054(1 205 2T! 4 05/09 '02 13=54 IDDUPONT ENV AFFAIRS FAH:1-804-383-3785 PAGE 19 STT-91-1 APPENDIX III ANALYTICAL DATA FOR LUG LABORATORY NO. 20152 14. TABLE OF CONTENTS CH2K firr.r. Laboratory No- 20152 . , List: of Organic Analytical Mathoda ............................ . Page No. i. List of OrganicEFA-defIned Qualifier a ............................... ii List at Organic Sample ID- Qualifiers .......................... ill SampleCross-Reference ................................... iv FC-- 143 DATA case Narrative .............................. -.................. 1-2 Analytical Results of Field Samples NUMBER 1 (LMG #20152001) 3 NUMBER 2 (LMG #20152002) 4 NUMBER 3 (LMG #20152003) ..... ....................... 5 NUMBER 4 (LMG #20152004) 6 NUMBER 5 (LMG #20152005) 7 NUMBER 6 (LMG (20152006) 8 Quality Control Data Results of QC Slant (W11211B1) .......... ...... ........ 9 C 4 0 - i.s <\JO tL\t Copy of Chain-of-cuatody 10 05/09 '02 13:54 IDDUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 20 STT-91-i APPENDIX III ANALYTICAL DATA FOR LHG LABORATORY NO. 20152 15. AHM.XTICAI. METHODS Organic Analysis Priority Pollutants: Water, soil and waste sample are analyzed in accordance with procedures described in Method 6QB, 624, and 625, EPA-60Q/4-82-057 (1982); Methods 8080, 8240, and 8270, Test Methods oxr Evaluating Solid Waste, 1986, SW-846, Third Edition; and methods outlined in the USEPA Contract Laboratory Program Statement of Work for Organics Analysis, February, 1988. Volatile Analysis (Safe Drinking Water Act); Water samples are analyzed in accordance with procedures described in Method 524.2, Federal Register (50 PR 46902), November 13, 1985. Chlorinated Phenoxyacid Herbicides: Samples are analyzed in accordance with procedures described in Method 8150, Test Methods for Evaluating Solid Waste, 1986, SW-846, Third Edition. organophosphorous Pesticides: Samples are analyzed in accordance with procedures described in Methods 614 and 622, EPA-600/4-79-019 (1979) and in Method 8140, Test Methods for Evaluating solid Waste, 1986, sw-846, Third Edition. Phenolic Acid Analysis by GC: Sample are analyzed in accordance with procedures described in Method 604, Federal Register, 40 CFR, Part 136 (July 1, 1987) and in Method 8040, Test Methods for Evaluating Solid waste, 198, SW-846, Third Edition. Polynuclear Aromatic Hydrocarbons (GC analysis): Samples are analyzed in accordance with procedures described in Method 610, Federal Register, 40 CFR, Part 136 (July 1, 1987) and in Method 8100, Teat Methods for Evaluating Solid Waste, 1986, SW-846, Third Edition. Ethylene Dibromide: Water samples are analyzed in accordance with procedures described in Method 504, Federal Register, (50 FR 46902), November 13, 1985. Trihalomethanes: Water samples are analyzed in accordance with procedures described in Method 501.2, Federal Register, Vol,. 44, No. 23i, Part XI, November 29, 1979. 05/09 '02 13=56 IDDUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 2 ST-91-1 APPENDIX III ANALYTICAL DATA FOB LMG LABORATORY NO, 20152 16. EPA - DEFINED QUALIFIERS ORGANICS Definitions for the EPA-defined qualifiers: U -- Indicates the compound was analyzed for but not detected. The number adjacent to the "u- qualifier indicates the quantitation limit for that compound. The detection limit can vary from sample to sample depending on dilution factors or percent moisture adjustment when indicated. J -- indicates an estimated value. This flag is used when the mass spectral data indicates the presence of a compound below the stated quantitation limit. The "Of- qualifier is not used with pesticide results. C -- This flag applies to pesticide results only. The "C" flag indicates the presence of this compound has been confirmed by GC/MS analysis. B -- This flag is used when the analyte is found in the associated blank as well as the sample. This notation indicates possible blank contamination and suggests the data user evaluate these . compounds and their amounts carefully. E -- This flag applies to GC/MS only. The "E- qualifier indicates a compound may be above or below the linear range of the instrument. If the particular compound level is deemed above the linear calibration range, then the sample should be reanalyzed at an appropriate dilution- Therefore, the "E- qualified amount is an estimated concentration. The results for the dilution will be reported on a separate Form I and will be flagged with a "D" if the dilution brings the concentration within proper calibration. ^ ~~ This flag identifies compounds which have been run at a dilution to bring the concentration of that compound within the linear range of the instrument. "D" qualifiers are only used for samples that have been run initially with results above acceptable ranges. For secondary dilutions the "DL" suffix is appended to the sample number on the Form I . A indicates the Tentatively Identified Compound {TIC) ig a suspected aldol-condensation product. X Indicates the compound concentration has been manually modified or the EPA qualifier has been manually modified or added. ax -- The compound was detected and quantitated below the Contract Required Quantitation Limit. . ii 05/09 '02 13=57 ID:DUPONT ENV AFFAIRS FAX:1-804-333-3785 PAGE 3 STT-91-1 APPENDIX III ANALYTICAL DATA FOR LHG LABORATORY NO. 20152 17. CLIENT SAMPLE ID QtJAi.1PIERS LEVEL 1 The qualifiers that GC/h s and g c use with the client sample ID are defined below; DL -- Dilution Run R -- Rerun (may be followed by a digit to indicate multiple reruns) RD -- Diluted Rerun RX --- Re-extraction Analysis MS -- Matrix Spike (may be followed by a digit to indicate multiple matrix spikes within a sample set) HSD --- Matrix spike Duplicate (may be followed by a digit to indicate multiple matrix spike duplicates within a sample sat) QCJBLftNX --- Method Blank (may be followed by a "W" for waters, "S" for soils run at a low level, or "SM" for soils run at a medium level ---- these letters may be followed by a digit to indicate multiple blanks of that type; if there are no letters, the digit indicates multiple blanks). These qualifiers allow GC/MS and GC to have unique client sample ID's so that the client can. get more accurate information from the data reported- 05/09 '02 13=57 IDDUPONT ENV AFFAIRS FAX=1-804-383-3785 PAGE 4 STT-91-i APPENDIX III ANALYTICAL DATA FOR IHG LABORATORY NO- 20152 18. TABUS 1 SAMPLB CROSS--REFERENCE SUMMARY CH2H HILL Laboratory Mo. 20152 CH2M HILL Sample Mo. 2O152O01 20152OO2 20152003 20152004 2015200S 20152006 samolo Description NUMBER 1 NUMBER 2 NUMBER 3 NUMBER 4 NUMBER 5 NUMBER 6 11/14/91 11/14/91 11/14/91 11/14/91 11/14/91 11/14/91 0830 0330 0830 0830 0830 0830 COMP COMP COMP COMP COMP GRAB 05/09 '02 13:57 IDDUPONT ENV AFFAIRS FAX:1-804-383-3735 PAGE 5 STT-91-1 APPENDIX III ANALYTICAL DATA FOR LHG LABORATORY NO. 20152 19. CASE NARRATIVE FOR FC-143 GAS CHROMATOGRAPHY SAMPLES LABORATORY ; CH2M HILL LABORATORIES CASE NO. s N/A La b n o . ; 20152 CLIENT; E. I. DUPONT CONTRACT NO,; N/A SDG NO.i N/A I- RECEIPT A. DATE; November 15, 1991 B. SAMPLE INFORMATION LAB ID 20152001 201S2Q2 20152003 20152004 201i)i2DSi 20152OQ5 W11211B1 CLIENT ID NUMBER 1 NUMBER 2 NUMBER 3 NUMBER 4 NUMBER 5 NUMBER 6 QC BLANK SAMPLE DATE EXTRACTION ANALYSIS MATRIX SAMPLED DATE date WATER WATER WATER WATER WATER WATER WATER 11/14/91 11/14/91 11/14/91 11/14/91 11/14/91 11/14/91 NA 11/21/91 11/21/91 11/21/91 11/21/91 11/21/91 11/21/91 11/21/91 11/22/91 11/22/91 11/22/91 11/22/91 11/22/91 11/22/91 11/22/91 C. Documentation Exceptions ; No exceptions were encountered 05/09 '02 13=57 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 6 STT-91-I APPENDIX III ANALYTICAL DATA FOR LUG LABORATORY NO, 20152 20. FC-143 LAB NO. 20152 PAGE 2 II. EXTRACTION A. Holding times* All holding times were met. B . ExtractIon Exceptions . The native pH of two samples were unusually extreme for environmental samples. The native pH of 20152001 (NUMBER 1) was 3 and the native pH of 20152003 (NUMBER 3) was 12. No other exceptions were encountered. III. ANALYSIS A. Holding times* All holding times were met. B . Analyt leal Exceptions * Sample 20152002 (NUMBER 2) was diluted by a large factor due to interferences not removed by our cleanup procedures. No other exceptions were encountered- IV. QUALITY CONTROL A. Method Blank : All associated method blanks met acceptable QC criteria. B. Surrogate Recoveries : Surrogate recoveries were not determined for four field samples due to large dilutions required for analysis. Surrogate recoveries were below 50% for sample 20152002 (NUMBER 2). All other samples mat acceptable QC Limits. C. Matrix Spike Results * Matrix Spike results have not been reported with this contract. I certify that this data package is in compliance with the terms and conditions of the contract, both technically and for completeness, for other than the conditions detailed above. Release of the data contained in this hardcopy data package has been authorized by the Laboratory Manager or his desginee, as verified by the following signature. 05/09 'OS 13=57 ID=DUPONT ENV AFFAIRS FAX=1-804-383-3785 PAGE 7 STT-91-1 APPENDIX III ANALYTICAL DATA FOR LHC LABORATORY NO. 20152 .2 1 ORGANICS ANALYSIS DATA SHEET Laboratory Name: c h 2m HILL/MGM Concentration: LOW Date Extracted: 11/21/91 Lab Sample ID: 2Q152001______ Sample Matrix: HATER Date Analyzed: 11/22/91 Client sample ID: NUh Bk h 1_____ Percent Moisture: ______ Dilution Factor: 2500 FC-143 CAS Number_______ ________________ __ uiq/L 3825--26-1 PC-143 . , , ........ 2400 CAS Number____________________ uo/L Parluorononanoic acid - SS ND Perluorodecanale acid - ss ND 1lH-Eicoaafluoroundec&nolc acid - SS ND D - Analyzed for bet not detected. JX - Present, concentration estimated- 3 -- Detected in QC blank. Ss -- Surrogate Standard reported as percent recovery. ND - Not determined. ' commentss Surrogate recoveries were not determined due to the large dilution -squired for analysis. Form I 05/09 '02 13:57 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 8 ST-91-1 APPENDIX III ANALYTICAL DATA FOR LHG LABORATORY NO. 20152 22. ORGANICS ANALYSIS DATA SHEET Laboratory Name: CH2M HILL/HOM Concentrations LOW Lab sample ID: 20I52Q02 __ Sample Matrix: WATER Client Sample ID: NUMBER 2______ Percent Moisture: Date Extracted: 1 1/21/91 Date Analysed: il/32/91 Dilution Factor: 10 FC--143 CAS Number uq/L 3825V ,-26-1 FC--1 4 3 ............ . . 1.8 CAS Number Perluorononanoic acid -- ss <50 a Perluorodecanaic acid - SS <50 % 11H--Bicoeafluoroundecanoic acid - SS <5Q % _______ uo/L tl - Analyzed for but not detected. JX - Present, concentration estimated. B - Detected in QC blank. SS - Surrogate Standard reported as percent recovery. Comments; This aample was diluted for analysis because of large non--target Cchromatographic peaks discovered when the sample was screened. Surrogate jcoveries could net be determined accurately because of chromatographic noise coupled with a large dilution factor. Form I 05/09 '02 13=58 IDDUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 9 STT-91-1 APPENDIX III ANALYTICAL DATA FOR LHC LABORATORY NO. 20152 24. ORGANICS ANALYSIS DATA SHEET Laboratory Name; CH2M HILL/Mg m Concentration: LOW Lab Sample ID: ,201,52004 Sample Matrix? WATER Client Sample ID: NUMBER 4_____ Percent Moisture: ,, """" Data Extracted; 11/21/91 Dace Analyzed: 11/22/91 Dilution Factor: ______ 20 FC--143 CAS Number 3825-26-1 FC-143 qq/L 22 CAS Number uq/L PerfluorOnonanoic acid - SS ND PerfluoradecanoLe acid - ss ND llM-Eicoeaflworoundecanoic acid - ss nd j . U ~ Analysed for but not detected. JX - Present, concentration estimated. . a - Detected in QC blank. ss - Surrogate standard reported as percent recovery. ND -- Not determined. Comments: Surrogate recoveries were not determined due to the large dilution "squired for analysis. Form I 05/09 '02 13:58 ID:DUP0NT ENV AFFAIRS ,FAK:1-804-383-3785 PAGE 10 STT-91-1 APPENDIX III ANALYTICAL DATA FOR LMG LABORATORY NO. 20152 25. ORGANICS ANALYSIS DATA SHEET Laboratory Names CH2H HILL/hGH Concentration: l o w Lab Sample ID: 20152QO5_____ Sample Matrix; WATER Client Sample ID: NUMBER S Percent Moisture: ____ _ ate Extracted: Date Analyzed: 11/22/91 Dilution Factor: 2Q FC-143 CAS Humber ___________________uc/L 3825-26-1 PC-143 . . ........ * 1 CAS Hiimhftr . ia /1 * Perfluoronon&nolc acid - ss NS Perfluorodacanaic acid - SS ND 11H--ElCoe&fluorOundecanoic acid -- SS ND 1 tl - Analysed for but not detected. . JX - Present, concentration estimated. . B - Detected in QC blank. SS - Surrogate Standard reported as percent recovery. ND - Not determined. . Comments: Surrogate recoveries were not determined due to the large dilution -squired for analysis. Form I 05/09 '02 13:58 ID:DUPONT ENV AFFAIRS FAX1-804-383-3785 PAGE 11 STT-91-1 APPENDIX III ANALYTICAL DATA FOR LMG LABORATORY NO. 20152 26. ORGANICS ANALYSIS DATA SHEET Laboratory Name!: CH2M HTT.T./mg m Concentrations LOW Data Extracted! 11/21/91 Lab Sample ID: 2Q1520Q6 Sample Matrix: WATER,. Date Analyzed: 11/22/91 Client Sample ID: NUMBER &______ Percent Moisture: __ _ Dilution Factor: 1.0 FC-143 CRS Number 382I5k-26-- 1 FC-143 uq/L CAS Number 0.1 u Parfluorononanoic acid - SS 86 % .PerfInorodecanoic acid - ss 75 % llH-Eicoaafluoroundecanoic acid - SS 83 % uq. U - Analyzed for but not detected. JX - Present, concentration estimated. B - Detected in QC blank. SS - Surrogate Standard reported as percent recovery. Comments: Form I 05/09 '02 13=58 ID:DUP0NT ENV AFFAIRS FAX:1-804-383-3785 PAGE 12 5TT-91-1 APPENDIX III ANALYTICAL DATA-FOR LG LABORATORY NO. 20152 27. L,-: ' ' ORGANICS ANALYSIS DATA SHEET Laboratory Name: CH2M HILt/MCM concentration: LOW Lab Sample ID: W112 U B I ______ Sample Matrix: WATER Client Sample ID: OC BLANK_______ Percent Moisture: _ ,. Data Extracted: 11/21/31 Date Analysed: 11/22/91 Dilution Factor: _____ 1.0 FC--143 CAs Number____ _____________________ Ud/L c a s Number 382S-26-- 1 FC-- 143 ................ 0 . 1 U ______________________ HsZL P e r fl u O r o n o n a n o i C acid -- SS 81 % Per fluarodeoa n a l e acid -- SS 52 % llH-Eicoaafluoroundecanoic acid - SS 53 % u - Analysed for but not detected. j X - present, coneantration estimated. B - Detected in QC blank. SS - Surrogate Standard reported as percent recovery. Commentes Form I