Document zzproLpZBxqDqGNrGk7me6V4R

AR226-2646 00 01 05/09'02 13:51 ' .< . ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 2 AR226-2646 REPORT NO.? DATE ISSUEDi COPY NUMBER? STT-91-1 01/16/92 ___ RICHMOND, VIRGINIA FIBERS DEPARTMENT SFRUANCE "TEFLON" TECHNICAL I. E. DO FONT DE NEHOURS & CO., INC. COMPANY CONFIDENTIAL TECHNICAL REPORT PERFLUORO OCTANOIC ACID CONCENTRATION (C8) IN BASTE STATER J. C. Moore REPORT (JBITTEN BY: TORK SUPERVISED BY; PREVIOUS RELATED REPORTSi 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 (Conaunity Exposure Guideline) of 1 ppb in water for aflimoniuin 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 FAX;1-804-383-3785 PAGE 5 i n . S T T - 9 1 - 1 TABLE OF CONTENTS 1. INTRODUCTION 1-4 2. DISCUSSION 1-4 A. EARLIER ISSUES B. TEFLON* DISPERSIONS C. PREVIOUS CONCERNS D. PRESENT ENVIRONMENTAL CONCERNS 3. REFERENCES 5 , 4. TABLES o JCM-l THE EFFECT OF HEAT ON EXTRACTABILITY OF C8 FROM YARN 6 5. FIGURES 1. MASS BALANCE OF C8 IN TEFLON* SPINNING 7 1. MASS BALANCE OF C8 IN SPKUANCE ffASTE SATER SYSTEM 8 3. PROPOSED MASS BALANCE OF C8 It TEFLON* SPINNING 9 4. PROPOSED MASS BALANCE AROUND STASTE WATER SYSTEH 10 6. APPENDIX I. II. III, SPRUANCE C8 ASSESSMENT SPRUANCE C8 ANALYSIS ANALYTICAL DATA FOR LliG LABORATORY NO. 20152 11 12 13-28 05/-09 '02 13:52 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 6 STT-91-1 1. 1. INTRODUCTION Teflon* colloidal dispersion is mixed with viscose in the manufactute of Teflon* fiber. The cellulose contained In che viscose is regenerated i-n die 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 surfactaots used is F-143, ammonium perfluoro octanoate (commonly referred to as C8), 2. DISCUSSION A. EARLIER ISSUES In 1978, the 3H 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) vere 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 (Ret. 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 3M and DuPont's Haskell Labs. B. TEFLON* DISPERSION Teflon* dispersion is produced in a batch operation at Washington fforks. 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 Ibs which contains 3000 Ibs of Teflon* monomer. A total of 4060 grams of C8 i6 added to the batch i.n the precharge and injection seeps. After polymerization is completed, the dispersion is decanted to obtain 60X solids- Washington Works estimates that 50X of the C8 is removed with the decanted superannuate and the other 502 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 Sipinning, the C8 will convert to the acid forai, perfluoro octanoic acid. 05/09 '02 13:52 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 7 $TT-91-1, 2. 2. DISCUSSION CONT'D C, PREVIOUS CONCERNS Previous research exawined employee potential exposure to C8 through handling of yarn. Sintered Teflon* yarn had non-detectable levels of C8 (Kef. 4). The Teflon* fiber sintering temperature is 325 C. The boiling point of perfluoro octanoic acid is 188 C. Yarns vith a Teflon* coating, which are not exposed to high temperatures did contain detectable levels of C8. Therwal treatment of these yarns was effective in removing the C8. The research shoved that the C8 removal was a function of time and temperature (Table l),(8ef. 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 niot 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 ENVIRQlNmiENTAL CONCERNS The present environmental concerns vith C8 are with ground water contamination. A CEG(Conununity Exposure Guidelines) of 1 ppb in water has been established by Haskell Labs. II.Samples of effluent from different spots in the Teflon* spin-ning 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 CH2H Hill is contained in Appendix The sample results do not allow for a complete mass balance. The measured concentrations in the effluent streams only accounts for about 50X of the C8,(Fig. 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 Sprvanee 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 uith 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 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 8 STT-91-1 3. 2. DISCUSSION CONT^ D. PRESENT EMVIRQNHfiMTAL CONCERNS CQNTID Previous work measured C8 on unsinterred Teflon* yarn at 60 ppm (Ref. 4). The concentration would need to be 700 ppaa to account for the Missing C8. The previous work concluded that the C8 carried with the unsinterred Teflon* yarn vould decompose during the sinterring process. This is in contradiction to ffashingcon Works process of recovering C8 from their "fine powder'1 exhaust stream. "Fine powder" Teflon* has been tested and found to contain little or no C8- The "fine powders1' are dried at 190 C. Bashington Works recovery of C8 froni 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, vater is sprayed in the exhaust hood to reduce the temperature down belou 65 C. The exhaust gas then passes through a vet scrubber and the final gas temperature is basically reduced to ambient conditions. The vater 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 CH2M Hill's lab. The exhaust scrubber effluent VAS analyzed to have 1.8 ppb of C8, and the detection of known amounts of surrogate material added was leas than 50Z. The explanation for the low surrogate recovery was 'due to the noise created by a large non-target chroniatographic peak coupled vith 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 vater samples ran from 52X to 86X. 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 lou by a factor of "2X would tie together the majority of the material. The 60 ppn measured concentration of C8 on the yarn only accounts for "5X of the total material. The other 95X exits the process in the yet portion of the spinning process, the washing step since the acid bath is 100% recycled. The 5X 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 leas than 0.02% of the total amount. 05^09 '02 13:53 ID:DUPONT ENV AFFAIRS FAK:1-804-383-3785 PAGE 9 STT-91-1 4. 2. DISCUSSION COtfTP 0. PRESENT ENVIRONMENTAL CONCERNS CONTD If 95X of the C8 exits the process vith the vash water, the concentration of Stt #2 sample should have been 4600 ppb. CH2H Hill's measured amount of 2400 ppb is 52X of that level. This percentage is in the range of report surrogate recoveries on distilled water* The nose conservative position in estimating the potential environmental Impact is to assume that all of the C8 ends up in the plant's uaste 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 Janes River is 5104 KHgpd- This would make the C8 concentration in the James River an estimated 0.06 ppb, The average annual prodluct;on rate for Teflon* fibers is I MM Ib. This would discharge 1490 Ib. of C8 to the James River annually* The estimated C8 concentration in the river would be 0.10 ppb. The maximum production rate for Teflon^ fibers is 4200 Ib./day. This could add 6.3 Ibs CS/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 HWgpd. 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 1.84 ppb. During the low flow periods, which should happen once every 10 years, production may need to be curtailed to 2300 Ib./day of Teflon* fiber to stay below the CECr of 1 ppb. 05/09 '02 13:53 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 10 STT-91-1 REFERENCES 1. Forte, H.A. - SpAB. 79-3 2. Forte, M.A., Hokhtar, A.H. - PCD Honthly. June, 1981 3. Shelburne, S.S. - PCD Monthly, December, 1981 4. Shelburne, S.S., Forte, H.A., Hokhtar, A-H. - SpAS 82-1 5. Burks, P.P., - TR 62-1 05/-09 '02 13:53 ID:DUPONT ENV AFFAIRS FAK: 1-804-383-3785 STT-91-1 TABLE 1 THE EFFECT OF HEAT ON EXTRACTABILITY OF C8 PBOM YARM (Ref. 2) Initial C8 concentration 011 9450 I & T yarn ~ 600 ppm X C8 BemaAning on Yarn Time of Heat (minutes) 150 C 175 C 200 C 10 75 41 H/D 20 72 12 N/D 30 72 M/D N/D 40 47 N/D N/D N/D Not detectable, < 5 ppm Least Square Fit for proposed 1st Order Decarboxylatlon 150*0 A - Ao * e'0-01256 (t-ainutea) 175BC A - A^ * e'0-^066 +10-C -> (0.106/0.0155) 0-1 - 2.16 (close to "rule of thuflib" for temperature dependency of kinetic reactions, +10''C roughly doubles reaction race) Extrapolation to 200"C using a power of 2.16 per lO-C @200'C A - Ao * e -o."St t - 10 min, Ao n 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 STT-91-1 FIGURE 1 MASS BALANCE OF C8 USING CHgflHILL TEST RESULTS TEFLON* SPINNING NOVEMBER 13 1991 ^ ^ 1a ^ '' S A -j: T rili-d^lVl^ "" -------- a e "fc? u ^ -is Aif1& 8 w 5 -i s- f """^ I ^ " \ ?^1?^11 i1 ^r- ^ fe i5 ^ Pt ^1 \ a fi 1^ ^A 1 Q ? i ? ^fl? tf 13 ^ ^ 4'n &L u- -5^ 3?3fl r - WiStff/ -aQUyf ^ > v-ttyfl.t-p - ^cK^y, e? (ya"? yit. ^ ^0- -y^Kf/U ^ysh ^ ^ ^r 0 ^.a ^ n S S ' ^N- -;?-.,?- 0 0 ?[ u u ^x a(q a o 3te3 , ' " n ti -^cvy'' fr --ij-- ^.9m'v-<fMyt ^) t*stfy W ' '3 9 * vt 6 o ^ ^ - - J a i p &'a^yt <* ^ f> C t . } i ^ y^ y - iQ m ^1 \ ^1. ? ? sh1*??3 S1 ^ ^ i. : , ^ 1 ? 8 P rt i -j J " ^ '<) <4 , l B a w < in 05/09 '02 13:53 ID:DUPONT ENV AFFAIRS - FAX:1-804-383-3785 STT-91-1 FIGURE 2 MASS BALANCE OF C8 USING CHgMHILL TEST RESULTS SPRUANCE WASTE'-HATER'TREAWENTSYSTEM NOVEMBER 13, 1991 'ptAt^r s&i-'eas '-EOlMS^' Aian ereeN^ vzaoym. &<.<.<u..yrt>en-t^^,,... . - 0^ pot: o.4a'-' loo/ o.'&'a * Q ' QO'2, o.afe" n"?/'o,63 = 50. i>y. 4-3.4% Av'tSttA&riE F^t>^> .3.S4 UM. yrn. Emeo ipM (iHirt Uit., -tesuija e-'T'MA.ii. Foit.-(7iVft '" o.o'anpfc 05/09 '02 13:53 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 STT-91-1 FIGURE 3 PROPOSED MASS BALANCE OF C8 IN TEFLON* SPINNING NOVEMBER 13, 1991 05/09 '02 13:54 ID:DUPONT ENV AFFAIRS FAX: 1-804-383-3785 STT-91-1 FIGURE 4 v PROPOSED MASS BALANCE AROUND WASTE WATER SYSTEM NOVEMBER 13, 1991 "^.-i-w aeuXK; A^cii-j^^c: F"-i=.x-> J,B4!AHi^pm, 4'=i.C><o opb 05/09 '02 13:54 ID:DUPONT ENV AFFAIRS FAX: 1-804-383-3785 PAGE 16 STT-9I-1 11. APPENDIX I SFRUANCE C8 ASSESSMENT E. I. DU FONT DE MEMOUB5 & CO., INC. Fibers Business Cc: G. L. Kennedy - Haskell G. A. Hapka - Legal R. A. Reich- Eiigt, -- Louviera J. D. Chidlfsy R. L. ;;.ji'sn , C. P. Mihail R. C. Xeatta D. M. Schwartz G. H. Sisson J. S. Tschrifcfcec SPRUANCE FIBERS PLANT Hichroond, Virginia December 4, 1991 TOs i^d. C. MOORE - TEEWN TECHNICAL FROM; T. V. BOBERTSON - E3WTBCNMEMTAL AFFAIRS SPBUftNOB C8 ASSESSMENT As 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 wastewatec treatment system for ainnioniu pecfluocooctanate (ca). The results are contained in the attached table. C8 is used as a dispersant to make PTFE at Parkersburg. IP'trB is used at Spruance to make Teflon*" fiber. CS is an impurity in PTFE and thus, is introduced into the process at Spcuance. The sampling scheme employed evaluated the C8 content at the wash water discharge in the spinning operation, in the air emissions control scrubbec effluent, in the area process sever, in the site composite process sewer (inlet to waste-water treatment system), and at the discharge o the MWTS which combines with the non-contact streams discharging to the James River. C8 content in these samples appear in line with your eacliec estimates, Assuming Outfall 002 flow of 10 MMGD, a total site effluent of 14.4 MMGD (winter time), and a James River low flow 7Q10 of 408 WGD, a civer concentration of 0.4 ppb is calculated as a worst case. I would appreciate your comments on these sample results. TVRsmcp 29:1.30 05/09 '02 13:54 ID:DUPONT ENV AFFAIRS FAH:1-804-383-3785 PAGE 17 STT-91-1 SAMPLE NO. 12, APPENDIX II SPRUANCB C8 ASSESSMENT SPRUANCE C8 ANALYSIS SAMPLE TYPE Composite* UXATIOM SM#2 wash Water Discharge C8 CONC. {p^A^ 2400 Composite* ScnAbec Effluent 1.8 Discharge 24 Hour Composite East Trench (Process 950 Sewer) 24 Hour Composite influent to MWTS 22 (Outfall 006) 24 Hour Composite Effluent from MWTS 18 (Outfall 002) Blank-Dl Water <MDL * 4 grab's collected over 8 hours and combined as one sample. MDL - detection limit 0.1 pq/^ 29:1.30 05/09 '02 13:54 ID;DUPO!MT ENV AFFAIRS FAX:1-804-383-3785 PAGE 18 STT-91-1 13. APPENDIX III ANALYTICAL DATA FOR LHG LABORATORY NO. 20152 Koveniber 2"?. t' U1G27317.XY Mr. Toia Robert son El DuPont de Neincmra & Co, Inc. Spruance Plant - East Office Bidg. P.O. Box 27001, Jesfferaon Davia Hwy, niCthmood, Virginia. 23261 RE; Analytical Data for me l,&boKatory No. 20l$2 Dear Hr. Robert son: On November 13, l^'Sl, the CH2M HILt. Hontgomary Laboratory received six Baaiplea with 9. request foe analysis of salectad organic parameters- The analytical, results and associated quality control data are enclosed. Any unusual difficulties encounteiced duci.o.g the analysts o these samples aea diacuaaed in the case narrative. If you should have any questi-ona concerning the data, please inquire, The CH2M HILL policy ia to store samples foe- up to 30 daya after reporting. 1C you desire, our laboratory will maintain your samples for a longer period at a coat of $S.OO per aampla par month- Samples detBrminad to be hazardous can either be returned to you or disposed o at a cost of $25.00 per aampla. Sincerely, ^OA^-C^-^^ Wanda L. Hall Data Package Supervisor Enclosures CHSMHIll. Quality At'l^h/fir-atf 'a^.-* ?567FaitianeDwe,PO flo<^30S-fl -'05??! 'M" 05/09 '02 13:54 ID:DUPONT ENV AFFAIRS , FAX:1-804-383-3785 PAGE 19 STT-91-1 14. APPENDIX III ANALYTICAL DATA FOR LUG LABORATORY NO. 20152 TABLE OF COtITKMTS CH2?'. riTLr. Laboratory No- 201S2 page No. Liat of Organic Analytical. Mathoda ,.,,..,,,...,........................, i List of Organic SPA-defined Qualifiers ........<.........-..------..-.... ii List at Organic Sample ID- Qualifiers ................................4. iii ,111|> Sawple Cross-Refecence .....-...-...-....-.-......,.....,.....-.--..-- iv 'Ijlljl FC-143 DAWA AcanoaelyNttacraral tRiveesu.lt.s..o.f..E.-.l.a.ld..S.a.m..p.le.s............................... 1-2 NUMBER 1 HfltMBER 2 (r^G (LHG #20152001) #20152002) ............................. 3 4 NUMBER 3 (LMG 120152003) ............................. 5 KUHBER 4 (LHO 120152004) .......................................................... 6 NOHBER 5 NUMBER 6 (LMQ (LMG (2Q.152Q05) (20152006) ............................. 7 8 Quality Control Data ............................. Reaults off QC Blanfc (W113HB1) ......................... 9 / C^(/^ 1'4-S.A ' (S ^0%?_ \S' ^ Copy of Chain-of-custody .......,....,......,.....,,,.,...,,..----.-.--- 10 05/"09 '02 13:54 ID:DUPONT ENV AFFAIRS .FAX:1-804-383-3785 PAGE 20 STT-91-1 15. APPENDIX III ANALYTICAL DATA FOR LMG LABORATOBY NO. 20152 AHM.XTICBX. METHODS Organic Analysis Priority Pollutants; Water, eoil and waste naffiple; are analyzed in accordance with procedurea daacribad in Methods 60B, 624, and 625, EPA-600/4-82-057 <19B2),? Methods 8080, 8240, and 8270, Teat Methoda for Evaluating Solid Waafce, 1986, SW-846, Third Edition; and methods outlined in the USEPA Contract laboratory Program Statement of Hock for Organics Analysi-a, Pebi^iary, 19B8. Volatile Analyata (safe Drinking Waiter Aet)i Water samplea are analyaed i-n accordance with pcoceduraa daacriJbed in Method 524.2, Federal Register (SO F& 46902). Hovembaf 3,3. 198S. Chlorinated Phenoxyacid HecbLcidea: Samplea are analyzed i-n aecordanca wi-th procedurea described in Method 8150, T6Bt Methodls for Evaluating Solid Waste, 1986, SH-846, Third Edition. organophosptioroua Pesti-cideas Samples are analyzed in accordance with procedures described in Methods 614 and 622, EP^-600/4- 79-019 (1979) and in Method 8140, Test Hathoda for Evaluating solid Waste, 1986, sw-a46, Thju-d Edition. Phenolic Acid ftnalyai.8 by GC; aampiea are analysed in accordajica with proceduraa deacribad in Method 604, Federal Ragistar, 40 CFR, Part 136 (July 1, 1987} and in Method 8040, Teat Methods foe Evaluating Solid Waste, l9e'6 SW-846, Third Edition. Polynucl&ar Aromatic Hydrocarbons (GC analyeifl): Samples are analyzed in accordance with pfoeedurea deacri-bed in Method 610, Federal Register, 40 OFR, Part 136 (July 1, 1987) and in Method 8100, Teat Methods for Evaluating Solid Waste, 1986, SW-846, Third Edition. Ebhylane Dibromide; Water samples are analyzed in accordance with procedures described in Method 504, Federal Register, (50 FR 46902), November 13, 1985. Trihaloine-thaneB; Water samples are analyzed in accordance with procedurea dMeosvecrroibbeerd 2$in, M19e7th9o. d 501,2, Federal Register, Vol., 44, No. 231, Part II, 05/09 '02 13:56 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE STT-91-l 16. APPENDIX III ANALYTICAL DATA FOB LMG LABORATORY NO. 20152 EPA - OePlHED QU&LIFIERa onnftNics Defi.niti.0na for Che EPA-defined quaUfiers; U "" Indicates the compound was analyzed for bufc not decocted,. The nmnber adjacent to the "U" qualifier indicates the quantitation limit for that compound. The detection limit can vary from aaropla too eartple depending on dilution factors or peccant moisture adjustment when indicated. J indicated an estimated value. This flag ia imed when the ma,aa spectral data indicates the presence of a compound below the stated quantitation limit. The J- qualifier ia not MQS with pesticide reaulta- C Thia flag applieis to. pesticide results only. The "C" flag indicates the presence of ttlia compound haa been confirmed by GC/MS analysis. This flag ia uoad when tha analyts ia found in the associated blank aa well as tha sample. This notation indicates possible blank, contaqiJInAtion and suggests the data uaar evaluate thasa conrpoundg and thair amounts careful Ly. E This flag applies to GC/HS only. Tha "E'' qualifier indicatea a compound may be above or below the linear ica.nge of the instrument* Xf the particular compound lava! is deemed above the lineal: calibration ranga, then tha sample should be reanalyzed at. an appropriate dilution. Tharefoce, tha "E" qualified amount is an estimated concentration. The results ror tha dilution will ba reported on a separate Foi-m I and will be flagged with a "D" if tha dilution brings the concentration within proper calibration. Thig flag identifies compounds which have been run at a dilution teo bring the concentration of that compound within the linear range of the instrument. "D" qualifiers are only used for samples that have bean run initially with results above acceptable ranges. For secondary dilutions the -OL" suffix, i-s appended to the sample number on the Foicm I. A indicates the Tentatively Identified Compound (TIC) ig a auflpee-ted aldol.-condenBafci.on product. Indicates the compound concentration has been manually modifiad 01the EPA qualifier has been manually (nodi-fied or added. JX The coinpuund was detected and quatititated below the Contract Required Quantitation (.trait. ii OS/Oa '02 13:57 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE STT-91-1 17, APPENDIX III ANALYTICAL DATA FOR LMG LABORATORY NO. 20152 CLIENT SAMPLB ID OOM..IPIERS LEVEL 1 The qualifiers that GC/HS and GC we with the client sample ID aca defj.ned below; DI^ -- R -- RD -- BX -- MS -- MSD QC BIANK Di-lution Run Rei^m (ittay be followed by a digit to indicate multiple reruns) DUutad Rerun Re-extraction Analyai.9 Matcix Spike (may be followad by a. digit to indicate multiple matrix apihaa within a sample got) Matrix Spika Duplicate (may ba followed, by a dig4.t. to i-ndi-cata multiple matrix spike duplicates within, a sample set) Method Blank (may be followod by a "W" for waters, "s" (01: BOila runi at a law l<evei, oc "SM" fias- soils run at a medium lavel -- ttwss lettarB may ba (oUoMBd by a digit to Indicate multipla blanks of that typa; if there are no lattars, the di^lit indicafcaa caultipla blanks). Thesa qnaliti.&rB allow GC/HS and GC to have uniqua cUent eainple ID'S go that the client can. get more accurate Information from tha data cepoctfed. 05/-09 '02 13:57 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 4 STT'91-l APPENDIX III ANALYTICAL DATA FOR LMG LABORATORY HO- 20152 CB2M HIU. SanHile KTO. 201.53001 20152002 20152003 20152004 20152005 20152006 TABLE 1 SAHPLB CROSS-REFBREMCB SUMMARY CH2M HIIA Laboratory Ho- 20152 S!SlS DttBOriDtl-on NUMBER 1 NUMBER a MrmaER 3 NUMBER 4 wtmaaR 5 NUMBER 6 11/14/91 11/14/91 11/14/91 11/14/91 11/14/91 11/14/91 0830 0830 0830 0830 0830 0830 COMP COMP COMP COMP COHP GRAB OS^OS '02 13:57 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 5 STT-91-1 19. APPENDIX HI ANALYTICAL DATA FOR LHG LABORATORY NO. 20152 CASE NARRATIVE FOR rc-lA3 GAS CHROMATOGRAPHY SAMPLES LABORATORY; CASE: NO. ; LAB NO. ; CH2M HILL LABORATORIES K/A 20152 CLIENT; CONTRACT NO.; SDG NO.i E. I. DUPONT R/A H/A I. RBCEXPT A. OATEt November 15, 1991 H. SAMPLE IM-ORMATION LAB ID 201S2001 20152002 20152003 20152004 30152005 20152006 W1121181 CLIENT ID NUMBER 1 NUMBER 2 NOMBeR 3 NUMBER 4 MOWER 5 NUMBER 6 QC BIANK SAMPLE MATRIX WATER WATER HATER WATER WATER WATBR WATSn DATE SAMPLED EXTRACTION DATE ANALYSIS DATE 11/14/91 11/14/91 11/14/91 11/14/&1 11/14/91 11/14/91 NX 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 11/23/91 11/22/&1 11/22/91 C. Documentation Eicceptiona ; Mo exceptiona were enicounfcecBd. 05/-09 '02 13:57 ID:DUPONT ENV AFFAIRS ,FAK:1-804-383-3785 PAGE 6 STT-91-1 20. APPENDIX III ANALYTICAL DATA FOR LUG LABORATORY NO, 20152 PC-14,3 LAB NO. PAGE 2 20152 II. III. IV. ErrtlACTION A. Holding timesi B. Ex1.facti.on Exceptions ANALYStS A. Holding tuneas B. Analytical Exceptions ; QUALITY CONTROL A. Method Blank ; B. $urrogata Recoveries c. Matrix Spika Results i All holding timea waro met. The native pH of two Bamplea were unusually extreme for environmental aainplea. rha nafciva pB ot 20152001 (NOHBER i) was 3 and the native pH of 20152003 (NUMBER 3) waa 12. Ho other exceptions were encountered. All holding times were meit. Sample 20152002 (NUMBER 2) was diluted by a larga factor dua to intoerfersncaa not reaioved by oui: cleanup proceduraa. No other exceptions were encountered- AlX associatedl method blanks awh acceptaUale QC criteria. Surrogate recoivwciea were not determined for four fiald aaaiplea dua to larga dilutions required far analysis. Surrogate r&coveriea were below S0 for sampla 2Q1S2002 (NUMBER 2). acceptable QC limits. All other BMiplaa mat Matrix apika reaulta have not ben reported with thia contract. I certify that this data package is in compliance with the tenna and conditiona of the contract, both technically and for completeness, for othar than the condition* dt^ta i \v^ above. Reluaa** of tha data contained in thia hardcopy data package haa been authorized by the Laboratory Manager or hia deaginea, aa verified by the following flignaturB. ///^7/4/ 05/09 '02 13:57 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 7 STT-91-1 21. APPENDIX III ANALYTICAL DATA FOR LMG LABORATORY NO. 20152 ORGANICS ANALYSIS DATA SHEET Laboratory Names Lpb Sample ID; Client sample ID: CH2H HTLL/MGM 2Q152001_____ NUMBER 1_____ Concentration! Sample Mdr.n?;: Percent Moisture; FC-143 LOW M^TS"- ____ Date Extracted; Date Analyzeo; Diluti-on l-'-actor; 11/21/91 11/22/91 2500 e&S..M_uinbeg____________ _____,, 3825-26-1 FC-.L43 ........ Partluoronoiianoic acid - SS Perfluorodecanoic acid - SS llH-EicoBafluocoundeca.nol.c acid - _.MC[/I; 2400 Nil Ko SS ND CAS Number____________________ug/I. 0 - Analyzed for but not. detected. JX - Praaftnt;< concaot-cattion estimated- 3 - Detacted in QC blank. as - Surrogaite Standard reportad g percent recovery. MD - Mot datiBrroined. Cortinenteas Surrogat, icecoveriaa were pen; detennined due to tha larga dilution -squired toi? analyeia. Form 1 0^ 05/09'02 13:57 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 8 STT-91-li . 22. APPENDIX III ANALYTICAL DATA FOR LMG LABORATORY NO. 20152 ORGANICS ANALYSIS DATA SHEET Laboratory Name; Lab samule ID; Client, sample ID; CH2M_HII.L/HQH 20152002 NUMBER ____ }._____ Concentrations Sample Matrix: Percent Moisture; LOW. WATER. __ B-C-143 Date Extracted; 11/21791 Satti AnAlys-.ed; 11/.32/91. Dilution Factor: _____10 CRS Nunibef______ug/L 3825-26-1 T^ PC-1-43 ......... 1.8 PerfluorononanQic aci-d - ss <SO PartlitOE'orilecanoi.c acid - ss <50 la-H-Eiicosatluocoundecaaioic acid - SS <SO CftS Number | U - Analyzad for but not detected- JX ~ Present;, Goncentration estimated. B - Det-actiad JLiB QC blank. SS - Surrogate Standard reported as parcant recovery. C'C-oharroosanttaa;togTrahips hpaieacaaikpala dwiaacsovdeilruetdedwhfaonethaanaelayreoipalebwecaasussBcreoef neladr.geSnuorirno--gtaatceget icovariea could not; b defceAined Accuxrately bocauaa of ehroitta-tographic noise coupled with a larga dilution factor. uq/L Fona I 0^ 05/09 '02 13:58 ID:DUPOIMT ENV AFFAIRS .FAX: 1-804-383-3785 PAGE 9 STT-91-1 24. nf APPENDIX III ANALYTICAL DATA TOR LMG LABORATORY NO. 20152 ORGAM1CS ANALYSIS DATA SHEET Laboratory NAnie; r.ab Sample ID: Client Sample ID; CH2M HILL/MGM 20152004_____ NUMBER 4_____ Concentration; Sample Matrix? pereenc Hoifltus-s; FC-143 LOW WArjR_ _____ Date fiKtractedt 11/21/91 Date Analyzed; U/Sg/0! Dilutiort Factor; _____20 CAS Number_____________________uq/L 3825-26-1 FC-143 ......... 22 PeE'fl.uorononanol.c acid - SS HD Perluoro4eeanoi.<i acid - S3 ND lia-EicoBitflMoroundecanoic acid - ss KD CM Kumber _"aZ& IjSSIII. ^ss^ vl ~ jx - a - . ss - ND -- Analysied foe but not detected. Present, concaotir&tion estimatad. Detected in QC hiank. Sucrogatee Standard reported as percent Hot; determined. recovery. CoiBmenta; Surrogate racovwieB were niot; detexmined due to teha larga dilution "squired for analysis. Form I 0^ 05/09 '02 13:58 ID:DUPO!MT ENV AFFAIRS FAX:1-804-383-3785 PAGE 10 STT-91-1 25. APPENDIX III ANALYTICAL DATA FOR LMG LABORATORY NO. 20152 ORGRMICS ANALYSIS DATA SHBET i-aboratory KaraiQs Lab Sample ID; Client Sample ID; CH2M HILL/HGM 2015200S NUMBER S Concentration; I.OW Sample Matrix; HftTEB Percent Moisture; Data extracted; 11/22/91, Date Analyzed; 11-Z.22/0'. Dilution Factort 20 E'0-143 CAS Huniber 3825-26-1 PC- 143 uo'/I. . < l6 Perfluorononanoi.c: aci-d ~ ss HO Perfluorodacanoic acid - SS ND llH-EttSoeafluoroundecanoic acid - SS MD CAS Mumibar . ^ua^l. ' U - Analysed foai- but not <iatact.ad. jx - PrBsante, concanitrateioit aBttmafeBd. . B - Datacteca in QC blank. SS - Suri-ogata s'handard reported aa pal-cent. rcovary. MD - Not: datBminad- Comman-fcB; Surrogate cacoveries wars aot datarmi-nad dua to tha laxgB dilution '"equl.red fOjC analyBis. Ponn I o^ 05/09 '0213:58 ID:DUPONT ENV AFFAIRS FAX; 1-804-383-3785 PAGE 11 STT-91-1 26. APPENDIX III ANALYTICAL DATA FOR LHG LABORATORY NO. 20152 ORGAN1CS ANALYSIS DATA SHEST X-aboicatory Nanies Lab Sample IS; Client Sample ID; CH2M HIJLLi/MgH 2Q152006_____ NUMBBR &_____ Coniserttraticins Sampl-e Matri-x; Percent Moisture; FC-143 LOW WRTER.. _____ Data Extracted! Date Analysed; 11/21/91 11/22/')! Dilution Factot-i ____1.0 CRS Mumbel-___________^_____^_____uq/I. 382S-26-1 . FC-143 ......... rarfluoconoinaooi.c acid - SS O.l.u 86 t .B'ertlnocotlecanoic acid - ss 75 t llH-Eicosafluonound&canoi-c acid - SS 83 ^Illy CRS Humbel 0 - Analyzed for bufc not datacted- JX - PrBBant, Gamsntrat:ion eattaaitad. B - Datacrfcad in QC blank. SS - Surrogate Standard reported ae parcante recovary. ccnmaents; "q/L POCTB I r\^/u^ 05/09 '02 13:58 ID:DUPONT ENV AFFAIRS FAX:1-804-383-3785 PAGE 12 STT-n-l 27. APPENDIX III ANALYTICAL DATA-yOR UIG LABORATORY NO. 20152 '^^ ORGANICS ANALYSIS DATA. SHEET t-alaoratory Name; Lab Sanipis ID; Clieni; Sample ID; CH2M HILL/MGM W11211B1_____ QC B^AJJK____^. Concentration: Saniple Matrix; Percent Moisture; LOW.. WATER __. PC-143 O&ta Extraoted; Date Analysed; Dilutiort Factor! 11/23/91 11/.'>2/91 ____1,0 C&s Numbeg 3Q2S-26-1 FC-143 \ uq/X. CftS Number- 0.1 U PerfluorononiinoiC acid - SS 81 Perfluaz-odacanolc add -- SS 52 % HH-EicoBafluoi-oundecaa-ioic acid - SS 53 *. ua/L n - Analyzed for but not detected. J3t. - P^aaant:, conca'ntration eBtunated. B - Detect-ad in Qft blank. SS - Suxcogate Standard reported aa percent recovery. Ccinuaents; PoriB I ^