Document 5L89y2vVN8kjEjo28zX40grmV

J Monsanto i _ SJEH/ESC --(Cb.7B1v./Dept .Tloca t foil) or ?<0 /> V 31 s 2 8tA> 3 vi 1/1 /i I 2 REPORT NO.: MSI-5738 ESC-UAG-86-46 J08/PR0JECT NO.: 6405 OATE: May 30, 1986 TITLE: ANALYSIS OF LULING SAMPLES AUTHORS: S. Gibson, S. Walker and R.W. Noble ABSTRACT: Sanples fro* lullng were received for the analysis of PCDOs, PCOFs, 2,3,7,8-TCDO, *etals, acid and base/ neutral extractables, pesticides and Aroclor forwlatlons. This report gives the results of these analyses. TECHNICAL APPROVAL: Environmental Sciences Center Senior Research Group Leader APPROVED BY: Environmental Sciences Center Quality Assurance Specialist APPROVAL OATE: ___ ii I MOMS 024035 COMPANY CONFIDENTIAL This document is the property of Monsanto Company and the recipient is responsible for its safekeeping and disposition. It contains CONFIDENTIAL INFORMATION which must not be reproduced, revealed to unauthorised persons or sent outside the Company without proper authorisation. DIST RIOUT IOM COPY NUMBER 1. 1. Adams - 1560 7. S.O. Gibson - U4F 3. *S.A. Walker - Ulf 4. R.W. Noble U1F 5. W.M. Nets - U4D 6. P.L. Sherman - U1F 7-9 Reports Library - R2C 10. Chesterfield Information Center - AA3A ABSTRACT ONLY H.A. Woltermann U4E COMPANY CONFIDENTIAL This report has been assigned to you. When it is no longer needed, yop ere responsible for reluming it to: H you transfer it to enyone else, pteese let your librarian know, so the records can be changed. HONS 024036 ANALYSIS REPORT BATE; 2? May 1996 ..... LOG NUMBER: U-86-03-14-01 _____ ....... PROJECT NUMBER: 6403 NOTEBOOK PAGE: 3353290 10:. L. Adams/ 156.0 . cc FXLES/Kees P. Sherman R. Noble Title: Analysis of Luling Samples Procedural see attached report Abstracti Sample* from Luling were received for the analysis of PCDDs, PCOPs, 2,3,7,8-TCDD, metals, acid and base/neutral axtractables, pesticides and Aroclor formulations. This report gives the results of these analyses. Analysts! S. Gibson, S. Walker and R. w. Noble ANALYST APPROVAL: RoyJ. Noble Senior Research Chemist l HONS 026037 ANALYSIS REPORT FOR LULING SAMPLES INTRODUCTION Nine soils, two sedinents and four wipe samples were received for selected analyses of polychlorinated dibenzo-p-dioxlne (PCDDs), polychlorinated dibenzofurans (PCDFs), 2,3,7,8-tetrachloro dlbenzo-p-dloxin (2,3,7,8-TCDD), selected aetals, acid and base/neutral axtractables, pesticides and Aroclor formulations. The aetals, acid and base/neutral axtractables, pesticides and Aroclor foraulation analyses on saaples #57 and #5 were performed by Environmental Testing and Certification Corporation (ETC) of Edison, NJ. The PCDD, PCDF and 2,3,7,8-TCDD analyses were performed in our laboratories. For Internal purposes the saaples were assigned Log number U-86-03-14-01. For quality assurance in the analyses we performed MRC Method <07-QAQC-R3 was followed. Briefly this method requires that for every set of saaples of the sane matrix type a replicate sample, a low spiked sample, a high spiked sample and a method blank must be analyzed. The reports for the analyses performed by ETC are attached at the end of this report. PREPARATION AND ANALYSIS Soil and sediaent samples of 10 g were weighed and spiked with appropriate internal standards. Wipes were spiked with carbon-13 labeled 2,3,7,8-TCDD prior to extraction. Then 15 aL of methanol (all solvents are Burdick and Jackson "distilled in glass* grade) and 150 aL of hexane are added. The samples are then shaken for 3 hours on a wrist action shaker and the hexane is decanted off. The hexane extracts were vashed with 40 aL of concentrated sulfuric acid (untill clter), :o aL of water and 43 aL of 1 n potassium hydroxide and 30 aL of water. The hexane was dried over sodium sulfate and concentrated to 3 aL. The samples were then placed on the head of a mixed phase liquid chromatographic column consisting of (top to bottoa) 2 g of silica, 4 g of silica plus 40t sulfuric acid, 1 g of silica, 2 g of silica plus 36% potassium hydroxide and 1 g of silica. The column was eluted with 50 aL of hexane which was subsequently concentrated to 3 aL. The hexane was then placed on the head of a column containing 2.5 g of Woelm basic alumina. This column was first eluted with 10 aL of 2% methylene chloride/hexane (v/v) mixture and this fraction discarded. An additional elution was made with 15 aL of a 50% methylene chloride/hexane (v/v) aixture to elute the PCDDs and PCDFs from the column. For soae of the saaples it was necessary to conduct further cleanup using the EPA Option D technique in order to analyze for TCDDs. Option D involves placing the sample on top of a column containing 18% Carbopak C on Celite packed to a depth of 2 cm in 2 MONS 026038 a 1.0 cm ID plpat. Tha column was than eluted with 1 mL of haxana, 1 mL of 1:1 cyclohexane/methylene chloride, 1 at, of 75:20:5 aathylana chloride/methanol/benzene and finally 2 mL of toluana. Tha toluana fraction vas collected to be concentrated. All saaplea had 50 ul> of dodecane containing tribroaobiphenyl as an Internal standard added to the eluant as a keeper and were then concentrated to 50 uL under a gentle streaa of purified nitrogen and were submitted for GC/MS analysis. Tha GC/HS analysis was conducted on a Hawlatt/Packard 5987 Instrument. The aass spectrometer was operated in the selected Ion monitoring mode analyzing for ions characteristic of the native (unlabeled) PCDOs, PCDFs and the internal standards. RESULTS The results of the analyses are given in Tables 1-5. Results are not corrected for recovery for the PCDD and PCDF analyses in Tables 1 and 3. Replicate analysis results for sample t 5 show a large variability due to the presence of shells in the sample causing homogeneity problems. Discussion with tha customer determined that these results met their needs. HOMS 029039 3 Table 1. PCDD RESULTS FOR SOIL AND SEDIMENT (in ppb) Sample Background Cl-4 ND Cl-5 ND Cl-6 ND Cl-7 0.4 1-8 1.2 Soil 15 600 0.7 3.3 1.5 3.1 Soil #5 R Soil 1) Soil |27 7500 0.9 2.1 ND ND ND 2.2 5.3 8.9 3.6 30 190 ND 0.4 1.5 Soil (35 0.7 ND 0.7 1.5 21 Soil (39 0.8 ND 0.8 1.6 18 Soil (51 ND ND 0.4 0.6 1.5 Soil (51 H % recovery pike level 10.1 107% 9.4 19.1 170% 11.4 11.6 103% 10.9 11.3 91% 11.8 11.9 109% 9.5 Soil (57 5.2 ND 1.4 0.8 1.4 Soil (59 4.8 ND 4.0 ND 0.2 Sediment 11 ND ND 3.0 38 160 Sedlsent (1 L 1.1 1 recovery not 1.2 100% 3.5 -a 29 104 -a a spike level 1.0 1.2 1.1 1.2 1.0 Sediment (2 BLANK 18 ND 0.3 8.0 89 420 ND ND ND ND MDL 0.5 0.5 0.5 0.5 0.5 MDL method detection limit ND none detected at method detection limit R replicate sample L,K low and high spiked samples a pika recovery can not be calculated as sample is three times the spike level. MQNS 024040 4 Tab!* 2. REPEATED PCDD RESULTS FOR SEDIMENT t 2 (in ppb) Sample ci-4 Cl-5 Cl-6 Cl-7 Sediment ( 2 15 ND 20 127 Sediment 1 2 R 13 ND 22 156 BLANK ND ND ND ND MDL 0.5 0.5 0.5 0.5 MDL aathod datactlon Halt ND non* datactad at aathod datactlon limit R rapllcat* aaapla Cl-8 1000 1500 ND 0.5 MOMS 02*041 5 Table 3. PCDP RESULTS FOR SOIL AND SEDIMENT tin ppb) Sample Cl-4 Cl-5 Cl-6 Cl-7 Background ND ND ND ND Soil 15 3.9 1.4 3.8 0.9 6oil <5 R 4.9 3.5 5.4 1.2 Soil 113 0.2 2.6 4.2 0.9 Soil 127 ND ND ND ND Soil 135 ND ND <0.9 0.4 Soil 139 ND ND <0.6 0.4 Soil 151 ND ND ND ND Soil 151 H * recovery spike level 5.0 37% 13.6 25 64% 29.4 32 64% 49.7 8.1 76% 10.7 Soil 157 ND ND ND ND Soil 159 ND ND ND ND Sediment 11 0.2 <1.6 <1.9 0.6 Sediment 11 L 0.7 4.7 4.3 1.0 % recovery 46% 100% 82% 90% spike level 1.0 1.2 1.1 1.2 Sediment 12 <0.6 <8.2 <22 1.9 BUNK ND ND ND ND MDL 0.5 0.5 MDL method detection limit 0.5 0.5 ND none detected at method detection limit R replicate sample L,H low and high spiked samples 1-8 ND 0.8 1.1 2.4 ND 0.9 1.0 ND 33 93% 35.3 ND ND 2.4 5.3 81% 1.0 5.5 ND 0.5 MOWS 024042 6 Tabl 4. 2378-TCDD RESULTS TOR SOIL AND SEDIMENT (in ppb) Sample Background Soil 15 Soil <5 R Soil 113 Soil 27 Soil #35 Soil #39 Soil #51 Soil #51 H Soil #57 Soil <59 Sediaent (l Sediment #1 L Sediaent #2 BLANK MDL 2378-TCDD ND 510 7000 1.8 1.8 0.9 0.7 0.1 8.2 5.2 2.6 ND 1.0 16.5 ND 0.2 ppb Added 9.4 1.0 ND none detected et method detection limit R replicate saaple L,H low and high spiked saaples 7 MOMS 024043 Table 5. 2378-TCDD RESULTS FOR WIPES (in ng) Sample 2378-TCDD ng Added Auger 1 Bit ND Auger 1 Handle ND Auger 2 Bit 3.4 Auger 2 Handle ND High Spike 44 48 Low Spike Blank 4.3 4.8 ND KDL 0.3 MDL method 3etectlon limit ND none detected at method detection limit HONS 024044 8 rT^ HVI*OHUtHfAL C / rciting * cc atia/cation Technical Report tor MONSANTO COMPANY 800 N.LINDBERGH BLVD. R3B ST.LOUIS, MO 63167 CM(* ir CMiMy am UIM : MONSANTO GWANY rTCJWtW. , t , C--Moy far |TC 0i litMiry /liNrti ' HONCORKNQ ' r KJ14 P**flHy S9M*t* P*ln4 Of Tim* t$S!r! John J.^ftzforild Vie* Pr*H*nl ****/eft *nc Op*r*io$ tcv>K*l Maart te r 1<41<I**m'<ki lem'itN ay itotsm* Oeta nar-ee*er>t leiM't - 2*4 MMTM CtMTtHPAtlKWAr OlSON. MJ 0*437 . (7*1) 22*-H*0------ HONS 024045 CYA tNVIAONMfNTAL C IV^ Tf*TINO * C$*7IP>CA7/ON TABLE OF CONTENTS introduction TaMs i: Results and Quality Aieurinca Data Table 2: Method Performance Data Methodology Qa Protocol Report Appendices Appendix A Mata Spectral Data tor Quantitated Compounds Appendix Cl - QC/MS Subsidiary Data - Blank Chromeloprame Appendix E * Chain of Custody Forms MOMS 024046 CTA tNVlAQNMt NTAt C I V TitltNQ wtf CltniflCATtON Introduction This report contains the analytical results on your soil sample, 5 06/03/14 it is designed to include comprehensive data from the entire analytical process m order to satisfy the needs of various levels of rsvisw. The results obtained from your temple are presented in tabular format immediately following this introduction. Quality eeeurence data <e tabulated along with the appropriate temple results tor verification. Depending on the analysts ordered, the quality assurance data may include results from blank, spiked Wank, spiked sample (i.e. matrix apika) and replicate sample as well at results from surrogate compound analyses Quality assurance data for verification of proper Instrument performance is also included where appropriate. The report appanages include the chain of Custody record for your sample and. where aoorooriete. the gas chromatograms and mass spectra. The procedures used in the analysis of tha sample are described in this report's methodology section. Ail analytical procedures within our laboratory are performed within a strictly enforced Quality Assurance Protocol. A description of this Protocol is mciuded in the report. Results Sample results. and associatad quality assurance data, ara alwaya tabulated in ona or mora o! this raport'a Quantitative Results Tables. Tha format of each tibia varies with tha dess of analysis. trinity SanariMi Tha priority pollutant compounds and elements ara listed with their NPDES (National Pollution Discharge Elimination System) numbers, and tha Method Detection Limit (MOL) published in the Federal Register. When e compound or element It present Delow its published MOL it is reported as BMOL (Below Method Detection Limit). Whan a compound or element it not present tt any detectable concentrations It Is raportad as NO (Not Detsetsd). MDL'1 for non-aquaous matrices ara based on USEPA published MDL'a but are adjusted as par tempi* weight. Matrix apika and replicate analysts, where included, were performed on temples randomly chosen within each quality assurance batch and are therefore not necessarily tplkts and rapllcatta of tNa raport'a sample. Surrogate compound recovery data and Instrument calibration data era included In the Method Performance Data Tables HONS 024047 HONS 024048 ev/t fwv'ftowirfwrA* ' ClV litlMQHtfCtttitKATIO* TABLE 1: QUANTITATIVE RESULTS and QUALITY ASSURANCE DATA BASE/NEUTRAL COMPOUNDS - QC/MS ANALYSIS DATA (QR03) Cft*> 1 CMtatfy *tt LVIM MNMffAOfrfMft T| **>( %. *#* *r ITC D*U MwxfwwU fewnary R^orta NOaDMfM MAIN tainir * *M NH tfek* 1S>|* An . IMA RONS 024049 HONS 024050 SI V tCtMOM<CCftT>r>CAftOM TABLE 1: QUANTITATIVE RESULTS and QUALITY ASSURANCE DATA Priority Pollutant Matala - Analysis Data (0R05) W* M CMMy Mi Ri4ii4 tm tTC Ml Mmumnw g--? ' U1M HONMKTS COTMft irct^fUHt. teM| HONCtSrCNS V Mt)l 'Hllr ta*h tiln toi* tta* 'aSD*" wv I IMi MOMS 024051 I--ETC TABLE 2: METHOD PERFORMANCE DATA Surrogate Recovery Son - OC/MS Data (OR20) U1M WNUmv C9NTf |M iMtft . (mihM VOUTIlf MMC110N TbImrb-M 1 ,}'DlchlrM(liiA`M ACID FJtACHW ntMtl-06 Hlwwhml M,l`MIrwio)n| MSf/WOTML FMCTION NltrAitM-M HlwrAlpM|il 1trtArl*DM HONCtNMMQ I Mill FMUiiy taagM *ami Bala aiS!t* IMi HP4 . Ill lit IN M M M t Ifmiry . . M M IN H II 49 Culr| UftlU lwr wpp* M IN M Ml M IN II IN at IN at IN M IM __ . M u_ " . -- - ------- - - --- -- -- - .. MON$ 024052 TABLE 2t hETHOO PERFORMANCE OATA CQR22) 6C/M5 Tuning Dt - C>caf luorotriphnylphopin* (DFTPP) for Acid* s*nlyi mst *1 68 69 70 127 197 196 199 27% 363 441 442 443 Ion Abundance Critor io >0-60* of moo 196 Looo thon 2* of moo 69 (reference only) Looo thon 2* of moo 69 40*60* Of OIOOO 196 l... th.n IK ef *.. 198 6000 peek, 100* rolotivo obundonco 9-9* of moo 198 10-30* of moo 196 Gretter thon 1* of moo 198 0-100* of moo 443 Greeter thon 40* of moo 196 17-29* of moo 442 * Relative Abundance Boo# Approprioto Peek Pook S'etut 48.92 .95 92.22 .29 47.23 0.00 100.00 6.94 20.47 2.39 9.10 95.69 10.99 46.32 1.81 92.22 .43 47.25 o.uo 100.00 6.94 20.47 2.33 82.74 33.89 19.07 Ok Ok Oh Ok Ok Ok Ok Ok Ok Uk 0k Ok Ok Injection Date* Inaction Tims Run No i Spoetrun Noi 14i59 > 19662 662 Ana)yetl Proeeetor* OC Boteh> Oft H>ii._..ZZy Samploot .LHZNfi. +Um32x ,Um3?ZL HONS 024053 TA8LE 21 METHOD PERFORMANCE DATA CQR23) GC/MS Tuning Data - Oacaf luorotr iphanylphespma <0FTPP) for Basa/Nautrsl Anlyi . Ion Abundonco i/t Cr i torio % Relative Abundonco Booo Appropriate Peek Status 91 68 69 20 12? 19? 198 199 273 369 441 442 443 30-60* of moot 199 Loo* than 2* of moot 69 (roforonco only) Loot than 2* of mass 69 40-60* of mass 196 Loot than 1* of maoo 198 Bass peak, 100* ralatiua abundanca 9- 9* of mass 198 10- 30* of mass 196 Greater than 1* of masa 198 0-100* Of mass 443 Greater than 40* of mass 198 17-23* of mass 442 90.?4 0.00 92.21 .26 48.40 0.00 100.00 7.32 22.40 2.43 10.96 74.07 13.79 90.?4 0.00 92.21 .90 48.40 0.00 100.00 7.32 22.40 2.43 76.79 74.07 18.97 Ok uk Ok uk Ok Ok Ok Cfc Ok Ok Ok Ok Qk Injection Data! Injection Timas Run Not Spactrun Not 04/01/96 00s4l >F63?4 400 Analyst il Procsssori __ QC Bat chi Samp I*, i UtitH-jjAH, Llsib -LlsiU, HONS 024054 ryA tHVItONUtHt Al CIO TttriNO 91*4 CitTtfilCATION Methodology for OC/MS Analysis of Priority Pollutant Compounds The methods employed m the QC/MS enelysis for priority poiiutante ere established Eph methods Rigid compiience with the instrument parameters and performance criteria of the puotished methods was achieved, in some cases, the precise amounts of sample used and the sample handling procedures very with the complexity of the sample matrix. Qualitative identification of the priority pollutants was performed using the relative retention times the relative sounoance of three characteristic ions and the aoundanca ratios. The entire mass spectrum was reviewed to confirm each identification. Quantitative analysis of detected compounds was performed by using a response factor generated by a major characteristic ion of the specific compound and an Internal standard. Compounds, m addition to those on the priority pollutant list, ware identified through a computer-aided search of the NBS-EPA spectra library. After review the identifications are included in a separate tabulation and labelled `tentatively identified*. Asia, fere/FfeufraJ and Aeaf/t/da Arlarl/r Aerfirranr Campoune* For the analysis of the Acid. Base/Neutral and Pesticide priority pollutants m a sod matrix a modification of EPA Method 62$ was used The method can be summarized as follows A $0 gm sem-wal sod sample is soxhiet extracted with a t:i mixture of acetone and hexane. The acetone la thermally stripped. The remaining hexane extract is diluted to 200 mf with methylene chloride end twice extracted with an eaueous NsOH solution followed by an extraction with deionized water. The methylene chloride extract is dried and concentrated to a 1 ml final volume. This concentrate is injected into a QC/MS Instrument configured for the analysis of Bate/Neutral priority pollutant compounds. The remaining aoueous extracts are combined and the pH adjusted to a value less than 2. The aoueous phase is serially extracted with 3 enouote of methylene chloride. The methylene chloride extracts are dried concentrated to a 1 rm tine) volume. The concentrate Is injected Into a QC/MS mstrunent configured for the analysis of add extractable priority pollutant compounds HONS 024055 CTT* tUmONMlNTAl CK/ TtStlNO /> CiatltlCATlON Methodology for Analysis of Metals AQUfOUS The determination of metai* tn aaueous samples is performed according to the methods published Dy Epa in "Methods for Chemical Analysis of water and wastes ' SPA-600/4-79-020. March. t963. and the Federal Register. October 26. 1963 Arsenic selenium and thallium are determined by furnace aa; silver, aluminum, barium, berytimm txxon, cadmium, caidurn. chromium, coooar. cobalt, iron, magnesium, manganese, molybdenum, nckei lead, sodium. antimony, tin. Mamum. vanadium, and z>nc are determined by ICP amission spectrometry, except where lower levels of detection are reouired: m these cases (eg teed n groundwater monitoring samples) furnace AA is used All furnace AA parameters are run py method of standard additions The determination of mercury is performed by coio vapor aa tp roxicny The determination of metais m aoueous EP Toxicity laachates is performed aecorang to the methods published by EPA m "Test Methods for Evaluating Solid waste* EPa $w-646. revised April. 1964 and the Federal Register. Oct. 26. 1963 I9r9. Saver, arsenic, barmm. cadmium, chromium, lead and selenium are determined by ICP emission spectrometry Mercury s determined using coio vapor aa. For leachates that ara orgemc m nature, the analyses are performed according to the methods described under ou/siubdf below. SOIL/ttDlUeNT The determination of siivar. beryllium, cadmium, chromium, copper, ncfcei. antimony, lead, and 2me m etdiment samples is performed according to methods published by EPA m "interim Methods for the Sampling and Analysts of Priority Pollutants tn Segments end Fish Tissue*. EPA 600/4-61-055. October 1960. Mercury is determined according to the eedment method published by EPA m "Method for Chemical Analysis of water and Wastes*. Epa 600/4-79-020. March 1963. Arsenic, seismum and theinum are determmsd by furnace aa using nitric acid m a closed decomposition vassal for sample digestion. QH/tLUOQt The determination of silver, aluminum, boron, barium, beryllium, caicmm. cadmium, cooper, chromium, cobalt. Iron, megnesium. manganese, molybdenum, eod*um, ruckei. lead, antimony. \n. titanium. vanadmm. and zinc in siudge/petroiium-pasad samples is performed by ICP emission spectrometry using s magnesium nitrate dry ashmo digestion techmoue Arsemc. seiemum and thallium are determined by turnacs AA using mine acid tn a closed decomposition vessel for sample digestion. Mercury is determined by cold vapor AA using the same digestion tachmout HONS 024056 rf/N gNVmONMtNTAL I rtSTlSH iiKf CtATIftCATION Summary of Quality Assurance/Quality Control Procedures (QA/QC) ETC bases its quality assurance protocols on the following government gudennes . 'Handbook for Analytical Quality Control m water and Wastewater laboratories*. EPA-600/4-79-019, March T979; . National Enforcement invaaligation Center Policies, end Proceduraa manual: EPA-330/9/79/00-R. October 1979: . the recommended guidelines for EPA Methods 674 and 62S. (Federal Regster, Oecemoer 3.1979; upcatad on October 26.1964); . "Manual of Analytical Methods for the Analysis of Pesticides m Humans eno Environmental Semples.' EPA 600/6-60*036. June i960; . "Determination of 2,3.7.6-TCDO m Son and Sediment" EPA, Region vti. Kansas City. September 1963; Or game Analysis: hMti-med'S. MuMi Concantralion-lFB wa4-a267; eno . D*o*n Analysis Soii/Sedrmenl Matrix; Multi-Concentration; Selected ion Monitoring with jar Extretion Procedure-IF6 WA64-A002 However, we heve modified our protocols to provide a higher level of QA/OC then the guidelines require. For example, we analyze e higher then required number of Quality control aamptas ana wt pay atpeciaiiy cartful attention to the certification of the 'reference standard' comoounos we use m analysis Below ere listed the key OA/OC elements for the methods we used AnalysIsot Vole tile Organic Compounds by Gas Chromatography/Mass Spectrometry - Each batch of 13 samples consists of 9 customer samples (at a maximun) one blank sample, one spiked blank, one spiked sample end one replicate sample. This amounts to e 30% quality control factor. - Three surroQeie compounds are added to each sample in the batch of V3 - A bund quality control sample is introduced to the laboratory for analysis on weekly bes*e. - Each GC/MS is checked end retuned, if necessary, at the begnmng of each day to ensure that its performance on bromofluorobenzene (BFB) meets the EPA criteria - a calibration curve for quantitation prepared using mixture of volatile Organic Priority Pollutant 'standards* at a mm*mum of 3 differ ant concentrations and using a mixture of 3 internal standards at a constant concentration. - Tht calibration curve rs verified with c mixture of priority pollutant standards avery day >f the response factors very greeter than 2$%. the instrument must be recalibrated. Analysis of Organic Compounds Extracted in Acid or Base/Ntutrai Solutions by Gas ChforfiVjoorfDhv/tyaii {fofqfr9fli*fY " -- - Each batch 01 20 samples consists Of 16 customer samples (St a maximum), on# blank sampit. one so* eo oianv dor water matrices), one sample spiked with the orionty pollutant ttendaro mixture ana a duplicate Customer sample. Tims amounts to a 20% Quality control factor. HONS 024057 glV TISTING tr,0 Cl*7lHCA7lON - Three surrogate compounds are aouea to each sample >n the batch for Base/Neufrj/ analysts. - T*e surrogate compounds are aoaeo 10 eac* sample n the etc* for aco ana' *s s a o*'hd duality control sample >s introduced to the laboratory for anatyS'S on a weeny oass - Each GC'MS is checked and retuned, if necessary, at the bev'*nng of each day to ensure tr.at ts performance on decafiuorotriohenyiphospnme <OFTPP> meets t*e 6a criteria A calibration curve for Quantitation is preoared using a mixture of standard* co^ooseo ot either the Organic Aod or Base'Neutral Extractable Comoounds et a minimum of 3 concentrations and usmg five internal standards for Quantitation Analysis of Mstais Ml - New standards are prepared for each batch of samples Normal ceiiorat'on is performed us "g a blank sample eno four standards that ha* been through the sample preparation procedure, a regression analysis is used to construct the calibration curve - aii EP Toxicity samples and an samples determined by furnace atomic absorption are calculated by the 'method of additions' For each sarnie analysis that requires the use of the 'method of additions* ttcnmoue a three po*nt calibration is performed using US- EPA 'Methods for Chenwcei Aneiyss of water ano wastes. 1979". Results are obtained using linear regression analysis Any regression with a coefficient of correlation below 0 990 is considered suspect, necessitating review of calibration date or sample re-anefysis. in constructing the normal calibration curves the lowest concentrat>omevis we use are values greater than or agoai to 5 times the instrumental Detection Limit oDo - am calibration standards ere analyzed >n duplicate, at a minimum. 'ir>dec>erfbfcnt reference standards are used to check the accuracy of calibration standards. - a check standard is analyzed every ten samples to validate the normal calibration curve. - One customer sample out of every ten is analyzed n triplicate. Htmoftnjout 9tmp/tt ftxc**/ ft Mprcury inuytit) Samples art analyzed m batches of 30 or less. For oatcnes m which the samoi matrices ere homogeneous. U>e OC program >s a minimum of 25% and consists of analyzing 3 sets of triplicate analyses: 2 Pepucete spikes: t independent reference standard. a Castration st vioaros (processed using the sample preparation method). - 4 cai'orai'On stanoaras (*.:fc.cui sample preparation), and - i F*ag*n: Bur* HONS 024058 CT/N fHVIfiONUtNTAL Xfls TitTINQtn4Ct*TMCATlON nOW (xepl_## Mtrtwiy Samples ere analyzed m batches of 30 or loss For batches m which the sample matrices er heterogeneous, the OC program is a minimum of 35% and consist* of analyzing - 3 sets of triplicate analyses: - 2 Repiieate spikes; - i Replicate independent reference standards; - 4 Calibration standards (processed using the sample preparation method). * t Procedural Blame * 4 Calibration standards (without samoia preparation); and - t Reagent Blank. Anfy4t of Marevry To analyze samples for mercury we group them by matrix in batches of 30 or lass Our OC program is a minimum of 30% and consists of analyzing - each of the 30 customer temples m duplicate; - 3 eats of triplicate eneyises. - 2 Recreate spikes: - 2 Replicate independent reference standards: - X) Calibration standard# (processed using the sample preperetion method), end - 2 Procedural Blanks. Analysis of Paatkidea, HerUcldaa and PCB't by Qas Chromatography Pesticide, herbicide and PCB tempias are grouped in batches of 16 customer aonpios o. ass according to the type of analysis to be performed. The OC program for each of these thrse types of analyses is a minimum of 20% end consists of analyzing: * t procedural blank sempie(e reagent blank is analyzed in the case of non-water matrices); * t spiked blank sample (the spiked blank is eliminated in the case of non-water metnces); - t rawtesta sample. - i replicate spiked sanpie; and - t known refernece OC sample for at (east each tOO samples analyzed The instrument is calibrated each run with three standards, and checked every to samptes Analysis of Cyanides. Phenols. Fluoride. Chloride. Nitrate and Nitrite * ah parameter* are analyzed us*ng a Tecnnicon Autoanaiyzer n gt - 3 calibration standards are analyzed at the oegmnmg and end of each batch MOMS 024059 ETC tNVlAONMfJV7JU rtSriMQ ane Ct*7tflCA7lON ` - Each batch (uo to 80 sampj#s) consists of analyzing on# blank, one so*keo wan* one duplicate and spiked sentpie every 20 samples, ano an EPA known reference sample Analysis of Total Organic Carbon (TOC) TOC *amoes art analyzed on a da*ty basts with the number oi samples anaiyzadpar day deoanoent on the reouest for duplicate or quadruplicate analyses The quality control pro^sm.s designed to maintain the eooropriate amount of QC and consists of the following elements - Daily instrument calibration One Wank * Standard receubration every 10 samples - Spiked semoies at a low and tvgh level - Every sample it run m duplicate at a minimum Analysis of Total Organic HaUda (TOX) - Blank reagent water for absolute carbon backround must contain lass than $ uo/t of halide (as chloride). - Using a tnehiorophenoi standard, the mean adsorption efficiency must be within /> 13% of the standard value. - Calibration standards are run every to samples. Every temple i run w duplicate at e minimum. Analysis of_2t3.?.*'?CQP (Worfn) by OC/MS (SIM) * Each sample It dosed with known ouantity of ^Cj9''2.3.7.8'*TCOO as mternei standard and 37Ct4-TCD0 as surogate standard. The action limits for surrogate standard results is /- 40% of the true value. Semples snowing surrogate steno*a results outside of these limits are reextracted and reanalyzed. - Two laboratory vnetnod oianks* are run along with each set 01 24 or fewer samples The method blank is also dosed with the internal standard and surrrogata standard - Aprtelcaiassiotno.ne per set of 24 samples is run in duplicate to determine tntraiaboratory - Ouehtative Requirements. The following are met m order to conirm the presence of native 2.3.7.6-TCOO: a. Isomer specificity must be demonstrated initially end verified once per 6-nour work shift. The verification consists of injecting e mixture containing TCOO isomers which elute dose to 2.3.7,8-TCOO. The 2.3.7.8-TCDD must be separated from interfering isomers, with no more than 25% valley relative to the 2.3.7.0-TCOO peak b. The 320/322 ratio is within tha range of 0.67 to 0.67. C. long 320. 322. and 2S7 are att present end maximize together the *.gni to "ea* noise ratio must be 2.5 to 1 or better tor ail 3 tons. d. The retention time is tauai (within 3 seconas) the retention time tor the isotopicaiiy labeled 2.3.7.6-tcdo. e At least one of the positives can be confirmed by obtaining partial scan spectra from mass t50 to mass 350 The partial scan guidelines are as follows: HONS 024060 iNVIHOHkltNTAl Civ TfSIlNQ SA* Ci*TtflCATION . the 320/324 ratio should Da 156 */- 0* . th 2S7/2S9 ratio should 0 1.03 4/- 0.10 * . the 194/196 ratio should be 1S4 */- o.is - On sampia is spiked with native 2.3,7.8-TCDO at a level of to PP8 (for soil) for each set of 24 or fewer samples. - in cases where no native 2.37.6-TCDD is detected, the actual detection limit is estimated and reported based on a signal to noise ratio of 2 5 to 1 at ions 320 an - For each sample, the internal standard is present with at least a to to i signal to no*se ratio for both mass 33? and mass 334 Also, the internal standard 332/334 ratio must be withn the range of 0.6? to 0.67. ubcontractgr_QA/QC Each aubeontractoer is required to maintain an appropriate level of Quality control To insure this, each subcontractor is required to submit to ETC the quality control data for an analyses it performs. This data is kept on file at ETC. in general, the amount of Quality control rtQu*eo >a one duplicate sample with one spiked sample for every tan analyses. heln-of -Custody The chain-of-custody procedure is part of oir quality assurance protocol. We believe our cham-of'Custody record fully complies with the legal requirements of federal, atata and local government agencies snd of the courts of law. The record covers: - labeling of samoia bottles, packing the Sample Shuttle and transferring the Shuitie under seal to the custody of e shipper; - outgoing shipping manifests; the chain-of-custody form completed by the persons) breaking the Shuttle seal, takmg the temple, reseating the Shuttle and transferring custody to s shipper, - ir.ccmmg shipping manifests. - breaking the Shuttle's reseat; * storing each labeled sample bottle m a secured area; - disposition of each sample to an analyst or technician; and - the use of the sample in each bottle m a testing procedure appropriate to tnc intended purpose of the temple. The records show for sch link in this process: * the person with custody; end - the time and data each parson accepted or relinquished custody. HOMS 024061 ETC tNvmONMgNTAL US1INQ hr* Ct*TlHCATlON Appendix A Mats Spectral Data tor Quantitated Compounds t) A total ion chromatogram tor aach aampia analyzed py a GC/m$ instrument. 2) a Quant, report used by tha analyst to determine Qualitative eno quantitative results of the compounds present. 3) a mess spectrum and a reference spectrum for each priority pollutant compound detected in the sample. HONS 024062 TOTftt ION CHtOMBTOCtOH _____ pii acu 'T17H4B Do to Ft lot >13667::U7 Nomot 860331 ACID I Mioct L7190A ,UA474>,S,30.0v,l Id Filoi IAC1D:iUS Tit lot PP/'ACID IDFILE Loot Colibrotiont 860331 14:52 Oporotor ID: JH2180 Ouont Timot 860331 21:36 Injoctod oti 860331 21:03 BlLHi HONS 024063 C|U*WT RtPOKY Oparator IDs Output Fila) Data Filat Nam#t 0609)1 Mites L7194A JH210O 'M3667ssAQ >l3667tiU7 AGIO 1 ,QA4?47,S,30.09,1 Quant Ravi 9 Quant Timas Injactad ats Dilution Factors 060331 21:3* 060391 21:03 l.uu BTL912 IO Filai lACIDsiUS T 11 (at FF/HUO luF IL Laat Calibrations 060391 14:92 . Compound R.T. Scant Araa Cone Un 11 a 1) *d4-1,4-Oschlorobanzana 6.27 179 12646 40.00 UG^m. 3) 2-Fluorophano1 8) Phanol-D9 11) *d0-NaphthaIona (SUM*) (SURA) 4.19 9.72 9.90 42 140 394 21999 24474 20006 90.20 UG/MC 66.32 UG'nc 40.00 uG/m. 12) 2,4-0ichlorophano1 9.22 949 1723 8.91 UG/ML 17) diO-Acanaphtnalana 14.62 649 20642 40.00 UG'NL 22) 2,4,6-Trichlorophano1 12.60 939 119696 909.99 UG/rtL 23->-------42*99- -W -------- 1797 . ------7.91 -UC'ML 29) 1 ;9t>c^i 1 orophtnol -------- 45-.G0----719- --29994- 167*94 24) #dlO-Phananthrana 19.07 099 *0940 40.00 UG/NL 2$) 2,4,6-Tribromophanol (SURR) 17.06 706 22399 99.76 UG/NL 26) Pantachloropnanol 10.79 089 904 3.67 ug/m. 26) *di2-Chryaana 27.34 1962 92200 40.00 OGxnt Q 9! , 91 4> 9: 9( 9; 9. 101 Compound i* I SID C9 9Clu HONS 024064 fiCrCKCMCC STRN0AKB SPECTRUM fFii">ilMS'`WlSTlUv. r 0*1* JiiiTyl I #*< Irii'of Ifc# fff? J< n t/tfl |p* MR 9999 *** 99*J.#a ain. *? M 1 491r ^r i>* I u SO IM IM ^I*a< ^ *fiTr jJo ~ "jif "" * Wo' ' ' SAMPLE SPECTRUM fOACKSROVHP SUOTRRCTCO) I7s U >!)((?MI33I HCIO.! 17I04A ,004747,1,31.19,i M .f X'M-a. SO ! I MS 200 371 (i f* / \ ^i.,ur * io* ' Wo SAMPLE SPECTRUM IUMRLTCRCOI - V>,Jj*f **3I -*"1 " 171 *44 "70A4747 ,S, MTO, 1 s<L* ,4( 9.22 Bin. / ?y 4,4 r TM , ,_Uu 14. SO IM lio sit 2S0 90s sio 400 Data Fi la t > I3667i*U7 Hamas 640331 ACID 1 Miaei L719*A ,QA4747,S,30.09,1 Quant Timms 060351 2136 lnjactad at> 600331 21*03 Compound Not 12 Compound Hamai 2,4-Dichiorophanol Scan Numba r\ 345 Ratantion Timai 9.22 min. Araai 1723 Concantrations 6.51 ug/hl q-valuai 90 til LSI 2 HONS 024065 (XTCiriCaC>HCuCJitTAWMO3ftl*tS#wSrfCeCTrA*UuH IbL b 9999 iptstr* *t ** ni$ 4 $<* 2313* ,M 9899. tin. $A**lt mCTRUH IMC*OVN $yT*CTE*> (TnT'TTi<>'w?i--wii------ niTO *tbw473';w:m,t-- ?<? pk lit 34C SU ** 10.M !". H 13| 13* << 11 ,1 till ill).. 11 [.I l Ilf nk 1 if 1 if so,l44!*r V-!^V-^-I..iii...... Vif........ji--.......i>-, SAMPLE SPCCTAUM (UNAlTCAC> r'li* >l3JJT ****! ACI8 ~^r *fpk At * ... r LM94A ,004747,S,30.I*,1 j" "' ||) IA. ' \ fIJTI * * jl). .H ?v4 DttA Filo* >I3667i*U7 Nomot 860331 ACID I Mitel L7194A ,UA4?47,S,30.U9,1 Qoont Timor 860331 21i36 Injoctod Ati 860331 21i03 Compound Noi 26 Compound Nomol Pontochlorophono1 Scon Numbort 883 Rotontion TimoJ 18.79 min. Aroor 984 Concontrot ions 3.67 UG^ML q-voluoi 89 biL MONS 024066 ACrCKCNCC STANDAM ffCCTIUH riit >ijh* fciSTUv". c i*t*l*tTun p*ctr* or <h uk ?'$< rot2 SAopft Ab 9999f *" 1ij49i1i2.aMa >AIi.n. mt L 4 4Xfir4Mf 49 iiT" *W tit" .1. ' JU SlUn.BCTtf I7TS. fitterseif 'tpk at l?e* I >4Ul .*,! < ti ( \( l lit i '/* I I *7 *" *> \ 4\. i it. it> '' tie " tie '' iie' "' lie' ' * .ii towic tetcTeun iuMu..cete> mV >ii* mmh" aci6 -- 17j/r*4 --.emuM.je.M.i- j,, let at 14114 tit tt.ttT.il, "1 I) .1. n... j r IN lit 2N 2(1 )+A )(t 4M Da to hill > 1366? 1 U7 Hamat 960351 ACID 1 FI 1 AC t L7194A ,QA4?47,8,30.09,1 OuAnt T ai 960331 21t36 tnjAdAd iti 860331 2H03 Compound Hot 22 Compound Nomot 2,4,6-"Tr ich lorophono ) 6con Numbort 539 RotAntion Timot 12.60 min. AroAi 115839 ConcontrAtiont 509.95 UG/'HL q*vAluot 9? eiLi2 HONS 02406? Data Fila: >F6389:U2 Namei 060331 #F B/N&PEST Miec: L 719 **9,084747,3,30.09,1 Id Filet FBNPitUS Title: B/N*PEST ID FILE .... .FOR F Laet Calibration: 660401 12:03 Operator lOi RAO197 Quant Tima: 660401 19:32 Injected at: 660401 18:44 050326 8TLei3 HONS 024068 quant report Operator ID: RA0157 Output File* *F6309*AQ Date Fi!: >F6389t*U2 Name* 860331 F B'N6PEST Miec* L7194B,QB4747,S,30.09,1 Quant Raul 5 Quant Time: Injected ati Oi lution Factori 860401 19:32 860401 16i44 1.00 BTU623 10 File: FBNPiiUS Title* B'N^PEST ID FILE .... FOR F Lett Calibration* 860401 12*03 850326 Compound R.T. Sc.nl Area Cone Unite 1) d4-1,4-Dichlorobansena 2) N-Nitroaodimethylemine 7) 1,3-Dichlorobeniene 6.50 249 19112 40.00 UC'ML --- --------- 3843------------ 56Pi-----------7r9 6^ML 8) 1,4-0ichlorobeniene 9) 1,2-0ichlorobeniene 6.96 275 ------7r*9 4JG**1L 5071 7.98 UG--ML 12) Nitrobeniane-D5 <SURR) 7.92 329 29944 37.90 UG'ML 16) d0-Nephthelene 9.74 433 64612 40.00 UG/ML 19) 2-Fluerobiphenyl (BURR) 13.13 63515 31.10 UG^ML 33) dlO-Acenephthelene 15.08 49813 40.00 UQ/ML 39) Dimethyl phthalata 86UG.'Mt 39) Dimethyl phthalata 1.76 UG^+L 41) 2.6-0 initrotoluene 11*29 UG-'riL 41) 2.6-Dinitrotoluene . 25 -OG-'ML 45) 2,4-Dinitrotoluene 46) Diethyl phthalata --r53 54) *dlO-Phenenthrene 40.00 UG>'ML 58) Phenenthrene ---,73- UG4AL 59) Anthracene ~ r*l UONL 60) Di-n-butyl phthalata 2*~r6?--1444 -3,06 UC^hl 61) rluorenthene 23.36 1200 1.63 UG^nt 63) Pyrane 73t*A- 4684 - 4 -?6- 4JC-4S. 72) *dl2-Chryeene 27.84 1452 40.00 UG-'ML 64) Terpheny1-D14 (BURR) 24.70 1275 24.51 UG'HL 86) Butyl bensyl phthalata 2*r5--IW 2r81 90) bie(2-Ethylhexyl)phthalate 26.+6--1486 6247 6.76 UG'ML q 97 100 96 96 95 87 93 Compound ie ISTD HONS 024069 t'C*CHCC STANft *JCfT*U (Tir* itHic i/tf* Ipk At 43*774 4AAAA*j V vh eft.it*. su zeeteA 49 A SAMPLE SPECTAUM tACKC*0UM9 SUITPACTEt) ITuf*r v 4*4*47,?,3*.**,r Ipk Ate SMS SVI SA J'S 4 .A' ain. till] IMA I 4-v,- 7( .. K . 4A 1 m u#r \.i,i IT iJp A 4| M 1 ''Hi' SAMPLE SPECTAUM (UMALTEAED) TiiVmzATWwr *r ~)/nipcsti7i*4i,014747,5,39.am Ipfc Ate ZA4l tAAA44#-j iaf *7* 4 am. /L Y y"1 ?- "f" 1 Data Filtt >F6389tU2 Name t 860331 AF B'NtPEST Mitect L7194B,064747,S,30.09,1 Ouont Tm#: 860401 19:32 JnjtectAd lit 860401 18:44 Compound No: 9 Compound Nom: 1,2-Oichlorobtnzene ScAn Numbor: 279 Rotention Tim*: 6.96 min. Artot 5071 Conctnlration: 7.98 UG^HL q-VAluo: 95 btla:3 *0NS 024O7Q PT/V tmmoNulHUki CfV USIlNOlMClKTIflCATION Appendix C1 GC/MS Subsidiary Data HONS 024071 TOTBl ION fnu ______ 4r.t-45#.t Kmf ' flfi r ocwm ,1*4747,1,1 D( Fi !< > 1366J iU7 N<*! 860331 AGIO I 0O747A #QA47471,1 Id Fi1i lACIDitUS TitUt PP^ACIO IOFIUE l.4*> Oibr**ion* 860331 14:52 Oprter IOi JH2180 Qunt Tins 860331 16*52 In,#ct*d ti 860331 14*19 01L| 0 HONS 024072 QUANT REPORT Operator 101 0H2180 Output File* AI9669t*AQ Data Filet > 196691*U7 Name* 860991 ACIO I nieet QCa7a7A ,QAa7a?,S,1,1 Quant Ravi 9 Quant Timet Injected att Dilution Factor* #60931 16*92 860971 1619 1.00 0TL 8 ID Fi Ui 1ACID* iUS Title* PP/ACID IOFILC Leet Calibration* 860991 14t52 Compound R.T. Scan# Area Cone Unit 1 > "d4-1,4'Dichlorobantana 11) *d8-Nephthe lane 17) dlO-Acenephthe lane 24) dlO-Fhenenthrene 78) dl2-Chrya#n# 6.17 9.26 14.46 18.92 27.02 175 949 642 899 1949 J940J 90499 94999 60065 18515 40.00 uC'nc 40.00 UG'MU 40.00 UG'ML 40.00 UO^ML 40.00 UC^ML * Compound it ISTD MOWS 024073 TOTAL tOM CMHOHATOCftflH Ooto Fi ill >F63841:U2 Noo 860331 #F 8/N4PEST fliftCi QC4747Bj084747, S > 3 0,1 Id FiUi FBNPmUS Tit lot 8/H*PST ID FILE .... FOP F Loot Colibr^tion: 860401 02:06 Oporotor ID: KU0786 Ouont Titooi 860401 09:86 Injoctod oti 860401 09:08 890326 BTLOte MOMS 024074 quant report Operator IQt KU0766 Output F i l: AF63B4tiAQ Oete FiIn >F6304:iU2 Niimi 860331 F B'NtPEST nie OC4747B#GB4747,S,30,1 Quant Reu: 5 Quant Timet Injected eti Di lution Factor : 8604Q1 09:56 860401 09:08 1.00 BTL910 ID Filei FBNPitUS Title: B/'NPEST 10 FILE .... FOR F Leet Calibration: 860401 02*06 850326 Compound 1) *d4-1,4-Dichlorobemen# 2) N-Nitroeodimethylemine 16) dS-N.pbth.l.n. 33) dlO-Acenephthelene 39) Dimethyl phthelete 94) *dlO-Phenenthrene 60) Di-n-butyl phthelete 72) dl2-Chryn* 90) bie(?-Ethylhexyl)phthalate ,, *> Kfc 4u< Compound to 1STD R.T. Scent Area Cone Unita 6.93 249 24624 40.00 uG/m. *-r*9-------- H---------44*8------ H,* 9.77 492 89791 40.00 UC/ML 19.06 732 41534 40.00 UG'HL ----- P38 ----- -------8r88- UC^HL 19.98 986 119392 40.00 UG'OL 21.89 1114 9574 3.24 UC^Tt. 27.62 1491 96921 40.00 ogxml 28.41 1484 53616 29.96 UC^ML Q 9 10 9 9 6 9. 9 10 9* moms 024075 CT/' CMVmOMMCNfAi C I v fisrwo ctrmFfCAiiQN Appendix E Chain-of Custody Forms 1) A field Chaln-of-Custody form (CCD It Included for ell templet thipped Oy ETC thuttle. 2) An In-house temple Chain-of Cuetody form It included for til templet noi thipped By ETC thuttle. 3) Any addUlonel Chaln-of-Custody materiel provided by t client or by t cnent'a sampling agent la alto included. 4) A tubcontrector't Chaln-of-Custody form it included for any analytical work not performed within ETC's laboratory. 5) Anti ytit and Extraction Custody forme are Included for the period the temple wet in ETC's possession. HONS 02*076 ETC fNVlAONM(*rji runwo cfmmgatiom CHAIM or CUSTODY Companyi__________ ________________________________________________ Job MO. Addrou Attention _ ttwplo Poaeriptlom CUSTOMER ID j> *r*fle J* g~7 DESCRIPTION ETC I Sbot& (UMpiti L1&H ___ J,______ ______ SaoploU) Rollnquishod byi Umti l : I S'__________ (ia** 31 Allic tost * ( Canplt(a) Rocolvod byi ____________________ TImi I ' Is Dto ?/>/** M4 JUttfAM CfW7fA PAMKWJkr (MOW. a*n &$$* J HONS 02407? chah or cvsioor ucou WC JM MM* _ */>f........................... f. 0 COMTKACT MM* _J?Q 1^0 fry _. CUS1CMCA KPRCSCNTAf IVC MC COMMCJ HMMM _,y V PlANl UH Oft COM _ ................__ _ ... C TM* UAMR __ <C4^ AJtfa (Snclflc InfonutfM on ooopUt U ovotloMo on otUcfcetf "Staple UentiMcttloa lop") SIimUtm lota Uttftr Verification/O' 0 ry, y- If UIlKtH SMfln: UA r^rC (IIkhKImA kr^V*< Receive* Oy: Otllnoolilwo *: ^ Received Oy: lOfftV-ln-ky: HtcatvM far AMljrtlt Hr: IktIM f ttlrml: A,r Otto !/<// Tta* m?/TM|01* hater of CanlolMrt __ JaHrycttoal (Soaplt praitryitlofi, w.rltjr, ioll.or, u, atc.J Rcairts fi-r^nr.!- h Cr< / S*iy,lt.*S .(*2 & title,) HONS 024078 * * fejRgt* Ltingk Wefeigmht^t(cgm) VbolrUecIlk N ACID UttW /#& IcLie. to_ j_ tjm A _ J5.J3 ... 10 1.0 Ml //$. /.o 1-0_ um __ 31.41 / 0 10 L63& y-0 $ 1/3/S' / JO-lfc / 0 1-0 LQlI 3). So j.e S.O U32Z r_i.... 31.*1 fo ro CmmimIi *OC fetch V79? SHE)/% AAarywi >T ____________ ^. ^,*1--Ciifrune^,/r) i ____ X*// . lit immd -I/ttpisl .Extraction Motttod: > ( fep.Purtotl _.. ... __ --_-- ~V^ fexMct . -- Other __ commin ' --" Lwtfif - *> -- &C 7.20 - s+*/6r r*J*,-e > TifcJ' */ < & /W /X/V-4^. -- ---- /v/J 7 * Sftrs/>~ Ww<--j'Tc ^*r r^.i/ je-/ -2_jyjry7 -- --Laa.u, . * 30.SI - 31.tt &ui>lm,<.(,}&i, t-fr-y. ffl 1.0 /o l-o -- / o 10 -- h*<J Iom4 fcxJ emot l'v "TV* F*.<*eTil (iecou.y oiny be eC, tr (v. fat-up &~t*SUjl Ld'Mi*..* N Cone..l.^!(^^ Cone.; jiil (KNWItM HONS 024079 rT/' CIV m LABORATORY CHRONICLE: OC-MS Oapartmant OATE --3/lljtt -... - SHIFT-- FRACTION____ K. J - - INSTRUMENT _ * ................... TUNE FILE___ SEQUENCE FILE xXX rn ii METHOD FILE _ A> 4C ID FILE___ ANALYST(S) i STANOAfiO CAOPNMC LOT MO bi*TVf i?-- ___A^Xid'$t4,_ t . _-- *> 4 cCr.mtl >* 5ST. . c-'O AiV i>naar*7if-<y. ___-ES?a*EZ//aA*jvAj-lJf.Eus-.:._._. _-- . . JL^_... IIfnltffVvsYl*f (*|Atl IMTuUJ CUftMNT CMS 9IATV9 tTANOARO* UAOATCO im|__$. *11 j/ji fiL-x ----.... ----------- . _______ ____ ___ __ _ . , ...... WOT i \,l - .. - . V-- -- KAMI OATA mi c Alt mi Mi TAW# tttCIAU (WWTIATO KM m JtsrTff . XASk 2_ l r^\ It TJiSI i _fk.v_.tij__ *_ -- C rcST V r tt to s~ zjyil u J?fTjt____________ 1 -- Dcnna jtJLUi .. / 1 CllrtX tO II -WMl- - __ lmzh9M . LHMSfl kit HiA SiJibX - rMf rsifo It -** IV <> LL3iSA ____ um._____ U?/i rj*ni UhJJr., -- TJjfJ n. n '/ -- - - - -- ............ -- -------- - -------------- ----------- - ---- SA &A ---- SA -- ---- > y y -------------------------- ---- J.----------- -- -- -- -------------------- ---------- -- HONS 02AOBO ETC l||MC M LABORATORY CHRONICLE: GC-MS 0p*rlmnt (''' SHIFT____ FRACTION__ /S/'l' ....... INSTRUMENT ... ...... Jr _ .. . TUNE FILE__ , fllJEllJ SEOUENCEFILE_ KVl/ ... . . METHOD FILE 3>*?F - /Ku3C... ANAIYST(S>_ SUPERVISOR'S**-^2 BATCH n_ki YJJS/j '` / -Z l*LUU MtTlAU CVMSNT CSM STATUS STANDARDS UAOATIO ACO ATI T NAIffC DATA IH. MLJ AIS xr7T:nj&& KEfcatf i*YW >r\HJ >?Jl / i _I >1-A>te -- _ V___ >nyn r b/Mf*-jkM;4kfr. >EiS2L Mn/UiM.dt/SfL >P' H 7 r _X3x//.#..... . >EVC i- Ilf/2. >P-ii2L L <3/7a >E}?> _ L M 2_____ >F Wt ?FjZ*7f_ u St)%2 >FCifo _ t/ofjb_____ ,, >FClH l r//>2 >k(jh $/) >F3fl _ bt'*?,/72 >-EUl _A . L <tJ<rf2X tn. T*'Ah//ij2u >1 J/2_ /}&/' >fC3fi t- 7/f*>* " >F3f1 L (MM 7*)/'r# . _.y___ I'l 73... .&_ /r /A n n X- JJ n 2i *_ TARSI ? SKOALS (WRITC A-TVK) . _________ < i* .................................. / f7-?J </. 1 ?bj7 T/>j ._ I '1 .... t~ - j . . -^A ^................................... --- - - , {--..................... " - Af`Zt ........................ - - HONS 024001 v> TC'ii>M!l*eMr#<i>0N LABORATORY CHRONICLE: QC-MS Dtpinnmmitnntt DATE. FRACTION____ . INSTRUMENT__ TUNE FILE- . SEOUENCE FILE___ METHOOFILE_____ ID FILE _ ANALYST(S)___ . SHIFT. .F SUPERVISOR/Stak- BATCH //*//. _ _ S iv ?" 7 AIAM Mlfu CUMINT CMC CTATUC TAN0AAD* UPOATfO CONC LOT NO. lot VOL Ml *ti w* t MAMK DnAuTA mWL Atlt >FWI ir U+ZtfiZ -- L ii/ij >F(Jti L tl/Sl >F(ltr JU U (U./2 >f(iK z* __L ___ >Fi\tb ...- \_ i!_ OIL TAM (WfMlfTCI AIATUTN) nUmN &FtU> ---- S& / -..... ........- ---- -- --... ------ - ---- -- -- .. -- ------ -- ------ --- -------- __ ____ ... ` ' - - -- - ----- -...- - - RONS 024082 ____ CT/"* tNviKOHnemtL t-- CIV tuim k* cenitfKAvoH LL 14ISO LABORATORY CHRONICLE: Department SampleeJ. 11 t 1.1195 Hg Prep AA/ICAP Prep^^jo Chemlel ysviL .MstuL ^fba Dele -V/jv/k, LebSupervleor-------.................................................. . Oele_4j4^fJ' Rons 024083 ETC ENVIRONMENTAL ____ TESTING AM CERTIFICATION * Technical Report for MONSANTO COMPANY 600 N.LINDBERGH BLVD. R3B ST.LOUIS, MO 63167 CM/A tf CNMMir Ml ElWilM Iff ire Ml MAMfMIMI IMNNI, AlMII M? I T9 kre **#/ MONSANTO COMPANY MONCOftPCNO 9 990214 *4C/fy ttmptt Mm Dxt T/im >'K tttmuO NmM i< r I5PI',i*vim ftre'MM e* UXCSTop** Oeie ner<*jfer>< fM MfUTAN CtNTfH PAAAWAV tf0f*O*. HJ 04437 <*1j ill StfW -- HONS 024084 MONS 024045 I--ETC lt$riNG $na CtMtflCATlQN Appendix A Mass Spectral Data for Quantitated Compounds 1) A total ion chromatogram for aach sample analyzed by a GC/ms instrument. 2) a Ouant. report used by the analyst to determine Qualitative ano Quantitative results of the compounds present. 3) A mass spectrum and a reference spectrum for each priority pollutant compound detected m the sample. HONS 02*0*6 `f V l. 4 - C, > -A- V i- 4 ; it : u-. !!t .......i ;; c i. i K* t- ' 'V. 1.:' U g ti.. i _ * s&->*vi rs * * HOMS 0240*7 t : l vino l 14. yn 1 H 1 'jfifif At t t '** o . ; <f ''.> 4. / .. jy ' <* /vy ' r> > e v-.y* i:, YdV -if.'. 3 i..-t .1 4 1'fet .i- -i ass1v !' - f .. j : * i ;.* L*. r.- no t>c& "feurtcl C f |f ' sliettt. i*r 41 acjvf }hi-a> HONS 024088 /* CC1T1//t trHesVrIi*N0f*lMsniNtf TC*ELRTIFICATION " Technical Report for MONSANTO COMPANY 800 N.LINDBERGH BLVD. R3B ST.LOUIS, MO 63167 CAR/* / CiiM)r Ml Aq/rtf f*f (TC Ml tfNMfMMif tf< IwM W, iMQNSANty COMMIT J"" OM|M8)f HQNCMPm * W MflU limMMiit Pit Km ****$ V/# T^.f amm h ar tNttf|*Nn>t venerate# r IOCHtm* ftn wre)xin lelM't tH lUAilAN CtNTt* PAHKWAf tOSOH. HJ OBtJT (UU125SMO----- i J HONS 0240*9 PTA tNVIHONMiNlAl C/v USTINOV CtATlflCATiON TABLE OF CONTENTS Introduction Table 1: Results and Quality Assurance Data Table 2 Method Performance Oats Methodology QA Protocol Report Appendices Appendix A - Maes Spectral Data lor Quantitated Compounds Appendix Cl * QC/MS Subsidiary Data - Blank Chromatograms Appendix E - Chain of Custody Forme MONS 024090 CT/N tNVI*OHkltN7AL ClVf TtSTlNQ trta CfATlflCATlON introduction This report contains the analytical results on your soil sample. 57 66/05'i4. ft 'S designed to include comprehensive data from the entire analytical process m order to satisfy the needs of venous levels oi review The resets obtained from your sample are presented m tabular format immediately following ins introduction. Quality assurance data is tabulated along with the appropriate sample results tor verification. Depending on the analyses ordered, the Quality assurance data may include results from blank, spiked blank, spiked sample (i.e. matrix spike) and replicate sample as wen es results from surrogate compound analyses. Quality assurance data for verification of proper instrument performance is ai$o included where appropriate The report appenpces include the cnam of custody record for your sample and. where appropriate, the gas chromatograms and mass spectra. The procedures used m the analysis of the sample are described in this report's metnodoiOQy section, am analytical procedures withm our laboratory art performed within a strictly enforced Quality Assurance Protocol, a description of this Protocol is included m the report Results Sample results, and associated quality assurance data, are always tabulated in one or more oi tins report s Quantitative Results Tables. The format of each table vanes with the class ot analysis Arrerffy Ao/rvfiftfi The priority pollutant compounds snd elements ar listed with their NPDES (National Pollution Discharge Elimination System) numbers, snd the Method Detection Limit (MOL) published m the Federal Register. Whan a compound or element is present below its published mol it te reported es BMDl (Below Method Detection Limit). When e compound or element is not present et any detectable concentrations it is raoortad as NO (Not Detected), mdls for pon-aqueous matrices ere bated on USEPA published MDt's but are adjusted as per sample weight. Matrix spike end replicate analyses, where included, were performed on samples randomly chosen withm each quality assurance batch and ara therefore not necessarily spikes and replicates of tNs report's sample Surrogate comoognd recovery data ano instrument calibration data are included >n the Method Performance Data Tables. 024091 HONS HONS 024092 HONS 024093 ETC TABLE 1: QUANTITATIVE RESULTS aiuf QUALITY ASSURANCE DATA BASE/NEUTRAL COMPOUNDS OC/MS ANALYSIS DATA (OR03) . CftohtfAwtotfyOsu to*** >TC tot# IT I* HONMWTI CBfW N laili *. tmrm, erB#i --i?TTT~ I i/M 1 , *( imu * fI MbimI [ NBRBClt rMlKBAB .}.>.4)p|rrit iMfiwrMl MfitrllilMMlilMM* H'|UrM4|B|lkylW|M N'|il(tls<i'li*TrM|ilialM lltlriimskMiilislH I liTtMililirikMiMi MMDM*NO IT Mui rM||lir lli NM It*. | NM I r! J TTBiTiliiT eirsr im isiM llui K Mlrii tiii; IlMl ftlli CM#M4M4 . /! twu ( H/k| << H/*! 1 )TM TTM KM ID sTO i ID #3 llff 3m $2m ITtcI ID . HONS 024094 HONS 024095 ETC TABLE Z METHOD PERFORMANCE DATA Surrogate Rocovory Soil - GC/MS Dote (OR 20) ' SiKlliiMli MOlrn(M OMOWII-------- 111*6 homsakti Cmrutf HMCMron w win IK 1*11 fc. I*#tt ttcllltt IttN Hitt Hit Iim 'Ififi* n 1. >Mt YOLMItf FRACTION UliMi'N R*lrOftOflr0RrA l.}-0MMoroolhM-D4 ACID FRACTION hwool-M MIiwhIiimI 2.4 .#-T UrM*D**tM1 MSf/WlRAI FRACTION MImfNIiAmiiI Tir|fcM|flaDM *MM *#* 9 iHHIff . . 100 03 10# 00 100 in M 70 00 70 M 40 (Mlrtl IMU * l*yr Rooor * 00 10# to 100 to 100 20 MO 20 M0 10 140 20 14# 20 140 20 ISO -- HONS 024096 TABLE 21 ffTHOD PERFORMANCE DATA (QR22> GC/'MS Tuning Data - Dscafloorotrtphanylpho#pin# tOFTPP) for Acid# An#|y# ''* 51 68 69 ?0 12? 19? 198 199 2?5 365 441 442 443 ion Abundanca Crt#n# % R#I#ttv# Abundant# B## Appropriata Pask Paak Status 30*60% of mat# 198 La## than 2% of nas# 69 (rsfsranca only) La## than 2% of mas# 69 40*60% of mass 198 Laaa than 1% of mas# 198 6a#a paak, 100% ralatiua abundant# 9-9% of oat# 198 10-90% of mass 198 Graatar than 1% of mass 198 0-100% of ma## 449 Graatar than 40% of mas# 198 l?-23% of mas# 442 48.92 .95 52.22 .23 4?.25 0.00 100.00 6.94 20.4? 2.33 9.10 55.89 10.99 48.32 1.81 52.22 .49 4?.25 0. U0 100.00 4.94 20.4? 2.33 82. ?4 55.89 19.6? Ok Oh Oh Ok Ok o. Ok Ok Ok Uk Ok Ok Ok In jac tion 0#tI Injection Tina: Run No I Sp#etrun No: 03'31/86 14:59 > 17462 662 An#ly#t: Proc##or t QC Botch: Samp la#* L2iaffJU*i2HLLThH'i .LSZHfi. UOm.,U3i ..u32i u-3?i_ MONS 024097 TABLE 21 METHOO PERFORMANCE OATA <0R2J) GC^MS Tuning Oete - DecefluorotriphenyIphoepme (OfTPP) for Beee/Neutrel Anolyo le Ion Abundoneo HlXf Criteria H Reletive Abundence 8a.a Appropriete Peak Peek Stotuo 6 o o j6 91 68 69 70 12? 19? 199 199 279 >69 441 442 443 70-608 oF meat 198 Loot then 2fc of meeo 69 (reference only) Leee then 2H of meeo 69 40-608 eF M 198 Loot then IK of meee 198 Beee peek. 100* reletive ebundence 9-98 eF Mae 198 10-308 eF Mae 198 Greeter then 1H of meeo 199 0*100)1 of meeo 443 Greeter then 40)1 of meeo 198 17-238 eF Mae 442 50.74 0.00 52.21 .26 49.40 0.00 100.00 7.32 22.40 2.43 10.56 74.07 13.79 50.74 0.00 52.21 .90 49.40 0.00 100.00 7.32 22.40 2.43 76.75 74.07 18.57 Ok Ok Ok Uk Injection Oetei 04X01/86 Injection Timet 00t41 Run Not >F63?4 Spectrun Not 400 Aneyett^^Mte4*rfv , QC Batch i ,. Same 1a. i UiViS-LtlMl ,19<W U*i>$, V MONS 024098 tNvmoNkttNTAl l\s TttTINO / ClATIflCATION Methodology tor GC/MS Analysis of Priority Pollutant Compounds The rnethoos employed m the GC/ms analysis tor pnonty pollutants are astonished EeA methoos Pigio compliance with the instrument parameters and performance criteria of the published methods was achieved in some eases, the precise amounts of sample used end t*e sample handling procedures vary with tht complexity pf the aampia matrix. Qualitative identification of the priority pollutants was performed using the relative retention timet. the relative eoundance of three characteristic ions end the abundance ratios. The entire mass spectrum was reviewed to confirm each identification. Quantitative analysis of detected compounds was performed by using a response factor generated by a major characteristic ion of the specific compound and an internal standard. Compounds, m soaoion to those on the priority pollutant list, were identified through a computer-aided search of the nBS-EPa spectra iiprary. After review the identifications are included m a separate tabulation end labelled `tentatively identified'. Atm. $*tt/Ntutrl Atttltm* Arlttlty Atliutt/M For the analysis of the Acid. Base/Neutraf and Pesticide priority pollutants m e $0*1 matrix, a modification of EPa Method 625 was used. The method can be summarized as follows a 30 gm semi-wet son tempts is soxhiet extracted with a tt mixture of acetone and hexane Tne acetone is thermally etrippeo. The remaining hexene extract t diluted to 200 ftf with methylene chloride and twice extracted with an aoueous NaOH solution foiiowao by an extraction with detonate water. The methylene chloride extract is onto eno concentrated to e t mi final volume. This concentrate is injected into e GC/MS instrument configured for the analysis of Bese/Neutrei priority pollutant compounds. The remaining aoueous extracts ere combined end the pH adjusted to a value less than 2. The aoueous phase is serially extracted with 3 anquots of methylene chloride. The methylene chloride extracts ere dned. concentrated to a t mi final volume. The concentrate is injected into e GC/MS instrument configured for the analysis of acid extractable priority pollutant compounds HONS 024099 rTA tNVtHQNHtNTAl CIV T$7N0 !> C*A7>A/CA7>OW Methodology for Analysis of Metals 40l/(0</* The determination of mete's in aqueous samples rs performed according to tht methods published by CPA m "Methods for Chemical Analysis of water and wastes' EpA-600'4-79-020. March. 1963. end the Federal Register. October 26. (993 Arsenic selenium and thallium are determined by furnace AA; silver, aluminum, barium, beryUHm boron cadmium, calcium, chromium, copper, cobalt, iron, magnesium, manganese. moiybdemmC rucheT lead, sodium, antimony, tin. titanium, venadwm. and zinc art determined by ICP amission spectrometry, except where lower levels of detection ere reouired: m these cases (eg lead m groundwater monitormg samples) furnace aa is used ah furnace aa parameters are run cy method of standard additions. The determination of mercury it performed by co>d vapor aa iP TOXICITV The determination of metais in aqueous CP Toxicity leachates is performed accorong to the methods published by EPa m "Test Methods for Evaluating Solid waste* EPa $w-646 revised April. 1964 end the Federal Register. Oct. 26. 7963. 7979. Sever. arsenic, barium. ce**um chromium, lead and seitnium art determined by ICP emssion spectrometry. Mercury is determined using cold vapor aa For leachates that ere organic m nature, the analyses ere performed according to the methods described under ou/su/ooi below. SOU/ttOtVtNT The determination of silver, beryllium, cadmium, chromium, copper, nickel, antimony, lead end zinc in sediment temples is performed according to methods published by EPA w\ interim Methods for the Sampling end Analysis of Priority Pollutants in Sediments end Fish Tissue* EPA 600/4-61-055. October i960. Mercury is deternvned according to the eedenent method pifththed by CPA in "Method for Chemical Analysis of Water and wastes*. EPA $00/4-79-020. March 1963. Arsenic, selenium end thallium ere determined by furnace aa using nitric sad in s closed decomposition vassal for sample digestion. ou/stuooc Tne determination of sitvar, aluminum, boron, barium, beryllium, calcium, cadmium, cooper, chromium, cobalt. iron, magnesium, manganese, molybdenum, sodium, ntckst. lead, antimony, tm titanium, vanadium, end zinc m eiudge/petroieum-baseo temples is performed by ICP emission spectrometry usmg e magnesium ntrate dry ashing dotation technique, atsame, eetemum eno thallium art determined by furnece AA using mtnc add m e closed decomposition vessel for tempi* digsstiufu Mercury is detenwnsd by cold vapor aa usmg the asms digestion teenraque HONS 024100 ETC iNVmONMtNTAt TtSUNQ A0 CtHTlfiCAUON Summary of Quality Assurance/Quality Control Procedures (QA/QC) ETC oases its Quality assurance protocols on the following government guidelines . 'Handbook for Analytical Quality Control w water and wastewater Laboratories*. EPA-600/4-79-019. March >979; . National Enforcement investigation Center Policies, end Procedures manual' EPA-330/9/7g/00f-ft. Octooar 1979; . the recommended guidelines tor gpa Methods $?a no 62S. (Federal Register. Decemoer 3. >979; uodatad on October 2$. 1964); . -Manual of Analytical Methods for the Analysis of Pesticides in Humans sno Environmental Samples." EPA 600/6*60*03$. June i960; 'Determination of 2.3.7,6-TCOO n Sort and Sediment" EPA. Region vit. Kansas City. September 1963: . Organic Analyses. Mufti-media. Multi Concentration-iFB wa$4>a2$?; and . Dioxin Analysis Soit/Sediment Matrix; Multi-Concentration, Selected ion Monitoring with Jar Extfetion Procedure-IFB WA64-A002 However, w# have modified our protocols to provide a higher level of OA/OC than tha guKfennes require For example, we analyze e higher than required number of quality control samples and we pay especially careful attention to the certification of the "reference standard" compounds we use m analysis Below are listed the kay QA/QC aiements for the methods we used Anaiyaia of Volatile Organic Compound# by Gas Chrematography/Mae* Spectrometry - Each batch of 13 samples consists oi 9 customer samples (at a maximun). one blank tempi*, one spiked blank, one spiked sample and one replicate sample. This amounts to a 30% Quality control factor. Three surrogate compounds are added to each sample n the batch of 13 - a blind qualify control sample *s introduced to the laboratory for analysis on a weekly basis - Each GC/MS is checked and retunea. >1 necessary, at thabagnning of seen day to ensure that its performance on bromofluorobenzene (BFB) meets the EPA criteria - a calibration curve lor Quantitation is prepared using a mixture of volatile Organic Priority Pollutant "standards* at a minimum of 3 different concentrations ana using a mixture of 3 internal standards at a constant concentration - The calibration curve is verified With a m>vture Of priority pollutant standards every day if the response lectors vary greater than 25%. the instrument must be recalibrated. Analysis of Organic Compounds Extracted in Acid or Base/Neulrei Solutions by Gas - Each patch Of 20 samples consists Of t6 Customer samo`S (at a maximum), on# b'anw sample one so<i ec warn- 'to* water matrices' one sample so^ed with the priority pollutant standard mature ano a Ouancate customer sample This amounts to a 20% Quantv control tiC^O' HONS 024101 rTA iHVifiOHMINTAi ' C I V/ r<J7/W0 /> Ct*TlflCA7lON - tiv66 surrogate compounds are aooed to each sample m the oatch for SaserNeufrai anaiy&s , - Three surrogate comoounas are aooed to each sample in the oaten for ado anaiys-s a oiind Quauty control sample is mtroouceo to me laboratory tor analysis on a w*euiy oasis. - Each GC/ms is checked and retuned, if necessary, at the bey-ming of each oay to ensure that its performance on decaliuorotnphenyiphosphine (DF7PP)meets me Pa criteria. - A calibration curve for quantitation is prepared using a mixture of standards composed of either the Organic Aod or Base'Neutrai Extractable Compounds at a minimum of 3 concentrations ana us*ng fie internal standards for quantitation. Analysts of Metals Ml samples - New standards are prepared for each patch of samples * Normal calibration is performed us ng a blank sample and four standards mat nave been through the sample preparation procedure, a regression analysis is used to construct the calibration curve - ad EP Toxicity samples and an sampias determined by furnace atomic absorption are calculated by the 'method of additions'. - For each sample analysis that requires the use of the 'method of additions' technique three point calibration is performed using U S. EPA "Methods for Cherrecai AWySiS 0* water and wastes. 1979'. Results are obtained usmo linear regression analysis Any regression with a coefficient of correlation below 0.990 is considered suspect, necessitating review of calibration data or samote re-anaiys*. - in constructing the normal calibration curves the lowest concentration fevers we use ere values greeter than or equal to 5 times the instrumental Detection limit OCX.). - ad calibration standards are analyzed m duplicate, at e minimum. - independent reference standards are used to check the accuracy of cetibretion standards. - a check standard is analyzed every ten samples to validate the normal cei*brt>o^ curve. - One customer sample out of every ten is analyzed m triplicate timpitt (*eppt f* V'Cvry Miylt) Samoies ere analyzed <n batches of 30 or less. For ostchts m which the samote matrices art homogeneous, the QC program is a minimum of 25% and consists of analyzing - 3 set* of triplicate analyses. - 2 Pepncate spikes. - i independent reference standard; a Calibration standards (processed usmg the sample preparation method); 4 Calibration standards (without sample preparation); and - i Reagent giant MOMS 024102 ffA fNVI*0NkliN7Al C I V 7i$HNQ CtnriftCAflON *rroft/>fo</ S9mpi9t (9*C9pt tor Af*/e4/ry*fl*/y,; Samples are analyzed in Patches of 30 or less. For Patches n which the sample matrices are heterogeneous, the OC program is a mmmum of 3S% and consists of analyzing 3 sets of triplicate analyses; - 2 Recreate spikes: - 1 Replicate independent reference standards; - 4 Caiipration standards (processed using the sample preparation method): - 1 Procedural Blank; - 4 Calibration standards (without sample preparation), and - t Reagent Blank. Anttytit pt Mercury To analyze samples for mercury w group them py matrix in patches of 30 or less Our OC program <s a minimum of 30% and consists of analyzing. - each of tha 30 customer samples m duplicate: - 3 sets of triplicate anayises; - 2 Replete spikes; - 2 Replicate independent reference standards; - 10 Caiipration standards (processed using the sample preparation method); anp - 2 Procedural Blanks. Analysis of Pesticides^ HerbicidMandPCBs by pee Chromatography Pesticide, nerbicide end PCB samples are grouped tn patches of it customer samples or less according to the type of enefyeie to oe performed. The OC program for aach of these three types of analyses >s a rmmmum of 20% end consists of analyzing - t procedural dank sampie(a reagent blank is analyzed n the case of non-water matrices); - i spiked blank sample (the spiked blank is eliminated m the case of non-water matrices); * t repucate sample; - i replicate spiked sample; eno - t known refemece OC temple for at least each too samples analyzed Tr>e instrument -$ cahorated each run with lives standards, and Checked every to samoies Analysis of Cyanides. Phenols. Fluoride. Chloride Nitrate and Nitrite - a.- parameters are analyzed using a Teem,c~r Autoanaiyzer u O'. - : c# lira*.standards are ana'yred a: ti-e oes-nmog anc e^<j 0r eac* te'-r- MOMS 024103 pTA tNVlMONMiNTAt C fv TfSTfWO CiMlHGAJtON - Each batch (up to 60 samples) consists of analyzing one blank, ona p*to bem 0<- Oucmcata ana spiked sample every 20 samples, and an EPA known reference san-pte Analysts of Total Organic Carbon (TOC) TOC samples are analyzed on a daily basis with the number of samples analyzed per oay daoenoent on the request for duplicate or quadruplicate analyses. The Quality control proyam is designed to maintain the appropriate amount of OC and consists of the following elements Oeuy instrument calibration - One Dienk Standard reeahbration every to samples Spiked samples at a low and high level - Every sample is run in duplicate st s minimum Analysis of Total Organic Halide (TOX) - Blank reagent water for absolute carbon backround must contain lass than S ug/i of haiioa (as chloride). - usmg a tncNoropnenoi standard, the mean adsorption efficiency must be withm */15% of the standard value. * Calibration standards are run avsry 10 samp's*. * Every sample is run in duplicate at a minimum. Analysts of 2.3.7.6-TC&0 (Dtoxtn) by PC/MS (SIM) Each temple is dosed with s known Quantity of 13Cj2-2.37.6-7CDO as internal standard and 37CU"TCDD as surogats standard. The action iimts for surrogate standard reamta is /- 40% of the true value. Semoiee showing surrogate standard results outside of these lirwts ere reextracted end reanalyzed. - Two laboratory `method blanks* art run along with each set of ke or tawsr samples The method blank is also dossd with ths internal standard and surrogate stanoaro - At least one per set of 24 samples is run in duplicate to determine rntrataboratory precision. - Qualitative Requirements- The following ere met in order to confirm the presence of native 2.37.6-TCOO: a. isomer specificity must be demonstrated initially end verified once per 6-hour work shift. The verification consists of injecting a mixture contammg TCOO isomers which sluts doss to 2.3.7.6-TCDO. Ths 2.3.7.6-TC00 must be asperated from interfering isomers, with no mors than 25% valley relative to the 2.3.7.6-TCOO peak 0. The 320/322 ratio within the range of 067 to 067. c. Iona 320. 322. and 257 are an present and maximize together the signal to mean noise ratio must be 2 5 to i or better for an 3 ions. d The retention time is eauai (withm 3 seconds) the retention time for ihe isotocwceiiy labeled 2.37.6-TCOO. e At least one of the positives can be confirmed by obtaining partial scan scactra from mass tSO to mass 350. The partial scan guidelines are as follows MONS 024104 CT/\ tNViHONMlNTAl c I W TttllHQ Cg*TlfifCAT/ON . the 320/324 ratio shouio be i.56 +/- 0 . the 25^/259 ratio should be 1.03 4/- O.tO . the 194/196 ratio shou`0 be V54 /- 0 iS * One sample >* spiked with native 2.3.7.6-TCOO at level of 1.0 PP0 (for soi) for each et of 24 or fewer semoies. - in cases where no netrve 2.3.7.6-TCDD >s detected, the actual detection i*tmi is estimated and reported based on a signet to noise ratio of 2 5 to t *t tons 320 and - For each sampit. the interne) standard is present with et least a K) to i signet to no*se ratio tor both mess 332 end mess 334. Also, the internal standard 332/334 rat>o mu: be within the range of 0.67 to 0.07. Subcontractor QA/QC Eecn luocontrectoer is required to maintain an appropriate level of duality control. To msurt ths. each subcontractor >$ reduced to submit to ETC the duality control data for an analyses it performs. This date is Kept on fue et ETC n general, the amount of Quality control rtouteds one duplicate sample with one spiked sample for every ten analyses. jhem-of -Custody The cham-of-custody procedure is pert of our Quality assurance protocol We believe our chem-of'Custody record fully complies with the legal requirements of federal, state and local government agencies end of the courts of tew. The record covers: - labeling of sample bottles, pecking the Sample Shuttle and transferring the Shuttle unoer seal to the custody of a shipper; * outgoing shipping manifests; * the chem-of-custody form completed by the pereon(s) breaking the Shuttle sea' taking the sample, reseating the Shuttle and transferring custody to a shipper. - incoming shipping manrtasts; - breaking the Shuttia's reseai; - storing each labeled sample bottle m a secured area. * deposition of each sample to an analyst or technician, end ~ the use of the sample m each oottie m a testing procedure approbate to the intended purpose of the sample Tne records show for each link in this process: - the person with custody: end r tne time ana aete each person accepted or relinquished custody. HONS 024105 CTA INVIfiONMiHTAL c I V T#*T/W0 Ci*TlflCAT/OH Appendix A Maes Spectral Data for Ouantltatad Compounds 1) a total ion chromatogram for tach sampia anaiyzadOy a GC/MS mstrumant. 2) A Quant raoort ustd py tha analyst to datarmma quaiitativa *>d ouantitativa rasuita of tha compounds prasant. 3) a mats tpsctrum sn<j a rafaranca apactrum for aach priority pollutant compound da tactad in tha sampia. MONS 024106 total low c*0naT09*H Oct* FlII >136641IU7 Nam*i 860331 ACID I niaci L7199A ,QA4747,5,31.99,1 Id Filai IACID11US Tit la i PP/-ACID IOF1LE Laat Calibration! 860731 14192 Oparator ID: JH2160 Quant Tima: 860331 17:39 Injactad ati 860331 17i02 BTL# 9 HONS 024107 QUANT REPORT Operator ID: JH2160 Output Fi1* *13664*lAQ Data Filai > 136641U7 Mini 860331 ACID I Ml.cl 17199A ,QA4747,S,31.99,1 Quant Ravt 5 Quant Tina: Injactad at * Dilution Faetort 86U331 860331 8TL 9 17:35 17*02 1.00 ID Ftl.l IACIDllUS I 11 I I PP/HCIU I DM LE L.. t C.libr.tioni 860331 14192 Compound R.T. Scan# Araa 1) d4-l,4-Dlehlorobansana 6.18 >> 2-F luorophanol lSURR > 4.17 H -8riwrophtnol ----- ---------- (SURR) 4.37 8) Phono1-D5 (SURR) 5.63 id d8-Naphthalano 9.25 17) dlO-Aeanaphthalana 14.46 24) dl0-PhananlKrona 18.91 29) 2,4,6-Tr tbromophano1 (SURR) 16.89 28) d!2-Chryaana 27.03 175 62 ?3 144 348 641 892 779 1349 36478 54499 -------- *98 66909 77959 32493 55542 17427 29131 Compound ia 1STD Cone Unit* 40.00 UG'hL 90.15 UG'HL - 1 rOl 83.11 UG/PIL 40.00 UG/ML 40.00 uG/m 40.00 UG/ML 113.12 UG'HL 40.00 ug^ml cs Hit q 9 4, *: y* 9 9'. 9< y* 10: HOMS 024108 O.t. Fil*i >F6390:iU2 Nihi 660JJ1 #F B/NtPEST Mi.ei L?195B,QB4?4?,S,J1.99,1 Id Fi1st FBNP: MJS Tit l*i B'NrPEST It> FILE ____ FOR F L*.t Caliorttiom 860401 12>U> Op.r.tor 10: RAO15? Ou.nt Tin.: 660401 20>26 Inj.ct.d 6ti B60401 19iJ8 890326 B7L9I4 HONS 024109 QUANT REPORT Operator ID: RA0157 Output Fila: aF6390mAQ )ata FiUt >F6390* IU2 <Jama: 860731 #F B^NOPEST liac t L7i958,Qe4747,S,J1.99,l Quant Rev: 5 Quint Tim#: Injactid t: Di lution Factor * 860401 20:26 860401 19:38 1.00 BTLI24 ID Fi!: FBNPitUS Title* B/N*PST ID FILE ____ FOR F .eat Calibration: 660401 12*03 850326 Compound R.T. Scan# Area Cone Unite 1) d4-1,4-0ichlorobenxene 6.90 12) Nitrobanzana-05 CSURR) 7.92 249 329 18099 25391 40.00 UG'ML 39.17 UG-'HL 18) *d8-Naphthalana 19) 2-Fluorobiphenyl *3) dlO-Acenephthalana >8) 2-Chlorenaphthalana tSURR) 9.76 433 73275 13.11 622 61804 15.08 733 46487 I****------ 649--------- 1985 - 40.00 UG'ML 35.03 ug^hl 40.00 uG'HL -1.47 UG>#tL 61) 2,6-Dinitrotoluene 14) dlO-Phananthrana >9; 46 --73> --------5675-- -48.77U8t*ML 19.64 990 99920 40.00 UG^NL >B> Phenanthrene 19r69 -- 993- ---2616 - --Ir93 UG^tlL 19) Anthracene 19.69 -'993- - 8616 - - -*rt t>U SI) F luoranthena 24.36-19*1- 116410----- 93.51 -U&'HL S3) Pyrana 2*rG--1254- -1*6410 101.08 UC^HL >2) *dl2-Chryaana 27.84 1451 17811 40.00 UG'NL >5) Endoeulfen I 34) Tarphanyl-D14 U) Butyl benzyl phthaleta 24.30 1852 4mi 156.82 uc^hl (SURR) 24.90 1286 25927 23.90 UG/ML 29-r94--*949 --------1681 - - 9.21 UC'WL ?0) bia(2-Ethylhaxy1)phthalete 24. 2* -1474 -- *931 -- - 4.-82 UG^ML >0) b ie(2-Ethylhexyl>phthelate 2*r44--1483- ------- 375* - -30.40 UC-'HL q 96 80 93 97 95 68 86 9* 2 80 82 82 108 61 94 73 92 94 Compound la ISID HONS 024110 I--ETC tNVmOHMtNfl TIStINQ ** CitrineAT ION Appendix Cl OC/MS Subsidiary Data MOMS 024111 TrTOL fOH CH0(*aTO*ON Data F i la i >1366)1iu? Nanai 8603)1 ACIO I riiae 0C4747A ,QA4747,S,1,1 Id Filai IACIOilUS Tillai PP/ACIO IOF1LE Laat Calibration! 840331 14i$2 Oparater IDi OH2180 Ouant Tioai 860)31 16>2 Injactad at* 8603)1 16>19 B'L* 8 HONS 024112 QUANT REPORT Operator ID: JH2180 Output Fila: "136631:AQ Data F:la: >13663::U7 Nemo: 860331 ACID I fliac: QC4747A ,QAa747,S,l,1 ID Filai IACID::US Tula: PP'ACIO IDFIlE Laat Calibration: 860331 14:02 Quant Rav: 5 Quant Timi Injactad at: Oilution Factor: 860331 16:$; 860331 16il 1.00 BTLI 8 Compound 1) 11) d8-Nophtholone 17) dlQ-Aconophtholono 2*> d10-Phononthron# 28) dl2-Chryoono * Compound :a ISTD R.T. Scon# 6.17 9.26 14.46 18.92 27.02 179 349 642 893 1949 Aroo 39403 90499 34903 60069 18919 Cone Un 1 x 40.00 UGr'ML 40.00 UGsnc 40.00 UC^ML 40.00 UG>TL 40.00 UC/T1L HONS 024113 Date Fi la; >F6384: :U2 Nam; 860731 F 0/N4PES7 tliaet QC4747B,084747,S,JO,1 Id FiIa; FBNP;;US Titla; B'N*PEST 10 FILE .... FOR F Laat Calibration; 860401 02;06 Oparator ID; *010784 Quant Tiaa; 860401 0f;96 Injactad at; 860401 09;08 850326 BTL613 MONS 024114 QUANT REPORT Operator I0i KU0796 Output Fila : 'F6394::AO Data Fi)a: >F6394::U2 Name: 960391 F 0/N6PEST Miac: OC4?47B,QB4747,S,30,1 Quant Reu: 5 Quant Timi Injactfd at: Dilut ion Fac tor: 9*0401 09:56 960401 09:09 1.00 BTtf19 10 Fi la: F8NP:US Tula* B'NPEST 10 FILE .... FOR F Laat Calibration: 960401 02:06 950326 Compound 1) d4-1,4-Dichlorobanxana 2) N-Ni troaodima thylamina 16) d9-Nephthalana 33) dlO-Acanaphthalana 39) Dimethyl p'lthelete 54) dlO-Phananthrana 60) Oi-n-butyl phthalata 72) dl2-Chryaana 0> bia(2-Ethylhexyl>phthe late Compound i. I5T0 R.T. Scan# Area Cone Unite 6.83 249 24624 t-r-19 --------M-------- 4429 9.77 432 99791 16.08 732 41534 --?W--- 19.56 996 119392 21.99 1116 9574 27.92 1451 99921 28.41 1484 83616 40.00 UG/fl ----- 18.4. UC 'XL 40.00 UG.'nL 40.00 UG^nt ------- 6.-34-UG.'KL 40.00 UC^ML 3.24 UCsm 40.00 UG^nt 28.86 UG'nL 0 9 IQ 9 9 6 9 9 10 9 MOMS 024115 C Irr/% tNVItONMfNTAI. W tiSTlNQ t/> CitriFlCATlON Appendix E Chaln-of Custody Forms 1) A field Ch*ir-ol-Custody form (CC1) M Included for oil iinvln thlppod by ETC sfuttls. 2) An In-house sompio Chsln-of Cuotody form lo included for ell eemptee not shipped by ETC (buttle. 3) Any (ddUionel Chsln-of-Cusjody meteriM provided by e client or by ( client'* MmpAne (gent I* ei*o Included. 4) A supeontrector's Chsin-ol-Cuetody form I* Included for eny onelyticel work not performed within ETC's leborttory. 5) Andyde tnd Extreetlon Custody forme sri Included for the period the sempie w* in ETC's possession. HONS 024116 eT/t fNVlAONMKMTU CIV TttTMO M# CWtPKAVOH CHAIM or CUSTODY Company jylostnnTc,Job Ho. Addraaa Attantlon t__________ Sawpla Daacrlptlom CUSTOMER ID 6*rL * g~7 DESCRIPTION 1 A ETC z. /<?*y Z7<^ Saiapla(a) Rallnquiahad by Tina i / ' !____________ Data i Sainplt(t) Racaivad byi Tlaa i \ ' ! f___________ Data i JSHJlL V. tn ejuntju etnrie tMtwtr tenon. *j men an mum HONS 02AUV chaib or aniooy ucom wcjooio_ fo COHTAACl MMfl l^oS^ly _. ................... anioHti ocMtHoiMw _ MCCONTMCT NMAGCO U nAHiiiw oocoot _ ....................... me tuhicaoca_ <C,, u AM* (ShcIMc tafamattaa w laaplai ts avallabla m attaebaO 'Saapla Untlflcatlea laj') Tm Ultftr f UIlKtN A*H*QUIm4 fcy: ^ St|MUrii /T? \J. 7M< Kkc1*4 by: iKilid by: o*u TIm >*> 01o Iciirtt OacalaaO far Aaatjrala by: IktboO af tblpaant: A;r f*T__ ..... Ibaibar af Caatalaan; / ifIO) llllrKlHai JSaapla traurajtlM, aatarlty. Oallaary to, ate.) iir . - HONS 02*118 BTC 'liwS'I'lV'Mo"o* LABORATORY CHRONICLE: Sample Preparation Departr Ml-up: ON HCOMttN ^-tl'^VcW Cane.: ^ Jrrrr r wx. /. CiJuiu-fLf s(ttk HONS 02*119 m ETC 'iimmmu'iwo W LABORATORY CHRONICLE: QC-MS Dapirtmant date ^3/vJSL..... . SHIFT-- FRACTION____ AtJ INSTRUMENT___*....................... TUNE FILE__ iVTiWi - SEOUENCE FILE_ Zr* ** rJ METHOD FILE__ A*,4T._ _ ID FILE -FV1- .. ANALYST(S) STANOAAO CONC LOT PPM NO T'f? Vu'O __ A i 4*4 t i 5 f*- __Ar'd s' ~ fi*i ^ .&ia_ smL fiT . -. _____ __E(/Ai.,A _S____ /frV Jeo *4 /SO iaiy 1*0 f <L J3?I . _ , 1^0 . lA'Lj tot VOC --V AUIIIMTMU CMCCUMSTttANTTUS STUAPN0DAATRID0S -* - Mfl 1/Jf ** Jjj.of____ ------------- .. ----- -----.... *. - NAMC DnAuTA I1N11J AL*S Dlt TAPI* (WSMPTCSOAATITSPQ PvImSS S>rrff _ *xsks* t - A.. J c.\ ar X/k S"* / ^c-4 f.\ AT A ST .JCJkV- __ W III i VJkSS j X-tiJlL. _ V j? z.tite S" Jx.tf'/'v-' X2M.iJ-- __ (a J>fT/P________ -LBlii__ 1 ocmi'in rjtd _t 17199ft TJti3. f LhM9* to** 4? L9M9H tML / LrfitfA FJ*T fl ivavMs IJlkT n LiMM riill ;v u,im rskft> .. /<. LLil>K TJt 7*- n LllUA Ul 7J PTS7 ____ ..... ......... > SA y 4A V -- -- ------ -- -- ------- -- ----- - --------- --- -- -- -- ............... ............. ____ TC FORM tm HQHS 024120 LABORATORY CHRONICLE: GC-MS Dspsrtmsnl ./ ' '/ ^ DATEtSft't-yJ'Ml. SHIFT-- FRACTION A/4' ________ tTANOARO CROfNMC - NIOOT. INSTRUMENT F . . _____________ TUNEFILE- . ___ SEQUENCE FILE__ KV2J. _________ METHOD FILE _ FILE____ i-. x-*'- > /----------- ANALYST____ vf SUPERVISOR>&i* y?P BATCH rTUUp.) &^Y7Y?" ffji r* ----- Z6J> ,lwitrer __a-__1__________C_Jjt&l_.%F/a&_ATL*d_ZJ*tZi_**Z.4_?_c--___._--_____________.___._.___. ._a&c^oH&i __ ____ -..1_A*0A. _ -tab_ tr .. fai?J2U7 ri't/A ior vov IMMIINSTIAU CURRENT CMC CTATWC ETANOARDt UR0ATC0 - CO w* ____ Mtl BY l\ , ___ ... ' " ___- __ .. ..- _ trtcuu. (tnUTIATYFO *a3lrJ*MJk A? &/A* rJJ* ZT(Mfffi. teiMAMjr* w. g ..Liza*. A2fj t <J/7 6 t L S*/\&_______ T rjtoj _ '3i(Jrt __ fbivhyj . i_ 4 WWW _...... A' Art A. Zf'kAiiWtn. I t7/f^ LT/fs-i 1__ I t` F *nie fA HONS 024121 ll ETC'mmSiatvttm LABORATORY CHRONICLE: GC-MS Dtpannxnl HONS 024122 ETf* CNVIAOHUlHtAL Cfv nvmo nt ctmncAitOH LL iH I6(. LABORATORY CHRONICLE: Matali Dapartmant SamplaaW. _; L^U*i5 Hfl Prap ___ AA/ICAP Prap'S^a^_< Chamlat -1- ____ Oala Jf/AHlfc Lab Suparvlaor____ Datai._J /> HONS 024123 FT INVmOMUfMrAL ^ I w resriNG me ctATtficATiON Technical Report tor MONSANTO COMPANY 800 N.LINDBERGH BLVD. R3B ST.LOUIS, MO 63167 M2IS0 fTC CM* t OMI A//# f* fTC Ml MN*MlN Hmn MONSANTO COMPANY MONCOftPCItt ST N03M ....... C+*P**y _______fx/Nry Sum** MM Of ftm* *lftJrV rn lf.`r>i<| Report to tn jNS|t|**v*c* PO'tlM P lOOtl'M 0( Nepw'l Soft**** - - iH *A*17AM CtNTe* 0AAKWA7 tOi$o*. hj etnt <tei> name -- - HONS 024124 HOMS 024125 rr/N fNVimONMtNTAl CfW 1*7INQ tna Ct*7iflCA7lON Appendix A Mats Spectral Data for Quantitatad Compounds D A total ion chrometoqrem for each sample analyzed by a QC/MS instrument. 2) A Quant. report used by th# analyst to determine qualitative and auantitativa results of the compounds present. 3) A mass spectrum and a reference spectrum for each priority pollutant compound detected m the sample. HONS 024126 > *-l - t^ j? It fi j if i fc- i 1 i U*. 7 ( i I *4 3 i *i( 40 4 HQHS 024127 t-'. \ HOMS 02412A * * ':! \ I HONS 024129 MMI Biatmt HONS 024130