Document 2Q8OJdvV4y5kREOZ3GQwrXzg

I Monsanto 1056 copy/ MONSANTO NtSIANCM CONDONATION / DAYTON LANONATONY / DAYTON. OHIO 4I4D7 EASC - Dyton <01n /MCTCMt RfPORT NO.: MDA-295 Analytical IVH o9 M^oai . ftCPOAT RECEIVED jos/paqxct no. 482.5040 OATS: 5 April 1982 An'O-DAYTON Ho HAlOO COVMCD: ir'jv. riLCS m Ok T1TLI: ANALYSIS OP DECATUR WATER SAMPLE FOR PRIORITY m POLLUTANTS AUTHORS: Robert r. Ivory >U S8 A water sample from the Decatur Plant was analyzed for the U.S. EPA designated prio rity pollutants* and a number of pollutants as designated by the NPOES Consolidated Permits as Group B pollutants* Results of these analyses are shown in this report. FILE Approved by: Hobart F. Ivory _ srEnvironmental Analytical Sciencaa COPY Centor Service Project Manager DO NOT. REMOVE FROM FILE Approval date: V/r/^2- RBSTUCTED DISTRIBUTION (see over I COMPANY CONFIDENTIAL HONS 022352 DISTFUBUfJON COPV NUMBER 1 Ha Matthews 2 R. r. Ivory 3 T. J. Hoogheea 4 Central Filet 5 Technical Reports Library 1260 1260 1250 1250 R3C ABSTRACT ONLY R. K. Fliteraft-1250 R. M. Scott-1250 NOTE: Distribution of this report is restricted. Requests for additional copies should be made through the principal contact at the Monsanto location involved or the Manager. Environmental Analytical Sciences Center. Dayton Laboratory, Dayton, Ohio. ACKNOWLEDGMENT Contributions of the following Dayton Laboratory personnel to this project are gratefully acknowledged: Analyses: S. A. Barksdale J. T. Miller A. Ford D. E. Sharp H. M. Strickland HONS 022353 i. httboouctiom A water sample collected at the Dacatur Plant was subadLtted to the Dayton Laboratory for priority pollutant screening ana lyses. The analyses were conducted in accordance with the U. S. Environmental priority pollutants. |1|. 2. SUMMARY All analyses were conducted according to the procedures deve loped and recomaended by the U.S. EPA 11-51. The organic pri ority pollutants found in the Decatur Plant water sample are shown in Table 1 and Table 2 shows the applicable quality control data. Although all the organic priority pollutants listad in Table 3 were investigated through GC/MS screening analysis, only those pollutants observed in the samples are reported. None of the Aroclors or pesticides listed in Table 4 were detected above their screening levels. The analytical results for the priority and nonpriority pollutant metals, as determined by atomic absorption (AA) and inductively coupled plasma (ICP) spectroscopy, are shown in Table 5. Table < shows the quality control data for the metals analyses. Table 7 shows the detection limits for the metals concentrations. Table I shows the analytical results for the total phenol and cyanide concentrations in the water samples, and the applicable quality control data. Table 9 shows the results of analyses for a number of the Group B pollutants as designated by the NFDES consolidated permit. The Quality Control data for these analyses are shown in Table 10. 3. SAMPLE COLLECTION Samples were collected by Dacatur Plant personnel. Samples uere received at .the Dayton Laboratory la the designated spahppcoTod sampling containers. HONS 022354 . miomnr fomutmt rnntmcM. phocedupes Analytical procedural developed and racomended by CPA (1) were uaad throughout this project. Zt ia important to realito that the analyaia scheme for analyting for organic priority pollutanea la a acreening procedure, and ie therefore a qualitative semiquantitative analyaia. SoaM of the organic priority pollutant analytical methods are atill under developaient and require further verification and validation. Therefore, the data preaented for organic tpeclea serve to Identify which of the organic pollutanea were present and to indicate their general concentration ranges. The accuracy of these data may vary by a factor of 2 to 10. depending on the overall composition and concentration of the materials present. Two of the 129 priority pollutants were not determined in the project: 2,3,7,S-tetrachlorodibenxo-p-dioxin (TCDD) and asbestos. The EPA Environmental Monitoring and Support Laboratory (EMSL) recommends that TCDO be omitted because of its extreme toxicity and the potential health hasard involved in preparing standard solutions in the laboratory from the pure compound [11. and there fore, the compound is not included as part of our routine screen ing procedures. There is presently no EFA-approved method for the determination of asbestos fibers in wastewater. The analytical procedures uaad (1] divides the 129 priority pollu tants into six basic categories: volatile organics, extractable organics, metals, cyanide, total phenol and asbestos. The follow ing sections outline the analytical proceduraa and the EPAapproved Dayton Laboratory's modifications for analysing each group of priority pollutants. HONS 022355 .l Intractable Praanlcs The 129 priority pollutants contain II eolvent-extractablo organic compounds that can ho taparated by gaa chroaatographic nathoda. Extractable organica arc divided into thraa groupa (or analyaia: base/neutral organica, add erganica (pbaaola), paaticidai and Aroclors. Compounds claaaifiad aa axtractabla organica arc liatcd by theac groupa in Table 3. The analytical procedure for extractable organica ia described in Reference l. Figure 1 depicts the saaple processing scheae (or Figure 1. saaple processing achaag for the analyaia of the base/ neutral and add fractions of extractable organica. 3 HONS 022356 the baae/neutral and acid fractions. A 1-liter aliquot of the extractable organics was Bade alkaline~(pH*>'Tl) with sodls* hydroxide, and the organic base/neutral compounds extracted with ethylene chloride. The residual aqueous phase was acidified (pH <2) with hydrochloric acid, and the organic acids wars then extracted with methylene chloride. The aethylene chloride extracts, one containing the base/neutral organics and the other the acidic organics, were dried on coluans of anhydrous sodiuu sulfate. These dried extracts were concen trated to 1.0 mL in Kuderna-Danish (K-D) evaporative concentrators. The concentrates were sealed in septua-capped vials and stored at 4*C until analysis. Gas chromatographic/Bass spectroeetric (GC/ MS) analysis was conducted using SP-22S0-DB and SP-1240-DA GC columns for the base/neutral and acid extracts, respectively. Each sample was spiked with deuterated anthracene (an internal standard) immediately prior to analysis at the CC/MS. The samp1e processing scheme used for pesticides and Aroclors is shown in Figure 2. A 1-liter aliquot of the original extractable organics sample was adjusted to a pH of 4.5 to 7.S using either SOX MaOH or concentrated HC1, and the pesticides and Aroclors were extracted into a 1S% methylene chloride/hexane solution. The organic phase was separated and the saaple cleaned up by acetonitrile partition. Following the cleanup procedure, the saaples were screened by gas chronatogrsphy on SP-22S0/SP-2401 and 3X ov-ioi coluans, utilizing an electron capture detector. 4.2 Volatile Oroanics Table 3 lists those priority pollutants classified as volatile organics. The recoaaeaded aethod for volatile organic analysis was designed by DA for determining those rhea(cal species which 4 HONS 022357 Figure 2. Saaple processing acheae for patticides and Aroclor analysis. are aaenaile tu the teller purge and trap method (1). Hetactical ly mealed 4G a- glass vialt collected frea each of the stapling points were cor.posited in the laboratory for one analysis of each sampling point. Two laboratory composite solutions were prepared, one for analysis and one as a backup staple. Figure 3 is a siaplified diagran of the analytical scheae used for volatile organics analysis. An internal standard, 1,4-dichlorobutane. was added to 5 aL of the composited sample, and this spiked sample was sparged with heliua onto a Tenax-GC silica-packed saaple tube. Analyses were completed using a Hewlett-Packard SMI GC-aass spectrophotometer with a 5937 data systea. Saaple tubes were heated to 1S0*C over a 1-ainute period and held at that tcaperature for 4 minutes to desorb the compounds onto a Carbovax 1500 coluan held at -40*C. For compounds with boiling points below room temperature, cryogenic trapping at -40*C (liquid nitrogen cooling) generally provides better reproducibility of retention tine than does the suggested protocol teaperatnre of 30*C. After desorption, the GC column teaperatnre was raised at S*C/niaata to 170*C- r HONS 022358 Figure 3. Analytical scheme for volatile organic analysis. Qualitative identification of a compound was aade using the three criteria listed in the protocol (11: 1) the characteristic ions must be found to maximize in the sane spectrum. 2) retention time must coincide with known retention tines, and 3) ratios of the three characteristic masses most stand in the proper known pro portions. Quantification of volatile organics was made using response ratios to the 1,4-dichlorobutane standard. 4.3 Metals In addition to extractable and volatile organics, the 129 priority pollutants include 13 metals which are to be analyzed for under the protocol. Four metals (arsenic, mercury, selenium, and thalli) are.analysed by atomic absorption (AA) spectroscopy. All other metals were determined by an inductively coupled plasma (1C9) excitation techtaigue.* c *QNS 022359 4.4 Total Cyanide Total cyanida waa determined according to tha convantlonal oat chemistry tachniqua daacribad in Reference 1. Independent atandarda vara included with tha plant aamplea for quality aaauranca. 4.5 Total Phenol In addition to apacific phenolic compounds and phenol measured by GC/MS, total phenol was also measured by typical wet chemistry techniques (1-31. Independent phenol standards were also analyzed for quality assurance. 4.6 Non-Priority Pollutant Compounds A number of pollutants as designated by the NPDES Consolidated Permit as Group B pollutants were analyzed in accordance with approved EPA methods for specified compounds. (2,31. 1 HONS 022360 S. WfPWCB 1. Draft Final Reportt Sampling and Analyais Procedures for Screening of Industrial effluents for Priority Pollutants. U.S. Environmental Protection Agency. Cincinnati. Ohio. April 1977. 145 pp. 2. Manual of Methods for Chemical Analysis of Hater and Hastes. EPA-60014-79-020. U.S. Environmental Protection Agency, EMSL, Cincinnati, Ohio, March 1979. }. Standard Methods for Examination of Hater and Hastewater. Fourteenth Edition. American Public Health Association. Hashington, D.C., 1976. 1193 pp. 4. EPA Guidelines Establishing Test Procedures for the Analysis of Pollutants, Proposed Regulation, Federal Register, Monday, December 3, 1979. 5. U.S., Federal Register, Book 3, Vol. 45, :<o. 99, Monday, May 1, 1910. 9 HONS 022361 TABU 1. ANALYTICAL RESULTS fOR ORGANIC PRIORITY POLLUTANTS ugL (ppb) Sanple ID Analvta Extractable orqanica Method Blank CCO, 2/27/12 o V Bis-(2-ethylheyl)phthalate 190 Fluoronthtnc Pyrana <10 <10 <10 NDb Chryrene <10 ND Phonol NO <25 Volatile orqanica Methylene Chloride Chloroform Trichloroothylono Mnxint Acrylonitrile Toloono NO NO 10 <10 ND <10 <10 <10 <10 <10 900 <10 *<-Coapound was observed, but balow screening level bN^Conpound not datactad HONS 022362 TABLE 2: ORGANIC ANALYSIS QUALITY CONTROL SATA Prent Racovstv In uneli Anaivt* Mount of Soikn. uaL D,-Diehlorobenzne 100 Di-Phenol 100 D-Pyrene 100 D,,-Chrysene 100 Method Blank 16 27 61 58 CCO, 2/27/02 24 22 42 42 10 HONS 022363 TABLE 3. FRIORITT FOLLUTAXT SCREENING LEVELS CC/HS AMALTSIS or OKSMIICS III INDUSTRIAL EULUIWS Aflk J-TMGraphene) J'K.If ?>*) 9 !! 2.4*5;i*lhr Jjhawel : 4.>?rirMer9pfl*fi*l 4,1 -:.f.itio-e-e*Bol ;.4r;7:uo;NA:i - ?, leie*B- bmI h^tr!iireptiu) VS.Bt.:i l.:7j*iv,i V.*,. c- *.Br. f . -11T .s Tr'..ire f 1 .:i:*ftr4nr ;.;-:;r'.ri:v. )*;*. : .i :cM:re<tran4 Cirier. mrcriondt 4,i-2izr.l6zc}TSp*m Lisr#*crrjjr9*tn#** hr.ii'.i vinyl lllwi transfer* iersttryiiiM 1. i J,MUBs>lrMUw* ? :mm C^UiMtMtrw tlh> 1MU4M Dirwt U)tufelMi Acr*)m Arrylr.iuil kriOMBi IomI. M/t 25 35 35 35 35 35 153 350 35 25 35 K 30 10 10 1C 1C JO JO JO 10 10 10 10 10 10 10 10 10 10 10 10 JO 10 10 10 IO 10 10 10 . 10 300 100 (Mt/vmnli i 1'5-MoMovoOomom l,0-034Bl*MM-- >*irtlifMHam 1,1-ffcHnOlM-- Blat2~cBlarla*fr*pyl) tlwr nwrtlBMOmiio* 1.2.4-TrlcMnlwui>i ^iumKn Blal3*oBloroo*J>yl) nJwi OaMft>|r*nrr1oq**i oil i* lUOtSMIBI Blaf3*ehlorMCho*y) mUtM 2~Oil*r***p*tJlaf* Arvnayhclty 1 a** AeaMpfcuwn* iMfhBfBM riwtsM J>DtamBi9lMi 1.3* 5iykfBrl5y5rutM 2, -Dtiutr**lmm H'RIUMBitpiWflyllWM HtsschlBieBfMIRt 4-Bra--phawyl yMstyl lUMf CNMBtJl/tM/MtJtfaeSM Dl--thy) pktlMlBU bulky) ybOuliti riBMUtjMBt PyroM M*ff0*yl pkUBlau iMllfUW Butyl Busty! pMJiBtotf OtryitM Blal2-JiylJMwyll fkltelBU --r ,ftT`*rr>r-- --!) fl**rlatlsoag Bomo U > floornB-- BonMlaiyyroM Mm*11,2.B-atf)yyrm* MIbbi Ib.5)mUhs*w OoMoff.li. llyotyloM ^MUMBdlMthrlalM iPoltTmll o yupylia>*o -OQa*opB--jl yBoayl otBtc r T* tirtiliBoBonoUlM Pt * *0I|1 pMBlMI BOSKlClBOO M IWlWI BOtOMiOf loool. N/l 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 35 35 35 10 10 10 10 10 10 11 MONS 022364 TABLX 4. PRIORITY POLLUTANT PESTICIDES AND AAOCLOR5 Compound 6-Endosulfan a-BHC y-bhc B-BHC Aldnn Heptachlor Heptachlor epoxide o-Endosulfan Dieldnn 4,4*-DDE 4,4'-DDO 4.4'-DDT Endnn Endosulfan sulfate 6-BHC Chlordane Toxaphene Endiin aldehyde nethoxychlor Aroclor 1242 Aroclor 1254 Aroclor 1221 Aroclor 1232 Aroclor 1248 Aroclor 1260 Aroclor 1016 GC/MS Screen, Pd/L 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 GC/EC, pq/L 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 12 HONS 0223*5 TABLE 5. ANALYTICAL RESULTS FOR PRIORITY AMO RONPRIORITY METAL POLLUTANTS, wg/L <ppbl S--pi. ID AnalyteCCO. 2/27/82 Priority until pollutants Arsenic4 Mercury4 Selenium4 Thallium Antimony Beryllium Cadmium Chromium Copper Lead Nickel Silver. Zinc 3.3 <0.8 4.9 <63 <730 <23 <30 <36 <52 <880 102 <80 432 Nonpriority metal pollutants Aluminum Barium Boron Calcium Cobalt Iron Magnesium Manganese Molybdenum Potassium Sodium Strontium Tin Titanium Vanadium 740 16 8.4 x 10s 1.3 x 10* <99 2.3 x 10s 1.2 x 10 35 <130 2.5 x 10* 4.2 x 10* 31 <5.3 x 10* 16 <150 4Analyses by AAi all others by icp MOTEt ICP values are an average of duplicate analyses 43 MONS 022366 TABLE 6. QUALITY CONTROL TOR METALS ANALYSES iq/L (PPB) Analyte Aluminum Barium Beryllium Calcium Cadmium Cobalt Chroaiua Copper Iron Manganese Nickel Lead Antimony Titanium Vanadium line Arsenic*^ Selenium Mercury4, Thallium* Reference Standard ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP ICP SRMA SJtHA Tm-CL Spex A Observed True Value Value 969 1,060 1,00 1.060 1.020 1.100 1.100 1,020 1,050 1,090 1,110 1,050 1,100 1,070 1.090 1,050 80 12 19 981 1.000 1,000 1,000 1,000 1.000 1,000 1,000 1,000 1.000 1,100 1,100 1,100 1.100 1,100 1.100 1,100 77 20 1,100 t Recovery 97 10< 109 104 10 110 110 10. 105 109 in 105 100 107 109 105 104 111 93 98 `Analyses by AA: all others by ICP 14 HONS 022367 TABLE 7. LOO* Valuaa for ICP METALS aa Of 3/23/*2 Analyta Aluminum Antimony Barium Baryl1ium Boron Cadmium Calcium Chromium Cc'aalt Copper Iron Lead Maqnatium Kangannse Molybdenum Nickel Silver Tin Titanium Vanadium line LOO Valua, .g/L Ippbl 480 ?30 13 23 580 JO 1 I * 10* 36 99 23 17 880 63 5 130 30 80 5. x 10 6 150 7 'lowit obitrvifela quantity TABLE 8. TOTAL PHENOL AND CYANIDE CONCENTRATIONS ug/L (ppb) Saaela ID Phanol Cyanida CCO, 2/27/B2 11 SO Kafaranca Standard Total Phanol Cyaalda QUALITY CONTROL DATA Obaarvad Valoa, */L 222 Troa Valua, 1IO/1 250 110 10 IS 1 Kicovtry <9 MONS 022308 TABLE 9. ANALYTICAL KESULTS-FOR NON-PRIORITY POLLUTANTS IN DECATUR SAMPLE Analyte Total organic nitrogen Surfactants Oil and grease Nitrate/Nitrile as N Sulfate Sulfite Sulfide Total Phosphorous Sample ID CCO, 2/27/B2, ma/L 33.6 0.04 2 0.8 974 150 1.0 26.2 TABLE 10. QUALITY CONTROL DATA FOR NON-PRIORITY POLLUTANTS Analyte Standard Oil t Craaae Oil a Craaae Total Organic Nitrogen Sulfate (ERA 3253) Nitrate (ERA 3253) Total Phoaphate (BRA yellow) Obaerved Value ma/L 16 25 5.4 221 4.5 3.4 True Value ma/L 19 26 5.4 221 4.0 3.3 1 Recovery 84 96 100 100 111 103 1C MONS 022369