Document Bpvqg6N6rXOxd7pyojNp1KZL

f/ i-e - 0Z b 'o y ^ y MONSANTO COMPANY / DAYTON LABORATORY / DAYTON, OHIO 45407 ESC/DAYTON (Department/Section) ANALYTICAL (Type of Report) a a 0 H1 CO rm% (N COS ti- CO u a. a, o o ? cn k C>O < z< V) U aJ H UO vLfOl o z S > ft 28 a REP.ORT NO.: MDA-56 5 JOB/PROJECT NO.: 484.4420 DATE: 8 January 1985 PERIOD COVERED: TITLE: Analyses of Wipes for 2,3,7,8- TCDD AUTHORS: G * L * Thomas ABSTRACT: w ipe samples from the Nitro plant were analyzed for possible concentrations of 2,3,7,8-TCDD. The results of these analyses are shown in this report TECHNICAL APPROVAL a_ J/ P. L. Sherman Sr. Research Group Leader APPROVED BY R. F. Iv.ory a Environmental Sciences Center Service Project Manager APPROVAL DATE: RESTRICTED DISTRIBUTION: (see over) 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 unauthorized persons or sent outside Monsanto Company without proper authorization. CONFIDENTIAL SUBJECT TO PROTECTIVE ORDER. C11059  ) D IS T R IB U T IO N COPY NUMBER 1-3 M. Townsend, Nitro Plant 4 F. Kearney, St. Louis-E3NA 5-7 T. Bistline, St. Louis-E2ND 8 G. Thomas 9 R. F. Ivory 10 Technical Reports Library - R2C 11 Central Files ABSTRACT ONLY H. A. Woltermann 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 Sciences Center, Dayton Laboratory, Dayton, Ohio. ACKNOWLEDGEMENT Contributions of the following Dayton Laboratory personnel to this project are gratefully acknowledged: Analyses: G. L. Thomas fl-1 0 6 S (C ) it--"iii i T I A L SUBJECT TO PROTECTIVE ORDER. C11060 DOCUMENT CONTENTS Cover Sheet . . ................ Document Contents .............. Report ........................ Document Inventory Form ........ Sample Receipt Form ............ Chain of Custody Form .......... Analysis Request Form .......... Monsanto Notebook Pages For: a. Extraction/Preparation b. Analysis/Data Reduction Instrument Logbook Pages . . . . Computer Output and Chromatograms Additional Documentation . . . . Page 1 3 4 9 10 11 13 14 15 16 17 70 (UjOO' -- i --. n-- a * Li.* JV ANALYSIS REPORT FOR 2,3,7,8-TCDD IN NITRO SAMPLES INTRODUCTION On 18 Dec 84 eight wipe sample* were received for the analysis of 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD). For Internal purposes, the samples were assigned HRC Log #1-84-12-18-01. The samples were analyzed according to the September 1983 EPA Region VII method "Determination of 2,3,7,8-TCDD in Soil and Sediment". For quality control purpose* MRC Method #07-QAQC-R3 was followed. Briefly this method requires that for every set of samples of the same matrix type a replicate sample, a low (9.6 ng In this case) spiked sample, a high (96 ng in this case) spiked sample, and a method blank must be analyzed. PREPARATION AND ANALYSIS (UIPES) The wipes were spiked with 24.0 ng of carbon-13 labeled 2,3,7,8-TCDD and 9.6 ng of chlorlne-37 labeled 2,3,7,8-TCDD. Then ten grams of washed anhydrous sodium sulfats was added and the samples were stirred, allowed to stand and stirred again. Samples were mixed again immediately prior to addition of extraction solvents. The extraction process involved the addition of 15 mL of methanol (all solvents are Burdick and Jackson "distilled in glass" grade), stirring and the subsequent addition of 150 mL of hexane. The samples were then shaken for one hour on a wrist action shaker and the extraction solvent removed. The solvent was then successively extracted with 50 mL of water, concentrated sulfuric acid (until clear), water, 20% potassium hydroxide and water. The hexane was then dried with 10 grams of anhydrous sodium sulfate. Each sample was then placed on the head of a mixed phase column consisting of (top to bottom) 2 g of silica, 4 g of silica plus 40% sulfuric acid; 1 g of silica, 2 g of silica plus 36% potassium hydroxide and 1 g of silica. The column was^eluted directly onto a column containing 2.5 g of Voelm basic alumina. The alumina column was first eluted with 10 mL of 2% methylene chloride/ hexane (v/v) and this fraction discarded. An additional elution was made with 15 mL of a 50% methylene chloride/hexane (v/v) solution to elute the TCDO off the column. All samples had 50 uL of dodecane keeper added to them and then were concentrated under a gentle stream of nitrogen and submitted for GC/MS analysis. The GC/MS analyses were conducted on a Hewlett/ Packard 5987 GC/MS instrument. The analysis was conducted using a 60 m SP2330 capillary column. The mass spectrometer was operated in the selected Ion monitoring mode analyzing for ions characteristic of both the native (unlabeled) 2,3,7,8-TCDD (m/z 257,320,322), chlorlne-37 labeled 2,3,7,8-TCDD (m/z 328), and carbon-13 labeled 2,3,7,8-TCDD (m/z 332,334). CONF^EM TIAL 00004 - SUBJECT TO PROTECTIVE ORDER. I Cl1062 w: ^ STANDARDS Standard solution war prepared from standards that had bn cross validated with a standard provided as a check aampIs by tho EPA. Concentration of the Internal standard conformed to the levels specified by the method. RESULTS The results of the analyses are given in tables 1-3. The tables also give all pertinent QA/QC Information. SUBJECT TO PROTECTIVE ORDER. C11063 TOP WTOREPORT NCKUtfTO CtW W . paVTi LSSCftATCRY ccra.aai sptoo RFNATIVEl ,39 rf amwiaiti \.n\ SAWX NtifflFR ( fc 3 4W 4 7 ft 8 HIGHSPIKE SUS) EITR NO ANALYTICAL sm 332 X KIWI CLEAN TOT O.L. DATE TI* 322 334 ACC 320 322 257 3 3 334 N J PC U 5 _ 12/19 1041 .30 .80 108. 4210. 5238, 3404, 119452. 105329. 132008. J EC .94 -- 12/19 1101 .92 .81 103. ` 1981. 4881, 3180. 130100. 121234. 1475. J PC w .37 12/19 1122 .81 108. 0. 0, 0. 87404, 72743. 70242. I .1 BC NO ,u t2/l9 1142 HH .80 108. 0. 0. 0. 202749, 177474. 222731. I J EC >0 .1ft 12/19 1202 IIH .80 104. 0. 0. 0. 115823. 104544. 129927. I J BC 1,2 -- 12/19 1242 .81 .80 107. 7473. 0978. 18. 192439. 170592. 213347. J RC 1.2B -- 12/19 1302 .BO .81 10$. S934, 7449. 3984, 131415, 1348. lAAflfll- J BC .9 -- 12/19 1322 .83 .81 107. 4525. 5437. 3918. 14U43, 143444. 17798?. J V w .(4 12/19 1342 ttH .81 103. 0. 0. 0, 152741, t356?4. 147033. X J BC 104.74 -- 12/19 1442 .80 .79 109. 394327. 493503, 145039. 122085. 104074. 131320. P RS'J E D FOR CONTRIBUTION BY NATIVE TO T (SUBTRACT .009 OF */E 322) W TECO CESl I I ISOTOPE RATIO OUT CF ACCEPTABLE RAWS Yl X ACaSACT OUT OF ACCEPTABLE RANGE iffw e n co BLWK PrfARTT. SCAN SEPARATE ICICHING WO W K Ip 0 > n R .icA T F(iN m A a ) FW IELO BUUC L-H -W TM TCTO SPINES XfcNOT DETECTED DLDETECTION L IB IT > ja r FILEVAfE -TC0D33 SUBJECT TO PROTECTIVE ORDER. C11064 TABLE 2. CALIBRATION SUMMARY ug/Kg NATIVE TCDD ' 0.5010 5.010 50.10 1.2515 12.515 125.15 RRF (NATIVE) 0.9668 0.8551 0.8558 0.9019 0.8881 0.8551 DATE 12/19 12/19 12/19 12/19 12/19 11/27 TIME 1001 1021 1222 1422 1505 1525 RRF (SURROGATE) 1.123 1.224 2.174 1.017 1.895 1.798 GTT2X 00007 AJNb SDENT3AL SUBJECT TO PROTECTIVE ORDER. C11065 TABLE 3 QUALITY CONTROL SUMMARY ITEM SURROGATE ACCURACY SPIKE RECOVERY # DATA POINTS 10 1 MEAN S.D. 107.2 1.7 * * Not technically correct to report recoveries for internal standard calculated results. GTT3X 4^*1 ,^v r\ 00008 1 t "''V \p ry C 11066 DOCUMENTATION INVENTORY FORM Monsanto Research Corporation Dayton Laboratory I. Sample Information Sample Identification: M Number of Samples: ^ Analyte: `2/3/7/*5? -*7^7) Matrix: \N t7 ^ S Method:'peterm i * c^o flf" y ? j 7 j? -- T d >D in Soil 3 *<k II. Documentation Control Copies Attached Initials (a) Sample Receipt Form (b) Internal Sample Tracking Form Cc) Sample Tags (d) Airbill (Number ^ " _____ ) (e) Chain of Custody Form (f) Analysis Request (Log Number / (g) Extractlon/Freparatlon notebook pages (NBP) JL 9 4 |J * l <?__ (h) Analysis NBP A 7 3 ' 7 t * Instrument Logbook pages //?" 9 D Computer Data Files _____________ hard copy output Chromatograms <i) Data Reduction NBP 23 7 3 ^ 7 6 (j) Final Report (k) Additional Documentation (note Immediately upon acquisition) S 't t i n d a r c j s P r e r < * fi - K s n e f a 73 i4j x n u t s File Complete OOno9 SUBJECT TO PROTECTIVE ORDER. y -- -- -- \s V tirfu C T ' \s 0-/U <? 1/ & u < r' . 3 & (cu T * 1/ \S f a m T \S fa ta r (signature) /- (date) C11067 Sample Receipt Form Monsanto Research .Corporation Dayton Laboratory t Customer Id e n t if ic a t io n : H f t X O ______________________ MRC Log Number: V B i ' O - f g I___________________ A i r b i l l Number: ------ Date: i *b ~ l ) c 0 M Sample Receipt Inform ation: (a) Shipping Containers (b) Custody Seals (c) Chain o f Custody Forms (d) Sample Tags (e) Sample Containers (f ) Agreement o f Sample Documentation In itia ls (T n t a c t ^ ) damaged (d e s c r ib e below) No. \ kr present /absenj)(describe ^ i e a l l n g below) In t a c t ___ < a r ^ p re se n t absent N O .^. C e re s en t O ^TntagV absent No. 8 damaged (d e sc rib e below) N o . 'S z C EP no (d e sc rib e d is c r e p a n c ie s ) n A d d itio nal D e sc rip tio n (1 f sample numbers not lis t e d on chain o f custody form, l i s t here and con tact SMO). ) T ft? oonio s -- "rvv V C11068 CHAIN OF C im O D t RECOUD r.. N. C C i'w -- --j --iv' 1X4 oooii su b je c t to pro tec tiv e o r d er . HRC JOB NUMBER __ _______________ _____________ CLTjTUDtR I't'PRESCHTAIIVL K i . r M i I CONTRACT NUMBER ._______________________ MRC CONTRACT MANAGER PLANT NAME OR CODE fyl iV La^ V ^.W > KV. TEAH LEADER ( S p e c if ic In fo rm a tio n on samples 1s a v a ila b le on attached 11Sample Id e n t if ic a t io n L o g *) Signatures Date Time Team Leader V e r if ic a t io n o f C ollected Samples: Relinquished by: Received by: Relinquished by: Logged-1n-by: . Received *3-/f,T% Y l g f $ 0 Received fo r A n a ly sis by: Method o f Shipment: Humber o f C o n ta in e rs: Remarks Sp e cial In stru c t io n s (Sample p re se rva tio n , se c u rity , d e liv e ry to , e tc .) --------------------------- e=^----- -y. 1^------------------- /b.t f o -j /U crC rC jt ...... _ /% A n g __ C ___________________ :_______________ __ ~0c^ VtJVi__ _____________________ 1___________________ _ __ _____________ ____ iS f _ J & Q -licr/c*.^ / J } ^ _________________________________________ / Ofigb y f Y o y SAMPLE lO E firin C A T IO H LOG KRC'Job-Ns. _______ .______ .______ __ C o n tra c t No. ' _____________ Pl ant Name o r Code ________ Custo^p RepresenUtlve ( V l. u fe'SL HRC C o n tract Manager _____________ Team Leader ___________________ __________________ Samtil ir,g Location m . / 2 Mi 3 VJo <7 ' M a f. Mi ^ U. 7 U$ Rur, Gate Type of Sample h Number Sampled No. of Containers LA& \i-'4 MlTT^O PAM CAfl At MlTU^ 9A^ G iit*-- Analysis Required 3 . S 7 V - 7>6t) Sample recovered ey (Initials) and Cogent* oo 'hAYT^n "pArt "S^n/C TvlVTB^> iOP s-that+LC. OAr m 9at> TbP i>P UcJvf h*uJ4 nm^o "PAft V/ -7 4 *3/aifc /11 nco "PAr> i 1 L_ ! i \ !! i| 1i _ *-1r~-- - _ - ' .* ' ;;Lj 00012 __ C11070 -'3,7,3-7 c>> KNOWN HEALTH HAZARD PRESENTED BY SAMPLE: REFERENCE TO PREVIOUS WORK (REQUEST#, JOURNAL,ETC.) COMPLETION DATE TIME ALLOTED FOR ANALYSES ANALYST HOURS INST, TIME ANALYTICAL TECHNIQUE GAS CHROMATOGRAPHY NMR ; ULTRAVIOLET HPLC 1 VISIBLE XRD 1 INFRARED ICP EMISSION . ATOMIC ABSORPTION EDAX XRF MICROSCOPY MASSSPEC 13<C/MS ! 1 1 OTHER OUAL AUTO ANALYZER 1 I SEMI QUANT. _ . QUANT. . REQUIRED QA/QC C Q * y i o E a r i A L u o .i l a o b j e c t t u p r o t e c t i v e o r d e r .' SAMPLE DISPOSAL AFTER REPORT COMPLETE DISCARD O RETURN HOLD FOR D 30 DAYS tut* TucooMiTTnw MIKT RF SIIPPITFD BY ANALYSIS REQUEST ORIGINATOR D O DAYS C1I7T OT ECT /ill^o UJt MONSANTO COMPANY N? 2831620 paepaaeo by uignatuaei- , OATE >1 S iit i /ft Vit- M itro U J i f i S . ^ M 3 H tkD,ShMt by 13. R. CL-rfe JCoJc No. T P - ftmC. -to V t3 * .7 j#//tA/itocA &hlc____ ----- ,--- : - ------- - 300ff_ l/Zj'faf&cf fyf/fc . 3 W v j aY^ o B i ; t 3 0 .1 o #y c w . i d s/Mk 3 0 1 1 ff.5" jplL f W 7 9 5 W >0.10 C P w ta A L * 7 ? . 122 >&"v *79 > n ' l # 5 yt/> tel ffc, 7 ? _37.1S Shc*/-&lo*k. r w * * fb - ttH * Lo V/<f _ 3 2 7 7 _M: Spi K/ /fc.UAf /i'iL-i'Wrrtijo cur. pfjCil Ca (O ^C/ (V . V/ 1/ rtf.ri* * i/ tut a{ Mhr#ti \J J L \/ u > j y 't > . ''* / I l/l 1/ V J 1/ j /Om ! jnt 1/ l/ ^'/lo ilS^A ClATfT -A. y 1W fa M a.1?gl7 _ *V 't * ------------ * SUBJECT TO PROTECTIVE ORDER. OC014 OATC11072