Document JNRL4XZQ1pM1jgRbrGLE7MYqX

f a j e , N jJ !^ MONSANTO COMPANY / DAYTON LABORATORY / DAYTON, OHIO 45407 ESC/DAYTON (Department/Section) ANALYTICAL (Type of Report) REPORT NO. MDA-565 JOB/PROJECT NO. 484.4420 DATE 8 January 1985 PERIOD COVERED aa 0 b1* TITLE Analyses of Wipes for 2,3,7,8-TCDD CQ AUTHORS : G L Thomas o tu W fwt b Ao CO b* K CO s U <z< VI U 06 QH in iInD ^T~ 22 ABSTRACT: Wipe samples from the Nitro plant were analyzed for possible concentrations of 2,3,7,8-TCDp. The results of these analyses are shown in this report TECHNICAL APPROVAL: a cv-- ..,--*".AJtte-****** P. L. Sherman Sr. Research Group Leader APPROVED BY: R. F. Iv.ory Environmental Sciences Center Service Project Manager APPROVAL DATE: /-~J RESTRICTED DISTRIBUTION: (see over) COMPANY CONFIDENTIAL This document ia 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 persona or sent outside Monsanto Coapany without proper authorization. CONFIDENTIAL S U B JFC T TO p p n rr rr n / r n o n c o G11059 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 R-1068(C) COLMSE? EXE CGN* 3A L SUBJECT TO PROTECTIVE ORDER. C11060 DOCUMENT CONTENTS Pag Cover S h e e t ......................................................... 1 Document C o n t e n t a ............................ 3 R e p o r t .................... 4 Document Inventory Forra ........................................... 9 Sample Receipt F o r m .............................................. 10 Chain of Custody F o r m ................................................ 11 Analysis Request F o r m ............................................... 13 Monsanto Notebook Pages For: a. Extraction/Preparatlon .................................. 14 b. Analysls/Data Reduction ................................ 15 Instrument Logbook Pages ........................................... 16 Computer Output and Chromatograms ................................ 17 Additional Documentation . . . ................................. . 70 (morn ;fc:V C11061 ANALYSIS REPORT FOR 2,3,7,8-TCDD IN NITilO SAMPLES INTRODUCTION On 18 Osc 84 aight wipe samples 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 MRC 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 purposes 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 (WIPES) The wipes were spiked with 24.0 ng of carbon-13 labeled 2,3,7,8-TCDD and 9.6 ng of chlorine-37 labeled 2,3,7,8-TCDD. Then ten grams of washed anhydrous sodium sulfate 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" grads), 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 tfoelm 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 chlorlde/hexane (v/v) solution to elute the TCDD 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) 2,3,7,0-TCDD (m/z 257,320,322), chlorine-37 labeled 2,3,7,8-TCDD (m/z 328), and carbon-13 labeled 2,3,7,8-TCDD (m/z 332,334). CON? AL 00004 SUBJECT TO PROTECTIVE ORDER. 011062 STANDARDS' Standard solutions wart prepared from standards that had basn cross validated with a standard provided as a check sample by the 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 PROTECTIVF O R n ro C11063 TOT SATA REPORT WSAJiTOCCfWW. PAYTONLASCnATCBY CCfCUitH SPM30 Bf NATIVE* ,390 Bf a s B W T E i 1,1?; SAfTLE lemm t *t 3 4 r 7 B *9 HIGH SPIKE sim ETTR NR ANALYTICAL 320 332 t KTW CLEAN TOT D.L. DATE T I 322 33* ACC 329 m 257 323* 332 33* N J PC 1.15 -- 12/19 1041 .00 .00 108. 4210. 5238, 3606* 119652. 105329. 132008, J BC ,94 -- 12/19 1101 .07 .81 103. ' 3981. *881. 3180. 130100. 12123*. 1*9500. J PC w .27 12/19 1122 HM .81 108. 0. 0. 0. 87*06, 72763. 90262. I .J BC NO .11 12/19 11*2 MM .80 108. J BC tt .1 12/19 1202 IM .80 100. 0. 0. 0. 707749. 17769*. 222731. I 0. 0. 0. 113823, 10*544. 129927. I <1 BC 1.2* -- 12/19 12*2 .03 .80 107. 7473. 8970. 4860. 192439. 170592. 213347. . J RC 1.20 -- 12/19 1302 .00 .01 100. 5934. 74*9. 3904, 151413. 13*008. 166R51. JR .09 -- 12/19 1322 .83 .81 107. 4525. 5*37, 3918. 161143. 143664. 177982. J BC W .1* 12/19 13*2 HM .81 100. 0. 0. 0. 15274t. 135626. 167033. I J BC 106.74 -- 12/19 1**2 .80 .79 109. 396327. *93503, 165039. 1220S5. 106076. 134320. CrmECTCD FOR WTMBUTICN BY NATIVE TO T (SUBTRACT .0 0 * OF H/E 3221 NOTE CODES* I I ISOTOPE RATIO OUT CF ACCEPTABLE P A * VI X ACdRACY OUT (F ACCEPTABLE RANGE flW C TC B B LA * P-PARTTAL SCAN R-SEPWATE ICICHIW AKQ W W F M XFi.rCBTFIW TEH .A il FB-FTE1.0 BLAMC L .m * T lU E TO T SPIKES KW*OT PFTECTED (W FTECTION U N IT > JA R FILENAME TOT33 ' C O i C r ' i 'JUai 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) 0.9863 0.8551 0.8558 0.9019 0.6881 0.8551 DATE 12/19 12/19 12/19 12/19 12/19 11/27 TIME RRF (SURROGATE) 1001 1021 1222 1422 1505 1525 1.123 1.224 2.174 1.017 1.895 1.798 GTT2X 00007 .^1IR JCY'T" "TY^ DDATT/^m /r An 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 srn- T'. 0 0 n r)8 7~\7S" \7 C11066 DOCUMENTATION INVENTORY FORM Monsanto Research Corporation Dayton Laboratory I. Sample Information Sample Identification: f* I7 K O Number of Samples: Analyte: Matrix: \y Method :'pcfSrM;0*vtifrfO tf" 3 j7 >$ -- TC-i>D ih Soil a n d Stdi #\e*t 11. Documentation Control Copies Attached Initials (a) Sample Receipt Form (b) Internal Sample Tracking Form (c) Sample Tags <d) Airbill (Number *--- ------ ) (e) Chain of Custody Form (f) Analysis Request (Log Number / 'ihff t'f) (8) Extraction/Preparation notebook pages (NBP) 2 9 3 | L 3 00 Analysis NBP __________________ Instrument Logbook pages //T(- 7 Computer Data Files _____________ hard copy output . Chromatograms <i) Data Reduction NBP 23 7 3 7 > .(j) Final Report (it ) Additional Documentation (note immediately upon acquisition) S'fXncfa rd S Prepare* f/a-ns y -- -- -- y y y \y y t/ </ y y y /rtucr' jfrfiud jr#uCT~ Sfftcr' rfKUTZ Pr/UliT File Complete (signature) 00009 co n fidential n i ir t /-y-y r (date) C11067 Sample R eceipt Form Monsanto Research Corporation Dayton Laboratory Customer Id e n t if ic a t io n : HhX O ____________________ MRC Log Number: V Q'i' I * ' I________________. A i r b i l l Number: ----- Date: i Qz""D c. M Sample R eceip t In fo rm a tio n : (a ) Shipping Containers (b) Custody Seals (c ) Chain o f Custody Forms (d ) Sample Tags (e ) Sample C ontainers ( f ) Agreement o f Sample Documentation J n t a c t j damaged (d e s c rib e below) No. present ^ absenj)(describe 'se alin g below) In t a c t ____ p resen t absent N o.JX 5'senQ absent No. & ^ T n tag V damaged (d e s c rib e below) No.?> Q yesT? no (d e s c rib e d is c re p a n c ie s ) In itia ls 6*t ar <ZT <rr &i~r ll A d d itio n al D e sc rip tio n ( 1 f sample numbers not lis t e d on ch ain o f custody form , l i s t here and co n ta ct SMO). ) StrtUiD v e n t Ttft-K/tfG T f \ ? E c i1r r h r-r*r r f\ o p n T E C T lV E O RD ER* ,n !O O Q CHAIN OF CUSTODY RECORD MRC JOD NUKCCR ______________________________________ ________ MLCUSTOMER I'EPRESCHiAIIWL Ke,irH CONTRACT NUMBER _____________________________________ ________ MRC CONTRACT MANAGER __________________ PLANT NAHE OR CODE fyl iV Lo^ ^ V ^ .'W > MRC TEAM LEADER (S p e c if ic In fo rm atio n on samples 1s a v a ila b le on attached " Sample Id e n t if ic a t io n Log*) S ig n a tu re s Team Leader V e r if ic a t io n o f C o llected Samples: Relinquished by: Received by: Relinquished by: Received Logged-1n-by: . Received fo r A n alysis by: Method o f Shipment: Date Time Remarks f &L0 Number o f C o n ta in e rs : . Sp ecial In stru c tio n s (Sample p re se rv a tio n , s e c u r ity , d e liv e ry to , e t c .) "=Tt lJ i. fjLS'J-ts -- & X jty-t, D&'is) tSTvv is~<r ________ _ . 7 Ja oh.f i'U . rf\ Vv 'u r s HSVQ7 O t `-- o CD <o SAMPLE lOttTlFICAI ION LOG HRC Jot. Ha, C o n t r a c t No. Plant Name or Codi V^-g-ltH(V).Custo.Twr Representative CUi. MRC C o ntract Manager ___ Team Leader Samniing Location to.. / to- 3 u. H to. f w. U7 U1 i _ Run D a te Type o f Sample & Number Sampled No. o f C o n tain ers LA0. \Z -`M WtT^o PAQ C A ii _ L ____ i m it t i^OAT________ OAG & U --L. E)N'/70Y\ PAp CAQ tlSlu "h A fT ^ "part .. 9 9 "SC^n/c 'pAYTVt^T>AHi fOf> hai+kC, QAfttn P*/) TOP oP" Oc.lv* Kuf<6 n \j _ n irr^ I *74 '3/*^ i f\i tKo 'PAh i ! ______ j _________ i! * A n a ly sts Required 3 . 3 . 7 * - -nrPD 1.,. t \ ir i i i . 1_ 1 iIi 1i .. . Sample re co ve re d By "" ( i n i t i a l s ) and Cormenti i _________1 _ - .. .j 0 0 0 1 2 1 C l 1070 ANALYSIS REQUEST - ft- I MONSANTO RESEARCH CORPORATION REQyUUESITLEAR V i7Kn / K, `'iDAYTON LABORATORY . I CHARGE NO.** -AMPLE DESCRIPTION NUMBER OF B0TTLE5: > 3NUMBER OF SAMPUS 9 REPORT RESULTS TO FILES/KULIK it V - *u wr M O . I U \ S U V 'i L ' v . M ' 7 5 '3 '- AN ALYSIS REQUEST * FILES iS ? * r i - ; * - ^) - C * ifi N A . r--, / \ - ' -* ~ i; (< \ i.) ) \ f -* W t ,r - ! -; S l - V " j ,/ -- t i 7 V ` u l r 1- ' J S t ; ^ ` - H ' *' ; \ iV i i\ ! * ^ M RECORDED BY: / *"s~)]A4 REQUIRED ANALYSIS' SAMPLES FOR; W - r :'S SAMPLE LOCATION > 3 ,7 ,3 - - 7 c v KNOWN HEALTH HAZARD PRESENTED BY SAMPLE: REFERENCE TO PREVIOUS WORK (REQUEST!, JOURNAL,ETC.) COMPLETION DATE TIMEALLOTED FOR ANALYSES ANALYST HOURS INST. TIME ANALYTICAL TECHNIQUE GAS CHROMATOGRAPHY ULTRAVIOLET VISIBLE INFRARED EMISSION. EDAXXRF MICROSCOPY OTHER _________ QUAI_________ SEMIQUANT. REQUIRED QA/QC NMR HPLC XRD ICP ATOMIC ABSORPTION . MASS SPEC ISs^C/MS ' AUTO ANALYZER _____QUANT__________ S D S f H A k U it SUBJECT TO PROTECTIVE ORDER. -SAMPLE DISPOSAL AFTER REPORT COMPLETE D DISCARD O RETURN HOLD FOR Q 30 DAYS TUTC TweftDMiTTriM M IKT RF HIPPITFO BY ANALYSIS REQUEST ORIGINATOR Q DAYS U1107T OT ts MONSANTO COMPANY A J i T T o A]if> INO. PRPARCO Y IJ1GNATURCU , N ? 2831620 OATK ? m cSV ; SUBJECT TO PROTECTIVE ORDER. 0CO14 RRAO AHO UMOKRSTOOO OATC 1 1 0 7 2