Document 8VKJoy7xxYvNp7yjOx70LQZqK

distribution COPY NUMBER 1-3 M. Townsend, Nitro Plant 4 F. E. Kearny, St. Louis-E3NA 5-7 T. Bistline, St. Louis-E2ND 8 G. Thomas 9 R. 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 COMPANsYSstCQNFI DENTrA Ir CONFIDENTIAL C11131 9 .t (Cl n n n -n rm V F ORDER DOCUMENT CONTENTS Paga Cover S h e e t .......................................................... Document Contente .................................................... 1 3 Report .............................................................. 4 Document Inventory Form ............................................. 9 Sample Receipt F o r m .................................................... 10 Chain of Custody Form . . . . . . . . . . . ........................ 11 Analysis Request Form . . . . . . . . ........... . . . . . . . . . 14 Monsanto Notebook Pages For: a. Extraction/Preparation ................................... 15 b. Analysis/Data Reduction ................................ 16 Instrument Logbook Pages ........................................... 17 Computer Output and Chromatograms ................................ 18 Additional Documentation ................... . .................... 79 CONFIDENTIAL SUBJECT TO PROTECTIVE ORDER, r> Cl1132 ANALYSIS REPORT FOR 2,3,7,8-TCDD IN NITRO SAMPLES INTRODUCTION On 27 Nov 84 eleven wipe sample were received for the analysis of 2,3,7,0-tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD). For internal purposes, the samples were assigned MRC Log #1-84-11-27-01. Tho 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 w r l s t 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/hexarie (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) 2,3,7,8-TCDD (m/x 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). STANDARDS cSrtoasnsdarvdalivdoaluttaidonwsitwharas praparad standard iron standards that provided as a check had baan sample by tha SPA. Concentration of the internal standard conformed to the levels specified by tha method. RESULTS The results of the analyses are given in tables 1-3. The tables also give all pertinent QA/QC information. 00DO5 TTC3 TA B*FT rra w n ) to ra rt. vrc* labtrattwy OC o v n a SP2TB e? WTTVEl .914 f f SJSnCATFl 1.283 i T tE Ann -- l 2 *3 A s 14 17 H 19 1 10 11 LiW SPIKE h iw s p iu 8 ETTS HTHO J J J J J J J J J 4 J J J J CLFM - tt BC BC BC BC BC BC BC BC BC K BC K*. BC W TOO ---- t.io .99 .8 7 .7 8 .7 3 1.84 .9 6 1.03 .6 2 .7 3 . 7 3.87 70.62 HO D.L. -- . SB* AWlYTimt 320 33?- X MTE TD t 322 334 ACC ---- -- - -- 11/27 1631 .75 .61 97. 11/77 1631 .63 .78 98. 11/77 1711 .73 .85 102. 11/27 1734 .84 .81 96, 11/27 1734 .49 .62 96, 11/27 1834 .83 .81 93. 11/77 1853 .83 .61 T7. 11/77 1913 .81 .80 96. 11/27 1933 .67 .81 96, 370 -- 971g. 9958. 9924. 10119. 71 . 21036. 12593. 11422. 11323. 322 -- 13006. 11719. 13521. 12107. 11350. 26634. 14812. 14072. 13044. 257 3289 332 334 ---- ---- 5718. 304793. 7/6028. 3739W . 6709. 3334U . 274021. 350377. 8333. 417910. 352124. 412431. 7331. 614253. 360867. 7126. 5605. 391320. 335065. 409731. 11288. 360041. 3)4376. 39046} . 8796. 420294. 362W7- 9 * . 7241. 363177. 31371. 3W613. 6678. 631972. 377533. 467178. 11/27 1953 .77 .80 96. 9381. 17118. 7398. 617618. 362763. 653825. 11/77 2033 .74 .79 96. 8505. 11672. 4819. 349120. 317922. 404090, U /27 2053 .79 .83 112. 36931. 71786. 31878, 373563. 2R2007. 339968. 11/77 2113 .81 .84 102. 653026. 807944. 300140. 317PEL 765313. 3177 . 11/27 2133 .68 .80 101. 3780. 5594. 0. 321927. 265654. 331450, CTRECTED FOR O KTRIH m BY NATIVE TOO (SJBTOCT .009 OF 3221 ' k te gees* U lO TIFE RHO OUT f f iCEPTM U W6CE yj i s w c r a n of actip t a s e rm pe p**rt:#. sc DB-SaSF'fUiWTTEI<IlfHKTXEIt^GMUMO I C K * FWIEU) -WA: l.HMATIVE TOD SPIKES detected 1HXFTECT LtfllT >.R FILHWf TCK06 oann6 CONFIDENTIAL SUBJECT TO PROTECTIVE ORDER. C11135 TABLE 2. CALIBRATION SUMMARY us/Ks NATIVE TCDD 0.5010 5.010 50.10 1.2515 12.515 125.15 RRF (NATIVE) 1.0199 0.8902 0.8713 0.9030 0.9096 0.6862 DATE 11/27 11/27 11/27 11/27 11/27 11/27 TIME 1551 1611 1814 2013 2153 2213 RRF (SURROGATE) 1.318 1.224 1.238 1.240 1.329 1.350 GTT2X 00007 CONFIDENTIAL SUBJECT TO PROTECTIVE ORDER. . C11136 TABLE 3. QUALITY CONTROL SUMMARY ITEM SURROGATE ACCURACY SPIKE RECOVERY * DATA POINTS 14 2 MEAN S.D. 98.7 4.5 * * Not technically correct to report recoveries for internal standard calculated results. GTT3X 00n n 8 C l1137 DOCUMENTATION INVENTORY FORM Monsanto Research Corporation Dayton Laboratory I. Sample Information Sample Identification: Number of Samples: H Analyte: 2 j 3^7j ? ~ T `>r>P Matrix: i Method: i V t ^ r n l ^ - b 'c r ^ d f II. Documentation Control 'r C P O in S a H Copies Attached Initials (a) Sample Receipt Form (b) Internal Sample Tracking Form (c) Sample Tags -- - (d) Airbill (Number * * 4 % 71) fi- < !& i x P si & (e) Chain of Custody Form (f) Analysis Request (Log Number K (g) Extraction/Preparation notebook pages (NBP) l $ h / 3 (h) Analysis NBP J 2 7 3 z 7 r7 y' Instrument Logbook pages f*5~ L7& 0 Computer Data Files hard copy output Chromatograms (i) Data Reduction NBP U 7 3 A 7 7 (j) Final Report 0 0 Additional Documentation }/ (note Immediately upon acquisition) &7U*V Sm uT MST Z Z l S a L V j &"2 J 3 2 GSFile Complete 7 , ,, (signature) ' c-<2 C O N F I i i i i ^ ii A l a SUBJECT TO PROTECTIVE ORDER. ^ DO0 0 3 1 -y-rC (date) C11138 Sample Receipt Form Monsanto Research Corporation Dayton Laboratory Customer Id en tificatio n : N( i fco_______________ MRC Log Number: / ' &*/ ilV 7 O I___________ A irb ill Number: ___________P C&H&T~7 Date: fK7 Hq \J S V ________________________ Sample Receipt Information: (a) Shipping Containers (b) Custody Seals (c) Chain of Custody Forms (d) Sample Tags (e) Sample Containers (f) Agreement of Sample Documentation intact. damaged (describe below) No.J_ present <^absenj?`(describe "sealing below) absent intact No. p absent No.1 L damaged (describe below) No. f f no (describe discrepancies) In itia ls s2c: r SL lL Additional Description ( i f sample numbers not lis te d on chain of custody form, l i s t here and contact SMO). ) S fc f lc > VM-Trt 0O10 :v - -, WHITE. H U M - CANARY. ACCnttuTMin p a & m m & es* HV OPHTICCTthUNIFORM STRA IG H T B il l O F LADING ORIGIN A t NOT N EGO TIABLE a ~...,[5kTca":;ggg UTTER uAnmir 7J!RXfillxMlisACbNTN u O d t S S T S S RAX PE004877 ORAL AIRPORT O T. AIRPORT f ROM COURANT NAMC4CONSIGNOA] A'/. .*?/ -- -j STREET AOOftEM OXORTUSf O R O U H O TO COL <1(RECIPIENT) ' T-j, /V -*7 C' STREET ADORESS q U lIM lf MU*I*M<Al M o o t TIC )'Z i\ CITY I STATE CITY -A' ^ STATE __ I P.O. OR REFERENCE NO. SNIPPER'S SIGNATURE ZIP CODE (REOUIRCOi f 1; i f ,7T h lp o PARTY AUE A N D A D O R ES* COURIER GUARO SIGNATURE y < ,4 ROUTE DATE t * 0 * OITAGOOIi*OuNn tST*J _ L X* NOr a EGOTUSLE DILL OF LADING SUBJECT TO CONOmONS OF CODTUCT SET FORTH ON RE VERSE SIDE OF SMPFER S COPT. DESCRIPTION OF CONTENTS / Sr\*LL f k 'J t n I* -- I mN I | m il M lll' t l t tft#l f O M I ta> H*ntoN*iion MIMCtlAdA*'-- fllut ( MCWM N itH , I C , FREIGHT PIECES w eigh t DECLARED VALUE | Di m e n s i o n s 1L W M _ I _______1 ` ADV. 4VALUATION m c k k C M t 0 AMOUN I tqtal l niASfOONO|ICH(HAl(*l6tlsyt|MIOtmilOHH !(|tt/l W W O * J f AS C O A * in i M l S M I rw*01AlO"i M l I M H 1 A d O# COPT m O . * K M M tntvC TO * MOUNTAIN STATE ENGINEERING SUPPLY C w 'Ya" 4 00011i - L r V L t SUBJECT TO PROTECTIVE ORDER. . C11140 CHAIN F U iS O Y RtCOHD Hnc JOB HUHBER__________________________________________________ CUSTOMER 1'EPHESEHTArlVl S ./W /'/ft's- ' CONTRACT NUMBER___________________________________________________ HRC CONTRACT MANAGER______________________________________ PLANT NAHE OR CODE /flu - /l^ r/fO . HRC TEAH LEADER ______________________________________ (Sp ecific Information on samples 1s available on attached "Sample Identification Log*) Signatures Tea Leader V erificatio n of Collected Samples: Relinquished by: Received by: Relinquished by: Received Logged-ln-by: ~UJfXA^ Received for Analysts by: ^ Method of Shipment: Date Time "/A S*GKfc`ary / fL A d / m ' T,3o Remarks Humber of Containers: Special Instructions (Saniple preservation, s e cu rity f delivery to, e t c . ) 00012 C1114 r ^7 z /t-T ^ /Ue/x, _______ n/J/o_____________ 17 SAMPLE IDENTIFICATION LOG HRC Oot ______________________________ CusUmer Represented ve /C-. s%'//{rs Contract No. ______________________________ *RC Contract Manager __________________ _ Plant Name or Code A^r/Q0 Team Lea d er__________________ ;_________________ Samni i r.g Location j Alt Date Type of~Sample L hunter Sanpled No. of Containers Sz ^ aJ *! g - 7 9 x>/=> 0 ^ } jp y 1 / t J P iaZf * z ./ / " /z (rh n /z l. / u /a t. tft# M . * / 6 rjc/?-T r* A J G f T t f /*A*<>vP S o i / T H S-'/'C C s?'# v i s l >o & r j y S A JQ & T V *<? V y V f> /z& // 0 4i ft it V n J-tA //f**-4 ' 7 n fiSo& Ttf e/zsT /a - j w r * C f-jrtrs i3 i Vo1 y c^ rfi/p .? fW l e * e / </(<$ '// ! . _ ,! i ,, ' * ft tt '/ *F Analysis Required z s 7 J rco v U t. *1 1 '1 M n { < Sample recovered" By ( I n i t i a l s ) and Comnent - - CONFIDENTIAL oom3 C11142 ANALYSIS REQUEST DATE 21 LOG NO. MONSANTO RESEARCH CORPORATION REQUESTER" CHARGE NO" DAYTON LABORATORY A `fa'1 /zCuOr-v SAMPLE DESCRIPTION fiJMBER OF BOTTLES: / j i)DUMBER OF SAMPLES & gU\r }& " L Ja 11 2-] ( AJ A-^" K l* UJ<?^/ V i S ^ A J L f k)< '/ M U Ji * S s : M e.., H t At S A f-A * JtJb Cx^U-s- ^ H K i r U ) q ii 2 / r v r j 14 S l* tlU )a U H i ' * ' J REQUIRED ANALYSIS** ORECOROED BY; " U .in r H REPORT RESULTS TO* RSk c r < ,,, > ANALYSIS REQUEST 1 n\ss/mrr, e 5 7 T/'f~r\. ?? A j otJr 6 . " 77 (,,,,. SAMPLES FOR: SAMPLE LOCATION 3/20 1~ ~ C V D KNOWN HEALTH HAZARD PRESENTED BY SAMPL: v SY `i l O / c W ^ REFERENCE TO PREVIOUS WORK (REQUEST#, JOURNAL,ETC.) COMPLETION DATE TIME ALLOTED FOR ANALYSES ANALYST , HOURS INST. TIME ANALYTICAL TECHNIQUE * * GAS CHROMATOGRAPHY ULTRAVIOLET VISIBLE INFRARED EMISSION EDAXXRF ' MICROSCOPY OTHER OIJAl SEMIOUANT. NMR HPLC XRD G ICP ATOMIC ABSORPTION MASS SPEC -^ G C/M S AUTO ANALYZER _ OUANT. . . REQUIRED QA/QC rr\e < u 7- ______________________ onni 4 C O N F ID E N T ! A Y ^ TO PROTECTIVE" ORDER " SAMPLE DISPOSAL: AFTER REPORT COMPLETE DISCARD RETURN HOLD FOR d 30 DAYS Of- rimn. rcn O V A U & I Y d REQUEST ORIGINATOR 0 w DAYS _ J _________ 07} -T t t i ir e -- MONSANTO COMPANY /(Atro {Jipo-JUlViCT P ' q y '^v J O NO. 7 kOMX ^ N? 2S31613 OAT( %7 aJso -L/-\uL '(cfJn ,, 8 j OCj Mn. Sot AJlx A /iiro l/Ji'p e s ShdeX Ct>Jc Mo. fJ,ir0 T p 1 i /"i7. oj-r.^h UT 3/79 HI SUnt u r 3/80 )rY ^ kcuir f 7 ) i/ r 3181 J 3 V k 4 y </</ /JT 3182 y aj& ifilU r B<4,c/ /)T 316? * <=r 5. PUr VA/ UT ?\f9 *?,, i e c mer t/-A7" 7 /?f/7 7?oc/n 8aul^ ~Uil 7 ) UJ 00 UT 31 8(o 0 /VrfJpJ ' fi're ilh 11 LA / , UT 3187 5#y a i / - py'rr ///< // V 5 UT 3188 #/0 cftr r FTrr U/i/( IcmI y fc i i)T 318 9 - // Z L w PL U// 3rdlesti % i' ITT 9\ 90 Lo 5p>ke. UT 319 / M" ip`7c UT 3i92 5a/inP 75lo*y (our 0 t-ywJJ..^l)nj ------------------------------------- Sf.trtl t>y _& f f 1 C-L/t H? ouf. /j^c a' Ma Wi Co ^/j _L2. j s Cor',me yy y y Q.cki*fk feUrvt* / y IQOuioP(nkr*i !5k. y y a i V ^ A , '9 ^ / y in t\a-cxA* y/ y/ yy yy y vo*/ U1d/u.l /y 1 y / HiAt pbJ&'fk. . / . Z - .y TTD y / f*. Plo-ac&er ! cocer. tt?p kcJ qucL p re p o fJl i\1 de. /?uz>irter T '^ S S jC 'tiA dsce,e<jO A paqc %ty uJtcc u3odCe.d up in ^Lvb 3 9 q.ud 5 L 3 Z s ^ ji't m esi escerti S Tadards-