Document 71roN33yz8dNYxDxKmwXN0JzR

TITLE: ANALYSES O f TEXAS C l fY S O IL SAMI 1.1 s I HR PO I.VCIII OH JNATI |J` 1)1 H liN lO P IIIO X I NS ( I ' CHHs) A M I POl.Yl IILOH I N M I I I III T ill NYI.S 11036 COPY | Monsanto MONSANTO RlSiARCH CORPORATION / DAYTON LABORATORY / DAYTON. OHIO 4S4Q7 EA5C - DAYTON lOIRT /SICTONi ANALYTICAL TVSf 0 RI0*T RERORT REPORT WO.. MPA- 30 3 JOR/MOJECT WO. 3 . d 1 P and 4 8 : . 2'1 0 DATE; My S , 1933 PERIOD COVERED TITLE; ANALYSIS OF TEXAS CITY SOIL SAMPLES FOR POLY CHLORINATED DIBE-NCO-P-DIOVINS (PCFilHJ and POLY CHLORINATED BIPHENYLS fPCBs) AUTHORS; Frederick D. Hileman B. Major. Hughes ABSTRACT; Three soil samples were received from Monsanto Texas City for the analysis of polychlorinated dibento-p-dioxins (PCDDs) and polychlorinated biphenyls (PCBs). The result? of these analyses are discussed in this reoort. RECEIVED Approved by: JUN 1 !9?r Robert F. Ivory (y MONSANTO-DAYTON Environmental Analytical ScieCBNTNAL FILES Center Service Project Manager Approval date: ii i MOMS 220719 niSTRlBUTION COPY NUMBER 1 G. Rinaldi 1 F. D. Hileman 3 S. M, Hughes 4 R. f. Ivorv s Central Tiles 6 Tech. Reports 1890 l.'SO i; so l 1: sn R3C A0STRACT ONLY R. K. Flitcraft`1. R. M. Scott-12SO J. D. Vi Ison'G3WG \OTf : 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, Lnvironmenta) Analytical Sciences Center (TiSC), Dayton Lahoratorv, Dayton, Ohio. AChAOKLhXLMI1. 7 The contributions of the following Dayton Laboratory employes are gratefully acknowledged: Sample Preparation: D. kirk COMPANY COI\lf ID! N T I A [ When no longer needed, or upon requoet. return tMa report to Control Filet, Dayton. HOMS 220720 ] Three soli staples labeled TP*1 (Saaple A)t TP*S (Staple B), and TP-SiSK (Staple C) were received for the analysis of polychlori nated diben:o*p-dioxlns (PCOOs) and polychlorinated biphenyls (PCBs). These staples were assigned MRC Log number 1-82-0S-0701. Table 1 shows the results of the dioxin analyses, while Table 2 shows the results of the analyses for PCBs. SAMPLE PREPARATION The staples were prepared for analyses by weighing S grams of soil into a 250 al bottle. Forty aL of petroleum ether was added to the bottle which was then sealed and shaken for IS minutes. The petroleua ether was decanted out of the bottle into a centri fuge tube. Fifteen aL of methylene chloride was added to the bottle and then shaken for S ainutes- The aethylene chloride was also decanted into the centrifuge tube with the petroleua ether and these extracts were concentrated to 2 al. The extract was applied to a column containing 4 grams of silica gel which had been preeluted with IS al of hexane. This extract was then eluted through the coluan with 4S aL of methvlene chloride and the eluant solvent exchanged to hexane concentrate and this concentrate was then placed onto a coabination column containing silica gel, silica gel plus HS0, and silica gel plus KOH. This coluan was eluted with 45 ml of hexane and this eluant wag concen trated to laL. The final chromatographic separation was carried out on a 2,5 grass column of Woela B alumina. The first elution consisted of 10 mL of 2t aethylene chloride/hexane (v/v) which was concen trated to 1 aL and submitted for PCB analysis. A second elution of this coluan was Bade using 15 aL of SOt aethylane chloride/hexane (v/v) to which was added 500 wL of dodecane keeper and the eluant was then concentrated to 300 uL and submitted for CC/MS analysis for PCDDs. Quality control was carried out by spiking Saaple B with both PCBs and PCDDs. This saaple was selected for spiking since it appeared to be the most contaainated and would thus give a worst case situation for the recovery studies. A replicate and a method blank were also prepared and analyzed. DISCUSSION OP PCDD ANALYSIS The GC/MS analyse* for PCDDs were carried out on a Hewlett Packard S9BSB GC/MS systta uslaf a 30 aetar SE-S4 capillary coluan for the separation prior to mass spectral detection. The ness spec* tremoter was operated In the selected ion aonltoring nods following a/s values characteristic of nonochloro through octachlorodlbenzo* p-dioxln. 1 HONS 220721 No PCDDf were detected' in any of the samples at the detection Halts given In Teble 1. Rasults from the quality control saaplas arc also given. Not* that tha detactlon limit for dichlorodibenzo-p-dioxin were higher than tha spike levels in both tha low lavel and avan tha Men level spike. Therefora no racovery Information could ba given for thesa dichlorodibemo-p-dioxins. For the other PCDDs tha recoveries are not particularly good but in light of how contami nated the samples were and tha short time constraints, these results were considered adequate. DISCUSSION OF PCB ANALYSIS Three saaple extracts, one replicate and two spiked samples ware analyzed for Aroclor formulations. Eight PCB isomers ware quanti fied and froa these levels of Aroclors 124B, 1254, and 1262 were determined. The low Aroclor 124S and 1254 concentrations reported for Sample A may be due to instrument contamination from the the higher concentrations of these Aroclor foraulations present in Samples B and C. The Sample B plus 0.16 wg/g can be treated as a rep licate of Sample B, since tha spiking level is ten times less the amount of Aroclor 124B present in Sample B. Recovery of Aroclor 1?js, added to Sample B at a concentration of 1.6 ug/g, was measured to be 7St. The levels of Aroclor 1254 and 1262 are only order of magnitude estimates, due to the large number of inter fering compounds present. 2 MOMS 220722 TABLE 1. ANALYSIS OF SOIL SAMPLES FOR CHLORINATED DIBENIO- P- DOXINS Sample ID Sample A Sample Sample B (rep) Sample C Blank Method Detection Lini t Spike Level B (spiked) Recovery t Spike Level B (spiked) Recovery 1 ne Diox in/ SoTT (POh) err Clj_ ci. Cl ft "rr C1t ND* ND ND XD ND XD XD ND ND XD ND ND ND XD XD ND XD XD ND ND ND ND ND ND ND XD ND XD XD ND XD ND ND ND XD 2 SO 2 2 2 ? 2 4 343334 3 XD 2 3 2 3 7S - SO 100 67 67 7S IS 34 3S 26 33 32 3S 22 XD IS 20 IS 20 23 63 39 71 4S 63 66 n, ND ND ND ND ND 2 3 2 67 26 12 43 VXD mm detected it the Method detection Halt ft . HONS 220723 TABLE LEVELS OT AROCLOR FORMULATION'S MEASURED IN SAMPLE EXTRACTS Sample ID Concentrations fuc/c) Troclor l:iS Aroclor i:ia Aroclor 1 .'57 Sample A 0,0SSa 0. nis*' <o. n; Sample B Sample B (rep) 7* fl. 06? 0. 0A7 0.0*5 0.04S B - 0.16 ug/g Aroclor HAS o.o6: 0.061 Sample C 1.6 0. is 0.3* B 1.6 -g/g Aroclor HAS 3. Jc 0.10 n.c? Aroclor formulation/g sample. Eight PCB isomers were used to identify the Aroclor formulation and estimate the relative amounts. ^Possible instrument contamination from analysis of Samples I ( c, cThis value for Aroclor 124B concentration represents a recovery of TS1 of Aroclor 124B added to Sample B. MOWS 220724