Automation of a dual open column chromatographic cleanup technique for samples containing chlorinated dibeno-p-dioxins and dibenzofurans (Technology Transfer Conference, 1991. Proceedings) PDF
Preview Automation of a dual open column chromatographic cleanup technique for samples containing chlorinated dibeno-p-dioxins and dibenzofurans (Technology Transfer Conference, 1991. Proceedings)
_____ L LI 0 L ISSN 0825—4591 PROCEEDINGS L i ENVIRONMENTAL RESEARCH: Is - 1991 TECHNOLOGY TRANFER CONFERENCE November 25 & 26, 1991 J Four Seasons Inn on the Park L J Toronto, Ontario VOLUME II FEATURE PRESENTATIONS L J EMISSIONS AND EFFLUENTS ENVIRONMENTAL TECHNOLOGIES PROGRAM L PREVENTION, TREATMENT AND REMEDIATION TECHNOLOGIES/BIOTECHNOLOGY Is a Sponsored by Research and Technology Branch Environment Ontario Ontario, Canada II s - Lu ________________________ AUTOMATION OF A DUAL OPEN COLUMN CHROSATOGBMHIC CLEANUP TECHNIQUE FOR SAMPLES CONTAINING CHLORINATED DIBENZO-p-DIOXINS AND DIBENZOFURANS — R.T.Taylor. R.S.H.rcer. H.Bonek-Ocie•a nd Z.J.Rsin.r Ontario Ministry of the Environment, Rexdale. Ontario, M9W SL1 — J Au lttreac hntriqaucee tloe vaeulsto m(papteq ) thoef cclhelaonruinpa tsetadg ed iboef nszapm-pp-ledsi oxaninasly z(ePdCD Dfo5)r and dibenzofurans(PCDF5) has been researched by the Ontario Ministry of the Environment (MOE) The Fluid Management System (FMS - Nortech Controls) replaces . a manual two stage open column a J cleanup technique used in the Dioxin Unit. Tuhnea ttPe11n5d euds eda nidn atuhteo mDiaotxicianl lyUn itth raotu gthh e a MOsEe t proofc etswsoe s cofliuvmen ss.a mplTehse first contains three treated silica gel packings and the second — column contains alumina. Two fractions per sample are collected, the first contains polychlorinated biphenyls (Pens) while the second fraction contains PCDDs and PCDFs. this automated system saves the chromatographer a full day in the — sample preparation process. When done manually, the dual column cleanup takes two day; one day per column set with a solvent concentration step in-between columns. The FMS will process one sample extract through two columns in one hour. Samples are run in series, so a sot of five samples takes five hours, Once all — columns are packed and sample extracts and glassware are in place the system is ready to perform the cleanup unattended. This system has been optimized for dioxin and furan recoveries. — These recoveries are equal to or greater than those achieved by manual column chromatography. No carryover has been observed — provided column capacity has not been exceeded. Method __J — Hand packed silica and alumina columns were placed in the positions shown in Figure 1. The first step in this automated cleanup was to wet the columns with hexane before sample addition, When this task was complete the sample wass taken from a roundbottom flask and placed on the column. After sample addition, clean hexane was — pumped from the sovent reservoir into the roundbottom before being eluted through the column. This step rinsed the roundbottom to help maximize surrogate recoveries. Once all hexane rinses passed through the columns (silica and — — alunina) the dioxins and furans were present only on the alumina. Any PCB interferences present were removed with the 2% dichloromethane(DCM):hexane (v/v) elution of the alumina column. The PcDD5 and PCDF5 were then collected by elution with 25% —J ________ I I 0l0i4n:esh exwaenree f(lvu/vs)h.e d Awfittehr hceoxlalneec.t ion was complete all of the cofinOn TABLE 2 puseirncge ntP 345R ecovery of Spiking Solution on Dual Columns Aapvl ualmml vpioiicnfnr ggot phsrceyoo scnsteettsmreosp.ols r cdOoetnmsocca enr cdiaosb n eptwdrro eogwrlaee m rse tah hvacede a drvb raeialenevndde woruesrtwci tiatutleslcneih ndigfn o gart th aeesaa cFhwlMaSe ltsealwm rh ipadcsleha tehtthha. ees M"isas(cepnnuH1 tdire3kh rew-oeoalPtddgcheC hatDed stDt eeo ov clPfsve oasulectlrtonlkahoepatneg cmrd aewtdatec nraedotds5 n .8sg wt9hftae0aresn)annI ecdn c.r tia ariturrogdiSnrnrao iosmleutt ehhdp r aawsoon otfeua u rfgltheryt ho ashbm deeay t sh na tceas ea lpw2ytrcier,rzokra3yelie,u odn 7mv gt,ceh n8afrrcs oro lrruscea iguhasehbe nrdsce d tkcseti oooostuvlcs tuvearo tiermbecybnpdteyt la d e.o wiGs fisC a to-bwhmTEeoth eCrvhreeaeDe run by CC-MS (Finn 4500). zxp.riasnttl 1 A five minute delay before elution of the alumina column was programed into the method to ensure all of the hexane eluted Aamfuone tltolohomopwdtaie tmedwd ize breyemd etmhtohepao ntdincm uoaimzl epRmdlee etcteuho sovisdeni rlgiwi ecasast h/aueols fue smdti hliaiensc a a aP CsbDycaDosstl5ue emmluin nssie( nT gfaa oblorlten h seee2 )t ua(Tupta obomlfe a tthe1ed) 2 oTtfhhfie s tschuoerl rucomognla utmesne ts bpweiafksoe r.es piaTkdhededi twliieotvnhe loasf fotflh yead si2ho% xDeiCxnMts:r haeacxntad n aefs.u rwaenlsl aisn the were approximately 5 to 50 ng of tetra through octa. fl.ultt and DiSCUSSiOn overall the recoveries are acceptable but should be improved to handle high level samples ptpre efficently. The high levels of TABLE i Percent Recovery of Spiking Solution on Silica Columns dioxins and furans in the may have overloaded the columns. using FMS A carryover study was at the sane time. The fraction collected from the cg'Iumn set following the flyash extract contained approximatel/.0.l ng of hexa through octa dioxin. This Volume of I4pxane (mL) works out to be a 0.2%fcarryover. If the volume of hexane used to Isomer rinse to connon lines/is increased the carryover may be eliminated. '1C1,T4CDD 88 Floionke ptruonmiinsgi nogf. thTeh em eatdhvoadn tiasg esst itlol tnheiesd esdy.s temP rialriem isniagrnyi firceasnutlltys "C12P5CDD 56 73 reduced preparation times as well as the reduced human exposure to highly toxic chemicals. "CH6CDD 65 "C13H7CDD 67 101 63 75 H 713 712 S D U)*J RflJATE COLA C C HL RE LI C SU SI OF PRES CIOR U TION OVER DETE A L O :S U R O F E NIQUANS w4s U HR u CU L TEOF cc NE A U DISED ALUMIN N A S N XI O DI P- O Z 8flJ DI 1 E FIGUR PCRZ S N % XI 25 O DI U U (7099) TD/5/143
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