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3M ModbW Departfnent L%cNdno Huft Physics IndustW Hygiene ToxkmiM 3M CerterBldg.220-2E-02 SL PaulM,N 55144-1000 612f7331110 Analyticaanld ResearcPhroperti-e3sM IndustriHsydgienelabomtory January1993 Scope Thisisa methodforthedeterminatoifoNn-EthyPlerfluorooctanesulfonamide in air. Summary ofMethod: Airisdrawn throughsilicgaelsmpling tubes.The N-Ethyl Perfluorooctanesulfonamidiesadsorbedon the sificgael.The primaryand backup sectionsof thetubesareextractedseparatelwyithmethanol.The liquidisthen analyzedina gas chromatographwithflame ionizatioonr electroncapturedetector. Apt)amtus: I. Silicgaelsamplingtubes(suchas SKC #226-10 or equivalent) Availablefrom: SKC, Inc. 334 ValleyView Road EightFour,PA 15330 2. Sampling pumps: Batteryoperatedpumps capableof drawingairthroughthe sample tubesata rateof 50-500 mi/niin. 3. Gas Chromatograph (suchas Hewlett-Packard5880A or equivalentw)ith capillarcyolumn (RestecStabflwax0.53X 30 ni,I micrometerfilmcapillary column)and flameionizatiodnetector(FM) orelectrocnapturedetector (ECD). SamplinL,Procedure: Sample intheemployee!sbreathingzone ata rateof 50-500 mYnfu4 dependingon desiredlengthof samplingtime. The maximum volume of airsampledper tubeshould be 30 litersL.ocal conditionsuch as veryhighhumiditymay requirea unaller volume. The airflow throughthesampletubeshouldbe as indicatebdy thedirectionalrrow on thetube. At the end ofthesamplingperiod,thetubesshouldbe capped withthesuppliedcaps. Analyticaalnd Research Properties Page 2 January 1993 Analysis: Extaction: Aftersampling,theprimaryand backup sectionsofthesamplipgtubescan be extractedseparatelwyith I ml ofreagentgrade methanolinan maosampling vial and shaken for30 minutes. Analysis:The samples can be injecteidntothegas chromatograph(2 W iqiectiona)nd analyzedby FID or ECD usinga RestecStabUwax 0.53mm IIDX 30 m, I micrometer filmcapillarcyolunul The GC conditionwse used were: 125*C for2 minutes 10*C/minuteto 225*C Hold for 10 minutes InjectoTremperature: 225*C FID Temperature:225*C Under theseconditionstheretentiotnimewas 6.85minutes. The lower quantitatioEnmitwas -10 microgramswithan FID. A lower quantitation limitof -0.1 micrograms was seenwithan ECD. Recovery Study: Fiftyto 1000 micrograms ofN-EthylPerfluorooctanesLffonamiwdaes spikedonto the primarysectionsof silicgaelsample tubes.Thirtyliterosfprecleanedairwas then passedthroughthe sample tubesat 1.0liter/minutlel.e sampleswere analyzedas describedabove. The regressionequationforthestandardmaterialwas: ggs analyte*= 0.0138 analytearea- 15.3for concentrationfsrom 25-1000 ggs (r2-0.99). * N-ethylPerfluorooctanestffonaniide Based on thiscalibratiocnurve,theaveragerecovery95 11%. There was no breakthroughfrom theprimarysectiontso thebackup sectionusnder theconditions describedabove. (SDS127-A&APROP)