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1、10.3.01calmodificationofFPDtocorrectaboveproblemsareavailablefromAOACOfficalMethod974.22«DivisionofChemistryandPhysics,U.S.FoodandDrugAdministra-OrganophosphorusPesticideResiduestion,Washington,DC20204USA.)Usehighlystabilized0–750VdcCarbonColumnCleanupMethodvariable
2、powersupplycapableof10maoutput(KeithleyInstruments,FirstAction1974Inc.,28775AuroraRd,Cleveland,OH44139USA,orequivalent),FinalAction19766.3Vacignitorpowersupply,electrometerwithbuckingcapabilityofSurplus1994-61´10A(TracorInstruments,Inc.,orequivalent),andvariabletran
3、sformercapableofdelivering150wattstocontroltemperature(CH3CNextractionandcharcoalcleanupcolumnusingKClthermi-offlamehousing.Stripchartrecordershouldbecompatiblewithonicorflamephotometricdetectorforresiduesofparathion,electrometer.paraoxon,carbophenothionanditsOanalo
4、g,andEPNonapplesandgreenbeans.)(f)Hydrogen.—FromcylinderofcompressedH2gas.Equipcyl-inderwithregulator,deliveryline,andvariableflowcontrollercapa-A.Reagentsbleof200mL/mindelivery.Meteringshut-offvalveisrequired(a)Solvents.—Redistilledfromglass(see970.52A[seeseparatef
5、romcontroller.10.1.01]):ethylacetate,CH2Cl2,benzene,hexane,CH3CN,and(g)Air.—Cylinderofcompressedairequippedasin(f)todeliverisopropanol.upto100mL/min.Separateshut-offvalveisnotneeded.(b)Acid-treatedcharcoal.—Slurry200gacid-treatedchar-(h)Oxygen.—CylinderofcompressedO
6、2gasequippedasin(f)coalwith500mLHCl,coverwithwatchglass,andstirmagneti-todeliverupto50mL/min.Combinewithairusingstandardcallywhileboiling1h.Add500mLH2O,stir,andboiladditionalSwagelokteebeforedetectorinlet.30min.CollectcharcoalinBüchnerandwashwithH2Ountil(i)Flamephot
7、ometricdetectoroperation.—Adjusttemperaturewashingsareneutraltouniversalindicatorpaper.Dryat130°Cinofburnerhousingtoca170–180°Cbeforeignitingflame.Tempera-forced-draftoven.turewillrise20–30°Cafterignition.Donotallowdetectortoexceed(c)Magnesiumoxide.—See970.52B(k)(se
8、e10.1.01).220°C.Adjustgasflowsatcontrollerstoca150–300mL/minH2,(d)Adsorbentmixture.—Mixonepartacid-treatedcharcoal,50–100mL/minair,and5–20
