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1、10.6.09acetoneandfollowwith$3rinsingswithhexaneorAOACOfficialSurplusMethod958.08iisooctane,accordingtouse.Allacetonemustbep-ChlorophenylPhenylSulfoneremoved.CleanheavilycontaminatedglasswarewithchromicacidcleaningsolnfollowedbythororinsingPesticideResidueanddrying.Sp
2、ectrophotometricMethod29.077ReagentsFinalAction1965(a)Hexane.—Bp60–70E(SkellysolveBorSurplus1969equiv.).(b)Isooctane.—Puregrade,2,2,4-trimethylpentane(PhillipsPetroleumCo.,orEnjayCo.,11thed.Inc.,60W.49thSt,NewYork,NY10020).Aat230,240,and250nmagainstHOshouldbe2#0.100;
3、29.075Principlesotherwisepurifybyshaking15minwith5gsilicagel(28–200mesh)foreach100mLing-sbottle.KeepinTech.gradeSulphenonecontainsca80%p-dark;filterwhenneeded.SampleandstdAaredetdchlorophenylphenylsulfone(p-CIDPS);theremainderagainstisooctaneblank.Solv.inbothcellsmus
4、tbeconsistsalmostentirelyofrelatedsulfones,bis(p-fromsamebatchoffilteredsolv.chlorophenyl)sulfone(p,pN-CIDPS)anddiphenyl(c)Ethylether,anhydrous.—(MallinckrodtA.sulfone(DPS).R.orequiv.).Evap.20mLat40–50EanddissolveHexanestripsolnsareextdwithCHCN3residuein20mLisooctane
5、.Aat230,240,and250nmwhichsepsSulphenonecomponentsfrombulkofagainstisooctaneshouldbe#0.020.DifferentialA,A240waxes,coloringmatter,andtosomeextentfromotherpesticides.TheCHCNresidueischromatographedon—0.5(A230+A250),shouldbe#±0.003.3(d)Hexane-ethersolventmixture.—Distil
6、lMagnesolcolumnwithhexane-anhyd.ether.Thehexane,rejectingfirst5%andlast10%.Mix700mLresidueoffractioncontgp-CIDPSisdissolvedinhexanewith300mLanhyd.ether.Storeing-sbottle.isooctanefordetnofUVA.(e)Acetonitrile.—Practicalgrade.Magnesolcolumnsepsp,pN-CIDPS,(f)Magnesol.—In
7、dustrialregulargrade(FMCp-CIDPS,andDPSinthatorder.DDT,TDE,Corp.,InorganicChemicalsDiv.,6333rdAve,Newmethoxychlor,andotherhighlyabsorbingpesticidesareYork,NY10017).Mixbathbytumblinginlargejar.elutedwithinthresholdvol.forp-CIDPS.AfewKeepinsmall,tightlyclosedcontainers.
8、pesticides(phenothiazineandmalathion),whenpresent(g)Sulphenonestdsoln.—0.5mg/mL.inamtswellovertheirtolerances,showslightDissolve50m
