AOAC41.1.69AOACOfficialMethod999.02OilinOilseeds.pdf

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41.1.69Beforeinitialuseoftheextractorandperiodicallythereafter,ex-AOACOfficialMethod999.02tractreplicate400mgtestportionsofsoybeanoilongranularOilinOilseedsdiatomaceousearthusingthedesiredsetofconditionsanddryingSupercriticalFluidExtraction(SFE)Methodproceduretoverifyequipmentcondition,collectionefficiency,andFirstAction1999procedure.Recoveryoftheoilshouldbe>99%andnooilaerosolshouldbeobservedrisingabovetheglasswoolduringextraction.AOCS–AOACMethod(b)Extractioncells.—5–10mLinternalvolume.(c)Glassextractcollectionvessels.—Suitableforextractionsys-(Applicabletodeterminationofoilcontentofsoybeans,cottonseed,tem.Vesselsmustbecapableofholding³1.0glooselypackedglasscanolaseed,safflowerseed,andsunflowerseed.)wool.(d)Analyticalbalance.—Accurateto±0.0001g.Caution:SFEusescompressedgasesasanextractionfluid.See(e)Vacuumovenandpump.—MaintainingdryingconditionsasAppendixB,LaboratorySafety,forsafehandlingandoutlinedin926.12(see41.1.02)withpermissibleoventemperaturestorageofcompressedgascylinders.SFEequipment20–25°CabovebpofH2Oatworkingpressure£100mmHgmustbeconstructedandmaintainedinproperworking(13.3kPa;72–77°±1°Cat100mmHgworkingpressure;ordertominimizethechanceofanyexplosivedecom-58–63°±1°Cat50mmHgworkingpressure).pressionofextractionfluid.AlthoughCO2isanon-(f)Forced-airoven.—Operatingat130±1°C.Useifvacuumtoxicgas,adequateventilationinthelaboratorymustovenisnotavailable.bemaintainedtoavoidthepossibilityofdisplacingtoomuchoxygen.Adequateventilationmustalsobemain-C.Reagentstainedwhenusingmodifierstoavoidthetoxiceffects(a)Carbondioxide.—Weldingorindustrialgradewithdiptube.ofbreathingorganicvapors.PurergradesofCOmaybeused,butarenotrequired.2(b)Ethanol,absolute.—HPLCgradeorequivalent;moistureSeeTables999.02A–Cfortheresultsoftheinterlaboratorystudycontent<1mg/kg.Denaturingsolventtypeisunimportant.TMsupportingtheacceptanceofthemethod.(c)Diatomaceousearth,granular.—Hydromatrix(SamplePreparationProducts,24201FramptonAve,HarborCity,A.PrincipleTMCA90710,USA),WetSupport(Isco,4700SuperiorSt,Lincoln,OilisextractedfrompreparedoilseedwithasupercriticalfluidNE68504,USA),orLecoDryTM(LecoCorp.,3000LakeviewAve,(liquidCO2)anddepositeddirectlyontoglasswoolcontainedinaSt.Joseph,MI49085,USA),orequivalent,aresuitable.collectionapparatus.Afterevaporationofmoistureandanyresidual(d)Glasswool.—Borosilicateglass.modifierfromglasswoolandcollectionapparatus,theweightofex-tractedoilisdeterminedandusedtocalculatethepercentoilintheD.Determinationtestsample.(a)CO2-onlyextractiontosimulateplantprocessextrac-tion.—PreparetestsampleasdescribedinsectionAoftheAOCSB.ApparatusOfficialMethodsandRecommendedPractices,5thEd.,American(a)Supercriticalfluidextractor.—ProducingapressureofOilChemists’Society,Champaign,IL,USA,usingthemethodspe-51.7kPaandatemperatureof100°C;equippedwithaheatedcificforoilseedbeinganalyzed.restrictor(adjustableorfixedflow)keepingthetemperatureoftheAccuratelyweigh2±0.0001gtestportionintoextractioncell,evolvingCO2above40°C.ForextractionswithCO2+15%ethanol,B(b),withoutletendcapinplace.Tapcellseveraltimesonworksur-useanon-linemodifierpump.LowoilvaluescanresultfromleaksfacetopackmaterialintoanevenlypackedpluginoutletendoftheintheSFEinstrumentorinefficientcollectionoftheextractedoil.cell.Uppersurfaceofplugshouldbeeven.FillremainingvoidinTable999.02AInterlaboratorystudyresults(17laboratories)ofAOCSSFEMethodAm3-96usingCO2alonefordeterminationofoilcontentofoilseedsaStudysampleoilseedLabsacceptedNo.ofoutliersxsrrsRRRSDr,%RSDR,%A/M(Soy4)14319.20.300.830.451.271.62.4E/I(Soy7)14319.20.902.510.912.554.74.8G/R(Sun1)15238.91.022.861.684.702.64.3C/P(Sun3)15241.61.654.622.306.454.05.5K/Q(Can4)15239.80.451.260.902.511.12.3D/J(Can3)15237.70.671.881.032.891.82.7B/S(Saf2)14336.61.392.251.664.653.84.6H/N(Saf1)14335.70.862.401.083.032.43.0F/T(Cot1)14319.10.461.280.511.442.42.7L/O(Cot2)14318.40.340.950.381.061.92.1aOilseedsfrom1995–1996AOCSSmalleyLaboratoryProficiencyProgram.Soy,soybean;Sun,sunflower;Can,canola;Saf,safflower;Cot,cottonseed.©2002AOACINTERNATIONAL Table999.02BInterlaboratorystudyresults(15laboratories)ofAOCSSFEMethodAm3-96usingCO2withEtOHmodifierfordeterminationofoilcontentofoilseedsaStudysampleoilseedLabsacceptedNo.ofoutliersxsrrsRRRSDr,%RSDR,%A/M(Soy4)12320.50.431.190.772.162.13.8E/I(Soy7)13220.40.581.630.872.432.94.3G/R(Sun1)12339.70.441.221.654.631.14.2C/P(Sun3)12343.00.631.781.644.591.53.8K/Q(Can4)12343.50.371.041.323.680.93.0D/J(Can3)14140.20.862.421.434.002.23.6B/S(Saf2)12338.00.772.151.143.182.03.0H/N(Saf1)12336.70.671.861.484.151.84.0F/T(Cot1)12319.70.180.500.521.460.92.7L/O(Cot2)14119.30.350.980.521.461.82.7aOilseedsfrom1995–1996AOCSSmalleyLaboratoryProficiencyProgram.Soy,soybean;Sun,sunflower;Can,canola;Saf,safflower;Cot,cottonseed.cellwithgranulardiatomaceousearth,C(c).Wipeanyspilledfilleradditionalglasswooltoensuredeeppositioningoftherestrictorormaterialfromoutsideofextractioncell.transfertubewithintheglasswool.Take³1gglasswool,C(d),andpackintoeachcollectionvessel,Loadeachextractioncellontheinstrumentreel(automatedsys-B(c),untiltopofresultingplugisatleast2.5cmfrombottomofves-tem),orinstalleachextractioncellontotheextractor(manualload-sel.Accuratelyweighcollectionvesselwithglasswooltoingsystem).Orientthecellssothattestportionisintheoutletend.±0.0001g.(Note:CapsorseptaoncollectionvesselarenotrequiredExtractfor30minwithCO2underthefollowingconditions:unlesstheSFEinstrumentrequirestheiruse.)51.7kPa;100°C;nominalliquidflowrate,3.4g/min(2.6–3.4g/minInstalleachcollectionvesselonthecollectionreeloftheextractorispermissible);andrestrictortemperaturesuchthatCOevolvesat2(automaticsystem)orinstalleachcollectionvesselwiththebetween80–100°C(40–130°Cisacceptable).ThetemperatureofrestrictorortransfertubeleadingfromtherestrictorinsertedastheexpandingCO2inthecollectionvesselwilldirectlyaffectthedeeplyaspossibleintotheglasswoolplug(manualloadingsystem).amountofmoistureand/ormodifierentrainedintheextractedoilSomeinstrumentsmayrequireadjustmentoftherestrictordepthorTable999.02CComparisonofmethods:SFEversussolventextractionaOilseedandmethodxsrrsRRSDr,%RSDR,%Soybean4SFE-CO2alone19.20.300.0830.451.62.4SFE-CO2+15%ethanol20.50.431.190.772.13.8bAOCSAc3-4419.00.030.080.360.21.9Soybean7SFE-CO2alone19.20.902.510.914.74.8SFE-CO2+15%ethanol20.40.581.630.872.94.3bAOCSAc3-4419.30.050.140.390.32.0Sunflowerseed1SFE-CO2alone38.91.022.861.682.64.3SFE-CO2+15%ethanol39.70.441.221.651.24.2bAOCSAi3-7538.50.100.281.240.33.2cAOCSAm2-9341.8Sunflowerseed3SFE-CO2alone41.61.654.622.304.05.5SFE-CO2+15%ethanol43.00.631.781.641.53.8bAOACAi3-7542.70.090.250.500.21.2cAOCSAm2-9346.0aOilseedsfrom1995–1996AOCSSmalleyLaboratoryProficiencyProgram.bSolventextraction,Butttubeextractionmethod,AOCSOfficialMethodsappropriatetooilseed,SmalleyLaboratoryProficiencyProgramresultsfor1995–1996.cSolventextraction,AOCSOfficialMethodAm2-93,FOSFAInternationalmethod.©2002AOACINTERNATIONAL andthesubsequenttimerequiredtoremoveitbeforetheweightcan3mmtotightenpackingandinstallinletendcap.Extractfor60minbedetermined.Overheatingcancauselossofthemorevolatileoils.withCO2+15%ethanol,C(b),underthefollowingconditions:Consultinstrumentmanufacturerforrestrictor/collectiontempera-51.7kPa;100°C;nominalfluidflowrate,2.1g/min(1.6–2.6g/minturesettingsthatwillminimizemoisture(andmodifier,ifused)re-ispermissible);andrestrictortemperaturesuchthatCO2evolvesatmovaltime.AlowerexpandingCO2temperaturemaybeusedwithbetween80–100°C(40–130°Cisacceptable).Seecommentsoninstrumentsthatincludeheatingofthecollectionvessels.Somein-restrictor/collectiontemperatureinprocedureforCO-onlyextrac-2strumentsmaynotrequiresubsequentremovalofmoistureormodi-tion.Removeeachcollectionvesselfrominstrumentand,ifneces-fierfromtheextract.Verifybydryingtheextractsaccordingtosary,removeresidualmoisturebydryingtoconstantweightas926.12(see41.1.02)toensurethatnosignificantweightlossisob-describedaboveforCO-onlyextraction.Recordfinalcollection2servedbeforeeliminatingthedryingstep.vesselweightto±0.0001g.Removeeachcollectionvesselfromtheinstrumentand,ifneces-E.Calculationssary,removeresidualmoisturebydryingtoconstantweightusingvacuumoven,B(e),(preferred),orforced-airoven,B(f),withrec-Calculatepercentoilasfollows:ommendedtemperaturesandpressures.Recordfinalcollectionves-selweightto±0.0001g.Oil,%=100(b)CO2+15%ethanolextractiontosimulateexhaustiveextrac-tion.—Preparetestsample,weightestportionintoextractioncell,Reference:AOCSOfficialMethodsandRecommendedPractices,andprepareandinstallextractioncellandcollectionvesselinthe5thEd.,1988,AmericanOilChemists’Society,Cham-SFEinstrumentasdescribedabovefortheCO2-onlyextraction.Af-paign,IL61826,USA,OfficialMethodAm3-96.terfillingcellvoidwithdiatomaceousearth,depressuppersufacecaRevised:March2002©2002AOACINTERNATIONAL