丙酮EP80

EP8.0各论：丙酮01/2008:0872(中英文）EP7.001/2008:0872ACETONE丙酮C3H6O[67-64-1]Mr58.08【定义】Propanone丙酮。【CHARACTERS性状】Appearance:volatile,clear,colourlessliquid外观：挥发性、澄清，无色液体。Solubility:misciblewithwaterandwithethanol(96%percent).溶解性：与水和乙醇（96%）互溶。Thevaporisflammable.蒸气易燃。【IDENTIFICATION鉴别】A.Relativedensity(seeTests)A：比重（见检查项）。B.To1mL,add3mLofdilutesodiumhydroxidesolutionRand0.3mLofa25g/LsolutionofsodiumnitroprussideR.Anintenseredcolurisproducedwhichbecomesvioletwiththeadditionof3.5mLofaceticacidR.B：于1ml样品中，加3ml稀氢氧化钠溶液（R），0.3ml的25g/L硝普钠（亚硝酰铁氰化钠）（R）溶液。应呈深红色，加3.5ml醋酸（R）后变为紫色。稀氢氧化钠溶液配制方法：SodiumHydroxideSolution,DiluteAn8.5%w/vsolutionofsodiumhydroxide(about2M).硝普钠：SodiumNitroprussideSodiumpentacyanonitrosylferrate(III)dihydrate;Na2[Fe(CN)5(NO)],2H2O=298.0(13755-38-9)Analyticalreagentgradeofcommerce.Reddishbrownpowderorcrystals）C.To10mLofa0.1percentV/Vsolutionofthesubstancetobeexaminedinethanol(50percentV/V)R,add1mLofa10g/LsolutionofnitrobenzaldehydeRinethanol(50percentV/V)Rand0.5mLofstrongsodiumhydroxidesolutionR.Allowtostandforabout2minandacidifywithaceticacidR.Agreenish-bluecolourisproduced.C：取10ml的0.1%（V/V）样品在乙醇中（50%V/V）（R）稀释液，加1ml的10mg/L对硝基苯甲醛（R）乙醇（50%V/V）溶液，加0.5ml浓氢氧化钠溶液（R）。放置约2分钟，用醋酸（R）酸化，应显蓝绿色。浓氢氧化钠溶液（R）：SodiumHydroxideSolution,StrongA42%w/vsolutionofsodiumhydroxide(about10M).【TESTS检查】Appearanceofsolution.To10mLadd10mLofwaterR.Thesolutionisclear(2.2.1)andcolourless(2.2.2,MethodII).溶液外观：取10ml样品，加10ml水，溶液应澄清（附录2.2.1）无色（附录2.2.2，方法Ⅱ）。Acidityoralkalinity.To5mLadd5mLofcarbondioxide-freewaterR,0.15mLofphenolphthaleinsolutionRand0.5mLof0.01Msodiumhydroxide.Thesolutionispink.Add0.7mLof0.01Mhydrochloricacidand0.05mLofmethylredsolutionR.Thesolutionisredororange.酸碱度：取样品5ml，加5ml无二氧化碳的水（R），0.15mL酚酞试液（R）与0.5ml的0.01M氢氧化钠，溶液显粉色。加0.7ml的0.01M盐酸，0.05ml甲基红指示液（R），溶液显红色或橙色。酚酞试液：PhenolphthaleinSolutionDissolve0.1gofphenolphthaleinRin80mlofalcoholRanddiluteto100mlwithwaterR.Complieswiththefollowingtest.TestforsensitivityTo0.1mlofthephenolphthaleinsolutionadd100mlofcarbondioxide-freewaterR.Thesolutioniscolourless.Notmorethan0.2mlof0.02Msodiumhydroxideisrequiredtochangethecolourtopink.ColourchangepH8.2(colourless)topH10.0(red)甲基红试液：MethylRedSolutionDissolve50mgofmethylredinamixtureof1.86mlof0.1Msodiumhydroxideand50mlofethanol(96%)andaddsufficientwatertoproduce100ml.Complieswiththefollowingtest.SensitivityAmixtureof0.1mlofthesolution,100mlofcarbondioxide-freewaterand0.05mlof0.02MhydrochloricacidVSisred.Notmorethan0.1mlof0.02MsodiumhydroxideVSisrequiredtochangethecolourofthesolutiontoyellow.ColourchangepH4.4(red)topH6.0(yellow).Relativedensity(2.2.5):0.790to0.793.比重（附录2.2.25）：0.790~0.793Reducingsubstances.To30mLadd0.1mLof0.02Mpotassiumpermanganateandallowtostandinthedarkfor2h.Themixtureisnotcompletelydecolorized.还原性物质：取样品30ml，加0.1ml的0.02m高锰酸钾，在黑暗中放置2小时，混合物不得全褪色。Relatedsubstances.Gaschromatography(2.2.28).有关物质：气相（附录2.2.28）Testsolution.Thesubstancetobeexamined.供试液：待检样品Referencesolution(a).To0.5mLofmethanolRadd0.5mLof2-propanolRanddiluteto100.0mLwiththetestsolution.Dilute1.0mLofthissolutionto10.0mLwiththetestsolution.对照液（a）：取0.5ml异丙醇（R）加于0.5ml甲醇（R）中，用供试液稀释至100.0ml。移取1.0ml用供试液稀释至10.0ml。Referencesolution(b).Dilute100uLofbenzeneRto100.0mLwiththetestsolution.Dilute0.20mLofthissolutionto100.0mLwiththetestsolution.对照液（b）：取100μL苯（R）于100.0mL容量瓶，用供试液稀释至刻度。移取0.20ml该溶液用供试液稀释至100.0ml。Column:色谱柱：--material:fusedsilica,——色谱柱材料：熔融石英--size:l=50m,D=0.3mm——尺寸：l=50m，D=0.3mm--stationaryphase:macrogol20,000R(filmthickness1um).——固定相：聚乙二醇20000R（膜厚1μm）Carriergas:heliumforchromatographyR.载气：高纯氦气（HeliumHe=4.003(7440-59-7)Laboratorycylindergradeofcommercecontainingnotlessthan99.995%v/vofHe）.Linearvelocity:21cm/s.线速度：21cm/sSplitration:1:50分流比：1：50Temperature升温程序Time时间（min分钟）Temperature温度（℃）Column柱温0-1145→10011-20100Injectionport进样口150Detector检测器250Detection:flameionization.检测器：FIDInjection:1uL.进样量：1μLRetentiontime:impurityC=about7.5min保留时间：杂质C（苯）=约7.5分钟Systemsuitability:系统适用性：--resolution:minimum5.0betweenthepeakduetoimpurityA(2ndpeak)andthepeakduetoimpurityB(3rdpeak)inthechromatogramobtainedwithreferencesolution(a).——分离度：对照液（a）中杂质A（第2个峰）与杂质B（第3个峰）分离度不小于5.0--signal-to-noiseration:minimum5forthepeakduetoimpurityCinthechromatogramobtainedwithreferencesolution(b).——信噪比：对照液（b）色谱图中杂质C（苯）的信噪比不小于5。Limits:限度--impuritiesA,B:foreachimpurity,notmorethanthedifferencebetweentheareasofthecorrespondingpeaksinthechromatogramobtainedwithreferencesolution(a)andtheareasofthecorrespondingpeaksinthechromatogramobtainedwiththetestsolution(0.05percentV/V).——杂质A，B：各杂质峰面积不大于对照液（a）色谱图中相应峰面积与供试液色谱图中对应峰面积差值（0.05%V/V）--impurityC:notmorethanthedifferencebetweentheareaofthepeakduetoimpurityCinthechromatogramobtainedwithreferencesolution(b)andtheareaofthecorrespondingpeakinthechromatogramobtainedwiththetestsolution(2ppmV/V).——杂质C（苯）：杂质C面积不大于对照液（b）色谱图中杂质C峰面积与供试液色谱图中杂质C面积差值（2ppmV/V）--anyotherimpurity:foreachimpurity,notmorethanthedifferencebetweentheareaofthepeakduetoimpurityAinthechromatogramobtainedwithreferencesolution(a)andtheareaofthecorrespondingpeakinthechromatogramobtainedwiththetestsolution(0.05percen