玻璃器皿及实验操作

InstrumentandExperimentOperation实验仪器及实验操作Partone:StandardLaboratoryGlasswarebeaker(awidecylindricalglassvessel,usedasalaboratorycontainerandmixingjar.)testtube(acylindricalglasstubeusuallyopenatoneendandroundedattheother,usedinlaboratoryexperimentation.)testtubeclamp/testtubeholderalcoholburner/alcohollamp（Alampthatburnsalcoholorotherliquidfuel.）measuringcylinder/graduatedcylinderevaporatingdishironstandbalancethermometer(aninstrumentformeasuringtemperature.)funnel（usedtochanneltheflowofasubstance,asintoasmall-mouthedcontainer.）droppingfunnelSeparatingfunnel/separatoryfunnelBuchnerfunnelfilterflask(suctionflask)beakerflask/conicalflaskround-bottomedflaskBunsenflask/Florenceflaskvolumetricflask/measuringflaskcondensertube/condenserpipegaswashingbottlepipette/pipet（Anarrow,usuallycalibratedglasstubeintowhichsmallamountsofliquidaresuctionedfortransferormeasurement.）burette/buret（Auniform-boreglasstubewithfinegradationsandastopcockatthebottom,usedespeciallyinlaboratoryproceduresforaccuratefluiddispensingandmeasurement.）acidburettealkaliburettecrucible（Avesselusedformeltingandcalciningmaterialsathightemperatures.）benchstopcock（Adevicethatregulatestheflowoffluidthroughapipe）stopperfilterpaper（Porouspapersuitableforuseasafilter）Parttwo:instrumentinfrareddryervacuumdryingovenconstanttemperaturewaterbathpHmeterrotaryevaporatormufflefurnaceparticlesizeanalyzer红外干燥箱真空干燥箱恒温水浴PH计旋转蒸发仪马弗炉粒度分析仪AtomicEmissionSpectrometer（AES）原子发射光谱仪Ultraviolet-VisibleSpectrophotometer（UV-Vis）紫外-可见光分光光度计AtomicAbsorptionSpectroscopy（AAS）原子吸收光谱仪AtomicFluorescenceSpectroscopy（AFS）原子荧光光谱仪FourierTransformInfraredSpectrometer（FTIR）傅立叶变换红外光谱仪FT-RamanSpectrometer傅立叶变换拉曼光谱仪GasChromatograph（GC）气相色谱仪HighPressure/PerformanceLiquidChromatograph（HPLC）高压/效液相色谱仪IonChromatograph离子色谱仪X-RayFluorescenceSpectrometer（XRF）X射线荧光光谱仪X-RayDiffractometer（XRD）X射线衍射仪EnergyDisperseSpectroscopy（EDS）能谱仪MassSpectrometer（MS）质谱仪GC-MS气相色谱-质谱联用仪NuclearMagneticResonanceSpectrometer（NMR）核磁共振波谱仪heat加热cool冷却dissolve溶解dry干燥stir搅拌filter过滤dilute稀释titrate滴定purify纯化Partthree:ExperimentOperationseparate分离extract萃取treat处理evaporate蒸发reflux回流crystallize结晶precipitate沉淀centrifugalize离心distill蒸馏eg.DistillationGuideOverview:»Distillationisanextremelyusefultechniquethatisusedtopurifyreagentsandseparatecrudeproductmixtures.Therearetwovarietiesofdistillation-atmosphericpressureandreducedpressure.Theformeriseasier,whilethelatterinvolvessomemorecomplicatedtechniques.Glassware:»Distillationsrequirespecialglasswarethatisuniquetothistechnique.Thereareseveraltypesofset-ups,butwewilluseonlytwo.Inbothcaseswewilluseashortpathdistillationhead，varyingonlyintheuseofaVigreuxcolumn.Eventhoughwewon'tuseotherset-upsin5.301,youshouldbecomefamiliarwiththemthroughyourreading.StepsforRunninganAtmosphericPressureDistillation:»1)Collectthenecessaryglassware:shortpathdistillationhead,thermometerandadapter,receivingflasks(atleasttwo),Vigreuxcolumn.»2)Preheatoilbathorheatingmantle.Iftheboilingpointisunknown,thisstepshouldbeomitted.Keepinmindthatformostdistillationstheheatingapparatusmustbe20–30°Chigherthantheboilingpointofthedistillate.Note:Duetothermalbreakdownandpossibleignition,oilbathsareonlyusefulfortemperaturesbelow200°C.»3)Recordweightoflabeledreceivingflasks.»4)Putcompoundtobedistilledinaround-bottomedflaskwithstirbar.(Thestirbarwillpreventbumping.)Thesizeoftheroundbottomflaskisveryimportant.Itshouldberoughlyhalftotwo-thirdsfull;anyhigheranditmayboiloverprematurely,anylessanditmaytaketoolongtodistill.»5)Assembleglassware,makingsurealljointsaresnug.Alargeassemblyofglasswareshouldinvolveatleasttwoclamps-whenindoubtusemoreclamps!Also,nojointgreaseisnecessaryforatmosphericpressuredistillations.(Note:forairorwatersensitivecompoundstheapparatusshouldbeflamedriedanddistilledunderN2orAr.)»6)Insulatethecolumn.WhenusingaVigreuxcolumn,itshouldbewrappedwithglasswoolandaluminumfoil.Withoutinsulation,theseset-upstendtotakeaverylongtime.»7)Connectthecondensertothewaterlines,turnonthewater,andcheckforleaks.»8)Raisethestirplateandheatingapparatustotheflaskandbeginheating.Note:Variacgaugesdonotcorrespondtotemperature.Settingthedialat70willnotheatyouroilbathto70°C-itwillactuallygomuchhigher.Also,differentoilbathsandheatingmantleswillheattodifferenttemperaturesatthesameVariacsettings.»9)Lowerthehoodsash.Thisisalwaysagoodpracticeincaseofaccident,butitalsokeepsthedistillationapparatusawayfromtheairconditioningofthelab.Thiswillcoolyourset-upandmakeyourdistillationtakelonger.»10)DONOTHEATTOOQUICKLY!!!Patienceisthekeytodistillation.»11)Slowlyincreasethetemperatureoftheheatingapparatusuntilthesolutionisrefluxing.»12)Waittoseethedistillationthermometerrespond.Ifnothinghappensafterabout10minutesthenraisethetemperatureslightly.»13)Repeatstep#12untilyouseethedistillationthermometerrespond.Oncethishappens,preparetocollect.»14)Trytokeeptheapparatusataconstanttemperature-atleastwithin5degreesofthetemperaturewhenthedistillationthermometerregistered.»15)Collectuntiladramaticchan