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项目八:常规物理常数与性能分析任务一:粒径的测定粒径的测定课程:工业分析中文Scenario8:PhysicalconstantsandperformancetestingTask1:DeterminationofparticlesizeDeterminationofparticlesizeCourse:IndustrialAnalysisEglish定义:粒径是指固体物质颗粒的大小
。粒径的测定方法有多种,根据测定要求的不同,可选择不同的方法,一般有筛分法、微粒度测定法等。
只能测定粒径范围可以测粒径分布和平均粒径中文Definition:Particlesizereferstothesizeofsolidmaterialparticles.Therearevariousmethodsformeasuringparticlesize,anddifferentmethodscanbeselectedaccordingtodifferentmeasurementrequirements,generallyincludingsievingmethod,particlesizemeasurementmethod,etc.CanonlymeasureparticlesizerangeCanmeasureparticlesizedistributionandaverageparticlesizeEglish1、方法原理利用系列筛孔尺寸不同的筛网来测定颗粒粒度的分布,将筛网按孔径大小依次叠好,把被测试样从顶上倒入,盖好筛盖,置于振筛器上振荡(或人工振筛),使试样通过一系列的筛网,然后在各层筛网上收集,通过称量各筛网中留存的试样的质量,以粒度来表示一定的粒径范围的颗粒质量占总试样质量的百分数。一、筛分法测定粒径中文1、MethodprincipleThesievingmethodusesscreenswithdifferentmeshsizestodeterminethedistributionofparticlesize.Whenmeasuring,stackthesievemeshinorderofporesize,pourthetestedsamplefromthetop,coverthesievecover,andplaceitonthevibratingscreentoshake(ormanuallyshake),sothatthesamplepassesthroughaseriesofsievemeshes,andthencollectoneachlayerofsievemesh.Byweighingthemassoftheretainedsampleineachsievemesh,thepercentageofparticlemasswithinacertainparticlesizerangetothetotalsamplemassisrepresentedbyparticlesize.一、DeterminationofparticlesizebysievingmethodEglish2、仪器孔径分别为1.0mm、2.0mm、2.8mm、4.0mm等的筛网一套,并附有筛盖和底盘,如图所示,振筛器(没有振筛器则采用人工振筛)及托盘天平。筛网筛盖和底盘中文2、InstrumentAsetofscreenswithaperturesof1.0mm,2.0mm,2.8mm,4.0mm,etc.,equippedwithscreencoversandchassis,asshowninthefigure.Thevibratingscreen(ifthereisnovibratingscreen,manualvibratingscreenwillbeused)andatraybalancewillbeused.screenmeshscreencoverandchassisEglish3、筛网目数与尺寸对应关系
中文3、TherelationshipbetweenthenumberofsievemeshanditssizeMeshcountmicronEglish4、测定步骤称取试样适量(一般200g),精确到1g。将筛网按孔径大小依次叠好(若仅测定规定粒度范围的测定,只在用两个确定孔径的筛网),孔径大(4.0mm)的在上层,小的在下层。试样置于孔径最大的筛网上,盖好筛盖。将筛网置于振筛器上,夹紧,振荡5min。称量未通过4.0mm孔径筛网的试样及底盘上的试样(通过所有筛网的小颗粒物),精确到1g。
中文4、MeasurementstepsWeighanappropriateamountofthesample(usually200g),accurateto1g.Stackthesievesinorderofporesize(ifonlymeasuringthespecifiedparticlesizerange,onlytwosieveswithdeterminedporesizesareused),withthelargerporesize(e.g.4.0mm)ontheupperlayerandthesmalleroneonthelowerlayer.Placethesampleonthesievewiththelargestporesizeandcoveritwiththesievecover.Placethesieveontheshaker,clampit,andoscillatefor5minutes.Weighthesamplethatdidnotpassthe4.0mmaperturesieveandthesampleonthechassis(smallparticlespassingthroughallsieves),accurateto1g.Eglish5、数据处理
中文5、Resultcalculation
Theparticlesizeofthesampleisexpressedasthefractionofparticleswithamassof1-4mmtothetotalmassofthesample:D--Theparticlesizeofthesample;m--Massofthesample,g;m’--Thesumofthelargeparticlesamplethatdidnotpassthe4mmaperturesieveandthesmallparticlesamplethatpassedallsieves,gEglish1、方法原理
固体质点在液体介质中的沉降速度因质点直径大小不同而不同,通过离心力的作用,加速固体质点的沉降速度,固体质点按粒径大小先后到达仪器的光束位置而被检测器检测。二、微粒度仪法(离心沉降法)中文1、Methodprinciple
Thesettlingspeedofsolidparticlesinliquidmediavariesdependingontheparticlediameter.Throughtheactionofcentrifugalforce,thesettlingspeedofsolidparticlesisaccelerated.Solidparticlesreachthebeampositionoftheinstrumentinorderofparticlesizeandaredetectedbythedetector.二、Particlesizeanalyzermethod(centrifugalsedimentationmethod)Eglish2、操作要点(1)试样的分散选择合适分散剂如乳化剂制成稳定的悬浮液(2)沉降液的选择密度、黏度合适,密度应低于固体密度且不使固体颗粒溶胀,常用水、甘油水、蔗糖水为沉降液中文2、Operationpoint(1)DispersionofsamplesChooseappropriatedispersantssuchasemulsifierstocreatestablesuspensions(2)SelectionofsettlingsolutionThedensityandviscosityofthesettlingsolutionareappropriate,andthedensityshouldbelowerthanthesoliddensitywithoutcausingthesolidparticlestoswell.Water,glycerolwater,andsucrosewaterarecommonlyusedassettlingsolutionsEglish(3)缓冲液的选择缓冲液是为了使沉降液产生适当的密度梯度常用甲醇水溶液、乙醇水溶液、蒸馏水中文(3)SelectionofbuffersolutionBuffersolutionisusedtocreateanappropriatedensitygradientinthesettlingsolutionMethanolaqueoussolution,ethanolaqueoussolution,anddistilledwaterareoftenusedasbuffersolutionsEglish项目八:常规物理常数与性能分析任务二:熔点的测定毛细管法测定苯甲酸熔点课程:工业分析中文Scenario8:PhysicalconstantsandperformancetestingTask2:DeterminationofmeltingpointDeterminationofthemeltingpointofbenzoicacidbycapillarymethodCourse:IndustrialAnalysisEglish1、样品的填装及装置搭建一、提勒管式热浴取一根长约15cm,直径1~1.5mm,两端封闭的毛细管,从中央割断,即得两根毛细管为熔点管。将少量样品(约0.1g)放在干净表面皿上,研成很细粉末堆在一起。将熔点管开口向下插入粉末,然后开口向上在桌面轻轻敲击,使粉末落入管底。中文1、Samplefillinganddeviceconstruction一、TillertubehotbathmethodTakeacapillarytubeapproximately15
cmlong,withadiameterof1-1.5
mmandclosedends,cutitfromthecentertoobtaintwocapillarytubesasmeltingpointtubes.Placeasmallamountofsample(about0.1g)onacleansurfacedish,grinditintofinepowderandstackittogether.Insertthemeltingpointtubeopeningdownwardsintothepowder,andthengentlytapthemeltingpointtubewiththeopenendfacingupwardsonthedesktoptoallowthepowdertofallintothebottomofthetube.Eglish取一根30~40cm长的玻璃管,垂直放于一个干净的表面皿上,将熔点管开口向上从玻璃管上端自由落下,反复数次,使样品夯实。重复数次,使样品高约2—3mm。粘在管外的样品要擦干净,以免污染热浴液体。将熔点管绑在温度计上,插入提勒管中,搭建实验装置。中文Takeaglasstubewithalengthof30-40cmandplaceitverticallyonacleansurfacedish.Placetheopenendofthemeltingpointtubeupwardsandfreelyfallfromtheupperendoftheglasstube.Repeatthisprocessseveraltimestocompactthesample.Repeatseveraltimestomakethesampleabout2-3mmhigh.Thesamplestuckoutsidethetubeshouldbewipedcleantoavoidcontaminatingthehotbathliquid.Tiethemeltingpointtubetothethermometer,insertitintotheTillertube,andsetuptheexperimentalinstrument.capillaryglasstubewatchglassSampleloadingthermometerRubberbandcapillarysampleWoodenstopperswithnotchesLiquidlevelofheatcarrierat200℃LiquidlevelofheatcarrieratroomtemperaturecapillaryRubberbandheatcarrierlampEglish2、加热介质选择传热液体要求:沸点比待测物熔点高,性能稳定、清澈透明、黏度较小实验室常用热浴是提勒管(Thiele)又称b形管,内盛浓硫酸、磷酸、甘油、石蜡油或有机硅油。甘油、石蜡油适用于150℃以下,浓硫酸适用于220以下,高温分解出三氧化硫。磷酸、硅油可以在300℃以下使用。中文2、SelectionofheatingmediumRequirementsforheattransferliquids:boilingpointshouldbehigherthanthemeltingpointofthetestedsubstance,withstableperformance,clearandtransparentproperties,andlowviscosityThecommonlyusedhotbathequipmentinthelaboratoryisaThieletube,alsoknownasaB-shapedtube,whichcontainsconcentratedsulfuricacid,phosphoricacid,glycerol,paraffinoil,ororganicsiliconeoil.Glycerolandparaffinoilaresuitableformakingheattransferliquidsbelow150℃;Concentratedsulfuricacidissuitablefortemperaturesbelow220andwilldecomposeintosulfurtrioxideathightemperatures.Phosphoricacidandsiliconeoilcanbeusedbelow300℃.Eglish3、注意事项熔点管必须洁净。如含有灰尘等,能产生4-10℃的误差。熔点管底未封好会产生漏管或浴液进入熔点管中。样品粉碎要细,填装要实,否则产生空隙,不易传热,造成熔程变大。样品不干燥或含有杂质,会使熔点偏低,熔程变大。样品量太少不便观察,而且熔点偏低;太多会造成熔程变大,熔点偏高。用橡皮圈将熔点管和温度计系在一起(注意,橡皮圈不能沾着热浴液体)中文3、Note
Themeltingpointtubemustbeclean.Ifitcontainsimpuritiessuchasdust,itcancauseanerrorof4-10℃inthemeltingpoint.Ifthebottomofthemeltingpointtubeisnotsealedproperly,itwillallowthebathliquidtoenterthemeltingpointtube.Samplecrushingshouldbefine,andfillingshouldbesolid,otherwisegapswillbeformed,makingitdifficulttoheattransferandcausinganincreaseinmeltingrange.Ifthesampleisnotdryorcontainsimpurities,itwilllowerthemeltingpointandincreasethemeltingrange.Thesamplesizeistoosmalltoobservethemeltingpoint,andthemeltingpointistoolow;Excessivesamplesizecancauseanincreaseinmeltingrangeandahighermeltingpoint.Tiethemeltingpointtubeandthermometertogetherwitharubberband(notethattherubberbandshouldnottouchthehotbathliquid)Eglish熔点测定至少要有两次重复数据,每一次测定都必须用新的熔点管新装样品,不能使用已测过的熔点管。同时必须待导热液温度冷至熔点以下约30℃左右才能再进行测定。测定完成后,必须将导热液冷至室温,方可倒回试剂瓶里。刚用完的温度计不能立即用水冲洗,待其冷却后用纸擦去导热液,再用水冲洗,以避免温度计炸裂。第一次测过熔点后,有时有些物质会产生部分分解,有些会转变成具有不同熔点的其它结晶形式中文Whenmeasuringthemeltingpoint,itisnecessarytorepeatthemeasurementatleasttwice,andanewmeltingpointtubemustbeusedforeachmeasurement.Previouslymeasuredmeltingpointtubescannotbeused.Atthesametime,itisnecessarytowaitforthetemperatureofthethermalconductivityliquidtocooltoabout30℃belowthemeltingpointtemperaturebeforeproceedingwiththemeasurement.Afterthemeasurementiscompleted,thethermalconductivityliquidmustbecooledtoroomtemperaturebeforebeingpouredbackintothereagentbottle.Newlyusedthermometersshouldnotbeimmediatelyrinsedwithwater.Aftertheyhavecooleddown,wipeofftheheattransferfluidwithpaperandrinsewithwatertopreventthethermometerfromexploding.Eglish4、测定过程粗测:以每分钟约5℃的速度升温,记录当管内样品开始塌落即有液相产生时(始熔)和样品刚好全部变成澄清液体时(全熔)的温度,此读数为该化合物的熔程。精测:待热浴的温度下降大约30℃时,换一根样品管,再作精确测定。中文4、MeasurementprocessRoughmeasurement:Heatupatarateofabout5℃perminute,andrecordthetemperatureatwhichaliquidphaseisformedwhenthesampleinthetubebeginstocollapse(initialmelting)andwhenthesamplejustturnsintoaclearliquid(fullmelting).Thetwotemperaturerangesarethemeltingrangeofthecompound.Precisionmeasurement:Whenthetemperatureofthehotbathdropstoabout30℃belowthemeltingpoint,replacethesampletubeandperformprecisemeasurements.Eglish精测开始升温可稍快(每分钟上升约10℃),待热浴温度离粗测熔点约10℃时,改用小火加热(或将酒精灯稍微离开Thiele管一些),使温度缓缓而均匀上升(每分钟上升1一2℃)。当接近熔点时,加热速度要更慢,每分钟上升0.2~0.3℃。记录刚有小滴液体出现和样品恰好完全熔融时的两个温度读数。这两者的温度范围即为被测样品的熔程。中文Precisionmeasurement:Atthebeginning,theheatingratecanbeslightlyfaster(increasingbyabout10℃perminute).Whenthehotbathtemperatureisabout10℃awayfromtheroughmeltingpoint,reducetheheatingrate(orslightlyremovethealcohollampfromthetube),sothatthetemperatureslowlyanduniformlyrises(increasingby1-2℃perminute).Whenapproachingthemeltingpoint,theheatingrateisslower,increasingby0.2-0.3℃perminute.Recordthetwotemperatureswhenasmalldropletofliquidappearsandwhenthesampleiscompletelymelted.Thetemperaturerangeofthesetwoisthemeltingrangeofthetestedsample.Eglish5、温度计的校正温度计的读数与所测定温度有一定偏差,温度计产生偏差的主要原因有两个方面:一方面是温度计标定时的条件与使用时的条件不完全相同。全浸式和半浸式另一方面温度计的毛细管也不会绝对均匀,温度计长期处于高温或低温会使毛细管永久变形。中文5、CalibrationofthermometersThereisacertaindeviationbetweenthereadingofthethermometerandthemeasuredtemperature,andtherearetwomainreasonsforthedeviationofthethermometer:Ontheonehand,thecalibrationconditionsofthethermometerarenotexactlythesameastheconditionsduringuse.
FullimmersionandsemiimmersionOntheotherhand,thecapillaryofathermometerisnotabsolutelyuniform,andlong-termexposuretohighorlowtemperaturescancausepermanentdeformationofthecapillary.Eglish温度计校正的两种方法
(1)标准物质校正法:
测熔点时我们假定温度计是正确的,用它来测样品的熔点;而在校正时则是反过来。用一系列的标准物质测熔点,以观察到的熔点作横坐标,测得的熔点与应有熔点差作纵坐标,绘成曲线。任意温度的矫正值可以从曲线读出。中文Twomethodsforthermometercalibration
(1)Calibrationusingstandardsubstances:
Whenmeasuringthemeltingpoint,weassumethatthethermometerreadingisaccurateanduseittomeasurethemeltingpointofthesample;Andduringcalibration,itistheopposite.
Measurethemeltingpointsofaseriesofstandardsubstances,usingtheobservedmeltingpointasthex-axisandthedifferencebetweenthemeasuredmeltingpointandthestandardmeltingpointasthey-axis,anddrawacurve.Thecorrectionvalueforanytemperaturecanbereadfromthecurve.Eglish(2)标准温度计校正法:将要校正温度计和标准温度计同时悬于油浴中,位置靠近,机械搅拌,升温速度2—3℃/min,每隔5℃记下两温度计的读数并且列表作图,求出校正值。(标准温度计读数—被校正温度计读数)中文(2)CalibrationusingastandardthermometerThethermometertobecalibratedandthestandardthermometershouldbehungintheoilbathatthesametime.Thepositionsofthetwothermometersshouldbeclose,mechanicallystirred,andtheheatingrateoftheoilbathshouldbecontrolledat2-3℃/min.Thereadingsofthetwothermometersshouldberecordedforevery5℃increase.Finally,achartshouldbecreatedtocalculatethecalibrationvalue.(Standardthermometerreading-calibratedthermometerreading)Eglish温度计校正曲线图0℃中文Thermometercalibrationcurvechart0℃Standardthermometer(℃)calibratedthermometer(℃)Correctionvalue
(℃)Eglish6、结果表示中文6、ResultrepresentationIntheformula:Thecorrectedmeltingpointofthesample,
℃;Measurementvalueofmeltingpoint,℃;Correctionvalueofinternalstandardthermometerreading,℃;Correctionvalueoftheexposedsectionofthemercurycolumninaninternalstandardthermometer,℃Eglish二、双浴式热浴法样品装填及测定过程同提勒管式热浴,按图搭建实验装置15cm载热体装入2/3量1-圆底烧瓶,2-试管,3、4-胶塞,5-温度计,6-辅助温度计,7-熔点管中文二、DoublebathhotbathmethodThesamplefillingandmeasurementprocessisthesameastheTillertubehotbathmethod,andtheexperimentalsetupisbuiltaccordingtothediagram15cmTheamountofheatcarrierloadedis2/3ofthevolumeoftheflask1-Roundbottomflask;2-Testtube;3,4-Rubberstopper;5-Thermometer;6-Auxiliarythermometer;7-MeltingpointtubeEglish项目八:常规物理常数与性能分析任务三:沸点和沸程的测定煤油沸程的测定课程:工业分析中文Scenario8:PhysicalconstantsandperformancetestingTask3DeterminationofboilingpointandboilingrangeDeterminationofboilingrangeofkeroseneCourse:IndustrialAnalysisEglish一、煤油沸程测定装置沸程测定装置图中文一、DeviceformeasuringtheboilingrangeofkeroseneEglish装好仪器后,先记录大气压力,后开始对蒸馏瓶均匀加热。第一滴馏出液从冷凝管滴入量筒时,记录此时的温度作为初馏点(经过的时间为10~15min)。初馏点后,移动量筒,使其内壁接触冷凝管末端,让馏出液沿着量筒内壁流下。此后蒸馏速度要均匀,每分钟馏出4-5毫升,这速度一般应相当于每10秒馏出20-25滴。在收集到10、20、30、40、50、60、70、80、90、95毫升馏出液时,要记录蒸馏温度计上的读数。二、测定方法中文Afterinstallingtheinstrument,recordtheatmosphericpressurefirst,andthenstartheatingthedistillationflaskevenly.Whenthefirstdropofdistillateisdroppedfromthecondenserintothegraduatedcylinder,recordthetemperatureatthistimeastheinitialboilingpoint(thetimeelapsedis10-15minutes).Aftertheinitialboilingpoint,movethegraduatedcylindersothatitsinnerwallcontactstheendofthecondensertube,allowingthedistillatetoflowdownalongtheinnerwallofthegraduatedcylinder.Afterwards,thedistillationspeedshouldbeuniform,distilling4-5millilitersperminute,whichisgenerallyequivalenttodistilling20-25dropsevery10seconds.Whencollecting10,20,30,40,50,60,70,80,90,and95millili二、MeasurementmethodEglish当量筒中馏出液达到90mL时,如蒸馏汽油,允许对加热强度作适当调整,要求在3-5分钟内达到干点。在蒸馏喷气燃料、煤油或轻柴油的过程,当量筒中的馏出液达到95mL时,不要改变加热强度,从95mL到终点所经过的时间不超过3min。当不能测到干点时,记录蒸馏温度计上观测到的最高温度作为终点三、注意事项中文Whenthedistillateintheequivalentcylinderreaches90mL,ifgasolineisbeingdistilled,appropriateadjustmentstotheheatingintensityareallowed,anditisrequiredtoreachthedrypointwithin3-5minutes.Whendistillingjetfuel,kerosene,orlightdiesel,donotchangetheheatingintensitywhenthedistillateintheequivalentcylinderreaches95mL,andthedistillationtimefrom95mLtotheendpointshouldnotexceed3minutes.Whenthedrypointcannotbemeasured,recordthehighesttemperatureobservedonthedistillationthermometerastheendpoint三、NoteEglish当遇到活性分解时,通常在蒸汽和浓烟雾迅速放出后蒸馏温度逐渐下降。如不出现预期的温度下降,则在达到95%之后5分钟,记下蒸馏温度计上观测到的最高温度。并记录为“终点,5min”。这表示真正的终点未能在给定的时间范围内达到。无论如何,终点不应超过95%以后5分钟。中文Whenencounteringthedecompositionofactivesubstances,thedistillationtemperatureusuallygraduallydecreasesaftertherapidreleaseofsteamandconcentratedsmoke.Ifthereisnoexpectedtemperaturedrop,recordthehighesttemperatureobservedonthedistillationthermometer5minutesafterthedistillationvolumereaches95%.Andrecordas"Endpoint,5minutes".Thisindicatesthatthetrueendpointhasnotbeenreachedwithinthegiventimeframe.Anyway,theendpointshouldnotexceed5minutesafterthe95%fraction.Eglish四、分析数据的收集及处理记录初馏点,收集到5、10、20、30、40、50、60、70、80、90、95毫升馏出液时温度计最高温度,终馏点,蒸馏出的液体体积,残留的液体体积计算回收百分数、残留百分数、损失百分数中文四、Collectionandcalculationofanalyticaldatarecord:Initialboilingpoint,maximumtemperatureofthermometerwhencollecting5,10,20,30,40,50,60,70,80,90,and95millilitersofdistillate,finalboilingpoint,volumeofdistilledliquid,andvolumeofresidualliquidcount:Recoverypercentage,residualpercentage,losspercentageEglish项目八:常规物理常数与性能分析任务三:沸点和沸程的测定
沸点和沸程概念及测定方法课程:工业分析中文Scenario8:PhysicalconstantsandperformancetestingTask3:DeterminationofboilingpointandboilingrangeTheconceptsandmeasurementmethodsofboilingpointandboilingrangeCourse:IndustrialAnalysisEglish
沸腾:当液体受热后温度升高,它的蒸气压也随之上升,当液体的蒸气压与大气压相等时,称为沸腾。沸点:在标准状态下,液体沸腾时的温度。标示为Tbp。沸程:挥发性有机液体样品,在标准规定下蒸馏,第一滴馏出物从冷凝管末端落下的瞬间温度(初馏点)至蒸馏瓶底最后一滴液体蒸发的瞬间温度(终馏点)之间的温度间隔。一、基本概念中文
Boiling:Whenaliquidisheatedanditstemperaturerises,itsvaporpressurealsoincreases.Whenthevaporpressureoftheliquidisequaltoatmosphericpressure,itiscalledboiling.Boilingpoint:Thetemperatureatwhichaliquidboilsunderstandardconditions.MarkedasTbp.Boilingrange:Thetemperatureintervalbetweentheinstanttemperature(initialboilingpoint)atwhichthefirstdropofdistillatefallsfromtheendofthecondensertubeandtheinstanttemperature(finalboilingpoint)atwhichthelastdropofliquidevaporatesatthebottomofthedistillationflask,whenavolatileorganicliquidsampleisdistilledunderstandardspecifications.一、BasicconceptsEglish
初馏点:是指油品在规定的条件下进行馏程的测定中,当冷凝管中流出第一滴冷凝液时的气相温度,以℃表示。
终馏点:是指油品在规定的条件下进行馏程的测定,蒸馏过程中的最高气相温度,以℃表示。
馏分:是指在某一温度范围蒸出的馏出物。如汽油馏分、煤油馏分、柴油馏分及润滑油馏分等。温度范围窄的称为窄馏分,温度范围宽的称为宽馏分。
干点:蒸馏烧瓶底部最后一滴液体汽化的瞬间所测得的气相温度,以℃表示。中文Initialboilingpoint:referstothegasphasetemperatureofanoilproductwhenthefirstdropofcondensateflowsoutofthecondensertubeduringdistillationunderspecifiedconditions,expressedin℃.Finalboilingpoint:referstothehighestgasphasetemperatureduringthedistillationprocessofanoilproductunderspecifiedconditions,expressedin℃.Distillate:referstothedistillatedistilledwithinacertaintemperaturerange.Suchasgasolinefraction,kerosenefraction,dieselfraction,andlubricatingoilfraction.Anarrowtemperaturerangeiscalledanarrowfraction,whileawidetemperaturerangeiscalledawidefraction.Drypoint:Thegasphasetemperaturemeasuredatthemomentwhenthelastdropofliquidatthebottomofthedistillationflaskvaporizes,expressedin℃.Eglish
馏出温度:油品在规定的条件下进行馏程的测定中,量筒内回收的冷凝液达到某一规定体积(mL)时所同时观察的温度,以℃表示。50%馏出温度:是指油品在规定的条件下进行馏程的测定中,当馏出物体积为装入试样的50%时,蒸馏瓶内的气相温度,以℃表示。中文Distillationtemperature:Thetemperatureobservedwhentherecoveredcondensateinthegraduatedcylinderreachesaspecifiedvolume(mL)duringdistillationofanoilproductunderspecifiedconditions,expressedin℃.50%DistillationTemperature:referstothegasphasetemperatureinsidethedistillationbottlewhenthevolumeofthedistillateis50%ofthesamplewhentheoilisdistilledunderspecifiedconditions,expressedin℃.Eglish
回收百分数:是指油品在规定的条件下进行馏程的测定中,观察到的最大回收体积所占加入试样的百分数。
残留物百分数:是指油品在规定的条件下进行馏程的测定中,用总回收百分数减回收百分数之差,或者直接测定残留物体积(mL)所占加入试样的百分数。
总回收百分数:指油品在规定的条件下进行馏程的测定中,所得烧瓶里残留物百分数和回收百分数之和。损失百分数:指油品在规定条件下进行馏程的测定中,用100减总回收百分数之差。中文
Recoverypercentage:Thepercentageofthemaximumrecoveryvolumeobservedwhentheoilisdistilledunderspecifiedconditionstothevolumeoftheaddedsample.Residuepercentage:Thepercentageofresidualvolume(mL)intheflasktothevolumeofthesampleaddedwhentheoilisdistilledunderspecifiedconditions.Totalrecoverypercentage:Thesumofthepercentageofresidueintheflaskandtherecoverypercentagewhentheoilisdistilledunderspecifiedconditions.Losspercentage:Whentheoilisdistilledunderspecifiedconditions,thedifferencebetween100andthetotalrecoverypercentageisthelosspercentage.Eglish在脂肪族化合物的异构体中,直链异构体比有侧链的异构体的沸点高。侧链越多,沸点越低。在醇、卤代物、硝基化合物的异构体中,伯异构体沸点最高,仲异构体次之,叔异构体最低。
在顺反异构体中,顺式异构体沸点比反式高。
在多双键的化合物中,有共轭双键的化合物有较高的沸点。
卤代烃、醇、醛、酮、酸的沸点比相应的烃高。
在同系列中,相对分子量增大,沸点增高,但递增值逐渐减小。二、沸点(或沸程)与分子结构的关系中文Intheisomersofaliphaticcompounds,straightchainisomershaveahigherboilingpointthanthosewithsidechains.Themoresidechainsthereare,thelowertheboilingpoint.Amongtheisomersofalcohols,halogenatedcompounds,andnitrocompounds,theprimaryisomerhasthehighestboilingpoint,followedbythesecondaryisomer,andthetertiaryisomerhasthelowestboilingpoint.Incistransisomers,theboilingpointofcisisomersishigherthanthatoftransisomers.Incompoundswithmultipledoublebonds,compoundswithconjugateddoublebondshavehigherboilingpoints.Halogenatedhydrocarbons,alcohols,aldehydes,ketones,andacidshavehigherboilingpointsthantheircorrespondinghydrocarbons.Inthesameseries,therelativemolecularweightincreases,theboilingpointincreases,buttheincrementgraduallydecreases.二、Therelationshipbetweenboilingpoint(orboilingrange)andmolecularstructureEglish1、沸点测定方法三、沸点和沸程测定方法标准方法毛细管法中文1、Methodfordeterminingboilingpoint三、MethodfordeterminingboilingpointandboilingrangestandardmethodcapillarymethodEglish(1)标准方法
在标准状况下,液体的沸腾温度即为该液体的沸点。当液体温度升高时,其蒸气压上升,当蒸气压与大气压力相等时,开始沸腾,温度不再上升,此时温度即为沸点标准方法测定装置1-烧瓶,2-试管,3、4胶塞,5-主温度计,6-辅助温度计,7-侧孔,8-温度计中文(1)Standardmethod
Understandardconditions,theboilingtemperatureofaliquidisitsboilingpoint.
Whenthetemperatureofaliquidrises,itsvaporpressurerises.Whenthevaporpressureisequaltotheatmosphericpressure,boilingbeginsandthetemperaturenolongerrises.Atthispoint,thetemperatureistheboilingpointDevicediagramformeasuringboilingpointusingstandardmethods1-flask;2-testtube;3,4-rubberplugs;5-mainthermometer;6-auxiliarythermometer;7-sidehole;8-ThermometerEglish(2)毛细管法样品量很少或样品珍贵时用该法。测定时将少量样品装入沸点管,内插一支上端封口的毛细管作内管。加热至有连续气泡从内管逸出,停止加热,当气泡停止逸出而液体刚要进入内管时的温度为沸点。中文(2)CapillarymethodThismethodisusedwhenthesamplesizeissmallorthesampleisprecious.Duringthemeasurement,asmallamountofsampleisloadedintoaboilingpointtube,andacapillarytubewithanupperendsealedisinsertedastheinnertube.Heatuntilcontinuousbubblesescapefromtheinnertube,stopheating,andthetemperatureatwhichthebubblesstopescapingandtheliquidisabouttoentertheinnertubeistheboilingpoint.boilingpointtubeinnertubethermometerEglish2、沸程的测定对100mL试样进行蒸馏,观察初馏温度和终馏温度,或观察一定馏出体积时对应的温度范围,或在规定温度范围内馏出的体积1-冷凝管,2-冷凝器,3-进水管,4-排水,5-蒸馏烧瓶,6-接收器,7-温度计,8-石棉垫,9-上罩,10-加热器,11-下罩沸程测定装置中文2、DeterminationofboilingrangeDistill100mLofthesample,observetheinitialandfinaldistillationtemperatures,orobservethetemperaturerangecorrespondingtoacertaindistillationvolume,orobservethevolumeofdistillationwithinthespecifiedtemperaturerange1-condensingtube,2-condenser,3-inletpipe,4-drainagepipe,5-distillationflask,6-receiver,7-thermometer,8-asbestospad,9-uppercover,10-heater,11-lowercoverDevicediagramforboilingrangemeasurementEglish项目八:常规物理常数与性能分析任务四:液体密度的测定
密度基本知识课程:工业分析中文Scenario8:PhysicalconstantsandperformancetestingTask4:DeterminationofliquiddensityBasicknowledgeofdensityCourse:IndustrialAnalysisEglish1、什么是密度指在规定的温度下,单位体积物质的质量,用符号
表示一、密度基本知识中文1、WhatisdensityReferstothemassperunitvolumeofasubstanceataspecifiedtemperature,representedbyasymbol一、BasicknowledgeofdensityItisgenerallystipulatedthatthetemperaturemaynotbeindicatedwhenmeasuringat20℃,butmustbeindicatedwhenmeasuringothertemperaturesEglish2、密度的单位
国际单位制中密度的单位:kg/m3常用的单位是:g/cm3,g/mL。1g/cm3=1000kg/m33、密度与温度的关系
通常:Tr
中文2、Unitofdensity
TheunitofdensityintheInternationalSystemofUnits:kg/m3Thecommonlyuseddensityunits:g/cm3,g/mL。
1g/cm3=1000kg/m33、Therelationshipbetweendensityandtemperature
generally:TρEglish二、密度与分子结构的关系同系列化合物中,相对分子质量增大,密度随之增大,但增量逐渐减小。在烃类化合物中,当碳原子数相同时,不饱和度越大,密度越大。分子中引入极性官能团后,其密度大于其母体烃。分子中引入能形成氢键官能团后,密度增大。
戊烷(0.63)<戊醇(0.8144)中文二、TherelationshipbetweendensityandmolecularstructureInthesameseriesofcompounds,astherelativemolecularweightincreases,thedensityalsoincreases,buttheincrementgraduallydecreases.Inhydrocarboncompounds,whenthenumberofcarbonatomsisthesame,thehighertheunsaturation,thehigherthedensity.Afterintroducingpolarfunctionalgroupsintothemolecule,itsdensityishigherthanthatofitsparenthydrocarbon.Afterintroducingfunctionalgroupsthatcanformhydrogenbondsintothemolecule,thedensityincreases.pentane(0.63)<amylalcohol(0.8144)Eglish三、密度测定的意义中文三、Thesignificanceofdensitymeasurement1.Identifyingcompounds2.Determinethepurityofthecompound50%ethanoldensityis0.930100%ethanoldensityis0.791Eglish四、液体密度的测定方法密度瓶法:准确度高,但不适合易挥发样品31韦氏天平法:挥发、不易挥发样品均可测量2密度计法:挥发、不挥发样品均可测量,操作简单但准确性差3中文四、MethodformeasuringliquiddensityDensitybottlemethod:
Highaccuracy,butnotsuitableforvolatilesamples31Websterbalancemethod:bothvolatileandnonvolatilesamplescanbemeasured2Densitymetermethod:bothvolatileandnon-volatilesamplescanbemeasured,withsimpleoperationbutpooraccuracy3Eglish项目八:常规物理常数与性能分析任务三:沸点和沸程的测定乙醇沸点的测定课程:工业分析中文Scenario8:PhysicalconstantsandperformancetestingTask3DeterminationofboilingpointandboilingrangeDeterminationofboilingpointofethanolCourse:IndustrialAnalysisEglish一、标准方法测定乙醇沸点1-烧瓶,2-试管,3、4胶塞,5-主温度计,6-辅助温度计,7-侧孔,8-温度计1、搭建实验装置载热体为甘油,加入量为烧瓶体积一半试管内液面低于加热体液面主温度计在被测
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