《工业分析 Industrial Analysis》课件-项目二：工业浓硝酸质量分析

项目二：工业浓硝酸质量分析任务一：液体样品采样方法液体样品采样工具和采样方法课程：工业分析中文Scenario2:QualityanalysisofindustrialconcentratednitricacidTask1:SamplingmethodforliquidsamplesSamplingtoolsandmethodsforliquidsamplesCourse:IndustrialAnalysisEglish液态物料具有流动性，组成比较均匀，易采得均匀样品。液态物料一般装在容器中贮存和运输取样前根据容器情况和物料特性选择采样工具与采样方法中文Liquidmaterialshavefluidity,arelativelyuniformcomposition,andareeasytoobtainuniformsamples。LiquidmaterialsaregenerallystoredandtransportedincontainersSelectsamplingtoolsandmethodsbasedoncontainerconditionsandmaterialcharacteristicsbeforesamplingEglish一、液体样品采样工具1、采样勺适合于表面样品的采集，材质有塑料、不锈钢、黄铜等，根据样品性质选择相应材质采样勺。中文一、Samplingtoolsforliquidsamples1、SamplingspoonThesamplingspoonissuitableforcollectingsurfacesamples,withmaterialssuchasplastic,stainlesssteel,brass,etc.Whensampling,selectthecorrespondingmaterialofthesamplingspoonaccordingtothenatureofthesample.Multiplespecificationsincluding5mLEglish2、采样瓶和采样罐可用于任意深度液体试样采集，材质有不锈钢、黄铜、有机玻璃等，根据样品性质选择相应材质。中文2、Samplingbottleandsamplingtank

Samplingbottlesandcanscanbeusedforcollectingliquidsamplesatanydepth,andtheirmaterialsincludestainlesssteel,brass,organicglass,etc.

Thecorrespondingmaterialsareselectedaccordingtothepropertiesofthesamples.Eglish3、采样管抽拉式采样管，泛应用于药品、食品、化妆品、化工等行业粘稠液体浸膏、乳化液、乳膏、洗发液、油类等的取样，材质有不锈钢和玻璃。中文3、SamplingtubeThepull-outsamplingtubeiswidelyusedforsamplingviscousliquidointments,emulsions,creams,shampoos,oils,etc.inindustriessuchaspharmaceuticals,food,cosmetics,andchemicals.Thematerialsusedincludestainlesssteelandglass.Eglish二、采样方法1、一般液体样品采集小贮存器中样品小瓶装

按取样数随机抽取几瓶，每瓶倒出等量液体混匀大瓶或小桶装

搅拌混匀后用采样管采样大桶装

搅拌混匀后用采样管采样，或不搅拌采部位样品混匀中文二、Samplingmethod1、Samplingofgeneralliquidsamples(1)SampleinsmallstoragecontainerSmallbottlepackaging

Randomlyselectseveralbottlesaccordingtothenumberofsamples,pouroutanequalamountofliquidfromeachbottleandmixwellLargebottleorsmallbarrelpackaging

Afterstirringandmixing,useasamplingtubetorandomlysampleLargebarrelpackaging

Afterstirringandmixing,useasamplingtubeforsampling,ormixthecollectedsampleswithoutstirringEglish大贮存器中样品卧式贮罐一般按比例采上、中、下部位样品，混合后作为测试样品。槽车用采样瓶采上中下部位样品，等比例混匀立式贮罐一般按比例采上、中、下部位样品，混合后作为测试样品。船舱用采样瓶从排料口取样从顶部取上中下部位样品混匀作最终样品中文(2)Samplingofsamplesinlargestoragetanks

VerticalstoragetankandhorizontalstoragetankGenerally,upper,middle,andlowersamplesarecollectedinproportionandmixedastestsamples.

CabinTakeasamplefromthedischargeportusingasamplingbottleTakesamplesfromthetop,middle,andbottompartsMixwelltomakethefinalsample

tankcarUseasamplingbottletocollectsamplesfromtheupper,middle,andlowerparts,andmixthemevenlyinequalproportionsEglish从输送管道采样

自动管线采样器采样探头采样管道出口端采样：出口端放一容器，周期性采样中文SamplingfromtheconveyingpipelineUsinganautomaticpipelinesamplerforsamplingSamplingwithaprobeSamplingattheoutletofthepipeline:PlaceacontainerattheoutletandsampleatacertainperiodEglish2、特殊性质液体样品采集在制造厂的最终容器中采样：用采样管或勺取部位样品混匀即可在制造厂产品装桶时采样：按规律从放料口采样混匀即可在交货容器中采样：混匀样品后用采样管或勺取部位样品混匀即可粘稠液体的采样中文2、SamplingofliquidsampleswithspecialpropertiesSamplinginthefinalcontainerofthemanufacturingplant:UseasamplingtubeorspoontotakethesampleandmixwellSamplingduringproductbarrelloadinginthemanufacturingplant:SampleandmixevenlyfromthedischargeportaccordingtothepatternSamplinginthedeliverycontainer:Aftermixingthesample,useasamplingtubeorspoontotakethesampleandmixitwellSamplingofviscousliquidsEglish液化气体的采样注意采样点的布置能保证采得有代表性的样品，如不能可制定协议规定采样方法和采样点稍加热即成为流动态的化工产品在样品呈液态时用采样勺或采样管采样，可在厂家交货罐装时采样，也可将固化后的样品熔化后取样中文SamplingofliquefiedgasesPayattentiontothelayoutofsamplingpointstoensurethecollectionofrepresentativesamples.Ifnotpossible,aprotocolcanbeestablishedtospecifythesamplingmethodandsamplingpointsChemicalproductsthatbecomeaflowingstateuponslightheatingWhenthesampleisinliquidform,useasamplingspoonorsamplingtubetotakesamples.Samplescanbetakenwhenthemanufacturerdeliversthecontainer,oraftermeltingthesolidifiedsample,samplescanbetakenEglish三、采样注意事项样品容器必须洁净、干燥、严密采样设备必修清洁、干燥，不能用与被采取物料起化学作用得材料制造采样过程中防止被采取物料受到环境污染和变质取样者必须熟悉被采取产品的特性、安全操作的有关知识及处理方法中文三、PrecautionsduringsamplingThesamplecontainermustbeclean,dry,andtightSamplingequipmentmustbecleananddry,andcannotbemanufacturedwithmaterialsthathaveachemicalreactionwiththematerialbeingtakenPreventenvironmentalpollutionanddeteriorationofmaterialstakenduringthesamplingprocessThesamplermustbefamiliarwiththecharacteristicsoftheproductbeingtaken,relevantknowledgeofsafeoperation,andhandlingmethodsEglish项目二：工业浓硝酸质量分析任务一：液体样品采样方法采样的目的、要求和基本术语课程：工业分析中文Scenario2:QualityanalysisofindustrialconcentratednitricacidTask1:SamplingmethodforliquidsamplesThepurpose,requirements,andbasicterminologyofsamplingCourse:IndustrialAnalysisEglish

工业分析的任务是从大批物料中确定某种或某些组分的平均质量分数。工业分析测定步骤：采样、制样、分解样品、消除干扰、方法的选择、结果的计算和数据的评价。中文

Thetaskofindustrialanalysisistodeterminetheaveragemassfractionofacertainorcertaincomponentfromalargenumberofmaterials.

Industrialanalysisandmeasurementsteps:sampling,samplepreparation,sampledecomposition,interferenceelimination,methodselection,resultcalculation,anddataevaluation.theobtainedsamplesmustberepresentativeEglish一、采样的基本术语1、采样单元：具有界限的一定数量物料，其界限可能是有形的也可能是无形的。2、子样（份样）：用采样器从一个采样单元中一次取得的一定量物料。3、样品：从数量较大的采样单元中取得的一个或几个采样单元，或从一个采样单元中取得的一份或几个子样。4、原始平均试样：合并所有采取的子样中文一、Basicterminologyofsampling1.Samplingunit:Acertainquantityofmaterialwithboundaries,whoseboundariesmaybetangibleorintangible.2.Subsample:Acertainamountofmaterialobtainedatoncefromasamplingunitusingasampler.3.Sample:Oneorseveralsamplingunitsobtainedfromalargenumberofsamplingunits,oroneorseveralsubsamplesobtainedfromasinglesamplingunit.4.Originalaveragesample:ThesampleobtainedbycombiningallthesubsamplestakenEglish5、分析化验单位：应采取一个原始平均试样的物料的总量。6、实验室样品：为送往实验室供检验或测试而制备的样品。7、备考样品：与实验室样品同时同样制备的样品，在有争议时，它可为有关方面接受用作实验室样品。8、部位样品：从物料的特定部位或在物料流的特定部位和时间取得的一定数量或大小的样品。9、表面样品：在物料表面取得的样品，以获得关于此物料表面的资料。中文5.Analysisandtestingunit:Thetotalamountofmaterialinanoriginalaveragesampleshouldbetaken.6.Laboratorysample:Asamplepreparedforsendingtothelaboratoryforinspectionortesting.7.Preparationsample:Asamplepreparedsimultaneouslywithalaboratorysample,whichcanbeacceptedbyrelevantpartiesasalaboratorysampleincaseofdispute.8.Partsamples:Acertainquantityorsizeofsamplesobtainedfromaspecificpartofamaterialorataspecificpartandtimeinthematerialflow.9.Surfacesample:Asampleobtainedonthesurfaceofamaterialtoobtaininformationaboutitssurface.Eglish二、采样要求

采取有代表性的实验室样品时，应根据物料的堆放情况及颗粒大小，从不同部位和深度选取多个采样点，采取一定量的样品，混合均匀。采取的份数越多越有代表性。但是采样量过大，会给后面的制样带来麻烦。中文二、Samplingrequirements

Whentakingrepresentativelaboratorysamples,multiplesamplingpointsshouldbeselectedfromdifferentpartsanddepthsbasedonthestackingsituationandparticlesizeofthematerials.Acertainamountofsamplesshouldbetakenandmixedevenly.Themorecopiestaken,themorerepresentativetheyare.Butifthesamplingamountistoolarge,itwillcausetroubleforthesubsequentsamplepreparation.Eglish1、采样原则中文1、SamplingprinciplesUnevenmaterials:generalrandomsamplingUniformmaterial:canbesampledfromanypartSamplingprinciplesUniformmaterialreferstotheaveragevalueofthecharacteristicsofeachpartofthematerialwithinthemeasurementerrorrangeUnevenmaterialreferstotheaveragevalueofthecharacteristicsofeachpartofthematerialthatisnotwithinthemeasurementerrorrangeEglish2、采样量采样的数量一式三份供检验、复检和备查用满足3次检验需要量中文2、SamplingamountThreecopiesofthesamplingquantityareprovidedforinspection,retesting,andreferencepurposesSamplingsteps:DeterminethenumberofsamplingunitssampleineachunitDeterminationofthenumberofsamplingunitsn(Nisthetotalnumberofpieces):Whenthenumberofunits>500,

Whenthenumberofunitsislessthan500,takesamplesaccordingtothespecifiednumberofpiecesEglish中文OverallmaterialunitOverallmaterialunitMinimumunitsselectedMinimumunitsselectedTotalunitsRegulationsonthenumberofsamplingunitsEglish三、采样记录书写

采样时，要认真填写采样记录，写明样品的生产日期、批号、采样条件、方法、数量、包装情况等。外地调入的食品还应结合运货单、商检机关和卫生部门的化验单、厂方化验单等，了解起运日期、来源地点、数量、品质及包装情况。同时注意其运输及保管条件，并填写检验目的、项目及采样人。中文三、Writingmethodforsamplingrecords

Whensampling,itisnecessarytocarefullyfillinthesamplingrecord,statingtheproductiondate,batchnumber,samplingconditions,method,quantity,packagingsituation,etc.ofthesample.Thefoodtransferredfromotherplacesshouldalsobecombinedwiththewaybill,inspectionandhealthdepartment'stestreport,factory'stestreport,etc.tounderstandthedateofshipment,placeoforigin,quantity,quality,andpackagingsituation.Atthesametime,payattentiontothetransportationandstorageconditionsofthesamples,andfillintheinspectionpurpose,items,andsampler.Eglish项目二：工业浓硝酸质量分析任务二：硝酸性质及取样方法硝酸性质、生产工艺及安瓿球取样方法课程：工业分析中文Scenario2:QualityanalysisofindustrialconcentratednitricacidTask2:PropertiesofnitricacidandsamplingmethodNitricacidproperties,productionprocess,andampouleballsamplingmethodCourse:IndustrialAnalysisEglish一、硝酸的物理性质颜色：气味：状态：密度：挥发性：溶解性：纯硝酸无色有刺激性气味液体1.50g／cm3易挥发与水以任意比例互溶为什么有色？中文一、ThephysicalpropertiesofnitricacidColor:Odor:Status:Density:Volatility:Solubility:PurenitricacidcolourlessHasapungentodorliquid1.50

g/cm3volatileSolublewithwaterinanyproportionWhycolored?ConcentratednitricacidEglish常见硝酸的质量分数约为69%，98%以上的硝酸为“发烟”硝酸，硝酸越浓越易分解。1、不稳定，易分解4HNO3光或加热（条件）=2H2O+O2↑+4NO2↑（黄色）启迪思考：如何保存硝酸棕色试剂瓶、暗处、低温中文Themassfractionofcommonnitricacidisabout69%,andnitricacidwithacontentofover98%iscalled"smoky"nitricacid.Thehighertheconcentrationofnitricacid,theeasieritistodecompose.1、Unstableandeasilydecomposable4HNO3=2H2O+O2↑+4NO2↑（Yellow）Thinking:HowtopreservenitricacidBrownreagentbottle,darkplace,lowtemperature

Lightorheating(condition)Eglish在抢险过程中，运来的石灰石有什么作用？2、硝酸具有强酸性CaCO3

+

2HNO3

=

Ca(NO3)2

+

H2O

+

CO2↑3、硝酸具有强氧化性中文Whatistheroleofthelimestonetransportedduringtherescueprocess？2、NitricacidhasstrongacidityCaCO3

+

2HNO3

=

Ca(NO3)2

+

H2O

+

CO2↑3、NitricacidhasstrongoxidizingpropertiesEglish硝酸具有强的氧化性，几乎可以氧化所有金属（金、铂除外）。Cu+4HNO3（浓）=Cu(NO3)2+2NO2↑+2H2O

3Cu+8HNO3（稀）=3Cu(NO3)2+2NO↑+4H2O例硝酸与金属反应不放出氢气浓硝酸被还原成NO2，稀硝酸被还原成NO，二、硝酸的化学性质中文Nitricacidhasstrongoxidizingpropertiesandcanoxidizealmostallmetals(exceptgoldandplatinum).Cu+4HNO3（concentrated）=Cu(NO3)2+2NO2↑+2H2O

3Cu+8HNO3（dilute）=3Cu(NO3)2+2NO↑+4H2OExampleNitricacidreactswithmetalswithoutreleasinghydrogengasConcentratednitricacidisreducedtoNO2,whiledilutenitricacidisreducedtoNO二、ThechemicalpropertiesofnitricacidReactwithmetalsEglish常温下，浓硝酸与铁、铝发生反应吗？铁、铝遇冷浓HNO3发生钝化，其原因是在铁、铝表面氧化生成一层致密的氧化膜，阻止反应进一步发生。可以用铝制或铁制容器装浓硝酸中文Doesconcentratednitricacidreactwithironandaluminumatroomtemperature?IronandaluminumundergopassivationreactionswhenencounteringcoldandconcentratedHNO3.Thereasonforthisisthatadenseoxidefilmisformedonthesurfaceofironandaluminum,whichpreventsfurtherreactionfromoccurring.ConcentratednitricacidcanbestoredinaluminumorironcontainersReactwithmetalsEglish浓硝酸与非金属反应（C、S、P)，一般将非金属氧化为最高价氧化物或最高价含氧酸；自身被还原为NO24HNO3（浓）+C=CO2+4NO2+2H2O

与还原性物质浓硝酸能将含S2-、SO32-、Fe2+、I-等的化合物氧化。中文Concentratednitricacidreactswithnon-metals(C,S,P),generallyoxidizingnon-metalstothehighestvalenceoxideorhighestvalenceoxygen-containingacid;RestoredtoNO2byitself4HNO3（Concentrated）+C=CO2+4NO2+2H2O

ReactwithreducingsubstanceConcentratednitricacidcanoxidizecompoundscontainingS2-,SO32-,Fe2+,I-,

etc.ReactwithNon-metalsEglish小知识帮你记忆1:3一·三能“消·炎”硝酸盐酸

3体积浓盐酸与1体积浓硝酸的混合物叫做王水，它的氧化能力更强，金（Au）和铂（Pt）不溶于硝酸，但溶于王水。中文LittleknowledgeHelpyouremember1:3One·Threecan"eliminateinflammation"nitricacidhydrochloricacid

Amixtureof3volumesofconcentratedhydrochloricacidand1volumeofconcentratednitricacidiscalledaquaregia,whichhasstrongeroxidationability.Gold(Au)andplatinum(Pt)areinsolubleinnitricacid,butcanbedissolvedinaquaregia.Eglish1、实验室制法NaNO3(s)+H2SO4(浓)NaHSO4+HNO3

微热三、硝酸的生产工艺中文1、LaboratorypreparationmethodNaNO3(s)+H2SO4(concentrated)NaHSO4+HNO3

Microheating三、TheproductionprocessofnitricacidEglish2、工业制法-氨催化氧化法2NO+O2=2NO2(2)一氧化氮被氧气氧化成二氧化氮3NO2+H2O=2HNO3+NO(3)用水吸收二氧化氮生成硝酸(1)氨在催化剂的作用下与氧气发生反应生成一氧化氮4NH3+5O2====4NO+6H2O催化剂中文2、Industrialpreparationmethod-ammoniacatalyticoxidationmethod2NO+O2=2NO2(2)Nitricoxideisoxidizedbyoxygentonitrogendioxide3NO2+H2O=2HNO3+NO(3)Nitrogendioxideisabsorbedbywatertoformnitricacid(1)Ammoniareactswithoxygenundertheactionofacatalysttoproducenitricoxide4NH3+5O2====4NO+6H2OcatalystEglish中文ProcessforpreparingnitricacidusingindustrialmethodsairairheatexchangerAbsorberConvertercatalyzer,etc,etcEglish四、硝酸的取样方法硝酸具有易挥发性，取样分析时不能像称量固体样品那样直接称量，必须借助安瓿球的帮忙。直径约20mm，毛细管端长约60mm使用时先对球部微微加热，赶出球内空气，然后将毛细管插入硝酸中，待硝酸进入球内达到需要量后，取出，擦干毛细管，熔封即可中文四、TheweighingmethodofnitricacidNitricacidisvolatileandcannotbeweigheddirectlylikesolidsamplesduringsamplingandanalysis.Thehelpofampouleballsisnecessary.Approximately20

mmindiameter,withacapillaryendlengthofapproximately60

mmWhenusing,firstslightlyheattheballtoexpeltheairinsidetheball,theninsertthecapillaryintonitricacid.Aftertherequiredamountofnitricacidenterstheball,removeit,wipethecapillary,andsealitEglish项目二：工业浓硝酸质量分析任务三：

硝酸质量分析硝酸含量测定原理及方法课程：工业分析中文Scenario2:QualityanalysisofindustrialconcentratednitricacidTask3:QualityanalysisofnitricacidPrinciplesandmethodsformeasuringnitricacidcontentCourse:IndustrialAnalysisEglish·工业浓硝酸产品标准GB/T337.1-2002《工业硝酸浓硝酸》项目98酸97酸硝酸质量分数，%≥98.097.0亚硝酸质量分数，%≤0.501.0硫酸质量分数，%≤0.080.10灼烧残渣质量分数，%≤0.020.02中文·ProductstandardforindustrialconcentratednitricacidGB/T337.1-2002《Industrialnitricacid

concentratednitricacid》project98acid97acidMassfractionofnitricacid，%≥98.097.0Massfractionofnitrousacid，%≤0.501.0Massfractionofsulfuricacid，%≤0.080.10Massfractionofignitionresidue，%≤0.020.02Eglish硝酸质量分析过程

根据分析对象性质设计分析方案准备分析用仪器准备分析用试剂准确称取样品进行分析对结果进行评价中文Nitricacidqualityanalysisprocess:DesignananalysisplanbasedonthenatureoftheanalysisobjectPrepareanalyticalinstrumentsPrepareanalyticalreagentsAccuratelyweighthesampleandanalyzeitEvaluatetheresultsEglish一、方法原理硝酸是强酸，可用酸碱滴定法测定将样品加入过量的氢氧化钠标准滴定溶液中，用甲基橙为指示剂用硫酸标准溶液进行返滴定。

中文一、TheprincipleofmeasurementmethodsNitricacidisastrongacidandcanbedeterminedbyacid-basetitrationAddnitricacidsampletoexcesssodiumhydroxidestandardtitrationsolution,andperformbacktitrationwithsulfuricacidstandardsolutionusingmethylorangeastheindicator.Eglish二、测定所用仪器硝酸易挥发，取样分析时不能像称取性质稳定的固体那样直接称量，必须借助安瓿球的帮忙。此外需滴定分析常规仪器和碘量瓶中文二、InstrumentsusedformeasurementNitricacidisvolatile,andwhensamplingandanalyzing,itcannotbedirectlyweighedlikeastablesolidsample.Ampouleballsmustbeusedtoweighnitricacid.Inaddition,conventionalinstrumentsfortitrationanalysisandiodinevolumetricflasksarerequiredAmpouleballiodinevolumetricflasksSucknitricacidsampleContainerforholdingnitricacidsamplesandtitrationEglish三、测定所用试剂

氢氧化钠标准滴定溶液：c(NaOH)=1mol/L硫酸标准滴定溶液：(1/2H2SO4)=1mol/L甲基橙指示液：1g/LNaOH和H2SO4标准溶液浓度要准确标定中文三、Reagentsusedfordetermination

Sodiumhydroxidestandardtitrationsolution：c(NaOH)=1mol/LSulfuricacidstandardtitrationsolution：(1/2

H2SO4)=1mol/LMethylorangeindicator：1g/LAccuratedeterminationofNaOHandH2SO4standardsolutionconcentrationEglish四、检验步骤将安瓿球预先称准至0.0002g，然后在火焰上微微加热安瓿球的球泡。将安瓿球的毛细管端浸入盛有样品的瓶中，并使冷却，待样品充至1.5mL-2.0mL时，取出安瓿球。用滤纸仔细擦净毛细管端，在火焰上使毛细管端封闭，不使玻璃损失。称量含有样品的安瓿球，称准至0.0002g，并根据差值计算样品质量。中文四、Inspectionsteps

First,accuratelyweighthemassoftheampouleball,andthenslightlyheatthebulboftheampouleballonaflame.Immersethecapillaryendoftheampouleballintothebottlecontainingthesampleandletitcool.Whenthesampleisfilledto1.5mL-2.0mL,removetheampouleball.Carefullywipethecapillaryendwithfilterpaperandsealitontheflametopreventglassloss.

Weightheampoulecontainingthesampleandcalculatethesamplemassbasedonthedifferencebetweenthetwomasses.Eglish

将盛有样品的安瓿球，小心至于预先盛有100mL水和用移液管移入50mL氢氧化钠滴定溶液的锥形瓶中，塞紧磨口塞。然后剧烈震荡，使安瓿瓶破裂，并冷却至室温，摇动锥形瓶，直至酸雾全部吸收为止。

取下塞子，用水洗涤，洗液收集于同一锥形瓶内。加1-2滴甲基橙指示剂溶液，然后用硫酸标准滴定溶液将过量的氢氧化钠标准滴定溶液滴定至溶液呈橙色为终点。中文

Carefullyplacetheampouleballcontainingthesampleintoaconicalflaskprefilledwith100mLofwaterandpipette50mLofsodiumhydroxidetitrationsolution,andtightenthegroundstopper.Thenshakevigorouslytobreaktheampoule,continueshakingtheconicalflaskuntilthea