《工业分析 Industrial Analysis》课件-硅酸盐试样制样方法（双语）

项目七：硅酸盐分析任务二：硅酸盐试样制样方法硅酸盐试样制样方法课程：工业分析中文Scenario7:SilicateAnalysisTask2:PreparationmethodofsilicatesamplesPreparationmethodofsilicatesamplesCourse:IndustrialAnalysisEglish一、硅酸盐试样的处理制备过程：破碎过筛混匀磨碎：取样前研细至粒径≤0.080mm试样的烘干：用烘干法除去试样吸附的水分过筛混匀缩分缩分中文一、TreatmentofsilicatesamplesPreparationprocess：crush过筛混匀Grinding:Finegrindtoaparticlesizeof≤0.080mmbeforesamplingDrying:Usethedryingmethodtoremovethemoistureadsorbedonthesamplesievemix缩分reduceEglish二、硅酸盐试样的分解1、试样分解目的

2、试样的分解要求（1）完全简单快速（2）分解无损失（3）无干扰引入中文二、Decompositionofsilicatesamples1、Thepurposeofsampledecomposition

2、Sampledecompositionrequirements(1)Complete,simple,andfast(2)Decompositionwithoutloss(3)WillnotintroduceinterferingsubstancessolidsampleconvertsamplesolutionEglish3、试样分解的原理（理论依据）中文3、Theprincipleofsampledecomposition(theoreticalbasis)AlkalinemetaloxidesSmallratio,easilysolublebyacidHighratio,easilysolublebyalkaliMarble,limestoneCementclinkerAlkalineslagRawmaterials,clayIronoreEglish4、试样的分解处理方法中文4、Sampledecompositionmethodinclude:Dissolutionmethod:water

soluble,acidsoluble,otherdissolutionmethodsMeltingmethod:reagentSemimeltingmethodEglish（1）酸溶解法SiO2碱金属氧化物比值越小，碱性越强，越易被酸溶解硅酸盐分析中所用的酸：HCl，HNO3，H2SO4，H3PO4，HF等。中文（1）AciddissolutionmethodSiO2AlkalimetaloxideThesmallertheratio,thestrongerthealkalinity,andtheeasieritistobedissolvedbyacidAcidsusedinsilicateanalysis:HCl，HNO3，H2SO4，H3PO4，HF,etc.EglishHCl：系统分析中HCl是良好的溶剂特点：

a.生成的氯化物除AgCl、Hg2Cl2、PbCl2外都能溶于水，给测定带来方便。（硅酸盐样品中几乎不含Ag+、Hg22+、Pb2+）

b.Cl-与某些离子生成络合物FeCl63-促进试样分解

c.浓HCl沸点较低（bp108℃），用重量法测SiO2易于蒸发除去

d.大多数硅酸盐样品不能被HCl分解（熟料碱性矿渣可以）中文HCl：HClisagoodsolventinsystemanalysisFeatures:a.Thegeneratedchlorides,exceptforAgCl,Hg2Cl2,andPbCl2,aresolubleinwater,makingthedeterminationconvenient.(ThesilicatesamplecontainsalmostnoAg+,Hg22+,Pb2+)b.Cl-formscomplexeswithcertainions,FeCl63-promotessampledecompositionc.ConcentratedHClhasalowerboilingpoint(bp108℃),makingiteasiertoevaporateandremovehydrochloricacidwhenmeasuringSiO2usingthegravimetricmethodd.ThedisadvantageisthatmostsilicatesamplescannotbedecomposedbyHClEglishHNO3、H2SO4、H3PO4：在系统分析中很少用HNO3、H2SO4溶样a.HNO3溶样，重量法测SiO2，加热蒸发过程中易形成难溶性碱式盐沉淀b.H2SO4易形成溶解度小、或不溶的碱土金属硫酸盐，干扰测定c.H3PO4（缩合的H3PO4）200~300˚C溶解能力很强，能溶解一些难溶于HCl、H2SO4的样品，如铁矿石、钛铁矿等，但只适用于单项测定。特点：中文HNO3,H2SO4,H3PO4：HNO3andH2SO4arerarelyusedtodissolvesamplesinsystemanalysisa.WhendissolvingsampleswithHNO3andmeasuringSiO2usingthegravimetricmethod,insolublealkalinesaltprecipitatesareeasilyformedduringtheheatingandevaporationprocessb.H2SO4easilyformsalkalineearthmetalsulfateswithlowsolubilityorinsolubility,whichinterferewiththedeterminationc.Between200and300

℃,H3PO4hasastrongsolubilityandcandissolvesomesamplesthataredifficulttodissolveinHClandH2SO4,suchasironore,ilmenite,etc.,butitisonlysuitableforsingleitemdetermination.Features:Eglish但有干扰，如HF及HF-H2SO4、HF-HClO4混酸大多数的硅酸盐样品均能被HF分解。残渣为除Si外的其它盐类，以水提取加酸溶解，或熔融法处理成试样溶液。

中文Butthereisinterference,suchasHF,HF-H2SO4,HF-HClO4MostsilicatesamplescanbedecomposedbyHF.

TheresidueisasaltotherthanSi,whichisextractedwithwateranddissolvedinacid,orprocessedintoasamplesolutionbymeltingmethod.

Eglish（2）熔融或半熔法什么是熔融法或半熔法？（干法）将试样与熔剂混合在高温下加热熔融，使欲测组分变为可溶于水或酸中的化合物（K、Na盐、硫酸盐、氯化物）熔融或半熔的目的？利用熔剂，借助高温熔融或半融的方法，增加碱金属氧化物的比值，使本来不能被酸直接分解的试样能被酸分解。中文（2）MeltingorsemimeltingmethodWhatisthemeltingmethodorsemimeltingmethod?(Drymethod)Mixthesamplewiththefluxandheatitathightemperaturetomeltthedesiredcomponentintocompounds(K,Nasalts,sulfates,chlorides)thataresolubleinwateroracidThepurposeofmeltingorsemimelting?Byusinghigh-temperaturemeltingorsemimeltingmethods,theratioofalkalimetaloxidesisincreased,sothatsamplesthatcannotbedirectlydecomposedbyacidcanbedecomposedbyacid.Eglish熔剂：碱金属的化合物：Na2CO3，K2CO3，NaOH，KOH，Na2O2，K2S2O7

熔融法分类：碱熔法：用碱性溶剂，熔酸性试样，如Na2CO3酸熔法：用酸性溶剂，熔碱性试样，如K2S2O7中文Meltingsolvent：basicmeltingsolvent：Na2CO3，K2CO3，NaOH，KOH，Na2O2acidmeltingsolvent：K2S2O7

Classificationofmeltingmethod:Alkalimeltingmethod:usingalkalinesolventstomeltacidicsamplesAcidmeltingmethod:usinganacidicsolventtomeltanalkalinesampleEglishMnClAlClSiOH如HCl酸分解)(MnONaOAlONaSiONaC1000150CONa23324232232o32熔融物锰酸钠铝酸钠硅酸钠硅酸盐×-当硅酸盐与Na2CO3熔融时，硅酸盐便被分解为碱金属硅酸钠、铝酸钠、锰酸钠等复杂的混合物。熔融物用酸处理时，则分解为相应的盐类并析出硅酸。中文

WhensilicatesaremixedwithNa2CO3andmelted,theyaredecomposedintocomplexmixturessuchasalkalimetalsodiumsilicate,sodiumaluminate,andsodiummanganeseoxide.Whenthemoltenmaterialistreatedwithacid,itdecomposesintocorrespondingsaltsandprecipitatessilicicacid.MnClAlClSiOH酸分解)(MnONaOAlONaSiONaC1000150CONa23324232232o32熔融物SodiummanganatesodiumaluminateSodiumsilicatesilicate×-decomposewithacidEglish如高岭土Al2O32

SiO2

2

H2O

+

3

Na2CO3

=

2

Na2SiO3

+

Na2O

Al2O3

+

3

CO2

+

2

H2OHCl处理Na2O

Al2O3

+

8

HCl2

AlCl3

+

2

NaCl

+

4

H2ONa2SiO3

+

2

HCl

H2SiO3

+

2

NaCl熔样过程中文example：kaolinAl2O32

SiO2

2

H2O

+

3

Na2CO3

=

2

Na2SiO3

+

Na2O

Al2O3

+

3

CO2

+

2

H2OTreatwithHCl

Na2O

Al2O3

+

8

HCl2

AlCl3

+

2

NaCl

+

4

H2ONa2SiO3

+

2

HCl

H2SiO3

+

2

NaClEglish器皿：坩埚（灼烧、熔融、烧结试样）有：瓷、石英坩埚，铁、镍、银、铂金、黄金坩埚中文Vessel:Crucible(usedforburning,melting,andsinteringsamples)Thereare:porcelain,quartzcrucibles,iron,nickel,silver,platinum,andgoldcruciblesRulesforvesselselection：◆Selectaccordingtothepropertiesoftheflux:acidicfluxescannotbeusedinAg,FeandNicrucibles;Alkalinefluxcannotbeusedinquartzorporcelaincrucibles;Strongalkalinityandstrongoxidizingflux