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項(xiàng)目六:鋼鐵分析任務(wù)一:鋼鐵種類及制樣方法鋼鐵分類及各元素作用課程:工業(yè)分析中文Scenario6:SteelanalysisTask1:TypesofsteelandsamplepreparationmethodsClassificationofSteelandtheEffectsofVariousElementsCourse:IndustrialAnalysisEglish一、鋼鐵種類鋼和鐵主成分都是鐵,區(qū)別是根據(jù)含碳量的多少生鐵:含C>1.7%鋼:含C0.05%~1.7%熟鐵:含C<0.05低碳鋼:0.05~0.25%中碳鋼:0.25~0.60%高碳鋼:0.60~1.4%中文一、ClassificationofsteelThemaincomponentofbothsteelandironisiron,andthedifferencebetweenthemistheircarboncontentPigiron:containingC>1.7%Steel:containingC0.05%~1.7%Wroughtiron:containingC<0.05low-carbonsteel:0.05~0.25%mediumcarbonsteel:0.25~0.60%high-carbonsteel:0.60~1.4%Eglish1、生鐵
鐵礦石和焦炭、石灰石按一定比例配合,經(jīng)過高溫煅燒、冶煉,則鐵礦石被焦炭還原,生成粗制的鐵,稱生鐵。反應(yīng)歷程較復(fù)雜,可用下式代表:中文1、PigironIronoreismixedwithcokeandlimestoneinacertainproportion,andafterhigh-temperaturecalcinationandsmelting,theironoreisreducedbycoketoproducecrudeiron,whichiscalledpigiron.Thereactionprocessiscomplexandcanberepresentedbythefollowingequation:(removeSiO2)
Ironoremainlycontainsothermetallicornon-metallicimpuritiespresentinsilicatestate.Aftersmelting,mostoftheimpuritiesareconvertedintoslag,separatedandremoved,andasmallamountofimpuritiessuchasC,Mn,Si,S,Pareresidualinpigiron.Eglish2、碳素鋼如果將生鐵與其他輔助材料配合,進(jìn)一步冶煉,則雜質(zhì)被進(jìn)一步氧化除去,同時(shí)控制含碳量降至一定限度,硅錳等元素含量很低,硫磷等雜質(zhì)降至0.05%以下,則成為鐵及碳的合金碳素鋼。中文2、carbonsteelIfpigironiscombinedwithotherauxiliarymaterialsforfurthersmelting,impuritiesarefurtheroxidizedandremoved.Atthesametime,thecarboncontentiscontrolledtoacertainlimit,andthecontentofelementssuchassiliconandmanganeseisverylow.Impuritiessuchassulfurandphosphorusarereducedtobelow0.05%,makingitanalloycarbonsteelofironandcarbon.IronorelimestonecokeHightemperaturecombustionpigironauxiliarymaterialssmeltcarbonsteelEglish3、特種鋼
若適當(dāng)提高鋼中Si或Mn含量,或加入一定量的Ni,Cr,W,Mo,V,Ti等金屬,成為特種鋼(鐵合金或合金鋼)。
加Ni、Cr、W、Ti等又分別稱為Ni鋼、Cr鋼、W鋼、Ti鋼。加Ni增強(qiáng)鋼的強(qiáng)度及韌性,多用于承受沖擊或強(qiáng)大壓力的制件;含Ni36%鑄鋼受熱時(shí)幾乎不膨脹,可制精密儀器中文3、SpecialSteel
IftheSiorMncontentinthesteelisappropriatelyincreased,oracertainamountofmetalssuchasNi,Cr,W,Mo,V,Tiareadded,thesteelwillbecomespecialsteel(ferroalloyoralloysteel).
SteelcontainingNi,Cr,W,Ti,andotherelementsisalsoknownasNisteel,Crsteel,Wsteel,andTisteel,respectively.
Nienhancesthestrengthandtoughnessofsteel,whichiscommonlyusedinpartsthatneedtowithstandimpactorstrongpressure;Caststeelcontaining36%Nihardlyexpandswhenheated,makingitsuitableforprecisioninstrumentsEglish
加Cr的鋼耐熱耐腐蝕性較強(qiáng),多用于制造滾珠軸承或工具;含Cr12.5-18%的鉻鋼或含鉻0.6-1.75%、Ni1.25%的鎳鉻鋼,又稱不銹鋼,可制高壓鍋。
加W的鋼有極強(qiáng)的耐熱性,受熱至白熱化仍不軟化,常制運(yùn)轉(zhuǎn)的機(jī)件或刀具。
高速切削鋼:含W15–18%、V1–3%中文
ThesteelwithaddedCrhasstrongheatandcorrosionresistance,andismostlyusedformanufacturingballbearingsortools;ChromiumsteelwithCr12.5-18%ornickelchromiumsteelwithCr0.6-1.75%andNi1.25%,alsoknownasstainlesssteel,canbeusedtomakepressurecookers.
SteelwithaddedWhasextremelystrongheatresistanceanddoesnotsoftenevenwhenheatedtowhiteheat.Itiscommonlyusedforoperatingmachineryorcuttingtools.
Highspeedcuttingsteel:containingW15-18%andV1-3%Eglish二、各元素在鋼中的形態(tài)和作用
1、碳碳是鋼鐵的主要成分之一,它直接影響著鋼鐵的性能。碳是區(qū)別鐵與鋼,決定鋼號(hào)、品級(jí)的主要標(biāo)志。形態(tài):一般含碳增加,鋼鐵強(qiáng)度和硬度,但韌性和塑性,正是由于碳的存在,才能用熱處理方法來調(diào)節(jié)和改善其機(jī)械性能。中文二、Theformsandfunctionsofvariouselementsinsteel
1、CarbonCarbonisoneofthemaincomponentsofsteel,whichdirectlyaffectsitsperformance.Carbonisthemainsymbolthatdistinguishesironfromsteelanddeterminesthegradeofsteel.Generally,asthecarboncontentincreases,thestrengthandhardnessofsteelwilldecrease,butthetoughnessandplasticitywillincrease.Itispreciselybecauseofthepresenceofcarbonthatheattreatmentmethodscanbeusedtoregulateandimprovethemechanicalpropertiesofsteel.forms:freestatecompoundform:Eglish2、硅形態(tài)主要以硅化物:FeSi、MnSi、FeMnSi存在在高硅鋼中,一部分以SiC存在,有時(shí)也形成固熔體或硅酸鹽。作用
增強(qiáng)鋼的硬度、彈性及強(qiáng)度,提高抗氧化能力及耐酸性促使C以游離態(tài)石墨狀態(tài),使鋼高于流動(dòng)性,易于鑄造中文2、Siliconform:Mainlyexistingintheformofsilicides:FeSi,MnSi,FeMnSiInhighsiliconsteel,aportionofitexistsasSiCandsometimesformsasolidmeltorsilicate.role:
Enhancethehardness,elasticity,andstrengthofsteel,improveitsoxidationresistanceandacidresistancePromoteCtobeinafreegraphitestate,makingthesteelhigherinfluidityandeasiertocastEglish
形態(tài)主要以MnS或FeS狀態(tài)存在若:
使鋼產(chǎn)生“熱脆性”——有害成分原因:為什么產(chǎn)生熱脆性?
FeS的熔點(diǎn)較低,最后凝固,夾雜于鋼鐵的晶格之間。當(dāng)加熱壓制鋼鐵時(shí),F(xiàn)eS熔融,鋼鐵的晶粒失去連接作用而脆裂。3、硫國(guó)家標(biāo)準(zhǔn)規(guī)定,碳素鋼硫含量≤0.05%,優(yōu)質(zhì)鋼硫含量≤0.02%中文
form:MainlyexistinginMnSorFeSstateSulfurcauses"thermalbrittleness"insteel-harmfulcomponentsReason:Whydoessulfurcausesteeltodevelopthermalbrittleness?ThemeltingpointofFeSisrelativelylow,anditsolidifiesduringsteelmaking,withinclusionsbetweenthelatticeofthesteel.Whenheatingandpressingsteel,FeSmelts,andthegrainsofthesteellosetheirconnectionandbecomebrittle.3、SulfurAccordingtonationalstandards,thesulfurcontentofcarbonsteelis≤0.05%,andthesulfurcontentofhigh-qualitysteelis≤0.02%generateconversely,S+FeEglish形態(tài):以Fe2P或Fe3P狀態(tài)存在
作用磷化鐵硬度較強(qiáng),以至鋼鐵難于加工,并使鋼鐵產(chǎn)生“冷脆性”,也是有害雜質(zhì)。P↑→流動(dòng)性↑→易鑄造,并可避免在軋鋼時(shí)軋輥與壓件粘合4、磷磷含量≤0.06%中文
form:ExistinginFe2PorFe3Pstate
role:Ironphosphidehasastronghardness,makingitdifficulttoprocesssteelandcausingittodevelopcoldbrittleness.Phosphorusisalsoaharmfulimpurityinsteel.P↑→mobility↑→Easytocastandcanavoidadhesionbetweenrollersandpressedpartsduringsteelrolling4、PhosphorusPhosphoruscontent≤0.06%Eglish形態(tài)
主要以MnS狀態(tài)存在,如S含量較低,過量的錳可能組成MnC、MnSi、FeMnSi等,或以固熔體狀態(tài)存在。作用
增強(qiáng)鋼的硬度,減弱延展性,使鋼鐵具有良好的彈性和耐磨性。5、錳中文form:
ManganesemainlyexistsintheMnSstateinsteel.IftheScontentislow,excessmanganesemayformMnC,MnSi,FeMnSi,etc.,orexistinasolidmeltstate.role:
Manganesecanenhancethehardnessofsteel,weakenitsductility,andmakesteelhavegoodelasticityandwearresistance.
5、ManganeseEglish
綜上所述:
C是確定鋼鐵型號(hào)及用途→主要指標(biāo)
Si、Mn直接影響鋼鐵性能(有益的)→控制一定量
S、P有害成分→嚴(yán)格降至一定量因此,對(duì)于生鐵和碳素鋼:C、Si、Mn、S、P等五種元素的含量是冶金或機(jī)械工業(yè)化驗(yàn)室日常生產(chǎn)控制的重要指標(biāo).中文Insummary:Cistodeterminethetypeandpurposeofsteel→mainindicatorsSiandMndirectlyaffecttheperformanceofsteel(beneficial)→controlacertainamountSandPareharmfulcomponents→strictlyreducetoacertainamountTherefore,forpigironandcarbonsteel,thecontentofC,Si,Mn,S,andPisanimportantindicatorfordailyproductioncontrolinmetallurgicalormechanicalindustrylaboratoriesEglish項(xiàng)目六:鋼鐵分析任務(wù)二:鋼鐵中碳的測(cè)定鋼鐵中碳的測(cè)定課程:工業(yè)分析中文Scenario6:SteelanalysisTask2:DeterminationofcarboninsteelDeterminationofcarboninsteelCourse:IndustrialAnalysisEglish一、鋼鐵中碳的測(cè)定方法介紹碳的存在形式游離碳:不溶于酸化合碳:能溶于酸而破壞測(cè)定各種形態(tài)的碳屬于相分析;在成分分析中,一般鋼樣只測(cè)定總碳量。生鐵試樣除測(cè)定總碳量外,常分別測(cè)定游離碳和化合碳的含量。中文一、IntroductiontothedeterminationmethodofcarboninsteelTheexistenceformofcarbonFreecarbon:insolubleinacidsCompoundcarbon:candissolveinacidandbedestroyedTheoperationofmeasuringvariousformsofcarbonbelongstophaseanalysis;Incompositionanalysis,generallyonlythetotalcarboncontentismeasuredforsteelsamples.Inadditiontomeasuringthetotalcarboncontent,thecontentoffreecarbonandcombinedcarboninpigironsamplesisoftenmeasuredseparately.Eglish總碳量的測(cè)定方法有很多,但通常都是將試樣置于高溫氧氣流中燃燒,使之轉(zhuǎn)化為二氧化碳再用適當(dāng)方法測(cè)定,具體又分為以下幾種:燃燒-氣體容量法燃燒-庫侖法燃燒-非水滴定法中文Therearemanymethodsformeasuringtotalcarboncontent,andthemostcommonlyusedmethodisusuallytoburnthesampleinahigh-temperatureoxygenflow,convertitintocarbondioxide,andthenuseappropriatemethodstomeasureit.Specifically,thereareseveraltypes:combustiongascapacitymethodcombustioncoulombmethodcombustionnonaqueoustitrationmethodEglish1、燃燒-氣體容量法燃燒-氣體容積法是目前國(guó)內(nèi)外廣泛采用的標(biāo)準(zhǔn)方法。本法成本低,有較高的準(zhǔn)確度,測(cè)得結(jié)果是總碳量的絕對(duì)值。其缺點(diǎn)是要求有較熟練的操作技巧,分析時(shí)間較長(zhǎng),對(duì)低碳試樣測(cè)定誤差較大。中文1、CombustiongascapacitymethodThecombustiongasvolumemethodiscurrentlywidelyusedasastandardmethodbothdomesticallyandinternationally.Thismethodhaslowcostandhighaccuracy,andthemeasuredresultistheabsolutevalueoftotalcarboncontent.Itsdisadvantageisthatitrequiresproficientoperationalskills,longeranalysistime,andlargermeasurementerrorsforlow-carbonsamples.Measurementprocessstep1●Placethesampleinahigh-temperaturefurnaceandburnitafteroxygenisintroducedStep2ThegeneratedgascontainingCO2iscollectedinameasuringtubetomeasureitsvolume,andthenCO2isabsorbedbyKOHStep3MeasurethechangeingasvolumeinthemeasuringtubebeforeandafterabsorptionStep4CalculatetheresultsbasedonthetemperatureandpressureduringmeasurementEglish2、燃燒-庫侖法Ba(ClO4)2+CO2+H2OBaCO3+HClO4中文2、CombustioncoulombmethodBa(ClO4)2+CO2+H2OBaCO3+HClO4Measurementprocessstep1●Placethesampleinahigh-temperaturefurnaceandburnitafteroxygenisintroducedStep2ThegeneratedCO2isabsorbedbyaBa(ClO4)2solution,whichchangesthepHofthesolutionStep3ElectrolysisreturnsthepHofthesolutiontoitsinitialstateStep4CalculatecarboncontentbasedontheamountofelectricityconsumedbyelectrolysisEglish3、燃燒-非水滴定法中文3、CombustionnonaqueoustitrationmethodMeasurementprocessstep1step2step3Placethesampleinahigh-temperaturefurnaceandburnitafteroxygenisintroducedThegeneratedCO2isabsorbedbyanethanolethanolaminesolutionTitrationofabsorptionsolutionwithpotassiumethanolsolutionEglish二、燃燒-氣體容量法測(cè)定鋼鐵中碳1、方法原理試樣在1200~1300℃的高溫O2氣流中燃燒,鋼鐵中的碳被氧化生成CO2:C+O2=CO24Fe3C+13O2=4CO2+6Fe2O3
Mn3C+3O2=CO2+Mn3O3FeS+5O2=Fe3O4+3SO23MnS+5O2=Mn3O4+3SO2用KOH吸收CO2除硫劑:活性二氧化錳中文二、Determinationofcarboninsteelbycombustiongasvolumetricmethod1、Methodprinciple
ThesampleburnsinanO2airflowathightemperaturesrangingfrom1200to1300℃,andthecarboninthesteelisoxidizedtoproduceCO2:
C+O2=CO24Fe3C+13O2=4CO2+6Fe2O3
Mn3C+3O2=CO2+Mn3O3FeS+5O2=Fe3O4+3SO23MnS+5O2=Mn3O4+3SO2UsingKOHtoabsorbCO2Desulfurizationagent:activemanganesedioxideEglish圖
氣體容量法定碳裝置1-氧氣瓶,2-氧氣表,3-緩沖瓶,4、5-洗氣瓶,6-干燥塔,7-玻璃磨口塞,8-管式爐,9-燃燒管,10-除硫管,11-容量定碳儀(包括:冷凝管a、量氣管b、水準(zhǔn)瓶c、吸收瓶d、小旋塞e、三通旋塞f),l2-球形干燥管,13-瓷舟,14-溫度自動(dòng)控制器,15-供氧旋塞2、測(cè)定儀器中文GasCapacityCarbonizationDevice1-Oxygencylinder,2-Oxygenmeter,3-Buffercylinder,4,5-Washingcylinder,6-Dryingtower,7-Glassgrindingplug,8-Tubefurnace,9-Combustiontube,10-Sulfurremovaltube,11-Capacitycarbonanalyzer(includingcondensertubea,measuringtubeb,levelbottlec,absorptionbottled,smallcocke,three-waycockf),12-Sphericaldryingtube,13-Porcelainboat,14-Temperatureautomaticcontroller,15-Oxygensupplycock2、measuringinstrumentEglish3、測(cè)定試劑氫氧化鉀吸收劑溶液(400g/L);除硫劑活性二氧化錳(粒狀)或釩酸銀;酸性氯化鈉溶液(250g/L);助熔劑:錫粒(或錫片)、銅、氧化銅、純鐵粉;高錳酸鉀溶液(40g/L);甲基橙指示劑(2g/L)。中文3、TestingreagentsPotassiumhydroxideabsorbentsolution(400g/L);Sulfurremovalagent:activemanganesedioxide(granular)orsilvervanadate;Acidicsodiumchloridesolution(250g/L);Fluxes:tinparticles(ortinsheets),copper,copperoxide,pureironpowder;Potassiumpermanganatesolution(40g/L);Methylorangeindicator(2g/L).Eglish4、測(cè)定步驟將爐溫升至1200~1350℃,檢查管路及活塞是否漏氣,裝置是否正常,燃燒標(biāo)準(zhǔn)樣品,檢查儀器及操作。稱取適量試樣置于瓷舟中,將適量助熔劑覆蓋于試樣上面,打開玻璃磨口塞,將瓷舟放入瓷管內(nèi),用長(zhǎng)鉤推至高溫處,立即塞緊磨口塞。預(yù)熱lmin,按照定碳儀操作規(guī)程操作,測(cè)定其讀數(shù)(體積或含量)。打開磨口塞,用長(zhǎng)鉤將瓷舟拉出,即可進(jìn)行下一試樣分析。中文4、Measurementsteps
Raisethefurnacetemperatureto1200-1350℃,checkforleaksinthepipelinesandpistons,ensurethedeviceisfunctioningproperly,burnstandardsamples,andinspectinstrumentsandoperations.
Weighanappropriateamountofsampleandplaceitinaporcelainboat.Coverthesamplewithanappropriateamountofflux,opentheglassgrindingplug,placetheporcelainboatintotheporcelaintube,usealonghooktopushittoahightemperature,andimmediatelytightenthegrindingplug.Preheatforlmin,followtheoperatingproceduresofthecarbonanalyzer,andmeasureitsreading(volumeorcontent).Openthegrindingplugandpullouttheporcelainboatwithalonghooktoproceedwiththenextsampleanalysis.Eglish5、結(jié)果計(jì)算當(dāng)固定稱樣量如0.2500g、0.5000g或1.000g時(shí)的含碳量,其結(jié)果可按下式計(jì)算:
f—溫度、壓力補(bǔ)正系數(shù)中文5、resultcalculation
Whenthefixedsamplesizeis0.2500g,0.5000g,or1.000g,thecarboncontentresultcanbecalculatedusingthefollowingformula:
f—TemperatureandpressurecorrectioncoefficientsEglish項(xiàng)目六:鋼鐵分析任務(wù)二:鋼鐵中碳的測(cè)定燃燒-氣體容量法測(cè)定鋼鐵中碳課程:工業(yè)分析中文Scenario6:SteelanalysisTask2:DeterminationofcarboninsteelDeterminationofcarboninsteelbycombustiongasvolumetricmethodCourse:IndustrialAnalysisEglish1、方法原理試樣在1200~1300℃的高溫O2氣流中燃燒,鋼鐵中的碳被氧化生成CO2:C+O2=CO24Fe3C+13O2=4CO2+6Fe2O3
Mn3C+3O2=CO2+Mn3O3FeS+5O2=Fe3O4+3SO23MnS+5O2=Mn3O4+3SO2中文1、Methodprinciple
ThesampleburnsinanO2airflowathightemperaturesrangingfrom1200to1300℃,andthecarboninthesteelisoxidizedtoproduceCO2:C+O2=CO24Fe3C+13O2=4CO2+6Fe2O3
Mn3C+3O2=CO2+Mn3O3FeS+5O2=Fe3O4+3SO23MnS+5O2=Mn3O4+3SO2Eglish生成的CO2與過剩的O2經(jīng)導(dǎo)管引入量氣管,測(cè)定容積,然后通過裝有KOH溶液的吸收器,吸收其中的CO2CO2十2KOH=K2CO3十H2O剩余的O2再返回量氣管中,根據(jù)吸收前后容積之差,得到CO2的容積,據(jù)此計(jì)算出試樣中碳的質(zhì)量分?jǐn)?shù)。中文
First,introducethegeneratedmixtureofCO2andexcessO2intothevolumetrictube,measurethevolumeofthemixture,andthenintroducethemixtureintoanabsorbercontainingKOHsolutiontoabsorbtheCO2inside:
CO2+2KOH=K2CO3+H2O
TheremainingO2isreturnedtothemeasuringtube,andbasedonthedifferenceinvolumebeforeandafterabsorption,thevolumeofCO2isobtained.Basedonthis,themassfractionofcarboninthesampleiscalculated.Eglish圖
氣體容量法定碳裝置1-氧氣瓶,2-氧氣表,3-緩沖瓶,4、5-洗氣瓶,6-干燥塔,7-玻璃磨口塞,8-管式爐,9-燃燒管,10-除硫管,11-容量定碳儀(包括:冷凝管a、量氣管b、水準(zhǔn)瓶c、吸收瓶d、小旋塞e、三通旋塞f),l2-球形干燥管,13-瓷舟,14-溫度自動(dòng)控制器,15-供氧旋塞2、測(cè)定儀器中文2、measuringinstrumentGasCapacityCarbonizationDevice1-Oxygencylinder,2-Oxygenmeter,3-Buffercylinder,4,5-Washingcylinder,6-Dryingtower,7-Glassgrindingplug,8-Tubefurnace,9-Combustiontube,10-Sulfurremovaltube,11-Capacitycarbonanalyzer(includingcondensertubea,measuringtubeb,levelbottlec,absorptionbottled,smallcocke,three-waycockf),12-Sphericaldryingtube,13-Porcelainboat,14-Temperatureautomaticcontroller,15-OxygensupplycockEglish3、測(cè)定試劑氫氧化鉀吸收劑溶液(400g/L);除硫劑活性二氧化錳(粒狀)或釩酸銀;酸性氯化鈉溶液(250g/L);助熔劑:錫粒(或錫片)、銅、氧化銅、純鐵粉;高錳酸鉀溶液(40g/L);甲基橙指示劑(2g/L)。中文3、TestingreagentsPotassiumhydroxideabsorbentsolution(400g/L);Sulfurremovalagent:activemanganesedioxide(granular)orsilvervanadate;Acidicsodiumchloridesolution(250g/L);Fluxes:tinparticles(ortinsheets),copper,copperoxide,pureironpowder;Potassiumpermanganatesolution(40g/L);Methylorangeindicator(2g/L).Eglish4、測(cè)定步驟將爐溫升至1200~1350℃,檢查管路及活塞是否漏氣,裝置是否正常,燃燒標(biāo)準(zhǔn)樣品,檢查儀器及操作。稱取適量試樣置于瓷舟中,將適量助熔劑覆蓋于試樣上面,打開玻璃磨口塞,將瓷舟放入瓷管內(nèi),用長(zhǎng)鉤推至高溫處,立即塞緊磨口塞。預(yù)熱lmin,按照定碳儀操作規(guī)程操作,測(cè)定其讀數(shù)(體積或含量)。打開磨口塞,用長(zhǎng)鉤將瓷舟拉出,即可進(jìn)行下一試樣分析。中文4、Measurementsteps
Raisethefurnacetemperatureto1200-1350℃,checkforleaksinthepipelinesandpistons,ensurethedeviceisfunctioningproperly,burnstandardsamples,andinspectinstrumentsandoperations.
Weighanappropriateamountofsampleandplaceitinaporcelainboat.Coverthesamplewithanappropriateamountofflux,opentheglassgrindingplug,placetheporcelainboatintotheporcelaintube,usealonghooktopushittoahightemperature,andimmediatelytightenthegrindingplug.Preheatforlmin,followtheoperatingproceduresofthecarbonanalyzer,andmeasureitsreading(volumeorcontent).Openthegrindingplugandpullouttheporcelainboatwithalonghooktoproceedwiththenextsampleanalysis.Eglish5、測(cè)定注意事項(xiàng)助熔劑中含碳量一般不超過0.005%樣品的放置要均勻地鋪在燃燒舟中定碳儀應(yīng)裝置在室溫較正常的地方(距離高溫爐約300~500mm)更換水準(zhǔn)瓶所盛溶液、玻璃棉、除硫劑、氫氧化鉀溶液后,均應(yīng)作幾次高碳試樣,使二氧化碳飽和后,才可進(jìn)行試樣測(cè)定。中文5、MeasurementprecautionsThecarboncontentinthefluxgenerallydoesnotexceed0.005%ThesampleshouldbeplacedevenlyinthecombustionboatThecarbonanalyzershouldbeinstalledinaplacewithrelativelynormalroomtemperature(about300-500mmawayfromthehigh-temperaturefurnace)Afterreplacingthesolution
inthelevelingbottle,glasswool,sulfurremovalagent,andpotassiumhydroxidesolution,severalhighcarbonsamplecombustionshouldbecarriedouttosaturatecarbondioxideinthesesubstancesbeforesampledeterminationcanbecarriedout.Eglish對(duì)測(cè)定含硫量較高的試樣(大于0.2%),應(yīng)增加除硫劑量或增加一個(gè)除硫管。吸收器、水準(zhǔn)瓶?jī)?nèi)溶液以及混合氣體三者的溫度應(yīng)基本相同,否則將產(chǎn)生正負(fù)空白值。如分析完高碳試樣后,應(yīng)空燒一次,才可以接著做低碳試樣分析。當(dāng)洗氣瓶中硫酸體積顯著增加及二氧化錳變白時(shí),說明已失效,應(yīng)及時(shí)更換。觀察試樣是否完全燃燒,如燃燒不完全,需重新分析。中文Forsampleswithhighsulfurcontent(greaterthan0.2%),thesulfurremovaldoseshouldbeincreasedorasulfurremovaltubeshouldbeadded.Thetemperatureoftheabsorber,thesolutioninthelevelbottle,andthemixedgasshouldbebasicallythesame,otherwisepositiveandnegativeblankvalueswillbegenerated.Afteranalyzingthehighcarbonsample,itshouldbeburnedoncebeforeproceedingwiththeanalysisofthelowcarbonsample.Whenthevolumeofsulfuricacidinthegascylindersignificantlyincreasesandmanganesedioxideturnswhite,itindicatesthatithasfailedandshouldbereplacedinatimelymanner.Observewhetherthesampleiscompletelyburned.Ifthecombustionisincomplete,reanalysisisrequired.Eglish爐子升溫應(yīng)開始慢,逐步加速,以延長(zhǎng)硅碳棒壽命。分析前,應(yīng)先檢查儀器各部分是否漏氣。工作開始前及工作中,均應(yīng)燃燒標(biāo)準(zhǔn)樣品,判定工作過程中儀器的準(zhǔn)確性。吸收前后觀察刻度的時(shí)間應(yīng)一致。吸收后觀察刻度時(shí),量氣管及水準(zhǔn)瓶?jī)?nèi)液面與視線應(yīng)處在同一水平線上。吸收器中氫氧化鉀溶液使用久后也應(yīng)進(jìn)行更換,一般在分析2000次后更換,否則吸收效率降低,使測(cè)定結(jié)果偏低。測(cè)定中應(yīng)記錄溫度與大氣壓力,以確定補(bǔ)正系數(shù)f。如附錄八所示。中文Theheatingofthefurnaceshouldstartslowlyandthengraduallyacceleratetoextendthelifespanofthesiliconcarbiderod.Beforeanalysis,eachpartoftheinstrumentshouldbecheckedforairleakage.Beforeandduringwork,standardsamplesshouldbeburnedtodeterminetheaccuracyoftheinstrumentsusedduringtheworkprocess.Whenobservingthescaleafterabsorption,theliquidlevelinthemeasuringtubeandlevelbottleshouldbeonthesamehorizontalline.Thepotassiumhydroxidesolutionintheabsorberisusuallyreplacedafter2000analyses,otherwisetheabsorptionefficiencywilldecrease,resultinginlowermeasurementresults.Duringthemeasurement,temperatureandatmosphericpressureshouldberecordedtodeterminethecorrectioncoefficientf.ThecorrectioncoefficientsareshowninAppendix8.Eglish6、結(jié)果計(jì)算當(dāng)固定稱樣量如0.2500g、0.5000g或1.000g時(shí)的含碳量,其結(jié)果可按下式計(jì)算:
f—溫度、壓力補(bǔ)正系數(shù)中文6、resultcalculation
Whenthefixedsamplesizeis0.2500
g,0.5000
g,or1.000
g,thecarboncontentcanbecalculatedusingthefollowingformula::
f—TemperatureandpressurecorrectioncoefficientsEglish項(xiàng)目六:鋼鐵分析任務(wù)三:鋼鐵中硫的測(cè)定燃燒-碘量法測(cè)定鋼鐵中硫課程:工業(yè)分析中文Scenario6:SteelanalysisTask3:DeterminationofsulfurinsteelDeterminationofsulfurinsteelbycombustioniodimetryCourse:IndustrialAnalysisEglish一、燃燒-碘量法測(cè)定鋼鐵中硫?qū)撹F試樣于1250~1350℃的高溫下通氧燃燒,使硫全部轉(zhuǎn)化為二氧化硫,將生成的二氧化硫用淀粉溶液吸收,用碘酸鉀標(biāo)準(zhǔn)溶液滴定至淺藍(lán)色為終點(diǎn):
燃燒:4FeS+O2=2Fe2O3+4SO23MnS+5O2=Mn3O4+3SO2
吸收:SO2+H2O=H2SO3
滴定:KIO3+5KI+6HCl=3I2+6KCl+3H2OH2SO3+I2+H2O=H2SO4+2HI中文一、DeterminationofsulfurinsteelbycombustioniodimetryThesteelsampleisignitedwithoxygenatahightemperatureof1250-1350℃,andallsulfurinthesteelisconvertedintosulfurdioxide.Thegeneratedsulfurdioxideisabsorbedwithstarchsolutionandtitratedwithpotassiumiodatestandardsolutionuntiltheendpointislightblue:
combustion:4FeS+O2=2Fe2O3+4SO23MnS+5O2=Mn3O4+3SO2
absorption:SO2+H2O=H2SO3titration:KIO3+5KI+6HCl=3I2+6KCl+3H2OH2SO3+I2+H2O=H2SO4+2HIEglish1、主要試劑碘酸鉀標(biāo)準(zhǔn)滴定溶液:[c(1/6KI03)=0.01000mol/L、0.001000mol/L、0.0002500mol/L]淀粉吸收液(10g/L)助熔劑:二氧化錫和還原鐵粉以3+4比例混勻中文1、MainreagentsPotassiumiodatestandardtitrationsolution:[c(1/6KI03)=0.01000mol/L、0.001000mol/L、0.0002500mol/L]Starchabsorptionsolution(10g/L)
Flux:Mixtindioxideandreducedironpowderina3+4ratioEglish2、主要儀器定硫儀的滴定部分裝置1-球形管,2-吸收杯,3-滴定管中文2、MaininstrumentsDevicediagramofthetitrationsectionofthesulfuranalyzer1-Sphericaltube,2-Absorptioncup,3-BuretteEglish3、測(cè)定步驟將爐溫升至1200~1350
C,檢查裝置是否正常,于定硫吸收杯中加入淀粉吸收液(硫小于0.01%用低硫吸收杯,加20mL吸收液;硫大于0.01%用高硫吸收杯,加60mL吸收液),以600~1500mL/min的流速通氧,用碘酸鉀標(biāo)準(zhǔn)滴定溶液滴定至淺藍(lán)色不褪,作為終點(diǎn)色澤,關(guān)閉氧氣。中文3、Measurementsteps
Raisethefurnacetemperatureto1200-1350°C,checkifthedeviceisfunctioningproperly,addstarchabsorptionsolution(forsulfurlessthan0.01%,usealowsulfurabsorptioncup,add20mLofabsorptionsolution;forsulfurgreaterthan0.01%,useahighsulfurabsorptioncup,add60mLofabsorptionsolution)toafixedsulfurabsorptioncup,passoxygenataflowrateof600-1500mL/min,titratewithpotassiumiodatestandardtitrationsolutionuntillightbluedoesnotfadeastheendpointcolor,andturnoffoxygen.Eglish稱取適量試樣,置于瓷舟中,加入適量助熔劑,將瓷舟推至高溫處,預(yù)熱0.5~1.5min,通氧,控制氧速為1500~2000mL/min,燃燒后的混合氣體導(dǎo)入吸收杯中,使淀粉吸收液藍(lán)色開始消褪,立即用碘酸鉀標(biāo)準(zhǔn)溶液滴定并使液面保持藍(lán)色,當(dāng)吸收液褪色緩慢時(shí),滴定速度也相應(yīng)減饅,直至吸收液的色澤與原來的終點(diǎn)色澤相同,間歇通氣后,色澤不變即為終點(diǎn)。中文
Weighanappropriateamountofsample,placeitinaporcelainboat,addanappropriateamountofflux,pushtheporcelainboattoahightemperature,preheatfor0.5-1.5minutes,introduceoxygen,controltheoxygenrateto1500-2000mL/min,andintroducethemixedgasaftercombustionintotheabsorptioncup,sothatthebluecolorofthestarchabsorptionliquidbeginstofade.Immediatelytitratewithpotassiumiodatestandardsolutionandkeeptheliquidsurfaceblue.Whentheabsorptionliquidfadesslowly,thetitrationspeedalsodecreasesaccordingly,Untilthecoloroftheabsorptionsolutionisthesameastheoriginalendpointcolor,andafterintermittentventilation,thecolorremainsunchanged,whichistheendpoint.
Eglish4、結(jié)果計(jì)算T—碘酸鉀標(biāo)準(zhǔn)溶液對(duì)硫的滴定度,g/mL;V—滴定試樣所消耗碘酸鉀標(biāo)準(zhǔn)溶液的體積,mL;V0—滴定空白時(shí)所消耗碘酸鉀標(biāo)準(zhǔn)溶液的平均體積,mL;m—試料的質(zhì)量,g。中文4、resultcalculationT—Titrationofpotassiumiodatestandardsolutionforsulfur,g/mL;V—Thevolumeofpotassiumiodatestandardsolutionconsumedintitratingthesample,mL;V0—Theaveragevolumeofpotassiumiodatestandardsolutionconsumedduringtitrationofblank,mL;m—Qualityoftestmaterials,g。Eglish項(xiàng)目六:鋼鐵分析任務(wù)三:鋼鐵中硫的測(cè)定鋼鐵中硫的測(cè)定方法介紹課程:工業(yè)分析中文Scenario6:SteelanalysisTask3:DeterminationofsulfurinsteelIntroductiontothedeterminationmethodofsulfurinsteelCourse:IndustrialAnalysisEglish一、鋼鐵中硫的危害硫是鋼鐵中有害元素,使鋼鐵產(chǎn)生熱脆性鋼鐵中硫燃燒生成SO2或SO3,會(huì)污染環(huán)境,腐蝕設(shè)備鋼鐵中硫在高溫下遇到氫會(huì)化合生成H2S,該氣體是劇毒氣體,對(duì)人體有害中文
一、ThehazardsofsulfurinsteelSulfurisaharmfulelementinsteel,causingittodevelopthermalbrittlenessThecombustionofsulfurinsteelgeneratesSO2orSO3,whichcanpollutetheenvironmentandcorrodeequipmentSulfurinsteelwillreactwithhydrogenathightemperaturestoformH2S,ahighlytoxicgasthatisharmfultohumanhealthEglish二、測(cè)定方法重量法燃燒法燃燒-滴定法燃燒-分光光度法燃燒-電導(dǎo)法燃燒-紅外光譜法中文二、MeasurementmethodgravimetricmethodCombustionCombustiontitrationmethodCombustionspectrophotometryCombustionconductivitymethodCombustioninfraredspectroscopyEglish1、重量法因硫酸鋇沉淀溶解而產(chǎn)生負(fù)偏差測(cè)定過程第一步第二步第三步樣品用酸分解成硫酸鹽試樣溶液加入氯化鋇使生成硫酸鋇沉淀過濾沉淀,洗滌灼燒,稱重計(jì)算中文1、gravimetricmethodNegativedeviationcausedbydissolutionofbariumsulfateprecipitationstep1step2step3
ThesampleisdecomposedintosulfatesusingacidAddingBaCl2tothesamplesolutiontogenerateBaSO4
precipitateFiltersediment,washandburn,weighandcalculateMeasurementprocessEglish2、燃燒法測(cè)定依據(jù)是讓鋼鐵燃燒,其中硫轉(zhuǎn)化為SO2而測(cè)定,方法缺點(diǎn)是硫的回收率低于90%,有時(shí)甚至更低,為提高測(cè)定準(zhǔn)確性,常需注意以下幾點(diǎn):燃燒溫度要高:1450~1510℃燃燒時(shí)間足夠注意減少SO2的吸附選用優(yōu)良的助熔劑防止SO2的接觸轉(zhuǎn)化中文2、CombustionmethodThedeterminationisbasedonthecombustionofsteel,inwhichsulfurisconvertedintoSO2.Thedisadvantageofthismethodisthattherecoveryrateofsulfurislessthan90%,sometimesevenlower.Toimprovetheaccuracyofthedetermination,thefollowingpointsshouldbenoted:Thecombustiontemperatureshouldbehigh:1450-1510℃SufficientcombustiontimePayattentiontoreducingtheadsorptionofSO2SelectexcellentfluxesPreventthecontactconversionofSO2Eglish(1)燃燒-滴定法碘量法:SO2經(jīng)水吸收成為亞硫酸,用碘滴定酸堿法:SO2經(jīng)過氧化氫水溶液吸收轉(zhuǎn)化為硫酸,用堿滴定硼酸鈉法:用0.2%硫酸鉀和4%過氧化氫水溶液吸收SO2,用硼酸鈉滴定生成的硫酸中文(1)CombustiontitrationmethodIodometricmethod:SO2isabsorbedbywatertoformsulfite,whichistitratedwithiodineAcid-basetitrationmethod:SO2isabsorbedandconvertedintosulfuricacidbyhydrogenoxideaqueoussolution,andthentitratedwithalkaliSodiumboratemethod:AbsorbSO2with0.2%potassiumsulfateand4%hydrogenperoxideaqueoussolution,anddetermineth
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