鋼鐵及合金化學(xué)分析方法

NACIS/CH011:2005PAGE1鋼鐵及合金化學(xué)分析方法ICP－AES法測定錳、鐵、鋁、磷、鉻、釩、鈦、銅、鈷、鎳、鉬、鈰、鈣、鎂、鋅、錫、銻和砷含量Methodsforchemicalanalysisofiron,steelandalloyTheICP－AESmethodforthedeterminationofmanganese,iron,Aluminium,phosphorus,chromium,vanadium,titanium,cupper,Cobalt,nickelmolybdenum,cerium,calcium,zinc,tin，antimonyandarseniccontent1范圍本方法用電感耦合等離子發(fā)射光譜法測定鋼鐵及合金中錳、鐵、鋁、磷、鉻、釩、鈦、銅、鈷、鎳、鉬、鈰、鈣、鎂、鋅、錫和銻含量。測定范圍：錳、鐵、鋁、磷、鉻、釩、鈦、銅、鈷、鎳、鉬、鈰、錫和銻0.005％～0.25％；鈣、鎂0.0005％～0.10％鋅0.001％～0.10％2方法提要樣品溶于鹽酸、硝酸混合酸中，定容。將溶液引入ICP－AES，測量每個元素分析線的發(fā)光強(qiáng)度，根據(jù)溶液中待測元素的強(qiáng)度與濃度成正比的關(guān)系，自動計(jì)算出待測元素的百分含量。3試劑和材料3.1鹽酸（優(yōu)級純），ρ1.19g／mL3.2硝酸（優(yōu)級純），ρ1.42g／mL3.3鈣標(biāo)準(zhǔn)溶液,10.0μg／mL,100μg／mL3.4鎂標(biāo)準(zhǔn)溶液,10.0μg／mL,100μg／mL3.5鐵標(biāo)準(zhǔn)溶液,100μg／mL3.6錳標(biāo)準(zhǔn)溶液,100μg／mL3.7鋁標(biāo)準(zhǔn)溶液,100μg／mL3.8磷標(biāo)準(zhǔn)溶液,100μg／mL3.9鉻標(biāo)準(zhǔn)溶液,100μg／mL3.10釩標(biāo)準(zhǔn)溶液,100μg／mL3.11鈦標(biāo)準(zhǔn)溶液,100μg／mL3.12銅標(biāo)準(zhǔn)溶液,100μg／mL3.13鈷標(biāo)準(zhǔn)溶液,100μg／mL3.14鎳標(biāo)準(zhǔn)溶液,100μg／mL3.15鉬標(biāo)準(zhǔn)溶液,100μg／mL3.16鈰標(biāo)準(zhǔn)溶液,100μg／mL3.17鋅標(biāo)準(zhǔn)溶液，10.0μg／mL，100μg／mL3.18錫標(biāo)準(zhǔn)溶液，10.0μg／mL，100μg／mL3.19銻標(biāo)準(zhǔn)溶液，10.0μg／mL，100μg／mL3.20高純鐵、鎳金屬（加入基體元素用）4儀器與設(shè)備等離子體光譜儀。Table1分析元素譜線分析元素譜線,nm可能出現(xiàn)光譜干擾的元素Mn257.610Co、Zr、W、Nb293.306293.930Fe259.940MoAl396.152Mo394.401Ni308.215Mn、V、MoP178.2213.618Cu、MoCr267.716Fe、Mn、VV309.311Al、Cr、Fe、Mg310.230Fe、Ni、Ti311.071TiTi337.280Ni、V308.8Cu327.396Nb、Mo324.154Nb、Mo、MnCo228.616Cr、Fe、Ni、TiNi231.604CoMo281.6Al、Mn、TiCe418.660Fe、V413.380Ca、Fe、V456.236Ca317.9Cr、Fe、V393.3VMg280.2Cr、Mn、V279.079Fe、MnZn202.548Ni、Cu206.200213.856FeSn189.989Sb206.883測定樣品時根據(jù)具體情況確定可能出現(xiàn)的譜線干擾及干擾程度篩選適合的譜線。5操作步驟5.1樣品溶液的制備準(zhǔn)確稱取試樣0.5000g，放入50mL玻璃燒杯中，根據(jù)不同的鋼鐵材料加入不同比例的鹽酸、硝酸10mL，在電熱板上加熱溶解，待試樣溶液冷卻后，轉(zhuǎn)入50mL容量瓶中定容，混勻。5.2標(biāo)準(zhǔn)溶液的制備選擇一系列與樣品基體匹配的標(biāo)鋼，按照樣品溶液的制備方法制備一系列標(biāo)準(zhǔn)溶液。如沒合適標(biāo)鋼，可用與試樣基體一致的純金屬打底，加入待測元素的標(biāo)準(zhǔn)溶液進(jìn)行配制。5.3光譜測量的準(zhǔn)備開機(jī)，使得測量前儀器至少正常運(yùn)行20min。根據(jù)廠商的指導(dǎo)調(diào)節(jié)儀器使之處于最佳狀態(tài)。調(diào)出程序，建分析方法。5.4測量依次測量標(biāo)準(zhǔn)溶液和樣品溶液的強(qiáng)度值。5.5標(biāo)準(zhǔn)曲線的繪制以標(biāo)準(zhǔn)溶液的強(qiáng)度比為橫坐標(biāo)，元素含量為縱坐標(biāo)，計(jì)算機(jī)自動繪制工作曲線。以質(zhì)量百分?jǐn)?shù)表示元素的含量。5.6計(jì)算測量樣品時，計(jì)算機(jī)自動給出樣品元素的含量。6附注6.1由于鈣、鎂和鋅易沾污，制備標(biāo)準(zhǔn)溶液時不適合與其它多元素混在一起，需單獨(dú)配制。測量時與其它元素分開測量。6.2分析鈣、鎂和鋅時要帶試劑空白。7允許差在95%置信水平下，平行測定結(jié)果之間的允許差不超過下表給出的值。Table2ManganesepermissibledeviationManganesecontent,%PermissibledeviationManganesecontent,%Permissibledeviation0.005~0.0100.002>0.100~0.2000.008>0.010~0.0500.004<0.2500.010>0.050~0.1000.006Table3IronpermissibledeviationIroncontent,%PermissibledeviationIroncontent,%Permissibledeviation0.005~0.0100.003>0.100~0.2000.010>0.010~0.0500.005<0.2500.015>0.050~0.1000.007Table4AluminiumpermissibledeviationAluminiumcontent,%PermissibledeviationAluminiumcontent,%Permissibledeviation0.005~0.0100.004>0.100~0.200.016>0.010~0.0500.008<0.2500.20>0.050~0.1000.013Table5PhosphoruspermissibledeviationPhosphoruscontent,%PermissibledeviationPhosphoruscontent,%Permissibledeviation0.005~0.0100.002>0.080~0.1000.008>0.010~0.0300.004>0.100~0.1500.010>0.030~0.0600.005>0.150~0.2000.012>0.060~0.0800.007<0.2500.014Table6ChromiumpermissibledeviationChromiumcontent,%PermissibledeviationChromiumcontent,%Permissibledeviation0.005~0.0100.003>0.100~0.2000.010>0.010~0.0500.005<0.2500.015>0.050~0.1000.007Table7VanadiumpermissibledeviationVanadiumcontent,%PermissibledeviationVanadiumcontent,%Permissibledeviation0.005~0.0100.004>0.100~0.2000.016>0.010~0.0500.008<0.2500.020>0.050~0.1000.013Table8TitaniumpermissibledeviationTitaniumcontent,%PermissibledeviationTitaniumcontent,%Permissibledeviation0.005~0.0100.004>0.100~0.2000.009>0.010~0.0500.006<0.2500.010>0.050~0.1000.007Table9CopperpermissibledeviationCoppercontent,%PermissibledeviationCoppercontent,%Permissibledeviation0.005~0.0100.004>0.100~0.2000.014>0.010~0.0500.008<0.2500.016>0.050~0.1000.007Table10CobaltpermissibledeviationCobaltcontent,%PermissibledeviationCobaltcontent,%Permissibledeviation0.005~0.0100.004>0.100~0.2000.016>0.010~0.0500.008<0.2500.020>0.050~0.1000.013Table11NickelpermissibledeviationNickelcontent,%PermissibledeviationNickelcontent,%Permissibledeviation0.005~0.0100.002>0.100~0.2000.008>0.010~0.0500.004<0.2500.010>0.050~0.1000.006Table12MolybdenumpermissibledeviationMolybdenumcontent,%PermissibledeviationMolybdenumcontent,%Permissibledeviation0.005~0.0100.002>0.100~0.2000.011>0.010~0.0500.005<0.2500.014>0.050~0.1000.008Table13CeriumpermissibledeviationCeriumcontent,%PermissibledeviationCeriumcontent,%Permissibledeviation0.005~0.0100.002>0.100~0.2000.0116>0.010~0.0500.006<0.2500.020>0.050~0.1000.010Table14CalciumpermissibledeviationCalciumcontent,%PermissibledeviationCalciumcontent,%Permissibledeviation0.0005~0.00100.0001>0.010~0.0500.00050.0010~0.0100.0003>0.050~0.1000.0006Table15MagnesiumpermissibledeviationMagnesiumcontent,%PermissibledeviationMagnesiumcontent,%Permissibledeviation0.0005~0.00100.0001>0.010~0.0500.00050.0010~0.0100.0003>0.050~0.1000.0008Table16ZincpermissibledeviationZinccontent,%PermissibledeviationMagnesiumcontent,%Permissibledeviation0.001~0.0100.0003>0.050~0.1000.0008>0.010~0.0500.0005Table17TinpermissibledeviationTincontent,%PermissibledeviationManganesecontent,%Permissibledeviation0.005~0.0100.002>0.100~0.2000.008>0.010