搜索
143(,430074)SiAlCaFeMgTiKBaMnVPbCrCuZn,0.1g10mL1mL,10mL4%,,94.2%102.3%;RSD5%,,,2002212216;2003204218(No.G1999022212,2002CB211602)1,,SiO2Al2O3,1,2,,SiNaOH700,HCl;AlCaFeMgTiMnKHClO4HFHCl;PbCrHClO4HFHNO322.1MARS25(CEM),100mL,()TraceScan(ThermoJarrellAsh)GBW08401()1000mg/LHClHNO3H2O2HFH3BO3,(HNO3HClH2O=129)24h,2.2ICP2AES2(mg/L):Al(20),Fe(10),CaMgTiBaKMn(5),VPbCrCuZn(3)Si(30)HNO3HFH3BO3:1150W,18L/min,1L/min,0.45L/min,30psi,1.85mL/min,10s2.30.1g(0.0002g),10mLHNO31mLHF,,,,,,31200311(FENXIHUAXUE)ChineseJournalofAnalyticalChemistry11136013636,1200W,110,15min,15min,4%(W/V)H3BO310mL,,,1200W,10015min,,50mL,,,,,BaMnVPbCrCuZn5mL,100mL,SiAlCaFeMgTiK61h33.1HNO3HNO32HFHNO32HCl2HFHNO32H2O22HF,:HNO3(HF),SiO2,Si(0.2%)HNO32H2O22HF,Si(12.5%),H2O230min,SiF4HNO32HFHNO32HCl2HF,HNO32HF,:0.1g10mLHNO31mLHF,AlCaMg(AlF3CaF2MgF2),H3BO3,,:4AlF3+3H3BO3+12H+4Al3++3HBF4+9H2O2CaF2+H3BO3+4H+2Ca2++HBF4+3H2O2MgF2+H3BO3+4H+2Mg2++HBF4+3H2OH3BO3,AlCaMgH3BO3,,,,H3BO3,H3BO3HF,,,H3BO3:H3BO3+3HFHBF3OH+2H2OHBF3OH+HFHBF4+H2O110140,:,,SiAlFeCa,,:200mg/LAlMn,,3Al200mg/L,3.2,,,,,,,,11,313.3,GBW0840114,294.2%102.3%;RSD5%,3.4GBW0840114,33,163111:141Table1AnalyticalwavelengthsanddetectionlimitsofelementsElement(nm)Wavelength(g/L)DetectionlimitElement(nm)Wavelength(g/L)DetectionlimitSi251.630.0Ba445.44.5Al308.215.0Mn257.62.2Ca317.914.0V292.438.0Fe259.95.2Pb220.316.0Mg285.23.5Cr267.79.1Ti334.93.6Cu324.72.6K766.468.0Zn313.810.52(n=5)Table2Recoveryofspikedelementsincoalflyash(n=5)ElementContent(mg/L)Added(mg/L)Found(mg/L)Recovery(%)RSD(%)Si23.8820.0043.0598.12.4Al12.9310.0022.5698.44.1Ca2.795.007.5496.82.0Fe7.655.0012.94102.33.1Mg0.541.001.5197.83.4Ti0.581.001.5095.01.5K1.011.001.9798.22.6Ba2.905.007.7898.54.3Mn2.365.007.3299.43.7V0.190.500.6695.53.8Pb0.0680.500.5394.21.9Cr0.120.500.6096.23.2Cu0.1060.500.5895.41.2Zn0.1220.500.6096.52.03Table3AnalyticalresultsoftheelementsincoalflyashElementFound(%)Certified(%)ElementFound(%)Certified(%)Si23.1223.88Ba0.14420.1450Al12.1012.93Mn0.12070.11780.0040Ca2.862.79V0.00930.00950.0009Fe7.787.650.14Pb0.00380.00340.0004Mg0.520.54Cr0.00640.00600.0007Ti0.570.58Cu0.00510.00530.0004K1.041.01Zn0.00560.00610.0007References1WangZijian(),XieShenmeng(),GaoYuxi(),PengAn().ChineseJ.Anal.Chem.(),1999,27(10):120012032WenXH,WuLZ,ZhangY,ChuY.FreseniusJ.Anal.Chem.,1997,357:111111153LiuDongyan(),ZhangYuanli().SpectroscopyandSpectralAnalysis(),2000,20(4):514517263131Determinationof14ElementsinCoalAshbyMicrowaveDigestionandInductivelyCoupledPlasmaAtomicEmissionSpectrometryLiuJing3,ZhengChuguang,JiaXiaohong,XuJieying(NationalLaboratoryofCoalCombustion,HuazhongUniversityofScienceandTechnology,Wuhan430074)AbstractAmethodofdetermining14elements(SiAlCaFeMgTiKBaMnVPbCrCuZn)incoalashbymicrowavedigestionandinductivelycoupledplasmaatomicemissionspectrometryisreported.Microwavedigestionsystemanddigestionconditionswereinvestigated.Coalashwasdigestedbynitricacidandhydrofluoricacid,andthenboricacidsolutionwasaddedtodecomposethefluoridedeposit.Themethodwasapplicableforthedeterminationoftheseelementsandtheresultswereingoodagreementwiththecertifiedvaluesofcoalflyashstandardreferencematerial.Thismethodissimpleandrapid.Testingresultsshowthatrecoveryfortheelementsdeterminedisfrom94.2%to102.3%,andRSDisbelow5%.KeywordsMicrowavedigestion,inductivelycoupledplasmaatomicemissionspectrometry,coalash,multielementanalysis(Received16December2002;accepted18April2003)2002CAChemicalAbstractsServiceSourceIndexQuarterlyNo.4,2002()79CA,(40)CACA1114214842184224903187234964()22224()5015256255196()2652654772762755383052857393092958810318306001132331619123693263913371336491438834651154183565216419366681742337()6701842738682194713968920()48340690()363111:14