原子吸收光谱.pdf

原子吸收光谱分析培训教材原子吸收光谱分析培训教材(基础知识与基本操作基础知识与基本操作)珀金埃尔默仪器(上海)有限公司 张扬祖 编 原子吸收光谱分析原子吸收光谱分析原子吸收光谱分析原子吸收光谱分析应用与仪器操作培训应用与仪器操作培训应用与仪器操作培训应用与仪器操作培训PerkinElmer Shanghai 张扬祖编課程內容課程內容課程內容課程內容1.1.原子吸收光谱分析的基本知识原子吸收光谱分析的基本知识原子吸收光谱分析的基本知识原子吸收光谱分析的基本知识1.11.1原子吸收光谱分析原理原子吸收光谱分析原理原子吸收光谱分析原理原子吸收光谱分析原理1.21.2原子吸收光谱仪器的组成原子吸收光谱仪器的组成原子吸收光谱仪器的组成原子吸收光谱仪器的组成1.31.3原子吸收光谱分析中的干扰及其消除原子吸收光谱分析中的干扰及其消除原子吸收光谱分析中的干扰及其消除原子吸收光谱分析中的干扰及其消除1.41.4原子吸收光谱分析的准确性保证原子吸收光谱分析的准确性保证原子吸收光谱分析的准确性保证原子吸收光谱分析的准确性保证2.2.原子吸收光谱仪器操作原子吸收光谱仪器操作原子吸收光谱仪器操作原子吸收光谱仪器操作2.12.1火焰法操作火焰法操作火焰法操作火焰法操作2.22.2石墨炉法操作石墨炉法操作石墨炉法操作石墨炉法操作2.32.3操作过程中的安全注意事项操作过程中的安全注意事项操作过程中的安全注意事项操作过程中的安全注意事项2.42.4仪器测定条件优化仪器测定条件优化仪器测定条件优化仪器测定条件优化2.52.5仪器维护保养仪器维护保养仪器维护保养仪器维护保养2.62.6测定数据处理测定数据处理测定数据处理测定数据处理现代无机元素分析的四种手段现代无机元素分析的四种手段现代无机元素分析的四种手段现代无机元素分析的四种手段1.1.原子吸收光谱分析原子吸收光谱分析原子吸收光谱分析原子吸收光谱分析(AAS)AAS)2.2.原子发射光谱分析原子发射光谱分析原子发射光谱分析原子发射光谱分析(ICPICP-OES)OES)3.3.原子荧光光谱分析原子荧光光谱分析原子荧光光谱分析原子荧光光谱分析(AFS)AFS)4.4.等离子体质谱等离子体质谱等离子体质谱等离子体质谱(ICPICP-MS)MS)Origins of Atomic SpectraOrigins of Atomic Spectra+eeeE=hvLightExcitedStatesDecay and Emission+eMoM*+Eback to ground state+E-E MoLightExcitation+eMoM*+Eexcited electron+EnergyPrinciple of Atomic SpectroscopyPrinciple of Atomic SpectroscopyHHeLiMEnergyEmission(e)Absorption(a)IonizationAbsorption(a)Emission(e)BeGround stateExcitation levelIonizationV:Ionizsation potentialEn,Em:Excitation potential E=En-Em=h EnEmVAAAA与与与与ICPICP-OES,OES,ICPICP-MSMS的检出限的检出限的检出限的检出限之比較表之比較表之比較表之比較表Atomic SpectroscopyAtomic Spectroscopy EMISSIONEMISSIONMMo o+heat +heat MM*MMo o+light+light ABSORPTIONABSORPTIONMMo o+light +light MM*原子吸收光谱分析原理原子吸收光谱分析原理原子吸收光谱分析原理原子吸收光谱分析原理(1)(1)pp锐线光源与连续光源锐线光源与连续光源锐线光源与连续光源锐线光源与连续光源A=log(IA=log(I0/It)0/It)A=log(I0+IA=log(I0+I)/(It+I)/(It+I)Atomic AbsorptionAtomic Absorptionsample absorptionsource emission0.003 nm0.001 nm原子吸收光谱分析原理原子吸收光谱分析原理原子吸收光谱分析原理原子吸收光谱分析原理(2)(2)pp相对测量方式相对测量方式相对测量方式相对测量方式pp基态原子吸收基态原子吸收基态原子吸收基态原子吸收pp溶液状态进样溶液状态进样溶液状态进样溶液状态进样pp元素总量测定元素总量测定元素总量测定元素总量测定可供选用的原子吸收测定技术可供选用的原子吸收测定技术可供选用的原子吸收测定技术可供选用的原子吸收测定技术火焰原子吸收法火焰原子吸收法火焰原子吸收法火焰原子吸收法(AIRAIR-C2H2,N2OC2H2,N2O-C2H2)C2H2)石墨炉原子吸收法石墨炉原子吸收法石墨炉原子吸收法石墨炉原子吸收法氢化物发生原子吸收法氢化物发生原子吸收法氢化物发生原子吸收法氢化物发生原子吸收法动注射动注射动注射动注射-火焰原子吸收法火焰原子吸收法火焰原子吸收法火焰原子吸收法动注射动注射动注射动注射-石墨炉原子吸收法石墨炉原子吸收法石墨炉原子吸收法石墨炉原子吸收法动注射测汞法动注射测汞法动注射测汞法动注射测汞法火焰原子发射法火焰原子发射法火焰原子发射法火焰原子发射法空气空气空气空气-乙炔火焰的应用乙炔火焰的应用乙炔火焰的应用乙炔火焰的应用特点特点特点特点:安全安全安全安全,稳定稳定稳定稳定,灵敏高灵敏高灵敏高灵敏高可测元素可测元素可测元素可测元素:Ag,As,Au,Bi,Ca,Ag,As,Au,Bi,Ca,CdCd,Co,Cr,Cs,Cu,Fe,Hg,In,Co,Cr,Cs,Cu,Fe,Hg,In,Ir Ir,K,Li,Mg,K,Li,Mg,MnMn,Na,Ni,Na,Ni,PbPb,Pd,Pt,Pd,Pt,RbRb,RhRh,RuRu,SbSb,Se,Se,TcTc,Te,Te,TlTl,ZnZn共共共共3232个元素个元素个元素个元素一氧化二氮一氧化二氮一氧化二氮一氧化二氮-乙炔火焰的应用乙炔火焰的应用乙炔火焰的应用乙炔火焰的应用特点特点特点特点:温高温高温高温高,化学干扰少化学干扰少化学干扰少化学干扰少,灵敏较低灵敏较低灵敏较低灵敏较低可测元素可测元素可测元素可测元素Al,B,Al,B,BaBa,Be,Be,DyDy,ErEr,EuEu,GaGa,GdGd,GeGe,HfHf,Ho,La,Lu,Mo,Ho,La,Lu,Mo,NbNb,NdNd,Os,P,Pr,Re,Sc,Os,P,Pr,Re,Sc,SiSi,SmSm,SnSn,SrSr,Ta,Tb,Ti,Tm,U,V,W,Y,Ta,Tb,Ti,Tm,U,V,W,Y,YbYb,Zr Zr 共共共共3636个元素个元素个元素个元素石墨炉原子吸收技术石墨炉原子吸收技术石墨炉原子吸收技术石墨炉原子吸收技术特点特点特点特点:灵敏高灵敏高灵敏高灵敏高,检出限低检出限低检出限低检出限低,样品用少样品用少样品用少样品用少,自动化程高自动化程高自动化程高自动化程高可测元素可测元素可测元素可测元素:Ag,Al,As,Au,B,Ag,Al,As,Au,B,BaBa,Be,Bi,Ca,Be,Bi,Ca,CdCd,Co,Cr,Cs,Cu,Co,Cr,Cs,Cu,DyDy,ErEr,EuEu,Fe,Fe,GaGa,GdGd,GeGe,Hg,Hg,In,In,Ir Ir,K,La,Li,Mg,K,La,Li,Mg,MnMn,Mo,Na,Mo,Na,NdNd,Ni,Os,P,Ni,Os,P,PbPb,Pd,Pt,Pd,Pt,RbRb,RhRh,RuRu,SbSeSbSe,SiSi,SmSm,SnSn,SrSr,Te,Ti,Tm,U,V,Y,Te,Ti,Tm,U,V,Y,YbYb,Zn ,Zn 共共共共5656个元素个元素个元素个元素空气空气空气空气-乙炔火焰发射的应用乙炔火焰发射的应用乙炔火焰发射的应用乙炔火焰发射的应用特点特点特点特点:无需灯光源无需灯光源无需灯光源无需灯光源,灵敏高灵敏高灵敏高灵敏高可测元素可测元素可测元素可测元素:Cs,K,Na,P,Cs,K,Na,P,RbRb,Se,Se,TcTc氢化物形成原子吸收测定氢化物形成原子吸收测定氢化物形成原子吸收测定氢化物形成原子吸收测定1.1.可测元素可测元素可测元素可测元素:As,Se,As,Se,SbSb,Bi,Bi,SnSn,Te,Hg,Te,Hg2.2.分析性能特点分析性能特点分析性能特点分析性能特点:灵敏高灵敏高灵敏高灵敏高,检出限低检出限低检出限低检出限低,基体干扰少基体干扰少基体干扰少基体干扰少3.3.灵敏度与测定元素的价态相关灵敏度与测定元素的价态相关灵敏度与测定元素的价态相关灵敏度与测定元素的价态相关原子吸收光谱仪的组成原子吸收光谱仪的组成原子吸收光谱仪的组成原子吸收光谱仪的组成12345Sample(1)Light source(hollow cathode lamp)(1)Light source(hollow cathode lamp)(2)Sample cell/Atom reservoir(flame or furnace)(2)Sample cell/Atom reservoir(flame or furnace)(3)Light separation(monochrometer)(3)Light separation(monochrometer)(4)Light measurement(detector)(4)Light measurement(detector)(5)Signal processing(computer/software)(5)Signal processing(computer/software)Typical AA Spectrometer ComponentsMonochromatorDetectorSample CellLight SourceResultsChopperE Electrodelesslectrodeless D Discharge ischarge L LampampLight SourceHollow Cathode Lamp+-Ne or ArFill GasEnd WindowAnodeCathodeHollow Cathode LampEmission Process+-+-+-+-1.Ionization2.Sputtering3.Excitation4.EmissionNeoNe+Ne+MoNe+MoM*M*MoLightConsiderations with EDLsAdvantages?Lower gain?Higher absorbances?Better sensitivity?Longer lifetime?Greater intensityDisadvantages?Require warm-up?May require separate power supplyAtomic Absorption SpectroscopyAtomic Absorption SpectroscopyppTypically heat is used to break molecular bondsTypically heat is used to break molecular bondsCaCaClClClClCaCaClClClClGraphite Furnace AAGraphite Furnace AAFlame AAFlame AAPrinciple of Flame Atomic Absorption(FLAAS)1ppm2ppmElement:CdWave length:228.8 nmSlit:0.4 nmAbsorbanceProblems of FLAAS-Poor sensitivity.-Not multi-element.-Narrow dynamic range.(Atomic Absorption Spectrometer)Flammable gas Inflammable gasDetectorSlitSlitGrating driven by motorHollow Cathode lampSampleFlameProcess in a Flame AAProcess in a Flame AADrainNebulizationSolutionSolidVaporizationMAMo+AoAtomizationMoM*ExcitationM*M+e-IonizationBurner AssemblyBurner AssemblyNew corrosion resistant New corrosion resistant nebulizernebulizer designdesignppHigh Sensitivity designHigh Sensitivity designppOne design for both airOne design for both air-acetylene and nitrous acetylene and nitrous oxideoxideppUses ceramic impact Uses ceramic impact beadbeadppSample tubing Sample tubing connected via a screw connected via a screw fitting for easy fitting for easy replacementreplacementBurner Head SelectionBurner Head Selection 10 10-cm head:general purpose for aircm head:general purpose for air-acetylene acetylene operationoperation 5 5-cm head:for nitrous oxide operation or short cm head:for nitrous oxide operation or short path length airpath length air-acetyleneacetylene 3 3-slot:high dissolved solids for airslot:high dissolved solids for air-acetylene acetylene operationoperationTemperature Distribution in a Temperature Distribution in a MassmanMassman-style style AtomizerAtomizerFork PlatformFork PlatformIntegrated PlatformIntegrated PlatformMassmanMassman-style Furnacestyle FurnaceTemperature Distribution in a TransverselyTemperature Distribution in a Transversely-Heated AtomizerHeated AtomizerTHGA TubesTHGA TubesOpen End and End CapOpen End and End CapTHGATHGAStandard and End Cap TubesStandard and End Cap Tubes00.10.20.30.40.500.10.20.30.40.5Integrated AbsorbaceAgCoCrPbPb*SeSe*VAgCoCrPbPb*SeSe*VStandardStandardEnd-capEnd-cap*with Matrix ModifierSingleSingle-beam Configurationbeam ConfigurationMonochromatorHollowCathode LampDetectorRotatingChopperSampleBeamDouble-beam ConfigurationMonochromatorDetectorReference BeamSampleBeamHollowCathode LampRotatingChopperTraditional GratingEchelle GratingIncident Light(all wavelengths)Echelle GratingAngle of Incidence()m=0(simple reflection)(all wavelengths)m=1=250nmm=2=250nmm=1=600nmm=50=600nmm=121=250nmm=119=250nmPerpendicular to face of gratingAngle of Diffraction()m=diffraction order number=wavelengthFunction of the Monochromator?Disperse polychromatic light into its various wavelengths?Allows for the isolation of specific wavelengthsPMTPMTAAnalystAAnalyst 700 and 700 and AAnalystAAnalyst 800 800 Customized SolidCustomized Solid-State DetectorState DetectorHighest quantum efficiencyIntegrated low noise CMOS charge amplifier arrayExceptional signal-to-noise ratio 原子吸收光谱分析时的干扰极其消除原子吸收光谱分析时的干扰极其消除原子吸收光谱分析时的干扰极其消除原子吸收光谱分析时的干扰极其消除1.1.物理干扰物理干扰物理干扰物理干扰*样品溶液与标准溶液物理性质不一样引起测量结果误差样品溶液与标准溶液物理性质不一样引起测量结果误差样品溶液与标准溶液物理性质不一样引起测量结果误差样品溶液与标准溶液物理性质不一样引起测量结果误差*电离干扰电离干扰电离干扰电离干扰*光谱干扰光谱干扰光谱干扰光谱干扰发射线干扰发射线干扰发射线干扰发射线干扰吸收线干扰吸收线干扰吸收线干扰吸收线干扰2.2.化学干扰化学干扰化学干扰化学干扰3.3.背景干扰背景干扰背景干扰背景干扰Matrix InterferenceMatrix Interference1%HNO35%H2SO4MIBKUptake RateNebulizerDroplet SizeViscosity and surface tension effectUptake rateDroplet sizeSensitivity.碱金属元素在空气碱金属元素在空气碱金属元素在空气碱金属元素在空气-乙炔火焰中的电离乙炔火焰中的电离乙炔火焰中的电离乙炔火焰中的电离元元元元素素素素电离比电离比电离比电离比(%)(%)1010-3 3MM溶液溶液溶液溶液Li 10Li 10Na 20Na 20K 60K 60Rb Rb 7575Cs 95Cs 95不同元素在不同火焰中的电离状况不同元素在不同火焰中的电离状况不同元素在不同火焰中的电离状况不同元素在不同火焰中的电离状况元元元元 素素素素电离能电离能电离能电离能(eVeV)溶液浓度溶液浓度溶液浓度溶液浓度(mg/l)mg/l)电离比电离比电离比电离比(%)(%)AirAir-C2H2 N2OC2H2 N2O-C2H2C2H2Be 9.3 2 Be 9.3 2 -0 0Mg 7.6 2 Mg 7.6 2 0 60 6Ca 6.1 5 Ca 6.1 5 3 433 43Sr Sr 5.7 5.5 13 5.7 5.5 13 8484Ba Ba 5.2 30 0 5.2 30 0 8888Yb Yb 6.2 15 6.2 15 -2020Al 6.0 100 Al 6.0 100 -1010原子处于激发态与基态的比例原子处于激发态与基态的比例原子处于激发态与基态的比例原子处于激发态与基态的比例元元元元素素素素波波波波长长长长NqNq/N0/N0(nm)2000K 3(nm)2000K 3000K000KNa 589.0 0.99Na 589.0 0.9910(10(5)5.835)5.8310(10(4)4)Mg 285.2 3.35Mg 285.2 3.3510(10(11)1.5011)1.5010(10(7)7)Ba Ba 553.6 6.83553.6 6.8310(10(6)5.196)5.1910(10(4)4)V 437.9 6.87V 437.9 6.8710(10(9)2.739)2.7310(10(6)6)Fe 248.3 2.29Fe 248.3 2.2910(10(9)1.319)1.3110(10(6)6)Cu 324.7 4.82Cu 324.7 4.8210(10(10)6.6510)6.6510(10(7)7)Pb Pb 283.3 2.83283.3 2.8310(10(11)1.3411)1.3410(10(7)7)AAnalystAAnalyst 700 and 700 and AAnalystAAnalyst 800800Optimization of Burner Position for Best AccuracyOptimization of Burner Position for Best Accuracy0501001502002503000510152025Height(mm)Absorbance A 50 mg/L Al50 mg/L ALin 0.1%SiInterference as a function of burner height:Al in silicon solutionN2O-C2H2-flameNegativeinterference at position of max.sensitivityAAnalystAAnalyst 700 and 700 and AAnalystAAnalyst 800800Optimization of Burner Position for Best AccuracyOptimization of Burner Position for Best Accuracy0501001502002500510152025height(mm)Absorbance mA3 ppm Ca and3 ppm Ca in1%PO4:Absorbance as function of theburner height:negative interferenceat position of maximum sensitivity3 mg/L Ca3 mg/L Ca in 1%PO4air-acetylene flame,no buffer文献中报道的可能产生文献中报道的可能产生文献中报道的可能产生文献中报道的可能产生结构背景的谱线干扰结构背景的谱线干扰结构背景的谱线干扰结构背景的谱线干扰(1)(1)pp分析元素分析元素分析元素分析元素发射谱线发射谱线发射谱线发射谱线干扰元素干扰元素干扰元素干扰元素吸收谱线吸收谱线吸收谱线吸收谱线ppFe 324.728 Cu 324.754Fe 324.728 Cu 324.754ppFe 327.445 Cu 327.396Fe 327.445 Cu 327.396ppFe 285.213 Mg 285.213Fe 285.213 Mg 285.213ppFe 352.424 Ni 362.454Fe 352.424 Ni 362.454ppFe 279.470 Fe 279.470 Mn Mn 279.482279.482ppCu 324.754 Cu 324.754 Eu Eu 324.753324.753ppFe 271.903 Pt 271.904Fe 271.903 Pt 271.904文献中报道的可能产生文献中报道的可能产生文献中报道的可能产生文献中报道的可能产生结构背景的谱线干扰结构背景的谱线干扰结构背景的谱线干扰结构背景的谱线干扰(2)(2)ppSi Si 250.690 V 250.690250.690 V 250.690ppAl 308.215 V 308.211Al 308.215 V 308.211ppGa Ga 403.298 403.298 Mn Mn 403.307403.307ppMn Mn 403.307 403.307 Ga Ga 403.298403.298ppHg 253.652 Co 253.649Hg 253.652 Co 253.649ppGe Ge 422.657 Ca 422.673422.657 Ca 422.673ppNe Ne 359.352 Cr 359.349359.352 Cr 359.349ppSb Sb 217.023 217.023 Pb Pb 216.999216.999文献中报道的可能产生文献中报道的可能产生文献中报道的可能产生文献中报道的可能产生结构背景的谱线干扰结构背景的谱线干扰结构背景的谱线干扰结构背景的谱线干扰(3)(3)ppI 206.163 Bi 206.170I 206.163 Bi 206.170ppAs 228.812 As 228.812 Cd Cd 228.802228.802ppZn 213.856 Fe 213.859Zn 213.856 Fe 213.859ppFe 287.417 Fe 287.417 Ga Ga 287.424287.424ppFe 460.765 Fe 460.765 Sr Sr 460.733460.733ppFe 338.241 Ag 338.289Fe 338.241 Ag 338.289ppFe 396.114 Al 396.153Fe 396.114 Al 396.153ppHg 359.348 Cr 359.349 Hg 359.348 Cr 359.349 文献中报道的可能产生文献中报道的可能产生文献中报道的可能产生文献中报道的可能产生结构背景的谱线干扰结构背景的谱线干扰结构背景的谱线干扰结构背景的谱线干扰(4)(4)ppHg 285.242 Mg 285.213Hg 285.242 Mg 285.213ppPb Pb 241.173 Co 241.162241.173 Co 241.162ppPb Pb 247.638 Pd 247.643247.638 Pd 247.643ppSb Sb 216.919 Cu 217.894216.919 Cu 217.894ppSb Sb 323.252 Li 323.261323.252 Li 323.261ppSb Sb 231.147 Ni 231.095231.147 Ni 231.095pp摘自摘自摘自摘自“Analytical Atomic Absorption Analytical Atomic Absorption SpectroscopeSpectroscope”,Jon C.Van Loon ,Jon C.Van Loon The STPF ConceptThe STPF Concept PyrolyticallyPyrolytically coated graphite tubescoated graphite tubes L L vovvov platformplatform Rapid furnace heatingRapid furnace heating Internal gas stopInternal gas stop Matrix modifiersMatrix modifiers Fast signal processingFast signal processing Peak areaPeak area ZeemanZeeman Background correctionBackground correction石墨炉测定石墨炉测定石墨炉测定石墨炉测定可能产生的分子光谱可能产生的分子光谱可能产生的分子光谱可能产生的分子光谱(1)(1)pp化合物化合物化合物化合物 最长波长最长波长最长波长最长波长(nm)nm)峰值波长峰值波长峰值波长峰值波长(nm)nm)ppLiCl LiCl 253 200,228253 200,228ppNaCl NaCl 287 200,236 287 200,236 ppKCl KCl 280 200,246280 200,246ppRbCl RbCl 277 200,249277 200,249ppCsCl CsCl 270 200,248 270 200,248 Correcting for Matrix InterferencesCorrecting for Matrix InterferencesppMatrix match all samples,standards,and blanksMatrix match all samples,standards,and blanksppAnalyze using Method of Standard Additions(MSA)Analyze using Method of Standard Additions(MSA)MSA:An ExampleMSA:An Example00.150.3-0.82012ConcentrationAbs00.150.3-0.82012ConcentrationAbsMethod of Standard AdditionsMethod of Standard Additions(MSA)(MSA)ppAccurate analyses are performed without Accurate analyses are performed without eliminating interferenceseliminating interferencesppThe instrument is calibrated in the presence of The instrument is calibrated in the presence of the matrix interferencethe matrix interferenceppA known amount of A known amount of analyteanalyte is added to the is added to the sample matrixsample matrixppIt is assumed the interfering material will affect It is assumed the interfering material will affect the samples and standards equallythe samples and standards equallyppAll samples must be in the linear rangeAll samples must be in the linear range石墨炉测定石墨炉测定石墨炉测定石墨炉测定可能产生的分子光谱可能产生的分子光谱可能产生的分子光谱可能产生的分子光谱(2)(2)pp化合物化合物化合物化合物最长波长最长波长最长波长最长波长(nm)nm)峰值波长峰值波长峰值波长峰值波长(nm)nm)ppLiF LiF 215 200215 200ppNaF NaF 245 215245 215ppKF 240 215KF 240 215ppRbF RbF 240 216240 216ppCsF CsF 225 211 225 211 Background AbsorptionBackground AbsorptionBackgroundAAAABGBackground Correction TechniquesBackground Correction Techniques Continuum sourceContinuum source SmithSmith-HieftjeHieftje ZeemanZeemanTypes ofTypes of ZeemanZeeman SystemsSystems DCDC ZeemanZeeman:permanent magnet oriented:permanent magnet orientedtransversetransverse to the optical pathto the optical path ACAC ZeemanZeeman:electromagnet oriented:electromagnet oriented transversetransverse to to the optical paththe optical path ACAC ZeemanZeeman:electromagnet oriented:electromagnet oriented longitudinallongitudinalto the optical pathto the optical path机体改进剂对石墨炉测定的影响机体改进剂对石墨炉测定的影响机体改进剂对石墨炉测定的影响机体改进剂对石墨炉测定的影响pp提高分析物能够承受的前处理温度提高分析物能够承受的前处理温度提高分析物能够承受的前处理温度提高分析物能够承受的前处理温度pp降低样品基体挥发或分解温度降低样品基体挥发或分解温度降低样品基体挥发或分解温度降低样品基体挥发或分解温度pp有利于分析元素原子化机理单一化有利于分析元素原子化机理单一化有利于分析元素原子化机理单一化有利于分析元素原子化机理单一化pp延长石墨管使用寿命延长石墨管使用寿命延长石墨管使用寿命延长石墨管使用寿命pp背景增加背景增加背景增加背景增加pp空白吸收增加空白吸收增加空白吸收增加空白吸收增加Reducing the Volatility of theReducing the Volatility of the AnalyteAnalyte00.050.10.150.24006008001000120014001600Pyrolysis TemperatureAbs-secSe+Pd/Mg(NO3)2Se with no modifier 目 录 1.火焰部分 1.1 开机 1.2 建立方法 1.3 装灯与点灯 1.4 点火 1.5 优化仪器条件 1.6 样品测定 1.7 熄火与关机 2.石墨炉部分 2.1 开机 2.2 建立方法 2.3 更换石墨管及石墨管的老化处理 2.4 调节自动进样器位置 2.5 样品测定 2.6 关机 3.数据处理 3.1 出报告 3.2 文件删除 2 1.火焰部分 1.1开机 确认仪器主机和计算机已经接入到合适的电源,按照下列步骤开机:1.1.1 开空气压缩机(将空气压缩机电源插头插入 220 伏电源插座上);1.1.2 打开氩气钢瓶阀门,使其次级压力在 350kpa;1.1.3 开计算机显示屏和计算机主机开关,使其进入到 WINDOWS 2000 或