电感耦合等离子体质谱仪教程-ICP-MS(日立公司仪器).ppt

書式設定,書式設定,第 2,第 3,第 4,第 5,Model P-5000 ICP-MS,Hitachi Ltd.Instruments,此文本为一会议报告，不属仪器分析课程要求的内容。有兴趣的同学可以看一看。,ICP/AES,Atomic Absorption,Furnace,Plasma/MS (ICP/MS,MIP/MS),ppt,ppb,ppm,Through-put(Elements/min),0.01 0.1 1 10 100,Single Element,Multi Element,Analysis Analysis,Atomic Absorption,Flame,P-5000,P-4010,Z-5010 series,P-6000,Atomic Absorption,Furnace&Flame,ICP-AES,ICP-MS,MIP-MS,Line Up for Elemental Analysis,Sensitivity,Ion trap type ICP-MS,Hi-Power MIP-MS,ICP-MS,电感耦合等离子体质谱仪,Inductively Coupled Plasma Mass Spectrometry,等离子体-离子源,质谱-按原子(分子)质量顺序排列 的图谱,质谱仪-质量分析仪,对带电粒子起作用,M/e,与离子强度,其他联用技术,GC-MS HPLC-MS,特点:,无机质谱,分析速度快,线性范围宽,可多元素测定 80多种元素,检出限低,PPT,Characteristics P-5000,的优势,Combination of an inductively coupled plasma ion source and an ion trap for elemental analysis.,1.Reduction of matrix ions derived from argon by using tandem mass spectrometry(MS,2,),2.Space charge effects suppressed by using filtered noise field(FNF),3.Ion concentration through trapping(a detection limit is,ppt,level for most elements),要点:,1.,ICP,和三维四极离子阱的结合是目前为止最佳的,ICP-MS,原因:,MS2,解决了分子离子的干扰,FNF,解决了空间电荷效应抑制问题,离子阱的储存离子功能提高灵明度,Introduction,P-5000 ICP-MS is the first ion trap type ICP-MS,in the world.,It offers:,1.Low Background signal,2.High sensitivity,3.Wide dynamic range,4.Easy operation,Structure of P-5000 ICP-MS,Detector,Ion trap,Ion guide,Sampling,cone,Skimmer,cone,Torch,Chamber,Nebulizer,Rotary pumps,Turbo molecular pumps,Peristaltic pump,Comparison of ion trap and conventional QMS,#Tandem mass spectrometry,#Relatively compact instrument,#,High transmission efficiency in the,selected ion monitoring(SIM)mode,QMS:transmitting type,Ion trap:trapping type,What is Ion trap?,提示:,离子阱全能,与,ICP,结合最佳,四极杆适合选择离子检测,与,GC,LC,配合更好,Ion trap basic action,(Entrance gate),(Exit gate),Ions,Detector,Ions trapping,Ion detection,Time,Multi function,analysis,What is Ion trap?,open,closeclose,closeclose,open,Entrance gate,Exit gate,1.,Low background signal,In a P-5000 system,collision-induced dissociation is used to eliminate the interference from,molecular ions,.,碰撞诱导分裂,2.,Hi-sensitivity and wide dynamic range,By changing the ion trapping time,it is possible to change the ion sensitivity.,阱的时间,3.,Easy measurement,Simultaneous analysis,qualitative,quantitative analysis.,4.,Ar-ICP ion source,RF:27 MHz,Maximum Power:1.4 kW,Main Features of P-5000 ICP-MS,Main problem of conventional ICP-QMS,Molecular ion,It is impossible to distinguish the ions with the same m/z.,Measurement ion,Same m/z,Se,+,ArAr,+,Se,+,ArAr,+,Impossible to distinguish,Main Features of P-5000 ICP-MS,:,Measurement Ion,:,Moleculars,:after dissociation,In the P-5000 system,next 2 stage,1.,Natural,decluster,自然去簇,2.,Collision-induced dissociation(CID),碰撞诱导分裂,is used to eliminate the interference from,molecular ions,.,Main Features of P-5000 ICP-MS,Elimination method for the molecular ions.,Main Features of P-5000 ICP-MS,Ion tap,Cool plasma,+QMS,Reaction cell,+QMS,Ar-molecular,ions,Sensitivity of other ions,Elimination,Metal-oxide ions,Possible,Possible,Possible,Possible,Impossible,Impossible,Good,bad,bad,Reaction gas,He,-,NH,3,H,2,Different of background spectrum,Main Features of P-5000 ICP-MS,ICP-QMS,P-5000,Ion trap ICP-MS,By changing the ion trapping time,possible to change the ion sensitivity.,Intensity,Ion trapping time,1 10 100 1000 10000,10000,1000,100,10,1,msec,Wide dynamic range,Main Features of P-5000 ICP-MS,Calibration Curve,1.000,0,50,100,Concentration(ppt),208,Pb,400,500,600,700,Intensity,11,B,R,2,=1.000,27,Al,R,2,=1.000,55,Mn,R,2,=1.000,56,Fe,R,2,=1.000,63,Cu,R,2,=1.000,66,Zn,R,2,=1.000,15000,0 50 100,Conc.(,ug,/L),35000,0 50 100,Conc.(,ug,/L),0,70000,0,0 25 50,Conc.(,ug,/L),70000,4000,0 150 300,Conc.(,ug,/L),0,80000,0 50 100,Conc.(,ug,/L),0,60000,0 50 100,Conc.(,ug,/L),0,52,Cr,R,2,=1.000,60,Ni,R,2,=1.000,75,As,R,2,=0.998,0 25 50,Conc.(,ug,/L),30000,2000,0 5 10,Conc.(,ug,/L),0,60000,0 5 10,Conc.(,ug,/L),50000,0,Analysis of tap water,80,Se,R,2,=0.998,98,Mo,R,2,=1.000,112,Cd,R,2,=1.000,121,Sb,R,2,=0.999,208,Pb,R,2,=1.000,238,U,R,2,=0.999,0 5 10,Conc.(,ug,/L),40000,0,0 40 80,Conc.(,ug,/L),25000,0 5 10,Conc.(,ug,/L),0,0 1.0 2.0,Conc.(,ug,/L),60000,5000,50000,0 25 50,Conc.(,ug,/L),50000,0,0 1.0 2.0,Conc.(,ug,/L),60000,0,0,Analysis of tap water,Background Spectrum,-Efficiency of ion trap ICP-MS(1)-,Pure water,2%HNO,3,2%,HCl,Background equivalent concentration,of,ArO,is 5 ppb(Fe).,Analysis of Fe at m/z=56,-Efficiency of ion trap ICP-MS(2)-,Calibration curve of,56,Fe,Calibration curve of g/L range can be obtained for Fe at m/z=56 under the hot plasma condition.,Intensity,Fe conc.(g/L),0,20,40,60,80,100,R,2,=0.999,Intensity,Fe conc.(g/L),0,3000,6000,0,5,10,Measurement for Fe in the standard sample of river water(NIST SRM1643d),measured,88.2,element,Fe,Quantity of Fe in,Nist,1643d,56,Fe,56,Fe(,Nist,1643d),(g/L),certified,87.3-95.1,Measurement for As in the standard sample of river water(NIST SRM1643d),measured,56.5,element,Fe,(g/L),certified,55.29-56.75,75,0.3%,NaCl,75,As(10,ug/L,)0.3%NaCl,I,ntensity,m/z,Mass Spectrum of As,Analysis of As,-Efficiency of ion trap ICP-MS(3)-,Quantity of As in,Nist,1643d,R,2,=0.999,Intensity,0,10,20,30,40,50,60,70,80,90,100,As conc.(,ug,/L),75,As(,Nist,1643d),0,200,400,600,800,1000,0,20000,40000,60000,80000,100000,120000,140000,160000,180000,80,Se,0,10,20,30,40,50,R,2,=0.999,80,Se Conc.(g/L),Intensity,Intensity,80,Se Conc.(,ng,/L),R,2,=0.999,Analysis of Se at m/z=80,-Efficiency of ion trap ICP-MS(4)-,Calibration curve of,ng,/L range can be obtained for Se at m/z=80 under the hot plasma condition.,Measurement for Se in the standard sample of river water(NIST SRM1643d),measured,11.6,element,Fe,Quantity of Se in,Nist,1643d,(g/L),certified,11.26-11.60,Calibration curve of,80,Se,80,Se(,Nist,1643d),Measurement of,80,Se(,ng,/L)by using CID,-Efficiency of ion trap ICP-MS(5)-,0,20,40,60,80,100,0,10000,20000,30000,40000,50000,Highly background,Concentration(,ng,/l),Count(,arb,.unit),0,20,40,60,80,100,0,1000,2000,3000,4000,5000,Count(,arb,.unit),R,2,=0.998,Concentration(,ng,/l),CID off,CID on,Eliminate,80,Se,80,Se,#,Interference of metal-oxide ion(,eg,.,CaO,)can be decreased.,#,56,Fe can be measured including the high matrix of Ca.,CID on,30,ppm,Ca,+,1 ppb Fe,CID on,30ppm Ca,CID off,30,ppm,Ca,m/z,55.5,56.0,56.5,0,Decreasing by CID,Cool plasma or collision cell can not decrease the interference of,CaO,Measurement of,56,Fe in Ca by using CID,-Efficiency of ion trap ICP-MS(6)-,Intensity(,arb,.unit),Simultaneous Measurement for the Sample,with Variety Concentration,-Efficiency of ion trap ICP-MS(7)-,The sample including the elements with over mg/L concentration and under g/L concentration can be measured simultaneously by changing the ion trapping time.,0,20,40,60,80,100,0,10000,23,Na,r,2,=0.9993,Intensity,Conc.(mg/L),0.0,0.5,1.0,1.5,2.0,0,12000,238,U,2,r,=0.9993,Intensity,Conc.(g/L),Calibration curve of g/L range of U,Calibration curve of mg/L range of U,Specifications,ICP ion source,Radio frequency:27.12 MHz,Power:0.7-1.4 kW,Fully computer controlled solid state RF generator,Stage:X-Y-Z automatic adjustable,Sample introduction,Torch:,Fassel,Type,Chamber:Scott Type(Option:cooled),Nebulizer,:Concentric,nebulizer,Peristaltic pump,Vacuum System,3 stage vacuum,Interface vacuum:Rotary pump,Ion lens chamber:Turbo pump,Analyzer chamber:Turbo pump,Analyzer,Ion trap type:Compact type,MS-MS function:,tandem mass spectrometry(MS,2,),Specifications,Ion detection,Electron multiplier,Mass range,5-300,amu,Detection limit:,ppt,level for most elements,Linear dynamic range:8 orders,Size and weight,Height:810 mm,Width:1180 mm,Depth:710 mm,Weight:300 kg,几种附件:,自动进样器,超声波雾化器,氢化物发生器,氢氟酸进样系统,应用(,I),*,生物和医学,金属蛋白络合物,人血清中的难溶元素,血浆中的,Mo,植物中的,Pt,尿样中的无机,Se,和有机,Se,应用(,II),*,环境与食品,气溶胶 大气中的微粒物质,海水中的微量金属,极地冰雪中的铁,环境荷尔蒙,Pb Cd,Hg,酒中生物配合物中的,Pb,应用(,III),*,地质 钢铁 稀土材料,贵金属 高纯物质分析,陶瓷 长石 锆石,矿石中的液体包容物,同位素比,销售目标:,*科研 主要市场,环境!,*检测 贵金属 地矿,稀土材料,经典市场!,说法:强调,MS,部分,1.,ICP,与离子阱是最好的联用方式,离子阱,MS,2,和储存离子提高灵敏度,2.分子离子干扰处理的很好,空间电荷效应抑制得到解决,这是其他常规,ICP-MS,做不到,3.碰撞诱导分裂-独特!,MS,2,的功能,4.目前只有日立有,ICP,与离子阱联用仪器,5.液相色谱附件,6.体积小巧,