感应藕合电浆放射光谱仪训练课程.ppt

Click to edit Master title style,Click to edit Master text styles,Second level,Third level,Fourth level,Fifth level,Page,page#0,感應藕合電漿放射光譜儀,訓練課程,博精儀器股份有限公司,技術專員付國偉,13962658312,課程內容,無機分析儀器,之介紹說明及比較,(AA,ICP-OES and ICPMS),ICP-OES,基本原理,A:sample introduction,樣品進樣系統,B:Plasma system,等離子基本原理,C:Optical system,光學系統基礎概念,問題與討論,Page,1,無機分析儀器,之介紹說明及比較,(AA,ICP-OES and ICPMS),Page,2,ICP-OES and Furnace&Flame AA,Flames AA-,火燄式原子吸收光譜儀,Furance,AA-,石墨式原子吸收光譜儀,感應藕合電漿放射光譜儀,感應藕合電漿質譜儀,Page,3,Bohr,原子模型,+,e-,M,o,基態,光譜儀基本原理,Page,4,M,o,M,*,+E,-E,M,o,原子放射過程,回到基態,+E,+,e-,e-,Light,光譜儀基本原理,Page,5,Principle of Atomic Spectroscopy,H,He,Li,M,Energy,Emission(,e,),Absorption(,a,),Ionization,Absorption(,a,),Emission(,e,),Ground state,Excitation level,Ionization,V:,Ionizsation,potential,En,Em,:Excitation potential,E=En-,Em,=h,En,Em,V,Be,Page,6,能級圖,激发,发射,能量,离子,激发,态,离子基态,a,b,c,d,a,b,激发,c,电离,d,离子,激发,e,f,g,h,e,离子,发射,f,g,h,元子,发射,激发,态,l,4,l,3,l,2,l,1,D,E=,h,n,=,hc/,l,Page,7,多种能量传输,发射光取决于能级间能量差,返回基态,发出光,+,激发,态,D,E=,h,n,=,hc/,l,h=Plancks,常数,n,=,频率,c=,光速,l,=,波长,原子光谱的产生,Page,8,原子发射光谱的定性原理,量子力学基本理论,:,1,）原子或离子可处于不连续的能量状态，该状态可以光谱项来描述；,2,）当处于基态的气态原子或离子吸收了一定的外界能量时，其核外电子就从一种能量状态（基态）跃迁到另一能量状态（激发态）；,3,）处于激发态的原子或离子很不稳定，经约,10-8,秒便跃迁返回到基态，并将激发所吸收的能量以一定的电磁波辐射出来；,4,）将这些电磁波按一定波长顺序排列即为原子光谱（线状光谱）；,5,）由于原子或离子的能级很多并且不同元素的结构是不同的，因此，对特定元素的原子或离子可产生一系列不同波长的特征光谱，通过识别待测元素的特征谱线存在与否进行定性分析。,Page,9,感應藕合電漿放射光譜儀與,AA,之比較,Flame,AA,Graphite AA,ICP/OES,ICP/MS,Page,10,BeerS Law in AA and ICP,Page,11,Quantitation,in Atomic Emission,Concentration,Light Intensity,I,：,光谱强度,K,：常数,N,：原子浓度,X,：接近,1,的指数,I=KN,X,Page,12,Comparison of analytical range,Flame AA,GFAA,ICP-OES,ICP-MS,1,1000,0.001,10%,0.000001,Concentration Linear Dynamic Range(mg/L),Axial View,Flame AA+GFAA,Page,13,Analysis speed and DL,偵測極限,V.S.,分析速度,Page,14,Detection limit-3,in g/l using flow spoiler.Impact bead improves up to 4x,Flame Elements&Detection Limits,Page,15,H,Li,0.04,Na,0.7,K,2,Rb,3,Cs,5,Fr,Be,0.05,Mg,0.03,Ca,0.06,Sr,0.03,Ba,0.04,Ra,Sc,0.06,Ti,0.2,V,0.3,Cr,0.2,Mn,0.08,Fe,0.1,Co,0.2,Ni,0.4,Cu,0.5,Zn,0.1,Al,1.5,Si,4.0,P,3,S,6,Cl,Ar,Ga,3.0,Ge,0.9,As,2,Se,3.0,Br,40000,Kr,B,1,C,N,O,F,Ne,In,1.0,Sn,1.0,Sb,2.0,Te,2.0,I,2.0,Xe,Tl,2.0,Pb,2.0,Bi,2,Po,At,Rn,Y,0.2,Zr,0.4,Nb,0.6,Mo,0.6,Tc,Ru,2,Rh,4,Pd,2.0,Ag,0.1,Cd,0.07,La,0.7,Hf,0.5,Ta,1.0,W,1.0,Re,0.2,Os,120,Ir,1.0,Pt,1.0,Au,0.8,Hg,2,Ac,Rf,Ha,Dy,0.5,Ho,60,Er,0.5,Tm,0.4,Yb,0.06,Lu,0.02,Ce,1.0,Pr,1.0,Nd,1.0,Pm,Sm,1.0,Eu,0.1,Gd,0.9,Tb,1.0,Cf,Es,Fm,Md,No,Lr,Th,2,Pa,U,8.0,Np,Pu,Am,Cm,Bk,He,Anthanides,Ctinides,EL,DL,I.D.L 0.1-1.0 ppb,Detection limit-3,in g/l using in ppb use Axial,GemCon,Cyclonic,ICP-OES Elements&Detection Limits,EL,DL,I.D.L 0.1 ppb,EL,DL,I,.D.L 1-10 ppb,Page,16,Atomic Spectroscopy comparison,Table,Page,17,ICP-OES,基本原理讲解,Section#,1,Page,18,吸收譜線與放射原子譜線,Page,19,Page,20,NON-Metals Applications,So why are there not more applications?,Page,21,电感耦合等离子体发射光谱仪系统,Page,22,Sample Introduction,System,Page,23,Section#2,样品,進樣系統,A.ICP,構造部分一,:,進樣系統,把溶液轉變成氣溶膠，通入到電漿中,樣品進樣條件通過電腦控制,Page,25,Peristaltic Pump,Type of Tubing for analysis,Pump rate,dependon,Different introduction system,Page,26,Sample Introduction Device,To ICP,Nebulizer,Sample,solution,Ar,carrier gas,To generate sample droplets by,nebulization,and,to introduce only fine droplets in the plasma.,Page,27,Pneumatic Nebulizers,Sample,Ar,nebulizer gas,Concentric nebulizerSample,Ar,nebulizer gas,Cross flow nebulizer,Page,28,Concentric nebulizer,Page,29,Cross flow nebulizer,Page,30,Nebulizers,Cross-Flow,交叉式,霧化器,Concentric,同心圓式霧化器,Page,31,Spray Chamber,Page,32,Cyclonic spray chamber,Nebulizer generates small droplets.,Spray chamber eliminates larger droplets and introduces only fine droplets into ICP.,Nebulizer,To drain,To ICP,Page,33,Page,34,Page,35,Section#,3,(,激发光源）,Plasma gas,Nebulizer gas,+sample droplets,Auxiliary gas,RF coil,Magnetic field,Eddy current,Plasma,B.ICP,構造部分二,:,電漿形成,點火過程,Page,37,ICP,Plasma,Statue,Plasma gas,Nebulizer gas,+sample droplets,Auxiliary gas,RF coil,Magnetic field,Eddy current,Plasma,Page,38,辅助气,冷却气,等离子体,RF,线圈,雾化气,+,样品气溶胶,环型电流,Page,39,Temperature distribution in Plasma,Page,40,Solid-state RF Generator,更高的信賴度及穩定度,點火測試操過,99,000,次,&still going,無使用壽命之限制,不需倍增管產生器,能量之穩定遠勝於倍增管產生器,不必作電頻校正,可提供更高的電頻效能,81%vs.50%for PA tube generator,節省空間,Section#,4,光学系统,Optical system,Page,43,感應耦合電漿放射光譜儀依光學系統及單光器之設計可分為傳統掃描式,(Sequential),及同步式,(Simultaneous),光學設計其差異性討論如下,;,a:,掃描式為利用單一光柵之轉動，將預分析之元素或波長依序少掃描到,PMT,倍增管中,為傳統之光學設計,(,如下圖,),。優點為可作背景掃描及價格便宜；無需熱機時間但需作每一波長之,PMT,電壓較正十分費時；期缺點為分析述速度十分緩慢，一般十個元素約需五到十分鐘之分析時間。目前漸漸為同步式,ICP,所起代,因目前同步式,ICP,皆已可作背景掃描。,b:,同步加掃描式,ICP,其原理為利用一,Echelle,光柵再加上一垂直擺置之菱鏡將光譜形成二度平面圖譜,而後於圖譜之特定波長上擺上極小之,CCD,或,SCD,素像來感光如同數位形型相機，依個別波長光之強度轉換成電流同時來判別其濃度高低如下圖,並可作背景之快速掃描,其速度為每分鐘可分析,75,個元素，不論元素之多寡。其優點為速度快，省成本,(,速度快氬氣用量較節省,),，感度較掃描式佳，偵測極限低，解析度較好,(,因二次分光,),及較優軟體功能較優。,Page,44,Polychrometer,system,(,同 步 式,),Fixed,grating,Ar,plasma,Slit,DetectorExit slit,Monochrometer,system,(,連 續 式,),S,lit,Detector,Slit,Grating driven by,motor,Echelle,type,(,Axial view),Slit,Echelle,Interface,CCD,Sample,aerosol,Sample,aerosol,光譜,Page,45,Refraction Through Prism,Incident Light,(all wavelengths),l,=782nm,l,=388nm,Wavelengths from 388nm to 782nm hit detector,Wavelengths shorter than 388nm or longer than 782nm do not hit detector,Prism,Page,46,Sequential Designs ICP-OES,Sequential AES,Design,AES.swf,Page,47,Simulates Optical system,Simulates,Optical-,AES.swf,Page,48,Total ICP Market Segmentation,Page,49,Thank you for your attention!,Page,50,