3.备考总结仪器分析复习

1、光谱、电化学复习要1. 【极性增加e红移，npie蓝移光谱、电化学复习要1. 【极性增加e红移，npie蓝移Lambert-Beer 定律，吸收系数（物理意义、表达形式部；8. 定量分析方法（工作曲线、标准加入、内标法 8. 定量分析方法（工作曲线、标准加入、内标法 0810CGC，HPLC比较 异 同 点TLC，经典液相，GC，HPLC（图示7.TCD8.三.计算 30123给出了三次测量值（如实验20DNA2009 简答：用流程图说明用玻璃膜电极和饱和甘 电机两次法测2009 简答：用流程图说明用玻璃膜电极和饱和甘 电机两次法测.举例说明如何用塔板理论评价柱效；速率理论对，HPLC的启示

2、.TLC、Classical，HPLC 过程框图和主要区别TCDDAy的故事2010 08级仪分期末考题计算题还是Lambert-beer定律和吸光系数的转换光学的计算不可能出其他的了吧电学（10分的填空题色谱计算题还是Lambert-beer定律和吸光系数的转换光学的计算不可能出其他的了吧电学（10分的填空题色谱5道选择 （1）（2）（3）（4）血液翻译，TswettDay2012 By10 计算题还是Lambert-beer4今年没考Davd光谱法莫斯鲍尔（射线）光谱法(Mossbaur) Dualerferometry 计算题还是Lambert-beer4今年没考Davd光谱法莫斯鲍尔（

3、射线）光谱法(Mossbaur) Dualerferometry 电化学： Coulometrytitrationmethod:库仑滴定法 Voltammetry method：伏安法erometrictitrationmethod:四种色谱法：absorptionchromatograph：吸附色谱法 Partition chromatography: 分配色谱法 Molecular翻色层分析（chroaorahyc）的发明对于二十世纪的化学，生物化学与医学上的贡献几乎 利用于叶绿素的分离研究。然而经过二十多年几乎被遗忘，于1931年再由三位德语系的化， ，洛桑与日内瓦接受教育，1891 内

4、瓦大学理学院念植物学，1896 年得博士学位。在他的博1896 洛桑与日内瓦接受教育，1891 内瓦大学理学院念植物学，1896 年得博士学位。在他的博1896 并做一些叶绿体化学上的研究，1901 1907 1918至 47，当时的叶绿素化学知识对于植物光合作用的了解一无帮助 28（21 1903注意并正确的解释色层分离过程;的德国化学，希望从当时最著名的有机化学家之一的维尔仕塔特（R.Willsttter）。We have noted the development of liquid chromatography prior to the advent of HPLC (Section

5、1.1). For a more complete account of this pre-1965 period, several review articles have writtenbyEttre,ourhistorianofprecursorstochromatography;developmentspriorto190010,invention of chromatography by M. S. Tswett in the early 1900s 12 rediscovery heearly1930sA.J.P.Martinsinventionofpartitionandrhee

6、arly1940s developmentoftheamino-yzerbyS.MooreandW.S.helate1950sdevelopment of the gel-permeationchromatographbyWaters he early 1960s CarlRunge, aGerman dye-chemist born in reportedcrude dye separations by means的德国化学，希望从当时最著名的有机化学家之一的维尔仕塔特（R.Willsttter）。We have noted the development of liquid chromat

7、ography prior to the advent of HPLC (Section 1.1). For a more complete account of this pre-1965 period, several review articles have writtenbyEttre,ourhistorianofprecursorstochromatography;developmentspriorto190010,invention of chromatography by M. S. Tswett in the early 1900s 12 rediscovery heearly

8、1930sA.J.P.Martinsinventionofpartitionandrheearly1940s developmentoftheamino-yzerbyS.MooreandW.S.helate1950sdevelopment of the gel-permeationchromatographbyWaters he early 1960s CarlRunge, aGerman dye-chemist born in reportedcrude dye separations by meansa technique similar to r chromatography 10, b

9、ut neither he nor others pursued the sibilitiesofthishelate 1890sDavidDayattheUS Geologicalsurveycarriedoutseparationsofpetroleumbyt resembles classical column chromatography 11; however, his goal was not development of a separation technique, but rather the t petroleum its different quality result

10、from their separation during migration through the ground. he of Rungeswork, Days investigations didnot proceedhe early 1900s, Mikhail inventedclassical column chromatography and demonstrated its ability to separate different extracts12. This was certainly the beginning of chromatography, but the va

11、lue of his work not ted for another two he early1930s,Tswettsworkwasrediscoveredleading to an explosive subsequent growth of chromatography. The invention of rchromatography by A.J.P. Martin followed in 1943 panied by the development thin-layer chromatography n the late 1930s and the mid-1950s 17. T

12、his short sarily omits numerousother contributions to the development of chromatography The amino-he late 1950s 15, was an important precursor to it was an automated means yzing mixtures of amino acids by use of ion-chromatography (Section 7.5). This was followed by the invention of gel chromatograp

13、hy (Section 13.7) by Moore 18 and roduction in the early 1960s of gel-permeation chromatograph by Waters tes 16. Each of these latter techniques close in concept to aterbecame HPLC, differing little from the schematic of Figure 1.1g. each case the solvent was pumped at high re through a reusable, sm

14、all-particle column, column effluent was continuously monitored by a detector, and the output ofthe device was chromatogramas in Figure 1.1h. What each of lacked, however, was an to separate yze other kinds of les.The amino-yzer was restricted to ysisofmixturesofaminoacids,whilethegel-permeationchro

15、matographwasusedfordeterminingthemolecularweightdistributionofsyntheticpolymers.InneithercasewerereadilyadaptablefortheseparationofotherDuring the early 1960s, two different groups embarked on the development of ysisofmixturesofaminoacids,whilethegel-permeationchromatographwasusedfordeterminingthemo

16、lecularweightdistributionofsyntheticpolymers.InneithercasewerereadilyadaptablefortheseparationofotherDuring the early 1960s, two different groups embarked on the development of a general-eHPLC system, under the leadership of Csaba he United es and Josef Huber （在20世纪60年代，两个不同的组织的Csaba Horvath 和欧洲的Jos

17、ef Huber的Each of these two men have described their early work on HPLC in a collection of recollections 19,andEttrehasprovidedadditionaldetailonearlyworkinHorvathslaboratory（Ettre还提供了其他的在HorvathThe immediate results of these two groups, plus relatedwork by t was carried out a yearslater,aredescribed

18、intappearedin1966to19682,在了 1966-1968 （roduction of l equipment for HPLC followed in the RODUCTION 1960s,withsystemsfromWaterstesandDuPontinitiallydominatingthe Other companies soon offered competing equipment, and research on HPLC began to accelerate (as seen from Fig. 1.2a). HPLC book had been pub

19、lished 25, and an HPLC short course was offered by American Chemical Society (Modern Liquid Chromatography, with J. J. Kirkland and L. Snyderascourse （1971 Progressive improvements in HPLC from 1960 2010 are illustrated by the separations of Figure 1.5af , which show separation times decreasing by s

20、everal orders magnitudeduringthis50-（1960-20101.5a-f中有代表性的分离画图，Figure 1.5g shows how this reduction in separation time (,) was related to increases in re drop across the column (- - -) and a he size of particles twere used pack the column.（1.5gIn the early days of HPLC the technique was sometimes re

21、ferred to as high-re chromatographyorhigh-speed liquidchromatography,for ggested by Figure Figure 1.5hshowscorrespondingchangesincolumnlength()andflowrate ()forthe separations of Figure 1.5ae.1.5g 1.5h 1.5a-e A theoretical foundation for the eventual development ofHPLCwas established well before the

22、 1960s. （20 60 ）In 1941, Martin reported t the mostA theoretical foundation for the eventual development ofHPLCwas established well before the 1960s. （20 60 ）In 1941, Martin reported t the most efficient columns . . . should be yusing very small particles and high-re across the length of the column;

23、 summarized the requirements for HPLC separation in a (as demonstrated by Fig. （1941够得到”，这总结了高效液相色谱在微小物质分离上的要求。In the early 1950s, the technique of gas chromatography was invented by Martin 28; its acceptance by the 29 led to a number of theoretical t would prove relevant to the later development 导致

24、了许多的后来将被证明与后来的高效液相色谱相关的理论研究）Giddings and extended this work for specific application to he early 1960s 30, t later to prove important for both column design and the selection of preferred experimental conditions. （Giddings2060年代早期这些在色谱专一的应用上的工作，这些工作后来被证明在色谱柱设计和更好的实验条件的选择上很重要）For a backgroundontheear

25、lydaysofHPLCsee19,3133.（ the collected biographies of several HPLC practitioners 34.(1980年后的高效液相色谱简答：用流程图说明用玻璃膜电极和饱和甘 电机两次法测流程和原理he 1890sDavidDayattheUSGeologicalsurveycarriedoutseparationsofpetroleumby a techniquet resembles classical column chromatography 11; however, his goalwasnotthedevelopmento

26、faseparationtechnique,but ratherthet itsofdifferentqualityhe 1890sDavidDayattheUSGeologicalsurveycarriedoutseparationsofpetroleumby a techniquet resembles classical column chromatography 11; however, his goalwasnotthedevelopmentofaseparationtechnique,but ratherthet itsofdifferentqualityresultfromthe

27、irseparationduringthroughtheground.notproceedhecaseofRungeswork,Daysinvestigationsheearly1900s,MikhailTswettinventedclassicalchromatographyanddemonstrateditsabilitytoseparatedifferentplant12.Thiswascertainlythebeginningofchromatography,butthevalueofhiswasnottedforanothertwoheearly1930s,Tswettsworkre

28、discovered13,leadingtoanexplosivesubsequentgrowthofTheinventionofrchromatographybyA.J.P.Martinfollowedin1943paniedbythedevelopmentofthin-layerchromatographynthe1930sandthemid-1950s17.ThisshortsummarysarilyomitsothercontributionstothedevelopmentofchromatographybeforeTheamino-helate1950s15,wasanprecur

29、sortoHPLC;itwasanautomatedmeansyzingmixturesofacidsbyuseofion-exchangechromatography(Section7.5).Thiswasfollowedtheinventionofgelpermeationchromatography(Section13.7)byMoore18heearly1960sofa gel-permeationchromatographbytes16.EachoftheselattertechniqueswascloseinconcepttobecameHPLC,differinglittlefr

30、omtheschematicofFigure1.1g.Ineachcasesolventwaspumpedathighrethroughareusable,small-particlethecolumneffluentwascontinuouslymonitoredbyadetector,andtheoutputthedevicewasachromatogramasinFigure 1.1h.Whateachoflacked,however,wasanabilitytoseparateyzeotherkindsofTheamino-yzerwasrestrictedtoysisofmixtur

31、esofaminowhilethegel-permeationchromatographwasusedexclusivelyfordeterminingmolecularweightdistributionofsyntheticpolymers.InneithercasewerereadilyadaptablefortheseparationofotherDuringtheearly1960s,twodifferentgroupsembarkedontheofageneral-eHPLCsystem,undertheleadershipofCsabaUnitedesandJosefHuberi

32、nEurope.Eachofthesetwo menhave theirearlyworkonHPLCinacollectionalrecollections19,andhasprovidedadditionaldetailonearlyworkinHorvathslaboratory20.immediateresultsofthesetwogroups,plusrelatedworkbytwas outafewyearslater,aredescribedintappearedin1966to2,2124.roductionoflequipmentforHPLC8late1960s,with

33、systemsfromWaterstesandDuPontinitially themarket.Othercompanies2,2124.roductionoflequipmentforHPLC8late1960s,withsystemsfromWaterstesandDuPontinitially themarket.Othercompaniessoonofferedcompetingequipment,andresearchHPLCbegantoaccelerate(asseenfromFig.1.2a).By1971,HPLChadbeenpublished25,andanHPLCshortcourse wasofferedbytheAmerican Chemical Society (Modern Liquid Chromatography), with J. J. Kirkland andL.R.Snyderascourse ProgressiveimprovementsinHPLCfrom1960to2010areillus