[金属材料精品] 红外光谱制样新技术应用与研究 毕业论文

A1A0A2A3A4A5A6A7A6毕业论文（设计）红外光谱制样新技术应用与研究RESEARCHOFIMPROVEMENTANDAPPLICATIONINSAMPLEPREPARATIONTECHNOLOGYFORINFRAREDSPECTRUM申请学位工学学士院系环境与材料工程学院专业金属材料工程姓名学号指导老师2011年6月5日A8A9A10A11红外光谱制样新技术应用与研究姓名导师2011年6月5日A12A13A14A15毕业论文（设计）任务书A16A17A18A19A20A21A22A23A24A25A26A27A28A16姓名学号毕业届别2011专业金属材料与工程毕业论文（设计）题目红外光谱制样新技术研究与应用指导教师学历硕士职称讲师所学专业环境工程具体要求主要内容、基本要求、主要参考资料等主要内容针对不同物相、不同分子量大小的化合物及其性质差异,介绍了现代红外光谱分析中的试样预处理和若干制样方法等制备技术。基本要求帮助读者确定合适的制样方法，得到高质量的红外光谱主要参考文献1刘立军,姜恒,宫红,苏婷婷红外光谱分析中样品处理方法的改进J光谱学与光谱分析,2004,012韩海洪,张德现代红外光谱分析中的试样制备技术J青海师G14551大学学G6265G14270G9994G12197学G10268,2003,01G22G51G85G68G80G68G81G68G47G68G86G72G68G85G68G80G68G81G68G81G71G76G81G73G85G68G16G85G72G71G86G83G72G70G87G85G68G82G73G69G76G82G80G82G79G72G70G88G79G72G29G24G16G68G80G76G81G82G88G85G68G70G76G79G44G81G71G76G68G81G36G70G68G71G72G80G92G82G73G54G70G76G72G81G70G72G86G57G82G79G26G19,G49G82G22G48G68G85G70G752G19G19G27G83G83G23G26G28G16G23G27G25G23G41G85G72G71G43G53G88G71G71G72G79G79,G77G82G75G81G43G48G82G81G87G74G82G80G72G85G92G72G85G81G68G81G76G88G80G48G50G54G87G72G70G75G81G82G79G82G74G92G73G82G85G76G81G73G85G68G16G85G72G71G71G72G87G72G70G87G82G85G86G49G88G70G79G72G68G85G44G81G86G87G85G88G80G72G81G87G86G68G81G71G48G72G87G75G82G71G86G76G81G51G75G92G86G76G70G86G53G72G86G72G68G85G70G75G36G24G26G22G112G19G19G26G12G25G24G16G25G26再加几篇文献进G5242G4445G65021G252G23G2620，G6922G19610G17176料G727G12544G24G2620G6564G1144G5332题G6265G2590G727G25G2521G22G2620G1901毕业论文G7271G23G2620G2033G1144G12307，G1474改G2530G6183G2372。1G24G971G25G2620G12584G17789。A29A30A31A32指导教师（G12626G4395）G5192G7388G7097院（系）意见教学G19510G19283（G1039G1231）（G12626G4395）G5192G7388G7097备注A29A30A31A321摘要A33A34A35A36A37A38A39A40A41A37A38A42A43A44A45A46A47A48A49A39A50A51A52A53A54A55A56A57A58A59A60A61A62A63A64A65A66A67A42A68A69A47A70A71A72A73A74A75A76A77A78A71A79A80A81A78A82A83A84A85A86A87A88A89A90A91A92A67A93A53A44A47A94A95A75A89A90A91A92A67A93A53A44A47A94A95A85A96A97A48A49A39A75A98A97A46A42A43A48A49A39A47A78A71A79A80A99A100A101A102A85A103A40A71A104A98A105A106A80A41A107A105A80A81A108A105A40A71A104A98A109A106A80A41A110A111A112A80A41A113A105A114A105A115A107A105A80A41A116A117A80A41A118A119A80A41A107A105A80A108A120A40A71A104A98A121A106A80A41A122A111A112A80A41A123A124A80A41A66A125A66A67A80A85A126A42A43A127A49A39A71A104A99A100A128A102A56A129A130A131A132A56A71A104A37A133A134A135A136A137A138A56A139A102A71A104A140A98A102A99A113A132A53A115A141A142A143A144A145A41A146A147A145A41A96A97A148A149A81A150A56A94A151A37A152A153A154A46A42A43A48A49A39A47A78A71A79A80A56A58A35A36A155A156A129A130A153A154A157A158A47A79A80A85A57A58A87A88A159A116A160A106A80A41A107A161A160A106A80A41A159A162A163A164A80A85A165A166A167A168A47A71A104A98A167A168A47A78A71A79A80A85A169A65A36A170A171A44A71A104A47A78A71A172A98A167A173A78A71A79A80A174A175A46A176A177A69A80A75A178A179A180A177A80A85A181A182A183A184A185A186A187A188A189A190A191A192A193A194A195A196A197A198A199A200A201A202A203A187A188A189A190A191A192A193A204A205A206A197A207A208A209A206A210A211A212A186A213A214A202A215A216A205A186A217A194A197A218A219A220A221A222关键字A187A188A189A190A223A224A192A223A191A225A226A227A228A229A230A2312ABSTRACTTHISPAPER,THEDIFFERENTPHASES,DIFFERENTMOLECULARWEIGHTCOMPOUNDSANDTHEIRDIFFERENTNATURE,INTRODUCESTHEMODERNINFRAREDSPECTRUMOFSAMPLEPRETREATMENTANDPREPARATIONOFANUMBEROFMETHODS,SAMPLEPREPARATIONTECHNIQUESALSOAFFECTTHEQUALITYOFIRSPECTRAIRSPECTRAOFFACTORSANDIMPACTOFTHEQUALITYFACTORINORGANICCOMPOUNDSANDORGANICSMALLMOLECULECOMPOUNDSMORETYPESOFSAMPLEPREPARATIONGASSAMPLESHAVELIQUIDMEMBRANE,SOLUTIONMETHOD,ETCLIQUIDSAMPLESWITHCOATINGMETHOD,TOTALREFLECTIONMETHOD,“LIQUIDLIQUID“SOLUTIONMETHOD,COMPRESSIONMETHOD,APASTEMETHOD,SOLUTIONMETHODSOLIDPHASESAMPLESWITHMEMBRANE,DIFFUSEREFLECTIONMETHOD,SUBLIMATIONMETHOD,PHOTOACOUSTICSPECTROSCOPYAWIDERANGEOFPOLYMERSAMPLES,THESITUATIONISCOMPLEX,DIFFICULTTOGRINDINTOPOWDERSAMPLES,MANYSAMPLESCONTAINAVARIETYOF“IMPURITIES“SUCHASPLASTICIZERS,ANTIOXIDANTS,INORGANICFILLERS,ETC,ITISNOTTHEUSEOFSMALLMOLECULECOMPOUNDSINPREPARATIONMETHODS,SPECIFICCONDITIONSTOUSETHEAPPROPRIATEMETHODINCLUDINGTHERMALDIEMEMBRANE,CASTINGSOLUTIONMETHOD,HOTMELTADHESIONMETHODSPECIFICSAMPLEHASASPECIFICSAMPLEPREPARATIONANOTHERSAMPLEPREPARATIONFORTRACESAMPLESALSOHAVEASPECIALSAMPLEPREPARATIONMETHODFORTHECONCENTRATIONMETHODANDTHETRIANGULARHOLEENRICHMENTMETHODTHISARTICLEALSODESCRIBESTHEKINDOFIRSYSTEMSHOULDPAYATTENTIONTOSOMEPROBLEMS,LIKEINTHEINFRAREDSPECTRUMSYSTEMPRONETOIRREGULARITIESISANALYZED,ANDTHECORRESPONDINGSOLUTIONSKEYWORDSA232INFRAREDSPECTRUMA233SAMPLEA233PREPARATIONA234A235A236A23731绪论11概述红外光谱法（G76G81G73G85G68G85G72G71G86G83G72G70G87G85G82G86G70G82G83G92）研究红外光与物质G19400相G1126G1328用的G12197学，G2375G1209G17842G13505G8886G19283的红外光G1038光G9316G10043G4568样品G5353G17227分子G6403G2172和G17728G2172G14033G13435G1055G19400G17303G17813，所G8991得的G2572G6922光谱G1038分子的G6403G17728光谱，G2460称红外光谱。红外光G7171G980G12193G8886G19283介G1122G2499G16277光G2318和G5506G8886G2318G1055G19400的G11017G11925G8886谱。G8886G19283G3324G19G26G27G794G22G19G19G173G80。G17902G5132G2460G6238G17837G1022G8886G8585分成三G1022G2318域，G2375近红外G2318G8886G19283G3324G19G26G27G7942G24G173G80（G8886数G332412G272G19G794G23G19G19G19G70G80G161），G2460称泛频G2318G727中红外G2318G8886G19283G33242G24G7942G24G173G80（G8886数G3324G23G19G19G19G794G23G19G19G70G80G161），G2460称基频G2318G727远红外G2318G8886G19283G33242G24G794G22G19G19G173G80（G8886数G3324G23G19G19G794G22G22G70G80G161），G2460称G17728G2172G2318。其中中红外G2318G7171研究、应用最多的G2318域。红外光谱G3324化学领域中G1039要用G1122分子结构的基础研究（G8991定分子的键G19283、键角等）G1209及化学组成的分析（G2375化合物的定性定量），但其中应用最广泛的还G7171化合物的结构鉴定，根据红外光谱的峰位、峰强及峰形，判断化合物中G2499G14033存G3324的官G14033团，从而推断出未知物的结构。有共价键的化合物（包括无机物和有机物）都有其特征的红外光谱，除光学异构体及G19283链烷烃同系物外，几乎没有两G12193化合物具有相同的红外G2572G6922光谱，G2375所谓红外光谱具有“指纹性”，因此红外光谱法用G1122有机药物的结构G8991定和鉴定G7171最重要的方法G1055G980。G980张高质量的G44G53谱图,要基线平稳、分辨率高、最高峰G3324透过率G11TG12G14551围内,很弱的峰亦G14033清晰的显示出来而不被噪音所掩盖,从而将化合物的结构单元信息尽G2499G14033多的反映出来。G3324仪器、样品及其G8991试条件都已确定G2530,试样的预处理和制样方法G7171谱图质量的决定因素A238A239A240。对此,本文结合工G1328实际,从影响G44G53谱图质量的因素、G44G53对样品的要求、样品的预处理和各类物相不同分子大小的样品制样方法等方面进行对比讨论,并对不同类型、不同性质的样品确定了其合理的制样方法。A241A242A243A244412红外光谱法的基本原理当G980束具有G17842G13505G8886G19283的红外光G17902过物质，物质分子中某G1022基团的G6403G2172频率或G17728G2172频率和红外光的频率G980样G7114，分子G4613G2572G6922G14033量G11013G2419来的基G5589G6403G11G17728G12G2172G14033G13435G17303G17813到G14033量G17751高的G6403G11G17728G12G2172G14033G13435，分子G2572G6922红外G17764G4568G2530G2469G10995G6403G2172和G17728G2172G14033G13435的G17303G17813，G16825处G8886G19283的光G4613被物质G2572G6922。所G1209，红外红外光谱光谱法实质G990G7171G980G12193根据分子内G18108G2419子G19400的相对G6403G2172和分子G17728G2172等信息来确定物质分子结构和鉴别化合物的分析方法。将分子G2572G6922红外光的G5785G1929用仪器G16772G5417G991来，G4613得到红外光谱图。2红外光谱图G17902G5132用G8886G19283G11G172G12或G8886数G11G179G12G1038G8190G3364G7643，G15932示G2572G6922峰的位G13634，用透光率G11TG12或者G2572光G5242G11G36G12G1038G13449G3364G7643，G15932示G2572G6922强G5242。当外G11040G11017G11925G8886G10043G4568分子G7114，G3926G10043G4568的G11017G11925G8886的G14033量与分子的两G14033G13435差相等，G16825频率的G11017G11925G8886G4613被G16825分子G2572G6922，从而G5353G17227分子对应G14033G13435的G17303G17813，G4451G16278G15932现G1038透G4568光强G5242G2476小。G11017G11925G8886G14033量与分子两G14033G13435差相等G1038物质G1147G10995红外G2572G6922光谱G5529G20047G9397G17287条件G1055G980，G17837决定了G2572G6922峰出现的位G13634。红外谱G5114的强G5242G7171G980G1022G6403G2172G17303G17813G8022率的量G5242，而G17303G17813G8022率与分子G6403G2172G7114G1610G7509G11709的G2476化大小有G1863，G1610红外G2572G6922光谱G1147G10995的G12544G1120G1022条件G7171红外光与分子G1055G19400有G1610合G1328用，G1038了G9397G17287G17837G1022条件，分子G6403G2172G7114其G1610G7509G11709G5529G20047G2469G10995G2476化。G17837实际G990G1457G16789了红外光的G14033量G14033G1268G17894G13485分子，G17837G12193G14033量的G1268G17894G7171G17902过分子G6403G2172G1610G7509G11709的G2476化来实现的。并G19762所有的G6403G2172都G1262G1147G10995红外G2572G6922，G2494有G1610G7509G11709G2469G10995G2476化的G6403G2172G6177G14033G5353G17227G2499G16278G8991的红外G2572G6922，G17837G12193G6403G2172称G1038红外G8975性G6403G2172G727G1610G7509G11709等G1122G19658的分子G6403G2172不G14033G1147G10995红外G2572G6922，称G1038红外G19762G8975性G6403G2172G7509G11709G2476化G5852大，谱G5114强G5242G5852大。G1610G7509G11709的G2476化与基团本G17535G3278有的G1610G7509G11709有G1863，G6937基团G7509性G17246强，G6403G2172G7114G1610G7509G11709G2476化G17246大，G2572G6922谱G5114G17246强G727分子的对称性G17246高，G6403G2172G7114G1610G7509G11709G2476化G17246小，G2572G6922谱G5114G17246弱。A241A242A243A244513红外光谱分析制样技术概况及应用现状G111G12制样技术G8022G1929红外光谱图G7171定性鉴定的G1393据G1055G980,G8503确的样品制备方法G727G980G14336G19668要G11023出的谱图基线G17751平,最强峰G1185G3324透过率G14551围内,弱峰还G14033清晰G11487出,并不被噪G3780所掩盖。显G9994G6496G6581G980G1135G12628单实用的样品制备方法,比G17751G5567G3332制备出质量G3921的谱图G7171很重要的。影响谱图质量最重要的因素G7171样品的G2414G5242。样品G3838G15192,峰G1262很弱,有G1135峰G1262被基线噪G3780掩盖G727相反,样品G3838G2414,峰形G1262G2476G4497,G10990G14279G7171平G3848峰。根据不同的样品,样品G2414G5242应有所不同。比G3926G2559G8699基团的G2572G6922很强,因而G2559G8699样品不G4464过G2414G727而G2559G20293和G13870G9923烃的样品G2029G2499G12257G2414,G6177G14033G1582出G17751理G5831的谱图。G2490外，样品G15932面反G4568的影响G1075G20047G13783G15397。G980G14336G15932面反G4568的G14033量G6451G3845G17751小,但G3324强谱G5114G19480近G6451G3845G2499G178101G24G1209G990。G4600其G7171G1314频G980G1403,G11013G1122样品的G6252G4568率G2476化很大,从而G1363G6252G4568和反G4568大G1038G3698G2164。G1038了改进光谱质量,G3324G1268G13491的G2464光束光G7641型光谱仪中,G2499G1209G3324G2454比光G17347中G6930G1849G980G1022组分相同但G2414G5242G17751G15192的样品,G17837样G2499G1209有G6940G15929G1619G11013反G4568G5353G17227的谱G5114G2476形G727对G1122G1625G18336G2506G2476G6454红外光谱仪，G3926G7536G8991试G7114出现干G9053条纹，G2499将G11925性品G3853的G980G1403用G24G80G80G5050G2503G2414的G3371G10378物G3455高，G2490G980G1403用G11925片将G3455片压住，G1363G3455片斜对着红外光G17347，G2499防止光经过G3455片G7114G2469G10995干G9053。G112G12制样现G10378及存G3324问题G5132用的红外光谱分析制样技术除了G1268G13491的溴化钾压片法和液膜法外,对G1122G3278体样品,G5132用的制样方法还有粉末法、G15192膜法、糊剂法、浸渍法。对G1122液体样品,G5132用的制样方法还有溶液法、G15192膜法。随着G1625G18336G2506G2476G6454红外光谱技术的G2469展，出现了许多新的红外制样技术。例G3926利用显G5506红外光谱技术G2499G1209G8991试G5506量样品，G2375G1363G7171G5506克G13435的G3278体或液体样品，利用显G5506红外技术G1075G2499G1209得到很G3921的光谱。对G1122单分子膜样品，G2499G1209利用掠角反G4568技术。G3926G7536要G5831G8991试G15192膜或片材G15932面样品的红外光谱，G2499G1209采用水平G36TG53（多次衰减全反G4568）或单次衰减全反G4568技术。目前的红外制样技术已走向逐渐成熟G19400断，但G7171红外光谱法对试样G1185具有G17751高的要求，例G3926G727试样要求G7171单G980组份的纯物质，纯G5242应大G1122G28G27或符合商业规格，G17837样G6177便G1122与纯物质的G7643准光谱进行对G10043。多组份试样G3324G8991定前G5529G20047要尽量预先用分馏、萃取、重结晶或色谱法进行分离G6564纯，否G2029各组份光谱相G1126重叠，难G1122判断。试样中要G1363其不G2559有游离水，水本G17535有红外G2572G6922，G1262严重干扰样品谱，而且G1262侵蚀磨具、盐窗等。试样的浓G5242和G8991试G2414G5242不易控制等，G17837都G1363得制样技术存G3324G980定的困难。A245A246A247A2486G11G22G12应用现G10378现代红外光谱分析技术广泛用G1122无机化合物和有机化合物的结构单元解析I。近G5192来,红外光谱G3324新兴的G10995命G12197学、材料G12197学、环境G12197学等领域G2469挥了重要G1328用。红外光谱G1209其操G1328G12628便、对样品无特殊要求、实验成本G1314、G14033够G6564供丰富的官G14033团信息而成G1038定性分析的G5529要手G8585。2红外光谱试样21红外光谱法对试样的要求G111G12样品的G2414G5242G11浓G5242G12样品G2414G5242G7171谱图质量最重要的影响因素。G2414G5242G3838G15192,大G18108分峰都很弱,有此峰G1262被基线噪音所掩盖G2414G5242G3838G2414G7114峰形G1262G2476G4497G10990G14279G1147G10995截顶。G112G12样品的性质样品的性质不同,G2414G5242应有所不同。比G3926G29G2559G8699基团的样品G2572G6922很强因而G2414G5242G4613不G4464过G2414而G20293和G13870G9923烃无强G2572G6922,G2029G2499G12257G2414G1135。G11G22G12样品的G15932面G6252G4568和反G4568G980G14336样品G15932面反G4568的G14033量G6451G3845G17751小,但G3324强谱G5114G19480近G2499G178101G24G1209G990,G4600其G7171G1314频G980G1403,G11013G1122样品的G6252G4568率G2476化的很大,从而G1363G6252G4568和反G4568大G1038G3698G2164。G1038了改进光谱质量,G1268G13491的G2464光束光G7641型光谱G11G3926岛津G44G53G16G23G19G27型G12解决的办法G980G14336G7171G3324G2454比光G17347中G6930G1849G980G1022组分相同但G2414G5242G17751G15192的样品,G17837G2499有G6940的G15929G1619G11013G1122反G4568而G5353G17227的谱G5114G2476形而G3324G1625立G2506G2476G6454红外光谱G11G3926美国G51E公司G41TG44G53G16G481G26G22G19型G12中G2029G2499G1209G17902过G980G1135技术处理来解决。G11G23G12试样应G16825G7171单G980组分的纯物质试样纯G5242应大G1122G28G27或符合商业规格,G17837样G6177便G1122与纯化合物的G7643准光谱进行对G10043。G17902G5132G3324分析前，样品G19668纯化。,否G2029各组分光谱相G1126重叠,G1209致谱图难G1122解析G11G24G12试样中不应G2559有水水G2499G1147G10995红外G2572G6922,G1262严重干扰样品的G2572G6922谱峰,而且G1262侵蚀G2572G6922池的G49G68CG79、KBG85或CG86G44盐窗。A249A250A251A252722试样的预处理和精制G19668要检G8991的样品大都G17751G1038复杂,绝大多数不G7171纯的化合物,而G7171已G2164G1849各G12193添G2164剂和助剂,因而G19668要先对样品进行预处理G2530G6177G14033制备,否G2029得到的谱图没有意义,无法得出G8503确的结论,因此样品的预处理很G1863键。G980G14336来说,G3324没有G7643样谱图的G5785G1929G991,杂质G2559量超出G1911G161,G4613G19668精制。而对混合物的定性分析,亦应尽G2499G14033的减少组分数。G5132用的预处理和精制方法,G2499G1393据试样的G10378G5589和性质采用重结晶、精馏、萃取、柱色谱、G15192层色谱和气液制备色谱等分离精制手G8585进行。G3324此过程中应防止试样的污染、G2476质G11G2469G10995化学G2476化G12G1209及水分的混G1849和相G5589结构的改G2476等。对G1122大分子物质,G3926天G9994或合成高分子G1147品、成品等G17902G5132都不G7171纯化合物,往往G7171G2164G1849了各G12193添G2164剂和助剂。因此,G19668将样品进行预处理精制G2530G6177G14033进行制样G8991定。最G5132用的预处理方法G1039要有溶解G252沉淀分离法和溶剂萃取法两G12193A253A254A255。G3926G7536G2494G7171分析无机填料、颜料等添G2164成分,而不分析有机化合物组分,G2029G2499G1209G17902过G12628单的溶解或灼烧,G4613G2499G1209除去有机组分。溶解法G7171用溶剂将化合物充分溶解G2530,再用离心、过G9400、G1554出等方法除去有机组分,G2109G991无机G18108分。G1075G2499用灼烧方法除去有机组分,得到无机物,G9994G2530G2499根据G19668要G1328G2469G4568光谱、G14033谱等定性分析。G3926G7536样品G7171G1095G10378液G11G9046料、G21667合剂等G12,G2029G11784G1095G2530G6177G2499G1209进行分离,G11784G1095G2499G17902过G2164G9921、G2164G18252、G2164无机盐或G1931G1935等方法来G4448成。对G1122线性G2499溶高分子材料,G2499G17885G6333G980G12193适当的溶剂G1363其G4448全溶解,过G9400或离心除去无机填料,G9994G2530G2164G1849G2490G980G12193过量溶剂G11沉淀剂G12G1363其G4448全沉淀,将G2499溶性添G2164剂组分G11053G3324溶液中。G17902过过G9400或离心除去有机沉淀G2530,G14988去溶剂,得到G17837G1135添G2164成分。G17885用的溶剂应G14033溶解有机添G2164剂,沉淀剂G5529G20047与溶剂G1126溶。但G7171G3324实验中往往分离不G4448全,G1039要G2419因有两G9869G29G980G7171G13870合物的分子量往往G7171G11013小到大组成系G2027,分离出的添G2164剂中有G1314分子量的G13870合物,称G1038G21796G13870物。G1120G7171沉淀出的高分子G8543G11053有少量添G2164剂,有G1135添G2164剂G1262与G13870合物形成某G12193结合G10294G3278的G13488合物,G2494有G17902过多次溶解G16沉淀过程G6177G14033分离G4448全。萃取法的目的G7171从G3278体材料中G6564取出有机添G2164成分,G17902G5132G7171G3698G3621剂等有机助剂。材料G3324溶剂中其实G7171G980G1022G6205G6967过程,G5332G3999G7114G13870合物有所溶G9084,G1813许溶剂G9195透进G1849内G18108,添G2164剂溶解G3324溶剂中,G3324G2334透膜两G17805形成浓G5242G7811G5242,G11464到G5326立浓G5242平G15925。萃取G1039要有两G12193方法,G980G12193G7171G3250G8981萃取,G2490G980G12193G7171用G13046G5347萃取器G11G14038G13950萃取器G12G17842G13505萃取。G3926G7536G13870合物中的G2499溶性添G2164剂G2559量G17751少,用G3250G8981萃取法G17751G1038方便,有G7114G1075G2499G1209不用G2164G9921G3250G8981,G2494G20047将样品G2011G11874G2530与溶剂混合G19757G13634并经G5132G6683G2172。添G2164剂G2559量G17751多G7114,不G14033用此法萃取,因G1038溶解G1262G17810到G20293A249A250A251A2528和而G13468止,应用G14038G13950萃取器萃取,G6940G7536G17751G3921。萃取G17885用的溶剂,应G18003G1825与试样中的组分G2469G10995反应,还应G18003G1825溶剂将样品与添G2164剂G980同溶解,萃取所用样品的比G15932面要大。得到的混合物应用G15192层色谱等方法进行分离,得到各G1022组分的纯品。G3324实际工G1328中,G19668要经过多次G6732G13046和试G6518,G6177G14033确定合适的分离和纯化方法,有G7114两G12193方法G1075G19668要反复G1144G7379G1363用。3红外光谱制样方法对不同的样品采用不同的制样方法G7171现代红外光谱研究中取得G8503确G2499G19764信息的G1863键,要G8892意到化合物红外光谱图中的特征谱G5114频率不同而G2499G14033G5114来的G2476化。因此,G17885用合适的制样方法要从被G8991样品和实验目的两方面G13783G15397,G11013G1122红外光谱的试样G2499G1209G7171气G5589、液G5589或G3278G5589,根据试样物相的不同,其制样方法及其适用对G16949G1075不同。31无机化合物和有机小分子化合物的制样方法红外光谱G1328G1038化合物结构定性分析的G1039要手G8585G1055G980,G3324无机及有机小分子化合物方面显得最G1038G12373出,其红外光谱的制样方法G17751多4。（1）气相样品的制样方法G1038气体G2572G6922池法。G19668要的G1039要设备G1038不同规格G13796压G10639G10839气G8145（两G12483G12908透红外光的单晶盐片）。G1039要操G1328G1038将气G8145G6289G11507G12366G2530将样品G8892G1849。G4439适用G1122气体样品，G1075适用G1122G1314G8844G9869和某G1135G20293和G14988G8785压大的液体样品。（2）液相样品有液膜法、溶液法、G9046膜法全反G4568法、液液溶液法G3247G12193方法。其中，溶液法适用G1122G1314G8844G9869且易挥G2469的液体或溶液样品，G7171红外光谱定量分析G5132用的方法G727G9046膜法适用G1122G12908G5242大的样品G727全反G4568法特别适用G1122G1314G8844G9869液体和水溶液样品，要求G3324红外光G2318有G7509强的G2572G6922G727液液溶液法G1039要用G1122G16278G4531G8694键或G18242G5347G9923G18267G5347平G15925。（G22）G3278相样品G1039要有压片法、糊G10378法、溶液法、G15192膜法、G9471反G4568法、G2331G2338法、光G3780光谱法G983G12193方法。压片法最G5132用，适用G1122大多数易研磨的G3278体样品。糊G10378法特别适用G1122G14033G2476成G13466粉末的易G9538或G17947G12366气G1147G10995化学G2476化的G3278体样品。溶液法适用G1122易溶G1122红外G5132用溶剂的G3278体，G3324红外光谱G3278体定量分析中最G5132用。G15192膜法分G1038G10088G15713G15192膜法、溶液G15192膜法、G11507G12366G14988着法、G19480着法，特别适用G1122G10088G9869G1314的G3278体样品，多用G3324红外光谱定性分析G990。G9471反G4568法特别适用G1122粉末样品的G8991定。G2331G2338法适用G1122某G1135G17947G12366气不稳定或高G9213G991易G2331G2338的G3278体样品。光G3780光谱法A249A250A251A2529适用G1122G9157色、G11840G12902、G19762G3355G2260的G3278体样品。32有机高分子化合物即高分子聚合物的制样方法G11013G1122高分子G13870合物样品G12193类G13333多,G5785G1929复杂,样品不易研磨成粉末,许多样品G2559有多G12193“杂质”G3926G3698G3621剂、防G13781剂、无机填料等,因此不G14033采用小分子化合物的制样方法,要针对具体G5785G1929采用适当的方法5。（1）G9921压G19148膜法对G1122G1314G17731化G9213G5242且不易G9921G19489解的高G13870物,G3926G13870G1069G9923、G13870G1005G9923等G3621料G2499采用G9921压G19148膜法来制备试样。将高G13870物试样G13466G12902G3853G3324有G6255光面的G16277方,G2414G13434的两G1022不G19164G19062G3371G1055G19400,G13634G11017G9821G990G2164G9921G14279G11065高G1122试样的G17731化G9213G5242,G5465试样G17731化G2530立G2375G12239到G8845压机G990G2164压,G1931G2376G2530G6593G991G15192膜进行G8991定G1038了G18003G1825试样G15192膜G12908G3324金属G3371G15932面而难G1122G2105离,G6117G1216预先G3324金属G3371G15932面G6987G1209G15192G19121G12648,G17837类G7592G17731的G15192膜易G1122从G1931G2376G2530的高G13870物膜G990G2105除。对G1122G17731化G9213G5242G17751G1314的试样,G3324金属G3371G15932面G9046G6285G11719G15605G8845或G1973士G7531G1075有防G12908着的G6940G7536,但G20047对制得的G15192膜G1192G13466清G8939,G1209去除G8543G11053的G11719G15605G8845或G1973士G7531,G1209G1825G1147G10995干扰。用G17837G12193方法制备的G13870G1069G9923、G4624G5079G980等高G13870物试样,都G14033得到相当理G5831的红外光谱图。G11013G1122高G9213G2499G14033G5353G17227高G13870物的G19489解,所G1209对G1122G17731化G9213G5242G17751高的高G13870物试样,不G4464采用G9921压法,G2499G1209G13783G15397改用溶解G19148膜法来制样。（2）溶解G19148膜法将高G13870物试样溶解G1122某G12193G1314G8844G9869溶剂中进行G19148膜G980G14336G2499G14731得G1260G14403的光谱。所G17885溶剂G5529G20047G7171不与试样G2469G10995化学反应的,并且挥G2469G2530不G11053G991G8543G1325物质。G6117G1216G5132用的溶剂有G8707G1235、苯、甲苯、G1120甲苯、G3247G8707化碳等,G2499G17902过试验进行G17885G6333G1363用。溶解G19148膜法的具体操G1328过程G3926G991先将高G13870物试样G2011G11874浸泡G3324G17885定的溶剂中,G5465溶解G2530用G6289气法G1363溶剂G14988G2469,G5465溶液浓缩G14279G12908稠G10378G7114用G10639G10839棒G12908几滴G9869G3324G10639G10839平板G990摊G15192并G14988G2469成膜。膜的G2414G5242G1393试样的G12193类G17902过试验调整而定。先G3324室G9213G991进行缓慢G14988G2469,G1209G1825G3324G19148膜G990G11053G991气孔,当G19148膜G3278化G7114再G2331高G14988G2469的G9213G5242,G1209去除G8543G11053的溶剂。G3324溶剂G14988G2469干G1055前,G2499G1209用G10639G10839棒将G10639G10839板G990某G980G1403的溶液摊G15192,G1209得到G980G2414G5242渐G2476的G19148膜,从而G17885G6333最合适G2414G5242的G18108位来G167