岛津气相色谱维护培训教材.pdf

SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875岛津气相色谱维护培训岛津气相色谱维护培训2006年9月 南通 Foxit Reader-(C)Foxit Software Company,2005-2006 SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875岛津气相色谱维护培训岛津气相色谱维护培训气相色谱构造气相色谱构造GC-2010GC-2010GC-14GC-14系列系列SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875气相色谱质谱仪的基本流路图气相色谱质谱仪的基本流路图 钢瓶He载气控制进样口色谱柱检测器数据处理SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875气相色谱仪的流动相气相色谱仪的流动相气相色谱仪的流动相气相色谱仪的流动相-载气载气载气载气尾吹气（纯度）助燃气（纯度）燃烧气（纯度）载气（纯度）检测器种类N2 He 等99.999%以上Ari 空气钢瓶空压机也可H2 等99.999%以上N2 He 等99.999%以上FID高灵敏度分析N2 He 等99.995%以上Ari空压机H2 等99.995%以上N2 He 等99.995%以上FID一般分析He N2 Ar等99.999%以上He N2 Ar等99.999%以上TCD高灵敏度分析He N2 Ar等99.995%以上He N2 Ar等99.995%以上TCD一般分析SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875气相色谱的进样方式气相色谱的进样方式WBIWBI进样口进样口毛细柱分流毛细柱分流/无分流进样口无分流进样口冷柱头进样冷柱头进样PTVPTV进样口进样口SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875热进样和冷进样热进样和冷进样热进样分流/无分流进样直接进样（WBI）宽口毛细柱和填充柱冷进样PTV进样冷柱头进样SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875歧视效应和热分解歧视效应和热分解 热进样(SPL,WBI)存在歧视现象和样品热分解冷进样 (OCI,PTV)进样是在较低温度下进行定量精度高歧视效应和热解效应的影响小SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875歧视效应的产生歧视效应的产生歧视歧视:蒸溜现象蒸溜现象 形成气溶胶形成气溶胶 分溜现象分溜现象 低沸点组分百分比偏高低沸点组分百分比偏高 进针进针 退针退针高沸点组分残留高沸点组分残留SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875减小热进样歧视现象的方法减小热进样歧视现象的方法快速进样法快速进样法 溶剂冲洗法溶剂冲洗法热针法热针法SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875溶剂冲洗法溶剂冲洗法蒸溜和分蒸溜和分溜减少溜减少溶剂溶剂 空气空气 样品样品 空气空气(%)(%)(%)(%)0.5 1.0 2.0 3.0 4.0(0.5 1.0 2.0 3.0 4.0(0.5 1.0 2.0 3.0 4.0(0.5 1.0 2.0 3.0 4.0(uLuLuLuL)52 51 50 49 4852 51 50 49 4852 51 50 49 4852 51 50 49 48n-C4n-C4n-C4n-C4n-C9n-C9n-C9n-C9SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875冷进样冷进样概念概念样品是在冷状态样品是在冷状态-低于样品沸点的温度下进样低于样品沸点的温度下进样 (依据溶剂依据溶剂)气化室快速升温使样品气化气化室快速升温使样品气化PTVPTV进样方式进样方式分流进样分流进样(高浓度样高浓度样)无分流进样无分流进样 (低浓度样低浓度样)大体积进样大体积进样LVILVI(痕量分析痕量分析)OCI柱头进样只适用于0.53内径的柱子无分流流路，不能分析高浓度样品（污染柱子），进样量一般小于2ulSHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875进样体积上限进样体积上限无分流进样无分流进样 (SPL,PTV)(SPL,PTV)2uL2uL高压进样高压进样 (SPL,PTV)(SPL,PTV)5uL5uL直接进样（直接进样（全量进样）全量进样）3uL3uL 用宽口径毛细柱用宽口径毛细柱冷柱头进样（冷柱头进样（OCIOCI）2uL2uLSHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875进样口的结构（进样口的结构（1 1）WBIWBI进样口进样口毛细柱进样口毛细柱进样口隔垫吹扫出口分流出口载气玻璃衬管F2F1隔垫吹扫出口载气玻璃衬管填充柱SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875进样口的结构（进样口的结构（2 2）冷柱头进样口冷柱头进样口(OCI)(OCI)PTVPTV进样口进样口隔垫吹扫出口分流出口载气玻璃衬管F2F1加热-250/min隔垫吹扫出口载气不锈钢衬管0.53mm内径宽孔毛细柱SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875色谱柱的类型色谱柱的类型填充柱填充柱柱材：不锈钢，玻璃内径：2.6-3mm长度：0.5-6m填料：担体和固定液的种类固定液的浓度 1-30%担体有硅藻土、玻璃、石英、塑料担体（TPA）等。SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875毛细柱柱材：熔融石英、铝内径：0.2mm-0.53mm长度：10-100m固定相种类：OV-1，PEG-20M，OV-17等固定相膜厚：0.2-5m 色谱柱的类型SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875几种代表性固定液的极性几种代表性固定液的极性(Mc Reynolds(Mc Reynolds 常数常数)SqualaneSqualane0 0 （非极性）非极性）PEG20M(DBWAX)322PEG20M(DBWAX)322（强极性）强极性）SE30SE301515 FFAP FFAP 340 340OV101(DB1)OV101(DB1)1717 PEG1000 PEG1000 347 347SE54(DB5)SE54(DB5)33 33（弱极性）弱极性）EGAEGA 372 372DC550DC5507474 DEGS DEGS 484 484OV17OV17119119（中极性）中极性）TCEPTCEP 593 593（超强极性）超强极性）BCEFBCEF 690 690名称I BenzeneI Benzene 名称 I BenzeneI BenzeneSHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875色谱柱的选择色谱柱的选择固定液极性的选择（按相似相溶原则）固定液极性的选择（按相似相溶原则）非极性固定液非极性固定液-有按沸点顺序溶出倾向有按沸点顺序溶出倾向极性固定液极性固定液-沸点相同时，按极性由小到大沸点相同时，按极性由小到大的顺序溶出的顺序溶出固定液的浓度或毛细管柱的膜厚固定液的浓度或毛细管柱的膜厚对低沸点化合物对低沸点化合物 高浓度（高浓度（10%10%30%30%)高膜厚高膜厚(1 15 5mm)对高沸点化合物对高沸点化合物 低浓度（低浓度（1%1%5%5%)低膜厚低膜厚(0.250.250.50.5mm)SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875内径对毛细柱分离的影响内径对毛细柱分离的影响0.22mm x 25mSHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875膜厚对毛细柱分离的影响膜厚对毛细柱分离的影响CBP1-W25-100膜厚 1umCBP1-W25-500膜厚 5umSHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875毛细柱的内径、膜厚及柱容量毛细柱的内径、膜厚及柱容量内径膜厚柱容量SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875各公司常用毛细柱商品名及固定液对照表固定相岛津J&WSGE信和化工FrontierLABRESTECSUPELCOCHROMPACK聚甲基硅氧烷OV-1CBP1DB-1BP-1HR-1Rtx-1SPB-1CP Sil 5 CB聚苯基甲基硅氧烷（5%苯基）SE-52CBP5DB-5BP-5HR-52Rtx-1,MXT-5SPB-1,PTE-5SAC-5CP Sil 8 CB聚苯基甲基硅氧烷（20%苯基）OV-7Rtx-20聚苯基甲基硅氧烷（50%苯基）OV-17,DB-17DB-17thRtx-50SP-22506%腈乙基甲基硅酮Rtx-1301OVI-G4314%腈乙基甲基硅酮OV-1701CBP10DB-1701BP-10HR-10Rtx-1701SPB-1701CP Sil 19 CB50%三氟丙基甲基硅氧烷OV-210DB-210Rtx-200CP Sil 43 CB50%腈乙苯基甲基硅酮DB-225HR-225Rtx-22550%腈乙基甲基硅酮DB-23聚乙二醇（硝苯二酸修饰）FFAPDB-FFAPStabilwax-DANukolCP Wax 58 CB,FFAP-CB聚乙二醇PEG-20MCBP20DB-WAXBP-20HR-20MALLOY-CWStabilwaxSupecolwax-10Carbowax 20MCP Wax 52 CB,联苯基聚甲基硅氧烷（14%联苯基）DB-XLB聚苯基甲基硅氧烷（65%苯基）ALLOY-TRGRtx-65TAP-CB90%二丙腈基10%腈乙苯基甲基硅酮Rtx-2330SP-2380SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875色谱柱的老化色谱柱的老化为什么必须进行色谱柱老化？为什么必须进行色谱柱老化？新色谱柱含有溶剂和高沸点物质，所以基线不新色谱柱含有溶剂和高沸点物质，所以基线不稳，出现鬼峰和噪声；旧柱长时间未用，也存稳，出现鬼峰和噪声；旧柱长时间未用，也存在同样问题。在同样问题。一般一般 采用升温老化，即从室温采用升温老化，即从室温程序升温到最高温度，并在高温段保持数小时。程序升温到最高温度，并在高温段保持数小时。新柱老化时，最好不要连接检测器。新柱老化时，最好不要连接检测器。每天都要进行老化吗？每天都要进行老化吗？视仪器基线情况，确定是否需要老化以及老化视仪器基线情况，确定是否需要老化以及老化时间。时间。SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875高压气瓶使用注意事项高压气瓶使用注意事项钢瓶应放置在通风条件好，避免光照并遵钢瓶应放置在通风条件好，避免光照并遵守液化气使用注意事项守液化气使用注意事项温度温度4040度以下，度以下，2M2M内禁止烟火内禁止烟火 燃烧气应配燃烧气应配备灭火器材备灭火器材工作前检漏工作前检漏每每3 3个月检查钢瓶及减压阀个月检查钢瓶及减压阀固定钢瓶固定钢瓶使用无油减压阀使用无油减压阀SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护进样口进样口更换进样垫更换进样垫更换更换“O O形圈形圈”更换玻璃衬管更换玻璃衬管 检测器检测器SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护选择选择 System System 中的中的 InjInj Maintenance Maintenance（PF menuPF menu）进样口，柱温箱，检测器自动降温，低于进样口，柱温箱，检测器自动降温，低于5050度时度时可进行维护操作。可进行维护操作。进样垫更换进样垫更换玻璃衬管更换玻璃衬管更换SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护进样垫日常维护进样垫 SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护(Press the SYSTEM key)Select(Press the SYSTEM key)Select Analysis in the PF menu.The GC will be Analysis in the PF menu.The GC will be readied automatically readied automatically 选择选择 DIAG DIAG 中的中的“3.Analysis Counter3.Analysis Counter”从从中选择中选择“Counter for SeptumCounter for Septum”并并 “ResetReset”键键对计数器进行清空对计数器进行清空SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护进样垫种类进样垫种类SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护进样垫有一定的使用温度，如果使用进样垫有一定的使用温度，如果使用温度不当，会产生杂峰。温度不当，会产生杂峰。将进样垫放入盛有正己烷的烧杯中，将进样垫放入盛有正己烷的烧杯中，放置放置1212小时。小时。将处理好的进样垫，自然晾干后，放将处理好的进样垫，自然晾干后，放入烘箱中入烘箱中120120度度2 2小时。小时。SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护 O O形圈形圈SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护O O 形圈分为两种适用于不同时使用温形圈分为两种适用于不同时使用温度度SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护玻璃衬管日常维护玻璃衬管SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护(Press the SYSTEM key)Select(Press the SYSTEM key)Select Analysis in the PF menu.The GC will be Analysis in the PF menu.The GC will be readied automatically readied automatically 选择选择 DIAG DIAG 中的中的“3.Analysis Counter3.Analysis Counter”从从中选择中选择“Counter for Insert Counter for Insert”并并 “ResetReset”键对计数器进行清空键对计数器进行清空SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护玻璃衬管的惰性化处理玻璃衬管的惰性化处理现象:某些农药的峰重现性差，有偏差。吸附，分解，峰变小。原因:进样口的玻璃衬管或石英棉活性过高，产生吸附、分解。DMCS(二甲基氯硅烷化)处理 玻璃衬管、石英棉用丙酮等有机溶剂清洗，凉干后在5%DMCS(二甲基二氯硅烷)/正已烷溶液中浸泡一夜。(2)取出浸泡一夜的玻璃衬管、石英棉，立即用甲醇清洗2、3次，然后再在甲醇中浸一小时左右。(3)从甲醇中取出，凉干后，放于干燥器中保存。SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护分子筛更换日常维护分子筛更换SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护日常维护SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护检测器日常维护检测器FIDFIDTCDTCDSHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护检测器日常维护检测器检查更换喷嘴检查更换喷嘴 所需工具所需工具 8mm 8mm 内六角套筒内六角套筒SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护检测器日常维护检测器降温并关闭机器降温并关闭机器SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护检测器日常维护检测器SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护检测器日常维护检测器SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护检测器日常维护检测器SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护检测器日常维护检测器SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护检测器日常维护检测器SHIMADZUSHIMADZUSHIMADZUSHIMADZUSolutions for Science Solutions for Science Solutions for Science Solutions for Science Since 1875Since 1875Since 1875Since 1875GC-2010 GC-2010 日常维护检测器日常维