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气相色谱仪的分流条件设置1有EPC系统的气相的分流条件设置(智能设置)2无EPC系统的气相的分流条件设置(手动设置)3案例讲解(以福立GC9790为例)1有EPC系统的气相的分流条件设置(智能设置)安捷伦6890、7890及岛津2010等高端气相的核心技术在于EPC系统的应用!1页带EPC系统气相(6890)分流/不分流进样口–部件进样垫衬管衬管O-圈镀金密封垫毛细管柱2页SeptumSEPTUMPURGEVENTInletSplitPort带EPC系统气相(6890)分流/不分流进样口–部件(进样口+EPC)3页FLOWSENSORPROPORTIONALVALVE1PRESSURESENSORSEPTUMPURGEREGULATORPURGEVALVEOPENTOTALFLOWCONTROLLOOPSPLITVENTGOLDSEALINPUTPRESSUREPROPORTIONALVALVE280PSI0ML/MINSPLITVENTTRAP0PSI带EPC系统气相(6890)分流动画–缺省条件4页FLOWSENSORPROPORTIONALVALVE1PRESSURESENSORSEPTUMPURGEREGULATORPURGEVALVEOPENTOTALFLOWCONTROLLOOPSPLITVENT205ML/MINGOLDSEALINPUTPRESSUREPROPORTIONALVALVE280PSIPRIMARYFLOWPATHREDUCEDFLOWPATH205ML/MINSPLITVENTTRAP0PSI带EPC系统气相(6890)分流动画–总流量设定5页FLOWSENSORPROPORTIONALVALVE1PRESSURESENSORSEPTUMPURGEREGULATORFIXED@3ML/MINPURGEVALVEOPENTOTALFLOWCONTROLLOOPGOLDSEALINPUTPRESSUREPROPORTIONALVALVE280PSIPRIMARYFLOWPATHREDUCEDFLOWPATH205ML/MINSPLITVENTTRAP10PSISPLITVENT200ML/MINCOLUMNFLOW2ML/MINPRESSURIZEDGASBACKPRESSURECONTROLLOOP带EPC系统气相(6890)分流动画–进样口压力设定6页FLOWSENSORPROPORTIONALVALVE1PRESSURESENSORSEPTUM(隔垫)PURGEREGULATOR(调节器)FIXED@3ML/MINPURGEVALVEOPENTOTALFLOWCONTROLLOOPINPUTPRESSUREPROPORTIONALVALVE280PSI205ML/MINSPLITVENTTRAP针阀前压强10PSISPLITVENT200ML/MINCOLUMNFLOW2ML/MINBACKPRESSURECONTROLLOOPSplitRatio-100:1Mode:SplitTemp250250Pressure10.010.0SplitRatio100SplitFlow200TotFlow205.0205.0GasSaverOFF压力感应器感知压强变化,传导给分流出口压力控制器,控制器改变针型阀开合的程度,继而控制进样衬管内和分流出口的压强差,如图所示:进样口为80PSI(此高压可以将气体以2mlmin压入色谱柱),分流出口为10PSI(此低压以200mlmin分流大量的气体);需要将流速调为1mlmin时,恒流阀1与流速传感器联动,智能调节总流量至104mlmin,然后恒流阀2与压力感应器联动,智能调节分流比为100:1,使色谱柱流量变为1mlmin。而低端气相仅调节针型阀的闭合程度:有时闭合度过小,导致压差太大,分流比过高;有时则反之。仪器无法自动感知压强变化,只能人工盲目调节。带EPC系统气相(6890)分流动画–准备进样分流与吹扫切换阀,在不分流模式下使用。7页FLOWSENSORPROPORTIONALVALVE1PRESSURESENSORSEPTUMPURGEREGULATORFIXED@3ML/MINPURGEVALVEOPENTOTALFLOWCONTROLLOOPGOLDSEALINPUTPRESSUREPROPORTIONALVALVE280PSI205ML/MINSPLITVENTTRAP10PSISPLITVENT200ML/MINCOLUMNFLOW2ML/MINBACKPRESSURECONTROLLOOPSplitRatio-100:1带EPC系统气相(6890)分流动画–插针8页FLOWSENSORPROPORTIONALVALVE1PRESSURESENSORSEPTUMPURGEREGULATORFIXED@3ML/MINPURGEVALVEOPENTOTALFLOWCONTROLLOOPGOLDSEALINPUTPRESSUREPROPORTIONALVALVE280PSI205ML/MINSPLITVENTTRAP10PSISPLITVENT200ML/MINCOLUMNFLOW2ML/MINBACKPRESSURECONTROLLOOPSplitRatio-100:1带EPC系统气相(6890)分流动画–进样9页FLOWSENSORPROPORTIONALVALVE1PRESSURESENSORSEPTUMPURGEREGULATORFIXED@3ML/MINPURGEVALVEOPENTOTALFLOWCONTROLLOOPGOLDSEALINPUTPRESSUREPROPORTIONALVALVE280PSI205ML/MINSPLITVENTTRAP10PSISPLITVENT200ML/MINCOLUMNFLOW2ML/MINBACKPRESSURECONTROLLOOPSplitRatio-100:1GlassWool带EPC系统气相(6890)分流动画–样品蒸发10页FLOWSENSORPROPORTIONALVALVE1PRESSURESENSORSEPTUMPURGEREGULATORFIXED@3ML/MINPURGEVALVEOPENTOTALFLOWCONTROLLOOPINPUTPRESSUREPROPORTIONALVALVE280PSI205ML/MINSPLITVENTTRAP10PSISPLITVENT200ML/MINCOLUMNFLOW2ML/MINBACKPRESSURECONTROLLOOPSplitRatio-100:1SmallerO.D.LinerOpenSplitFlowPathGlassPositioningBeadGlassWoolTaperedLinerAgilentSplitLiner-5183-4647带EPC系统气相(6890)分流动画–良好的衬管设计?11页FLOWSENSORPROPORTIONALVALVE1PRESSURESENSORSEPTUMPURGEREGULATORFIXED@3ML/MINPURGEVALVEOPENTOTALFLOWCONTROLLOOPINPUTPRESSUREPROPORTIONALVALVE280PSI205ML/MINSPLITVENTTRAP10PSISPLITVENT200ML/MINCOLUMNFLOW2ML/MINBACKPRESSURECONTROLLOOPSplitRatio-100:1带EPC系统气相(6890)分流动画–分流继续12页FLOWSENSORPROPORTIONALVALVE1PRESSURESENSORSEPTUMPURGEREGULATORFIXED@3ML/MINPURGEVALVEOPENTOTALFLOWCONTROLLOOPINPUTPRESSUREPROPORTIONALVALVE280PSI205ML/MINSPLITVENTTRAP10PSISPLITVENT200ML/MINCOLUMNFLOW2ML/MINBACKPRESSURECONTROLLOOPSplitRatio-100:1带EPC系统气相(6890)分流动画–分流完成13页FLOWSENSORPROPORTIONALVALVE1PRESSURESENSORSEPTUMPURGEREGULATORFIXED@3ML/MINPURGEVALVEOPENTOTALFLOWCONTROLLOOPINPUTPRESSUREPROPORTIONALVALVE280PSI205ML/MINSPLITVENTTRAP10PSISPLITVENT200ML/MINCOLUMNFLOW2ML/MINBACKPRESSURECONTROLLOOPSplitRatio-100:1带EPC系统气相(6890)分流动画–样品分离并检测14页FLOWSENSORPROPORTIONALVALVE1PRESSURESENSORSEPTUMPURGEREGULATORFIXED@3ML/MINPURGEVALVEOPENTOTALFLOWCONTROLLOOPINPUTPRESSUREPROPORTIONALVALVE280PSI55ML/MINSPLITVENTTRAP10PSISPLITVENT50ML/MINCOLUMNFLOW2ML/MINBACKPRESSURECONTROLLOOPSplitRatio-100:1Mode:SplitTemp250250Pressure10.010.0SplitRatio100SplitFlow200TotFlow205.0205.0GasSaverONSaverFlow50.0SaverTime0.5带EPC系统气相(6890)分流动画–在进样完成后,省气模式–设定55ml/min返回目录15页2无EPC系统的气相的分流条件设置(手动设置)福立9790等低端气相没有配置EPC系统,因而价格低廉,但是分流设置繁琐且不易实现准确控制。下文所示的压强和流速数值,仅用于示例讲解,不是实际数值!!!16页无EPC系统气相(福立9790)分流动画–总流路图17页无EPC系统气相(福立9790)分流动画–各部分设置(步骤1)240PSI先用稳压阀调节总压(步骤4)?10PSI,压差70PSI?200ml/min由开到关调节,最终闭合程度小(步骤6)?70PSI,压差6PSI?3ml/min由关到开调节,最终闭合程度大(步骤3)?78PSI,压差4PSI?2ml/min被动调节•安捷伦、岛津等需要输入色谱柱规格信息,EPC系统计算得出隔垫吹扫、分流出口特定流速需要的合适压强,然后根据压力传感器的反馈信息不断调节针型阀使其达到所需的流速和分流比。低端气相无法实现此功能!!!(步骤2)100PSI,压差140PSI?225ml/min再用稳流阀确定合适的总流量(步骤5)?此处70PSI,压差20PSI?20ml/min由关到开调节,最终闭合程度大较低压差(40PSI)下从总氮气流量中分走较少的流量。18页无EPC系统气相(其他型号-独立尾吹管路,类似于6890)分流动画–各部分设置(步骤1)210PSI先用稳压阀调节总压(步骤6)?74PSI,压差6PSI?3ml/min阀门闭合程度大(步骤4)?10PSI,压差70PSI?200ml/min阀门闭合程度小(步骤3)?76PSI,压差4PSI?2ml/min被动调节安捷伦、岛津等需要输入色谱柱规格信息,EPC系统计算得出隔垫吹扫、分流出口特定流速需要的合适压强,然后根据压力传感器的反馈信息不断调节针型阀使其达到所需的流速和分流比。低端气相无法实现此功能!!!(步骤2)80PSI,压差130PSI?205ml/min再用稳流阀确定合适的总流量(步骤5)?此处160PSI,压差80PSI?20ml/min阀门闭合程度大较低压差(40PSI)下从总氮气流量中分走较少的流量。返回目录1
本文标题:技能培训-3-20170211-无EPC的气相色谱仪的流速、分流比、隔垫吹扫及尾吹气的设置
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