安捷伦液相色谱仪常见故障排除.docx

安捷伦液相色谱仪常见故障排除.docx

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安捷伦液相色谱仪常见故障排除

安捷伦液相色谱仪常见故障排除

液相色谱仪常见故障排除

HPLC故障排除

症状类型可能的原因解决方案

随机性,污染物积聚冲冲洗柱;净化样品;使用HPLC级溶剂

连续性,检测器灯故障更换紫外灯（寿命为1000小时）基线噪声大

偶然性,外部电气干扰使用LC系统专用稳压器

样品量过大进样量应为流动相进样量的1/6

样品量过大进样量应为流动相进样量的1/6

进样溶剂过强使用较弱的进样溶剂或流动相

更换并使用0.5μm孔隙率的在线过滤滤芯堵塞器

柱有空隙或气沟用玻璃珠或填料填充空隙;重填柱双峰

进样器流路不通畅更换进样器转子

柱头有空隙使用填料或玻璃珠填充柱顶部

使用更高负载量的固定相增加色谱柱柱上样品超载内径减少样品量

单峰,存在干扰性组分净化样品;预分离

开始出双峰请参见双峰

减少接头的数量确保进样器密封垫紧存在未扫的死体积密确保接头正确固定拖尾峰碱性化合物,硅醇相互作用换成聚合物固定相

使用更强的流动相或添加竞争碱（例如，碱性物质,硅醇相互作用三甲胺

硅胶基,柱降解使用特种色谱柱;聚合物柱或空间位阻

进样量过大降低进样溶剂的强度以集中溶质

进样阀中的峰扩散在进样前/后引入气泡以减少扩散

数据系统的采样速率过低增大采样

峰展宽

检测器时间常数低调节时间常数使之与峰宽匹配

流动相粘度过高提高柱温

检测器池容积过大使用尽可能小的池容积（系统中无热交formorethan60yearsofruralseniorpartymembercarefunds;Systemofregulatingtheactivitiesofgrass-rootspartyorganizations,andenhancethesenseofbelongingofgrass-rootspartymembers;Holdfasttoimplement"redcredit","redstake"twomajorprojectopportunities,strivetoexplorenewwaysofdevelopmentofvillagecollectiveeconomy,ruralcollectiveeconomyachievebreakthrough;AprogressreviewbytheSecretaryofthepartyworkofgrass-rootspartyorganizations,strengthenstheresponsibilityofgraspingpartybuilding,PartySecretary.Second,strengtheningtheconstructionofcleanandhonestGovernmentandfightagainstcorruption.Seriouslyimplementthehonestresponsibility,activelycarryouttheindependentCommissionagainstcorruptioninterviewsystem,increasetheleadershipandtheday-to-daysupervisionofpartymembersandcadresatalllevels,strengthenthenotWindsofspecialtreatment,treatmentof"laid-backluxuryandarrogance"and"three-pronged"problem,non-gang,nationalpublicofficers,servinginleadershippositionsisnotland,above-standardequippedwithbusesandcarsforprivatepurposes,andrecreationalcityofgifts,hospitality,luxuryandwaste,"emptiedtherating"specialrectificationwork.Adheretotherotwillbepunishing,corruptSu,and1village,4disciplinaryadministrativecadresandworkers.Threeistostrengthenpeacetocreateawork.Strengthensourcemanagement,adheretoprevention,focusingonprevention.Carryoutthe"bigreception,bigtour"campaign,petitioningforthecadresofthe

换器）

注射器体积过大减少进样量

保留时间长使用梯度洗脱或较强的流动相

单向阀泄漏更换单向

压力波动泵密封垫泄漏更换泵密封

微粒积聚过滤样品;在线过滤器;过滤流动相

微粒积聚过滤样品;在线过滤器;过滤流动相压力渐增

水/有机系统,缓冲液沉淀测试缓冲液-有机混合物;确保兼容性保留超出总渗透体积体积排阻,特异性相互作用添加流动相改性剂或更改溶剂

柱温不断变化使柱恒温;绝缘;保证实验室温度恒定

平衡时间不足以适应梯度洗脱要求，或等确信在溶剂改变或梯度结束后至少10

度洗脱流动相起变化个柱容积通过色谱柱

减少氦气的剧烈脱气;保持溶剂贮器盖流动相组分选择性蒸发好;制备新的流动相保留时间不断变动缓冲能力不足用>20mM浓度的缓冲液

保证梯度系统输送恒定组成;与手动制在线流动相混合不一致备流动相核对

污染积聚冲洗色谱柱以去除污染物

用浓样品进样冲洗柱，使其处于正常状最初几次进样—吸附在活性部位态

流速在增加检查泵以确保正确;否则需重调保留时间逐渐缩短柱上进样超载减少样品

键合固定相的流失保持流动相pH值在2-8.5间

解决液流中的漏液现象，更换泵密封垫，流速在减慢检查泵的涡流和气泡

硅胶填料的活化点使用流动相改性剂

键合固定相的流失保持流动相pH值在2-8.5间保留时间逐渐增加

流动相组成在变化确保流动相容器盖好

硅胶填料的活化点流动相中加竞争碱

硅胶填料的活化点固定相用更高覆盖度的填充料灵敏度问题峰位于检测器线性范围之外稀释或浓缩使之处于线性区内formorethan60yearsofruralseniorpartymembercarefunds;Systemofregulatingtheactivitiesofgrass-rootspartyorganizations,andenhancethesenseofbelongingofgrass-rootspartymembers;Holdfasttoimplement"redcredit","redstake"twomajorprojectopportunities,strivetoexplorenewwaysofdevelopmentofvillagecollectiveeconomy,ruralcollectiveeconomyachievebreakthrough;AprogressreviewbytheSecretaryofthepartyworkofgrass-rootspartyorganizations,strengthenstheresponsibilityofgraspingpartybuilding,PartySecretary.Second,strengtheningtheconstructionofcleanandhonestGovernmentandfightagainstcorruption.Seriouslyimplementthehonestresponsibility,activelycarryouttheindependentCommissionagainstcorruptioninterviewsystem,increasetheleadershipandtheday-to-daysupervisionofpartymembersandcadresatalllevels,strengthenthenotWindsofspecialtreatment,treatmentof"laid-backluxuryandarrogance"and"three-pronged"problem,non-gang,nationalpublicofficers,servinginleadershippositionsisnotland,above-standardequippedwithbusesandcarsforprivatepurposes,andrecreationalcityofgifts,hospitality,luxuryandwaste,"emptiedtherating"specialrectificationwork.Adheretotherotwillbepunishing,corruptSu,and1village,4disciplinaryadministrativecadresandworkers.Threeistostrengthenpeacetocreateawork.Strengthensourcemanagement,adheretoprevention,focusingonprevention.Carryoutthe"bigreception,bigtour"campaign,petitioningforthecadresofthe

最初几次进样—样品在样品池或柱中被用浓样品处理样品池/柱吸附自动进样器流路阻塞

自动进样器流路阻塞检查流量情况，确保无阻塞现象

进样器样品定量管未充满确保样品池中已充满样品

用内标法在制备样品，优化样品制备方在样品制品时有关的样品流失法柱平衡时间减慢（离长链离子对试剂平衡时间慢使用较短的烷链试剂子对现象）

液相基线噪音问题的排查思路

常见色谱故障——基线噪音

液相常见压力问题的原因分析

1.常见色谱故障——压力波动

可能的原因:

溶剂进口过滤芯堵塞

溶剂未脱气

泵的密封垫老化

出口单向阀失效

主动阀失效

最常见的原因是:

泵内有气泡

formorethan60yearsofruralseniorpartymembercarefunds;Systemofregulatingtheactivitiesofgrass-rootspartyorganizations,andenhancethesenseofbelongingofgrass-rootspartymembers;Holdfasttoimplement"redcredit","redstake"twomajorprojectopportunities,strivetoexplorenewwaysofdevelopmentofvillagecollectiveeconomy,ruralcollectiveeconomyachievebreakthrough;AprogressreviewbytheSecretaryofthepartyworkofgrass-rootspartyorganizations,strengthenstheresponsibilityofgraspingpartybuilding,PartySecretary.Second,strengtheningtheconstructionofcleanandhonestGovernmentandfightagainstcorruption.Seriouslyimplementthehonestresponsibility,activelycarryouttheindependentCommissionagainstcorruptioninterviewsystem,increasetheleadershipandtheday-to-daysupervisionofpartymembersandcadresatalllevels,strengthenthenotWindsofspecialtreatment,treatmentof"laid-backluxuryandarrogance"and"three-pronged"problem,non-gang,nationalpublicofficers,servinginleadershippositionsisnotland,above-standardequippedwithbusesandcarsforprivatepurposes,andrecreationalcityofgifts,hospitality,luxuryandwaste,"emptiedtherating"specialrectificationwork.Adheretotherotwillbepunishing,corruptSu,and1village,4disciplinaryadministrativecadresandworkers.Threeistostrengthenpeacetocreateawork.Strengthensourcemanagement,adheretoprevention,focusingonprevention.Carryoutthe"bigreception,bigtour"campaign,petitioningforthecadresofthe

2.常见色谱故障——压力过低可能的原因:

溶剂进口过滤芯堵塞,连接管路泄漏或其它备件（泵头

密封垫）

溶剂或流速改变

主动阀失灵

四元比例阀失灵

单向出口阀失灵

色谱柱失效（固定相流失）

3.常见色谱故障——压力过高可能的原因:

柱子进口过滤芯被污染,PURGE阀过滤芯被污染,色谱柱被污染

连接管路，尤其是针座毛

细管堵塞

进样器旋转密封阀被堵

塞

进样针或针座被阻塞formorethan60yearsofruralseniorpartymembercarefunds;Systemofregulatingtheactivitiesofgrass-rootspartyorganizations,andenhancethesenseofbelongingofgrass-rootspartymembers;Holdfasttoimplement"redcredit","redstake"twomajorprojectopportunities,strivetoexplorenewwaysofdevelopmentofvillagecollectiveeconomy,ruralcollectiveeconomyachievebreakthrough;AprogressreviewbytheSecretaryofthepartyworkofgrass-rootspartyorganizations,strengthenstheresponsibilityofgraspingpartybuilding,PartySecretary.Second,strengtheningtheconstructionofcleanandhonestGovernmentandfightagainstcorruption.Seriouslyimplementthehonestresponsibility,activelycarryouttheindependentCommissionagainstcorruptioninterviewsystem,increasetheleadershipandtheday-to-daysupervisionofpartymembersandcadresatalllevels,strengthenthenotWindsofspecialtreatment,treatmentof"laid-backluxuryandarrogance"and"three-pronged"problem,non-gang,nationalpublicofficers,servinginleadershippositionsisnotland,above-standardequippedwithbusesandcarsforprivatepurposes,andrecreationalcityofgifts,hospitality,luxuryandwaste,"emptiedtherating"specialrectificationwork.Adheretotherotwillbepunishing,corruptSu,and1village,4disciplinaryadministrativecadresandworkers.Threeistostrengthenpeacetocreateawork.Strengthensourcemanagement,adheretoprevention,focusingonprevention.Carryoutthe"bigreception,bigtour"campaign,petitioningforthecadresofthe

formorethan60yearsofruralseniorpartymembercarefunds;Systemofregulatingtheactivitiesofgrass-rootspartyorganizations,andenhancethesenseofbelongingofgrass-rootspartymembers;Holdfasttoimplement"redcredit","redstake"twomajorprojectopportunities,strivetoexplorenewwaysofdevelopmentofvillagecollectiveeconomy,ruralcollectiveeconomyachievebreakthrough;AprogressreviewbytheSecretaryofthepartyworkofgrass-rootspartyorganizations,strengthenstheresponsibilityofgraspingpartybuilding,PartySecretary.Second,strengtheningtheconstructionofcleanandhonestGovernmentandfightagainstcorruption.Seriouslyimplementthehonestresponsibility,activelycarryouttheindependentCommissionagainstcorruptioninterviewsystem,increasetheleadershipandtheday-to-daysupervisionofpartymembersandcadresatalllevels,strengthenthenotWindsofspecialtreatment,treatmentof"laid-backluxuryandarrogance"and"three-pronged"problem,non-gang,nationalpublicofficers,servinginleadershippositionsisnotland,above-standardequippedwithbusesandcarsforprivatepurposes,andrecreationalcityofgifts,hospitality,luxuryandwaste,"emptiedtherating"specialrectificationwork.Adheretotherotwillbepunishing,corruptSu,and1village,4disciplinaryadministrativecadresandworkers.Threeistostrengthenpeacetocreateawork.Strengthensourcemanagement,adheretoprevention,focusingonprevention.Carryoutthe"bigreception,bigtour"campaign,petitioningforthecadresofthe