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 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0.5 μm 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equipment, components, equipment, temporary construction facilities, processed with strict compliance with provisions of construction floor plans, smooth roads and drainage, site formation. ----3, the site looks dignified and elegant and tidy, advertising slogans to write eye-catching appearance, walls to be clean and tidy. 4, "six-second figure"----cards to complete, custom, eye-catching, hanging in the obvious place. Management----5, district administration, "launch of Qing dynasty" focuses on managing the "cleaning, recycling, use," four Central Bank; the work is finished, clean, clear, work product protection in all procedures to periodically check the appraisals in a timely manner. 6, clean health----engineering work sites, temporary facilities clean and tidy inside and outside. 7, mechanical health----engineering machinery, vehicles are maintained in good condition, looks clean, and free from dirt, dust, electrical switchgear (box) complete with lock, mechanical safety protection equipment and complete, sensitive and reliable. 8, fire, defend----perfect fire system, set in accordance with requirements of fire equipment, set up obvious fire safety signs and signage, provide effective fire-fighting equipment, establishment of a security system, and out of the site staff to wear to work, marks and signs, implements 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>20 mM 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 equipment, components, equipment, temporary construction facilities, processed with strict compliance with provisions of construction floor plans, smooth roads and drainage, site formation. ----3, the site looks dignified and elegant and tidy, advertising slogans to write eye-catching appearance, walls to be clean and tidy. 4, "six-second figure"----cards to complete, custom, eye-catching, hanging in the obvious place. Management----5, district administration, "launch of Qing dynasty" focuses on managing the "cleaning, recycling, use," four Central Bank; the work is finished, clean, clear, work product protection in all procedures to periodically check the appraisals in a timely manner. 6, clean health----engineering work sites, temporary facilities clean and tidy inside and outside. 7, mechanical health----engineering machinery, vehicles are maintained in good condition, looks clean, and free from dirt, dust, electrical switchgear (box) complete with lock, mechanical safety protection equipment and complete, sensitive and reliable. 8, fire, defend----perfect fire system, set in accordance with requirements of fire equipment, set up obvious fire safety signs and signage, provide effective fire-fighting equipment, establishment of a security system, and out of the site staff to wear to work, marks and signs, implements 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 equipment, components, equipment, temporary construction facilities, processed with strict compliance with provisions of construction floor plans, smooth roads and drainage, site formation. ----3, the site looks dignified and elegant and tidy, advertising slogans to write eye-catching appearance, walls to be clean and tidy. 4, "six-second figure"----cards to complete, custom, eye-catching, hanging in the obvious place. Management----5, district administration, "launch of Qing dynasty" focuses on managing the "cleaning, recycling, use," four Central Bank; the work is finished, clean, clear, work product protection in all procedures to periodically check the appraisals in a timely manner. 6, clean health----engineering work sites, temporary facilities clean and tidy inside and outside. 7, mechanical health----engineering machinery, vehicles are maintained in good condition, looks clean, and free from dirt, dust, electrical switchgear (box) complete with lock, mechanical safety protection equipment and complete, sensitive and reliable. 8, fire, defend----perfect fire system, set in accordance with requirements of fire equipment, set up obvious fire safety signs and signage, provide effective fire-fighting equipment, establishment of a security system, and out of the site staff to wear to work, marks and signs, implements 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 equipment, components, equipment, temporary construction facilities, processed with strict compliance with provisions of construction floor plans, smooth roads and drainage, site formation. ----3, the site looks dignified and elegant and tidy, advertising slogans to write eye-catching appearance, walls to be clean and tidy. 4, "six-second figure"----cards to complete, custom, eye-catching, hanging in the obvious place. Management----5, district administration, "launch of Qing dynasty" focuses on managing the "cleaning, recycling, use," four Central Bank; the work is finished, clean, clear, work product protection in all procedures to periodically check the appraisals in a timely manner. 6, clean health----engineering work sites, temporary facilities clean and tidy inside and outside. 7, mechanical health----engineering machinery, vehicles are maintained in good condition, looks clean, and free from dirt, dust, electrical switchgear (box) complete with lock, mechanical safety protection equipment and complete, sensitive and reliable. 8, fire, defend----perfect fire system, set in accordance with requirements of fire equipment, set up obvious fire safety signs and signage, provide effective fire-fighting equipment, establishment of a security system, and out of the site staff to wear to work, marks and signs, implements equipment, components, equipment, temporary construction facilities, processed with strict compliance with provisions of construction floor plans, smooth roads and drainage, site formation. ----3, the site looks dignified and elegant and tidy, advertising slogans to write eye-catching appearance, walls to be clean and tidy. 4, "six-second figure"----cards to complete, custom, eye-catching, hanging in the obvious place. Management----5, district administration, "launch of Qing dynasty" focuses on managing the "cleaning, recycling, use," four Central Bank; the work is finished, clean, clear, work product protection in all procedures to periodically check the appraisals in a timely manner. 6, clean health----engineering work sites, temporary facilities clean and tidy inside and outside. 7, mechanical health----engineering machinery, vehicles are maintained in good condition, looks clean, and free from dirt, dust, electrical switchgear (box) complete with lock, mechanical safety protection equipment and complete, sensitive and reliable. 8, fire, defend----perfect fire system, set in accordance with requirements of fire equipment, set up obvious fire safety signs and signage, provide effective fire-fighting equipment, establishment of a security system, and out of the site staff to wear to work, marks and signs, implements