气相色谱仪的基线不能调零有哪些主要的原因?

2025-02-16 14:43:08
推荐回答(2个)
回答1:

气相色谱仪点火后不能调零故障的原因有:离子室积水;极化电压接反;气路、检测器污染;柱流失严重;气流调节不当;基线补偿无作用。
气相色谱仪热导检测器基线不能调零故障的解决办法:
1 衰减挡试验
在发现基线相对于零点有一偏移时,将衰减挡由小到最大调整,观察基线偏离是否逐渐减小。
2 调零旋钮作用检查
分别旋动粗、中、细调旋钮,观察基线有否反应。
3 双路流量检查
在气路试漏的基础上,用皂膜流量计分别测试两气路的流量值,观察是否相差太大。
4 热丝电阻值间误差检查
对热导池各级热丝引出端插座进行电阻值测量。一般,各组热丝之间电阻值的差值不应超过0.2——0.5Ω,如超出此值,应按6处理。
5 热丝碰壁或沾污
热丝碰壁可通过测量热丝与池体之间的绝缘电阻加以证实。热丝的严重沾污,可通过对热导池池体的清洗而消除或部分消除。
6 热丝不对称或引线接错
如测得热丝组间电阻误差在0.5——3Ω之间,可用在热导调零电路的电阻两端并联电阻的方法加以解决;热丝不对称的另一种解决办法就是将电阻值最大者与最小者搭配成一组,电阻值中等的两个热丝配成一组,这样搭配后往往能更好地解决热导调零文档。
7 双路流量相差太大或气路泄漏的处理,两路流量相差过大,可通过调节气路控制阀加以解决,但此时两气路不应有泄漏。
8 调零电路有开路。
9 记录器开路或无反应。

回答2:

可能是柱子老化的不好,或检测器受污染
如果是高温段出杂峰很正常,本身就相当于烧柱子,除非你烧柱子的温度远大于高温段温度。还有就是样品较赃,进几个样就“烧”一下,也可有效防止杂峰的出现。
1.老化柱子
2.把柱子两端截掉一小段
如果仅仅是高温段有杂峰的话,估计不是检测器的问题
还应该是柱子
分流不分流进样口的话——
我的经验:不进样品,运行一次程升得到的基线谱图与样品谱图比较,看看高温段是否也有毛刺类杂峰,很简单如果没有说明是样品的问题,如果也有一样的杂峰说明是仪器或柱子问题。那么楼主已经老化过柱子了,问题仍然存在,说明问题在仪器上!然而问题到底在前面(汽化室)还是在后面(检测器)?
故障分析:注意,很多时候检测器是被冤枉的!同时衬管出问题可能性不大,一般是汽化室下端口分流板脏(镀金密封垫)和汽化室分流出口及分流管脏,即一些高聚物长期聚集的结果,所以使用分流时随着程升过程系统压力或流速的改变高温下的这些杂物就从柱子流出被检测到。
解决办法:1.清洗或更换镀金密封垫;2.疏通分流出口,清洗或更换分流管;3.系统地维护一次汽化室部分。

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