CN105436144B - 氢火焰离子化检测器的清洗方法 - Google Patents

氢火焰离子化检测器的清洗方法 Download PDF

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CN105436144B
CN105436144B CN201510929692.2A CN201510929692A CN105436144B CN 105436144 B CN105436144 B CN 105436144B CN 201510929692 A CN201510929692 A CN 201510929692A CN 105436144 B CN105436144 B CN 105436144B
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陈艺琳
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Beijing Boya joint environmental protection technology Co., Ltd.
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Abstract

氢火焰离子化检测器的清洗方法，它包括以下步骤：（1）、切断氢气源，将色谱柱取下，用一根管子将进样口与检测器连接起来，通载气将检测器恒温箱升至100‑110℃；（2）、从进样口注入10‑14uL的重蒸水保温20‑30min；（3）、通入50‑60mL的丙酮‑氟利昂混合溶剂进行清洗，丙酮与氟利昂的体积比为1:3；（4）、排空检测器，从进样口注入体积比为2:1的甲醇‑苯混合液浸泡，超声清洗10‑20min；（5）、排空检测器，从进样口注入无水乙醇进行清洗5‑9min后排空检测器，通入氮气吹干检测器内部。本发明的有益效果是可得到清洁如初的氢火焰离子化检测器，延长其使用寿命，保证基线平稳度。

Description

氢火焰离子化检测器的清洗方法
技术领域
气体组分检测领域，尤其涉及气相色谱仪中氢火焰离子化检测器的清洗方法。
背景技术
气相色谱仪在石油、化工、生物化学、医药卫生、食品工业、环保等方面应用很广。它除用于定量和定性分析外，还能测定样品在固定相上的分配系数、活度系数、分子量和比表面积等物理化学常数。一种对混合气体中各组成分进行分析检测的仪器。气相色谱仪的型号种类繁多，但基本结构是一致的。它们都是由气路系统、进样系统、分离系统、检测系统、数据处理系统和温度控制系统六大部分组成。将分析样品在进样口中气化后，由载气带入色谱柱，通过对欲检测混合物中组分有不同保留性能的色谱柱，使各组分分离，依次导入检测器，以得到各组分的检测信号。按照导入检测器的先后次序，经过对比，可以区别出是什么组分，根据峰高度或峰面积可以计算出各组分含量。通常采用的检测器有：热导检测器，火焰离子化检测器，氦离子化检测器，超声波检测器，光离子化检测器，电子捕获检测器，火焰光度检测器，电化学检测器，质谱检测器等。
氢火焰离子化检测器使用一段时间后会产生污染，或是分析时的不当操作导致喷口、收集极形成洁碳和污染，导致噪声增大，收集效率降低从而影响使用，如果不进行及时的清洗会导致基线不平稳，影响正常检测。
发明内容
本发明要解决的技术问题是现有的氢火焰离子化检测器使用中会产生污染，没有系统的清洗方法，为此提供一种氢火焰离子化检测器的清洗方法。
本发明的技术方案是：氢火焰离子化检测器的清洗方法，它包括以下步骤：（1）、切断氢气源，将色谱柱取下，用一根管子将进样口与检测器连接起来，通载气将检测器恒温箱升至100-110℃；（2）、从进样口注入10-14uL的重蒸水保温20-30min；（3）、通入50-60mL的丙酮-氟利昂混合溶剂进行清洗，丙酮与氟利昂的体积比为1:3；（4）、排空检测器，从进样口注入体积比为2:1的甲醇-苯混合液浸泡，超声清洗10-20min；（5）、排空检测器，从进样口注入无水乙醇进行清洗5-9min后排空检测器，通入氮气吹干检测器内部。
本发明的有益效果是经过通入重蒸水进行初洗，再通入丙酮-氟利昂混合溶剂进行二次清洗、接着通入甲醇-苯混合液进行深度的超声清洗，可以有效的去除检测器内的各种污染物和杂质，最后使用氮气吹干即可得到清洁如初的氢火焰离子化检测器，延长其使用寿命，保证基线平稳度。
具体实施方式
下面结合实施例对本发明做进一步说明。
实施例1：氢火焰离子化检测器的清洗方法，它包括以下步骤：（1）、切断氢气源，将色谱柱取下，用一根管子将进样口与检测器连接起来，通载气将检测器恒温箱升至100℃；（2）、从进样口注入10uL的重蒸水保温20min；（3）、通入50mL的丙酮-氟利昂混合溶剂进行清洗，丙酮与氟利昂的体积比为1:3；（4）、排空检测器，从进样口注入体积比为2:1的甲醇-苯混合液浸泡，超声清洗10min；（5）、排空检测器，从进样口注入无水乙醇进行清洗5min后排空检测器，通入氮气吹干检测器内部。
实施例2：氢火焰离子化检测器的清洗方法，它包括以下步骤：（1）、切断氢气源，将色谱柱取下，用一根管子将进样口与检测器连接起来，通载气将检测器恒温箱升至105℃；（2）、从进样口注入12uL的重蒸水保温25min；（3）、通入55mL的丙酮-氟利昂混合溶剂进行清洗，丙酮与氟利昂的体积比为1:3；（4）、排空检测器，从进样口注入体积比为2:1的甲醇-苯混合液浸泡，超声清洗15min；（5）、排空检测器，从进样口注入无水乙醇进行清洗7min后排空检测器，通入氮气吹干检测器内部。
实施例3：氢火焰离子化检测器的清洗方法，它包括以下步骤：（1）、切断氢气源，将色谱柱取下，用一根管子将进样口与检测器连接起来，通载气将检测器恒温箱升至110℃；（2）、从进样口注入14uL的重蒸水保温30min；（3）、通入60mL的丙酮-氟利昂混合溶剂进行清洗，丙酮与氟利昂的体积比为1:3；（4）、排空检测器，从进样口注入体积比为2:1的甲醇-苯混合液浸泡，超声清洗20min；（5）、排空检测器，从进样口注入无水乙醇进行清洗9min后排空检测器，通入氮气吹干检测器内部。
氢火焰离子化检测器对烃类组分的检测灵敏度较高，使用时容易在检测器内部吸附烃类气体杂质，用一般的清洗方法无法有效去除，而使用过程中的各种误操作如色谱柱的固定相没有在最高使用温度下充分老化、气化室硅橡胶垫没有事先高温老化、FID收集极积水而绝缘下降、空气不足燃烧不完全等都会导致基线不稳定。
本发明利用重蒸水先对检测器内部进行大致的清洗，再通入体积比为1:3的丙酮-氟利昂混合溶剂，可以有效去除检测器内部的结碳和其它污染物，接着使用体积比为2:1的甲醇-苯混合液在超声环境下进行深度清洗，有效剥离检测器内壁死角吸附的污染物，最后通入无水乙醇和氮气进行后续清洗干燥，去除检测器内的微量烃类组分，维持基线的稳定。

Claims (1)

1.氢火焰离子化检测器的清洗方法，其特征是它包括以下步骤：（1）、切断氢气源，将色谱柱取下，用一根管子将进样口与检测器连接起来，通载气将检测器恒温箱升至100-110℃；（2）、从进样口注入10-14μ L 的重蒸水保温20-30min；（3）、通入50-60mL的丙酮-氟利昂混合溶剂进行清洗，丙酮与氟利昂的体积比为1:3；（4）、排空检测器，从进样口注入体积比为2:1的甲醇-苯混合液浸泡，超声清洗10-20min；（5）、排空检测器，从进样口注入无水乙醇进行清洗5-9min后排空检测器，通入氮气吹干检测器内部。
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1407337A (zh) * 2001-09-03 2003-04-02 株式会社资生堂 液相色谱系统、进样器、清洗装置和清洗方法
CN203621029U (zh) * 2013-11-08 2014-06-04 中国石油天然气股份有限公司 一种气相色谱分析用注射器清洗装置
CN204074619U (zh) * 2014-10-24 2015-01-07 王峰 一种色谱柱或保护柱超声清洗装置
CN104690047A (zh) * 2013-12-10 2015-06-10 中国科学院大连化学物理研究所 一种液相色谱进样通道清洗装置

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JP2012117945A (ja) * 2010-12-02 2012-06-21 Hitachi High-Technologies Corp 液体クロマトグラフ，液体クロマトグラフ用試料導入装置、および液体クロマトグラフ用試料導入装置の洗浄方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1407337A (zh) * 2001-09-03 2003-04-02 株式会社资生堂 液相色谱系统、进样器、清洗装置和清洗方法
CN203621029U (zh) * 2013-11-08 2014-06-04 中国石油天然气股份有限公司 一种气相色谱分析用注射器清洗装置
CN104690047A (zh) * 2013-12-10 2015-06-10 中国科学院大连化学物理研究所 一种液相色谱进样通道清洗装置
CN204074619U (zh) * 2014-10-24 2015-01-07 王峰 一种色谱柱或保护柱超声清洗装置

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