水中甲醇和丙酮的测定——气相色谱法毕业论文_生态学毕业论文

水中甲醇和丙酮的测定——气相色谱法毕业论文

2021-04-27更新

摘 要

工业生产中含有甲醇和丙酮的废水排入河流、湖泊会引起一系列的环境安全问题,随着工业的快速发展,水中甲醇和丙酮的监测越来越受到重视。本研究采用静态顶空气相色谱法,探讨了色谱柱、顶空条件、干扰物质对本方法的影响,从定性分析的角度对水中甲醇和丙酮的测定进行方法优化,主要研究结果如下:

1.毛细管色谱柱DB-624(30m×320m×1.8m)和DB-WAX(30m×320m×0.5m)

均能对水体中的甲醇和丙酮达到完全分离,峰形呈对称型。

2.顶空条件中,最佳平衡温度是80℃,最佳平衡时间是30min。

3. DB-WAX柱有更好的抗干扰性。选用的12种干扰物质中对甲醇和丙酮的测定干扰最强的是乙酸甲酯,5000mg/L以下四氢呋喃、500mg/L以下丙烯醛、1000mg/L以下二氯甲烷、25mg/L以下乙酸乙酯对甲醇和丙酮无干扰,其他物质正己烷、乙醛、二硫化碳、乙醇、乙腈、正丙醇和丙烯醇不会产生干扰。

关键词:甲醇;丙酮;静态顶空;气相色谱;水

Optimization of the method to analyze methanol and acetone in water by gas chromatography

ABSTRACT

Industrial waste containing methanol and acetone into rivers or lakes, raises a number of environmental safety problems, with the rapid development of industry, monitoring of methanol and acetone in water are more and more attention. This study,uses static headspace gas chromatography to discuss column, headspace conditions and interfering substances on the method, from the perspective of qualitative analysis to optimize the determination of methanol and acetone,in water,main findings are as follows:

1.Capillary column DB-624(30m×320m×1.8m)and DB-WAX(30m×320m×0.5m)is able to achieve complete separation of methanol and acetone in water, peak shape is symmetrical type.

2.On the headspace conditions, the optimal equilibrium temperature is 80 ℃, the optimal equilibrium time is 30min.

3.DB-WAX column has better immunity from the choice of 12 kinds of interfering substances,acetate has the strongest interference with the determination of methanol and acetone in water,5000mg / L or less tetrahydrofuran, 500mg / L or less acrolein, 1000mg / L or less methylene chloride, 25mg / L or less acetic acid Ethyl alcohol and acetone without interference, other substances n-hexane, acetaldehyde,carbon disulfide, ethanol, acetonitrile, n-propanol and allyl alcohol are not interfering.

Key words:methanol; acetone; static headspace; GC; water

目 录

1 前言………………………………………………………………………………………………………….1

1.1 研究背景………………………………………………………………………………………………………………………..1

1.2 国内外相关研究进展………………………………………………………………………………………………………2

1.3 气相色谱法及其应用………………………………………………………………………………………………………..3

1.3.1 气相色谱法简介……………………………………………………………………………………………………..3

1.3.2 顶空的原理…………………………………………………………………………………………………………….4

1.3.3 静态顶空气相色谱法的应用……………………………………………………………………………………4

1.4 研究目的及意义……………………………………………………………………………………………………………..5

2 材料与方法………………………………………………………………………………………………………………………………6

2.1 仪器与试剂………………………………………………………………………………………………………………………6

2.2 实验方案设计…………………………………………………………………………………………………………………6

2.2.1 气相色谱条件…………………………………………………………………………………………………………6

2.2.2 色谱柱的选择…………………………………………………………………………………………………………6

2.2.3 顶空条件的优化……………………………………………………………………………………………………..7

2.2.4 抗干扰性实验…………………………………………………………………………………………………………7

3 结果与分析………………………………………………………………………………………………………………………………9

3.1 色谱柱的选择…………………………………………………………………………………………………………………..9

3.2 顶空条件的优化……………………………………………………………………………………………………………11

3.2.1 平衡温度的确定……………………………………………………………………………………………………11

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