摘要本文建立了一种环境空气中典型醛类化合物的气相色谱法(GC/ECD)分析方法。本方法探究了空气中甲醛、苯甲醛的采样、测定方法。采用自制的采样管,采样管内填充固体吸附剂硅胶,硅胶表面均匀涂布衍生剂五氟苯肼(PFPH),空气采样器与采样管连接进行采样及在线衍生反应。采样后用乙腈洗脱硅胶,洗脱液中加入内标物(对-氟苯甲醛)、催化剂(甲酸)后,经气相色谱检测分析。在选定的气相色谱条件下甲醛和苯甲醛的衍生物分离良好,该方法检出限低,精密度和准确度良好。59866
以300mL/min的采样速率采样30min,平均采样效率可达99%以上。甲醛的线性范围为0.814 μg/mL~81.4 μg/mL,检出限为19.8μg/L,标准曲线的相关系数为0.9985;苯甲醛的线性范围为0.1046μg/mL~10.46μg/mL,检出限为7.5μg/L,标准曲线的相关系数为0.9988。方法精密度为1.97%,加标回收率为88.2%~107.6%。
毕业论文关键词 甲醛 苯甲醛 衍生反应 采样管 气相色谱
毕业设计说明书(论文)外文摘要
Title Research on the Determination of Typical Airborne Aldehyde Compounds
Abstract A GC-based method for the determination of typical airborne aldehydes was developed in this paper. The sampling process and determination method of formaldehyde and benzaldenhyde were evaluated comprehensively. A new kind of sampling tube was invented with silica gel as the solid sorbent, which was coated with pentafluorophenyl hydrazine(PFPH) as the derivatizing agent. Therefore, the sampling process of formaldehyde and benzaldenhyde was accompanied with online derivatization. The silica gel was then eluted by acetonitrile after sampling, followed by the addition of catalyst HCOOH, internal standard 4-fluorobenzaldehyde and GC /ECD analysis of the PFPH –derivatives. Favorable separation of formaldehyde and benzaldenhyde, high precision and accuracy were obtained by the optimized GC-ECD method. Average collection Efficiency was above 99% with the sampling rate of 300mL/min and sampling time of 30min. There was a good linear range between 0.814μg/mL~81.4μg/mL with a detection limit of 19.8μg/L for formaldehyde, 0.1046μg/mL~10.46μg/mL with a detection limit of 7.5μg/L for benzaldenhyde. The correlation coefficient of calibration curves was 0.9985 for formaldehyde and 0.9988 for benzaldenhyde. Average precision and spike recovery of the method were 1.97% and 88.2%~107.6%, respectively.
Key words formaldehyde benzaldehyde derivatization agent sampling tubes GC/ECD
1 绪论 1
1.1 甲醛简介 1
1.1.1 甲醛的性质与用途 1
1.1.2 甲醛的来源 2
1.1.3 甲醛对人体健康的危害 2
1.2 苯甲醛简介 3
1.2.1 苯甲醛的性质和用途 3
1.2.2 苯甲醛的来源 4
1.2.3 苯甲醛的危害 4
1.3 环境空气中的醛类物质的检测方法 4
1.3.1 分光光度法 4
1.3.2 高效液相色谱法(HPLC) 5
1.3.3 气相色谱法 5
1.3.4 传感器技术法 5
1.4 小结 6
2 原理部分 7
2.1 衍生化反应原理