流动注射在甲醛分析检测中的应用
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摘要
随着人们环保意识加强和生活水平不断提高,食品卫生和室内环境质量越来越受到重视。深入研究甲醛的毒性、来源、产生机理以及检测方法,保护人体健康,已经成为当前研究的重点和热点之一。本文建立了分光光度法、化学发光法与流动注射结合的甲醛检测方法,详细地研究了反应条件等因素对检测方法的影响,探索了其在涂料甲醛分析中的应用。
第一章对甲醛的性质、毒性、来源和含量标准等做了相应介绍,总结了常见的甲醛的检测方法;并着重介绍了流动注射这种灵敏度高、分析速度快、省力、操作简便的技术;阐明了它与分光光度法及化学发光法联用的原理及在甲醛测定中的应用。
第二章主要对传统分光光度法进行了改进,采用了流动注射技术与分光光度法的结合,基于甲醛与3-甲基-2-苯并噻唑酮腙(简称酚试剂)反应生成嗪,嗪在酸性溶液中被高铁离子氧化形成蓝绿色化合物这一现象,以及该化合物颜色与甲醛浓度呈正相关关系,通过比色,对甲醛含量进行检测。这种方法既具有分光光度法选择性强、抗干扰能力强的特点,又具有流动注射分析方法速度快、耗用试剂少、操作简单的优点。
第三章利用了化学发光法的灵敏度高,检测下限低等优点,基于甲醛对没食子酸-过氧化氢-氢氧化钟(或氢氧化钠)化学发光体系有很强的增敏作用,并结合流动注射技术,据此建立测定微量甲醛的方法,设备简单,操作方便、快速、重现性好、线性范围较宽,避免了传统分析法的操作复杂,提高了分析样品的速率和精度,此方法已被应用于测定水性涂料中甲醛的含量。
In order to ensure healthy food supply, to improve the quality of indoor environment and to protect human health, it is quite important to study the toxicity, source, producing mechanism and the detection method of formaldehyde. In this paper, spectrophotometry and chemiluminescence combined with flow injection method for the determination of formaldehyde were carried out. The analytical conditions were optimized. Formaldehyde in coating was analyzed.
In chapter one, the characteristics, toxicity, sources and the concentraion standard of formaldehyde were briefly reviewed. Methods for formaldehyde analysis were summarized. Flow injection method and its application in spectrophotometry and chemiluminescenece were introduced.
In chapter two, a flow analysis system with spectrophometric detection for formaldehyde detemination was developed. The method was based on the reaction of formaldehyde with 3-methyl-2-benzothiazolinone hydrazone hydrochloride, which formed pyrazine that could be oxygened into bluish green compound by Fe~(3+) in acid solution. There was a positive correlation between the colour depth and the formaldehyde concentration. This method has the advantages of both spectrophotometry and flow injection such as simple, fast, high sensitivity, strong anti-interference capability and less consumption of reagents.
In chapter three, a modification of the Trautz-Schorigin reaction into a flow-injection analysis configuration was described. Different approaches were used at the optimization of chemiluminescence determination of formaldehyde in water based on the reaction of formaldehyde, gallic acid and hydrogen peroxide in an alkaline solution. Due to simple instrumentation, speed, reproducible, selectivity and sensitivity, the proposed FIA-CL method can be advantageously used for the routine determination of formaldehyde in the water-based coating.
第一章对甲醛的性质、毒性、来源和含量标准等做了相应介绍,总结了常见的甲醛的检测方法;并着重介绍了流动注射这种灵敏度高、分析速度快、省力、操作简便的技术;阐明了它与分光光度法及化学发光法联用的原理及在甲醛测定中的应用。
第二章主要对传统分光光度法进行了改进,采用了流动注射技术与分光光度法的结合,基于甲醛与3-甲基-2-苯并噻唑酮腙(简称酚试剂)反应生成嗪,嗪在酸性溶液中被高铁离子氧化形成蓝绿色化合物这一现象,以及该化合物颜色与甲醛浓度呈正相关关系,通过比色,对甲醛含量进行检测。这种方法既具有分光光度法选择性强、抗干扰能力强的特点,又具有流动注射分析方法速度快、耗用试剂少、操作简单的优点。
第三章利用了化学发光法的灵敏度高,检测下限低等优点,基于甲醛对没食子酸-过氧化氢-氢氧化钟(或氢氧化钠)化学发光体系有很强的增敏作用,并结合流动注射技术,据此建立测定微量甲醛的方法,设备简单,操作方便、快速、重现性好、线性范围较宽,避免了传统分析法的操作复杂,提高了分析样品的速率和精度,此方法已被应用于测定水性涂料中甲醛的含量。
In order to ensure healthy food supply, to improve the quality of indoor environment and to protect human health, it is quite important to study the toxicity, source, producing mechanism and the detection method of formaldehyde. In this paper, spectrophotometry and chemiluminescence combined with flow injection method for the determination of formaldehyde were carried out. The analytical conditions were optimized. Formaldehyde in coating was analyzed.
In chapter one, the characteristics, toxicity, sources and the concentraion standard of formaldehyde were briefly reviewed. Methods for formaldehyde analysis were summarized. Flow injection method and its application in spectrophotometry and chemiluminescenece were introduced.
In chapter two, a flow analysis system with spectrophometric detection for formaldehyde detemination was developed. The method was based on the reaction of formaldehyde with 3-methyl-2-benzothiazolinone hydrazone hydrochloride, which formed pyrazine that could be oxygened into bluish green compound by Fe~(3+) in acid solution. There was a positive correlation between the colour depth and the formaldehyde concentration. This method has the advantages of both spectrophotometry and flow injection such as simple, fast, high sensitivity, strong anti-interference capability and less consumption of reagents.
In chapter three, a modification of the Trautz-Schorigin reaction into a flow-injection analysis configuration was described. Different approaches were used at the optimization of chemiluminescence determination of formaldehyde in water based on the reaction of formaldehyde, gallic acid and hydrogen peroxide in an alkaline solution. Due to simple instrumentation, speed, reproducible, selectivity and sensitivity, the proposed FIA-CL method can be advantageously used for the routine determination of formaldehyde in the water-based coating.
引文
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[10]郑春生,王建清,杨南,景作亮.室内空气中甲醛的快速测定.北京工商大学学报.2004,22(4):8-11.
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