流动注射化学发光法测定环境水中有机污染物的研究
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摘要
流动注射化学发光法是化学发光分析和流动注射技术二者相联合而建立起来的一种快速痕量的分析方法。它是根据化学发光反应在某一时刻的发光强度来直接或间接测定待测物含量的。此方法具有灵敏度高、线性范围宽、分析速度快、重现性好、仪器设备和操作简单,易于实现自动化和连续分析等优点。目前,此方法被应用到环境监测、药物分析、临床化验、食品检验、工农业在线分析等领域,流动注射化学发光分析法是当前分析化学领域中研究的热点,其具有广阔的发展前景。
本论文主要研究了流动注射化学发光分析法对环境水样中污染物质和生活生产中有潜在危害的物质的测定。内容大致可分为以下两个部分:
1.分别简述了流动注射技术和化学发光分析法的原理、优点、发展史和发展趋势,介绍了流动注射和化学发光分析技术的实验装置和几种重要的化学发光试剂,以及流动注射化学发光分析法在环境中的应用。
2.利用流动注射化学发光分析技术对环境水样中的对甲氧基苯胺、2,4,6-三氯酚、三聚氰胺进行了比较详细的研究测定。
(1)流动注射化学发光法测定环境水样中的对甲氧基苯胺
研究发现,在酸性条件下,罗丹明B与甲醛能对高锰酸钾氧化对甲氧基苯胺有一定的曾敏作用,基于此,结合流动注射技术建立了一种间接测定对甲氧基苯胺的新方法。该方法线性范围为6.0×10~(-2)~1.0μg/mL,检出限3.3×10~(-2)μg/mL,对0.06μg/mL的对甲氧基苯胺测定的相对标准偏差为1.38%(n=11),该方法可用于环境水样中对甲氧基苯胺的测定,取得令人满意的结果。
(2)流动注射化学发光法测定环境中的三氯酚
碱性介质中, 2,4,6-三氯酚对鲁米诺-高锰酸钾体系有较强的曾敏作用,结合流动注射技术建立了测定氯酚类的化学发光分析法,本方法测定2,4,6-三氯酚的线性范围为0.11~1.1μg/mL,检出限为0.046μg/mL,对0.55μg/mL2,4,6-三氯酚进行连续测定,测定的相对标准偏差为1.24%(n=11),此方法可应用于环境水中2,4,6-三氯酚的分析测定,结果令人满意。
(3)流动注射化学发光分析法测定环境水体中的三聚氰胺
在碱性介质中,三聚氰胺对Luminol-H_2O_2化学发光体系有较强的抑制作用,据此采用流动注射技术建立了一种测定三聚氰胺的化学发光新方法,本方法在最优条件下测定三聚氰胺的线性范围为5.0×10~(-2) ~1.0μg/mL,检出限为1.07×10~(-3)μg/ mL,对0.1μg/mL三聚氰胺进行11次连续测定,测定的相对标准偏差为1.04%(n=11),该方法可应用于环境水样中三聚氰胺的测定,结果令人满意。
Flow- injection Chemiluminescence analysis (FI-CL) which is the combination of FIA with CL detection is a high sensitive trace method. It detects the concentration of the analyte according to the CL intensity at some points of certain chemiluminescence reaction.This analysis technique has so many advantages, such as high sensitivity, rapidity and reproducibility in signal detection, convenient apparatus and operation, easy to realize automatic and continuous analysis etc.nowadays, FI-CL has been applied to areas of environmental ,medicament analysis, clinic test, immunoassay, food analysis, analysis of dustry and agriculture online and so on.FI-CL has been researched in analytical chemistry recently,It has vast development foreground.
This thesis mainly focused on its applications of determination of environmental pollutants of waters with FI-CL. The paper includes two parts:1. It depicts the basic principle and advantages of CL, FIA and FI-CL, recent development of the research of FI-CL analysis. The paper summarized the familiar CL system and various CL reagent and the applications of FI-CL in the field of environmental analysis.2. In this paper, we mainly studied the FI-CL for determination of trace p-Anisidine, Melamine and Trichlorophenol in environmental water samples.
(1) Determination of p-anisidine in environmental water samples with Flow-Injection Chemiluminescence techicque.
In acidic medium, rhodamine and formaldehyde could enhance the intensity of chemiluminescence produced by the reaction between KMnO4 and p-anisidine, based on his phenomenon, combined with flow of injection, a simple and sensitive method for determination of p-anisidine was established, under the optimum condition, the concentration range of linear response was 6.0×10~(-2)~1.0μg/mL, the detection limit was 3.3×10~(-2)μg/mL with a relative standard deviation of 1.38% for the determination of 0.06μg/mL of p-anisidine (n=11), the method was used to detect the concentration of p-anisidine in water samples with satisfactory result.
(2) Determination of trace trichlorophenol in natural water using flow-injection chemiluminescence analysis
2,4,6-trichlorophenol could enhance the intensity of chemiluminescence produced by the reaction between KMnO4 and Luminol, a method for determination of trichlorophenol was established, under the optimum, the concentration range of linear response was 0.11~1.1μg/mL,the detection limit was 0.046μg/mL, a relative standard deviation is 1.24% for the determination of 0.55μg/mL of 2,4,6-trichlorophenol (n=11),the method was used to detect the concentration of 2,4,6-trichlorophenol in water samples with satisfactory result.
(3) Determination of trace melamine in environmental water samples using flow-injection chemiluminescence analysis
Based on the inhibition effect of melamine on the chemiluminescence generated from the Luminol-H_2O_2 reaction in alkaline medium, Under optimized conditions, the decrease of chemiluminescence intensity was linear with melamine concentration in the range of 5.0×10~(-2)～1.0μg/mL, and the limit of detection is 1.07×10~(-3)μg/mL, The relative standard deviation(n = 11)is 1.04% for 0.1μg/mL melamine, The method was applied to the determination of melamine in water samples with satisfactory results.
本论文主要研究了流动注射化学发光分析法对环境水样中污染物质和生活生产中有潜在危害的物质的测定。内容大致可分为以下两个部分:
1.分别简述了流动注射技术和化学发光分析法的原理、优点、发展史和发展趋势,介绍了流动注射和化学发光分析技术的实验装置和几种重要的化学发光试剂,以及流动注射化学发光分析法在环境中的应用。
2.利用流动注射化学发光分析技术对环境水样中的对甲氧基苯胺、2,4,6-三氯酚、三聚氰胺进行了比较详细的研究测定。
(1)流动注射化学发光法测定环境水样中的对甲氧基苯胺
研究发现,在酸性条件下,罗丹明B与甲醛能对高锰酸钾氧化对甲氧基苯胺有一定的曾敏作用,基于此,结合流动注射技术建立了一种间接测定对甲氧基苯胺的新方法。该方法线性范围为6.0×10~(-2)~1.0μg/mL,检出限3.3×10~(-2)μg/mL,对0.06μg/mL的对甲氧基苯胺测定的相对标准偏差为1.38%(n=11),该方法可用于环境水样中对甲氧基苯胺的测定,取得令人满意的结果。
(2)流动注射化学发光法测定环境中的三氯酚
碱性介质中, 2,4,6-三氯酚对鲁米诺-高锰酸钾体系有较强的曾敏作用,结合流动注射技术建立了测定氯酚类的化学发光分析法,本方法测定2,4,6-三氯酚的线性范围为0.11~1.1μg/mL,检出限为0.046μg/mL,对0.55μg/mL2,4,6-三氯酚进行连续测定,测定的相对标准偏差为1.24%(n=11),此方法可应用于环境水中2,4,6-三氯酚的分析测定,结果令人满意。
(3)流动注射化学发光分析法测定环境水体中的三聚氰胺
在碱性介质中,三聚氰胺对Luminol-H_2O_2化学发光体系有较强的抑制作用,据此采用流动注射技术建立了一种测定三聚氰胺的化学发光新方法,本方法在最优条件下测定三聚氰胺的线性范围为5.0×10~(-2) ~1.0μg/mL,检出限为1.07×10~(-3)μg/ mL,对0.1μg/mL三聚氰胺进行11次连续测定,测定的相对标准偏差为1.04%(n=11),该方法可应用于环境水样中三聚氰胺的测定,结果令人满意。
Flow- injection Chemiluminescence analysis (FI-CL) which is the combination of FIA with CL detection is a high sensitive trace method. It detects the concentration of the analyte according to the CL intensity at some points of certain chemiluminescence reaction.This analysis technique has so many advantages, such as high sensitivity, rapidity and reproducibility in signal detection, convenient apparatus and operation, easy to realize automatic and continuous analysis etc.nowadays, FI-CL has been applied to areas of environmental ,medicament analysis, clinic test, immunoassay, food analysis, analysis of dustry and agriculture online and so on.FI-CL has been researched in analytical chemistry recently,It has vast development foreground.
This thesis mainly focused on its applications of determination of environmental pollutants of waters with FI-CL. The paper includes two parts:1. It depicts the basic principle and advantages of CL, FIA and FI-CL, recent development of the research of FI-CL analysis. The paper summarized the familiar CL system and various CL reagent and the applications of FI-CL in the field of environmental analysis.2. In this paper, we mainly studied the FI-CL for determination of trace p-Anisidine, Melamine and Trichlorophenol in environmental water samples.
(1) Determination of p-anisidine in environmental water samples with Flow-Injection Chemiluminescence techicque.
In acidic medium, rhodamine and formaldehyde could enhance the intensity of chemiluminescence produced by the reaction between KMnO4 and p-anisidine, based on his phenomenon, combined with flow of injection, a simple and sensitive method for determination of p-anisidine was established, under the optimum condition, the concentration range of linear response was 6.0×10~(-2)~1.0μg/mL, the detection limit was 3.3×10~(-2)μg/mL with a relative standard deviation of 1.38% for the determination of 0.06μg/mL of p-anisidine (n=11), the method was used to detect the concentration of p-anisidine in water samples with satisfactory result.
(2) Determination of trace trichlorophenol in natural water using flow-injection chemiluminescence analysis
2,4,6-trichlorophenol could enhance the intensity of chemiluminescence produced by the reaction between KMnO4 and Luminol, a method for determination of trichlorophenol was established, under the optimum, the concentration range of linear response was 0.11~1.1μg/mL,the detection limit was 0.046μg/mL, a relative standard deviation is 1.24% for the determination of 0.55μg/mL of 2,4,6-trichlorophenol (n=11),the method was used to detect the concentration of 2,4,6-trichlorophenol in water samples with satisfactory result.
(3) Determination of trace melamine in environmental water samples using flow-injection chemiluminescence analysis
Based on the inhibition effect of melamine on the chemiluminescence generated from the Luminol-H_2O_2 reaction in alkaline medium, Under optimized conditions, the decrease of chemiluminescence intensity was linear with melamine concentration in the range of 5.0×10~(-2)～1.0μg/mL, and the limit of detection is 1.07×10~(-3)μg/mL, The relative standard deviation(n = 11)is 1.04% for 0.1μg/mL melamine, The method was applied to the determination of melamine in water samples with satisfactory results.
引文
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