流动注射化学发光体系测定化学需氧量和有机磷农药残留的分析研究
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摘要
本论文分为两部分：综述和研究报告。综述部分对化学需氧量(COD)测定方法作了简要综述，内容涉及标准法、光度法、电化学法、火焰原子吸收法和其它测定方法的研究进展，最后对化学需氧量快速测定作了展望。研究报告包括三个方面：一、流动注射化学发光法快速测定化学需氧量(重铬酸钾法)；二、流动注射化学发光法快速测定化学需氧量(高锰酸钾法)；三、流动注射化学发光法测定有机磷农药残留。
第二部分研究报告
一、流动注射化学发光法快速测定化学需氧量—重铬酸钾法
基于酸性从cr20:在消解水体中的有机污染物时被还原为cr(m)，而Cr(m)
可以催化Luminol一HZO:体系产生强的化学发光，建立了一种测定COD的流动
注射化学发光法。本方法不需要催化剂，不需要长的消解时间，可以采用较低
的酸度，适合于在线连续检测水体COD。本方法检测COD的线性范围为
20一l000omg/L，检测限为10mg/L，对20mg/L COD的11次平行测定的RsD小
于5%，己成功应用于地表水样COD的测定。
二、流动注射化学发光法快速测定化学需氧量—高锰酸钾法
基于酸性KMno4被水体中的还原性物质还原为Mn(H)，而Mn(n)可以催
化Luminof一HZO:体系产生强的化学发光，建立了一种快速测定COD的流动注
射化学发光新方法。在本体系中，为了将KMnO;和Mn( 11)分开，采用了一个
强酸性阳离子微交换柱将Mn(ll)富集起来，待KMn04通过比微交换柱流走后，
再用洗脱剂将Mn(n)洗脱下来。该法测定COD的线性范围为4~4 00Omg/L，检测
限Zmg/L，整个过程(包括洗脱和采样)为1 .smin，每小时可测4。个样。对
10 mg/L的CoDll次平行测定的RSD为4.4%。该法不需要催化剂，不需要长
的消解时间，可以采用较低的酸度，而且快速、自动化程度高，适于在线连续
测定水体COD值，己成功用于水样COD的测定。
三、流动注射化学发光法测定有机磷农药残留
基于过硫酸钾在紫外光催化下可将有机磷消解为正磷酸盐，而正磷酸盐在
酸性条件下可与铝酸盐、钒酸盐形成具有氧化性的磷铝钒杂多酸，其可直接氧
化碱性鲁米诺产生强的化学发光，本文结合流动注射技术，提出了一种测定有机
磷农药残留的化学发光新方法，其线性范围为1.0x10’9一1.oxlo一sg/mL，检出限
为8.0xl0’1。岁mL。对2.ox10-v创mL的磷进行11次平行测定，其RsD为4.8%。
This thesis includes two parts. In part one, the recent development of the analytical methods of chemical oxygen demand is reviewed. The review involves the development of the spectrometry, the electrochemistry, the flame atomic absorption spectrometry and other analysis means. The research reports are focused on: (1)Chemiluminescence rapid determination of aquatic COD with flow injection analysis (the K2Cr2O7 method); (2) Chemiluminescence system for automatic determination of chemical oxygen demand using flow injection analysis (the KMnO4 method); (3) Chemiluminescence rapid determination of Organophosphorous pesticides with flow injection analysis.
Part One Summary The development of the analysis of chemical oxygen demand
In all kinds of contaminates, the organic contaminate is the fastest increasing and most serious one, Chemical Oxygen Demand (COD) is just the comprehensive index to valuate the degree of organic pollution. It's also the important parameter in supervising the water quality. COD is defined as the amount of oxygen equivalents consumed in the oxidation of organic compounds by strong oxidants (such as dichromate, permanganate), represents the total pollutants load of most wastewater discharges (it should be converted into oxygen's mass concentration (mg/L)). And it will be rather meaningful for water pollution preventing and supervising to grasping and controlling the amount of COD of water in time. This review introduces different methods of the determination of COD value, especially by spectrometry, electrochemistry, flame atomic absorption spectrometry and other analysis means. The procedures of the evaluation COD methods are complicated, and not suitable for analyzing the batch samples and monitoring on line
.
Flow-injection Chemiluminescence (CL) is known to be a powerful analytical technique that promises high sensitivity, wide linear range, simple instrumentation, and rapid, reproducible means of detection, and has been applied successfully to the determination of many environmental pollutants. In this paper, tow simple CL system
for on-line determination of COD using flow injection analysis is proposed.
Part Two Research Reports 1% Chemiluminescence Rapid Determination of Aquatic COD With Flow Injection
Analysis
A novel chemiluminescence (CL) combined with flow injection system for rapid determination of chemical oxygen demand (COD) of aquatic system is described in this paper. It is based on that the acidic K2Cr2O7 can be reduced into Cr(III)by reducible matter in the water, and the generated Cr(III)can catalyze the luminol- H2O2 system to produce the strong CL emission. In this method, the reduction reaction does not need other catalyzer and analysis can be completed on-line. The linear range is 20-10000 mg/L with the detection limit of 10mg/L. The system has been applied to determine the COD of the water sample with satisfactory results.
2 , Chemiluminescence System for Automatic Determination of Chemical Oxygen Demand Using Flow Injection Analysis
A novel chemiluminescence (CL) system for automatic determination of chemical oxygen demand (COD) combined with flow injection analysis is proposed in this paper. In this system, potassium permanganate is reduced to Mn2+ which is first adsorbed on a strongly acid cation-exchange resin mini-column to be concentrated during chemical oxidation of the organic compounds at room temperature, while the excessive MnO4- passes through the mini-column to be waste, then the concentrated Mn2+ is eluted reversely and measured by the luminol-H2O2 CL system. The calibration graph is linear in the range of 4-4000 mg /Land the detection limit is 2 mg/L. A complete analysis could be performed in 1.5 min including washing and sampling, giving a throughout of about 40/h. The relative standard deviation was 4A% for 10 mg/L COD (n=11), This CL flow system for determination of COD is very simple, rapid and suitable for automatic and continuous analysis. The presented system has been applied successfully to the determination of COD of water samples.
第二部分研究报告
一、流动注射化学发光法快速测定化学需氧量—重铬酸钾法
基于酸性从cr20:在消解水体中的有机污染物时被还原为cr(m)，而Cr(m)
可以催化Luminol一HZO:体系产生强的化学发光，建立了一种测定COD的流动
注射化学发光法。本方法不需要催化剂，不需要长的消解时间，可以采用较低
的酸度，适合于在线连续检测水体COD。本方法检测COD的线性范围为
20一l000omg/L，检测限为10mg/L，对20mg/L COD的11次平行测定的RsD小
于5%，己成功应用于地表水样COD的测定。
二、流动注射化学发光法快速测定化学需氧量—高锰酸钾法
基于酸性KMno4被水体中的还原性物质还原为Mn(H)，而Mn(n)可以催
化Luminof一HZO:体系产生强的化学发光，建立了一种快速测定COD的流动注
射化学发光新方法。在本体系中，为了将KMnO;和Mn( 11)分开，采用了一个
强酸性阳离子微交换柱将Mn(ll)富集起来，待KMn04通过比微交换柱流走后，
再用洗脱剂将Mn(n)洗脱下来。该法测定COD的线性范围为4~4 00Omg/L，检测
限Zmg/L，整个过程(包括洗脱和采样)为1 .smin，每小时可测4。个样。对
10 mg/L的CoDll次平行测定的RSD为4.4%。该法不需要催化剂，不需要长
的消解时间，可以采用较低的酸度，而且快速、自动化程度高，适于在线连续
测定水体COD值，己成功用于水样COD的测定。
三、流动注射化学发光法测定有机磷农药残留
基于过硫酸钾在紫外光催化下可将有机磷消解为正磷酸盐，而正磷酸盐在
酸性条件下可与铝酸盐、钒酸盐形成具有氧化性的磷铝钒杂多酸，其可直接氧
化碱性鲁米诺产生强的化学发光，本文结合流动注射技术，提出了一种测定有机
磷农药残留的化学发光新方法，其线性范围为1.0x10’9一1.oxlo一sg/mL，检出限
为8.0xl0’1。岁mL。对2.ox10-v创mL的磷进行11次平行测定，其RsD为4.8%。
This thesis includes two parts. In part one, the recent development of the analytical methods of chemical oxygen demand is reviewed. The review involves the development of the spectrometry, the electrochemistry, the flame atomic absorption spectrometry and other analysis means. The research reports are focused on: (1)Chemiluminescence rapid determination of aquatic COD with flow injection analysis (the K2Cr2O7 method); (2) Chemiluminescence system for automatic determination of chemical oxygen demand using flow injection analysis (the KMnO4 method); (3) Chemiluminescence rapid determination of Organophosphorous pesticides with flow injection analysis.
Part One Summary The development of the analysis of chemical oxygen demand
In all kinds of contaminates, the organic contaminate is the fastest increasing and most serious one, Chemical Oxygen Demand (COD) is just the comprehensive index to valuate the degree of organic pollution. It's also the important parameter in supervising the water quality. COD is defined as the amount of oxygen equivalents consumed in the oxidation of organic compounds by strong oxidants (such as dichromate, permanganate), represents the total pollutants load of most wastewater discharges (it should be converted into oxygen's mass concentration (mg/L)). And it will be rather meaningful for water pollution preventing and supervising to grasping and controlling the amount of COD of water in time. This review introduces different methods of the determination of COD value, especially by spectrometry, electrochemistry, flame atomic absorption spectrometry and other analysis means. The procedures of the evaluation COD methods are complicated, and not suitable for analyzing the batch samples and monitoring on line
.
Flow-injection Chemiluminescence (CL) is known to be a powerful analytical technique that promises high sensitivity, wide linear range, simple instrumentation, and rapid, reproducible means of detection, and has been applied successfully to the determination of many environmental pollutants. In this paper, tow simple CL system
for on-line determination of COD using flow injection analysis is proposed.
Part Two Research Reports 1% Chemiluminescence Rapid Determination of Aquatic COD With Flow Injection
Analysis
A novel chemiluminescence (CL) combined with flow injection system for rapid determination of chemical oxygen demand (COD) of aquatic system is described in this paper. It is based on that the acidic K2Cr2O7 can be reduced into Cr(III)by reducible matter in the water, and the generated Cr(III)can catalyze the luminol- H2O2 system to produce the strong CL emission. In this method, the reduction reaction does not need other catalyzer and analysis can be completed on-line. The linear range is 20-10000 mg/L with the detection limit of 10mg/L. The system has been applied to determine the COD of the water sample with satisfactory results.
2 , Chemiluminescence System for Automatic Determination of Chemical Oxygen Demand Using Flow Injection Analysis
A novel chemiluminescence (CL) system for automatic determination of chemical oxygen demand (COD) combined with flow injection analysis is proposed in this paper. In this system, potassium permanganate is reduced to Mn2+ which is first adsorbed on a strongly acid cation-exchange resin mini-column to be concentrated during chemical oxidation of the organic compounds at room temperature, while the excessive MnO4- passes through the mini-column to be waste, then the concentrated Mn2+ is eluted reversely and measured by the luminol-H2O2 CL system. The calibration graph is linear in the range of 4-4000 mg /Land the detection limit is 2 mg/L. A complete analysis could be performed in 1.5 min including washing and sampling, giving a throughout of about 40/h. The relative standard deviation was 4A% for 10 mg/L COD (n=11), This CL flow system for determination of COD is very simple, rapid and suitable for automatic and continuous analysis. The presented system has been applied successfully to the determination of COD of water samples.
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