复合汞膜溶出伏安法在环境、食品中的分析应用研究
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摘要
人体的健康与微量元素的含量有着密切的关系。简便、快速、灵敏、干扰少的微量元素定量分析方法在环境科学、药品、食品及临床分析中具有重要的作用。化学修饰电极是70年代发展起来的一门新兴技术,它也是目前最活跃的电化学和电分析化学的前沿领域之一。在制备修饰电极的诸多材料中,以普鲁士蓝为代表的多核金属铁氰化物因其良好的化学和电化学稳定性,在包括催化、电化学传感器、功能材料、离子识别、固态电池和分子磁性物质等方面得到了广泛的应用。我们结合类普鲁士蓝修饰电极和传统汞膜电极的优点,在玻璃碳基质上进行了新型铕离子掺杂类普类鲁士蓝复合汞膜电极的制备并开展了一些分析应用研究。本文创新点是利用电化学沉积法制备的铕离子掺杂类普鲁士蓝复合汞膜电极建立了环境样品中铅、镉、铜、铋及维生素B_2的测定方法。该电极所呈现的显著特点是灵敏度高、稳定性好、抗干扰能力强和使用寿命长等优点,具有潜在的应用价值,测定结果令人满意。
论文的主要研究内容包括以下四部分:
第一章综述
第一节概述了复合汞膜的发展历史和概况,对化学修饰型复合汞膜电极的制备方法及应用进行了简单介绍;第二节概述了溶出分析技术的分类及其应用,并对阳极溶出伏安法和阴极溶出伏安法进行了重点介绍;第三节对使用阳极溶出伏安法检测环境样品中重金属离子的分析应用进行了综述;第四节对食品中的水溶性维生素成份的性质进行了简介,并重点综述了电化学方法测定食品中水溶性维生素的方法。最后介绍了本论文的研究目的和意义。这部分共引用文献100篇。
第二章复合汞膜阳极溶出法检测城市绿化树叶上的附着铅
采用示差脉冲阳极溶出伏安法对城市绿化树叶上附着铅的含量进行了检测,并根据测得结果分析了树叶上附着铅的主要污染来源。结果表明:采用新型铕离子掺杂类普鲁士蓝复合汞膜电极(PB-Eu/MFE)为工作电极,在0.01mol/L HNO_3底液中,铅离子于-0.472V(vs.SCE)处产生一个灵敏的阳极溶出峰。在最佳实验条件下,其溶出峰电流与铅的浓度在2.4～300μg/L(r=0.9991,n=11)之间呈良好的线性关系,检测下限为0.2μg/L(S/N=3),RSD为1.35%。用该法检测了兰州市三个不同采集地点的城市绿化白蜡树叶上的附着铅含量,回收率为97.3%～102%。由测定结果可知汽车尾气污染是树叶上附着铅的重要来源,附着铅的含量与邻近交通要道的车流量之间有正相关性。
第三章复合汞膜阳极溶出法检测废电池中的铋铜铅镉
本文建立了用示差脉冲阳极溶出伏安法同时测定废旧电池中铋铜铅镉的方法。结果表明:采用新型铕离子掺杂普鲁士蓝复合汞膜电极(PB-Eu/MFE)为工作电极,在1M KCl-10%乳酸底液中,铋铜铅镉离子分别于-0.21V、-0.34V、-0.55V、-0.75V(vs.SCE)处产生灵敏的阳极溶出峰。在最佳实验条件下,其溶出峰电流与浓度(μg/L)分别在4.0～160(r=0.9986,n=8),2.0～160(r=0.9992,n=8),2.0～240(r=0.9990,n=8),8.0～360(r=0.9989,n=8)之间呈良好的线性关系;检测下限分别为0.4μg/L、0.4μg/L、0.2μg/L、0.6μg/L(S/N=3);RSD分别为3.80%、3.61%、2.37%、3.88%。用该法实测了四种不同品牌的废旧电池中这四种金属的含量,回收率为97.4%～104%。本法操作简便、准确、灵敏度高、结果重现性佳。
第四章复合汞膜吸附阴极溶出法测定药片及软饮料中的核黄素(VB_2)
本文建立了一种用复合汞膜电极示差脉冲吸附阴极溶出伏安法检测药片及软饮料中的核黄素(VB_2)含量的分析方法。结果表明:采用新型铕离子掺杂类普鲁士蓝复合汞膜电极(PB-Eu/MFE)为工作电极,在0.04mol/L KCl-0.01mol/LHNO_3底液中维生素B_2于-0.25V(vs.SCE)处产生一个灵敏的吸附阴极溶出峰。在最佳实验条件下,维生素B_2的浓度与还原峰电流在16～1600μg/L(r=0.9989,n=9)范围内呈现出良好的线性关系,最低检测下限为1.2μg/L(S/N=3),其相对标准偏差(RSD)为1.58%。用该法实测了药片维生素B_2,复合维生素及美汁源果粒橙饮料中维生素B_2的含量。
The content of trace elements has great relation to human health.The determination of trace elements plays an important role in the essay of environmental science,medicine,food and clinic.The chemically modified electrode(CME) has been one of the most flourish research realms in the electrochemistry and electroanalytical chemistry since it was developed in the 1970th.Among various of modified materials used to fabricate chemically modified electrode,polynuclear metal hexacyanometallate have been extensive studies for the applications in electrocatalysis,electrochemical sensors,functional materials,molecular sieves, solid-state batteries and molecular magnetism due to their good chemical and electrochemical stability,profuse electrochemical activities.Combined analogue of prussian blue modified electrode and the traditional advantages of mercury film electrode,this thesis studies the preparation and electroanalytical application of the modified PB-Eu composite mercury film electrode(PB-Eu/MFE) on glass carbon substrate.The PB-Eu/MFE has successfully apply to determine trace levels of bismuth,copper,lead,cadmium and vitamin B_2 in environmental samples by differential pulse stripping voltammetry.The PB-Eu/MFE remarkably shows higher sensitivity,perfect stability,long-lived and good date repeatability and also more and more potential application in the field of electroanalysis future and satisfactory results are obtained.
The main researches are summarized as follows:
Chapter One Review
The first section has reviewed the history,current situation and future trend of composite mercury film.The preparation and application of chemically modified composite mercury film electrode are introduced simply.In the second section,the type and application of stripping voltammetry are summarized in detail,paying attention to anodic stripping voltammetry and cathodic stripping voltammetry.The present application researches of anodic stripping voltammetry in analysis of environmental samples are introduced in the third section.The fourth section summarizes the vitamins feature in food and pays more attention to the determination of using water-solubility vitamins matters electrochemical methods.At last,the purpose and meaning of this work are discussed.Totally 100 references are cited in the chapter one.
Chapter Two Determination of adhesive lead(Ⅱ) of leaves in city using anodic stripping voltammetry with composite mercury film electrode
Adhesive lead(Ⅱ) of leaves in city is determined by differential pulse anodic stripping voltammetry and the main causation that made tree contaminated is deduced by the experimental data.The results reveals that a stripping peak potential of lead is observed at -0.472 V(vs.SCE) in 0.01 mol/L HNO_3 using the PB-Eu composite mercury film electrode as working electrode.Under the optimum conditions,good linearity is obtained in the concentration range of 2.4～300μg/L(r=0.9991,n=11) with a detection limit of 0.2μg/L(S/N=3) and RSD is 1.35%.This method is used for the determination of lead adhered to the surface of leaves,which is sampled in three different locals of Lanzhou city.The recoveries of the method are 97.3%-102%.The results showed that the lead pollution on tree leaves is from automobile tail-gas mainly and its lead content is positively correlative with the traffic presented on city streets near the tree.
Chapter Three Determination of bismuth,copper,lead and cadmium of waste dry batteries using anodic stripping voltammetry with composite mercury film electrode
A PB-Eu composite mercury film electrode is developed for simultaneous determination bismuth,copper,lead and cadmium of waste dry batteries by differential pulse anodic stripping voltammetry.The results reveals that stripping peak potentials of bismuth,copper,lead and cadmium are observed at -0.21 V,-0.34 V,-0.55 V,-0.75 V(vs.SCE) in 1 M KCl-10%lactic acid using the PB-Eu composite mercury film electrode as working electrode.Under the optimum conditions,the method has good linearity in the ranges of 4.0～160μg/L for bismuth(r=0.9986,n=8), 2.0～160μg/L for copper(r=0.9992,n=8),2.0～240μg/L for lead(r=0.9990,n=8)and 8.0～360μg/L for cadmium(r=0.9989,n=8);detection limits are 0.4μg/L,0.4μg/L, 0.2μg/L and 0.6μg/L(S/N=3);RSD are 3.80%,3.61%,2.37%and 3.88%for bismuth, copper,lead and cadmium,respectively.This method is used for the simultaneous determinations of bismuth,copper,lead and cadmium of waste dry batteries,the recoveries of the method are 97.4%-103%.The results show that the advantages of this method are simple and fast,its operation is stable and reliable,it is applied to simultaneous determination of these elements in waste dry batteries samples with satisfactory results.
Chapter Four Determination of VB_2 in tablets and soft beverage using cathodic adsorptive stripping voltammetry with composite mercury film electrode
VB_2 in tablets and soft beverage is determined by differential pulse adsorptive cathodic stripping voltammetry with composite mercury film electrode.The results reveal that an adsorptive stripping peak potential of VB_2 is observed about -0.25 V (vs.SCE) in 0.04mol/L KCl-0.01mol/L HNO_3 support electrolyte.Under the optimum conditions,good linearity is obtained in the concentration range of 16～1600μg/L(r=0.9989,n=9) with a detection limit of 1.2μg/L(S/N=3) and RSD of 1.58%. This method is used for the determination of VB_2 in tablets and soft beverage.The satisfactory results are obtained.
论文的主要研究内容包括以下四部分:
第一章综述
第一节概述了复合汞膜的发展历史和概况,对化学修饰型复合汞膜电极的制备方法及应用进行了简单介绍;第二节概述了溶出分析技术的分类及其应用,并对阳极溶出伏安法和阴极溶出伏安法进行了重点介绍;第三节对使用阳极溶出伏安法检测环境样品中重金属离子的分析应用进行了综述;第四节对食品中的水溶性维生素成份的性质进行了简介,并重点综述了电化学方法测定食品中水溶性维生素的方法。最后介绍了本论文的研究目的和意义。这部分共引用文献100篇。
第二章复合汞膜阳极溶出法检测城市绿化树叶上的附着铅
采用示差脉冲阳极溶出伏安法对城市绿化树叶上附着铅的含量进行了检测,并根据测得结果分析了树叶上附着铅的主要污染来源。结果表明:采用新型铕离子掺杂类普鲁士蓝复合汞膜电极(PB-Eu/MFE)为工作电极,在0.01mol/L HNO_3底液中,铅离子于-0.472V(vs.SCE)处产生一个灵敏的阳极溶出峰。在最佳实验条件下,其溶出峰电流与铅的浓度在2.4～300μg/L(r=0.9991,n=11)之间呈良好的线性关系,检测下限为0.2μg/L(S/N=3),RSD为1.35%。用该法检测了兰州市三个不同采集地点的城市绿化白蜡树叶上的附着铅含量,回收率为97.3%～102%。由测定结果可知汽车尾气污染是树叶上附着铅的重要来源,附着铅的含量与邻近交通要道的车流量之间有正相关性。
第三章复合汞膜阳极溶出法检测废电池中的铋铜铅镉
本文建立了用示差脉冲阳极溶出伏安法同时测定废旧电池中铋铜铅镉的方法。结果表明:采用新型铕离子掺杂普鲁士蓝复合汞膜电极(PB-Eu/MFE)为工作电极,在1M KCl-10%乳酸底液中,铋铜铅镉离子分别于-0.21V、-0.34V、-0.55V、-0.75V(vs.SCE)处产生灵敏的阳极溶出峰。在最佳实验条件下,其溶出峰电流与浓度(μg/L)分别在4.0～160(r=0.9986,n=8),2.0～160(r=0.9992,n=8),2.0～240(r=0.9990,n=8),8.0～360(r=0.9989,n=8)之间呈良好的线性关系;检测下限分别为0.4μg/L、0.4μg/L、0.2μg/L、0.6μg/L(S/N=3);RSD分别为3.80%、3.61%、2.37%、3.88%。用该法实测了四种不同品牌的废旧电池中这四种金属的含量,回收率为97.4%～104%。本法操作简便、准确、灵敏度高、结果重现性佳。
第四章复合汞膜吸附阴极溶出法测定药片及软饮料中的核黄素(VB_2)
本文建立了一种用复合汞膜电极示差脉冲吸附阴极溶出伏安法检测药片及软饮料中的核黄素(VB_2)含量的分析方法。结果表明:采用新型铕离子掺杂类普鲁士蓝复合汞膜电极(PB-Eu/MFE)为工作电极,在0.04mol/L KCl-0.01mol/LHNO_3底液中维生素B_2于-0.25V(vs.SCE)处产生一个灵敏的吸附阴极溶出峰。在最佳实验条件下,维生素B_2的浓度与还原峰电流在16～1600μg/L(r=0.9989,n=9)范围内呈现出良好的线性关系,最低检测下限为1.2μg/L(S/N=3),其相对标准偏差(RSD)为1.58%。用该法实测了药片维生素B_2,复合维生素及美汁源果粒橙饮料中维生素B_2的含量。
The content of trace elements has great relation to human health.The determination of trace elements plays an important role in the essay of environmental science,medicine,food and clinic.The chemically modified electrode(CME) has been one of the most flourish research realms in the electrochemistry and electroanalytical chemistry since it was developed in the 1970th.Among various of modified materials used to fabricate chemically modified electrode,polynuclear metal hexacyanometallate have been extensive studies for the applications in electrocatalysis,electrochemical sensors,functional materials,molecular sieves, solid-state batteries and molecular magnetism due to their good chemical and electrochemical stability,profuse electrochemical activities.Combined analogue of prussian blue modified electrode and the traditional advantages of mercury film electrode,this thesis studies the preparation and electroanalytical application of the modified PB-Eu composite mercury film electrode(PB-Eu/MFE) on glass carbon substrate.The PB-Eu/MFE has successfully apply to determine trace levels of bismuth,copper,lead,cadmium and vitamin B_2 in environmental samples by differential pulse stripping voltammetry.The PB-Eu/MFE remarkably shows higher sensitivity,perfect stability,long-lived and good date repeatability and also more and more potential application in the field of electroanalysis future and satisfactory results are obtained.
The main researches are summarized as follows:
Chapter One Review
The first section has reviewed the history,current situation and future trend of composite mercury film.The preparation and application of chemically modified composite mercury film electrode are introduced simply.In the second section,the type and application of stripping voltammetry are summarized in detail,paying attention to anodic stripping voltammetry and cathodic stripping voltammetry.The present application researches of anodic stripping voltammetry in analysis of environmental samples are introduced in the third section.The fourth section summarizes the vitamins feature in food and pays more attention to the determination of using water-solubility vitamins matters electrochemical methods.At last,the purpose and meaning of this work are discussed.Totally 100 references are cited in the chapter one.
Chapter Two Determination of adhesive lead(Ⅱ) of leaves in city using anodic stripping voltammetry with composite mercury film electrode
Adhesive lead(Ⅱ) of leaves in city is determined by differential pulse anodic stripping voltammetry and the main causation that made tree contaminated is deduced by the experimental data.The results reveals that a stripping peak potential of lead is observed at -0.472 V(vs.SCE) in 0.01 mol/L HNO_3 using the PB-Eu composite mercury film electrode as working electrode.Under the optimum conditions,good linearity is obtained in the concentration range of 2.4～300μg/L(r=0.9991,n=11) with a detection limit of 0.2μg/L(S/N=3) and RSD is 1.35%.This method is used for the determination of lead adhered to the surface of leaves,which is sampled in three different locals of Lanzhou city.The recoveries of the method are 97.3%-102%.The results showed that the lead pollution on tree leaves is from automobile tail-gas mainly and its lead content is positively correlative with the traffic presented on city streets near the tree.
Chapter Three Determination of bismuth,copper,lead and cadmium of waste dry batteries using anodic stripping voltammetry with composite mercury film electrode
A PB-Eu composite mercury film electrode is developed for simultaneous determination bismuth,copper,lead and cadmium of waste dry batteries by differential pulse anodic stripping voltammetry.The results reveals that stripping peak potentials of bismuth,copper,lead and cadmium are observed at -0.21 V,-0.34 V,-0.55 V,-0.75 V(vs.SCE) in 1 M KCl-10%lactic acid using the PB-Eu composite mercury film electrode as working electrode.Under the optimum conditions,the method has good linearity in the ranges of 4.0～160μg/L for bismuth(r=0.9986,n=8), 2.0～160μg/L for copper(r=0.9992,n=8),2.0～240μg/L for lead(r=0.9990,n=8)and 8.0～360μg/L for cadmium(r=0.9989,n=8);detection limits are 0.4μg/L,0.4μg/L, 0.2μg/L and 0.6μg/L(S/N=3);RSD are 3.80%,3.61%,2.37%and 3.88%for bismuth, copper,lead and cadmium,respectively.This method is used for the simultaneous determinations of bismuth,copper,lead and cadmium of waste dry batteries,the recoveries of the method are 97.4%-103%.The results show that the advantages of this method are simple and fast,its operation is stable and reliable,it is applied to simultaneous determination of these elements in waste dry batteries samples with satisfactory results.
Chapter Four Determination of VB_2 in tablets and soft beverage using cathodic adsorptive stripping voltammetry with composite mercury film electrode
VB_2 in tablets and soft beverage is determined by differential pulse adsorptive cathodic stripping voltammetry with composite mercury film electrode.The results reveal that an adsorptive stripping peak potential of VB_2 is observed about -0.25 V (vs.SCE) in 0.04mol/L KCl-0.01mol/L HNO_3 support electrolyte.Under the optimum conditions,good linearity is obtained in the concentration range of 16～1600μg/L(r=0.9989,n=9) with a detection limit of 1.2μg/L(S/N=3) and RSD of 1.58%. This method is used for the determination of VB_2 in tablets and soft beverage.The satisfactory results are obtained.
引文
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