多组分污染物在金刚石膜电极上的电化学行为与同时测定
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摘要
金刚石膜(Boron-doped diamond，简称BDD)电极具有独特的电化学特性如低的背景电流、宽的电势窗口、化学惰性、耐腐蚀性等，使之既适合环境污染物的分析，又适合环境污染物的降解。基于BDD电极其独特的电化学优势，针对环境污染物往往具有化学组分结构和性质相近、难以分离、多组分复杂体系等特性，探讨多组分污染物在BDD电极上的电化学行为及其同时测定将具有重要的研究意义。
本文主要在研究了多组分有机污染物、多种重金属离子在BDD电极上的电化学行为及其相互作用的基础上，采用循环伏安法、微分脉冲伏安法、微分脉冲溶出伏安法等多种电分析方法探讨BDD电极进行多组分环境污染物直接电化学伏安法分离和同时测定的方法可行性，建立了具有快速、简便、廉价等优点的多组分环境污染物同时测定的直接检测新方法。
同时，基于BDD的宽电势窗口特性，研究了难生化、难氧化的典型芳香分子在BDD电极上的电化学氧化可行性和氧化特征行为，为BDD电极直接电化学氧化降解芳香烃污染物奠定了研究基础，具有重要的理论研究意义。
(1)研究了多组分有机污染物在BDD电极上的电化学行为与同时测定。采用循环伏安法(CV)、微分脉冲伏安法(DPV)等电化学方法研究了苯酚、苯二酚、硝基苯酚在BDD电极上的氧化还原电化学行为；探讨了多组分酚类化合物在电极的吸附竞争情况；实现了苯酚—对苯二酚、苯酚—对硝基苯酚、对苯二酚—对硝基苯酚、苯酚—对苯二酚—对硝基苯酚等多组分有机污染物的电化学分离；建立了多组分酚类污染物同时测定的简便、灵敏的方法。
(2)研究多种共存的重金属离子在BDD电极上的电化学行为，建立多种重金属离子同时测定的实验方法。以银离子、铜离子、铅离子、镉离子、亚锡离子等重金属离子为研究对象，采用循环伏安法、微分脉冲溶出伏安法等电化学方法，分别以硝酸介质和醋酸盐缓冲溶液介质，考察了单离子体系、多种离子组成混合体系在BDD电极上的电化学氧化还原行为，研究了多种金属离子共存在BDD电极上的共沉积、相互作用。探讨了多种重金属离子在BDD电极上的电化学伏安分离的可行性，实现了多种重金属离子的电化学同时测定。
(3)研究了芳香分子污染物在BDD电极上的电化学氧化特性。采用线性扫描伏安法和微分脉冲伏安法，以苯、甲苯、对二甲苯、间二甲苯、乙苯五种典型芳香分子为研究对象，以0.5mol．L~(-1)的硫酸溶液为支持电解质，研究了这五种芳香分子在BDD电极上的电化学氧化行为，采用计时电量法研究芳香分子在BDD电极上的吸附，并采用恒电位计时电流法进一步探讨芳香分子电化学氧化
的机理。循环伏安法研究各种芳香分子在BDD电极上的氧化和还原行为的实验
发现，在整个循环伏安的负向扫描过程中均无还原峰出产生，这表明芳香分子在
BDD电极上的氧化反应是不可逆的。苯、甲苯、间二甲苯、对二甲苯、乙苯在
BDD电极上的氧化峰数目分别为2、3、3、3、4，这一结果与理论计算得到的
芳香分子结构中的不同电荷密度的H原子的种类数目正好相差1，而其中最高的
氧化电位恰好位于BDD电极析氧电位(2.4V)之后，推测是由苯环氧化开环产
生的氧化峰，而最低氧化电位处的氧化峰则是由苯环上的电荷密度几乎相等的H
原子的氧化产生的，而介于最低氧化电位与最高氧化电位的多个氧化峰依次是有
苯环取代基—CH_2—与—CH_3上的H原子的氧化密切相关的。苯环上有取代基，
且取代基上H的种类越多，则芳香分子在BDD电极上的氧化峰个数越多，芳香
分子初始氧化电位越低，如苯、甲苯、乙苯的初始氧化电位依次为1.91V、1.75V、
1.67V；而当苯环上取代基相同时，取代基越多，芳香分子越易于氧化，如对二
甲苯和甲苯的初始氧化电位分别为1.63V和1.75V；而取代基的取代位置基本不
影响氧化性质，如对二甲苯和间二甲苯的初始氧化电位为1.63V和1.64V。这是
非常有意义的研究结果。由此表明，芳香分子能够在BDD电极上发生直接的电
化学氧化，且在不同的氧化电极电位下，可有效地控制芳香分子的氧化程度和氧
化产物结构。
BDD is one of the most popular electrode materials. It exhibits several excellent electrochemical properties, including a wide electrochemical potential window in either aqueous or non-aqueous media, very low background current, corrosion resistance and etc., which make it a promising electrode material for both the determination and the degradation of environmental pollutants. However, it is well-known that environmental pollutants have several special properties, such as the similarity for both their component structure and quality, difficulty of separation, the complex multi-components and etc. So based on BDD electrode's unique electrochemical advantages, it is of utmost significance to study the electrochemical behavior of multi-component pollutants and to realize the simultaneous determination of them.
In this paper, we firstly studied the electrochemical behavior and interaction of multi-component organic pollutants and of several kinds of heavy metal ions at BDD electrode. Then cyclic voltammetry, differential pulse voltammetry, differential pulse stripping voltammetry and other electrochemical techniques were adopted to investigate the feasibility of voltammetric separation and simultaneous determination of mutil-pollutant system at BDD electrodes. Finally, an analytic method for the direct and swift determination of multi-component environmental pollutants with low-cost was established satisfyingly.
Consequently, our research job which is concerning the feasibility of electrochemical oxidation of representative non-biodegradable and refractory aromatic compounds at boron-doped diamond electrode is a challenging and primary one for the further research of direct electrochemical oxidation and degradation of aromatic compounds.
(1) Simultaneous electrochemical determination of multi-component system of organic pollutants was realized at BDD electrode. Here, cyclic voltammetry and differential pulse voltametry were adopted to study the electrochemical redox behavior of phenol, hydroquinone, 4-nitrophenol at BDD electrode. We also discussed the absorption competition among organic pollutants primarily in this work; And then the separation of multi-component systems, such as phenol and hydroquinone, phenol and 4-nitrophenol, hydroquinone and 4-nitrophenol, phenol, hydroquinone and 4-nitrophenol, has been implemented. As a result, a simple and sensitive method for
simultaneous determination of multi-component of hydroxybenzene pollutants has been established.
(2) With the electrochemical behavior of multi-metal-ion system investigated, a method of simultaneous determination of multi-metal-ion system has also been set up. Choosing Ag~+, Cu~(2+), Pb~(2+), Sn~(2+) as our research objects, cyclic voltammetry, differential pulse voltammetry, differential pulse stripping voltammetry and other electrochemical techniques were used here to investigate the electrochemical redox behavior of both single-metal-ion system and multi-ion system at BDD electrode in nitric acid solution or in acetate buffer solution respectively. Whereafter, the interaction among metal ions was studied during their co-deposition process at BDD electrode. And the feasibility of electrochemical separation of multi-metal-ion system was discussed. Finally, the simultaneous determination of multi-metal-ion system at BDD electrode was realized.
(3) The electrochemical oxidation of aromatic compounds at BDD electrode was studied. For this purpose, linear sweep voltammetry and differential pulse voltammetry were adopted for the investigation of electrochemical oxidation of benzene, toluene, m-xylene, p-xylene and ethylbenzene at BDD electrode in 0.5 M H2SO4 solution as a supporting electrolyte. The absorption of aromatic compounds at BDD was studied by chronocoulometry, the electrochemical oxidation mechanism of aromatic compounds was further dicussed by chronoamperometry and the redox behavior of aromatic compounds at BDD electrode was investigated by cyclic voltammetry. As a result of these explorations, it was found that there was no reduction peak emerged during the whole negative scanning process of cyclic voltammetry, which means that the redox reaction of aromatic molecules should be irreversible. To prove this assumption, our following research was mainly focused on analysing the redox behavior of aromatic molecules at BDD electrode during the positive linear sweeping process. And our experimental results indicated that the oxidation peak quantity of benzene, toluene, m-xylene, p-xylene and ethylbenzene at BDD electrode is 2, 3, 3, 3 and 4 respectively. And the difference between these data and the varieties of H atoms with different charge density on the aromatic molecules calculated theoretically is found to be only 1. The highest oxidation potential was located at a potential higher than the oxygen evolution potential at BDD electrode, which may be caused by the opening of benzene ring. Simultaneously, the oxidation peak emerged at the lowest oxidation potential may be induced by the oxidation of H atoms on benzene ring with the same charge density. So according to the above results, we believe that there should be a very close relationship between the multiple oxidation peaks which are amidst the two oxidation peaks located at both the lowest potential and the highest potential and the oxidation of H atoms located on the benzene substituent groups, such as-CH_2-and-CH_3 respectively. According to our supposition, if substituent existed, then the greater the varieties of H atoms on the substituent are, the more oxidation peaks of aromatic molecules at BDD electode would be, and the lower the initial oxidation potential of aromatic molecules would be. For example, the initial oxidation potentials of benzene, toluene and ethylbenzene are 1.91V, 1.75V and 1.67V respectively. If the substituents on benzene ring were the same ones, then the larger the quantity of substituents is, the more easily the aromatic would be oxidized. For example, the initial oxidation potentials of p-xylene and toluene are 1.63V and 1.75V respectively. Besides, it was observed that the substituent location would have no effect on the property of oxidation. For example, the initial oxidation potentials of p-xylene and m-xylene are 1.63V and 1.64V respectively. The results are interesting and promising. It indicates that the direct electrochemical oxidation of aromatic molecules at BDD electrode can be realized, Under different oxidation potentials, both the oxidation extent and the oxidized products' structure of aromatic molecules can be under control effectively.
本文主要在研究了多组分有机污染物、多种重金属离子在BDD电极上的电化学行为及其相互作用的基础上，采用循环伏安法、微分脉冲伏安法、微分脉冲溶出伏安法等多种电分析方法探讨BDD电极进行多组分环境污染物直接电化学伏安法分离和同时测定的方法可行性，建立了具有快速、简便、廉价等优点的多组分环境污染物同时测定的直接检测新方法。
同时，基于BDD的宽电势窗口特性，研究了难生化、难氧化的典型芳香分子在BDD电极上的电化学氧化可行性和氧化特征行为，为BDD电极直接电化学氧化降解芳香烃污染物奠定了研究基础，具有重要的理论研究意义。
(1)研究了多组分有机污染物在BDD电极上的电化学行为与同时测定。采用循环伏安法(CV)、微分脉冲伏安法(DPV)等电化学方法研究了苯酚、苯二酚、硝基苯酚在BDD电极上的氧化还原电化学行为；探讨了多组分酚类化合物在电极的吸附竞争情况；实现了苯酚—对苯二酚、苯酚—对硝基苯酚、对苯二酚—对硝基苯酚、苯酚—对苯二酚—对硝基苯酚等多组分有机污染物的电化学分离；建立了多组分酚类污染物同时测定的简便、灵敏的方法。
(2)研究多种共存的重金属离子在BDD电极上的电化学行为，建立多种重金属离子同时测定的实验方法。以银离子、铜离子、铅离子、镉离子、亚锡离子等重金属离子为研究对象，采用循环伏安法、微分脉冲溶出伏安法等电化学方法，分别以硝酸介质和醋酸盐缓冲溶液介质，考察了单离子体系、多种离子组成混合体系在BDD电极上的电化学氧化还原行为，研究了多种金属离子共存在BDD电极上的共沉积、相互作用。探讨了多种重金属离子在BDD电极上的电化学伏安分离的可行性，实现了多种重金属离子的电化学同时测定。
(3)研究了芳香分子污染物在BDD电极上的电化学氧化特性。采用线性扫描伏安法和微分脉冲伏安法，以苯、甲苯、对二甲苯、间二甲苯、乙苯五种典型芳香分子为研究对象，以0.5mol．L~(-1)的硫酸溶液为支持电解质，研究了这五种芳香分子在BDD电极上的电化学氧化行为，采用计时电量法研究芳香分子在BDD电极上的吸附，并采用恒电位计时电流法进一步探讨芳香分子电化学氧化
的机理。循环伏安法研究各种芳香分子在BDD电极上的氧化和还原行为的实验
发现，在整个循环伏安的负向扫描过程中均无还原峰出产生，这表明芳香分子在
BDD电极上的氧化反应是不可逆的。苯、甲苯、间二甲苯、对二甲苯、乙苯在
BDD电极上的氧化峰数目分别为2、3、3、3、4，这一结果与理论计算得到的
芳香分子结构中的不同电荷密度的H原子的种类数目正好相差1，而其中最高的
氧化电位恰好位于BDD电极析氧电位(2.4V)之后，推测是由苯环氧化开环产
生的氧化峰，而最低氧化电位处的氧化峰则是由苯环上的电荷密度几乎相等的H
原子的氧化产生的，而介于最低氧化电位与最高氧化电位的多个氧化峰依次是有
苯环取代基—CH_2—与—CH_3上的H原子的氧化密切相关的。苯环上有取代基，
且取代基上H的种类越多，则芳香分子在BDD电极上的氧化峰个数越多，芳香
分子初始氧化电位越低，如苯、甲苯、乙苯的初始氧化电位依次为1.91V、1.75V、
1.67V；而当苯环上取代基相同时，取代基越多，芳香分子越易于氧化，如对二
甲苯和甲苯的初始氧化电位分别为1.63V和1.75V；而取代基的取代位置基本不
影响氧化性质，如对二甲苯和间二甲苯的初始氧化电位为1.63V和1.64V。这是
非常有意义的研究结果。由此表明，芳香分子能够在BDD电极上发生直接的电
化学氧化，且在不同的氧化电极电位下，可有效地控制芳香分子的氧化程度和氧
化产物结构。
BDD is one of the most popular electrode materials. It exhibits several excellent electrochemical properties, including a wide electrochemical potential window in either aqueous or non-aqueous media, very low background current, corrosion resistance and etc., which make it a promising electrode material for both the determination and the degradation of environmental pollutants. However, it is well-known that environmental pollutants have several special properties, such as the similarity for both their component structure and quality, difficulty of separation, the complex multi-components and etc. So based on BDD electrode's unique electrochemical advantages, it is of utmost significance to study the electrochemical behavior of multi-component pollutants and to realize the simultaneous determination of them.
In this paper, we firstly studied the electrochemical behavior and interaction of multi-component organic pollutants and of several kinds of heavy metal ions at BDD electrode. Then cyclic voltammetry, differential pulse voltammetry, differential pulse stripping voltammetry and other electrochemical techniques were adopted to investigate the feasibility of voltammetric separation and simultaneous determination of mutil-pollutant system at BDD electrodes. Finally, an analytic method for the direct and swift determination of multi-component environmental pollutants with low-cost was established satisfyingly.
Consequently, our research job which is concerning the feasibility of electrochemical oxidation of representative non-biodegradable and refractory aromatic compounds at boron-doped diamond electrode is a challenging and primary one for the further research of direct electrochemical oxidation and degradation of aromatic compounds.
(1) Simultaneous electrochemical determination of multi-component system of organic pollutants was realized at BDD electrode. Here, cyclic voltammetry and differential pulse voltametry were adopted to study the electrochemical redox behavior of phenol, hydroquinone, 4-nitrophenol at BDD electrode. We also discussed the absorption competition among organic pollutants primarily in this work; And then the separation of multi-component systems, such as phenol and hydroquinone, phenol and 4-nitrophenol, hydroquinone and 4-nitrophenol, phenol, hydroquinone and 4-nitrophenol, has been implemented. As a result, a simple and sensitive method for
simultaneous determination of multi-component of hydroxybenzene pollutants has been established.
(2) With the electrochemical behavior of multi-metal-ion system investigated, a method of simultaneous determination of multi-metal-ion system has also been set up. Choosing Ag~+, Cu~(2+), Pb~(2+), Sn~(2+) as our research objects, cyclic voltammetry, differential pulse voltammetry, differential pulse stripping voltammetry and other electrochemical techniques were used here to investigate the electrochemical redox behavior of both single-metal-ion system and multi-ion system at BDD electrode in nitric acid solution or in acetate buffer solution respectively. Whereafter, the interaction among metal ions was studied during their co-deposition process at BDD electrode. And the feasibility of electrochemical separation of multi-metal-ion system was discussed. Finally, the simultaneous determination of multi-metal-ion system at BDD electrode was realized.
(3) The electrochemical oxidation of aromatic compounds at BDD electrode was studied. For this purpose, linear sweep voltammetry and differential pulse voltammetry were adopted for the investigation of electrochemical oxidation of benzene, toluene, m-xylene, p-xylene and ethylbenzene at BDD electrode in 0.5 M H2SO4 solution as a supporting electrolyte. The absorption of aromatic compounds at BDD was studied by chronocoulometry, the electrochemical oxidation mechanism of aromatic compounds was further dicussed by chronoamperometry and the redox behavior of aromatic compounds at BDD electrode was investigated by cyclic voltammetry. As a result of these explorations, it was found that there was no reduction peak emerged during the whole negative scanning process of cyclic voltammetry, which means that the redox reaction of aromatic molecules should be irreversible. To prove this assumption, our following research was mainly focused on analysing the redox behavior of aromatic molecules at BDD electrode during the positive linear sweeping process. And our experimental results indicated that the oxidation peak quantity of benzene, toluene, m-xylene, p-xylene and ethylbenzene at BDD electrode is 2, 3, 3, 3 and 4 respectively. And the difference between these data and the varieties of H atoms with different charge density on the aromatic molecules calculated theoretically is found to be only 1. The highest oxidation potential was located at a potential higher than the oxygen evolution potential at BDD electrode, which may be caused by the opening of benzene ring. Simultaneously, the oxidation peak emerged at the lowest oxidation potential may be induced by the oxidation of H atoms on benzene ring with the same charge density. So according to the above results, we believe that there should be a very close relationship between the multiple oxidation peaks which are amidst the two oxidation peaks located at both the lowest potential and the highest potential and the oxidation of H atoms located on the benzene substituent groups, such as-CH_2-and-CH_3 respectively. According to our supposition, if substituent existed, then the greater the varieties of H atoms on the substituent are, the more oxidation peaks of aromatic molecules at BDD electode would be, and the lower the initial oxidation potential of aromatic molecules would be. For example, the initial oxidation potentials of benzene, toluene and ethylbenzene are 1.91V, 1.75V and 1.67V respectively. If the substituents on benzene ring were the same ones, then the larger the quantity of substituents is, the more easily the aromatic would be oxidized. For example, the initial oxidation potentials of p-xylene and toluene are 1.63V and 1.75V respectively. Besides, it was observed that the substituent location would have no effect on the property of oxidation. For example, the initial oxidation potentials of p-xylene and m-xylene are 1.63V and 1.64V respectively. The results are interesting and promising. It indicates that the direct electrochemical oxidation of aromatic molecules at BDD electrode can be realized, Under different oxidation potentials, both the oxidation extent and the oxidized products' structure of aromatic molecules can be under control effectively.
引文
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