碳纳米管复合材料修饰电极的制备及其分析应用研究
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摘要
目前,运用纳米材料、特别是碳纳米管及其复合材料作为化学修饰电极新的修饰材料是化学修饰电极新的发展方向。这对于建立新的高灵敏度、高选择性的分析方法有重要意义。
本文采取多种方法制备了几种新型的碳纳米管复合材料修饰电极,结合各种表征手段对其进行了研究。提出了几种运用碳纳米管复合材料修饰电极对环境,生命科学等领域物质的分析方法。具体地说,本论文主要开展了以下几方面的创新研究工作:
1、首次通过电聚合酸性铬蓝K于多壁碳纳米管修饰的玻碳电极上制备了Poly-ACBK/MWNTs/GC电极。运用SEM及循环伏安法等方法研究了修饰电极的性能。考察了苯二酚异构体在Poly-ACBK/MWNTs/GC电极上的电化学表现,结果表明Poly-ACBK/MWNTs/GC电极对苯二酚异构体的氧化表现出优异的电催化性能和选择性能。在1×10-6-1×10-4mol·L-1的范围内,苯二酚异构体的阳极峰电流与其浓度有线性关系。依此发展了一种运用Poly-ACBK/MWNTs/GC电极同时伏安分析苯二酚三种异构体的方法。
2、首次通过电聚合溴酚蓝于多壁碳纳米管修饰的玻碳电极上制备了Poly-BPB/MWNTs/GC电极。运用SEM及循环伏安法等方法研究了修饰电极的性能。考察了苯二酚异构体在Poly-BPB/MWNTs/GC电极上的电化学表现,结果表明Poly-BPB/MWNTs/GC电极对苯二酚异构体的氧化表现出优异的电催化性能和选择性能。在1×10-6-1×10-4mol·L-1的范围内,三种苯二酚异构体的阳极峰电流与其浓度有线性关系。依此发展了一种运用Poly-BPB/MWNTs/GC电极同时伏安分析苯二酚三种异构体的方法。
3、制备了一种新的纳米银覆盖多壁碳纳米管复合材料修饰电极(nano-Ag/MWNTs/GC电极)。第一次提出了利用nano-Ag/MWNTs/GC电极对痕量硫氰酸根的测定的方法。运用扫描电镜方法(SEM)与X衍射测试方法(XRD)对纳米银覆盖多壁碳纳米管复合材料进行表征。采用循环伏安法研究了硫氰酸根在nano-Ag/MWNTs/GC电极的电化学表现。结果发现:随着硫氰酸根的加入,阳极峰电流逐渐降低。在2.5×10?9-5×10?8mol·L-1及5×10?8-1×10?6mol·L-1之间,阳极峰电流的降低与硫氰酸根浓度成正比,检测限为1×10?9mol·L-1(S/N=3)。提出方法的检测限优于其他测定硫氰酸根浓度的方法。同时,提出的方法对实际生物样品人唾沫与人尿中的硫氰酸根进行了测定并获得了良好的结果。
4、利用电吸附血红蛋白(Hb)于Ag/CNT/GC电极上,制作了Hb/Ag/CNT/GC电极。循环伏安法研究了该修饰电极的电化学性质,发现对氧气还原有明显的电催化作用。在一定的范围内,还原峰电流的大小与通入的空气量成正比。据此提出了一种可以测定水中的含氧量的电化学方法。
5、采用纳米银覆盖多壁碳纳米管复合材料制作了纳米-Ag/MWNTs/GC电极,用(XRD)和循环伏安法对修饰电极进行了表征。研究发现修饰电极对过氧化氢还原有催化作用。修饰电极可用来直接测定过氧化氢。在3.5×10-4-5.5×10-3 mol·L-1与5.5×10-3-1.5×10-2 mol·L-1范围内,阴极微分脉冲峰电流与过氧化氢浓度成正比,检测限为2×10-4 mol·L-1。对实际样品进行测定,获得较好的结果。
6、利用纳米银覆盖多壁碳纳米管复合材料制备了修饰电极。循环伏安法研究了氯离子在纳米银覆盖多壁碳纳米管修饰玻碳电极的电化学表现。结果发现:随着高浓度氯离子的加入,阳极峰电流逐渐降低。在8×10?3-0.1 mol·L-1之间,阳极峰电流的降低与氯离子浓度成正比。因此,发展了一种修饰电极测定高浓度氯离子的方法。采用提出的方法对自来水中高浓度氯离子含量进行测定。
7、建立了一种新型聚亚甲基蓝/单壁碳纳米管修饰玻碳电极,成功的应用于NADH的测定。研究了修饰电极对NADH的协同催化作用,结果发现在5.0×10-6- 7.0×10-4 mol·L-1浓度范围内,氧化峰电流与加入的NADH量有良好的线性关系。
At present, the application of nano-materials, especially carbon nanotubes and its composites as new chemically modified materials is a new direction in the field of chemically modified electrodes. It is important to establish new analytical methods with high-sensitivity and selectivity.
In this paper, a variety of new carbon nanotubes composites modified electrodes were proposed. The properties of the carbon nanotubes composites modified electrodes were characterizd by several methods. Several methods for analyzing substances in environmental sciences and life sciences have been developed. The main works of this thesis are summarized as follows:
1. A novel modified electrode was fabricated by electropolymerization of acid chrome blue K at a glassy carbon electrode modified with multi-walled carbon nanotubes and used for simultaneous voltammetric determination of dihydroxybenzene isomers. The Poly-ACBK/MWNTs/GC electrode was characterized with scanning electron microscopy (SEM) and cyclic voltammetry(CV). The electrochemical performance of dihydroxybenzene at the Poly-ACBK/MWNTs/GC electrode has been investigated by cyclic voltammetry. It was found that Poly-ACBK/MWNTs/GC electrode has excellent electrocatalyse and selectivity toward oxidation of dihydroxybenzene. A linear relationship between anodal peak current and concentration of hydroquinone, catechol and resorcinol was obtained in the range of 1×10-6~(-1)×10~(-4) mol·L~(-1).
2. A novel modified electrode was fabricated by electropolymerization of bromophenol blue at a glassy carbon electrode modified with multi-walled carbon nanotubes and used for simultaneous voltammetric determination of dihydroxybenzene isomers. The Poly-BPB/MWNTs/GC electrode was characterized with SEM and CV. The electrochemical performance of dihydroxybenzene at the Poly-BPB/MWNTs/GC electrode has been investigated by CV. It was found that Poly-BPB/MWNTs/GC electrode has excellent electrocatalyse and selectivity toward oxidation of dihydroxybenzene. A linear relationship between anodal peak current and concentration of hydroquinone, catechol and resorcinol was obtained in the range of 1×10-6~(-1)×10~(-4) mol·L~(-1).
3. A novel nano-silver coated multi-walled carbon nanotubes composites modified electrode was prepared. The application of the modified electrode for determination of trace thiocyanate is demonstrated for the first time. The property of nano-silver coated multi-walled carbon nanotubes composites was characterized with SEM, X-ray powder diffraction (XRD) and CV. The electrochemical behaviour of thiocyanate at the nano-Ag/MWNTs/GC electrode was investigated by CV. It was found that there was a linear relationship at the range 2.5×10?9 to 5×10?8 mol·L-1 and 5×10?8 to 1×10?6 mol·L-1 of thiocyanate with the decrement of anodal DPV peak currents. The limit of detection was 1×10?9 mol·L-1(S/N=3)and is better than the other thiocyanate-determination methods. Actual urine and saliva samples of smoker and non-smoker were analyzed and satisfactory results were obtained.
4. A novel modified electrode was fabricated by electro-absorbption of hemoglobin (Hb) at Ag/CNT/GC electrode. The electrochemical properties of the modified electrode were investigated by CV. It was found that the modified electrode has obvious electrocatalysis toward the reduction of oxygen. There was a linear relationship between the currents of reduced peak with the volume of pumped air. An ectrochemical method for the determination of oxygen in water has developed.
5. The nano-Ag/MWNTs/GC electrode has been fabricated with nano-silver coated multi-walled carbon nanotubes composites. The modified electrode was characterized with SEM and CV. It was found that the modified electrode has electrocatalysis toward the reduction of hydrogen peroxide. The modified electrode could be used to direct determination of hydrogen peroxide. There were linear relationships in the range 3.5×10-4~5.5×10-3 mol·L-1 and 5.5×10-3~ 1.5×10-2 mol·L-1of hydrogen peroxide, respectively, with the of cathodic differential pulse voltammetric peak currents. The limit of detection was 2×10-4 mol·L-1. Actual samples were analyzed and satisfactory results were obtained.
6. A nano-Ag/MWNTs/GC electrode has been fabricated with nano-silver coated multi-walled carbon nanotubes composites. The electrochemical properties of chloride ion at the modified electrode were investigated by CV. It is found that the differential pulse voltammetry (DPV) currents of anode peak decreased with the addition of high concentration chloride ion. There was a linear relationship at the range 8×10?3-0.1 mol·L-1 with the decrement of anodic DPV peak currents. The application of the modified electrode for determination of high concentration chloride ion has developed. Actual tap water samples were analyzed by this method.
7. A new poly-methylene blue/single-wall carbon nanotubes modified glassy carbon electrode was proposed and applied to detect NADH successfully. The synergistic electrocatalytic effect of the modified electrode toward oxidation of NADH has been investigated. It was found that there was a linear relationship at the range 5.0×10-6- 7.0×10-4 mol·L-1with the anodal peak currents and the concentration of NADH.
本文采取多种方法制备了几种新型的碳纳米管复合材料修饰电极,结合各种表征手段对其进行了研究。提出了几种运用碳纳米管复合材料修饰电极对环境,生命科学等领域物质的分析方法。具体地说,本论文主要开展了以下几方面的创新研究工作:
1、首次通过电聚合酸性铬蓝K于多壁碳纳米管修饰的玻碳电极上制备了Poly-ACBK/MWNTs/GC电极。运用SEM及循环伏安法等方法研究了修饰电极的性能。考察了苯二酚异构体在Poly-ACBK/MWNTs/GC电极上的电化学表现,结果表明Poly-ACBK/MWNTs/GC电极对苯二酚异构体的氧化表现出优异的电催化性能和选择性能。在1×10-6-1×10-4mol·L-1的范围内,苯二酚异构体的阳极峰电流与其浓度有线性关系。依此发展了一种运用Poly-ACBK/MWNTs/GC电极同时伏安分析苯二酚三种异构体的方法。
2、首次通过电聚合溴酚蓝于多壁碳纳米管修饰的玻碳电极上制备了Poly-BPB/MWNTs/GC电极。运用SEM及循环伏安法等方法研究了修饰电极的性能。考察了苯二酚异构体在Poly-BPB/MWNTs/GC电极上的电化学表现,结果表明Poly-BPB/MWNTs/GC电极对苯二酚异构体的氧化表现出优异的电催化性能和选择性能。在1×10-6-1×10-4mol·L-1的范围内,三种苯二酚异构体的阳极峰电流与其浓度有线性关系。依此发展了一种运用Poly-BPB/MWNTs/GC电极同时伏安分析苯二酚三种异构体的方法。
3、制备了一种新的纳米银覆盖多壁碳纳米管复合材料修饰电极(nano-Ag/MWNTs/GC电极)。第一次提出了利用nano-Ag/MWNTs/GC电极对痕量硫氰酸根的测定的方法。运用扫描电镜方法(SEM)与X衍射测试方法(XRD)对纳米银覆盖多壁碳纳米管复合材料进行表征。采用循环伏安法研究了硫氰酸根在nano-Ag/MWNTs/GC电极的电化学表现。结果发现:随着硫氰酸根的加入,阳极峰电流逐渐降低。在2.5×10?9-5×10?8mol·L-1及5×10?8-1×10?6mol·L-1之间,阳极峰电流的降低与硫氰酸根浓度成正比,检测限为1×10?9mol·L-1(S/N=3)。提出方法的检测限优于其他测定硫氰酸根浓度的方法。同时,提出的方法对实际生物样品人唾沫与人尿中的硫氰酸根进行了测定并获得了良好的结果。
4、利用电吸附血红蛋白(Hb)于Ag/CNT/GC电极上,制作了Hb/Ag/CNT/GC电极。循环伏安法研究了该修饰电极的电化学性质,发现对氧气还原有明显的电催化作用。在一定的范围内,还原峰电流的大小与通入的空气量成正比。据此提出了一种可以测定水中的含氧量的电化学方法。
5、采用纳米银覆盖多壁碳纳米管复合材料制作了纳米-Ag/MWNTs/GC电极,用(XRD)和循环伏安法对修饰电极进行了表征。研究发现修饰电极对过氧化氢还原有催化作用。修饰电极可用来直接测定过氧化氢。在3.5×10-4-5.5×10-3 mol·L-1与5.5×10-3-1.5×10-2 mol·L-1范围内,阴极微分脉冲峰电流与过氧化氢浓度成正比,检测限为2×10-4 mol·L-1。对实际样品进行测定,获得较好的结果。
6、利用纳米银覆盖多壁碳纳米管复合材料制备了修饰电极。循环伏安法研究了氯离子在纳米银覆盖多壁碳纳米管修饰玻碳电极的电化学表现。结果发现:随着高浓度氯离子的加入,阳极峰电流逐渐降低。在8×10?3-0.1 mol·L-1之间,阳极峰电流的降低与氯离子浓度成正比。因此,发展了一种修饰电极测定高浓度氯离子的方法。采用提出的方法对自来水中高浓度氯离子含量进行测定。
7、建立了一种新型聚亚甲基蓝/单壁碳纳米管修饰玻碳电极,成功的应用于NADH的测定。研究了修饰电极对NADH的协同催化作用,结果发现在5.0×10-6- 7.0×10-4 mol·L-1浓度范围内,氧化峰电流与加入的NADH量有良好的线性关系。
At present, the application of nano-materials, especially carbon nanotubes and its composites as new chemically modified materials is a new direction in the field of chemically modified electrodes. It is important to establish new analytical methods with high-sensitivity and selectivity.
In this paper, a variety of new carbon nanotubes composites modified electrodes were proposed. The properties of the carbon nanotubes composites modified electrodes were characterizd by several methods. Several methods for analyzing substances in environmental sciences and life sciences have been developed. The main works of this thesis are summarized as follows:
1. A novel modified electrode was fabricated by electropolymerization of acid chrome blue K at a glassy carbon electrode modified with multi-walled carbon nanotubes and used for simultaneous voltammetric determination of dihydroxybenzene isomers. The Poly-ACBK/MWNTs/GC electrode was characterized with scanning electron microscopy (SEM) and cyclic voltammetry(CV). The electrochemical performance of dihydroxybenzene at the Poly-ACBK/MWNTs/GC electrode has been investigated by cyclic voltammetry. It was found that Poly-ACBK/MWNTs/GC electrode has excellent electrocatalyse and selectivity toward oxidation of dihydroxybenzene. A linear relationship between anodal peak current and concentration of hydroquinone, catechol and resorcinol was obtained in the range of 1×10-6~(-1)×10~(-4) mol·L~(-1).
2. A novel modified electrode was fabricated by electropolymerization of bromophenol blue at a glassy carbon electrode modified with multi-walled carbon nanotubes and used for simultaneous voltammetric determination of dihydroxybenzene isomers. The Poly-BPB/MWNTs/GC electrode was characterized with SEM and CV. The electrochemical performance of dihydroxybenzene at the Poly-BPB/MWNTs/GC electrode has been investigated by CV. It was found that Poly-BPB/MWNTs/GC electrode has excellent electrocatalyse and selectivity toward oxidation of dihydroxybenzene. A linear relationship between anodal peak current and concentration of hydroquinone, catechol and resorcinol was obtained in the range of 1×10-6~(-1)×10~(-4) mol·L~(-1).
3. A novel nano-silver coated multi-walled carbon nanotubes composites modified electrode was prepared. The application of the modified electrode for determination of trace thiocyanate is demonstrated for the first time. The property of nano-silver coated multi-walled carbon nanotubes composites was characterized with SEM, X-ray powder diffraction (XRD) and CV. The electrochemical behaviour of thiocyanate at the nano-Ag/MWNTs/GC electrode was investigated by CV. It was found that there was a linear relationship at the range 2.5×10?9 to 5×10?8 mol·L-1 and 5×10?8 to 1×10?6 mol·L-1 of thiocyanate with the decrement of anodal DPV peak currents. The limit of detection was 1×10?9 mol·L-1(S/N=3)and is better than the other thiocyanate-determination methods. Actual urine and saliva samples of smoker and non-smoker were analyzed and satisfactory results were obtained.
4. A novel modified electrode was fabricated by electro-absorbption of hemoglobin (Hb) at Ag/CNT/GC electrode. The electrochemical properties of the modified electrode were investigated by CV. It was found that the modified electrode has obvious electrocatalysis toward the reduction of oxygen. There was a linear relationship between the currents of reduced peak with the volume of pumped air. An ectrochemical method for the determination of oxygen in water has developed.
5. The nano-Ag/MWNTs/GC electrode has been fabricated with nano-silver coated multi-walled carbon nanotubes composites. The modified electrode was characterized with SEM and CV. It was found that the modified electrode has electrocatalysis toward the reduction of hydrogen peroxide. The modified electrode could be used to direct determination of hydrogen peroxide. There were linear relationships in the range 3.5×10-4~5.5×10-3 mol·L-1 and 5.5×10-3~ 1.5×10-2 mol·L-1of hydrogen peroxide, respectively, with the of cathodic differential pulse voltammetric peak currents. The limit of detection was 2×10-4 mol·L-1. Actual samples were analyzed and satisfactory results were obtained.
6. A nano-Ag/MWNTs/GC electrode has been fabricated with nano-silver coated multi-walled carbon nanotubes composites. The electrochemical properties of chloride ion at the modified electrode were investigated by CV. It is found that the differential pulse voltammetry (DPV) currents of anode peak decreased with the addition of high concentration chloride ion. There was a linear relationship at the range 8×10?3-0.1 mol·L-1 with the decrement of anodic DPV peak currents. The application of the modified electrode for determination of high concentration chloride ion has developed. Actual tap water samples were analyzed by this method.
7. A new poly-methylene blue/single-wall carbon nanotubes modified glassy carbon electrode was proposed and applied to detect NADH successfully. The synergistic electrocatalytic effect of the modified electrode toward oxidation of NADH has been investigated. It was found that there was a linear relationship at the range 5.0×10-6- 7.0×10-4 mol·L-1with the anodal peak currents and the concentration of NADH.
引文
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