基于纳米金和三维自组装膜界面的环境电化学传感器制备及应用
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摘要
本论文借助“种子媒介纳米金生长法”,制备了新型纳米金修饰玻碳电极(Au/GCE);并在此基础上,将纳米金粒子与自组装膜技术相结合构建了新型三维自组装膜修饰电极。通过场发射扫描电子显微镜(FE-SEM)、紫外-可见光谱分析(UV-vis)、电化学分析等测试技术,对修饰电极的表面形貌、结构以及电化学性能进行了详细研究;并以Au/GCE电极为基础,制备了系列环境电化学传感器,成功用于水体中NO2-、多种痕量苯酚类衍生物、尿酸(UA)和抗坏血酸(AA)以及Cu2+的电化学检测。主要研究结果如下:
(1)实现了粒径为50-90 nm的纳米金修饰玻碳电极的制备;证明了纳米金粒子能有效促进电极表面的电子传递速率;发现L-半胱氨酸(L-cys)组装膜的电化学氧化产物(L-cysoxid)在纳米金修饰电极表面出现了氧化还原反应;[Fe(CN)6]3-/[Fe(CN)6]4-在三维自组装膜电极表面的电子传递速率是二维组装膜修饰电极的2.5倍;且纳米金表面的L-cys膜组装量随粒径的增加而增加。
(2) Au/GCE电极对NO2-的氧化反应表现出显著的电催化活性,响应峰电流是平面电极表面的1.6倍,并伴随有明显的氧化电位降低;NO2-的氧化过程受扩散步骤控制,传质系数α=0.3,同时不受溶液pH的影响;在1.0×10-5– 5.0×10-3 mol/L范围内,修饰电极表面的响应电流与NO2-浓度成很好的线性关系(r=0.9995),灵敏度为22.2μA/mmol·L-1;Au/GCE实现了对实际废水中NO2-浓度的准确测定,同时表现出良好的稳定性、抗干扰能力和明显的实际应用价值。
(3) Au/GCE电极对15种苯酚衍生物的电化学氧化过程表现出不同程度的电催化作用;与GCE和平面金电极相比,苯酚衍生物的氧化峰电流出现不同程度的增加,氧化电位的变化受待测物反应活性影响较大;修饰电极实现了对多种水中酚类物质的痕量测定;水杨酸在Au/GCE电极表面的响应迅速,响应灵敏度是GCE电极表面的1.8倍;同时建立了苯酚类衍生物在Au/GCE电极表面的氧化电位与分子结构参数之间的多元线性方程模型。
(4) Au/GCE电极对AA的氧化有明显的电催化作用,氧化电位比GCE表面降低了100 mV;实现了UA和AA氧化峰170 mV的分离;两者在修饰电极表面的分离效果受溶液pH影响显著,酸性条件有利于两者的同时测定;L-cysoxid/Au/GCE对AA的氧化有进一步的电催化作用;在pH为6.4时,UA和AA混合液在L-cysoxid/Au/GCE电极表面实现了150 mV的峰电位分离;L-cysoxid/Au/GCE电极对UA和AA的分离同样受到溶液pH的影响,但适用范围更宽,同时比Au/GCE电极具有更好的分离效果; L-cysoxid/Au/GCE修饰电极对UA和AA有较好的响应灵敏度,分别为10.065μA/mmol·L-1和18.101μA/mmol·L-1,线性检测范围:2.0×10-6– 1.0×10-3 mol/L。
(5) Cu2+在L-cys/Au/GCE表面有较好的响应电流;该氧化还原反应为表面控制过程,同时存在有质子得失,修饰电极在pH为7.0时具有最佳电流响应;L-cys膜的组装量对修饰电极的电流响应有显著影响;线性浓度测定范围:1.0 - 500.0μg/L;修饰电极具有良好的抗干扰能力、稳定性和重现性;3-巯基丙酸(3-MPA)三维自组装膜有效避免了溶出伏安法中的欠电位沉积(UPD)效应; pH对修饰电极同样存在明显的影响;在0.1 - 80.0μg/L的浓度范围内,3-MPA修饰电极表面的溶出电流-浓度成良好的线性关系(r=0.9993),且检测灵敏度比L-cys/Au/GCE在自然富集条件下的提高了10倍以上;3-MPA修饰电极实现了对实际水样中Cu2+的浓度测定,同时具有较好的重现性。
“seed-mediated gold nano-particles growth method”was introduced to electrode modification, and gold nano-particles modified glassy carbon electrode (Au/GCE) was prepared in this thesis. Based on Au/GCE, gold nano-particles and self-assembled monolayers were further combined in electrode modification to fabricate three-dimensional monolayer modified electrode. Field emission scanning electron microscope (FE-SEM), ultraviolet-visible (UV-vis) spectroscopy analysis and electroalaylsis were employed to study the morphology, structure of modified electrodes, and their electrochemical performances. Series of environmental-electrochemical sensors were prepared based on Au/GCE. These sensors have been successfully used in electrochemical determination of nitrite, phenolic compounds, uric acid (UA) and ascorbic acid (AA), and Cu2+. The main contents are listed as following:
(1) Gold nanoparticles modified glassy carbon electrode was fabricated successfully and the particle size was in the range of 50 to 90 nm. Electron transfer kinetics between the redox couple and the modified electrode interface was improved. The redox reaction of the oxidation product of L-cys assembled monolayer (L-cysoxid) could be observed on gold nano-particles, which has no faradaic current on planar gold. The unique three-dimensional monolayer structure could decrease the ordered and compact property of two-dimensional monolayer. Thus, the electron transfer kinetics of [Fe(CN)6]3-/[Fe(CN)6]4- on the former electrode was 2.5 higher than that on the latter electrode. In addition, the amount of L-cys monolayer was found to increase with the increase of the particle size.
(2) Excellent electrocatalytic activity for nitrite oxidation could be observed at Au/GCE. Compared with planar electrode, the response current of Au/GCE was 1.6 times as large as that of planar electrode, accompanied with the decrease of peak potential. The nitrite oxidation was controlled by the diffusion of nitrite to the Au/GCE electrode withα=0.3, and pH has no influence on the oxidation potential. The linear range of determination was 1.0×10-5– 5.0×10-3 mol/L with a regression coefficient of 0.9995. The sensitivity of modified electrode was 22.2μA/mmol·L-1. The accurate determination of nitrite in real wastewater was realized on Au/GCE with good long-term stability, anti-interfere ability and applicability.
(3) Au/GCE exhibited different electrocatalytic activity to the oxidations of 15 kinds of phenolic compounds. Their peak currents were all increased as compared with GCE and planar gold electrode. The oxidation potential was determined by the activity of analyte. Trace phenolic compounds determination could be realized on modified electrode. The prepared electrode had a good current response to salicylic acid, with good linear relationship to its concentration. And the response sensitivity was 1.8 fold than that obtained on GCE. Furthermore, the multiple linear regression model was developed for quantitative relationship between the electrochemical oxidation potential at modified electrode and molecular structures of phenolic compounds.
(4) The electrocatalytic activity of Au/GCE to the oxidation of AA was proved by the negative shift of oxidation potential with 100 mV. The oxidation peaks of UA and AA were divided on modified electrode with 170 mV separation, which only presented one fold peak on planar gold electrode. The pH presented prominence influence on separation and acidic solution could facilitate the simultaneous determination of UA and AA. And L-cysoxid/Au/GCE presented obviously electrocatalytic effect on AA oxidation. In 6.4 pH solution, 150 mV peak separation was observed on L-cysoxid/Au/GCE, which could not be realized on L-cysoxid/planar gold. Although the separation on L-cysoxid/Au/GCE was also influenced by pH, better separation and broader pH range were gained than that on Au/GCE. Response sensitivities of UA and AA on modified electrode were 10.065 and 18.101μA/mmol·L-1 respectively, in the concentration range of 2.0×10-6– 1.0×10-3 mol/L.
(5) Cu2+ exhibited a good electrochemical response on L-cys/Au/GCE and the best current response was obtained at 7.0 pH. And the amount of assembled L-cys had obvious effect on current response. The modified electrode presented good anti-interfere ability, stability and reproducibility with a linear detection range of 1.0μg/L-500.0μg/L. Under potential deposition (UPD) effect could be avoided and better current response could be obtained on three-dimensional 3-mercaptopropionic (3-MPA) monolayer in Cu2+ determination. And pH of supporting electrolyte had influence on response. Good linear relationship was obtained between response current and Cu2+ concentration in the range of 0.1-80.0μg/L. and the response sensitivity was improved by 10 fold than that obtained on L-cys/Au/GCE which was processed at open-circuit pre-concentration. And the concentration of Cu2+ in actual sample was determined at modified electrode with good reproducibility.
(1)实现了粒径为50-90 nm的纳米金修饰玻碳电极的制备;证明了纳米金粒子能有效促进电极表面的电子传递速率;发现L-半胱氨酸(L-cys)组装膜的电化学氧化产物(L-cysoxid)在纳米金修饰电极表面出现了氧化还原反应;[Fe(CN)6]3-/[Fe(CN)6]4-在三维自组装膜电极表面的电子传递速率是二维组装膜修饰电极的2.5倍;且纳米金表面的L-cys膜组装量随粒径的增加而增加。
(2) Au/GCE电极对NO2-的氧化反应表现出显著的电催化活性,响应峰电流是平面电极表面的1.6倍,并伴随有明显的氧化电位降低;NO2-的氧化过程受扩散步骤控制,传质系数α=0.3,同时不受溶液pH的影响;在1.0×10-5– 5.0×10-3 mol/L范围内,修饰电极表面的响应电流与NO2-浓度成很好的线性关系(r=0.9995),灵敏度为22.2μA/mmol·L-1;Au/GCE实现了对实际废水中NO2-浓度的准确测定,同时表现出良好的稳定性、抗干扰能力和明显的实际应用价值。
(3) Au/GCE电极对15种苯酚衍生物的电化学氧化过程表现出不同程度的电催化作用;与GCE和平面金电极相比,苯酚衍生物的氧化峰电流出现不同程度的增加,氧化电位的变化受待测物反应活性影响较大;修饰电极实现了对多种水中酚类物质的痕量测定;水杨酸在Au/GCE电极表面的响应迅速,响应灵敏度是GCE电极表面的1.8倍;同时建立了苯酚类衍生物在Au/GCE电极表面的氧化电位与分子结构参数之间的多元线性方程模型。
(4) Au/GCE电极对AA的氧化有明显的电催化作用,氧化电位比GCE表面降低了100 mV;实现了UA和AA氧化峰170 mV的分离;两者在修饰电极表面的分离效果受溶液pH影响显著,酸性条件有利于两者的同时测定;L-cysoxid/Au/GCE对AA的氧化有进一步的电催化作用;在pH为6.4时,UA和AA混合液在L-cysoxid/Au/GCE电极表面实现了150 mV的峰电位分离;L-cysoxid/Au/GCE电极对UA和AA的分离同样受到溶液pH的影响,但适用范围更宽,同时比Au/GCE电极具有更好的分离效果; L-cysoxid/Au/GCE修饰电极对UA和AA有较好的响应灵敏度,分别为10.065μA/mmol·L-1和18.101μA/mmol·L-1,线性检测范围:2.0×10-6– 1.0×10-3 mol/L。
(5) Cu2+在L-cys/Au/GCE表面有较好的响应电流;该氧化还原反应为表面控制过程,同时存在有质子得失,修饰电极在pH为7.0时具有最佳电流响应;L-cys膜的组装量对修饰电极的电流响应有显著影响;线性浓度测定范围:1.0 - 500.0μg/L;修饰电极具有良好的抗干扰能力、稳定性和重现性;3-巯基丙酸(3-MPA)三维自组装膜有效避免了溶出伏安法中的欠电位沉积(UPD)效应; pH对修饰电极同样存在明显的影响;在0.1 - 80.0μg/L的浓度范围内,3-MPA修饰电极表面的溶出电流-浓度成良好的线性关系(r=0.9993),且检测灵敏度比L-cys/Au/GCE在自然富集条件下的提高了10倍以上;3-MPA修饰电极实现了对实际水样中Cu2+的浓度测定,同时具有较好的重现性。
“seed-mediated gold nano-particles growth method”was introduced to electrode modification, and gold nano-particles modified glassy carbon electrode (Au/GCE) was prepared in this thesis. Based on Au/GCE, gold nano-particles and self-assembled monolayers were further combined in electrode modification to fabricate three-dimensional monolayer modified electrode. Field emission scanning electron microscope (FE-SEM), ultraviolet-visible (UV-vis) spectroscopy analysis and electroalaylsis were employed to study the morphology, structure of modified electrodes, and their electrochemical performances. Series of environmental-electrochemical sensors were prepared based on Au/GCE. These sensors have been successfully used in electrochemical determination of nitrite, phenolic compounds, uric acid (UA) and ascorbic acid (AA), and Cu2+. The main contents are listed as following:
(1) Gold nanoparticles modified glassy carbon electrode was fabricated successfully and the particle size was in the range of 50 to 90 nm. Electron transfer kinetics between the redox couple and the modified electrode interface was improved. The redox reaction of the oxidation product of L-cys assembled monolayer (L-cysoxid) could be observed on gold nano-particles, which has no faradaic current on planar gold. The unique three-dimensional monolayer structure could decrease the ordered and compact property of two-dimensional monolayer. Thus, the electron transfer kinetics of [Fe(CN)6]3-/[Fe(CN)6]4- on the former electrode was 2.5 higher than that on the latter electrode. In addition, the amount of L-cys monolayer was found to increase with the increase of the particle size.
(2) Excellent electrocatalytic activity for nitrite oxidation could be observed at Au/GCE. Compared with planar electrode, the response current of Au/GCE was 1.6 times as large as that of planar electrode, accompanied with the decrease of peak potential. The nitrite oxidation was controlled by the diffusion of nitrite to the Au/GCE electrode withα=0.3, and pH has no influence on the oxidation potential. The linear range of determination was 1.0×10-5– 5.0×10-3 mol/L with a regression coefficient of 0.9995. The sensitivity of modified electrode was 22.2μA/mmol·L-1. The accurate determination of nitrite in real wastewater was realized on Au/GCE with good long-term stability, anti-interfere ability and applicability.
(3) Au/GCE exhibited different electrocatalytic activity to the oxidations of 15 kinds of phenolic compounds. Their peak currents were all increased as compared with GCE and planar gold electrode. The oxidation potential was determined by the activity of analyte. Trace phenolic compounds determination could be realized on modified electrode. The prepared electrode had a good current response to salicylic acid, with good linear relationship to its concentration. And the response sensitivity was 1.8 fold than that obtained on GCE. Furthermore, the multiple linear regression model was developed for quantitative relationship between the electrochemical oxidation potential at modified electrode and molecular structures of phenolic compounds.
(4) The electrocatalytic activity of Au/GCE to the oxidation of AA was proved by the negative shift of oxidation potential with 100 mV. The oxidation peaks of UA and AA were divided on modified electrode with 170 mV separation, which only presented one fold peak on planar gold electrode. The pH presented prominence influence on separation and acidic solution could facilitate the simultaneous determination of UA and AA. And L-cysoxid/Au/GCE presented obviously electrocatalytic effect on AA oxidation. In 6.4 pH solution, 150 mV peak separation was observed on L-cysoxid/Au/GCE, which could not be realized on L-cysoxid/planar gold. Although the separation on L-cysoxid/Au/GCE was also influenced by pH, better separation and broader pH range were gained than that on Au/GCE. Response sensitivities of UA and AA on modified electrode were 10.065 and 18.101μA/mmol·L-1 respectively, in the concentration range of 2.0×10-6– 1.0×10-3 mol/L.
(5) Cu2+ exhibited a good electrochemical response on L-cys/Au/GCE and the best current response was obtained at 7.0 pH. And the amount of assembled L-cys had obvious effect on current response. The modified electrode presented good anti-interfere ability, stability and reproducibility with a linear detection range of 1.0μg/L-500.0μg/L. Under potential deposition (UPD) effect could be avoided and better current response could be obtained on three-dimensional 3-mercaptopropionic (3-MPA) monolayer in Cu2+ determination. And pH of supporting electrolyte had influence on response. Good linear relationship was obtained between response current and Cu2+ concentration in the range of 0.1-80.0μg/L. and the response sensitivity was improved by 10 fold than that obtained on L-cys/Au/GCE which was processed at open-circuit pre-concentration. And the concentration of Cu2+ in actual sample was determined at modified electrode with good reproducibility.
引文
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