石墨烯修饰电极电化学检测磺胺二甲基嘧啶方法的研究

发布时间：2018-01-01 23:33

本文关键词：石墨烯修饰电极电化学检测磺胺二甲基嘧啶方法的研究　出处：《山西农业大学》2016年硕士论文　论文类型：学位论文

【摘要】：本文以磺胺二甲基嘧啶为检测对象,探索了利用电化学法检测磺胺二甲基嘧啶,对磺胺二甲基嘧啶在石墨烯修饰电极上的电化学行为进行了研究,探究了电化学法检测磺胺二甲基嘧啶的影响因素,作为一种新的检测方法为今后磺胺二甲基嘧啶残留的检测提供理论依据。实验的研究结果如下：1)从金、铂、玻碳(Au、Pt、GC)三种电极中选择检测磺胺二甲基嘧啶的最佳工作电极,结果表明磺胺二甲基嘧啶在以玻碳电极为工作电极的电化学信号最明显。2)以石墨烯为工作电极的修饰材料,用循环伏安法(CV)进行测定,对比磺胺二甲基嘧啶在不同裸电极(Au、Pt、GC)和石墨烯修饰电极上的电化学行为。研究发现,以石墨烯为修饰材料制备出的电化学传感器,磺胺二甲基嘧啶的阳极电流响应明显提高,选用玻碳电极用于后续研究。3)对电化学检测磺胺二甲基嘧啶的实验条件进行筛选和优化,包括支持电解质、pH、扫速等参数的影响。实验结果表明测定磺胺二甲基嘧啶的最佳电解质为pH=3.5的0.05 mol/L醋酸缓冲溶液,氧化峰电流与扫速在10～150 mV/s范围内呈线性相关。4)用滴涂法和电化学沉积法修饰工作电极,对比两种修饰方法。结果表明：滴涂法修饰电极的最佳修饰剂量为30μL,用电化学沉积法制作的修饰电极不易脱落且效果明显优于滴涂法制作的修饰电极。5)用方波伏安法(SWV)、计时安培电流法(i-t)对不同浓度的磺胺二甲基嘧啶溶液进行了测定。结果表明方波伏安法检测磺胺二甲基嘧啶,电流信号与浓度在5.0×10~(-6)～1.0×10~(-3)mol/L范围内线性关系良好,相关系数R为0.99512,线性相关方程为i(μA)=7.905+1.284 LgC (μmol/L),检出限为3.0×10~(-6)mol/L;计时安培电流法(i-t)测定磺胺二甲基嘧啶,电流信号与浓度在7.0×10~(-7)～5.9×10~(-5) mol/L范围内线性关系良好,相关系数R为0.99921,线性相关方程为i(μA)=0.1245+0.01815×C (μmol/L),检出限为5.0×10~(-7) mol/L,计时安培电流法的检出限低于方波伏安法。6)利用计时安培电流法对猪饲料样品进行测定,电流信号与浓度在3.0x10~(-7)～2.3 ×10~(-5) mol/L浓度范围内线性关系良好,检出限为5.3×10-9mol/L,目关系数R为0.99843,线性方程i(μA)=0.29323+0.03086×C(μAmol/L)。
[Abstract]:In this paper, sulfadimethylpyrimidine was used to detect sulfadimethylpyrimidine by electrochemical method, and the electrochemical behavior of sulfamethazine on graphene modified electrode was studied. The factors affecting the detection of sulfamethylpyrimidine by electrochemical method were investigated. As a new method, it provides a theoretical basis for the detection of sulfadimethazine residues in the future. The experimental results are as follows: 1) gold. The best working electrode for the detection of sulfadimethazine was selected among the platinum, glassy carbon auttidine (PtGC) electrodes. The results showed that the electrochemical signal of sulfadimethylpyrimidine at glassy carbon electrode was the most obvious. 2) graphene was used as the modified material of the working electrode and was determined by cyclic voltammetry (CV). The electrochemical behavior of sulfadimethylpyrimidine on different bare electrode Au-PtPtGC) and graphene modified electrode was compared. The electrochemical sensor prepared with graphene as the modified material was found. The anodic current response of sulfadimethylpyrimidine was improved significantly. Glassy carbon electrode was used for further study. 3) the experimental conditions for electrochemical detection of sulfadimethazine were selected and optimized, including supporting electrolyte. The results showed that the best electrolyte for the determination of sulfadimethylpyrimidine was 0.05 mol/L acetic acid buffer solution of pH=3.5. The oxidation peak current was linearly correlated with the sweep velocity in the range of 10 ~ 150 mV/s. 4) the working electrode was modified by drop coating method and electrochemical deposition method. The results showed that the optimal modification dose of the modified electrode was 30 渭 L. The modified electrode prepared by electrochemical deposition method is not easy to fall off and the effect is obviously better than that of the modified electrode prepared by drop coating method. 5) the square wave voltammetry (SWV) method is used to fabricate the modified electrode. Different concentrations of sulfadimethylpyrimidine were determined by chronoamperometric amperometric method. The results showed that the square wave voltammetry was used to detect sulfamethylpyrimidine. There is a good linear relationship between the current signal and the concentration in the range of 1.0 脳 10 ~ (-1) ~ (-3) mol / L, the correlation coefficient R is 0.99512. The linear correlation equation is I (渭 A) 7.905 1.284 LgC (渭 mol / L), and the detection limit is 3.0 脳 10 ~ (-1) -6 mol / L; The linear relationship between the current signal and the concentration of sulfadimethylpyrimidine was found in the range of 7.0 脳 10 ~ (-7) ~ (7) ~ (5) 脳 10 ~ (10) ~ (-5) mol/L for the determination of sulfamethylpyrimidine by amperometric amperometric method. The correlation coefficient R is 0.99921, and the linear correlation equation is I (渭 Acanine 0.1245 0.01815 脳 C) (渭 mol / L). The detection limit was 5.0 脳 10 ~ (-7) mol / L, and the detection limit of chronoamperometric method was lower than that of square wave voltammetry. The linear relationship between the current signal and the concentration is in the range of 3.0 脳 10 ~ (-7) mol/L), and the detection limit is 5.3 脳 10 ~ (-9) mol / L. The linear equation I (渭 A) is 0.29323 0.03086 脳 C (渭 Amolr / L ~ (1)).
【学位授予单位】：山西农业大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O657.1

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