本文關(guān)鍵詞：石墨烯修飾電極電化學檢測磺胺二甲基嘧啶方法的研究　出處：《山西農(nóng)業(yè)大學》2016年碩士論文　論文類型：學位論文

  更多相關(guān)文章： 石墨烯修飾電極 電化學檢測 磺胺二甲基嘧啶

【摘要】：本文以磺胺二甲基嘧啶為檢測對象,探索了利用電化學法檢測磺胺二甲基嘧啶,對磺胺二甲基嘧啶在石墨烯修飾電極上的電化學行為進行了研究,探究了電化學法檢測磺胺二甲基嘧啶的影響因素,作為一種新的檢測方法為今后磺胺二甲基嘧啶殘留的檢測提供理論依據(jù)。實驗的研究結(jié)果如下：1)從金、鉑、玻碳(Au、Pt、GC)三種電極中選擇檢測磺胺二甲基嘧啶的最佳工作電極,結(jié)果表明磺胺二甲基嘧啶在以玻碳電極為工作電極的電化學信號最明顯。2)以石墨烯為工作電極的修飾材料,用循環(huán)伏安法(CV)進行測定,對比磺胺二甲基嘧啶在不同裸電極(Au、Pt、GC)和石墨烯修飾電極上的電化學行為。研究發(fā)現(xiàn),以石墨烯為修飾材料制備出的電化學傳感器,磺胺二甲基嘧啶的陽極電流響應(yīng)明顯提高,選用玻碳電極用于后續(xù)研究。3)對電化學檢測磺胺二甲基嘧啶的實驗條件進行篩選和優(yōu)化,包括支持電解質(zhì)、pH、掃速等參數(shù)的影響。實驗結(jié)果表明測定磺胺二甲基嘧啶的最佳電解質(zhì)為pH=3.5的0.05 mol/L醋酸緩沖溶液,氧化峰電流與掃速在10～150 mV/s范圍內(nèi)呈線性相關(guān)。4)用滴涂法和電化學沉積法修飾工作電極,對比兩種修飾方法。結(jié)果表明：滴涂法修飾電極的最佳修飾劑量為30μL,用電化學沉積法制作的修飾電極不易脫落且效果明顯優(yōu)于滴涂法制作的修飾電極。5)用方波伏安法(SWV)、計時安培電流法(i-t)對不同濃度的磺胺二甲基嘧啶溶液進行了測定。結(jié)果表明方波伏安法檢測磺胺二甲基嘧啶,電流信號與濃度在5.0×10~(-6)～1.0×10~(-3)mol/L范圍內(nèi)線性關(guān)系良好,相關(guān)系數(shù)R為0.99512,線性相關(guān)方程為i(μA)=7.905+1.284 LgC (μmol/L),檢出限為3.0×10~(-6)mol/L;計時安培電流法(i-t)測定磺胺二甲基嘧啶,電流信號與濃度在7.0×10~(-7)～5.9×10~(-5) mol/L范圍內(nèi)線性關(guān)系良好,相關(guān)系數(shù)R為0.99921,線性相關(guān)方程為i(μA)=0.1245+0.01815×C (μmol/L),檢出限為5.0×10~(-7) mol/L,計時安培電流法的檢出限低于方波伏安法。6)利用計時安培電流法對豬飼料樣品進行測定,電流信號與濃度在3.0x10~(-7)～2.3 ×10~(-5) mol/L濃度范圍內(nèi)線性關(guān)系良好,檢出限為5.3×10-9mol/L,目關(guān)系數(shù)R為0.99843,線性方程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)).
【學位授予單位】：山西農(nóng)業(yè)大學
【學位級別】：碩士
【學位授予年份】：2016
【分類號】：O657.1

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