基于联苯胺在预阳极化的铂电极上的催化氧化和不可逆电对的双安培检测原理,建立流动注射双安培直接检测联苯胺的新方法。使用经过恒电位预阳极化处理的双铂电极,在外加电压差为0.3V时,通过偶合联苯胺在一支电极上的氧化和氧化铂在另一支电极上的还原两个不可逆电极过程,建立一种快速准确的在线分析测定联苯胺的流动注射双安培检测法。结果表明:在pH5.2的KHC8H4O4-NaOH缓冲溶液中,外加电位差为0.3V时测得联苯胺的氧化电流与其浓度在8.0×10^-6~3.0×10^-3mol/L范围内呈线性关系(r=0.9962,n=11)。检出限为1.0×10^-6mol/L。连续20次测定1.0×10^-4mol/L的联苯胺溶液,电流值RSD=1.9%。电极的稳定性良好,常见无机离子和有机物均不干扰测定。用该方法对样品中联苯胺进行了测定,样品处理方法简单,且有很高的选择性和灵敏性。
A flow-injection electrochemical method for on-line determination of benzidine was established, which was based on the electrocatalytic oxidation of benzidine at an oxide modified platinum electrode and the principle of biamperometric determination of irreversible couple system. Using two preanodized platinum electrodes with the applied potential difference of 0.3 V, the biamperometric detection of system has been established by coupling the oxidation of benzidine and the reduction of platinum oxide. The results were as follows : the linear relationship between the oxidation current and concentration of benzidine was obtained in the range 8.0 ×10^-6mol/L - 3.0 ×10^-3 mol/L ( r = 0.9962, n = 11) with the detection limit of 1.0 ×10^-6mol/L in the potassium biphthalate-sodium hydroxide buffer solution (pH 5.2). The relative standard derivation was 1.9% for 20 successive determinations of 1.0 ×10^-4 mol/L benzidine. Most excipients do not interfere with the determination of benzidine. The method is sensitive, selective, rapid and suitable for the on-line determination of benzidine.