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用悬汞滴电极吸附阴极溶出伏安法测定了与试铝灵{3-[双(3-羧基-4-羟基-苯基)甲撑]-6-氧代-1,4-环已二烯-1-羧酸三铵盐}络合的U~(6+)。在试铝灵和脲存在下,一次扫描就可同时测定微量U~(6+)和Zn~(2+)。发现最佳测量条件是:累积时间,180~200s,累积电位,50mV(相对于Ag/Ag U电极);扫描速率,40mV·s~(-1);支持电解质,0.1mol·L~(-1)醋酸钠缓冲溶液,pH 6.5~7.0;试铝灵浓度,1×10~(-6)mol·L~(-1)。分别在2~33ng·ml~(-1)和30~120ng·ml~(-1)浓度范围内观测到真U~(6+)和Zn~(2+)的线性范围。检测限(S/N=3)是0.2ng·ml~(-1)(U)和30ng·ml~(-1)(Zn)。再现性良好,RSD=2.5%~4.0%(n=10)。采用脲掩蔽某些金属离子,该法具有较高选择性。
The results of cyclic voltammetry and cathodic stripping voltammetry were compared with those of the experimental aluminum ({3- [bis (3-carboxy-4-hydroxy-phenyl) Ene-1-carboxylic acid triammonium salt} complex U ~ (6+). In the presence of test alum and urea, trace amounts of U ~ (6+) and Zn ~ (2+) can be simultaneously measured in one scan. The best measurement conditions were as follows: cumulative time, 180 ~ 200s, cumulative potential, 50mV (relative to Ag / Ag U electrode); scan rate, 40mV · s -1; supporting electrolyte, 0.1mol·L ~ 1) sodium acetate buffer solution, pH 6.5 ~ 7.0; test aluminum concentration, 1 × 10 ~ (-6) mol·L -1. The linear ranges of true U ~ (6 +) and Zn ~ (2+) were observed in the range of 2 ~ 33ng · ml ~ (-1) and 30 ~ 120ng · ml ~ (-1) respectively. The limits of detection (S / N = 3) were 0.2 ng · ml -1 and 30 ng · ml -1 Zn. Good reproducibility, RSD = 2.5% ~ 4.0% (n = 10). The use of urea to mask some metal ions, the method has a high selectivity.