贵金属元素电化学分析研究——ⅩⅣ.吸附-阳极溶出伏安法测定微量锇

• 作 者: 张玉祥 卢繁 郭永晴 马昭礼
• 机 构: 兰州大学化学系,兰州大学化学系,兰州大学化学系,兰州大学化学系 兰州 730000,兰州 730000,兰州 730000,兰州 730000
• 出 处: 分析化学
• 发表日期: 1991年02期
• 关键词: 阳极溶出伏安法 贵金属 电解质体系 电化学分析 极谱仪 催化极谱法 吸附剂 峰高 试样 工作电极

本文通过大量实验,研究了一种新的锇的最佳支持电解质体系为:1.3×10~(-3)mol/LCH_4N_2S-6.3×10~(-2)mol/L ClCH_2COOH-0.1mol/L NaAc(pH=4.39)。在该体系中,以硫脲作吸附剂,并在直流极谱仪上于+0.55V(vs.SCE)发现一锐敏的锇峰。如在该体系中含有AS_2O_3(0.25μg/ml)时,测定锇的线性范围从0.037～0.224μg/ml扩展到0.037～0.37μg/ml,这很适宜于用As_2O_3吸附蒸馏试样。方法的灵敏度达37ng/ml。本法已成功地用于精矿测定,结果与原含量相符。

In this paper, a series of experiments were carried out to study a new osmium electrolyte system which is as follows: 1.3 × 10 ~ (-3) mol / LCH_4N_2S-6.3 × 10 ~ (-2) mol / L ClCH_2COOH-0.1mol / L NaAc (pH = 4.39). In this system, thiourea was used as an adsorbent and a sharp osmium peak was found at + 0.55V (vs.SCE) on a DC polarometer. When AS_2O_3 (0.25μg / ml) was used in this system, the linear range of osmium was extended from 0.037 ~ 0.224μg / ml to 0.037 ~ 0.37μg / ml, which was very suitable for the adsorption and desorption of As2O3. The sensitivity of the method is 37 ng / ml. This Law has been successfully used in the determination of the concentrate, the result is consistent with the original content.