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本文探讨了用催化容量法测定矿石中的微量锇和钌。利用在硫酸介质中微量锇或钌对四价铈和三价砷的催化反应,经过一定时间后,可加入一定量的亚铁,把催化反应过程中剩余的四价铈还原,使催化反应停止,然后用四价铈反滴定过量的亚铁,求出催化反应过程中剩余四价铈的量(以V表示)。实验结果指出,在10毫升2当量的硫酸溶液中,四价铈和三价砷的开始浓度分别为0.02和0.15当量,硫酸汞为0.2％,反应温度为25°.0C时,微量锇和钉的催化反应均为一级反应。当催化反应的时间固定为10分钟,并以1-logV对锇钉浓度作标准曲线,指出,锇的量在0—0.040微克,钌在0—0.0125微克,线性关系均良好。如样品中锇、钌的含量较大或较小时,可用缩短或延长催化时间的办法来绘制校准曲线,其线性关系仍然很好。
In this paper, the determination of trace osmium and ruthenium in ore by catalytic volumetric method is discussed. The use of a trace of osmium or ruthenium in sulfuric acid medium catalytic reaction of tetravalent cerium and trivalent arsenic, after a certain period of time, a certain amount of ferrous can be added, the catalytic reaction of the remaining tetravalent cerium reduction, the catalytic reaction is stopped , Followed by titration of excess ferrous iron with tetravalent cerium to determine the amount of tetravalent cerium remaining in the catalytic reaction (in V). The experimental results show that in 10 ml of 2 equivalent sulfuric acid solution, the starting concentrations of tetravalent cerium and trivalent arsenic were 0.02 and 0.15 equivalents of mercury sulfate was 0.2%, the reaction temperature was 25 ° .O0C, trace osmium and nails The catalytic reactions are first-order reaction. When the time of the catalytic reaction was fixed at 10 minutes and the concentration of osmium pestis was determined by 1-logV, it was found that the osmium concentration was 0-0.040 micrograms and the ruthenium was 0-0.0125 micrograms. The linear relationship was good. If the samples contain large or small amounts of osmium and ruthenium, the calibration curve can be drawn by shortening or prolonging the catalytic time, and the linearity is still good.