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本文用导数极谱法研究了氯化氧锆在0.1N 氯化钾底液中的极谱行为,克服了经典极谱法中氢波的干扰。利用 pH 作为溶液稳定情况的标志,发现:当溶液未经放置至 pH 稳定以前,锆的波高与浓度不成正比,经放置至 pH 稳定后才成正比。若先加氢氧化钾调节 pH 至固定值再作图可以缩短建立此正比关系所需的放置时间。若取新配的并加热至 pH 稳定的溶液,先加硷调节 pH 至固定值再作图则可不经放置立即测定,符合实用要求。方法简便迅速,不需通气除氧,不需加极大抑制剂,不需特殊试剂,已初步证实可用于铜合金中锆的直接测定。新配的 pH 未稳定的溶液,锆的 E_(1/2)随 pH 减小而向负移。放置一段时间至 pH 已稳定的溶液,共 E_(1/2)与氢离子浓度成直线关系。若先加硷调节 pH 至固定值再作图,则 E_(1/2)基本固定,仅畧随锆浓度增大而向负移。此外,本文对不同支持电解质进行了试验,并提出了在一定条件下有第二个锆波出现的看法。
In this paper, the polarographic behavior of zirconyl chloride in 0.1N potassium chloride solution was studied by the derivative polarographic method, which overcomes the interference of hydrogen wave in the classical polarographic method. Using pH as a sign of solution stability, it was found that the wave height of zirconium was not proportional to the concentration until the solution was stable to pH before it was stable until it became stable. If potassium hydroxide is added to adjust the pH to a fixed value before plotting, the time required to set up this proportional relationship can be shortened. If you take a new and heated to a stable solution of pH, pH first to adjust the pH to a fixed value and then plotting can be measured immediately without placing, in line with practical requirements. The method is simple and rapid, does not need aeration oxygen, without adding a great inhibitor, without special reagents, has been initially confirmed for direct determination of zirconium in copper alloys. The new solution of pH is not stable, zirconium E_ (1/2) negative shift with decreasing pH. After a period of time to pH has been stable solution, a total of E_ (1/2) and hydrogen ion concentration in a linear relationship. If the first increase in pH adjusted to a fixed value and then plotting, then E_ (1/2) is basically fixed, only 畧 with zirconium concentration increases and negative shift. In addition, different supporting electrolytes were tested in this paper, and the opinion of the second zirconium wave appeared under certain conditions.