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在柠檬酸铵-盐酸羟胺底液中,在示波极谱上观察到钴-丁二肟络合物的催化波,峰电位为-1.2伏(相对饱和甘汞电极)。波高随钴的浓度和盐酸羟胺的浓度增加而增高。当控制盐酸羟胺浓度一定时,可进行微量钴的测定。溶液pH在8~10对波高影响不大。在选定的底液条件下,最低可测0.1微克钴/30毫升;测定的线性范围是0.1~10微克/30毫升;10毫克锰,1毫克铬、钒、铜、锌,0.5毫克铁,0.3毫克镍不影响钴(10微克)的测定;大量铁使结果偏低,在微酸性溶液中(pH2.5~3.5)使铁以氟化物沉淀分离可以消除其干扰。方法快速,重现性较好,具有较高的灵敏度,适用于矿石及高纯物质中微量钴的测定。
The catalytic wave of the cobalt-butadiene dioxime complex was observed on the oscillopolarography in ammonium citrate-hydroxylamine hydrochloride, with a peak potential of -1.2 volts (vs. saturated calomel electrode). Wave height increases with increasing cobalt concentration and hydroxylamine hydrochloride concentration. When a certain concentration of hydroxylamine hydrochloride control, the determination of trace cobalt can be carried out. Solution pH at 8-10 has little effect on wave height. In the selected bottom conditions, the lowest measurable 0.1 micrograms of cobalt / 30 ml; Determination of the linear range of 0.1 to 10 micrograms / 30 ml; 10 mg of manganese, 1 mg of chromium, vanadium, copper, zinc, 0.5 mg of iron, 0.3 mg of nickel does not affect the determination of cobalt (10 μg); large amounts of iron lead to low results; iron is separated by fluoride precipitation in a slightly acidic solution (pH 2.5 to 3.5) to eliminate interference. The method is rapid, reproducible and has high sensitivity, suitable for the determination of trace cobalt in ores and high purity materials.