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本工作主要是试验了用磷酸溶样,在氨性介质中测定微量镍的方法。实验结果确定:①矿样经磷酸分解后,加入氯化钡,在氨性介质中进行示波极谱测定镍,可消除大量铬和铁等离子的干扰。介质最佳条件是3.6M NH_4OH—0.25M Na_2SO_3(50毫升溶液中)。②为保证50毫克矿样完全分解,磷酸的使用量为1毫升,在50毫升溶液中的浓度为0.27M。磷酸浓度大于0.32M时,镍的测定结果偏低。氯化钡的用量可高达1.1M;当其浓度为0.32M对,50毫克铁在氨性介质中沉淀完全,但大于此量时,镍的测定结果稍偏低。③126毫克三氧化二铬、13毫克钴、0.5毫克钒不影响镍的测定;高于此量时,镍的测定结果稍偏高。铜(Ⅱ)、镉(Ⅱ)、
This work is mainly tested with phosphoric acid solution, ammonia in the determination of trace nickel method. The experimental results confirm: (1) After the sample is decomposed by phosphoric acid, the barium chloride is added and the oscillopolarographic determination of nickel in ammoniacal medium can eliminate the interference of a large amount of chromium and iron plasma. The best conditions of the medium is 3.6M NH 4 OH 0.25M Na 2 SO 3 (in 50 ml solution). ② In order to ensure complete decomposition of 50 mg of mineral sample, the use of phosphoric acid was 1 ml, the concentration in 50 ml of solution was 0.27M. When the phosphoric acid concentration is more than 0.32M, the result of nickel measurement is low. The amount of barium chloride can be as high as 1.1M; when its concentration is 0.32M, 50 mg of iron is completely precipitated in ammonia medium, but when it is more than this amount, the determination result of nickel is slightly lower. ③ 126 mg chromium oxide, 13 mg cobalt, 0.5 mg vanadium does not affect the determination of nickel; above this amount, the results of the nickel slightly higher. Copper (Ⅱ), cadmium (Ⅱ),