铈量法快速测定镍钼矿硫酸介质加压浸出液中的钼
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摘要
镍钼浸出液中的大量Fe2+和Fe3+,采用氢氧化钠沉淀分离,以消除铈量法在测定钼时产生的干扰。通过在钼标准中加入Ni试验证明,测定体系中存在大量Ni 2+时,不干扰钼的测定。用草酸-硫酸联氨将Mo6+还原至Mo5+,用次甲基蓝作氧化促进剂,加快了滴定时的反应速度,终点突跃明显。拟定方法的样品加标回收率为95.0%~103.5%,相对标准偏差均<1%。在实际测定中,方法快速准确,值得推荐。
The sodium hydroxide precipitation method was used to separate a large number of Fe2+and Fe3+in the nickel-molybdenum leaching solution,so that the interference from the Fe2+and Fe3+to the determination of molybdenum can be eliminated.The test for addition of Ni to molybdenum standard assay system proved that the presence of large amounts of Ni 2+does not interfere with the determination of molybdenum.By using oxalic acid-sulfuric acid hydrazine to reduce Mo6+to Mo5+and together with the use of methylene blue as a pro-oxidant,the speed of the reaction are accelerated and the titration end point jump become more sharply.The addition recovery of the proposed method were between 95.0% to103.5%and the relative standard deviation was<1%.In the practical measurement,the method is fast and accurate.It is worth to recommend the method.
The sodium hydroxide precipitation method was used to separate a large number of Fe2+and Fe3+in the nickel-molybdenum leaching solution,so that the interference from the Fe2+and Fe3+to the determination of molybdenum can be eliminated.The test for addition of Ni to molybdenum standard assay system proved that the presence of large amounts of Ni 2+does not interfere with the determination of molybdenum.By using oxalic acid-sulfuric acid hydrazine to reduce Mo6+to Mo5+and together with the use of methylene blue as a pro-oxidant,the speed of the reaction are accelerated and the titration end point jump become more sharply.The addition recovery of the proposed method were between 95.0% to103.5%and the relative standard deviation was<1%.In the practical measurement,the method is fast and accurate.It is worth to recommend the method.
引文
[1]吴良士,白鸽,袁忠信.矿产原料手册[M].北京:化学工业出版社,2007:85-90.
[2]何美容,罗喜清,陈君.钼铁中钼的快速分析方法[J].中国无机分析化学,2011,1(3):53-54.
[3]北京矿冶研究总院.矿石及有色金属分析手册[M].北京:冶金工业出版社,2007:81-82.
[4]李荣志,左文家,王鑫.EDTA络合滴定法测定钼精矿中钼含量[J].品牌与标准化,2012(4):39.
[5]施先义.氯化亚锡-硫酸肼-硫酸铈滴定法测定铁[J].分析实验室,2002(2):21.
[2]何美容,罗喜清,陈君.钼铁中钼的快速分析方法[J].中国无机分析化学,2011,1(3):53-54.
[3]北京矿冶研究总院.矿石及有色金属分析手册[M].北京:冶金工业出版社,2007:81-82.
[4]李荣志,左文家,王鑫.EDTA络合滴定法测定钼精矿中钼含量[J].品牌与标准化,2012(4):39.
[5]施先义.氯化亚锡-硫酸肼-硫酸铈滴定法测定铁[J].分析实验室,2002(2):21.