Phase Analysis of Molybdenum Ores and Determination of Molybdenum by Catalytic Polarography
摘 要
为测定钼矿中钼的总量,将矿样与盐酸加热后加硝酸-硫酸(8+2)混合酸蒸发冒烟至干。用150 g·L-1氢氧化钠溶液溶解残渣取代了常用的碱融熔法,在所得上清液中测定总钼量。为溶解钼矿中不同相态,另取一份矿样先用氨水处理以溶解钼华矿(MoO3),在每次分相溶解中所得的残渣先后用40 g·L-1酒石酸溶液和150 g·L-1碳酸钠溶液处理依次溶解出钼钨钙矿[Ca(W,Mo)O4]和钼酸铅矿(PbMnO4),在溶解分去钼酸铅矿后的残渣中存在有辉钼矿(MoS2)。将其在580 ℃灼烧后按测定总钼的溶解方法处理,在所得溶液中测定辉钼矿的钼量。采用催化极谱法测定上述各溶液中的钼量,所用底液为含有氯酸钾、二苯羟乙酸、二苯胍及硫酸的混合液。按所提方法分析了3个钼矿标准样品,所测得每一试样中各物相中钼量之和与该样品的总钼量测定值一致,其相对标准偏差(n=5)均小于3.5%。
Abstract
For determination of total molybdenum in its ores, the sample was heated with HCl and fumed with mixed acid of HNO3 and H2SO4(8+2) to dryness. Instead of the alkali fusion, the residue was treated with 150 g·L-1 NaOH solution to transform molybdenum into molybdate, and content of total molybdenum was determined in the supernatant. For dissolution of different phases of molybdenum ore, a separate sample was first heated with aqueous ammonia to dissolve the molybdite (MoO3), and insoluble residues obtained from each step of dissolution were treated with 40 g·L-1 tartaric acid solution and 150 g·L-1 Na2CO3 solution in succession to separate the phases of calcitungstomolyoxide [Ca(W,Mo)O4] and lead molybdate (PbMoO4) respectively. The molybdenite (MoS2) was in the residue remained after dissolution of PbMoO4, and it was ignited at 580 ℃ and then treated in the same way as for determination of total molybdenum with HCl-HNO3-H2SO4 and NaOH solution, as described above. Finally, contents of molybdenum in each of the above mentioned solutions were determined by catalytic polarography in a base solution containing KClO3, diphenylglycollic acid, diphenyl guanidine and H2SO4. In the analysis of 3 standard samples of molybdenum ores, contents of sum of the 4 ore phases were found to check quite well with the contents of total molybdenum found, with values of RSD′s (n=5) less than 3.5%.
中图分类号 O657.14
所属栏目 工作简报
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收稿日期 2011/8/31
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联系人作者李清昌(may927@163.com)
备注李清昌(1966-),男,辽宁瓦店人,高级工程师,主要从事地质样品分析。
引用该论文: LI Qing-chang,XUE Jing. Phase Analysis of Molybdenum Ores and Determination of Molybdenum by Catalytic Polarography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(4): 420~422
李清昌,薛静. 钼矿石物相分析及催化极谱法测定钼[J]. 理化检验-化学分册, 2012, 48(4): 420~422
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参考文献
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【3】施小英.电感耦合等离子体原子发射光谱法应用于钼矿石物相分析[J].理化检验-化学分册, 2010,46(1):79-80,83.
【4】GB/T14352.2-1993钨矿石、钼矿石化学分析方法-硫氰酸盐光度法测定钼量[S].
【5】孙伟,王小治,盛海君.钼的测定方法研究进展[J].安徽农业科学, 2007,35(31):9845-9846.
【6】张世涛,徐艳秋,王宇.ICP-AES同时测定钼矿石中多种元素[J].光谱实验室, 2006,23(5):1043-1045.
【7】马永灵.催化波极谱法测定化探样品中的钨钼[J].青海国土经略, 2008(4):40-41.
【8】郑日云.催化极谱法同时测定岩石、矿物中微量钨和钼[J].矿产与地质, 1985,5(2):95-98.
【9】施小英.电感耦合等离子体原子发射光谱法测定钼原矿及钼精矿中钼[J].理化检验-化学分册, 2010,46(3):322-323.
【10】周天泽,邹洪.原子光谱样品处理技术[M].北京:化学工业出版社, 2006:21-38.
【11】贾玉萍,王湘玲,肖建平.改进的极谱法测定化探样品中的钨钼[J].岩矿测试, 2009,28(5):494-496.
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