极谱法测定钼矿石中的总钼氧化钼硫化钼

钼的物相分析要求测定硫化矿物相和氧化矿物相,常用比色法和电感耦合等离子体发射光谱法等对辉钼矿、钼华矿、钼钨钙矿、钼酸铅矿等钼矿石进行物相分析,但分离物相的品种较多,方法繁琐耗时。本文用王水-硫酸消解钼矿石样品,碱溶液复溶浸提得到钼总量,使其他大多数元素形成沉淀而分离,用碳酸钠-氢氧化铵混合溶液浸取钼的氧化矿物,将残渣进一步溶解得到硫化矿物含量,在硫酸-氯酸钾-二苯羟乙酸体系中用极谱法简单快速测定钼总量、氧化钼和硫化钼含量。方法的线性范围为0.04~0.4 mg/L,检出限为0.028 mg/L。对三种钼矿样品进行物相分析,氧化矿物与硫化矿物含量的加和与钼总量相当;总钼、氧化钼、硫化钼测定结果的相对标准偏差在1.69%~3.56%之间,与比色法测定结果相符。方法实用快速,易于推广,适于实际批量样品的测试。

Determination of Total Molybdenum, Molybdic Oxide and Molybdenum Sulfide in Molybdenum Ore by Polarography

Molybdenite is the major mineral in molybdenum ore. The phase analysis of molybdenum ore is required to determine sulfide minerals and oxide minerals. The phase analyses of molybdenum ores such as molybdenite, molybdite, powellite and molybdate galena were taken by photometry and Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES). In this paper, the molybdenum ore sample was dissolved with aqua regia-sulfuric acid. The total molybdenum was extracted by alkali solution and the majority of the other elements were separated by precipitation. Molybdic oxides were leached by sodium carbonate and ammonium hydroxide solution. Molybdenum sulfides were obtained to dissolve residue. The contents of total molybdenum, molybdic oxide and molybdenum sulfide were determined by rapid polarography in a sulfuric acid-potassium chlorate-diphenyl glycollic acid system. The linear range of the method was 0.04-0.4 mg/L, and the detection limit was 0.028 mg/L. Three molybdenum ore samples were carried on phase analysis and the results were consistent with those obtained by photometry. The sum contents of molybdic oxide and molybdenum sulfide conformed to the total molybdenum content. RSDs (n=8) were 1.69%-3.56% for total molybdenum, molybdic oxide and molybdenum sulfide. This method was fast and suitable for practical batch samples.