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本文对示波极谱法测定化探样品中钨、钼的方法从熔矿方式、体系酸度、测试温度、各底液浓度、平衡反应时间和共存物质的干扰与消除等方面进行了探讨和优化,钨的方法检出限为0.17μg/g,测定限0.51～200μg/g,钼的方法检出限为0.15μg/g,测定限0.45～150μg/g。方法经国家一级标准物质检验,测定结果与标准值吻合,方法精密度(RSD,n=12)钨、钼分别为:0.83%,2.81%。本法使测定灵敏度大为提高,且效率高、低成本、重复性好、测定结果准确可靠,已应用于大量的化探样品分析当中。
In this paper, the methods of oscillopolarographic determination of tungsten and molybdenum in geochemical exploration samples are discussed and optimized from aspects of melting method, system acidity, testing temperature, concentration of each end solution, equilibrium reaction time and interference of coexisting substances , The limit of detection of tungsten is 0.17μg / g, the limit of determination is 0.51 ~ 200μg / g, the limit of detection of molybdenum is 0.15μg / g and the limit of determination is 0.45 ~ 150μg / g. The method was tested by the national first-class reference materials. The measured results were in good agreement with the standard values. The precision of the method (RSD, n = 12) was 0.83% and 2.81% respectively. This method greatly enhances the sensitivity of the assay, and has the advantages of high efficiency, low cost, good repeatability, accurate and reliable determination results, and has been applied to a large amount of geochemical sample analysis.