基于二苯乙醇酸体系快速测定区域地质矿产调查样品中的钨钼

本文建立了一种快速分析区域地质矿产调查样品中钨钼的方法。试样经高温焙烧、碱熔分解，钨、钼与其它杂质元素所形成的氢氧化物沉淀分离；在二苯乙醇酸体系(0.25mol/L硫酸-0.04g/L二苯乙醇酸-0.10g/L二苯胍-20g/L氯酸钠)中，钼、钨分别于约-0.25V、-0.85V产生灵敏的平行催化波，根据极限扩散电流的大小同时测定这两种元素。该方法的测定下限(X0+3S)<0.10×10-6；准确度(|Δlog|)≤0.05；精密度(RSD)≤7.72%。国家标准物质测定值与标准值相符；实际样品测定值优于电感耦合等离子体发射质谱法。方法扩大了催化极谱法的适应性，提高了实际应用价值。

Catalytic polarography based on the benzilic acid system for fast determination of tungsten and molybdenum in samples from regional geological surveys.

This work developed a method for fast determination of tungsten(W) and molybdenum(Mo) in samples from regional geological surveys using catalytic polarography based on the benzilic acid system. Elements W and Mo are separated from precipitation of hydroxide of other heavy metals, which are developed by high-temperature calcined, alkali fusion. In the presence of benzilic acid system(0.25mol/L sulfuric,0.04g/L benzilic acid, 0.10g/L melaniline, and 20g/L sodium chlorate), the sensitive polarographic catalytic waves are generated at -0.25V and -0.85V for W and Mo, respectively, thus leading to a high limiting diffusion current signal. The limiting diffusion current intensity of the method increases with the increase of target ion concentration. Detection limits are 0.086×10-6 (ug/g) and 0.099×10-6 (ug/g) for W and Mo, respectively. Relative standard deviations measured on the certified reference materials are in the ranges 1.7%-7.7% and 2.6%-5.8% (N=12), respectively. The determination of trace W and Mo in real samples by this method is superior to the inductively coupled plasma-mass spectrometry. This new approach expands the adaptability of catalytic polarography and enhances its application values.