摘要：锆钛砂矿是一种极难消解的矿物，除氢氟酸外，几乎不溶于所有的酸，由于矿物中铪、钛、锆含量高，而铪、钛、锆又易水解形成难溶的偏铪酸、偏钛酸、偏锆酸析出，样品前处理给定量分析带来很大困难。传统的化学法繁琐费时，且只能进行锆(铪)合量的分析。本文建立了电感耦合等离子体发射光谱法(ICP-AES)测定锆钛砂矿样品中铪、钛、锆的方法。通过筛选四种溶矿方法，确定在刚玉坩埚中用过氧化钠于700℃时熔融样品，硝酸-EDTA浸取盐分前处理矿物，利用EDTA的强络合性质可使铪、钛、锆形成稳定的可溶络合物，制备出有代表性的样品溶液；在ICP-AES分析中，采用Re作为内标和大的高频功率消除了基体效应的影响。方法的精密度(RSD，n=11)低于1.3%，Hf、Ti、Zr的检出限分别为0.97 μg/g、0.86 μg/g、0.33 μg/g。实际样品的测定值与化学分析方法和X射线荧光光谱法的测定结果基本吻合。。本方法采用刚玉坩埚熔矿，提高了样品处理数量，降低了分析成本，适用于难熔锆钛砂矿样品的快速定量分析。

Determination of Hf, Ti and Zr in Zirconium-Titanium Placer by Inductively Coupled Plasma-Atomic Emission Spectrometry

ABSTRACT Zirconium titanium placer is an ore which is extremely difficult to be digested. It is almost insoluble in all kind of acid except HF. Moreover, Hf, Ti and Zr in the ore tends to hydrolyze to form insoluble partial hafnium acid, metatitanic acid and zirconium hydroxide which increases the difficulty for their qualitative determination. The traditional chemical method can only yield total amounts of Zr and Hf and involve a complex time-consuming chemical procedure. After comparing four different methods to melt the sample, it was found that extracting salt with HNO₃-EDTA and melting the sample with Na₂O₂ at 700℃ was a simple, highly efficient and practical method for sample digestion. Based on this melting method, an Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) method was set up for Hf, Ti and Zr detection in zirconium titanium placer. Re was used as an internal standard and high frequency power was applied to eliminate the matrix effect. The RSD (n=11) was less than 1.3% and the detection limits for Hf, Ti and Zr were 0.97, 0.86 and 0.33 μg/g, respectively. The results were much more precise and accurate than the traditional chemical method and X-ray Fluorescence Spectrometry. The method of melting the sample in a corundum crucible increased the number of samples and reduced the cost, which is beneficial for the fast determination of insoluble Zr-Ti placer samples.