为了给我国高纯石英技术发展提供测试分析技术支撑,以自主研制成功的4N高纯石英为实验样品,对高纯石英质量的ICP检测分析方法进行深入研究,结果表明:由于试样重量、 试剂组合、 试剂用量、 试剂纯度等因素都能够明显地影响ICP检测效果,因此高纯石英质量ICP检测技术的关键在于试样消解和溶矿条件的严格控制,其优化条件是:高纯石英试样重量≥2 000 mg;试剂纯度为高纯级(MOS或BV-Ⅲ),试剂组合为HF+HNO3;HF用量为25 mL;浓HNO3分3次使用,总用量≥5 mL。另外,为了避免铁质污染,不能使用钢筛筛分和制备样品;高纯石英的消解和溶矿若能在超净实验室条件下进行,对减少检测误差可能是有利的。
In order to provide the test analysis technology to support the technology development of China high-purity quartz, taking the 4N high-purity quartz made by ourself as experimental samples, we studied the ICP detection technology for the quality of high-purity quartz. The results showed that the digestion and soluble ore is the key of the ICP detection technology for the quality of high-purity quartz. The ICP detection results of high-purity quartz are influenced by the factors including sample weight, reagent combination, reagent consumption and reagent purity. The optimal condition is that: the sample weight is ≥2 000 mg; reagent combination is HF+HNO3; reagent purity is high purity level(MOS or BV-Ⅲ) HF dosage is 25 mL~ concentrated HNO3 are used by three times, and the total amount is ≥5 mL. In addition, the samples are not screened by steel sieve in order to avoid iron pollution. And the high-purity quartz should be dissolved in the super-clean laboratory, which may be good for reducing the detection error.