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提出了用电感耦合等离子体原子发射光谱(ICP-AES)法测定高纯六氟化钨中铬、锰、铁、钴、镍、铜、锌、镁、钙、钠、钾、铅及钼等金属元素的含量。六氟化钨极易与空气中的水分发生反应,为此设计了一套与空气隔离的密闭取样系统。在装有待测金属元素的取样器内,先后加入氨水、硝酸、氢氟酸使其溶解并定容,作为ICP-AES分析的待测溶液。在优化的实验条件下,得出各元素的检出限小于0.005mgL-1,方法的回收率在90.5%~104.2%之间,测定值的相对标准偏差(n=11)在3.2%~7.8%之间。最终试验分析结果表明,样品满足高纯六氟化钨技术指标的要求。
The method for the determination of chromium, manganese, iron, cobalt, nickel, copper, zinc, magnesium, calcium, sodium, potassium, lead and molybdenum in high-purity tungsten hexafluoride by inductively coupled plasma atomic emission spectrometry Such as metal content. Tungsten hexafluoride can easily react with the moisture in the air, therefore, a set of closed sampling system isolated from the air is designed. In the sampler with the metal element to be tested, ammonia, nitric acid and hydrofluoric acid were added successively to dissolve and set the volume as the solution to be tested by ICP-AES. Under the optimal experimental conditions, the detection limit of each element was less than 0.005mgL-1, the recoveries were between 90.5% and 104.2%, and the relative standard deviations (n = 11) were between 3.2% and 7.8% %between. The final test results show that the samples meet the high purity tungsten hexafluoride technical indicators.