提出了一种采用高温高压密闭溶样快速消解荧光粉晶体的前处理新方法.针对目前常用的稀土氧化物和稀土磷酸盐类、碱土金属铝酸盐类、碱土金属硅酸盐类四大类荧光粉,研究了消解时间、温度、消解溶剂种类和用量4个条件对样品消解程度的影响.采用电感耦合等离子体质谱法( ICP - MS)测定了最佳消解条件下消解的荧光粉中杂质元素Cu、Zn、Cd和Pb的含量.结果表明:稀土氧化物和稀土磷酸盐类荧光粉的最佳消解条件为2 mL HCl溶剂中120℃下消解3h;碱土金属铝酸盐类荧光粉的最佳消解条件为2 mL HCl溶剂中160℃下消解6h;碱土金属硅酸盐类的最佳消解条件为2 mLHCl+0.5 mLHF溶剂中160℃下消解3h.荧光粉中主要共存元素对所测杂质元素Cu、Zn、Cd和Pb的检测无干扰.该法线性范围宽、检出限低、灵敏度高,是荧光粉晶体中元素检测的较佳方法.%A new fast pretreatment method for crystal fluorescent powders which are digested by high temperature and high pressure ambient in bombs is discussed in this paper. The influence of four conditions; digested time, temperature, the species, and dosage of solvents on the digestion ability of four kinds of fluorescent powders, including rare earth oxides and rare earth phosphates, alkaline-earth metal aluminates and alkaline-earth metal silicates were studied. The contents of impurity elements Cu, Zn, Cd and Pb in these fluorescent powders which were digested in optimal conditions were determined by Inductively Coupled Plasma-Mass Spectrometry ( ICP-MS). The results show that the optimal digestion conditions are 2 mL HC1, 120℃ and 3 h for rare earth oxide and rareearth phosphate fluorescent powder; 2 mL HC1, 160℃ and 6 h for alkaline-earth metal aluminate fluorescent powder; 2 mL HC1 -0.5 mL HF, 160℃ and 3 h for alkaline-earth metal silicate fluorescent powder. The major coexisting elements had no obvious influence on the determination of Cu, Zn, Cd and Pb, the method had wide linear ranges, low limits of detection and high sensitivity, and was an optimal analytical method for determining elements of phosphor crystals.
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