微波消解-ICP-OES测定钒渣中钙、镁、铝，磷含量

Determination of Contents of Calcium,Magnesium,Aluminium and Phosphorus in Vanadium Slag by Microwave Digestion-ICP-OES

研究采用微波消解法溶解钒渣样品,并通过ICP-OES法测定其中钙、镁、铝和磷元素的含量,探究了不同测试条件对测定结果的影响。以6mL HCl,2mL HNO3,1 mL HF作为消解体系,微波消解条件选择为:在5 min内将功率从300 W升至600 W,并保持25 min。按此条件进行消解,可得到澄清透明的溶液,溶样效果良好。各元素的相对标准偏差均小于5%,检出限在0.008~0.030 mg·L^-1之间,加标回收率在96.7%~102.7%范围内。应用于实际样品的分析,得到了与化学法一致的结果。

Microwave digestion was used to dissolve vanadium slag samples,and the contents of Ca,Mg,Al and P in vanadium slag samples were determined by ICP-OES.The effects of different test conditions on the determination results were investigated.For microwave digestion process,6 mL HCl,2 mL HNO 3 and 1 mL HF were used as the digestion system.The optimum conditions for microwave digestion were as follows:the power was increased from 300 W to 600 W in 5 min and kept for 25 min.Clear and transparent solution could be obtained by digestion under the above conditions,and the sample dissolution effect was good.The relative standard deviations of the four elements were less than 5%.The detection limits were found in the range of 0.008~0.030 mg·L^-1,and the recoveries were between 96.7% and 102.7%.It was applied to the analysis of practical samples,and the results were consistent with those obtained by chemical method.