微波消解-ICP-OES标准加入法测定钽炉灰中的钽

以氢氟酸和硝酸为溶剂通过微波消解对钽炉灰进行溶解,经分取、稀释后制得样品溶液. 对样品溶液进行半定量分析,保证校准溶液加入合适的钽量,制得系列校准溶液. 选择 Ta 240. 063 nm 为分析谱线,采用标准加入法消除测定过程中的基体效应,在电感耦合等离子体发射光谱（ ICP-OES）上对钽炉灰中的钽含量进行测定. 结果显示,绘制的工作曲线线性相关系数均在 0. 999 以上,测定结果的相对标准偏差（ n = 7）小于 0. 50%,加标回收率在94. 6% ~ 107. 9%之间.

Determination of Tantalum in Tantalum Furnace Ash by Method of Microwave Digestion and ICP-OES Standard Addition

The tantalum furnace ash was dissolved by microwave digestion with hydrofluoric acid and nitric acid medium, and the samples were prepared after separation and dilution. A semi quantitative analysis was used to analyze the sample solutions, ensuring the preparation of calibration solutions to be suit for the amount of tantalum, and a series of calibration solutions were also prepared. Ta 240.063 nm was the selected as the analytical spectral line, and the standard addition method was used to remove the matrix effect, and then the contents of tantalum in tantalum ashes were determined by inductively coupled plasma emission spectrometry (ICP-OES). The results showed that the linear correlation coefficients of the standard curves were over 0.999, and the relative standard deviations (RSDs, n=7) were less than 0.50% with a recovery of 94.6%~107.9%.