ICP-OES法测定镍基耐热合金中钨的研究

Determination of Tungsten in Nickel-base Heat-resistant Alloy by ICP-OES

研究采用不同的酸溶解试样,运用电感耦合等离子体原子发射光谱法（ICP-OES）对镍基耐热合金中的钨进行测定.通过实验仪器的分析条件参数进行优化试验,对分析谱线及其光谱干扰情况进行研究,最后确定了最佳分析谱线及分析条件.通过试验对比,发现采用硫酸-磷酸混酸加盐酸-硝酸混酸溶样,结合应用基体匹配和以钇作内标物质,通过内标法制定标准工作曲线,再测定试样中的钨含量,能达到较理想的检测效果.使用标准物质进行加标回收试验及精密度试验,其回收率在95.6％～97.5％之间,相对标准偏差不大于2.5％,检测结果与认定值基本相符.

An investigation has been undertaken to determine the content of tungsten in nickel-base heat-resistant alloy by inductively coupled plasma optical emission spectrometer （ICP-OES）. The samples were decomposed with different acids. Proper analysis spectral lines and optimum parameters of instrument operation were got by optimization experiment. Comparing the results of the experiment, it is shown that dissolving the samples by H2SO4-H3PO4 and HCl-HNO3, using the matrix matching and internal standard method to make the standard working curves with yttrium as internal standard element, determination of tungsten in the samples can achieve really good result. Standard recovery test and precision test were carried out by using standard samples. The rate of recovery was 95.6 %-97.5 % and the relative standard deviation was less than 2.5 %. The determination result was in good agreement with the standard samples.