电感耦合等离子体原子发射光谱法测定钛合金中铁、硅不同溶解方法比较研究

Comparison of two different dissolution methods for inductively coupled plasma atomic emission spectrometric determination of iron and silicon in titanium alloy

考察了硫酸溶解和氢氟酸溶解两种钛合金的溶解方法。采用氢氟酸溶解试样,钛合金中的Fe和Si均可进行准确检测,而用硫酸溶解钛合金样品时,Si含量不能准确检测。进一步研究了硫酸溶解法中不同溶解温度对测量的影响,发现将电炉温度调至较高时,钛合金溶解速度较快,且对Fe的分析没有影响,因此用硫酸溶解钛合金时选择此种溶解方式进行Fe含量的分析。此外,系统考察了10余种不同牌号钛合金中基体元素和共存元素对Fe、Si分析谱线的光谱干扰情况,并进行了分析谱线的选择。Fe259.940nm、Fe238.204nm和Fe239.562nm三条谱线可作为钛合金中Fe元素的分析线;Si251.611nm则做为Si元素的分析谱线,但当钛合金中Mo含量大于1%时,制作校准曲线分析Si时需进行Mo元素含量匹配。硫酸溶解法Fe的检出限为0.089μg/mL,氢氟酸溶解法Fe和Si的方法检出限分别为0.016μg/mL和0.097μg/mL。

This report investigated two dissolving titanium alloy methods which were sulfuric acid dis solution method and hydrofluoric acid dissolution method. Fe and Si in titanium alloy could be deter mined accurately when the titanium alloy samples were dissolved by hydrofluoric acid dissolution method, and sulfuric acid dissolution method was not applied to Si element. After researching the influence of different dissolving temperature, the conclusion was obtained that high hotplate temperature was the best method for dissolving titanium alloys. Under such circumstance, titanium alloy could be dissolved rapidly, and there was no negative effect on the analysis of Feelement. Therefore, this dissolving method was selected when sulfuric acid was used in dissolving titanium alloys. Further more, the spectral interferences deriving from the basic element and coexistence elements in more than ten brands of titanium alloy in the determination of Fe, Si were investigated, and then analytical lines were selected. Fe 259.94nm, Fe 238.204nm, Fe 239.562nm and Si 251. 611nm were selected as analytical lines, but when content of Mo was above 1%, Mo element ought to be matched in calculating curve to analyze Si element. The detection limit of Fe of sulfuric acid dissolution method is 0.089 μg/mL, and the detection limit of Fe and Si of hydrofluoric acid dissolution method were 0. 016 mL and 0. 097 μg/mL, respectively.