电感耦合等离子体原子发射光谱法测定钛合金中镧铈钇

研究了用电感耦合等离子体发射光谱法(ICP-AES)测定钛合金中镧、铈和钇的条件并建立了分析方法。样品用硫酸或硫酸-氢氟酸溶解, 选择398.852 nm、394.274 nm和371.092 nm波长谱线分别作为镧、铈和钇的分析线, 基体效应对测定的影响采用基匹配方法消除。镧、铈和钇校准曲线的线性范围(质量分数)分别为0.001%～0.030%、0.005%～0.030%和0.001%～0.030%, 线性相关系数均为0.999 9, 检出限分别为0.003 μg/mL(镧)、0.015 μg/mL(铈)和0.001 μg/mL(钇)。对硫酸和硫酸-氢氟酸的溶样效果进行比较, 表明两种溶样方法都能实现镧、铈和钇的准确测定, 但硫酸-氢氟酸的溶样速度快, 可提高分析效率。在不含镧、铈和钇的钛合金样品中加入不同量的镧、铈和钇标准溶液进行精密度和加标回收试验, 测得镧、铈和钇的RSD值分别小于或等于1.7%、7.3%和0.59%, 回收率在92%～100%之间。方法用于钛合金样品中钇和镧的测定, 测定值与ICP-MS法的测定值一致;用于钛合金标样中铈和钇的测定, 测定值与认定值相符。

Determination of lanthanum,cerium, yttrium in titanium alloys by inductively coupled plasma atomic emission spectrometry

The conditions for determination of lanthanum, cerium and yttrium in titanium alloys by inductively coupled plasma atomic emission spectrometry (ICP-AES) was investigated and thus the analytical method was established. The sample was dissolved in sulfuric acid or sulfuric acid-hydrofluoric acid. The spectral lines with wavelengths of 398.852 nm, 394.274 nm and 371.092 nm were selected as the analytical lines for lanthanum, cerium and yttrium, respectively. The matrix effect on the determination was eliminated by the matrix matching method. The linear ranges (mass fraction) of the calibration curves for lanthanum, cerium and yttrium were 0.001 %-0.030 %, 0.005 %-0.030 % and 0.001 %-0.030 %, respectively. The linear correlation coefficients were 0.999 9. The detection limits were 0.003 μg / mL for lanthanum, 0.015 μg/mL for cerium and 0.001 μg/mL for yttrium. The dissolution of sample by sulfuric acid and sulfuric acid-hydrofluoric acid was compared and the results showed that both the methods achieved accurate determination of lanthanum, cerium and yttrium, but the method for dissolution of sample with sulfuric acid-hydrofluoric acid was faster and therefore increased the analysis efficiency. The precision and standard addition tests were conducted by adding different amounts of lanthanum, cerium and yttrium into titanium alloys samples containing no lanthanum, cerium and yttrium and the RSD values for lanthanum, cerium and yttrium were found to be less than or equal to 1.7 %, 7.3 % and 0.59%, respectively, and the recoveries were found to be between 92 % and 100 %. The method was applied to the determination of yttrium and lanthanum in titanium alloy samples and the results were consistent with thosed obtained by ICP-MS. The method was applied to the determination of cerium and yttrium in titanium alloy reference materials and the results were consistent with the certified values.