电感耦合等离子体原子发射光谱法测定钛合金中钼锆铌

发布时间：2019-08-03 16:32

【摘要】：对于0.100g钛合金试样,加入10mL硫酸(1+1)和2~3滴硝酸可将钛合金溶解成清亮的、能够长期稳定存在的溶液。通过研究钛合金中钼、锆、铌的谱线干扰情况,选择钼202.031nm、锆339.197nm和铌269.706nm为分析线,实现了电感耦合等离子体原子发射光谱法(ICP-AES)对钛合金中钼、锆、铌的测定。通过采用钛合金国家标准物质按照试样处理方法和采用钛打底加入钼、锆、铌标准溶液制备而成的系列钼、锆、铌标准溶液分别绘制校准曲线,所得校准曲线相关系数(r)均大于0.999。但因市场上同时含有钼、锆、铌的钛合金标准物质不多,建议采用钛打底加入钼、锆、铌标准溶液的方式进行标准系列溶液的配制。各元素的检出限均不大于0.005%。采用两种标准溶液配制方式绘制校准曲线,对同一个钛合金样品进行精密度考察,结果的相对标准偏差(RSD,n=10)均小于1.0%。采用实验方法分析国家标准物质,测定值与认定值一致,误差在国标允许误差范围内,能够满足生产和科研的需要。方法适用于含铌不超过5%的钛合金的测定。
[Abstract]:For 0.100g titanium alloy samples, the titanium alloy can be dissolved into a clear and stable solution by adding 10mL sulfuric acid (11) and 2 脳 3 drops of nitric acid. The interference of Mo, Zirconium and Niobium in titanium alloy was studied. Mo 202.031nm, Zirconium 339.197nm and Niobium 269.706nm were selected as analytical lines to determine Mo, Zirconium and Niobium in titanium alloy by inductively coupled plasma atomic emission spectrometry (ICP-AES). The calibration curves were drawn by using titanium alloy national standard materials according to the sample treatment method and a series of Mo, Zr and NB standard solutions prepared by adding Mo, Zr and NB standard solutions at the bottom of titanium. The correlation coefficients of the calibration curves were all greater than 0.99. 9. However, because there are not many standard materials for titanium alloys containing Mo, Zr and NB at the same time, it is suggested that the standard series solutions should be prepared by adding Mo, Zr and NB standard solutions to the bottom of titanium. The detection limit of each element is not more than 0.005%. The calibration curves were drawn by two standard solution preparation methods, and the precision of the same titanium alloy sample was investigated. The relative standard deviation (RSD,n=10) was less than 1.0%. The experimental method is used to analyze the national standard material. The measured value is consistent with the identified value, and the error is within the allowable error range of the national standard, which can meet the needs of production and scientific research. The method is suitable for the determination of titanium alloys containing less than 5% niobium.
【作者单位】：中国船舶重工集团公司第七二五研究所;
【分类号】：TG115.33

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