电感耦合等离子体原子发射光谱法测定铌铁合金中铌

发布时间：2018-05-11 21:36

本文选题：电感耦合等离子体原子发射光谱法 + 铌铁　；参考：《冶金分析》2015年09期

【摘要】：铌铁样品以氢氟酸和硝酸消解,直接在氢氟酸介质中使用电感耦合等离子体原子发射光谱法(ICP-AES)测定铌含量。试验考察了共存基体元素铁以及常量杂质硅、钛、铝、钽等对测定的基体效应、光谱干扰以及背景噪声等因素的影响。通过采取优化样品稀释比例、选择适宜灵敏度分析谱线及其检测积分与背景校正区域,优化仪器工作条件等措施,将铌元素的检测信号强度调控在适宜水平,以确保方法具有良好线性范围以及精密度和正确度水平。试验采用基体匹配法绘制校准曲线,并进行同步背景校正,检验周期仅需10~15min。结果表明:在铌质量分数为50%~80%范围内,校准曲线线性相关系数r0.999 5。按照实验方法进行测定,实际铌铁合金样品测定结果的相对标准偏差(RSD,n=8)不大于0.2%;铌铁标准样品的测定结果与认定值一致;实际铌铁合金产品的测试结果与纸上色层分离重量法的测试结果也一致。
[Abstract]:The samples of ferroniobiobiobiobium were digested with hydrofluoric acid and nitric acid, and the content of niobium was directly determined by ICP-AES- (inductively coupled plasma atomic emission spectrometry) in hydrofluoric acid medium. The influence of the coexisting matrix element iron and the constant impurities silicon titanium aluminum and tantalum on the matrix effect spectral interference and background noise were investigated. By optimizing sample dilution ratio, selecting appropriate sensitivity analysis spectrum line and its detection integral and background correction area, optimizing the working conditions of the instrument, the signal intensity of niobium detection is adjusted to the appropriate level. To ensure that the method has a good linear range and precision and accuracy level. The calibration curve was drawn by the matrix matching method, and the synchronous background correction was carried out. The inspection period was only 10 ~ 15 min. The results show that the linear correlation coefficient of calibration curve is r 0.999 5 when the mass fraction of niobium is 50%. According to the experimental method, the relative standard deviation of the determination results of the actual ferroniobiobiobiobium samples is not greater than 0.20.The results of the determination of the standard samples of ferroniobiobiobiobiobiobiobiobiobium are consistent with the determined values. The test results of the actual ferroniobium alloy products are in agreement with those obtained by the chromatographic separation gravimetric method on paper.
【作者单位】：攀钢集团研究院有限公司钒钛资源综合利用国家重点实验室;
【分类号】：TG115.33

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