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    熔融制样-X射线荧光光谱法测定钛铁中6种主、次量元素

    Determination of 6 Major and Minor Elements in Ferrotitanium by X-Ray Fluorescence Spectrometry with Melt Sample Preparation

    • 摘要: 取研磨好的钛铁样品(0.300 0±0.000 2) g置于铂金坩埚中,用2 mL水浸湿,逐滴加入1 mL氢氟酸,加盖表面皿,于室温静置15~20 min,加入0.5 mL硝酸冲洗表面皿,合并所有溶液,待溶液澄清后加入9.000 0 g混合熔剂(质量比67∶33的四硼酸锂-偏硼酸锂混合物),于200~250 ℃加热10 min。冷却后加入0.3 mL 400 g·L−1溴化铵溶液,于1 050 ℃熔融12 min,冷却后倒出玻璃熔片,采用X射线荧光光谱法测定其中主、次量元素(钛、硅、锰、磷、铜、铝)的含量。结果显示,6种目标元素的质量分数在一定范围内和荧光强度呈线性关系,5种次量元素的检出限为0.004 5%~0.038%。钛铁标准样品中6种目标元素测定值的相对标准偏差(n=8)为0.39%~4.1%,测定值相对误差的绝对值为0.058%~11%。方法用于2个实际钛铁样品的分析,各元素的测定结果均与对应国家标准方法的结果基本一致。

       

      Abstract: The ground ferrotitanium sample (0.300 0±0.000 2) g was taken, placed in a platinum crucible, and wetted with 2 mL of water, and 1 mL of hydrofluoric acid was added dropwise. A watch glass was covered, and the mixture was settled at room temperature for 15‒20 min. Then 0.5 mL of nitric acid was added to rinse the watch glass, and all solutions were combined. After the solution became clear, 9.000 0 g of the mixed flux (a mixture of lithium tetraborate and lithium metaborate at a mass ratio of 67∶33) was added, and the mixture was heated at 200‒250 ℃ for 10 min. After cooling, 0.3 mL of 400 g·L−1 ammonium bromide solution were added, and the mixture was fused at 1 050 ℃ for 12 min. After cooling, the glass fusion piece was poured out, and the major and minor elements, including titanium, silicon, manganese, phosphorus, copper, and aluminum in the glass fusion piece were determined by X-ray fluorescence spectrometry. As shown by the results, linear relationships between values of the mass fraction and the fluorescence intensity of the 6 target elements were kept in definite ranges, with detection limits of 5 minor elements in the range of 0.0045%‒0.038%. RSDs (n=8) of the determined values of the 6 target elements in ferrotitanium standard samples were found in the range of 0.39%‒4.1%, and the absolute values of the relative errors of the determined values were found in the range of 0.058%‒11%. This method was applied to the analysis of 2 actual ferrotitanium samples, the determination results of elements were basically consistent with those obtained by the corresponding national standard methods.

       

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