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出 处:《冶金分析》2015年第4期68-72,共5页Metallurgical Analysis
摘 要:采用盐酸、氢氟酸和硝酸混酸于150℃温度下加压消解样品2h,样品溶解完全后,采用电感耦合等离子体原子发射光谱法(ICP-AES)测定钛合金中钌。实验确定了以240.272{140}nm光谱线作为钌分析线,并对仪器的工作条件进行了优化。优化后最佳的仪器工作条件为:射频功率1 050 W,观测高度14mm,雾化气流量0.6L/min,辅助气流量1.0L/min,冷却气流量12L/min。基体对测定的影响可通过基体匹配的方法克服,铝和钒对测定没有干扰。在此工作条件下,对TC23钛合金样品中钌量进行测定,相对标准偏差(n=11)为1.4%,将分析结果与邻菲罗啉分光光度法的结果进行比对,基本一致。The sample was treated for 2 h by pressurized digestion with HCI, HF and HNO3 mixture at 150 ℃. After complete dissolution, the content of ruthenium in titanium alloy was determined by induc- tively coupled plasma atomic emission spectrometry (ICP-AES). The spectral line of 240. 272 ( 140) nra was selected as the analytical line for ruthenium. Moreover, the working conditions of instrument were also optimized. The optimal operation conditions of instrument were as follows- radio frequency power of 1 050 W, observation height of 14 mm, atomizing gas flow of 0.6 L/min, auxiliary gas flow of 1.0 L/min, and cooling gas flow of 12 L/min. The influence of matrix on the determination could be eliminated by matrix matching method. The determination of ruthenium was not affected by aluminum and vanadium. The content of ruthenium in TC23 titanium alloy sample was determined under the selected working conditions. The relative standard deviation (RSD, n= 11) was 1.4%. The analytical results were compared with those obtained by phenanthroline speetrophotometry. The consistency was good.
关 键 词:钛合金 钌 加压消解 电感耦合等离子体原子发射光谱法(ICP-AES) 参数优化
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