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建立了电感耦合等离子体原子发射光谱法(ICP-AES)直接同时测定钛合金中合金元素或微量杂质硅钒铁铝镍钼铬的分析方法。采用氢氟酸和硝酸混合试剂并且在室温或70℃水浴控制加热条件下消解样品,从而避免了待测元素的挥发损失以及确保了高浓度钛基体在低酸度介质中也不会发生水解反应。试验了钛基体和共存元素对测定的光谱干扰影响,采取以钇作为内标元素的内标校正法,并且优选了待测元素分析谱线、内标校正谱线、同步背景校正位置以及ICP光谱仪工作条件,有效地消除基体钛导致的物理干扰以及改善方法精密度和检出限水平;方法实际应用结果表明:方法的检出限为10～27μg/L,背景等效浓度5～38μg/L,相关系数r≥0.9992;回收率95.0%～105.0%;RSD≤2.27%。
A method for simultaneous and direct determination of alloying elements or trace impurities of silicon vanadium iron-aluminum-nickel-molybdenum-chromium in titanium alloy by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. Hydrofluoric acid and nitric acid mixed reagents and room temperature or 70 ℃ water bath under controlled heating digestion samples, thus avoiding the volatile elements to be measured and to ensure that the high concentration of titanium matrix in low acid medium hydrolysis reaction will not occur. The effect of titanium matrix and co-existing elements on the spectral interference was tested. The internal standard calibration method with yttrium as the internal standard was adopted. The elemental analysis line, internal calibration line, synchronous background correction position and ICP spectrometer Working conditions, effectively eliminating the physical interference caused by the matrix titanium and improving the precision and the detection limit of the method. The practical application results show that the detection limit of the method is 10-27μg / L and the background equivalent concentration is 5-38μg / L , The correlation coefficient r ≥ 0.992; recovery 95.0% ~ 105.0%; RSD ≤ 2.27%.