微波消解－ICP-OES测定钛渣中常量或微量杂质

Microwave Digestion—ICP-OES Determination of Common or Micro Impurities in Titanium Slag

中文关键词:  ICP-OES  钛渣  杂质  微波消解

英文关键词:ICP-OES  titanium slag  impurities  microwave dispels

中文摘要:

      钛渣样品采取高压密闭微波加热方式以HF、HNO3进行消解，采用电感耦合等离子体原子发射光谱法(ICP-OES)直接同时测定常量、微量杂质铁、铅、砷、铬、铜、磷、锰、钒、镁、钙。考察了消解条件、基体钛以及共存元素之间的干扰影响、等离子体参数等测定条件，通过优选元素分析谱线、以及采用基体匹配与同步背景校正相结合的方式消除光谱干扰和基体效应。测定50、60、70、80、90等不同品位钛渣中杂质元素的结果表明:方法检测范围涵盖了0.005%～10.0%的钙、镁、铁，以及0.005%～2.0%的铅、砷、铬、铜、磷、锰、钒，校准曲线相关系数大于0.999 2；背景等效浓度0.002%～0.0015%，检测限0.0009～0.0038%；含量不小于1.0%的RSD低于0.677%，在0.010%～0.10%含量范围内RSD低于3.85%；回收率为90.0%～108.0%。以本法对70、80、90 3个高钛渣标准样品的定值分析结果与传统化学方法对照一致。

英文摘要:

      Titanium slag samples were digested in the manner of high-pressure sealed microwave heating in HF, HNO3, and then the common or micro iron, lead, arsenic, chromium, copper, phosphorus, manganese , vanadium, magnesium and calcium impurities in the slag were determined directly by the inductive coupling plasma atomic emission spectrographic method (ICP-OES) simultaneous. Test conditions for the sample digestion, interfering effects of the titanium matrix and coexisted elements, and the plasma determination parameters conditions, etc were investigated. By optimizing the spectral lines for the elemental analysis, and by the use of the substrate matching and the synchronized background correction spectral interference and matrix effect were eliminated. The results of determination of a variety of 50,60,70,80,90 different levels of impurity elements in the slag showed that: in the detection range of 0.005% to 10.000% of calcium, magnesium, iron, and 0.005% to 2.000% of lead, arsenic, chromium, copper, phosphorus, manganese, vanadium, the calibration curve correlation coefficients were greater than 0.999 2, the background equivalent concentrations were 0.0020% ~ 0.0015%, the detection limits, 0.0009%~0.0038%, RSD≤0.677% when the contents≥1.0%, RSD≤3.85% when the concentration range were 0.010% ~ 0.100% and the recovery rates were 90.0%～108.0%, using this method the results of three standard samples of high titanium slag of 70,80,90 were consistent with the traditional chemical method.