ICP-OES测定草酸氧钒中硅铁钼钾钠

建立了电感耦合等离子体原子发射光谱法(ICP-OES)直接同时测定草酸氧钒中0.001%~0.100%硅铁钼钾钠的分析方法。试验考察了高浓度钒离子与草酸共存体系下光谱干扰、连续背景叠加和基体效应等干扰因素对测定的影响,总结得出草酸氧钒所产生的连续背景叠加和基体效应均对钾钠存在负干扰和对硅铁钼元素存在正干扰的试验结论,方法采用基体匹配和同步背景校正相结合措施消除草酸氧钒基体的影响。并且根据基体元素钒、碳对待测元素的光谱干扰试验,筛选出受到基体组分光谱干扰的候选谱线,从中优选得到了各元素适宜的分析谱线、背景校正区域以及光谱仪工作条件。结果表明:背景等效浓度-0.000 3%~0.000 3%,元素检出限0.000 1%~0.000 3%(0.005~0.015 mg/L),元素含量0.001%~0.010%范围内RSD小于10%,含量0.010%~0.050%范围内RSD小于5%,回收率91.6%~109.4%,测定结果与ICP-MS对照一致。

Determination of Silicon,Iron, Molybdenum,Potassium and Sodium in Vanadyl Oxalate by ICP-OES

The analyzing method directly and simultaneously detecting silicon (Si),iron (Fe),molybdenum (Mo),potassium (K) and sodium (Na) with the content of 0.001％ ～0.100％ in vanadyl oxalate (VOC2O4) using inductively coupled plasma atomic emission spectrometry (ICP-OES) was established.The influences of matrix effects,spectral interferences and continuous background superposition in the system with high concentrations of vanadium ion and oxalate coexistence,on the testing were studied,and the conclusions that the matrix effects and continuous background superposition of VOC2O4 have a negative interference to K and Na but a positive disturbance to Si,Fe and Mo in the system were obtained.Matrix matching coupled with synchronous background correction was employed to eliminate the matrix effects of VOC2O4.Based on the spectral interference from matrix elements vanadium (Ⅴ) and carbon (C),the candidates of spectral lines disturbed by the spectra of matrix components were selected,from which the appropriate analyzing spectral lines,background correction areas and operation conditions of spectrometer for the tested elements were determined.The results show that the RSD is less than 10％ with-0.000 3％ ～0.000 3％ of background equivalent concentration,0.000 1％ ～0.000 3％ (0.005 ～0.015 mg/L) of element detection limit and 0.001％ ～0.010％ of element content,while the RSD is less than 5％ with 0.010％ ～0.050％ of element content.The recovery rate is 91.6％ ～109.4％,and the testing results are in accordance with those by ICP-MS.