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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。
A direct and simultaneous determination method of 0.001% ~ 0.100% Fe, Si, Fe, Mo and K in vanadyl oxalate was established by inductively coupled plasma atomic emission spectrometry (ICP-OES). The effects of interference factors such as spectral interference, continuous background superposition and matrix effect on the determination were investigated in the presence of high concentrations of vanadium ions and oxalic acid. It was concluded that continuous background superposition and matrix effects produced by vanadyl oxalate were both negative for potassium and sodium Interference and the existence of positive interference with ferrosilicon ferro-molybdenum. The method uses the combination of matrix matching and synchronous background correction to eliminate the influence of vanadyl oxalate matrix. According to the spectral interference test of matrix elements vanadium and carbon on the elements to be tested, the candidate spectrums disturbed by the spectrum of the matrix components were screened out. The suitable analytical spectra, background correction area and spectrometer working conditions were optimized. The results showed that the background equivalent concentration was -0.000 3% to 0.000 3%, the element detection limit was 0.000 1% to 0.000 3% (0.005-0.015 mg / L), the RSD was less than 10% in the range of 0.001% to 0.010% The content of RSD was less than 5% and the recoveries were 91.6% -109.4% in the range of 0.010% to 0.050%. The results were in good agreement with ICP-MS.