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通过最佳微波消解条件、分析谱线和内标元素的选择,基体及共存元素间光谱干扰的研究,检测限的测定以及样品分析,建立了微波消解-电感耦合等离子体原子发射光谱法测定硼铁中硼的分析方法。测定时可选择182.641,208.959,249.773 nm 3条谱线作为硼的分析线。当选择前两条谱线时,铁的质量浓度在0.5~2 mg/mL范围对测定没有影响;但是当铁的质量浓度在2 mg/mL时,由于硼的分析线(249.773 nm)受铁谱线(249.782 nm)干扰,对测定产生影响,这种影响可通过基体匹配方法消除。与硼共存的硅、铝和微量元素对测定没有影响。用本法测定了硼铁标样和样品,测定结果与认定值及化学法测定值有较好一致性,相对标准偏差为0.28%~0.43%(n=11),加标回收率在96.8%~104.0%。
The microwave digestion - inductively coupled plasma atomic emission spectrometry was established for the determination of boron by microwave digestion conditions, the selection of spectral lines and internal standard elements, the study of spectral interferences between matrix and coexisting elements, the determination of detection limits and the analysis of samples. Analysis of boron in iron. Determination can choose 182.641,208.959,249.773 nm three lines as the analysis line of boron. When the first two lines were selected, the mass concentration of iron in the range of 0.5-2 mg / mL had no effect on the determination. However, when the mass concentration of iron was 2 mg / mL, the analysis line of boron (249.773 nm) Spectral line (249.782 nm) interference, the determination of the impact, this effect can be eliminated by matrix matching method. Silicon, aluminum and trace elements coexisting with boron have no effect on the determination. The standard samples of ferroboron were determined by this method. The results were in good agreement with the certified values and the measured values by chemical methods. The relative standard deviations (RSDs) were 0.28% -0.43% (n = 11), and the recoveries were 96.8% ~ 104.0%.