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

Determination of boron in ferroboron by inductively coupled plasma atomic emission spectrometry combined with microwave digestion

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，建立了微波消解一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182．641，208．959，249．773nm^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0．5～2mg／mL范围对测定没有影响；但是当铁的质量浓度在2mg／mL时，由于硼的分析线（249．773nm）受铁谱线（249．782nm）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％。

A method for determination of boron in ferroboron by inductively coupled plasma emission spectrometry has been developed. By studying on the conditions of microwave digestion,the selection of the analytical spectral lines and the internal standard element, and the interference of matrix and coexisting elements,the experimental conditions were optimized. Three spectral lines, 182. 641,208. 959 and 249. 773 nm could be selected as analytical spectral lines in determination of boron. When 182. 641 and 208. 959 nm spectral lines were selected,no influence from iron was found in the range of 0.5-2 mg/mL. However,when the concentration of iron was 2 mg/mL, B analytical spectral line（249. 773 nm）selected was affacted by Fe spectral line（249. 782 nm）. This influence could be eliminated by the method of matrix-matching. The co-existing elements, such as silicon, aluminium and some trace elements did not interfere in the determination. The ferroboron certified reference material and samples were tested by this method and the determination results were in good agreement with the certified value and the results obtained by chemical method, with the relative standard deviations（RSD）within 0. 28%-0. 43% （n =11）,the recoveries between 96.8% to 104.0%.