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赵秀宏, 王鑫焱, 郭沛, 刘彦春, 姜雨杉. 硝酸镧为基体改进剂石墨炉原子吸收光谱法测定煤样中的铍[J]. 岩矿测试, 2015, 34(1): 60-66. DOI: 10.15898/j.cnki.11-2131/td.2015.01.008
引用本文: 赵秀宏, 王鑫焱, 郭沛, 刘彦春, 姜雨杉. 硝酸镧为基体改进剂石墨炉原子吸收光谱法测定煤样中的铍[J]. 岩矿测试, 2015, 34(1): 60-66. DOI: 10.15898/j.cnki.11-2131/td.2015.01.008
Xiu-hong ZHAO, Xin-yan WANG, Pei GUO, Yan-chun LIU, Yu-shan JIANG. Beryllium-Determining in Coal by Graphite Furnace Atomic Absorption Spectrometry with Lanthanum Nitrate as Matrix Modifier[J]. Rock and Mineral Analysis, 2015, 34(1): 60-66. DOI: 10.15898/j.cnki.11-2131/td.2015.01.008
Citation: Xiu-hong ZHAO, Xin-yan WANG, Pei GUO, Yan-chun LIU, Yu-shan JIANG. Beryllium-Determining in Coal by Graphite Furnace Atomic Absorption Spectrometry with Lanthanum Nitrate as Matrix Modifier[J]. Rock and Mineral Analysis, 2015, 34(1): 60-66. DOI: 10.15898/j.cnki.11-2131/td.2015.01.008

硝酸镧为基体改进剂石墨炉原子吸收光谱法测定煤样中的铍

Beryllium-Determining in Coal by Graphite Furnace Atomic Absorption Spectrometry with Lanthanum Nitrate as Matrix Modifier

  • 摘要: 应用石墨炉原子吸收光谱法(GFAAS)测定煤、地球化学样品、土壤、空气等不同基质中的铍, 关键是基体改进剂的选择问题.本文采用一体化平台石墨管, 通过缓慢升温燃烧灰化煤炭样品, 在硝酸介质中, 比较了7种基体改进剂(硝酸镧、硝酸镁、硝酸铝、磷酸氢二铵、氯化钯、碳酸钙、酒石酸)对煤样中铍的增敏效果, 同时探讨了基体干扰及消除的问题.实验结果表明, 在2%的硝酸介质中, 以硝酸镧为基体改进剂, 石墨炉灰化温度提高到1100℃, 原子化温度仅为2300℃时, 即可消除基体中铝、铁、钙、镁、磷等共存元素的干扰.铍的浓度在0~8 μg/L范围内线性关系良好, 方法检出限为0.008 μg/g, 定量限为0.025 μg/g, 精密度(RSD, n=11) 为1.8%~2.8%, 标准样品的测定值在给定值的误差范围内.其作用机理是镧与干扰元素结合生成了热稳定的难熔、难蒸发、难解离的化合物, 将铍释放出来, 镧起到既提高灰化温度, 又相对降低原子化温度的双重作用, 消除了基体干扰的同时, 又延长了石墨管使用寿命.本方法操作简单, 无需对石墨管预处理, 降低了检测成本, 具有很强的稳定性和适应性, 适用于煤中铍的测定.

     

    Abstract: The key to beryllium-determining in coal, geochemical samples, soil, air and other different substrates by Graphite Furnace Atomic Absorption Spectrometry (GFAAS) is to choose a proper matrix modifier. The coal sample is slow burning ashed and then determined by integration platform graphite tube. In this paper, the sensitization effect of seven kinds of matrix modifier (lanthanum nitrate, magnesium nitrate, aluminum nitrate, diammonium phosphate, palladium chloride, calcium carbonate, tartaric acid) to beryllium in nitric acid solution is contrasted, and the elimination of matrix interference is discussed. The experimental results show that the interference of coexisting elements, such as aluminum, iron, calcium, magnesium and phosphorus, are eliminated under the condition of 2% nitric acid medium, lanthanum nitrate as matrix modifier, 1100℃ of ashing temperature and 2300℃ of atomization temperature. The limit of detection is 0.008 μg/L, the limit of quantification is 0.025 μg/L and the linear measurement is 0-8 μg/L. The RSD (n=11) of standard determination is 1.8%-2.8%, the measured values of standards are within the given range. The mechanism is lanthanum and interference elements combined to generate the thermal stability of refractory are indissoluble and difficult to evaporate to release beryllium. Lanthanum can not only improve the ashing temperature, but can also lower the atomization temperature to eliminate the matrix interference and prolong the service life of the graphite tube. This method is simple and less expensive than traditional methods, with strong stability and adaptability, and without pretreatment of graphite tubes. It is suitable for the determination of beryllium in coal.

     

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