用石墨炉原子吸收光谱法测定锗
Determination of germanium by graphite-furnace atomic-absorption spectrometry.
作者信息
Sohrin Y, Isshiki K, Kuwamoto T, Nakayama E
机构信息
Department of Chemistry, Faculty of Science, Kyoto University, Kyoto 606, Japan.
出版信息
Talanta. 1987 Mar;34(3):341-4. doi: 10.1016/0039-9140(87)80043-7.
The premature loss of germanium as volatile GeO results in low sensitivity and poor reproducibility in the determination of germanium by graphite-furnace atomic-absorption spectrometry. This interference can be eliminated by suppressing the premature reduction of GeO(2) to GeO during the ashing step, and dissociating the germanium oxides into the atoms simultaneously with their vaporization during the atomization step. The premature reduction of GeO(2) to GeO has been successfully prevented by several approaches: (1) diminishing the reducing activity of the graphite furnace by (a) oxidizing the graphite surface and intercalating oxygen into the graphite lattice with oxidizing acids, such as nitric or perchloric, in the sample solution, or (b) using a tantalum-treated graphite furnace; (2) keeping the analyte as germanium (IV) by addition of sodium or potassium hydroxide to the sample solutions.
在石墨炉原子吸收光谱法测定锗时，锗以挥发性的GeO形式过早损失，导致灵敏度低且重现性差。通过在灰化步骤中抑制GeO₂过早还原为GeO，并在原子化步骤中使锗氧化物在蒸发的同时分解为原子，可消除这种干扰。通过几种方法已成功防止了GeO₂过早还原为GeO：(1)通过以下方式降低石墨炉的还原活性：(a)在样品溶液中用硝酸或高氯酸等氧化酸氧化石墨表面并将氧嵌入石墨晶格，或(b)使用经钽处理的石墨炉；(2)通过向样品溶液中添加氢氧化钠或氢氧化钾使分析物保持为锗(IV)。
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