电感耦合等离子体质谱法测定煤矸石中微量锗和镓

建立了测定煤矸石中微量锗和镓的电感耦合等离子体质谱法。煤矸石试样经高温灰化,用硝酸-氢氟酸-高氯酸-磷酸分解,以电感耦合等离子体质谱法测定其中的锗和镓。通过在线三通加入内标元素铑,消除非质谱干扰;通过选择干扰元素的异质同位素进行定量测定,采用数学公式在线校正,消除质谱干扰。与分光光度法进行比对,锗、镓测定结果的相对偏差为-0.63%~0.28%。克服了常规化学分析方法步骤繁琐、耗时长、工作量大的不足。该法测定结果的相对标准偏差小于3%(n=6),加标回收率为97.4%~102.5%。该方法具有检出限低、快速、简便、线性范围宽、多元素同时测定等优点,分析误差满足化学分析法的要求,可用于煤矸石中锗和镓的测定。

Determination of micro-amounts of germanium and gallium in coal gangue by inductively coupled plasma mass spectrometry

A method of inductively coupled plasma mass spectrometry(ICP-MS)was established to determine microamount of germanium and gallium in coal gangue.After high temperature ashing,coal gangue samples were decomposed by HNO3-HF-HClO4-H3PO4 mixed acid,micro-amounts of germanium and gallium in sample solutions were directly determined by ICP-MS.The non-mass spectrum interference was eliminated by adding internal standard element rhodium into the on-line tee;the heterogeneous isotopes of interfering elements were selected for quantitative determination,and the mathematical formula was used for on-line correction to eliminate mass spectrum interference.The relative deviation of germanium and gallium was between-0.63%and 0.28%by comparison with spectrophotometry.The method overcomes the cumbersome procedure,time consuming,heavy workload of the conventional chemical analysis methods.The relative standard deviation was less than 3%(n=6),and the recovery of standard addition was 97.4%-102.5%.The method has the advantages of low detection limit,rapidity,simplicity,wide linear range and simultaneous determination of multiple elements.The analysis error meets the requirements of chemical analysis method and it is suitable for the determination of germanium and gallium in coal gangue.