采用氧化镁焙烧样品,热水浸提后不需分离富集,电感耦合等离子体质谱法直接测定钼矿石及钼精矿中铼.对不同焙烧熔剂、焙烧条件、浸提条件以及仪器测定条件进行了研究,结果表明:以氧化镁为焙烧试剂,在650℃保温90 min,趁热用热水浸提为最佳溶样条件,测定时选用103 Rh为内标元素,可有效校正仪器漂移,减小基体效应的干扰.方法检出限为0.005 μg/g,回收率在94％～102％之间.本方法经国家标准物质分析验证,结果与认定值吻合,相对标准偏差(RSD,n=5)≤3.6％,适合钼矿石及钼精矿中含量为0.05～300 μg/g铼的测定.%Molybdenum ore and molybdenum concentrate were calcined by magnesium oxide. After hot water extraction,the sample was directly determined by inductively coupled plasma mass spectrometry to obtain the content of rhenium. A study was conducted on the calcination solvent & conditions,extraction conditions and instrumental determination conditions. Results indicated that: magnesium oxide was taken as calcination solvent; the sample was kept at 650 °C for 90 min; the optimal dissolution conditions was to use hot water for leaching; 103Rh was selected as internal element to effectively correct instrumental drift and reduce the interference of matrix effect. The detection limit was 0. 005 μg/g and recoveries were between 94 % and 102 %. The method was tested by certified reference materials with the result consistent with certified value and RSD (n = 5) ≤ 3. 6 %. The method is suitable for the determination of rhenium with the content of 0. 05 ～ 300 μg/g in molybdenum ore and molybdenum concentrate.
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