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    微波灰化样品-电感耦合等离子体原子发射光谱法测定原油中微量金属元素

    ICP-AES Determination of Trace Amount of Metal Elements in Crude Oil with Microwave Assisted Ashing of Sample

    • 摘要: 原油样品(5g)于石英坩埚中,放入微波灰化炉中在800 ℃灰化1 h,残渣加入盐酸(1+1)溶液溶解并蒸发至近干,转入50 mL容量瓶加水定容后,供电感耦合等离子体原子发射光谱法测定原油样品中微量金属元素铁、钠、镍、钒和钙的含量。方法用于分析原油样品,所得相对标准偏差(n=6)在2.2%~6.5%之间,回收率在92.0%~108.4%之间。测定结果与常规灰化法测定结果对比,经t检验(α=0.05),无显著性差异。

       

      Abstract: Five grams of sample of crude oil was ignited for 1 h in microwave assisted ashing furnace at 800 ℃, and the residue was dissolved with HCl (1+1) solution and evaporated to near dryness. After taking up with water, the solution was diluted to 50 mL in a volumetric flask and used for ICP-AES determination of the trace metal elements, including Fe, Na, Ni, V and Ca. The proposed method was applied to the analysis of crude oil, the analytical results obtained by microwave ashing were compared with those by conventional ashing, and as verified by t-test at the confidence level of α=0.05, no significant difference was found between the two ashing methods. Values of recovery found by standard addition method were in the range of 92.0%-108.4%, with RSD′s (n=6) in the range of 2.2%-6.5%.

       

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