电感耦合等离子体发射光谱(ICP-OES)法测定锰矿石中五种氧化物

    Determining five oxides in manganese ores using inductively coupled plasma-optical emission spectroscopy

    • 摘要: 锰矿是钢铁行业中重要的原料之一,准确测定锰矿石中的主量组分是锰矿石分析的重要部分。本文对比王水溶样、四酸溶样和五酸溶样3种不同溶样体系,同时对盐酸、硝酸和王水3种不同的浸提条件做了研究,结合电感耦合等离子体发射光谱对锰矿中的5种氧化物进行测定。结果表明,四酸或五酸溶样,盐酸浸提,均能达到满意的测定结果;选择K 766.490 nm、Ca 184.006 nm、Na 589.592 nm、Mg 279.553 nm和Al 396.152 nm作为分析谱线,采用标准溶液基体匹配原则,可消除测定过程中可能存在的干扰;该方法Na、Mg、K、Ca和Al的检出限分别为2.7×10-6、2.1×10-6、1.5×10-6、1.7×10-6和2.3×10-6,选取2个锰矿石国家一级标准物质测定5种氧化物,相对标准偏差(RSD)均不超过5.0%,精密度较好;选取5个锰矿石标准物质进行验证,其5种氧化物相对误差(RE)均小于10%,准确度良好,测定值与推荐值基本吻合;对 5个未知含量的锰矿石中的5种氧化物进行加标测定,回收率在90%~110%之间,准确度满足分析测定的要求。该方法简化了样品前处理步骤,提高了效率,降低了成本,适合大批量样品分析,经标准物质验证,其准确度、精密度均达到行业标准的要求,适用于锰矿石样品中5种氧化物的测定。

       

      Abstract: Manganese ores are significant raw materials in the iron and steel industry. Accurately determining their major components is critical for the analysis of manganese ore composition. Based on three acid dissolution systems, i.e., aqua regia (HNO3+HC), tetracid (HNO3+HF+HClO4+HCl), and pentaacid (HNO3+HF+H2SO4+HClO4+HCl) solutions, and three extraction conditions, i.e., hydrochloric acid, nitric acid, and aqua regia, this study determined five oxides in manganese ores using inductively coupled plasma-optical emission spectroscopy (ICP-OES). The results indicate that the pentaacid or pentaacid solution and the extraction with hydrochloric acid achieved encouraging determination results. Spectral lines with wavelengths of 766.490 nm (K), 184.006 nm (Ca), 589.592 nm (Na), 279.553 nm (Mg), and 396.152 nm (Al) were analyzed. The possible interference in the determination process was eliminated based on the standard solution matrix matching principle. The detection limits of Na, Mg, K, Ca, and Al were 0.000 27%, 0.000 21%, 0.000 15%, 0.000 17%, and 0.000 23%, respectively. The determination results of all five oxides in two national primary reference materials for manganese ores showed relative standard deviations (RSD) not exceeding 5.0%, suggesting fair precision. The verification results of all five oxides in five reference materials showed relative errors (RE) below 10%, demonstrating high accuracy, with the measured values roughly consistent with the recommended values. The spiked determination of five oxides in five manganese ores with unknown content yielded recovery rates ranging from 90% to 110%, suggesting that the accuracy met the analytical requirements. Therefore, the ICP-OES method simplifies sample pretreatment, improves efficiency, and reduces costs, thereby applying to batch sample analysis. The verification using reference materials demonstrates that its accuracy and precision meet industrial standards, establishing the ICP-OES method as an effective approach for determining the five oxides in manganese ore samples.

       

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