微波消解-电感耦合等离子体质谱法测定铁矿石中铬砷镉汞铅
Determination of Cr, As, Cd, Hg and Pb in Iron Ores Using Inductively Coupled Plasma-Mass Spectrometry with Microwave Digestion
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摘要: 铁矿石中Cr、As、Cd、Hg和Pb不仅影响冶炼设备和产品性能,同时污染环境。文章以铁矿石标准物质为研究对象,对电感耦合等离子体质谱法(ICP-MS)测定铁矿石中Cd、As、Cr、Hg和Pb等5种元素进行了适用性探讨。结果表明,与常规的单元素原子吸收光谱法或多元素同步分析电感耦合等离子体发射光谱法相比,用微波消解方法处理铁矿石,具有样品消耗量少(0.1000±0.0200)g、消解用酸少(2.5 mL HCl+0.5 mL HF+1.0 mL HNO3)、排放降低、节约成本等优点,且无需配制铁底液,无需添加任何掩蔽剂,质谱干扰小,适用于分析Cr含量为5.5×10-10~2.5×10-4,As含量为7.6×10-10~1.9×10-4,Cd含量为4.5×10-11~5.5×10-6,Hg含量为1.88×10-9~1.9×10-7,Pb含量为1.2×10-10~3.2×10-5的铁矿石样品。优化后的前处理方法节约了能源、试剂和样品消耗,降低了二次污染和有效损失。Abstract: Cr, As, Cd, Hg and Pb in iron ores not only contaminate smelting facilities and affect the quality of final products, but also pollute the environment. Cr, As, Cd, Hg and Pb contents in five certified standard iron ore samples of BS105, JSS804-2, Euro680-1, JK42 and ASCM007 were measured using Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) with microwave. Compared with the routine methods of Atomic Absorption Spectrometric (AAS) and Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES), this method has the advantages of using a small sample weight of about (0.1000±0.0200) g, needing less acids for digestion as 2.5 mL HCl+0.5 mL HF+1.0 mL HNO3, less effluent and has a lower cost. There are small interferences without preparation of the Fe base solution and any addition of masking reagent. Results for Cr, As, Cd, Hg and Pb in the Fe ore samples are 5.5×10-10-2.5×10-4, 7.6×10-10-1.9×10-4, 4.5×10-11-5.5×10-6, 1.88×10-9-1.9×10-7 and 1.2×10-10-3.2×10-5, respectively. The optimized sample pre-treatment method saves energy, reagent and sample consumption, and reduces secondary pollution and actual loss.
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