过氧化钠熔融-电感耦合等离子体质谱法测定铅铋冶炼渣中的稀散元素

Determination of Scattered Elements in Lead-Bismuth Smelting Slag by Inductively Coupled Plasma-Mass Spectrometry with Sodium Peroxide Melting

  • 摘要: 稀散元素在电子、冶金、化工等领域是重要战略资源,高效回收铅铋冶炼渣中的稀散元素可缓解资源短缺问题。铅铋冶炼渣中铅含量在28.12%~29.45%之间,且主要以难溶性的硫酸铅形式存在,导致样品分解困难,进而影响电感耦合等离子体质谱法(ICP-MS)对该类样品中稀散元素的准确测定。本文利用X射线荧光光谱仪(XRF)和X射线衍射仪(XRD)明确了铅铋冶炼渣的基体组成与物相特性,为样品分解方法的选择以及优化ICP-MS分析测定条件提供依据。采用过氧化钠熔融样品,稀硫酸微热提取沉淀铅基体,选择71Ga、73Ge、78Se、111Cd、115In、205Tl和125Te作为分析同位素,数字校正方程解决了115In的质谱干扰,建立了ICP-MS准确测定铅铋冶炼渣中7种稀散元素的分析方法。实验优化了熔剂用量、熔融时间和浸取液体积比等实验条件,并研究了基体浓度对内标元素185Re回收率的影响。结果表明,各稀散元素的校准曲线相关系数(r)在0.9991~0.9999,方法检出限为0.0007~0.0221μg/g,定量限为0.0023~0.0737μg/g。采用铅矿石国家标准物质GBW07235和GBW07236验证方法的准确度和精密度,各稀散元素标准误差(RE)的绝对值在0~8.85%之间,相对标准偏差(RSD,n=7)在2.1%~4.2%之间。该方法应用于铅铋渣实际样品的测定,各稀散元素的RSD (n=7)在1.8%~3.9%之间,加标回收率在95%~104%,符合国家地质矿产行业标准DZ/T 0130—2006规定的加标回收率90%~110%范围。

     

    Abstract: Scattered elements have become indispensable strategic resources, and recycling from lead-bismuth smelting slag can alleviate the problem of resource shortage. Lead content in the lead-bismuth smelting slag ranges between 28.12% and 29.45%, primarily existing as insoluble lead sulfate. X-ray fluorescence spectroscopy (XRF) and X-ray diffraction (XRD) were employed to analyze the matrix characteristics of lead-bismuth smelting slag, providing guidance for sample pretreatment methods and optimization of ICP-MS analytical conditions. A method for the accurate determination of 71Ga, 73Ge, 78Se, 111Cd, 115In, 205Tl and 125Te by ICP-MS was established through sodium peroxide melting and dilute sulfuric acid extraction. The experimental conditions such as flux dosage, melting time and leaching solution were optimized. Experimental results show that correlation coefficient (r) value of the scattered elements is 0.9991-0.9999, method detection limit is 0.0007-0.0221μg/g, and quantitative limit is 0.0023-0.0737μg/g. The method was applied to GBW07235 and GBW07236, and the absolute value of the standard error (RE) ranges from 0 to 8.85%, and the relative standard deviation (RSD, n=7) was between 2.1% and 4.2%. This method is also applicable to the determination of scattered elements in actual samples of lead and bismuth slag and relative results are in accordance with the recoveries of 90%-110% specified by DZ/T 0130—2006.

     

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