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应用元素分析仪测定铅锌矿中的高含量硫

Determination of High-content Sulfur in Lead-Zinc Ore by Elemental Analyzer

  • 摘要: 目前对铅锌矿中高含量硫的测定主要采用传统的重量法和容量法, 但由于铅锌矿基体复杂, 干扰较多, 造成操作步骤繁琐; 而采用湿法仪器分析又受制于样品的前处理等问题使得测定结果的准确度较差。本文建立了应用元素分析仪测定铅锌矿中的高含量硫(1.0%~32.0%)的分析方法。将样品磨制成粒度小于0.075 mm的粉末, 样品制备时加入高纯二氧化硅作为稀释剂以降低铅锌矿的含硫量, 仪器测量时加入线状氧化铜作为添加剂以提高硫的氧化效果, 优先选用与实际测定样品相同性质的铅锌矿国家标准物质GBW 07287(硫的标准值为10.76%)建立标准曲线以减小基体效应。方法精密度(RSD, n=12) 小于1%, 实际样品分析的测定值与重量法的相对误差小于1%。本方法比化学分析方法的操作简单, 几乎没有干扰; 比湿法仪器分析方法的样品前处理步骤少, 待测元素硫的损失少, 测定结果可靠度高。

     

    Abstract: High-content sulfur in lead-zinc ore is commonly determined by gravimetric and volumetric methods. However, these methods are tedious and not easy to use due to the complex matrices involved. Wet chemical instrument analysis is also not suitable due to the chemical treatment and poor accuracy. The analytical method of high-content sulfur in lead-zinc ore (1.0%-32.0%) was established by Elemental Analyzer. The samples were grinded to particle size less than 0.075 mm, The content of sulfur in lead-zinc was reduced through adding high pure silica when the samples were prepared, and the effect of oxidation sulfur was improved through adding the linear copper oxide when the samples were determined. The standard curve for the method was established with national reference material GBW 07287 (the content of sulfur is 10.76%) which has similar composition to the actual samples, in order to eliminate the matrix effect. The RSD (n=12) is less than 1%, the relative error of the measured values is less than 1% between the proposed method and gravimetric method. This method is simple, quick, and easy to grasp, with minor interference compared with the gravimetric method. Moreover, the sample preparation was simpler than established methods and there was less sulfur loss. The result was reliable compared with wet instrument analysis. The method is also accurate without pollution, and suitable to determine the high-content sulfur in other ores.

     

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