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应用元素分析仪测定铅锌矿中的高含量硫

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徐国栋, 葛建华, 王凤玉, 程江. 应用元素分析仪测定铅锌矿中的高含量硫[J]. 岩矿测试, 2015, 34(2): 234-237. doi: 10.15898/j.cnki.11-2131/td.2015.02.014
引用本文: 徐国栋, 葛建华, 王凤玉, 程江. 应用元素分析仪测定铅锌矿中的高含量硫[J]. 岩矿测试, 2015, 34(2): 234-237. doi: 10.15898/j.cnki.11-2131/td.2015.02.014
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XU Guo-dong, GE Jian-hua, WANG Feng-yu, CHENG Jiang. Determination of High-content Sulfur in Lead-Zinc Ore by Elemental Analyzer[J]. Rock and Mineral Analysis, 2015, 34(2): 234-237. doi: 10.15898/j.cnki.11-2131/td.2015.02.014
Citation: XU Guo-dong, GE Jian-hua, WANG Feng-yu, CHENG Jiang. Determination of High-content Sulfur in Lead-Zinc Ore by Elemental Analyzer[J]. Rock and Mineral Analysis, 2015, 34(2): 234-237. doi: 10.15898/j.cnki.11-2131/td.2015.02.014
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应用元素分析仪测定铅锌矿中的高含量硫

  • 中国地质调查局成都地质调查中心, 四川 成都 610081

  • 基金项目: 西藏华钰股份有限公司资助项目(20121129)
详细信息
    作者简介: 徐国栋, 硕士, 工程师, 主要从事岩石矿物分析工作.E-mail: xgd1230@163.com
    通讯作者: 王凤玉, 工程师, 主要从事X射线衍射分析和岩石矿物分析工作.E-mail:wangfu59@163.com

  • 中图分类号: O657.3

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

  • Chengdu Geological Survey Center, China Geological Survey, Chengdu 610081, China

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    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。

    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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  • 表 1  添加剂种类对铅锌矿样品中硫含量测定结果的影响

    Table 1.  Effect of additives on the analytical results of sulfur in lead-zinc ore

    添加剂硫的含量(%)RSD
    (%)
    6次分次测定值平均值
    线状氧化铜14.35 14.31 14.28
    14.31 14.39 14.25    		14.310.3
    五氧化二钒14.33 14.24 14.37
    14.40 14.27 14.29    		14.330.4
    三氧化钨12.25 13.10 13.00
    12.40 12.55 12.85    		12.532.5
    下载: 导出CSV

    表 2  方法精密度

    Table 2.  Precision tests of the method

    样品编号硫的含量(%)RSD
    (%)
    12次分次测定值平均值
    样品120.3220.3720.2520.320.4
    20.2120.3920.25
    20.4020.2420.38
    20.2320.4220.35
    样品213.3413.2413.3513.330.6
    13.4113.2213.42
    13.2413.4413.28
    13.3413.3713.29
    样品39.859.799.809.860.6
    9.909.859.91
    9.879.959.88
    9.939.799.80
    下载: 导出CSV

    表 3  元素分析仪法与重量法测定结果比对

    Table 3.  Comparison of analytical results of sulfur determined with Elemental Analyzer and gravimetry

    样品编号硫的测定值(%)相对偏差
    (%)
    本法(元素分析仪)重量法
    样品120.3220.400.4
    样品213.3313.250.6
    样品39.869.770.9
    下载: 导出CSV
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出版历程
收稿日期:  2013-11-04
修回日期:  2015-02-08
录用日期:  2015-03-05
刊出日期:  2015-02-25

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