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[离子色谱法测定煤中的全硫]

[Determination of total sulfur in coal by ion chromatography].

作者信息

Li Shu-min, Ying Bo, Yue Yin-ling, Jing Kuan

机构信息

Institute for Environmental Health and Related Product Safety, Chinese Center for Disease Control and Prevention, Beijing 100050, China.

出版信息

Wei Sheng Yan Jiu. 2006 Jul;35(4):492-3.

Abstract

OBJECTIVE

To develop a method for determination of total sulfur in coal by ion chromatography.

METHODS

To pretreat the coal by high-temperature combustion with oxygen-flow in tube furnace, and the sulfur with any from in coal was oxidated and converted into oxid of sulfur, which became sulfate after oxidated by H2O2 absorption solution. The separation of sulfate was achieved on DionexAS12A anion exchange column with a carbonate eluent, and the detection is performed by the suppressed conductivity detector with the injection volume of 50 microl. The total sulfur in coals were obtained from the determined results.

RESULTS

The method had been compared with the National Standard Method "High-Temperature Combustion--Neutralization Method for Determination of Total Sulfur in Coal (GB/T214-1996)", and the RSD of the method was less than 2% . This method had good relativity of the linearity (r = 0.9998) at the range of 0 to approximately 15 microg/ml for sulfate. Two kinds of national certified reference materials (GBW11104c and GBWl1110d) were determined, and the RSD were 1.92% and 0.47% respectively.

CONCLUSION

Ion chromatography for determination of total sulfur in coal has simple operation, high accuracy, and fast analysis, and can be applied in determination of total sulfur in coal.

摘要

目的

建立离子色谱法测定煤中全硫的方法。

方法

将煤样在管式炉中于氧气流中高温燃烧进行预处理,煤中各种形态的硫被氧化转化为硫的氧化物,经过氧化氢吸收液氧化后变成硫酸盐。在Dionex AS12A阴离子交换柱上,以碳酸盐淋洗液进行硫酸盐的分离,采用抑制型电导检测器检测,进样体积为50微升,由测定结果得到煤中全硫含量。

结果

该方法与国家标准方法《煤中全硫的测定方法 高温燃烧中和法》(GB/T214 - 1996)进行了比较,方法的相对标准偏差小于2%。该方法在硫酸盐浓度0至约15微克/毫升范围内线性相关性良好(r = 0.9998)。对两种国家有证标准物质(GBW11104c和GBW11110d)进行测定,相对标准偏差分别为1.92%和0.47%。

结论

离子色谱法测定煤中全硫具有操作简单、准确度高、分析速度快等特点,可应用于煤中全硫的测定。

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