离子色谱法测定中总硫.docVIP

离子色谱法测定煤中总硫李淑敏1 应波1 岳银玲1 景宽2(1.中国疾病预防控制中心环境与健康相关产品安全所，北京 100050;2.北京工业大学) 摘要：目的：建立离子色谱法测定煤中总硫的方法。方法：以过氧化氢作为吸收液收集煤的热解气，在吸收液中硫的氧化物转化为SO42-，选用抑制型电导检测器，DionexAS12A 阴离子分析柱，以碳酸盐作为淋洗液，进样体积50μL。通过测定吸收液中SO42-的浓度，计算出煤中总硫的含量。结果：本方法与国家标准方法GB/T214-1996高温燃烧中和法进行了比较，其相对标准偏差小于2%，符合检验方法的要求。对国家煤标准参考物质GBW11104c和GBW11110d进行了测定，测定值与标准参考值相吻合。结论：离子色谱法测定煤中总硫具有方便，准确，快捷的优点，可用于煤炭中总硫的测定。关键词：煤中总硫，离子色谱法，二氧化硫　 　Determination of Total Sulfur in Coal by Ion ChromatographyLi Shumin1, Ying Bo1*, Jing Kuan2 National Institute for Environmental Health and Related Product Safety, Chinese Center for Disease Control and Prevention, Beijing 100050, China; 2. Beijing University of Technology，Beijing 100021,China) 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 with 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 50μL. 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%, two kinds of national certified reference materials (GBW11104c and GBW11110d) were determined, and was found to be in good agreement with the certified values. Conclusions 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. Key words: Coal; total sulfur; ion chromatography　　我国是煤炭消费大国,煤做为燃料在直接燃烧过程中，煤中各种形态存在的硫大部分以二氧化硫的形式排放到空气中, 成