高温燃烧水解-离子色谱法测定煤中的氟和氯
王芳1,王海峰2,徐建1,王茜2,史乃捷2
中国石油大学化学工程学院,北京;中国计量科学研究院,北京
Determination of Fluorine and Chlorine in Coal by High Temperature Combustion
王芳1,王海峰2,徐建1,王茜2,史乃捷2
(1. Institute of Chemical Engineering, China University of Petroleum, Beijing 102249, China; 2. National Institute of Metrology of China, Beijing 100029, China)
摘要:建立高温燃烧水解 -离子色谱法测定煤中氟和氯含量的方法。间隔测量煤标准物质和待测煤样,以煤标 准物质特性量值的变化扣除系统漂移的影响,提高了测定结果的准确度和重复性。氟含量在 0.042~2.018 μg/mL 范 围内与其色谱峰面积呈良好的线性关系,线性相关系数 r=0.995 8,检出限为 0.011 μg/g,测量结果相对标准偏差为 6.32% (n=6) ;氯含量在 0.046~2.292 μg/mL 范围内与其色谱峰面积呈良好的线性关系,线性相关系数 r=0.999 8 ,检 出限为 0.010 μg/g,测量结果的相对标准偏差为 0.7% (n=6)。用该方法对煤标准物质进行测定,氟、氯测定结果与标 准值一致。该方法简便快速,灵敏度高,结果准确,可用于煤中氟和氯含量的测定。
Abstract:The method of high temperature combustion hydrolyzing-ion chromatography for the simultaneous determination of chlorine and fluorine in coal was established. Focused on the elimination of system drift, the method of interval measuring coal certified reference materials and coal samples was used to reduce the system drift from the changes of coal certified reference material properties, and improve the accuracy and repeatability. The content of fluorine was linear with peak area in the range of 0.042-2.018 μg/mL, the linear correlation cofficient r=0.9958, the detection limit was 0.011 μg/g, and the relative standard deviation of detection results was 6.32%(n=6). The content of chlorine was linear with chromatographic peak area in the range of 0.046-2.292 mg/mL, the linear correlation coefficient r=0.9998, the detection limit was 0.010 μg/g, and the relative standard deviation of detection result was 0.7%(n=6). Coal certified reference material was detected with the method, and the detection results were consistent with standard value. This method is fast, sensitive, and accurate, it is suitable for the determination of fluorine and chlorine in coal samples.
关键词:高温燃烧水解;离子色谱法;煤;氟;氯;标准物质
Keywords:high temperature combustion hydrolyzing; ion chromatography; coal; fluorine; chlorine; certified reference material
基金:国家质量监督检验检疫总局公益性行业科研专项
本文引用格式:
王芳,王海峰,徐建,等.高温燃烧水解-离子色谱法测定煤中的氟和氯[J].化学分析计量,2016,25(4):27-30.
WANG F,WANG H F,XU J,et al.Determination of Fluorine and Chlorine in Coal by High Temperature Combustion[J]. Chemical analysis and meterage,2016,25(4):23-26.
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