高温燃烧水解-离子色谱法测定煤中的氟和氯

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0.042~2.018μg/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0.011μg/g,测量结果相对标准偏差为6.32%(n=6);氯含量在0.046~2.292μg/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0.010μg/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。

Determination of Fluorine and Chlorine in Coal by High Temperature Combustion Hydrolyzing-Ion Chromatography

The method of high temperature combustion hydrolyzing-ion chromatography for the simultaneous determination of chlorine andfluorine 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 offluorine was linear with peak area in the range of 0.042–2.018μg/mL, the linear correlation cofficientr=0.995 8,the detection limit was 0.011μg/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 coefficientr=0.999 8,the detection limit was 0.010μg/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 offluorine and chlorine in coal samples.