高频燃烧红外吸收法测定萤石中的硫  

Determination of Sulfur in Fluorite by High FrequencyCombustion Infrared Absorption

作　　者：冯丽丽 王成林 管嵩 宋飞 岳振艺 张庆建 齐小花[4] FENG Lili;WANG Chenglin;GUAN Song;SONG Fei;YUE Zhenyi;ZHANG Qingjian;QI Xiaohua(Technical Center for Qingdao Customs,Qingdao,Shandong 266500,China;Huize(Nanjing)Environmental Protection Technology Co.,Ltd.,Nanjing,Jiangsu 211100,China;Qingdao University of Technology,Qingdao,Shandong 266520,China;China Academy of Inspection and Quarantine,Beijing 100176,China)

机构地区：[1]青岛海关技术中心,山东青岛266500 [2]惠泽(南京)环保科技有限公司,南京211100 [3]青岛理工大学,山东青岛266520 [4]中国检验检疫科学研究院,北京100176

出　　处：《中国无机分析化学》2023年第5期484-489,共6页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家重点研发计划项目(2017YFF0108905);海关总署科研计划项目(2020HK250)。

摘　　要：为快速准确测定萤石中硫含量,通过优化样品预处理的温度与时间、最佳称样量、助熔剂及加入量等参数,选择740℃灼烧5 min的方法去除样品中水分,称样量0.2 g,0.5 g纯铁+0.2 g样品+0.2 g锡粒+1.6 g钨粒为熔样条件,利用高频燃烧红外碳硫分析仪快速测定萤石中的总硫含量。通过对萤石有证标准物质的测定以及与X射线荧光光谱标准方法测定结果的比对,对方法的准确度进行验证,方法的标准偏差在0.98%~5.3%,结果表明方法准确度好、精密度高,能够快速测定萤石中的硫含量。In order to determine the sulfur content of fluorite quickly and accurately,the parameters of sample pretreatment were discussed and optimized,such as temperature and time,optimal sampling weight,selection and addition dose of flux.The method of burning at 740℃for 5 min was selected to remove the water in the sample.The melting conditions were 0.2 g of sample,0.5 g of pure iron,0.2 g of tin particles and 1.6 g of tungsten particles.A method for the rapid determination of total sulfur in fluorite by high frequency combustion infrared carbon-sulfur analyzer was discussed.The accuracy of this method was verified by the determination of certified reference materials of fluorite and the comparison with the determination results of standard methods of X-ray fluorescence spectrometry.The standard deviation of this method was between 0.98%and 5.3%.The results show that this method has good accuracy and high precision,and could quickly determine the sulfur content in fluorite.

关 键 词：红外吸收光谱法 萤石 硫测定 

分 类 号：O659.2[理学—分析化学]