高频红外吸收法测定含黄铁矿等杂质的晶质石墨中固定碳的研究  

Determination offixed carbon in crystalline graphite containing pyrite by high frequency infrared absorption spectrometry

作　　者：王莎莎 周小平 杨凡燕 WANG Sha-sha;ZHOU Xiao-ping;YANG Fan-yan(Ningxia Institute ofBasic Geological Survey;Ningxia Institute ofNuclear Geological Survey,Yinchuan Ningxia 750021,China)

机构地区：[1]宁夏回族自治区基础地质调查院 [2]宁夏回族自治区核地质调查院,宁夏银川750021

出　　处：《煤炭加工与综合利用》2022年第6期93-97,共5页Coal Processing & Comprehensive Utilization

基　　金：宁夏自然科学基金支持(2020AAC03446)。

摘　　要：建立了利用高频红外碳硫仪快速测定含黄铁矿等杂质的晶质石墨中固定碳的分析方法,通过试验确定测试的最佳条件,当称样量为0.0500 g、前处理溶剂为1+4王水、样品前处理灼烧温度为350℃、灼烧时间为1 h、样品燃烧时间和分析时间分别为25 s和30 s,助溶剂加入顺序为纯铁燃剂、钨粒、锡粒,比例分别为0.3∶1.5∶0.1,固定碳的测试结果最佳。经验证,在此前处理和分析条件下,方法检出限为0.0024%,精密度(RSD)为0.27%~2.10%,标准物质的测定值与标准值的相对误差均小于0.5%,不同方法和不同实验室所测得的结果RSD在1.89%~4.87%,符合地质矿产实验室测试质量管理规范(岩石矿物样品化学成分分析)的要求。所建方法分析速度快、准确度高、灵敏度好,可适用于含黄铁矿等杂质的晶质石墨中固定碳的测定。The analysis method for fast determination of fixed carbon in crystalline graphite including pyrite by high-frequency infrared carbon-sulfur instrument was established and the optimal conditions for testing were also determined.When the sample quantity was 0.0500g,the pretreatment solvent was 1 plus 4 king water,the pre-treatment burning temperature was 350℃,the burning time was 1h,the sample combustion time and analysis time were 25s and 30s,respectively,the auxiliary solvent addition order were pure iron combustion agent,tungsten particle,tin particle,the ratio of 0.3∶1.5∶0.1 respectively,the test results of fixed carbon would be the best.It is proved that under previous treatment and analysis conditions,the detection limit was 0.0024%,precision RSD%was 0.27%~2.10%,the relative error of standard material and standard value was less than 0.5%,and the RSD%of different methods and different laboratories was 1.89%~4.87%,which meets the requirements of geological and mineral laboratory test quality management specifications(chemical composition analysis of rock and mineral samples).The built method has faster analysis speed,higher accuracy and better sensitivity,and can be suitable for the determination of fixed carbon in crystalline graphite containing pyrite and other impurities.

关 键 词：高频红外吸收法 晶质石墨 固定碳 

分 类 号：TQ533.1[化学工程—煤化学工程]