高频加热-红外光谱法测定氯化熔盐中碳含量  

Determination of Carbon Content in Chlorinated Molten Salt by High-Frequency Heating-Infrared Spectroscopy

作　　者：王勇 李国伟 郑欣 刘元清 WANG Yong;LI Guowei;ZHENG Xin;LIU Yuanqing(National Quality Supervision and Inspection Center of Vanadium and Titanium Products,Panxi Institute of Vanadium and Titanium Inspection and Testing,Panzhihua,Sichuan Province,617000 China;Quality Measurement and Testing Center of Pangang Group Vanadium&Titanium Resources Co.Ltd.,Panzhihua,Sichuan Province,617099 China)

机构地区：[1]攀西钒钛检验检测院国家钒钛制品质量检验检测中心,四川攀枝花617000 [2]攀钢集团钒钛股份有限公司质量计量检测中心,四川攀枝花617099

出　　处：《科技资讯》2024年第7期93-97,共5页Science & Technology Information

摘　　要：碳是熔盐氯化的重要反应物之一,其含量影响氯化反应的进度。因此,准确测定熔盐中碳含量,对指导生产有重要意义。氯化熔盐属高氯样品,目前用管式炉或高频炉燃烧,红外吸收法测定熔盐中碳含量时,存在无相应标准样品建立仪器标准工本曲线和燃烧产生的氯气易腐蚀仪器的问题。实验提出用氯化钠稀释石油焦标准样品,配制不同浓度的碳校准样品,同时对仪器试剂管改装,以石英砂-氢氧化钙(3∶1)吸收氯气,可以有效解决上述问题。此外,实验还研究了高频功率、助熔剂对碳测定的影响,以高频加热-红外吸收法测定氯化熔盐中碳含量。实验结果表明:加入0.5 g纯铁、1.0 g钨锡混合助熔剂,高频功率为70%时,碳完全氧化成二氧化碳;采用人工合成校准样品建立标准曲线,碳的质量分数在0.86%~6.46%范围内,线性良好,满足生产控制要求。Carbon is one of the important reactants in molten salt chlorination,and its content affects the progress of chlorination reaction,so accurately determining carbon content in molten salt is of great significance for guiding production.Chlorinated molten salt is a high-chlorine sample,which is currently burned by tube furnaces or highfrequency furnaces.and there are problems that there is a lack of corresponding standard samples to establish the standard cost curve of the instrument and the chlorine gas generated by combustion is easy to corrode the instrument when determining carbon content in molten salt by the infrared absorption method.The experiment proposes to dilute the standard samples of petroleum coke with sodium chloride and prepare carbon calibration samples with different con⁃centrations,modifies the reagent tube of the instrument,and absorbs chlorine gas with quartz sand-calcium hydroxide(3:1),which effectively solves the above problems.In addition,the experiment also studies the effects of high-frequency power and flux on carbon determination,and establishes a high-frequency heating-infrared absorption method to determine carbon content in chlorinated molten salt.Experimental results show that when the mixed flux of 0.5 g of pure iron and 1.0 g of tungsten tin is added and high-frequency power is 70%,carbon is completely oxidized to carbon dioxide,and that when artificially-synthesized calibration samples are used to establish standard curves,the mass fraction of carbon is in the range of 0.86%~6.46%,with good linearity,which meets production control requirements.

关 键 词：高频加热 红外光谱法 氯化熔盐 碳 

分 类 号：O659.2[理学—分析化学]