质量平衡法与DSC法测定正十六烷纯度  

Determination of purity of n-hexadecane by mass balance method and differential scanning calorimetry

作　　者：郑鹏 孙倩芸 李锋丽 何云馨 张喆 何东郡 Zheng Peng;Sun Qianyun;Li Fengli;He Yunxin;Zhang Zhe;He Dongjun(Shandong Institute of Metrology,Ji'nan 250014,China)

机构地区：[1]山东省计量科学研究院,济南250014

出　　处：《分析仪器》2024年第2期80-84,共5页Analytical Instrumentation

基　　金：国家市场监督管理总局科技计划项目(2023MK074)。

摘　　要：通过质量平衡法与DSC(差示扫描量热)法对正十六烷进行了纯度分析。质量平衡法中,采用气相色谱FID检测器面积归一化法测定正十六烷主成分及有机杂质,热重和卡尔费休法分析试剂无机组分和水分含量;DSC法通过测定试剂熔融吸热曲线,根据范特霍夫方程计算正十六烷纯度。质量平衡法测定正十六烷纯度为99.30%,不确定度为0.26%;DSC法测定正十六烷纯度为99.35%,不确定度为0.50%。两种正十六烷纯度测定方法一致性良好,其中质量平衡法考察因素较多,适用范围较广,不确定度较小;DSC法操作简单,试剂消耗较小,但其测量不确定度较高,需使用精确度较高的仪器。In determination by mass balance method,the content of main component was tested by gas chromatography FID detector area normalization method while inorganic components were analyzed by Karl Fischer's moisture and ignition methods.The purity of n-hexadecane was calculated according to van der Hoff equation by measuring the melting endothermic curve of reagent in determination by DSC method.The purity of n-hexadecane determined by mass balance method was 99.30%,and the uncertainty was 0.26%.The purity determined by DSC method was 99.35%,and the uncertainty was 0.50%.The two methods had strong consistency.The mass balance method involves more factors,has wide application range and low uncertainty.The DSC method has simple operation and low reagent consumption,but its measurement uncertainty is high,requiring higher precision instruments.

关 键 词：正十六烷 纯度 质量平衡法 DSC 

分 类 号：TQ221.1[化学工程—有机化工]