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硅烷偶联剂Si-69中单质硫与化合态硫的液相色谱分析研究
引用本文:吴艳青,李美江,张宁雯,王姗姗,蒋可志. 硅烷偶联剂Si-69中单质硫与化合态硫的液相色谱分析研究[J]. 杭州师范大学学报(自然科学版), 2014, 0(6): 575-578
作者姓名:吴艳青  李美江  张宁雯  王姗姗  蒋可志
作者单位:杭州师范大学有机硅化学及材料技术教育部重点实验室;
基金项目:国家自然科学基金青年科学基金项目(21205025)
摘    要:使用液相色谱及液质联用技术建立了硅烷偶联剂Si-69中单质硫和化合态硫各自含量的分析方法.以C8柱为液相分离柱,采用简单的甲醇-水流动相体系进行梯度淋洗,Si-69各组分得到了很好的分离.Si-69样品中鉴定出单质硫,并根据外标法测得其质量分数为16.8mg/g.同时,对样品中含硫化合物进行分析、鉴定,计算出化合态硫质量分数为28.26%,平均硫链长为3.55.本方法操作简单、快速,可用于Si-69的硫质量控制分析.

关 键 词:硅烷偶联剂Si-69  液相色谱  液质联用  单质硫  化合态硫

The Liquid Chromatography Analysis of the Elemental and the Combined Sulfur in Silane Coupling Agent Si-69
WU Yanqing,LI Meijiang,ZHANG Ningwen,WANG Shanshan,JIANG Kezhi. The Liquid Chromatography Analysis of the Elemental and the Combined Sulfur in Silane Coupling Agent Si-69[J]. , 2014, 0(6): 575-578
Authors:WU Yanqing  LI Meijiang  ZHANG Ningwen  WANG Shanshan  JIANG Kezhi
Affiliation:(Key Laboratory of Organosilicon Chemistry and Material Technology of Ministry of Education, Hangzhou Normal University, Hangzhou 311121, China)
Abstract:In this study,the method for analyzing the content of the elemental and the combined sulfur in silane coupling agent Si-69 is established by liquid chromatography and liquid chromatography-mass spectrometry.Every component in Si-69 is well separated by using gradient elution with the simple mobile phase system of methanol-water.Elemental sulfur is detected in Si-69 samples,and quantitated to be 16.8 mg/g according to the external standard method.In addition,the combined sulfur content is determined to be 28.26% and the length of average sulfur chain to be 3.55.This method is simple and fast,and suitable for sulfur quality control analysis of Si-69.
Keywords:silane coupling agent Si-69  liquid chromatography  HPLC-MS  elemental sulfur  combined sulfur
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