羟基封端聚丁二烯的临界点色谱定量方法研究  

Determination of hydroxy terminated polybutadiene in the blends by liquid critical condition chromatography

作　　者：汪明芳[1] 贾强强 王月荣[1] 章弘扬[1] 张敏[2] 胡坪[1] WANG Mingfang;JIA Qiangqiang;WANG Yuerong;ZHANG Hongyang;ZHANG Min;HU Ping(Shanghai Key Laboratory of Functional Materials Chemistry,School of Chemistry and Molecular Engineering,East China University of Science and Technology,Shanghai 200237,China;Shanghai Key Laboratory of New Drug Design,School of Pharmacy,East China University of Science and Technology,Shanghai 200237,China)

机构地区：[1]上海市功能性材料化学重点实验室,华东理工大学化学与分子工程学院,上海200237 [2]上海市新药设计重点实验室,华东理工大学药学院,上海200237

出　　处：《色谱》2020年第2期238-243,共6页Chinese Journal of Chromatography

基　　金：国家自然科学基金(81973285)~~

摘　　要：为建立混合物中羟基封端聚丁二烯(HTPB)的临界点色谱定量方法,以C18为固定相,考察了HTPB在四氢呋喃-乙腈和四氢呋喃-水两种流动相体系下的临界点色谱条件。结果表明,四氢呋喃-乙腈体积比为70.7∶29.3以及四氢呋喃-水体积比为92∶8时,HTPB的保留值与其相对分子质量无关。将该临界点色谱方法用于胶黏剂混合组分中HTPB的测定,结果表明,HTPB在46.7~216.4 mg/L范围内呈良好线性关系,相关系数(r)>0.99,检出限为4.2 mg/L。自配HTPB和矿物油双组分样品的加标回收率为89.2%~101.1%,相对标准偏差小于0.66%(n=6)。应用该方法对市售聚氨酯胶黏剂进行检测,测定结果为HTPB成分占26.6%。该方法快速、准确,能满足聚合物混合产品的生产质量控制和失效分析的要求。A method based on liquid critical condition chromatography(LCCC)was established for the quantification of hydroxy-terminated polybutadiene(HTPB)in polymer blends.The critical conditions for HTPB were investigated using a C18 column as the stationary phase,and tetrahydrofuran(THF)-acetonitrile(ACN)or THF-water as the mobile phase.Irrespective of the relative molecular mass,HTPB was eluted under the critical conditions of THF-ACN(70.7∶29.3,v/v)or THF-water(92∶8,v/v).Under the optimal conditions,the HTPB exhibited satisfactory linearity in the range of 46.7-216.4 mg/L,with a correlation coefficient(r)of 0.997.The limit of detection reached 4.2 mg/L.The recoveries of HTPB from the prepared mixtures of HTPB and mineral oil ranged from 89.2%to 101.1%,with a relative standard derivation of less than 0.66%(n=6).This method was successfully applied to the quantitative analysis of HTPB in a commercial polyurethane adhesive,and 26.6%of HTPB was detected in the product.This LCCC method is simple,convenient,highly selective,and reliable for quality control and failure studies of formulated products.

关 键 词：临界点色谱 羟基封端聚丁二烯 胶黏剂 定量分析 

分 类 号：O658[理学—分析化学]