羟基封端聚丁二烯的临界点色谱定量方法研究

引用本文: 汪明芳, 贾强强, 王月荣, 章弘扬, 张敏, 胡坪. 羟基封端聚丁二烯的临界点色谱定量方法研究[J]. 色谱, 2020, 38(2): 238-243. doi: 10.3724/SP.J.1123.2019.03042 shu

Citation: WANG Mingfang, JIA Qiangqiang, WANG Yuerong, ZHANG Hongyang, ZHANG Min, HU Ping. Determination of hydroxy terminated polybutadiene in the blends by liquid critical condition chromatography[J]. Chinese Journal of Chromatography, 2020, 38(2): 238-243. doi: 10.3724/SP.J.1123.2019.03042 shu

羟基封端聚丁二烯的临界点色谱定量方法研究

汪明芳 ^1, ,
贾强强 ^1, ,
王月荣 ^1, ,
章弘扬 ^1, ,
张敏 ^2, ,
胡坪 ^{1,
,}

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

通讯作者: 胡坪, E-mail:huping@ecust.edu.cn

基金项目:
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。

关键词:

English

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

1.
Shanghai Key Laboratory of Functional Materials Chemistry, School of Chemistry and Molecular Engineering, East China University of Science and Technology, Shanghai 200237, China;
2.
Shanghai Key Laboratory of New Drug Design, School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China

Corresponding author: HU Ping, huping@ecust.edu.cn

Received Date: 30 March 2019
Fund Project:
National Natural Science Foundation of China (No. 81973285).

Abstract: 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.

Key words:

liquid critical condition chromatography(LCCC)
/ hydroxy terminated polybutadiene(HTPB)
/ adhesive
/ quantitative analysis

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

羟基封端聚丁二烯的临界点色谱定量方法研究

通讯作者: 胡坪, E-mail:huping@ecust.edu.cn

English

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

Corresponding author: HU Ping, huping@ecust.edu.cn

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

羟基封端聚丁二烯的临界点色谱定量方法研究

通讯作者: 胡坪, E-mail:huping@ecust.edu.cn

English

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

Corresponding author: HU Ping, huping@ecust.edu.cn

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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