Quantitative NMR Analysis of PTMEG compounds

IF 0.4 Q4 BIOCHEMICAL RESEARCH METHODS Journal of the Korean magnetic resonance society Pub Date : 2016-03-20 DOI:10.6564/JKMRS.2016.20.1.007
Gilhoon Kim, Hoshik Won
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Abstract

glycol) is a polymer compound widely used as a wide range of applications in the textile industry. PTMEG sub-stance carrying various 1,800~2,000 molecular weight are mainly used as the raw material of the spandex production. Molecular weight and degree of polymerization value for 4 different PTMEG samples under pilot plant scale synthetic process were determined by a new quantitative NMR method. In NMR experiments, p -toluenesulfonic acid(TSOH) was used for external standard material of PTMEG quantitative analysis. were measuring The concentration of the primary standard TSOH was measured by UV/Vis spectroscopy. By using NMR peak assignments and the integral values of designated proton NMR peaks, We were able to measure the % composition of the synthetic PTMEG polymers, concentrations, molecular weight and the degree of polymerization that show the synthetic process of each manufacturing pilot plant. By utilizing a newly developed quantitative NMR method were able to obtain the molecular weight of PTMEG samples within 0.08 error % range.
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PTMEG化合物的定量核磁共振分析
乙二醇是一种广泛使用的高分子化合物,在纺织工业中有着广泛的应用。PTMEG物质的分子量在1800 ~ 2000之间,主要用作生产氨纶的原料。采用一种新的核磁共振定量方法测定了中试规模合成过程中4种不同PTMEG样品的分子量和聚合度值。在核磁共振实验中,对甲苯磺酸(TSOH)作为PTMEG定量分析的外标物。采用紫外/可见光谱法测定主要标准品TSOH的浓度。通过核磁共振峰分配和指定质子核磁共振峰的积分值,我们能够测量合成PTMEG聚合物的百分比组成,浓度,分子量和聚合程度,显示每个制造中试工厂的合成过程。利用新开发的定量核磁共振方法,可以在0.08 %的误差范围内获得PTMEG样品的分子量。
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Journal of the Korean magnetic resonance society
Journal of the Korean magnetic resonance society BIOCHEMICAL RESEARCH METHODS-
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