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Quantitative Analysis of Volatile Impurities in Diallyldimethylammonium Chloride Monomer Solution by Gas Chromatography Coupled with Liquid-Liquid Extraction

机译:气相色谱-液相萃取法定量分析二烯丙基二甲基氯化铵单体溶液中的挥发性杂质

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摘要

The quantitative analysis method for volatile impurities in diallyldimethylammonium chloride (DADMAC) monomer solution was established in this paper. The volatile impurities were quantitatively analyzed with trichloromethane as extraction solvent and n-hexane as internal standard by using gas chromatography (GC) coupled with solvent extraction, and the chromatographic conditions, quantitative methods, and extraction conditions were systematically investigated in detail. The results showed that excellent linear relationships of 5 volatile impurities (dimethylamine, allyldimethylamine, allyl chloride, allyl alcohol, and allyl aldehyde) were obtained in the range of 1–100 mg·L−1. The method also showed good specificity, recovery (95.0%–107.5%), and relative standard deviation (RSD, 1.40%–7.67%). This method could accurately detect the whole volatile impurities in DADMAC monomer solution quantitatively in one time with a low detection limit. Furthermore, this method is conducive to the preparation of highly pure DADMAC monomer and the development of national and international standards of the DADMAC monomer product quality, and the results could provide a strong foundation for the regulation and mechanism research of impurities on monomer reactivity in polymerization.
机译:建立了二烯丙基二甲基氯化铵(DADMAC)单体溶液中挥发性杂质的定量分析方法。以三氯甲烷为萃取溶剂,以正己烷为内标,通过气相色谱(GC)结合溶剂萃取对挥发性杂质进行了定量分析,并对系统的色谱条件,定量方法和萃取条件进行了系统地详细研究。结果表明,在1–100 mg·L -1 范围内,获得了5种挥发性杂质(二甲胺,烯丙基二甲胺,烯丙基氯,烯丙醇和烯丙醛)的良好线性关系。该方法还显示出良好的特异性,回收率(95.0%–107.5%)和相对标准偏差(RSD,1.40%–7.67%)。该方法可以一次定量准确地检测DADMAC单体溶液中的所有挥发性杂质,且检出限低。此方法有利于制备高纯度的DADMAC单体,并为制定国内外DADMAC单体产品质量标准提供了依据,该结果可为聚合反应中杂质对单体反应性的调控和机理研究提供坚实的基础。 。

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