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1H NMR assisted quantification of glycerol carbonate in the mixture of glycerol and glycerol carbonate
Talanta ( IF 5.6 ) Pub Date : 2017-09-01 , DOI: 10.1016/j.talanta.2017.08.103
Avneet Kaur , Ranjana Prakash , Amjad Ali

Glycerol carbonate (GLC) is a very important chemical having a variety of application viz., green solvent in organic synthesis, an electrolyte in lithium batteries, wetting agent in cosmetics and precursor in polymer and food industry for the synthesis of 1,3-sn-diglycerides. Hence, it is vital to find out the quick and simple method for the quantification of GLC when it is synthesized via dimethyl carbonate (DMC) assisted transesterification with glycerol (GL). Present study, proposes simple, accurate and non destructive quantitative proton nuclear magnetic resonance (qHNMR) method for the determination of GLC. Based upon the study, two different equations are proposed to calculate the GLC employing the data obtained from the 1H NMR spectra. qHNMR results were also validated by preparing the standard mixtures of varying concentrations of GL and GLC. Further, to conform the developed method for a real application, GLC concentration was also estimated during CaO catalyzed DMC transesterification with GL. The qHNMR assisted GLC quantification were found consistent with those obtained from high-performance liquid chromatography analysis (R2 = 0.99).



中文翻译:

1 H NMR辅助定量甘油和碳酸甘油酯混合物中的碳酸甘油酯

甘油碳酸酯(GLC)是具有多种应用的一个非常重要的化学即,在有机合成绿色溶剂,在锂电池中的电解质,在聚合物和食品工业化妆品和前体的润湿剂为1,3-合成SN -甘油二酯。因此,当通过碳酸二甲酯(DMC)辅助甘油的酯交换反应合成GLC时,找到一种快速简单的GLC定量方法至关重要。本研究提出了一种简单,准确,无损的定量质子核磁共振(qHNMR)测定方法。根据这项研究,提出了两个不同的方程式,以使用从1得到的数据来计算GLC。1 H NMR谱。还通过制备各种浓度的GL和GLC的标准混合物来验证qHNMR结果。此外,为了使开发的方法适合实际应用,还需要在CaO催化的DMC与GL酯交换过程中估算GLC浓度。发现qHNMR辅助的GLC定量与从高效液相色谱分析获得的定量一致(R 2 = 0.99)。

更新日期:2017-09-01
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