化学
分析物
产量(工程)
溶剂
分析化学(期刊)
质子核磁共振
内标
样品制备
核磁共振波谱
色谱法
质谱法
有机化学
材料科学
冶金
作者
Ruslan Muhamadejev,Renāte Melngaile,Paula Paegle,Ieva Zibarte,М. В. Петрова,Kristaps Jaudzems,Janis Veliks
标识
DOI:10.1021/acs.joc.0c02744
摘要
A nuclear magnetic resonance (NMR) spectrometer is a key instrument in the organic synthesis laboratory for structure determination, reaction control, and compound purity analysis. In addition to qualitative analysis, the application of NMR for quantitative analysis (qNMR) is gaining popularity. qNMR allows for simple quantification of crude product mixtures, determination of reaction yields, and purity of organic compounds. The determination of NMR yield requires the addition of an internal standard to each sample. Herein, we report a method where CDCl3 residual solvent signal is used as an internal standard for qNMR after quantification in the solvent batch. This method significantly simplifies sample preparation and allows straightforward recovery of the analyte by the simple evaporation of the NMR solvent. The accuracy of the method is comparable to qNMR with 1,3,5-trimethoxybenzene as an internal standard if the herein described guidelines are followed.
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