Collect. Czech. Chem. Commun.
1982, 47, 1973-1978
https://doi.org/10.1135/cccc19821973
Determination of alcohols in mixtures by 19F NMR spectroscopy using hexefluoroacetone reagent
Jiří Karhana, Zbyněk Ksandra, Jiřina Vlkováb and Věra Špatnác
a Department of Analytical Chemistry
b Laboratory of Synthetic Fuels, Prague Institute of Chemical Technology, 166 28 Prague 6
c The J. Heyrovský Institute of Physical Chemistry and Electrochemistry, Czechoslovak Academy of Sciences, 121 38 Prague 2
Abstract
The determination of alcohols by 19F NMR spectroscopy making use of their reaction with hexafluoroacetone giving rise to hemiacetals was studied on butanols. The calibration curve method and the internal standard method were used and the results were mutually compared. The effects of some experimental conditions, viz. the sample preparation procedure, concentration, spectrometer setting, and electronic integration, were investigated; the conditions, particularly the concentrations, proved to have a statistically significant effect on the results of determination. For the internal standard method, the standard deviation was 0.061 in the concentration region 0.032-0.74 mol l-1. The method was applied to a determination of alcohols in the distillation residue from an oxo synthesis.
