Derivatization of compounds containing -OH groups can be accomplished quantitatively with 1,3,2-dioxaphospholanyl chloride. The chemical shifts of phosphorus in the derivatives clearly differentiate alcohols from phenols and carboxylic acids. Quantitation is obtained by use of <sup>31</sup>P FT-NMR spectroscopy in the presence of 2,2,6,6-tetrameth-ylpiperidinyloxy free radical to shorten relaxation times. Compounds with phosphorus chemical shifts differing by as little as 0.1 ppm can be separately determined.

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