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A Primary Method for the Determination of Hydroxyl Value of Polyols by Fourier Transform Mid-Infrared Spectroscopy
Authors:M H Tavassoli-Kafrani  J M Curtis  F R van de Voort
Affiliation:1. Lipid Chemistry Group, Department of Agricultural, Food and Nutritional Science, University of Alberta, Edmonton, AB, T6G 2P5, Canada
2. McGill IR Group, Department of Food Science, McGill University, Ste. Anne de Bellevue, Quebec, H9X 2V9, Canada
Abstract:A primary Fourier transform infrared (FTIR) method was developed to determine the hydroxyl value (OHV) of polyols produced from edible oils. The method is a modification of American Society for Testing and Materials 1899‐08, using toluene as the solvent to dissolve the sample and to carry the reactive reagent p‐toluenesulfonyl isocyanate (TSI). TSI reacts with OH groups to produce a carbamate, a functional group that can be measured spectrally between ~1780 and 1690 cm?1 in the differential spectrum that is obtained from spectra collected before and after the reaction. Commercially available 1‐nonanol, which has a defined OHV, is used to develop a calibration. The OHV for a variety of 1° and 2° alcohols, as well as petrochemical and lipid‐based polyols, were then measured to evaluate the performance of the method and to assess the effects of moisture on the results. The FTIR OHV were in accord with the results obtained by AOCS method Cd 13‐60 and were demonstrated to be unaffected by the presence of moisture in the sample. The new TSI‐FTIR method is simpler, much faster (~10 min), and more reproducible and accurate than the AOCS OHV titrimetric methods and is not affected by carboxylic acids, amines or moisture.
Keywords:Alcohols  Polyols  p‐Toluenesulfonyl isocyanate  Carbamate  AOCS method Cd 13‐60  Hydroxyl value
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