Transesterification of fatty acid ethoxylates in supercritical methanol, then gas chromatography-mass spectrometric determination of the derived methyl esters, for identification of the initiators

Unknown fatty acid ethoxylate samples have been transesterified in supercritical methanol, using a loop made of a stainless-steel tubing as the reactor vessel. The initiator acids, now present as the corresponding methyl esters, were determined by gas chromatography-mass spectrometry (GC-MS). Quantitative transesterification is achieved by heating a solution of the ethoxylate sample in methanol at 280 degrees C for 10 min under pressure. The influence of reaction time, temperature, and presence of a Lewis acid catalyst has been investigated. The method of transesterification was optimized in respect of low cost, short reaction time, and availability to laboratories with standard analytical equipment.