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Determination of alkylphenols after derivatization to ferrocenecarboxylic acid esters with gas chromatography-atomic emission detection.

A method is described for the rapid determination of alkylphenols in nonpolar matrixes. The alkylphenols are derivatized with ferrocenecarboxylic acid chloride so that every phenol molecule is labeled with one iron atom. The resulting esters are analyzed by gas chromatography with atomic emission detection (AED) in the iron-selective detection mode. This method utilizes the AED's low detection limit (0.05 pg/s) for iron and the high selectivity versus carbon (3.5 x 10(6)) for the detection of the alkylphenols. Because the derivatization is performed before the first step of sample preparation, the risk of analyte loss by adsorption or volatilization is minimized. The total recoveries in the lower ppm concentration range vary between 79 and 125%. The quantification of 20 C0-C3-alkylphenols in crude oils is demonstrated by analyzing a shale oil (SRM 1580) and a petroleum crude oil (SRM 1582). The complete workup is easily carried out in only 45 min/sample.