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Chemical Determination of Sorbed Water and Structural Hydroxyl in Colloidal Minerals of Soils and Sediments¹

ABSTRACT

A method is described for the differentiation of sorbed water from structural hydroxyl ions for colloidal minerals of soils and sediments. It is based on the extraction of the sorbed water (including external surface sorbed and interlayer water) with methanol. The structural hydoxyl is determined by heating the sample in a silica tube oven, passing a gas through the tube, and collection of the liberated water in methanol. The water contents of the methanol solutions are determined titrimetrically by utilization of the Karl Fischer reagent. This method is preferred to the less satisfactory methods based on thermal weight-loss. Hydroxyl determinations are given some 2:1 layer silicates and other hydroxyl compounds as examples of the type of studies made possible by the technique.

¹ Contribution from the Department of Soils, University of Wisconsin, Madison. This work was supported in part by the University Research Committee through a grant of funds from the Wisconsin Alumni Research Foundation.

² Graduate Assistant and Professor of Soils, respectively.