Preparation and Characterization of Reduced-Charge Hectorites

William F. Jaynes, Samuel J. Traina, Jerry M. Bigham and Cliff T. Johnston
Agronomy Department, The Ohio State University, Columbus, Ohio 43210
Department of Soil Science, University of Florida, Gainesville, Florida 32611

Abstract: A series of reduced-charge (RC) hectorites were prepared by multiple heat (250°C) treatments of Mg-saturated hectorites (SHCa-1). Cation exchange capacity (CEC) measurements and alkylammonium exchange indicated that a decrease in layer charge occurred with each Mg-250 treatment. Chemical analyses showed that decreases in structural Li and increases in structural Mg contents coincided with charge reduction. Fluorescence measurements of adsorbed quinoline indicated that the hectorite surface was acidified during charge reduction; hydroxyl group deprotonation is a possible source for the acidity. Fourier transform infrared spectra (FTIR) indicated that the Mg-250 treatment induced the loss of structural Li and shifted the SiO stretch band to a position similar to that in talc. The relative intensities of the OH and SiO stretch bands in FTIR spectra suggest that some of the hydroxyl groups in hectorite were lost, possibly by deprotonation. However, thermogravimetric data (TG) reveal no significant difference in the hydroxyl contents of the hectorites.

The FTIR spectra, CEC, layer charge, chemical, and TG data all supported the view that Mg substitution for octahedral Li occurred which resulted in a more “talc-like” structure. Charge reduction in smectites is evidently a general phenomenon and can be induced by heat treatment with the proper exchangeable cation. The ability to reduce the charge of hectorites makes it possible to prepare a series of clays which vary in charge but lack structural Fe. Such RC smectites should be suitable for expandable clay mineral studies which utilize spectroscopic techniques that are sensitive to Fe content.

Key Words: Alkylammonium exchange • Cation exchange capacity • Dehydroxylation • Deprotonation • Fluorescence • Infrared spectroscopy • Quinotine • Surface acidity • Thermogravimetry

Clays and Clay Minerals; August 1992 v. 40; no. 4; p. 397-404; DOI: 10.1346/CCMN.1992.0400404
© 1992, The Clay Minerals Society
Clay Minerals Society (www.clays.org)