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A new method for the estimation of proton concentrations in montmorillonite catalysts was developed that makes use of the well-resolved thermal desorption of intercalated cyclohexylamine. The clay sample was emersed in liquid cyclohexylamine, dried, and its thermal desorption plotted by means of a thermal gravimetric balance fitted with differential thermal gravimetric analyzer (TGA-DTG). The differential thermogravimetric (DTG) desorption curves for this cyclohexylamine-adsorbed material had four distinct desorptive zones, one of which was assigned to the thermal desorption of intercalated cyclohexylammonium ions. The percentage weight loss corresponding to this region of the curve gave a measure of the concentration of cyclohexylammonium ions in the montmorillonite sample. This value was then expressed in terms of the concentration of protons in the clay available to cyclohexylamine. A comparison, for a series of Al13-exchanged and heat-treated montmorillonites, of these proton concentrations with the catalytic activities of the clays indicated that high proton concentration correlated with strong catalytic activity.

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