A multichambered apparatus for HF solvolysis experiments: reaction of cellulose HF solvolysis products with acetic acid and acetic anhydride

Abstract

Solvolysis of polysaccharides in anhydrous HF has not gained wide acceptance as an analytical tool despite superior reaction characteristics as compared to conventional hydrolytic agents. This reluctance seems primarily related to difficulties in handling HF. However, these difficulties are substantially reduced by an inexpensive, fully-enclosed, many-chambered reactor suitable for use in HF experiments as described in this article. The reactor has the advantages of multiple independent reaction vessels, means to precisely measure liquid HF, means to add measured volumes of reagents directly to the closed reaction vessels during the course of the solvolysis, and provision for rapid temperature changes and control. A series of experiments exploring the direct transition from HF solvolysis to acetolysis conditions by the addition of acetic acid and acetic anhydride, as an alternative to previously published solvolysis termination schemes, is also described.