X-Ray Diffractometer Thermal Technique for Study of Structural Changes in Cellulosic Compounds1

Previous x-ray diffraction studies of cellulose derivatives and other organic com pounds have shown that heat often has important effects, facilitating crystallization, transitions, and polymorphic transformations. However, the application of heat treat ments in conjunction with x-ray diffraction studies has usually been laborious, inexact, and at times ambiguous because of limitations of the technique. The present paper describes the adaptation of an x-ray furnace in conjunction with a two-pen potentiometer recorder and temperature-program controller to overcome some of the previous limita tions. A specially designed specimen holder is described. Thermal diffractograms of cellulose acetate and of benzyl and cyanoethyl cellulose are reproduced to demonstrate some of the advantages and possibilities of this technique.