Suggested guidelines for the publication of Rietveld analyses and pattern decomposition studies

Abstract

The filling of thin-walled glass capillaries is tedious and time consuming especially when the powder tends to agglomerate due to extremely fine grinding (<10 t~m) in a micronizing mill. While special devices have been designed for loading capillaries in a dry box (Larsen & Leddy, 1958; Lange & Haendler, 1972), a technique greatly facilitating routine loading is currently in use in our laboratory. It involves placing the capillary in a nearly upright position in a 50 ml Erlenmeyer flask filled with water. The best results were obtained when the water level in the flask was just below the base of the capillary funnel. The flask is then placed in an ultrasonic bath (filled to a depth of one inch with water) where the vibration promotes disaggregation and movement of the particles into the capillary. Occasional clogging of the capillary funnel during loading of highly agglomerating powders can be relieved by insertion of a fine wire probe during agitation. Loading, the rate of which depends in part on capillary diameter and particle size and density, normally requires less than five minutes of ultrasonic agitation.