Technical Notes - Industrial Minerals - Calcined Cold-Precipitated Hydrated Iron Oxide

AN X-ray diffraction pattern for "calcined cold precipitated ferric oxide" is reproduced dia-grammatically along with data for other iron oxides by R. C. Mackenzie.1' This pattern, which shows spacings higher than those for any other form of iron oxide, was obtained from material prepared and photographed at several different times over a period of weeks, but later attempts to reproduce the results were unsuccessful, the pattern of hematite being obtained every time.2 In an attempt to solve this problem, the original photographs showing the strange diffraction pattern were examined and a marked similarity to the hematite pattern was noticed, suggesting that the pattern was in fact due to hematite but corresponded to a shorter wavelength of X-rays than the Cu Ka which was assumed to have .been used. The eight strongest lines were provisionally identified with the strongest hematite lines and, by means of the corresponding hematite spacings, the X-ray wavelength was calculated for each line. This gave an almost constant value, with the exception of the innermost line which was somewhat diffuse, and confirmed the presence of hematite. The value obtained, 0.703 ± 0.015Å, corresponds to the molybdenum Ka wavelength. The X-ray tube used was a four-filament demountable tube with a copper target. Other photographs, mostly of soil clays, taken during the same period gave normal patterns of Cu Ka radiation with one exception. This was a calcined soil clay with a high iron content and also showed Mo Ka lines of the hematite structure. The explanation is almost certainly that the copper target was contaminated with molybdenum, but it is not known how this occurred. Specimens of alumino-silicates gave their normal Cu Ka pattern, but as the K absorption edge of iron is a little longer than the Cu Ka wavelength, specimens with a high iron content greatly reduced the intensity of the Cu Ka diffraction lines relative to that of the lines due to the shorter Mo Ka wavelength. The formation of hematite on calcining cold precipitated hydrated ferric oxide3 is thus confirmed. References R. C. Mackenzie: Investigations on Cold-precipi-tated Hydrated Ferric Oxide and its Origin in Clays. Problems of Clay and Laterite Genesis, p. 69, Fig. 4, F. AIME Symposium, St. Louis, Mo. Feb. 19-22, 1951. Published 1952. 'R. C. Mackenzie: Ref. 1. Note added on proof. V. C. Hansen and L. T. Brownmiller: Equilibrium Studies on Alumina and Ferric Oxide and on Combinations of These with Magnesia and Calcium Oxide. American Journal of Science (1928) 5, No. 15, pp. 225-242.