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This method describes equipment and a procedure for the identification by X-ray diffraction of crystalline compounds (1, 2, 3, 4) in deposits formed from or by water during its industrial use. The procedure is basically that of Hull (5) with the contributions of Hanawalt, Rinn, and Frevel (6). This method yields positive identification of the crystalline components of water-formed solids for which X-ray diffraction data are available or can be obtained. Without special treatment, amorphous phases cannot be identified. The sensitivity for a given component varies with a combination of such factors as the density, degree of crystallization, particle size, coincidence of strong lines of components, and the kind and arrangement of the atoms of the component. Minimum percentages for identification may therefore vary between the ranges of 5 to 40 per cent. N 1.—The practice and theory of X-ray diffraction have been described in detail in the Recommended Practice for Identification of Crystalline Materials by the Hanawalt X-ray Diffraction Method (ASTM Designation: E 43) and in other available reference works (7, 8, 9, 10, 11, 12).