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Spray drying is shown to be an effective and rapid method for preparing samples for quantitative analysis by x-ray powder diffraction. Previously intractable problems like the simultaneous analysis of multiple phases in orientation prone systems can be carried out. Using this method, and a computer controlled diffractometer, five and six phase analyses of Devonian shales can be accomplished in approximately forty minutes. A rapid and convenient method for using the absorption diffraction technique for x-ray quantitative analysis is described.