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A gas volumenometer for solid material is described. Using helium as a pressure medium an accuracy of about 1% or better is achieved for sample volumes of 0.2-0.3 cm 3 . The relative standard deviations range from 0.2 to 0.3%. A novel feature of the method is that a set of pressure and volume readings are collected and used in Boyle's law in the form p 0 /p = 1 + V /V 0 . Plotting these data gives a straight line whose slope is used to calculate V 0 . A standard volume is used for calibration of the apparatus. Sources of experimental error are discussed, and an error analysis of the obtained sample volume is performed. Air, argon, and helium have been used and are compared as pressure media. Mass and volume measurements have been obtained for six substances, and their observed densities are compared with x-ray densities taken from the literature.