Pulse techniques for the measurement of attenuation in solids have been extended and refined sufficiently to obtain dependable measurements over a frequency range from 5 to 50 megacycles. Understanding of the relative importance of beam spreading, geometrical boundaries, and method of coupling has been improved. Coupling by means of water buffer and direct mounting is discussed in detail. Attenuation measurements in the frequency range from 5 to 50 megacycles have been made on chrome molybdenum steel specimens, and these measurements have shown large differences in ultrasonic attenuation for samples of the same chemical composition but different heat treatment. The resulting differences are connected with anisotropy which appears in the photomicrographs. The attenuation measurements are quite sensitive to heat treatment and other factors. The application of the methods to metallurgical problems and the physics of solids is suggested.