Abstract: In this paper, the milk deteriorative process was experimentally studied by means of the method of ultrasonic spectral analysis for tissue characterization. The relation of ultrasonic spectral attenuation and the store time for the milk sample was obtained. This relation expresses the process of milk.deterioration. At the same time, it is demonstrated experimentally that the measurement temperature is the main factor which affect the milk deteriorative process. These experimental studies can be used to establish an experimental foundation for the nondestructive testing of emulsion food.