In the atomic energy pile at Chalk River, heavy water (deuterium oxide, D2O) is to be used as a moderator. Early in 1944, it became evident that frequent determinations of the isotopic composition of D2O samples would be required. For this purpose, there was obtained from the American authorities a mass spectrometer specially designed for routine hydrogen isotope analysis. This instrument was assembled and put into operation at McMaster in the summer of 1944. During the course of subsequent work, two other deuterium mass spectrometers were built in this laboratory, following the design of the instrument sent from the United States; one of these has now been installed at the plant site, and a second is to follow at an early date. The studies reported below involved the determination of operating conditions, the measurement of grid leaks, of the order of 10^10 ohms, and the investigation of further applications of the deuterium mass spectrometer. / Thesis / Master of Science (MSc)