This report, the fourth of a related series dealing with the isotopic analysis of uranium, describes the use of a hollow cathode source and a 4-m, direct-reading, Bausch and Lomb high-resolution spectrograph. A relative precision of ±3.0%, expressed at the 95% confidence level, was obtained with naturally occurring uranium for a single cathode determination of U<sup>235</sup> measured in twenty min. Evidence for a weak uranium line structure interfering with the U<sup>235</sup> measurement is presented. Minor isotopes, U<sup>234</sup> and U<sup>236</sup>, present up to a few percent at the higher U<sup>235</sup> concentrations, did not interfere with U<sup>235</sup> measurements. Measurements of U<sup>234</sup>, however, could not be made in the presence of high U<sup>235</sup> concentrations, thereby limiting the determination of total uranium necessary for calculating the percent U<sup>235</sup>. At the lower U<sup>235</sup> concentrations, the concentrations of minor isotopes are generally too small to significantly affect the total uranium content of the sample.
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