Radiation-induced segregation (RIS) has been implicated as a potential contributor to irradiation assisted stress corrosion cracking in light water reactor core components. To better understand changes to grain boundary chemistry during irradiation, RIS was measured in ultra-high purity (UHP) 304 stainless steel using Auger electron spectroscopy (AES). Variations in measured grain boundary concentration, both within a sample and between samples, are reduced by refinements in both the radiation and the AES techniques. These refinements include improvements in temperature control, uniformity of sample-to-sample dose, grain boundary acceptance criteria, amount of intergranular fracture, and amount of beam current used in analysis. AES measurements on samples irradiated at 400°C to 1.0 dpa show how implementing the technique refinements reduces the variability in the measured concentrations. Additionally, measurements from regions of ductile tearing in samples irradiated to 0.1 and 1.0 dpa at 400°C, to 1.0 dpa at 200°C, and from unirradiated samples show that sensitivity factors must be determined to obtain the most accurate measurement of grain boundary composition.