This project focuses on the use of the Prompt Gamma-ray Activation Analysis (PGAA) technique available at the Nuclear Engineering Teaching Laboratory of the University of Texas at Austin to precisely determine the hydrogen (proton) contents in layered oxide cathode samples obtained by chemical lithium extraction in order to obtain a better understanding of the factors limiting the practical capacities and overall performance of lithium ion battery cathodes. The project takes careful precautionary experimental measures to avoid proton contamination both from solvents used in chemical delithiation and from ambient moisture. The results obtained from PGAA are complemented by the data obtained from other techniques such as thermogravimetric analysis, redox titration, atomic absorption spectroscopy, X-ray diffraction, and mass spectroscopic analysis of the evolved gas on heating. The research results broaden our understanding of the structure-property-performance relationships of lithium ion battery cathodes and could aid the design and development of new better performing lithium ion batteries for consumer (portable and electric vehicles), military, and space applications.