Convergent beam electron diffraction (CBED) is a powerful method for the measurement of lattice parameters in small specimen volumes, such as single crystalline particles or different regions of one particle. In this article we investigate the suitability of the CBED method for measurements in LiCoO2 and correlate small changes in c-lattice parameters to variations in Li content. We find that higher order Laue zone (HOLZ) lines at the 10011 zone axis are well suited to monitor the c-lattice parameter and demonstrate that the best achievable accuracy is about 0.003 angstrom. Comparison between HOLZ line patterns of as-received LiCoO2 particles to HOLZ line patterns obtained of delithiated particles illustrates the effect of decreasing Li content on HOLZ line positions and provides insight into inhomogeneities in the delithiated sample. (C) 2008 Elsevier B.V. All rights reserved.