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We describe powder X-ray diffraction experiments on lithium intercalation compounds. Using a unique electrochemical cell which incorporates a beryllium X-ray window we are able to monitor changes in the host lattice which occur when the lithium concentration is altered electrochemically. The detailed design of the cells and experimental problems which arise when using the in situ X-ray diffraction technique are discussed. Results of experiments on LixTiS2 are reported for 0