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The discharge of a TiS2 electrode in an ambient temperature normalLi/TiS2 organic electrolyte cell has been investigated by dynamic x‐ray diffraction. The new technique involves a continuous in situ measurement of x‐ray diffraction simultaneous with electrochemical polarization. The investigation has provided additional information on electrolithiation of TiS2 . These include: (i) the onset of changes in 101 peak position right from the start of discharge, (ii) correspondence of x in LixTiS2 to state‐of‐charge from coulombic balance; and (iii) details of changes in the c axis during discharge, especially during the first 30% of discharge capacity. The results are discussed along with the cell design, operational details, and merits and limitations of the technique.