Ex-situ investigation of the structure of negative lead-acid electrodes faces the problem of fast electrode degradation when taken out of the electrolyte. Examining the formed negative electrode structure, whether by optical, chemical, or crystallographic means, retains its central purpose only if the electrode structure is preserved unchanged, at least during the measurement itself. The research showed that an appropriate choice of the solvent to wash the electrode after extraction from the cell is a crucial factor; the best results were obtained when using ethanol in combination with drying in a nitrogen atmosphere.