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The anodic oxidation of N2O4 in aqueous and anhydrous HNO3 has been investigated by controlled‐potential techniques and found to be an excellent method for the preparation of solutions of N2O5 in anhydrous HNO3 . The product solutions can be used directly for the nitrolysis of organic compounds. The oxidation is carried out at approximately +1.85V vs. SCE (aq) at platinum or titanium‐supported iridium oxide anodes. Up to 40g quantities of N2O5 have been prepared with good energy efficiency in a laboratory‐scale, divided cell with a porous Vycor or Nafion separator. Complete oxidation of the N2O4 occurs in a region of low solvent background current; however, the overall current efficiency is reduced to ∼65%, apparently because of transport losses of N2O4 and N2O5 to the catholyte. Several of the species resulting from the dissociation of N2O4 and N2O5 in the solutions have been identified by Raman spectroscopy.

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