Raman and infrared spectra of NH,HZ(I0,), and KH,(I03), were recorded and analysed. The observed splitting!? of the stretching modes of 10, -are due to the distortion of the 10, octahedra. In NH,H,(IO,), , the ammonium ion can rotate freely and the NH,' group forms only weak hydrogen bonds with the oxygen atom. Owing to Fermi resonance, three stretching bands are observed for the OH vibration in both compounds. The hydrogen bonds are slightly shorter in KH,(I03), than in NH,H,(IO,), .