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Phase transitions in triammonium hydrogen disulfate (NH4)3H(SO4)2 were studied by means of dielectric measurements and differential thermal analysis. Below room temperature three phase transitions were observed at −8, −132, and −140°C. The dielectric constant along the c*‐direction shows breaks at the −8 and −132°C transitions, while it shows a discontinuous change accompanied with a thermal hysteresis at the −140°C transition. In addition to the above‐mentioned transitions, a broad maximum of the dielectric constant was found at about −28°C along the c*‐direction. However, no thermal anomalies were observed around −28°C.

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