A calorimetric method is described for measuring very low dielectric loss angles at and near liquid helium temperatures and audio frequencies. The accuracy in loss angle is about 3 × 10−7 for thermoplastics. Changes of δ with frequency and temperature are resolved to an even smaller limit. The method is believed to be more sensitive than bridge methods at the same temperature, and is probably capable of considerable improvement. Preliminary measurements on samples of polypropylene, polyethylene, PTFE, poly(ethylene terephthalate) and a glass microscope cover slip give loss angles (at 1 kHz) of 3·7 × 10−6, 2·7 × 10−6, 1·2 × 10−6, 1·2 × 10−4 and 1·4 × 10−3 respectively. Polyethylene shows an interesting single-relaxation-time Debye peak, which may be connected with phonon-assisted tunnelling; at the lowest temperatures its height decreases with increasing voltage. A review is given of previous dielectric loss measurements on reasonably good insulators at helium temperatures and audio frequencies.