This paper is concerned with a new, rapid technique for the determination of total mercury in environmental and biological samples. This technique features the pyrolysis of the sample in a combustion tube at 750°C under an oxygen atmosphere, collection on a gold amalgamator and subsequent detection by atomic absorption spectrometry (AAS) using a silicon UV diode detector. This technique has the advantage of no sample pre-treatment and is free from matrix interference. Eight certified reference materials (CRMs) have been analysed and were found to give results in good agreement with the certified values. The levels determined ranged from 0.035 to 7.06 mg/kg with an average relative standard deviation of 3.6% (n = 8).