National Geophysical Research Institute, Hyderabad-500 007, India Manuscript received 14 December 1998, revised 28 April 1999. accepted 29 June 1999 A microwave dissolution method for the determination of gold in sample weight as high as 10 g has been described. The gold concentrations in several field samples and gold reference samples are estimated using ICP-MS after microwave dissolution. 103Rh is used as an internal standard. The gold values obtained compare well with the certified values. The average values obtained on the replicate determinations are within 10% RSD with comparable accuracy. The efficiencies of the microwave dissolution and the open-acid-digestion for the extraction of gold in a few field samples are compared. Microwave dissolution is found to be more efficient apart from giving faster dissolution. The detection limit of gold is found to be 0.02 ng/g using this method.