To determine mercury in geological materials, samples are digested with nitric acid and sodium dichromate in a closed teflon vessel. After bringing to a constant weight, the digest is mixed with air and a sodium chloride-hydroxylamine hydrochloride-sulfuric acid solution and then Hg(II) is reduced to Hg with stannous chloride in a continuous flow manifold. The mercury vapor is then separated and measured using cold vapor atomic absorption spectrophotometry (CV-AAS). For a 100 mg sample the limit of detection is 20 parts per billion (ppb) Hg in sample. To obtain a 1% absorption signal, the described method requires 0.21 ppb Hg solution (equal to 16 ppb in sample). Precision is acceptable at less than 1.2% RSD for a 10 ppb Hg aqueous standard. Accuracy is demonstrated by the results of the analysis of standard reference materials. Several elements do interfere but the effect is minimal because either the digestion procedure does not dissolve them (e.g., Au or Pt) or the; are normally of low abundance (e.g., Se or Te).