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Talanta. 2016 Feb 1;148:419-26. doi: 10.1016/j.talanta.2015.11.019. Epub 2015 Nov 6.

Determination of gold and silver in geological samples by focused infrared digestion: A re-investigation of aqua regia digestion.

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Department of Chemistry, Brock University, St. Catharines, Ontario, Canada L2S 3A1.
Department of Chemistry, Brock University, St. Catharines, Ontario, Canada L2S 3A1. Electronic address:


Focused infrared radiation-based digestions, for the determination of gold and silver, can be achieved in a timeframe as short as 10-15 min, making it an attractive candidate technology for the mining industry, where very large numbers of samples are analyzed on a daily basis. An investigation was carried out into gold and silver dissolution chemistry from geological samples using this novel digestion technique. This study investigated in-depth the issue of low recoveries of gold from aqua regia (AR) digestions, reported by a number of researchers. Conventional AR digestions consistently delivered gold recoveries in a range of 69-80% of the certified values for the four certified reference materials (CRM) employed (CCU-1d, SN26, OREAS 62c, and AMiS 0274), while silver recoveries were satisfactory. By gradually shifting the HCl:HNO3 ratio (v/v) from 3:1 to a reversed 1:3 ratio, recoveries of gold and silver exhibited inverse trends. At a HCl:HNO3 ratio of 1:3, complete recovery of gold was achieved with excellent reproducibility in all CRMs. Meanwhile, silver recoveries plunged significantly at this ratio in samples with higher silver concentrations. Silver values were recovered, however, when the silver was re-solubilized by adding a small volume of concentrated HCl to the cooled reverse aqua regia digests. Recoveries of base metals, such as Fe and Cu, were satisfactory throughout and were much less sensitive to changes in the digestion medium. Using four CRMs and five real-world gold/silver containing samples, the utility of the proposed reverse aqua regia was systematically studied. The uncomplicated nature of the digestion methods reported here, that are fast, effective and inexpensive, may be useful to analysts developing/optimizing their methods for the rapid determination of Au and Ag in a variety of mineral phases, particularly where rapid results are desirable, such as in prospecting and mine development.


Aqua regia; Gold; ICP-MS; Infrared; Reverse aqua regia; Sample digestion; Silver

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