Wang Yong, Baker Laura A, Brindle Ian D
Department of Chemistry, Brock University, St. Catharines, Ontario, Canada L2S 3A1.
Department of Chemistry, Brock University, St. Catharines, Ontario, Canada L2S 3A1.
Talanta. 2016 Feb 1;148:419-26. doi: 10.1016/j.talanta.2015.11.019. Epub 2015 Nov 6.
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.
基于聚焦红外辐射的消解方法可用于测定金和银,消解时间短至10 - 15分钟,这使其成为采矿业颇具吸引力的候选技术,因为采矿业每天要分析大量样品。利用这种新型消解技术对地质样品中的金和银溶解化学进行了研究。本研究深入探讨了一些研究人员报道的王水(AR)消解金回收率低的问题。对于所使用的四种认证参考物质(CRM)(CCU - 1d、SN26、OREAS 62c和AMiS 0274),传统的王水消解方法得到的金回收率始终在认证值的69 - 80%范围内,而银回收率令人满意。通过逐渐将HCl:HNO₃比例(v/v)从3:1变为反向的1:3比例,金和银的回收率呈现相反趋势。在HCl:HNO₃比例为1:3时,所有CRM中的金均实现了完全回收,且具有出色的重现性。与此同时,在此比例下,银浓度较高的样品中银回收率显著下降。不过,向冷却的反向王水消解液中加入少量浓盐酸使银重新溶解后,银的含量得以回收。整个过程中,铁和铜等贱金属的回收率令人满意,且对消解介质的变化不太敏感。使用四种CRM和五个实际含金银样品,系统研究了所提出的反向王水的实用性。本文报道的消解方法简单,快速、有效且成本低廉,可能对分析人员开发/优化其在各种矿相中快速测定金和银的方法有用,特别是在需要快速得到结果的情况下,如勘探和矿山开发。