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Development of a general acid method for the digestion of gold ore samples together with a comparison of extraction solvents for gold and determination by microwave-induced plasma-atomic emission spectrometry (MIP-AES)†
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2018-06-29 00:00:00 , DOI: 10.1039/c8ja00136g
Wryan Helmeczi 1, 2, 3, 4 , Erick Helmeczi 1, 2, 3, 4 , Laura A. Baker 1, 2, 3, 4, 5 , Yong Wang 1, 2, 3, 4, 6 , Ian D. Brindle 1, 2, 3, 4
Affiliation  

In this paper, we explore a variety of aqueous digestion techniques for the determination of gold, in a wide variety of mineral matrices. Acid digestion methods, based upon modified aqua regia in which a larger proportion of nitric acid (5 : 1 HNO3 : HCl) is involved, competes effectively with fire assay to deliver accurate and precise values for gold in a fraction of the time. Using this ratio of acids, simple sand-bath digestions deliver recoveries of 95 to 98% of gold certified reference values, after a digestion time of approximately 35 minutes. Focused infrared digestions, however, take only 15 minutes, and deliver higher recoveries, in the range of 95 to 104% of gold reference values. An ultrasonic digestion with 1,3-dibromo-5,5-dimethylhydantoin acting as a source of bromine, delivered mediocre recoveries of gold. Gold determinations were conducted using inductively coupled plasma-mass spectrometry (ICP-MS). Solvent extraction of gold from digestion solutions effectively preconcentrate gold and significantly reduces interference from major elements, except for those samples containing high concentrations of iron. The use of 2-octanone as extraction solvent exhibited greater sensitivity than the use of the conventional solvent, methyl isobutyl ketone (MIBK). Although 2-ethylhexanol was also effective at extracting gold, its lengthy time for phase separation and memory effects, which increased wash-in and wash-out times, made it a less attractive extraction medium. For solvent extraction methods, microwave induced plasma-atomic emission spectrometry (MP-AES) was used for the determination of gold.

中文翻译:

开发了一种用于消化金矿石样品的通用酸方法,同时比较了用于金提取的溶剂和通过微波诱导的等离子体原子发射光谱法(MIP-AES)进行测定的方法

在本文中,我们探索了多种水溶消化技术,用于测定多种矿物基质中的金。基于改良王水的酸消化方法,其中较大比例的硝酸(5:1 HNO 3 :HCl),可与火试验有效竞争,从而在短时间内提供准确和精确的金值。使用这种比例的酸,简单的沙浴消解在约35分钟的消解时间后可实现95%到98%的金标准参考值的回收率。但是,聚焦的红外消解仅需15分钟,回收率更高,达到金参考值的95%至104%。用1,3-二溴-5,5-二甲基乙内酰脲作为溴源进行超声波消解,回收的金量中等。使用电感耦合等离子体质谱法(ICP-MS)进行金的测定。从消化液中溶剂萃取金可有效地预浓缩金,并显着减少主要元素的干扰,除了那些含高浓度铁的样品。使用2-辛酮作为萃取溶剂比使用常规溶剂甲基异丁基酮(MIBK)具有更高的灵敏度。尽管2-乙基己醇在提取金方面也很有效,但其相分离和记忆效应的时间过长(增加洗入和洗出时间),使其吸引力不大。对于溶剂萃取方法,微波诱导等离子体原子发射光谱法(MP-AES)用于测定金。这就增加了洗入和洗出时间,使其成为一种吸引力较小的提取介质。对于溶剂萃取方法,微波诱导等离子体原子发射光谱法(MP-AES)用于测定金。这就增加了洗入和洗出时间,使其成为一种吸引力较小的提取介质。对于溶剂萃取方法,微波诱导等离子体原子发射光谱法(MP-AES)用于测定金。
更新日期:2018-06-29
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