O'Reilly John W, Shaw Matthew J, Dicinoski Greg W, Grosse Andrew C, Miura Yasuyuki, Haddad Paul R
Australian Centre for Research on Separation Science, School of Chemistry, University of Tasmania, Hobart.
Analyst. 2002 Jul;127(7):906-11. doi: 10.1039/b204118a.
A method for the separation of the polythionates (SxO6(2-), x = 3-5) in gold thiosulfate leach solutions using ion-interaction chromatography with conductivity and ultraviolet (UV) detection is described. Polythionates were eluted within 18 min using an eluent comprising an acetonitrile step gradient at 0.0 min from 15% v/v to 28% v/v, 3 mM TBAOH, and 2.5 mM sodium carbonate, operated using a Dionex NS1-5 micron column with guard. The developed method was capable of separating the gold thiosulfate complex ion in standard solutions, but quantification of this species in realistic leach solutions proved impractical due to a self-elution effect that caused the gold peak to be eluted as a broad band. Detection limits for polythionates using a 10 microL injection volume ranged between 1-6 mg L(-1) (5-23 microM) for conductivity and 0.8-13 mg L(-1) (4-68 microM) for UV detection, based on a signal-to-noise ratio of 2. Calibration was linear over the ranges 5-2000, 10-2000 and 25-2500 mg L(-1) for trithionate, tetrathionate and pentathionate, respectively. The technique was applied successfully to leach liquors containing 0.5 M ammonium thiosulfate, 2 M ammonia, 0.05 M copper sulfate and 20 % m/v gold ore.
本文描述了一种使用离子相互作用色谱法结合电导和紫外（UV）检测，分离金硫代硫酸盐浸出溶液中连多硫酸盐（SxO6(2-)，x = 3 - 5）的方法。使用一种洗脱液在18分钟内洗脱连多硫酸盐，该洗脱液在0.0分钟时为乙腈分步梯度，从15% v/v到28% v/v，含有3 mM氢氧化四丁铵和2.5 mM碳酸钠，使用带保护柱的戴安NS1 - 5微米柱进行操作。所开发的方法能够在标准溶液中分离金硫代硫酸盐络合离子，但由于自洗脱效应导致金峰以宽带形式洗脱，在实际浸出溶液中对该物种进行定量证明不切实际。基于2的信噪比，使用10微升进样体积时，连多硫酸盐的检测限对于电导检测为1 - 6 mg L(-1)（5 - 23 microM），对于紫外检测为0.8 - 13 mg L(-1)（4 - 68 microM）。连三硫酸盐、连四硫酸盐和连五硫酸盐的校准曲线分别在5 - 2000、10 - 2000和25 - 2500 mg L(-1)范围内呈线性。该技术已成功应用于含有0.5 M硫代硫酸铵、2 M氨、0.05 M硫酸铜和20% m/v金矿石的浸出液。
