建立了用于预富集硫化铜镍矿中钌铑钯铱铂5种铂族元素的铋锑试金方法。40.0 g 氧化铋、25.0 g硼酸、10.0 g 碳酸钠、1.00 g 淀粉与10.0 g 待测样品于120 mL 瓷皿中,充分混匀,850℃入炉,20 min 后升至1000℃,保留40 min,出炉后趁热倾倒熔渣,使铋试金于空气中自然冷却。设计两段灰吹流程,铋试金先在镁砂灰皿内灰吹,直至剩余直径约5 mm,而后直接转入盛有20 g 熔融锑粉的坩埚盖中继续灰吹,获得直径约1 mm 的试金合粒。所得合粒经微波消解,冷却后定容至10 mL。铂钯用 ICP-OES 分析；钌铑铱质量数选择99 Ru,103 Rh 和191 Ir,以115 In 和185 Re 为内标,应用 ICP-MS 分析。对标准物质 GBW07196平行测定12次,铂族元素相对标准偏差为7.0%~9.5%。在10 g 取样量条件下,方法对 Ru, Rh, Pd, Ir 和 Pt 的检出限分别为0.027,0.016,0.11,0.10和0.11 ng/ g。应用本方法处理标准物质 GBW07194,GBW07195和 GBW07196均获得了满意的结果。%A bismuth-antimony fire assay method for the preconcentration of ruthenium, rhodium, palladium, iridium and platinum in copper-nickel sulfide ores was developed. 40. 0 g bismuth trioxide, 25. 0 g boric acid, 10. 0 g sodium carbonate and 1. 00 g starch were mixed with 10. 0 g sample in a 120 mL porcelain bowl, which was put in a furnace at 850 ℃. After 20 min the temperature was raised to 1000 ℃ and held for another 40 min, and then the bowl was taken out, with the slag poured, which left the bismuth button to air cooling. A two-step cupellation procedure was developed. During the first step, the bismuth button was cupellated in a magnesia cupel until its diameter reached 5 mm or so, then it was transferred to a crucible cover containing 20 g melting antimony and kept cupellating, at last a bead with a diameter of 1 mm was obtained. The bead was microwave-digested, after cooling down to room temperature, the solvent of which was transferred to a volumetric flask and diluted to 10 ml with water. Pt and Pd were analyzed by inductively coupled plasma-atomic emission spectrometry ( ICP-AES), while 99 Ru, 103 Rh, 191 Ir were analyzed by inductively coupled plasma-mass spectrometry (ICP-MS), with 115 In, 185 Re as internal standard. RSD (n = 12) of the analysis results of five platinum group elements ( PGEs) in standard reference material GBW07196 ranged from 7. 04% to 9. 48% . Under the condition of 10 g sample, the detection limits (ng / g) for PGEs are 0. 027 for Ru, 0. 016 for Rh, 0. 11 for Pd, 0. 10 for Ir and 0. 11 for Pt. The method was applied to the determination of PGEs in GBW07194, GBW07195, GBW07196 with satisfactory results.
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