CAJ | 학술논문

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。
건립료용우예부집류화동얼광중조로파의박5충박족원소적필제시금방법。40.0 g 양화필、25.0 g붕산、10.0 g 탄산납、1.00 g 정분여10.0 g 대측양품우120 mL 자명중,충분혼균,850℃입로,20 min 후승지1000℃,보류40 min,출로후진열경도용사,사필시금우공기중자연냉각。설계량단회취류정,필시금선재미사회명내회취,직지잉여직경약5 mm,이후직접전입성유20 g 용융제분적감과개중계속회취,획득직경약1 mm 적시금합립。소득합립경미파소해,냉각후정용지10 mL。박파용 ICP-OES 분석；조로의질량수선택99 Ru,103 Rh 화191 Ir,이115 In 화185 Re 위내표,응용 ICP-MS 분석。대표준물질 GBW07196평행측정12차,박족원소상대표준편차위7.0%~9.5%。재10 g 취양량조건하,방법대 Ru, Rh, Pd, Ir 화 Pt 적검출한분별위0.027,0.016,0.11,0.10화0.11 ng/ g。응용본방법처리표준물질 GBW07194,GBW07195화 GBW07196균획득료만의적결과。
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.