详细研究了硫化镍试金预富集-ICP-AES测定矿石中的P t、Pd、Ir、Au的多种影响因素.结果表明硫化镍扣用盐酸溶解,多孔玻砂坩埚过滤溶液, 盐酸和双氧水溶解残渣是比较理想的分析方案.硫化镍扣溶解过程中,Pt、Pd的损失可忽略 .Au的损失相当高,仅能半定量.对于μg/g级的样品,Pt、Pd、Ir、Au的平均回收率在96% ～99%之间,相对标准偏差为1.7%～6.8%(n=5).拟定的方法已用于矿石、精矿的分析.
The effect of various factors on the determination o f Pt,Pd,Ir and Au by ICP-AES was investigated in detail using minified nickel su lfide fire assay preconcentration.The results indicated that after the nickel su lfide bead was dissolved in HCl,filtering the solution by fritted glass crucible and dissolving the residue with HCl+H2O2 were a comparatively ideal analyti cal scheme.During the bead dissolving the losses of Pt and Pd were negligible,th e loss of Au was quite high,and the determination of Au was only semiqantitative .The average recoveries for Pt,Pd and Ir ranged from 96% to 99% for the determin ation of μg/g level,the relative standard derivation(RSD) was 1.7 %～6.8%(n=5).The proposed procedure has been applied to analyse o f ores and concentrates.
参考文献
| [1] | Nogueina Claudio A;Figueiredo M G .Determination of platinumpalladiu miridium and gold in selected geological reference material by radiochemical ne utron activation analysis:comparison of procedures based on aqua regia leaching and sodium peroxide sintering[J].Analyst,1995,120:1441. |
| [2] | Herring D P;Price B D;Stablnton W P .Platinum group metals-an overvie w[C].Symp.Ser.-Australas Inst.Min.Metall,1987,54:123-126. |
| [3] | Bergeron Mario .Determination of PGE in rocks:review of analytical te chniques based on lead and nickel sulfide fire assay[J].CIM Bulletin,1990,83(936):108-113. |
| [4] | Dong Shouan .Modern instrumental analysis on multicomponent precious metals elements[J].Yejin Fenxi,1998,18(02):27. |
| [5] | 刘小荣,董守安.铂族元素和金的硫化镍试金预富集在现代仪器分析方法中的应用[J].贵金属,2002(01):45-52. |
| [6] | Colodner D C;Boyle E A;Edmond J M .Determination of rhenium and plati num in natural waters and sedimentsand iridium in sediments by flow injection i sotope dilution inductively coupled plasma mass spectrometry[J].Analytical Chemistry,1993,65(10):1419-1425. |
| [7] | Garbe-Schoenberg C D;McMurtry G M .In-situ micro-analysis of platinum and rare earths in ferromanganese crusts by laser ablation-ICP-MS[J].Fresenius'Journal of Analytical Chemistry,1994,350:264-271. |
| [8] | Schramel P;Wendler I;Lustig S .Capability of ICP-MS(pneumatic n ebulization and ETV)for Pt analysis in different matrices at ecologically relevant concentrations[J].Fresenius'Journal of Analytical Chemistry,1995,353:115-118. |
| [9] | Luedke C;Hoffmann E;Skole J et al.Particle analy sis of car exhaust by ETV-ICP-MS[J].Fresenius'Journal of Analytical Chemistry,1996,355:261-263. |
| [10] | Farago ME.;Blanks R.;Kelly J.;Kazantzis G.;Thornton I. Simpson PR.;Cook JM.;Delves HT.;Hall GEM.;Kavanagh P. .Platinum concentrations in urban road dust and soil, and in blood and urine in the United Kingdom[J].The Analyst: The Analytical Journal of the Royal Society of Chemistry: A Monthly International Publication Dealing with All Branches of Analytical Chemistry,1998(3):451-454. |
| [11] | James C. Ely;Clive R. Neal;James A. O'Neill Jr.;Jinesh C. Jain .Quantifying the platinum group elements (PGEs) and gold in geological samples using cation exchange pretreatment and ultrasonic nebulization inductively coupled plasma-mass spectrometry (USN-ICP-MS)[J].Chemical geology,1999(3-4):219-234. |
| [12] | Pan Yuanming;Xie Qianli .Extreme fraction of platinum group elements in volcanogenic massive sulfide deposits[J].Economic Geology,2001,96:645-651. |
| [13] | GB/T 15072.6-1994[S]. |
| [14] | Liu Xiaorong;Dong Shouan;Wu Changrong.Stu dy o n platinum group metals in ores by minified fire assay preconcentration[A].Kunming:Yunnan Science a nd Technology Press,1999:299. |
| [15] | Shazali I;Dack L;Gijbels R .Determination of precious metals in ores and rocks by thermal neutron activation analysis/γ-spectrometry after preconce ntration by NiS fire assay and precipitation with tellurium[J].Analytical Biochemistry,1987,196:49. |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%