提出了微波密闭消解难分解Rh、Ir粉及其合金、冶金物料、碎化砂矿的新方法;对比了它们的微波密闭消解和传统分(消)解法的条件;分析了消解后Rh、Ir、Pt、Pd和Au的含量.结果表明:上述各类物质对应消解时间分别为传统法的1/96～1/67、1/24～1/5、1/48～1/16和1/2,无论分析方法随微波密闭消解法的建立而改变与否,总分析流程均大大缩短;2种方法测得贵金属的含量基本吻合.
A novel microwave closed digestion method for treatment of difficultly dissolved Rh, Ir powders and their alloys, metallurgy material, reduced activating placers was developed. The comparison of the dissolving conditions of the proposed method with the traditional methods was conducted. The contents of Rh, Ir, Pt, Pd and Au were determinated. The results show that the digestion time of samples using the new method is 1/96～1/67, 1/24～1/5, 1/48～1/16 and 1/2 of those by traditional methods, respectively. Whether the determination methods change or not, because of the use of microwave closed digestion, the analytical processes are greatly shortened. The determination results of Rh, Ir, Pt, Pd and Au are in accord for the two methods.
参考文献
| [1] | Rudolf Bock.A Handbook of Decomposition Method in Analytical Chemistry[M].北京:中国标准出版社,1987 |
| [2] | Shumao Huang .A Teflon sealed-vessel for the dissolution of precious metal speciater[J].Precious Metals,1992,13(04):53-55. |
| [3] | GB/T 15072.6-1994.GB/T 15072.6-1994.A:27-28.Dissolution Method of Glasstube-chlorination for Difficultly Dissolved Precious Metals and Their Alloys[S]. |
| [4] | Xinhan Jing.Microwave Chemistry[M].北京:科学出版社,2001 |
| [5] | Irina V;Kubrakova.Microwave radition in analytical chemistry the scope and prospects for application[J].Russian Chemical Reviews,2002:283-289. |
| [6] | 周南.试样制备趋势国际研讨会议[J].分析试验室,2005(12):91-92. |
| [7] | Simpson LA;Hearn R;Catterick T .The development of a high accuracy method for the analysis of Pd, Pt and Rh in auto catalysts using a multi-collector ICP-MS[J].Journal of Analytical Atomic Spectrometry,2004(9):1244-1251. |
| [8] | Rumyana Djingova;Heike Heidenveich;Petya Kovacheva et al.On the determination of elements in environmental materials by inductively coupled plasma mass spectrometry and microwave digestion[J].Analytica Chimica Acta,2003,489(02):245-249. |
| [9] | K. Boch;M. Schuster;G. Risse;M. Schwarzer .Microwave-assisted digestion procedure for the determination of palladium in road dust[J].Analytica chimica acta,2002(2):257-265. |
| [10] | Niemela M;Kola H;Eilola K et al.Development of analytical methods for the determination of sub-ppm concentration of palladium and iron in methotrexate[J].Journal of Pharmaceutional and Biomedical Analysis,2004,35(03):433-439. |
| [11] | 张竹青,佘振宝,赵勇胜,李俊峰,张艳,洪梅.微波溶样流动注射分光光度法在线测定金矿石中的金[J].分析试验室,2004(03):12-14. |
| [12] | Ezerskaya, NA;Toropchenova, ES;Kaprielov, IB;Kiseleva, IN;Belov, SF .Controlled-potential coulometric determination of iridium in hexanitroiridate(III) with microwave sample preparation[J].Journal of Analytical Chemistry,2004(11):1097-1101. |
| [13] | Huszal S;Kowalska J;Krzeminska M;Golimowski J .Determination of platinum with thiosemicarbazide by catalytic adsorptive stripping voltammetry (AdSV)[J].Electroanalysis,2005(4):299-304. |
| [14] | Matti Niemela;Harri Kola;Paavo Peramaki;Juha Piispanen;Jarmo Poikolainen .Comparison of Microwave-Assisted Digestion Methods and Selection of Internal Standards for the Determination of Rh,Pd and Pt in Dust Samples by ICP-MS[J].Mikrochimica Acta: An International Journal for Physical and Chemical Methods of Analysis,2005(3/4):211-217. |
| [15] | Yinhai MA;Yongfang PENG;Liya ZHU et al.Solid phase extraction and spectrophotometric determination of gold with 5-(2-hydroxy-4-nitrophenylazo)-rhodanine as chromoqenic reagent[J].South African Journal of Chemistry,2005,58:116-119. |
| [16] | Lin H;Huang ZJ;Hu Q;Yang G;Zhang G .Determination of palladium, platinum, and rhodium by HPLC with online column enrichment using 4-carboxylphenyl-thiorhodanine as a precolumn derivatization reagent[J].Journal of analytical chemistry,2007(1):58-62. |
| [17] | HAITAO LIN;ZHU LIYA;ZHANGJIE HUANG .Studies on the Solid Phase Extraction and Spectrophotometric Determination of Palladium with 2-(2-Quinolylazo)-5-Dimethylaminoaniline as Chromogenic Reagent[J].Asian Journal of Chemistry: An International Quarterly Research Journal of Chemistry,2007(2):836-842. |
| [18] | 朱利亚,赵泽松,陶赛祥,谢宏潮,陈海云,金娅秋.难溶金锆系列合金的微波消解及锆的滴定[J].贵金属,2006(03):35-39,53. |
| [19] | 朱利亚,郑恩华,马媛,安中庆.微波密闭消解与几种分解测定难处理KAu（CN）2中Au的方法比较[J].贵金属,2004(03):39-44. |
| [20] | 朱利亚,杨光宇,刘云,胡秋芬,赵辉,尹海川.微波消解技术在难溶贵金属（铂）化合物分析中的应用[J].分析科学学报,2005(06):627-629. |
| [21] | Shouan DONG;Wei FANG;Liya ZHU.Modern Precious Metals Analysis[M].北京:化学工业出版社,2006 |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%