Abstract:The coloring reaction between 2-(5-iodine-2-pyridineazo)-5-dimethylaniline (5-I-PADMA) and palladium(Ⅱ) was investigated. The experimental results showed that, 5-I-PADMA could react with palladium(Ⅱ) to form blue stable complex with molar ratio of 1∶1 in 0.6 mol/L perchloric acid medium. The maximum absorption peak of this complex was at 613 nm. Beer’s law was obeyed for palladium(Ⅱ) concentration in the range of 0-0.6 μg/mL. Linear regression equation was △A=0.828 4 ρ(μg/mL)- 0.001 6 with correlation coefficient of 0.999 9 and apparent molar absorptivity of 8.82 × 104 L·mol-1·cm-1. The proposed method was applied to the determination of trace palladium in palladium molecular sieve and ore samples. The results were in accordance with those obtained by atomic absorption spectrometry, and the relative standard deviations(n=6)were 1.2%-1.4% .
杨晓慧, 霍燕燕, 王转莉, 韩权, 郑卫. 2-(5-碘-2-吡啶偶氮)-5-二甲氨基苯胺与钯显色反应的研究及其应用[J]. 冶金分析, 2013, 33(6): 47-51.
YANG Xiao-hui, HUO Yan-yan, WANG Zhuan-li, HAN Quan, ZHENG Wei. Color reaction of 2-(5-iodine-2-pyridylazo)-5-dimethylaniline with palladium and its application. , 2013, 33(6): 47-51.
Polak J, Mestek O, Suchanek M. Uncertainty of determination of palladium in road dust sample by inductively coupled plasma mass spectrometry[J]. Accreditation Quality Assurance, 2006, 10(6): 627-632.
[2]
Hassanien M M. FAAS determination of palladium after its selective recovery by silica modified with hydrazone derivative[J]. Microchimica Acta, 2009, 167: 81-89.
[3]
Ohta K, Ogawa J, Mizuno T. Determination of palladium by a new preconcentration method (Mg-W cell)-electrothermal atomic absorption spectrometry[J]. Fresenius Journal of Analytical Chemistry, 1997, 357(7): 995-997.
[4]
Schwarzer M, Schuster M, Hentig R V. Determination of palladium in gasoline by neutron activation analysis and automated column extraction[J]. Fresenius Journal of Analytical Chemistry, 2000, 368(2-3): 240-243.
[5]
Galtsev P A, Iokhin B S,Levunin S L,et al. X-ray fluorescence determination of palladium and other fission products in solutions used for reprocessing of spent nuclear fuel[J]. Atomic Energy, 1990, 69(2) : 692-693.
[6]
汪振辉,刘建允,董文举,等. 水杨醛肟修饰碳糊电极吸附溶出伏安法测定钯(Ⅱ)的研究[J].分析试验室(Chinese Journal of Analysis Laboratory),2000,19(4): 40-43.
[7]
Lin H, Huang Z J,Hu Q,et al. 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, 62(1): 58-62.
[8]
Bilba D, Paduraru C, Tofan L. Determination of trace amounts of palladium(Ⅱ) by solid-phase spectrophoto metry[J]. Microchimica Acta, 2004, 144(1-3): 97-101.
[9]
Mousavi M F, Rahmani A, Barzegar M, et al. A sensitive catalytic-photometric method for the determination of trace amounts of palladium(Ⅱ) by using a computerized probe-type photometer[J]. Journal of Analytical Chemistry, 2004, 59(1): 71-74.
[10]
Gureva P F, Savvin S B. Specrophotometric methods for determining noble metals [J]. Journal of Analytical Chemisty, 2002, 57(11): 980-996.
[11]
宾高远,曹秋娥,李崇宁,等. 1-(4-氨替比林)-3-(2-噻唑)-三氮烯的合成及其光度法测定钯(Ⅱ)[J]. 分析 试验室(Chinese Journal of Analysis Laboratory),2006,25(5): 19-22.
韩权,杨晓慧,吴启勋. 2-(3,5-二氯-2-吡啶偶氮)-5-二甲氨基苯胺与钯显色反应的研究[J]. 分析试验室(Chinese Journal of Analysis Laboratory),1992,11(5): 34-35.
[18]
韩权,张光,胡炎荣,等.2-(5-溴-2-吡啶偶氮)-5-二甲氨基苯胺与钯显色反应的研究[J].分析化学(Chinese Journal of Analytical Chemistry),1991,19(2): 214-216.
[19]
朱有瑜,俞彩娟.5-[(5-溴-2-吡啶)-偶氮]-2,4-二氨基甲苯分光光度法测定微量钯的研究[J]. 分析化学(Chinese Journal of Analytical Chemistry),1994,22(2):210.
[20]
Yang Heqing, Zhang Guang, Zhang Linlin, et al. Synthesis of 5-(5-nitro-2-pyridylazo)-2, 4-diaminotoluene and its application to spectrophotometric determination of microamounts of palladium[J]. Talanta, 1996, 43(5): 747-753.
[21]
杨晓慧,韩权,刘阿敏,等. 新显色剂4-(5-硝基-2-吡啶偶氮)-1,3-二氨基苯的合成及其与钯显色反应的研究[J]. 分析试验室(Chinese Journal of Analysis Laboratory),2008,27(10): 99-10.
[22]
韩权,霍燕燕,刘渊,等. 2-(5-碘-2-吡啶偶氮)-5-二甲氨基苯胺的合成及其与铑(Ⅲ)的高灵敏显色反应的研究[J]. 分析测试学报(Journal of Instrumental Analysis),2010,29(8): 797-801.