Abstract：The chromogenic reaction between a newly-synthetic reagent, 2-(5-nitro-4-methyl-2-pyridylazo)-5-dimethylaminoaniline (5-NO2-4-CH3-PADMA) and palladium(Ⅱ) was studied. In 0.6-2.4 mol/L H2SO4 medium, palladium(Ⅱ) reacted with 5-NO2-4-CH3-PADMA to form a green-blue complex (1∶1) whose the maximum absorption wavelength located at 621 nm. The apparent molar absorptivity was 6.05×104 L·mol-1·cm-1. Beer’s law was obeyed in the range of 0-3.2 μg/mL for palladium. Because the chromogenic reaction was conducted in strong acidic medium where other metal ions seldom developed color, the determination of palladium showed a high selectivity. Common metal ions as well as Rh(Ⅲ) in 100 times, Pt(Ⅳ) in 25 times, Ru(Ⅲ) in 20 times, Ag in 10 times, Os(Ⅲ) in 7.5 times , and Ir(Ⅲ) in 5 times did not interfere in the determination. This method was simple and rapid. It was used in the determination of micro palladium in catalyst and ores with satisfactory results.
杨晓慧, 陈虹, 霍燕燕, 韩权. 2-(5-硝基-4-甲基-2-吡啶偶氮)-5-二甲氨基苯胺分光光度法测定微量钯(Ⅱ)的研究[J]. 冶金分析, 2014, 34(8): 50-53.
YANG Xiao-hui, CHEN Hong, HUO Yan-yan, HAN Quan. Spectrophotometric determination ot micro palladium(Ⅱ) using a new reagent 2-(5-nitro-4-methyl-2-pyridylazo)-5-dimethylaminoaniline. , 2014, 34(8): 50-53.
韩权,霍燕燕,杨龙虎,等. 新试剂5-(5-碘-2-吡啶偶氮)-2,4-二氨基甲苯高选择性分光光度法测定微量Pd [J]. 分析科学学报(Journal of Analytical Science),2012,28(4):507-510.
[2]
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):99-101.
[3]
Hassanien M M. FAAS determination of palladium after its selective recovery by silica modified with hydrazone derivative[J]. Microchim. Acta, 2009, 167(1/2): 81-89.
[4]
杨龙虎,韩权,霍燕燕,等.浊点萃取-石墨炉原子吸收光谱法测定痕量钯[J].分析试验室(Chinese Journal of Analysis Laboratory),2013,32(4):67-69.
[5]
Kovacheva P, Djingova R. Ion-exchange method for separation and concentration of platinum and palladium for analysis of environmental samples by inductively coupled plasma atomic emission spectrometry[J]. Anal. Chim. Acta, 2002,464(1): 7-13.
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.
[8]
Schwarzer M, Schuster M, Hentig R V. Determination of palladium in gasoline by neutron activation analysis and automated column extraction[J]. Fresenius' J Anal. Chem., 2000, 368(2-3): 240-243.
[9]
Messerschmidt J, Bohlen A V, Alt F, et al. Separation and enrichment of palladium and gold in biological and environmental samples, adapted to the determination by total reflection X-ray fluorescence[J]. Analyst, 2000,125(3):397-399.
[10]
Gureva P F, Savvin S B. Specrophotometric methods for determining noble metals [J]. Journal of Analytical Chemisty,2002,57(11):980-996.
