Abstract：Trace palladium (Ⅱ) could inhibit the fading of methyl orange oxidized by potassium bromate. On basis of this, a new determination method of trace palladium by inhibition kinetic spectrophotometry was established. The optimum determination conditions were obtained as follows:0.9 mL of 1.0 mol/L sulfuric acid,2.0 mL of 0.01 mol/L potassium bromate solution and 1.1 mL of 0.25 g/L methyl orange solution were added into a colorimeter tube; after heating in water bath at 75 ℃ for 19 min, the absorbance difference (ΔA) between inhibitory reaction and non-inhibitory reaction was measured at 505 nm. The results showed that ΔA exhibited good linearity to the mass concentration of palladium in range of 6-30 ng/mL. The apparent rate constant was k =7.65×10-4/s, the apparent activation energy was Ea=400.46 kJ/mol, and the detection limit of method was 3.36×10-10 g/mL. The proposed method could be applied to the determination of trace palladium (Ⅱ) in dust. The relative standard deviation (RSD, n=6) was 3.9%-4.1%. The found results were basically consistent with those obtained by national standard method (GB/T 17418.3-2010 Graphite furnace atomic absorption spectrometry after enrichment with thiourea).
黄珍玉,张勤,胡克,等.等离子体质谱法直接测定地球化学样品中金铂钯[J].岩矿测试,2001,20(1):15-18.HUANG Zhen-yu,ZHANG Qin,HU Ke,et al.Direct determination of gold,platinum,palladium in geochemical smples by ICP-MS[J].Rock and Mineral Analysis,2001,20(1):15-18.
[2]
司云森,胡秋芬,朱利亚,等.高效液相色谱法测定汽车尾气催化剂中铂、钯和铑的研究[J].理化检验:化学分册,2005,41(3):162-164.SI Yun-sen,HU Qiu-fen,ZHU Li-ya,et al.HPLC determination of Pt Pd and Rh in catalyst for automobile tailgas[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2005,41(3):162-164.
[3]
羊波,刘飞,李银科,等.固相萃取富集-火焰原子吸收光谱法测定钯[J].光谱实验室,2012,29(3):1318-1321. YANG Bo,LIU Fei,LI Yin-ke,et al.Determination of palladium by flame atomic absorptionspectrometry with solid phase extraction[J].Chinese Journal of Spectroscopy Laboratory,2012,29(3):1318-1321.
[4]
刘先国,方金东.活性炭吸附-电感耦合等离子体发射光谱法测定化探样品中痕量金铂钯[J].贵金属,2002,23(1):33-35.LIU Xian-guo,FANG Jin-dong.Determination of Au,Pt and Pd in geological samples by inductively coupled plasma-atomic emission spectrometry after preconcentration using active carbon[J].Precious Metals,2002,23(1): 33-35.
[5]
韩权,郝甜甜,霍燕燕,等.5-(5-碘-2-吡啶偶氮)-2,4-二氨基甲苯双波长叠加分光光度法同时测定钴和钯[J].冶金分析,2015, 35(3):64-68. HAN Quan,HAO Tian-tian,HUO Yan-yan,et al.Simultaneous determination of cobalt and palladium by 5-(5-iodine-2-pyridylazo)-2,4-diaminotoluene dual wavelength overlapping spectrophotometry[J].Metallurgical Analysis,2015,35(3):64-68.
[6]
王烨,孙爱琴,李志伟.巯基棉富集-分光光度法测定地球化学样品中铂钯的野外快速分析方法研究[J].岩矿测试,2015,34(4):459-463.WANG Ye,SUN Ai-qin,LI Zhi-wei.Field rapid determination of platinum and palladium in geochemical samples by spectrophotometry with sulfhydryl cotton enrichment[J].Rock and Mineral Analysis,2015,34(4):459-463.
李祖碧,曹秋娥,徐其亨,等.丁基罗丹明B-高碘酸钾动力学光度法测定铑[J].分析化学,1999,27(2):198-201.LI Zu-bi,CAO Qiu-e,XU Qi-heng,et al.Kinetic-spectrophotometric determination of rhodium based on its catalytic effect on the betylrhodamine B-Potassium periodate reaction[J].Chinese Journal of Analytical Chemistry,1999,27(2):198-201.
[9]
王洪福,罗娅君,陈忠萍.催化动力学光度法测定痕量钯[J].四川师范大学学报:自然科学版,2007,30(4):516-518.WANG Hong-fu,LUO Ya-jun,CHEN Zhong-ping.Determination of trace palladium(Ⅱ) by catalytic kinetic spectrophotometry[J].Journal of Sichuan Normal University:Natural Science,2007,30(4):516-518.
[10]
周之荣,彭道锋.溴酸钾氧化偶氮胂Ⅲ动力学光度法测定钯[J].分析试验室,2001,20(4):9-11.ZHOU Zhi-rong,PENG Dao-feng.Kinetic spectrophotometric detetmination of trace palladium based on its catalysis for discoloring reaction of arsenzo Ⅲ with potassium bromate[J].Chaiese Journal of Analysis Laboratory,2001,20(4):9-11.
