Determination of palladium in ore by laser thermal lens spectrometry with 2-(5-nirtro-4-methyl-2-pyridylazo)-5-dimethylaminoaniline
HAN Quan1,2, CHEN Hong2, HUO Yan-yan1, YANG Xiao-hui1, HE Ya-ping1, ZHAI Yun-hui1
1. School of Chemical Engineering, Xi′an University, Xi′an 710065, China; 2. School of Chemistry and Chemical Engineering, Yanan University, Yanan 716000, China
Abstract：The laser thermal lens effect of the complex formed by palladium (II) and 2-(5-nitro-4-methyl-2-pyridylazo)-5-dimethylaminoaniline (5-NO2-4-Me-PADMA) was observed with He-Ne laser. The experiment results showed that 5-NO2-4-Me-PADMA could react with Pd (II) in 1.8mol/L H2SO4 medium in presence of 50% acetone (volume fraction, the aim was to enhance the intensity of thermal lens signal) to form a green-blue complex, which exhibited a maximum absorption peak at 623nm. It was closed to the output wavelength (i.e., 632.8nm) of He-Ne laser. Based on these experiments, a new method for determination of trace palladium by laser thermal lens spectrometry (TLS) was established. The results indicated that the intensity of thermal lens signal was linear to the mass concentration of Pd (II) in range of 5-250ng/mL with correlation coefficient of 0.9989. The detection limit of method was 1.5ng/mL. The proposed method had high sensitivity and good selectivity. The determination of palladium was not interfered by the common metal ions such as Fe3+, Co2+ and Cu2+ (800-fold), Ni2+ (500-fold), Pt (IV) (25-fold), and precious metal ions such as Au (III), Rh (III), Ru (III) and Os (VIII) (10-fold) and Ir (III) (5-fold). The content of trace palladium in ore was determined according to the experimental method, and the found results were basically consistent with those obtained by flame atomic absorption spectrometry (FAAS). The relative standard deviations (RSD, n=6) were between 0.57% and 1.3%
韩权, 陈虹, 霍燕燕, 杨晓慧, 何亚萍, 翟云会. 2-(5-硝基-4-甲基-2-吡啶偶氮)-5-二甲氨基苯胺激光热透镜光谱法测定矿石中钯[J]. 冶金分析, 2019, 39(6): 65-69.
HAN Quan, CHEN Hong, HUO Yan-yan, YANG Xiao-hui, HE Ya-ping, ZHAI Yun-hui. Determination of palladium in ore by laser thermal lens spectrometry with 2-(5-nirtro-4-methyl-2-pyridylazo)-5-dimethylaminoaniline. , 2019, 39(6): 65-69.
YANG H Q,ZHANG G,ZHANG L L,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.
[2]
HAN Quan,HUO Yan-yan,WU Jiang-yan,et al.Determination of ultra-trace rhodium in water samples by graphite furnace atomic absorption spectrometry after cloud point extraction using 2-(5-iodo-2-pyridylazo)-5-dimethylaminoaniline as a chelating agent[J].Molecules,2017,22,487-495.
[3]
霍燕燕,杜宇凤,韩权,等.双波长叠加5-(5-磺酸-2-吡啶偶氮)-2,4-二氨基甲苯光度法测定钯(II)[J].冶金分析,2017,37(9):76-80.HUO Yan-yan,DU Yu-feng,HAN Quan,et al.Determination of palladium by dual-wavelength overlapping spectrophotometry with 5-(5-sulfonic-2-pyridylazo-2,4-diaminotoluene[J].Metallurgical Analysis,2017,37(9):76-80.
[4]
郝甜甜,韩权,霍燕燕,等.5-(5-氰基-2-吡啶偶氮)-2,4-二氨基甲苯的合成及其与钯的显色反应[J].冶金分析,2015,35(2):18-22.HAO Tian-tian,HAN Quan,HUO Yan-yan,et al.Synthesis of 5-(5-cyano-2-pyridylazo)-2,4-diaminotoluene and its color reaction with palladium[J].Metallurgical Analysis,2015,35(2):18-22.
[5]
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(II)[J].分析科学学报,2012,28(4):507-510.HAN Quan,HUO Yan-yan,YANG Long-hu,et al.Highly selective spectrophotometric determination of trace palladium using a new reagent 5-(5-iodine-2-pyridylazo)-2,4-diaminotoluene[J].Journal of Analytical Science,2012,28(4):507-510.
[6]
杨晓慧,韩权,李海维.4-(5-硝基-2-吡啶偶氮)-1,3-二氨基苯光度法同时测定钴和钯[J].岩矿测试,2008,27(2):113-116.YANG Xiao-hui,HAN Quan,LI Hai-wei.Simultaneous determination of cobalt and palladium by spectrophotometry with 4-(5-nitro-2pyridylazo)-1,3-diaminobenzene[J].Rock and Mineral Analysis,2008,27(2):113-116.
[7]
杨晓慧,陈虹,霍燕燕,等.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的研究[J].冶金分析,2014,34(8):50-53.YANG Xiao-hui,CHEN Hong,HUO Yan-yan,et al.Spectrophotometric determination of micro palladium (II) using a new reagent 2-(5-nitro-4-methyl-2-pyridylazo)-5-dimethylaminoaniline[J].Metallurgical Analysis,2014,34(8):50-53.
[8]
韩权,闫宏涛.激光热透镜光谱分析法[J].化学进展,2002,14(1):24-31.HAN Quan,YAN Hong-tao.Laser thermal lens spectrometry[J].Progress in Chemistry,2002,14(1):24-31.
[9]
韩权,霍燕燕,孙丽娟,等.2-( 5-溴-2-吡啶偶氮)-5-二甲氨基苯胺激光热透镜光谱法测定痕量铑的研究[J].分析测试学报,2013,32(8):988-992.HAN Quan,HUO Yan-yan,SUN Li-juan,et al.Study on determination of rhodium by laser thermal lens spectrometry using 2-(5-bromo-2-pyridylazo)-5-dimethylaminoaniline[J].Journal of Instrumental Analysis,2013,32(8):988-992.
[10]
HAN Q,HUO Y Y,YANG X H,et al.Determination of ultra-trace cobalt in water and wheat flour samples using cloud point extraction coupled with laser thermal lens spectrometry[J].Anal.Methods,2018,10:634-640.
[11]
Ramis-Ramos G.Analytical characteristics,applications and perspectives in thermal lens spectrometry[J].Anal.Chim.Acta.,1993,283:623-634.
[12]
Arnaud N,Georges J.Cw-laser thermal lens spectrometry in binary mixtures of water and organic solvents:composition dependence of the steady-state and time-resolved signals[J].Spectrochimica Acta Part A,2004,60:1817-1823.
[13]
Proskurnin M A,Bendrysheva S N,Kuznetsova V V,et al.Criteria for assessing the effect of the composition of mixed media on analytical sensitivity in thermal lens spectrometry[J].Journal of Analytical Chemistry,2008,63(12):1168-1175.
