Determination of trace cobalt in water by laser thermal lens spectrometry after cloud point extraction using 2-(5-bromo- 2-pyridylazo)-5-dimethylaminoaniline as chelating agent
HAN Quan1,2, HUO Yan-yan1, YANG Xiao-hui1, YANG Na1
1. Department of Chemistry, Xi'an University, Xi'an 710065, China; 2. School of Chemistry and Materials Science, Shaanxi Normal University, Xi'an 710062, China
Abstract:Cobalt is an essential trace element for living species, so the establishment of determination method for cobalt in water sample is of great importance. In the buffer medium of HAc-NaAc at pH 5.0, the chelating agent 2-(5-bromo-2-pyridylazo)-5-dimethylaminoaniline (5-Br-PADMA) could react with Co(II) to form a hydrophobic chelate Co(II)-5-Br-PADMA with coordination ratio of 2∶1 after heating in water bath at 60℃ for 10 min. Maximum absorption wavelength was 611nm. The nonionic surfactant Triton X-114 was selected as extraction agent for cloud point extraction (CPE). The generated hydrophobic chelate could be extracted into surfactantmicelle phase. After phase separation, the micelle phase was dissolved with 0.45mL of 2mol/L HCl-ethanol solution, which was then transferred into a self-made quartz cell with optical path of 5mm. He-Ne laser (single model, λ=632.8nm) was employed both as exciting and probing beam for the thermal lens spectrometry (TLS). Consequently, a new determination method of ultra-trace cobalt by CPE-TLS was established. Under the optimized conditions, the TLS signal intensity of Co(II) had good linear relationship with the corresponding mass concentration in range of 0.40-6.0ng/mL. The correlation coefficient was 0.9978. The limit of detection was 0.05ng/mL. Based on the volume ratio of solution before and after enrichment, the enrichment factor was calculated, i.e., 22. The proposed method was applied for the determination of cobalt content in lake water and thermal spring water. The relative standard deviations (RSD, n=6) of determination results were less than 4%. The found results were consistent with those obtained by inductively coupled plasma mass spectrometry (ICP-MS). The spiked recoveries were between 96% and 101%.
韩权, 霍燕燕, 杨晓慧, 杨娜. 以2-(5-溴-2-吡啶偶氮)-5-二甲氨基苯胺作螯合剂浊点萃取-激光热透镜光谱法测定水中痕量钴[J]. 冶金分析, 2020, 40(5): 20-25.
HAN Quan, HUO Yan-yan, YANG Xiao-hui, YANG Na. Determination of trace cobalt in water by laser thermal lens spectrometry after cloud point extraction using 2-(5-bromo- 2-pyridylazo)-5-dimethylaminoaniline as chelating agent. , 2020, 40(5): 20-25.
Barceloux D G.Cobalt[J].J.Toxicol.Clin.Toxicol.,1999,37:201-206.
[2]
Vega M,Ven den Berg CMG.Determination of cobalt in seawater by catalytic adsorptive cathodic stripping voltammetry[J].Anal.Chem.,1997,69:874-881.
[3]
Benkhedda K,Infante H G,Ivanova E,et al.Electrothermal atomic absorption spectrometric determinationof cobalt in biological samples and natural waters using a flow injection system with on-line preconcentration by ion-pair adsorption in a knotted reactor[J].Fresenius.J.Anal.Chem.,2000,368:288-292.
[4]
Ranjbar L,Yamini Y,Saleh A,et al.Ionic liquid based dispersive liquid-liquid microextraction combined with ICP-OES for the determination of trace quantities of cobalt,copper,manganese,nickel and zinc in environmental water samples[J].Microchimica Acta,2012,177(1-2):119-127.
[5]
Chen S,Liu C,Yang M,et al.Solid-phase extraction of Cu,Co and Pb on oxidized single-walled carbon nanotubes and their determination by inductively coupled plasma mass spectrometry[J].J.Hazard. Mater.,2009,170(1):247-251.
[6]
Subramanian S,Woittiez J R W.Determination of cobalt in biological samples by radiochemical neutron activation analysis employing reversed-phase chromatography[J].Biol.Trace Elem.Res.,1994,43-45(1):117-124.
[7]
Dovichi N J.Thermo-optical spectrophotometries in analytical chemistry[J].Crit.Rev.Anal.Chem.,1987,17:357-423.
[8]
Ramis Ramos G.Analytical characteristics,applications and perspectives in thermal lens spectrometry[J].Anal.Chim.Acta,1993,283(1):623-634.
[9]
韩权,阎宏涛.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.
[10]
孙梅,刘桂建,吴强华.浊点萃取技术在环境样品痕量元素分析中的应用研究进展[J].环境化学,2013,32(6):1016-1024.SUI Mei,LIU Gui-jian,WU Qiang-hua.Progress and application of cloud point extraction in the analysis of trace elements in environmental samples[J].Environmental Chemistry,2013,32(6):1016-1024.
[11]
杜军良,杨双,胡杨,等.浊点萃取-火焰原子吸收光谱法测定人尿液中的痕量铅[J].化学研究与应用,2014,26(3):445-450.DU Jun-liang,YANG Shuang,HU Yang,et al.Cloud point extraction and flame atomic absorption spectrometry determination fo trace lead in urine[J].Chemical Research and Application,2014,26(3):445-450.
[12]
谢发之,张峰君,宣寒,等.正辛醇诱导低温浊点萃取-火焰原子吸收法测定环境样品中痕量铟[J].分析试验室,2014,33(3):273-276.XIE Fa-zhi,ZHANG Feng-jun,XUAN Han,et al.Determination of trace indium from environmental samples by flame atomic absorption spectrometry with actonol-induced cloud point extraction[J].Chinese Journal of Analysis Laboratory,2014,33(3):273-276.
[13]
王梅,龙军标,杨冰仪,等.水样中痕量汞的浊点萃取-分光光度法测定[J].分析科学学报,2013,29(6):870-872.WANG Mei,LONG Jun-biao,YANG Bing-yi,et al.Spectrophotometric determination of trace mercury in water after cloud point extraction[J].Journal of Analytical Science,2013,29(6):870-872.
[14]
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,2013,32(4):67-69.YANG Long-hu,HAN Quan,HUO Yan-yan.Determination of trace amounts of palladium by graphite furnace atomic absorption spectrometry after cloud point extraction[J].Chinese Journal of Analysis Laboratory,2013,32(4):67-69.
[15]
王慧丽,张加玲.浊点萃取-氢化物发生原子荧光光谱法测定水样中痕量铋[J].冶金分析,2010,30(9):54-58.WANG Hui-li,ZHANG Jia-ling.Determination of trace bismuth in water samples by hydride generation-atomic fluorescence spectrometry after cloud point extraction[J].Metallurgical Analysis,2010,30(9):54-58.
[16]
韩权,郝甜甜,霍燕燕,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微量钯[J].分析试验室,2014,33(5):574-577.HAN Quan,HAO Tian-tian,HUO Yan-yan,et al.Determination of palladium by laser thermal lens spectrometry using 2-(5-bromo-2-pyridylazo)-5-dimethylaminoaniline[J].Chinese Journal of Analysis Laboratory,2014,33(5):574-577.
[17]
朱贵云,杨景和.激光光谱分析法[M].北京:科学出版社,1989:132-171.
[18]
张光,韩权,胡炎荣,等.2-(5-溴-2-吡啶偶氮)-5-二甲氨基苯胺合成及其与钴反应的吸光光度研究[J].理化检验:化学分册,1990,26(4):219-220.ZHANG Guang,HAN Quan,HU Yan-rong,et al.Synthesis of 2-(5-bromo-2-pyridylazo)-5-dimethylaminoaniline and its color reaction with cobalt[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,1990,26(4):219-220.
[19]
贺忠翔,郝峰,仝青.电感耦合等离子体质谱法同时测定地下水中钴和钼[J].中国环境监测,2012,28(2):23-25.HE Zhong-xiang,HAO Feng,TONG Qing.Determination of mental elements (cobalt and molybdenum) in underground water by inductively coupled plasma mass spectrometry[J].Environmental Monitoring in China,2012,28(2):23-25.