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1 引言对复杂的分析体系,不经分离而直接迸行多组分的连续测定一直是分析化学中的一个重要研究课题.本文基于铜、钴和钯与5-(5-硝基-2-吡啶偶氮)-2,4二氨基甲苯(5-NO_2PADAT)显色酸度和络合物稳定性的差异,成功地实现了铜、钴和钯的连续测定.经对实际样品的分析,获得满意结果.2 实验部分2.1 仪器和试剂 岛津UV-260分光光度计;铜、钴、钯标准溶液浓度分别为10mg/L、4mg/L和10mg/L;5-NO_2-PADT乙醇溶液:1.0x10_(-3)mol/L;pH=5.2的HAc-NaAc缓冲溶液.所用试剂均为分析纯.2.2 实验方法 (1)铜的测定 于两只10mL比色管中分别加入同样比例的铜、钴、钯标准溶液,2mL缓冲溶液,1.0mL5-NO_2-PADAT溶液,摇匀,再加入1mLO.5%盐酸羟胺溶液、3mL95%乙醇溶液,于其中一只中再加入1mL0.01mol/LEDATA溶液.以水稀释至刻度,摇匀,放置10min分别用1cm比色皿于519nm处以试剂空白作参比测其吸光度A_1和A_2,A_1与A_2之差为铜的吸光度.(2)钴、钯的测定 于两只10mL比色管中分
1 Introduction For complex analytical systems, continuous determination of multicomponent without separation has been an important research topic in analytical chemistry.Based on the combination of copper, cobalt and palladium with 5- (5-nitro-2- Pyridine, azo) -2,4-diaminotoluene (5-NO_2PADAT), the continuous determination of copper, cobalt and palladium was successfully achieved.After the analysis of the actual samples, it was satisfied Results2 Experimental 2.1 Instruments and reagents Shimadzu UV-260 spectrophotometer; copper, cobalt, palladium standard solution concentrations were 10mg / L, 4mg / L and 10mg / L; 5-NO_2-PADT ethanol solution: 1.0x10_ (-3) mol / L, pH = 5.2 HAc-NaAc buffer solution. All reagents were of analytical grade.2.2 Experimental methods (1) Determination of copper Two 10mL colorimetric tube were added the same proportion of copper, cobalt , Palladium standard solution, 2mL buffer solution, 1.0mL5-NO_2-PADAT solution, shake, then add 1mLO.5% hydroxylamine hydrochloride solution, 3mL95% ethanol solution, in which one was added 1mL0.01mol / LEDATA solution to Water diluted to the mark, shake, place 10min respectively 1cm cuvette at 519nm reagent blank as a reference to measure the absorbance A_1 and A_2, A_1 and A_2 of the difference between copper Of absorbance. (2) cobalt, palladium determination in two 10mL colorimetric tube points