Determination of trace gallium in vanadium titano-magnetite by 1-(2-pyridylazo)-2-naphthol spectrophotometry
WU Lin, ZHU Xia-ping*, HAO Xing-jie, LAN Lu-mei
College of Materials & Chemistry & Chemical Engineering, Chengdu University of Technology, Mineral Resources Chemistry Key Laboratory of Sichuan Higher Education Institutions, Chengdu 610059, China
Abstract：Based on 1-(2-pyridylazo)-2-naphthol (PAN) could react with gallium to form red complex, a determination method of gallium in vanadium titano-magnetite by spectrophotometry was established. 2.0 mL of potassium hydrogen phthalate-hydrochloric acid buffer solution at pH 3.2, 4.0 mL of 0.5 g/L PAN solution and 3.0 mL of 95% ethanol was added into 25 mL colorimetric tube successively. The solution was diluted to the mark with water. After reaction for 10 min, the solution was determined by spectrophotometry at 545 nm with 1 cm cuvette. The results indicated that the Beer’s law was obeyed for the mass concentration of gallium in range of 0.05-3 μg/mL. The detection limit of method was 0.033 μg/mL. The apparent molar absorptivity was ε=3.0×104 L·mol-1·cm-1.AfterGBW 07226a vanadium titano-magnetite concentrate No.1# and GBW 07224 vanadium titano-magnetite original ore No.1#were treated by alkali fusion with sodium hydroxide and sodium peroxide, water leaching, filtration, acidification and reduction of iron,gallium was separated from matrix elements by butyl acetate extraction and water back extraction. Then,the contents of trace galliumin the two samples were determined by this proposed method. The results were consistent with the certified values. The relative standard deviation (RSD, n=3) was less than 15%.
赵宇侠, 许兴友, 马卫兴. 微乳液介质-4-(6-甲氧基-8-喹啉偶氮)-间苯三酚分光光度法测定痕量镓[J]. 理化检验:化学分册(Physical Testing and Chemical Analysis Part B:Chemical Analysis), 2009, 45(4): 410-412.
Anthemidis A N, Zachariadis G A, Stratis J A. Gallium trace on-line preconcentration/separation and determination using a polyurethane foam mini-column and flame atomic absorption spectrometry: Application in aluminum alloys, natural waters and urine[J]. Talanta, 2003,60(5): 929-936.
Piech R. Novel sensitive voltammetric detection of trace gallium with presence of catechol using mercury film silver based electrode[J]. Electroanalysis, 2009, 21(16):1842-1847.
[9]
彭敬东, 刘绍璞, 邓传跃. 以TAN反相高效液相色谱法分离测定镓、锇、钒、铜 [J]. 西南师范大学学报(Journal of Southwest China Normal University), 1998, 23(2): 181-184.
