1-(2-吡啶偶氮)-2-萘酚光度法测定钒钛磁铁矿中痕量镓  

Determination of trace gallium in vanadium titano-magnetite by1-(2-pyridylazo)-2-naphthol spectrophotometry

作　　者：吴琳[1] 朱霞萍[1] 郝星杰 蓝路梅[1] 

机构地区：[1]成都理工大学材料与化学化工学院,四川省矿产资源化学高校重点实验室,四川成都610059

出　　处：《冶金分析》2015年第6期61-64,共4页Metallurgical Analysis

基　　金：四川省教育厅科研项目(15ZA0071))

摘　　要：利用1-（2-吡啶偶氮）-2-萘酚（PAN）与镓反应生成红色络合物的特性,建立了光度法测定钒钛磁铁矿中镓的方法。实验表明：于25mL比色管中,依次加入2.0mL KHP-HCl缓冲溶液（pH 3.2）、4.0mL 0.5g/L PAN溶液、3.0mL 95%乙醇,用水定容后反应10min,用1cm比色皿,于545nm处采用分光光度法进行测定,镓（Ⅲ）的质量浓度在0.05-3μg/mL范围内符合比尔定律,方法检出限为0.033μg/mL,表观摩尔吸收系数ε=3.0×10^4 L·mol^-1·cm^-1。将GBW 07226a钒钛磁铁矿精矿一号和GBW 07224钒钛磁铁矿原矿一号样品经氢氧化钠和过氧化钠碱熔、水浸取、过滤、酸化还原铁等步骤后,采用乙酸丁酯萃取、水反萃取,使镓与大量基体元素分离,再采用方法对样品中痕量镓进行测定,结果与认定值一致,相对标准偏差（RSD,n=3）小于15%。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.2.0mL of potassium hydrogen phthalate-hydrochloric acid buffer solution at pH 3.2,4.0mL of 0.5g/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 1cm cuvette.The results indicated that the Beer＇s law was obeyed for the mass concentration of gallium （Ⅲ）in range of 0.05-3μg/mL.The detection limit of method was 0.033μg/mL.The apparent molar absorptivity wasε=3.0×10^4 L·mol^-1·cm^-1.After GBW 07226 avanadium titanomagnetite 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 gallium in 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%.

关 键 词：镓 钒钛磁铁矿 1-(2-吡啶偶氮)-2-萘酚(PAN) 光度法 碱熔 

分 类 号：TG115[金属学及工艺—物理冶金] TF041[金属学及工艺—金属学]