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机构地区:[1]昆明理工大学真空冶金国家工程实验室,云南昆明650093 [2]昆明冶金研究院,云南昆明650031
出 处:《冶金分析》2013年第8期64-67,共4页Metallurgical Analysis
摘 要:建立了以甲苯-甲基异丁基酮为萃取剂、罗丹明B为显色剂分光光度法测定黄磷电尘灰冶炼物料中镓的方法。试样采用体积分数10%硫酸溶解后,加入三氯化钛还原铁至二价,在6mol/L盐酸中用甲苯-甲基异丁基酮萃取罗丹明B与镓生成络合物,有机相经硫脲、三氯化钛和罗丹明B溶液洗涤后,在最大吸收波长560nm测定吸光度,同时采用校正法消除样品分解带来的方法系统误差。镓的质量浓度在0~1.0μg/mL时,吸光度与浓度呈线性关系,相关系数为0.999。将实验方法与传统溶样方法的测定值进行对照,结果一致。对6个黄磷电尘灰冶炼物料样品中镓进行测定,结果的相对标准偏差小于10%,加标回收率在96%~103%之间。A extraction spectrophotometry was established for the determination of gallium in smelting materials of yellow phosphorus electric dust using rhodamine B as chromogenic agent and toluene-MI- BK as extraction agent. The sample was dissolved in 10 ~ (V/V) sulfuric acid and then the titanium trichloride was added to reduce iron to ferrous . The complex formed by rhodamine B and gallium was extracted with toluene-MIBK in 6 mol/L HC1. After organic phase was washed with thiourea, titani- um trichloride and rhodamine B solution ,its absorbance was measured at maximum absorption wave- length of 560 nm. The system error of method caused by sample decomposition was eliminated by cor- rection method. The absorbance was linear to the concentration of gallium in range of 0--1.0μg/mL with correlation coefficient of 0. 999. The results of proposed method were compared with those ob- tained by conventional dissolution method, and both were consistent. The gallium in six smelting ma- terial samples of yellow phosphorus electric dust was determined, with relative standard deviation (RSD) less than 10 %, and the recoveries of standard addition between 96 %-103 %.
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