铬天青S光度法测定赤泥-钛白废水综合回收中的微量钪  

Determination of micro scandium in the comprehensive recovery of red mud-titanium dioxide wastewater by chromeazurol S spectrophotometry

作　　者：余荣旻 杨涛 邓志军 刘吉波 苏正夫 王志坚 

机构地区：[1]湖南稀土金属材料研究院,湖南长沙410126

出　　处：《冶金分析》2015年第1期63-67,共5页Metallurgical Analysis

基　　金：赤泥与钛白废液中有价元素综合回收利用课题(ZB2012CABBa1)

摘　　要：采用铬天青S作显色剂,研究了在赤泥-钛白废水综合回收过程中微量钪的分光光度法测定。考察了反应条件、共存离子等因素对检测结果的影响,确定了硫酸浸出液中钪的最佳检测条件为采用伯胺N1923为萃取剂,HCl为反萃剂,相比为1.0,萃取时间为10min,显色剂铬天青S（CAS）的体积为4.00mL,显色溶液的pH值为1.0-1.5,显色时间为30min。加入1.00mL盐酸羟胺溶液、2.00mL邻菲罗啉溶液作为掩蔽剂可消除残留于溶液中少量Fe的干扰。试验结果表明,络合物的最大吸收波长为615nm,表观摩尔吸光系数为2.85×10^5L·mol^-1·cm^-1,钪的质量浓度在0-0.18mg/L范围内符合比尔定律,校准曲线的相关系数为0.999 1。对钛白废水实际样品进行分析,实验方法与ICP-AES法测钪的相对误差在5%之内,钪测定结果的相对标准偏差（RSD,n〉6）为2.4%-4.1%。The spectrophotometric determination of micro scandium（Ⅲ） in the comprehensive recovery process of red mud-titanium dioxide wastewater with chrome auzrol S （CAS） as chromogenic reagent was sludied. The effect of reaction conditions, coexisting ions, etc. on the determination results was invesligated. The optimal conditions for scandium in sulfuric acid leaching solution were： primary amine N1923 as extraction agent, HCl as the stripping agent, phase ratio of 1.0, extraction time of 10 min, 4.00 mL of CAS as chro mogenic reagent at pH 1.0-1.5, ehromogenic time of 30 min. The interference of the small amount of resi due Fe（Ⅲ） could be masked by adding 1.00 mL of hydroxylamine hydrochloride and 2.00 mL of phenanthro line solution. The results showed that the maximal absorbance of the complex appeared at the wavelength of 615 mm; the apparent molar absorptivity was 2.85×10^5L·mol^-1·cm^-1. Beer＇s law was obeyed within the scandium （Ⅲ） mass concentration of 0-0.18 mg/L, and the correlation coefficient of the calibration curve was 0. 999 1. When it was applied to determine actual titanium dioxide wastewater, the relative error of proposed method and ICP-AES was within 5%, and the relative standard deviation （RSD, n〉6） was 2.4%-4. 1% .

关 键 词：钪 钛白废水 赤泥 分光光度法 铬天青S 伯胺N1923 

分 类 号：X832[环境科学与工程—环境工程]