实验拟定了镍冶炼渣回收钪的冶金工艺过程中钪的检测方法,主要研究了偶氮胂Ⅲ光度法测定钪过程中高含量铁、镍和少量钛、稀土元素对其测定结果的影响与消除.实验结果表明:pH值为2最佳酸度下,钪与偶氮胂Ⅲ形成稳定的紫红色络合物,吸收峰在波长680 nm处,在室温下显色5 min即可测定,且吸光度在6h内基本保持稳定;铁、镍、钛、稀土元素干扰钪的测定,采用PMBP-乙酸丁酯萃取和甲酸萃取与其分离,可消除干扰影响.在最佳测定条件下,钪质量浓度在0 ～ 1.0 μg/mL符合比尔定律,表观摩尔吸光系数为1.8×104 L/(mol·cm).该方法相对标准偏差(RSD)小于1％,测定结果与电感耦合等离子体原子发射光谱法测定结果对比,基本一致.
This paper designs a detection method of scandium content in the metallurgical process of scandium recovery form nickel smelting slag.The research focuses on the effect of high iron and nickel content as well small a mounts of titanium and rare earth metals on the determination results in Arsenazo Ⅲ spectrophotometry and its elimination.The result shows that when the optimum acidity is pH =2,scandium and Arsenazo Ⅲ will form a stable purple complex,the absorption peak is at 680 nm,it can be measured after 5 minutes' color rendering and the absorbancy remains stable in 6 hours;the interference elements such as Fe,Ni,Ti,and rare earth elements are separated by PMBP-butyl acetate extraction and formic acid extraction to eliminate the effect.Under optimum conditions,scandium con forms to the Beer's law in the range from 0 μg/mL to 1.0 μg/mL,and the apparent molar absorbance coefficient is 1.8 × 104 L/(mol · cm).The standard deviation (RSD) is less that 1％.The measurement results and those of the Inductively Coupled Plasma Atomic Emission Spectrometry are basically the same.
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