电感耦合等离子体原子发射光谱法测定钛白废酸萃取相中6种微量元素

建立了一种用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定钛白废酸萃取相中主要微量元素(钛、铝、钪、铁、钙和镁)方法。试样中大部分溶剂煤油经低温加热已挥发,剩余有机相用硝酸-硫酸混合酸在低温下消解,分解完全后冒三氧化硫白烟赶尽硝酸,冷却后,在选定的仪器工作条件下,以铟作为内标元素,对试液中钛、铝、钪、铁、钙和镁进行ICP-AES测定,共存元素之间基本没有干扰。方法的的检出限(μg/mL)分别为0.001(钛)、 0.016(铝)、0.004(铁)、0.015(钙)、0.002(钪)和0.005(镁)。方法用于钛白废酸萃取相样品中上述6种元素测定,相对标准偏差在0.35％～0.76％之间,加标回收率为97％～102％。

Determination of six trace elements in titanium oxide waste acid extraction phase by inductivelycoupled plasma atomic emission spectrometry

A method for simultaneous determination of major micro elements (Ti, Al, Sc, Fe, Ca, Mg) in titanium oxide waste acid extraction phase by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The most kerosene as solvent in the sample was volatilized by low-temperature heating.The left organic phase was digested with HNO₃ and H₂SO₄ mixture at low temperature to decompose completely, then HNO₃ was removed by smoking of sulfur trioxide. After cooling, Ti, Al, Sc, Fe, Ca, Mg in the sample solution were determined by ICP-AES with indium as internal elements under selected operating conditions of instrument. There was basically no interference between coexisting elements. The detection limits(μg/mL)were 0.001 for Ti, 0.016 for Al, 0.004 for Fe, 0.015 for Ca, 0.002 for Sc and 0.005 for Mg. The proposed method has been applied to determine the above six elements in titanium oxide waste acid extraction phase, with relative standard deviation (RSD) of 0.35%-0.76% and standard addition recovery of 97%-102%.