无氟酸溶ICP-AES同时测定铝及铝合金中低含量硅

Simultaneous Determination of Micro Silicon in Aluminium and Aluminiun Alloys by ICP-AES with Non-fluoric Acid Digestion

提出了一种基于无氟酸溶、电感耦合等离子体原子发射光谱(ICP-AES)法同时测定铝及铝合金中低含量硅的方法。铝及铝合金中低含量硅,以无定形硅、固溶体、金属间化合物形式存在。探讨了样品与酸、碱的反应,以及各种溶解体系的分解行为,表明强氧化剂存在,能有效抑制硅烷生成。结合化学热力学、动力学,过氧化氢-稀盐酸溶解样品,Si 288.158 nm为分析线,测定范围0.01%~1.0%,校准曲线的线性相关系数0.9996,ICP-AES同时测定铝及铝合金中低含量硅以及铜、镁、锰、铁、锌、镍、钛等元素。方法操作简便、准确、快速、稳定,经济实用,结果满意。

A rapid method for simultaneous determination of micro silicon in aluminium and aluminiun alloys by ICP-AES based on non-fluoric acid digestion was proposed.The micro silicon in aluminium and aluminiun alloys usually exists as amorphous silicon,solid solution and intermetallics.The reaction between the specimen and acid or base was discussed,and the reaction between the sample and a series of acid digested systems was investigated in detail.The results showed that the production of slane could be effectively inhibited under the pre-existence of a strong oxidant during the digestion.Combined with chemical thermodynamics and chemical kinematics,the sample is dissolved by HCl(1+3)in the presence of hydrogen peroxide.Si 288.158 nm is selected as the analytical line,and determining range of silicon lies in 0.01%~1.0% with linear correlation coefficient 0.9996,the micro silicon and other elements such as Cu,Mg,Mn,Fe,Zn,Ni,Ti etc.in aluminium and aluminiun alloys are simultaneously determined by ICP-AES.The proposed method is satisfactory with the advantages of simplicity,accuracy,rapidity,stability and practicality.