氢化物发生-原子荧光光谱法测定锌锭中锡铅锑铋

Determination of tin,lead,antimony,bismuth in zinc ingot by hydride generation atomic fluorescence spectrometry

锌锭样品用盐酸溶解后，在氨性介质中加入Al^3＋，锡铅锑铋离子与氢氧化铝共沉淀后，用盐酸（2＋98）溶解沉淀，氢化物发生-原子荧光光谱法测定锡铅锑铋。选择0．10mol／L的Al^3＋加入量为4．0～5．0mL，共沉淀时间为30min，用10mL 0．1mol／L的氨水洗涤沉淀符合共沉淀要求且不会造成沉淀损失。基体锌及试液中引入的Al^3＋对测定均不产生干扰。方法用于锡铅锑铋的质量分数大于0．001％的锌锭中几种离子的测定，结果满足分析要求。

After zinc ingot was dissolved with HCl,Al^3＋ was added in ammoniacal medium. Tin,lead, antimony and bismuth were co-deposited with Al（OH）3. The precipitations were dissolved with HCl （2＋98） ,and then Sn,Pb,Sb and Bi were determined by hydride generation atomic fluorescence spectrometry,respectively. The dosage of Al^3＋ at 0.10 mol/L was 4.0-5.0 mL and the co-deposition time was 30 min. The washing of precipitates with 10 mL of ammonia at 0.1 mol/L met the demands of codeposition and caused no loss. The matrix zinc and introduced Al^3＋ in solution did not interfere in the determination. The method was applied to the determination of Sn, Pb, Sb and Bi with mass fraction higher than 0. 001 % in zinc ingot,and the results fulfilled the requirement of analysis.