食品科学 ›› 2000, Vol. 21 ›› Issue (1): 49-50.

• 分析检测 • 上一篇    下一篇

有机共沉淀一原子吸收法测定黄酒中铅

李毓贵,张久春,陈治强   

  1. 天津商学院与生物工程系
  • 出版日期:2000-01-15 发布日期:2011-11-25

 LI  Yu-Gui, ZHANG  Jiu-Chun, CHEN  Zhi-Qiang   

  • Online:2000-01-15 Published:2011-11-25

摘要: 黄酒样品的硝酸一高氯酸消化液,在 0.2mol/L硝酸介质中,加入吡咯啶二硫代甲酸铵(APDC),与铅作用形成难溶配合物和其沉淀,离心除去清液,沉淀液用甲基异丁基甲酮(MIBK)溶解,将有机相引入空气一乙炔火焰中,以原子吸收法测定铅,该方法的各种条件经选择和优化,它的特征浓度是0.28ug/ml/1%,检测限量是0.09ug/ml(K=3),线性范围是2-40ug/2ml,测定样品的相对标准偏差小于4.5%,在样品中加入0.2和0.4mg/L标准铅时,回收率分别为102%和98.5%,应用本法测定了多种黄酒中痕量铅,其结果令人满意。

关键词: 有机共沉淀, APDC, 火焰原子吸收法, 黄酒, 据测定

Abstract: It is reported that a method of measuring lead in rice wine was introduced with air acetylene flame atomic absorption spectroscopy (FAAS)after being preconcentrated by organic copreciplation. The method was based on the reac- tion that complex coprecipitate was formed between lead and pyrrolidine dithio carboxylic acid ammonium slat(APDC)as complexing agent and coprecipitator. The complex was separted out by centrifugation and dissolved with 4-methy 1-2- pentanone (MIBK). The lead in organic phase was measured by air-acetylene FAAS.The conditions of the method were elaborated. The characteristic concentration was 0.28 un/ml 1%.the detection limit 0.09ug/ml (K=3)and the relative stan- dard deviation less than 4.5%. The recovery rates were 102% and 985%respectively to 0.2 and 0.4mg/L lead added in samples. Thus this method has been successfully applied tp determine trace lead in rice wine.

Key words: Organic coprecipitate, Annomium pyrrolidine dithiocarbamate, Flame atomic