有机共沉淀一原子吸收法测定黄酒中铅
作 者：
李毓贵;张久春;陈治强
单 位：
天津商学院与生物工程系
关键词：
有机共沉淀;APDC;火焰原子吸收法;黄酒;据测定
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：
Organic coprecipitate; Annomium pyrrolidine dithiocarbamate; Flame atomic absorption spectrometry Rice wine; Lead determination
摘 要：
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.
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