氢化物发生-原子荧光光谱法测定木薯干及其发酵产物酒精中铅量  

HG-AFS Determination of Lead in Cassava and Its Fermentation Product-Alcohol

作　　者：侯晋[1] 倪鹏[1] 梅少博[1] 张文国[1] 

机构地区：[1]南通出入境检验检疫局,南通226005

出　　处：《理化检验（化学分册）》2010年第9期1063-1065,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：南通市指导性社会发展科技计划(No.S2007008)

摘　　要：提出了用氢化物发生-原子荧光光谱法测定木薯干及其发酵产物（主要指用木薯干发酵所产生的酒精）中铅量的方法。其中木薯干样品系用硝酸-高氯酸（4＋1）的混合酸在微波消解仪中作消解处理,将所得溶液蒸发至近干后,用盐酸（1＋19）溶液溶解残渣。先后加入铁氰化钾溶液及草酸溶液分别消除铜（Ⅱ）及铁（Ⅲ）、钼（Ⅵ）、镍（Ⅱ）所引起的干扰。然后按所优选的条件用氢化物发生-原子荧光光谱法测定溶液中铅（Ⅱ）量。测得铅（Ⅱ）的质量浓度在1-280μg·L^-1范围内与相应的峰面积测量值之间呈线性关系,其检出限（3S/N）为5μg·L^-1（对木薯干样品）及1μg·L^-1（对酒精样品）。以木薯干和酒精为基体添加标准溶液,木薯干和酒精的平均加标回收率分别为97.9%和93.8%,测定结果的相对标准偏差（n=8）依次为2.68%及2.14%。A method for determination of lead in cassava and its fermentation products（especially alcohol produced by fermentation of cassava） by HG-AFS was proposed.Cassava sample was digested with HNO3＋HClO4（4＋1） mixture in microwave sample digestor.The solution was evaporated to near dryness and the residue was taken up with HCl（1＋19）.Solutions of potassium ferricyanide and oxalic acid were added to eliminate interferences from Cu2＋ and Fe3＋,Mo（Ⅵ）,Ni2＋ respectively.Lead（Ⅱ） in the solution was then determined by HG-AFS under the optimized conditions.Linear relationship between values of peak area and mass concentration of Pb（Ⅱ） was obtained in the range of 1-280 μg·L^-1with detection limit（3S/N） of 5 μg·L^-1for cassava and 1 μg·L^-1for alcohol.Recovery of the method was tested by stanadrd addition method using samples of cassava and alcohol as matrixes,giving values of average recovery of 97.9%（for cassava） and 93.8%（for alcohol）.Values of RSD′s（n=8） found from the analytical results of sample of cassava and alcohol were 2.68% and 2.14% respectively.

关 键 词：原子荧光光谱法 氢化物发生 铅(Ⅱ) 木薯干 酒精 

分 类 号：O657.31[理学—分析化学]