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微波消解样品-氢化物发生-原子荧光光谱法测定枸杞中砷 被引量:2

HG-AFS Determination of Arsenic in Lycium Chinense with Microwave Assisted Sample Digestion
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摘要 采用氢化物发生-原子荧光光谱法测定枸杞中砷的含量。样品经硝酸-过氧化氢混合溶液消解,在盐酸(5+95)溶液中,加入20.0g.L-1硼氢化钾溶液使与溶液中砷(Ⅲ)离子反应生成氢化物。分析中采用载气及屏蔽气的流量依次为400mL.min-1及1 000mL.min-1。试样溶液中加入硫脲-抗坏血酸混合溶液作为预还原剂。砷的质量浓度在0.05~10μg.L-1范围内与荧光强度呈线性关系,方法的检出限(3S/N)为0.032μg.L-1。应用此法对菠菜标准物质(GBW10015)进行分析,测定结果与认定值相符合。 HG-AFS was applied to the determinations of arsenic in Lycium chinense.Sample was dissolved with HNO3 and H2O2,and hydride of As(Ⅲ) was generated from HCl(5+95) solution by reacting with 20.0 g·L-1 KBH4 solution.Flow-rates of 400 mL·min-1 for carrier gas and 1 000 mL·min-1 for shielding gas were taken in the analysis.Mixed solution of thiourea and ascorbic acid was added to the sample solution as pre-reductant.Linear relationship between the fluorescence intensity and mass concentration of As found was in the range of 0.05-10 μg·L-1,with detection limit(3S/N) of 0.032 μg·L-1.The proposed method was applied to the analysis of a CRM of spinach(GBW 10015),giving results in consistency with the certified values.
出处 《理化检验(化学分册)》 CAS CSCD 北大核心 2011年第11期1305-1306,1309,共3页 Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词 微波消解 氢化物发生-原子荧光光谱法 枸杞 Microwave assisted sample digestion HG-AFS Lycium chinense Arsenic
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