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出 处:《理化检验(化学分册)》2011年第10期1170-1172,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
摘 要:采用氢化物发生-原子荧光光谱法测定海产品中总砷的含量。样品经硝酸-高氯酸(4+1)混合酸消解,样品溶液中加入硫脲和抗坏血酸混合溶液作为预还原剂。于盐酸(5+95)溶液中加入10g.L-1硼氢化钾-5g.L-1氢氧化钾溶液使与溶液中砷离子反应生成氢化物。分析时采用载气流量为400mL.min-1,屏蔽气流量为800mL.min-1。砷的质量浓度在20μg.L-1以内与荧光强度呈线性关系,方法的检出限(3s/k)为0.015μg.L-1。应用此法对3种海产品进行分析,测定值的相对标准偏差(n=6)在3.4%~4.2%之间,回收率在98.5%~101.0%之间。HG-AFS was applied to the determination of total amount of arsenic in seafood. Sample was digested with mixed acid of HNO3 HClO4 (4+1), and prereduced with mixed solution of thiourea and ascorbic acid. Hydride of As( Ⅲ) were generated from HCl(5+95) solution using solution of 10 g·L^-1 KBH4 dissolved 5 g·L^-1 KOH solution as reducing reagent. Flow-rates of 400 mL·min^-1 for the carrier gas and 800 mL·min^-1 for the shielding gas were taken in analysis. Linear relationship between the fluorescence intensity and mass concentration of As was found in the range within 20μg·L^-1 , with detection limit (3s/k)of 0. 015 μg·L^-1. Using 3 samples of seafood as matrixes, tests for recovery and precision were made by standard addition method, values of recovery and RSD's (n=6)found were in the range of 98.5%--101.0% and 3.4%-4. 2% respectively.
关 键 词:氢化物发生-原子荧光光谱法 海产品 总砷
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