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机构地区:[1]吉林农业大学测试中心,农业部参茸产品质量监督检验测试中心,长春130118 [2]靖宇特产管理总站,靖宇135200
出 处:《理化检验(化学分册)》2009年第10期1203-1205,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
摘 要:提出了香菇中硒的氢化物发生-原子荧光光谱测定方法。样品经硝酸消化后蒸发至约2 mL,在6 mol·L^(-1)盐酸10 mL介质中煮沸使硒(Ⅵ)完全还原至硒(Ⅳ),分取部分试液加入铁氰化钾后供氢化物发生-原子荧光光谱法测定。氢化物发生系在5 g·L^(-1)氢氧化钾介质中加入硼氢化钾浓度为20 g·L^(-1)时进行。测定中采用标准曲线法,其硒的质量浓度范围为60μg·L^(-1)以内。方法的检出限(3s/k)为0.26μg·L^(-1)。应用此方法测定标准物质(GBW 085036)中硒量,测定值(0.046μg·g^(-1))与证书值(0.049±0.014)μg·g^(-1)相符,其相对标准偏差(n=6)为2.1%。HG-AFS was applied to the determination of Selenium in dried mushrooms. Dried mushroom sample was digested with eonc. HNO3. The solution was evaporated to ca. 2 mL, and kept boiling gently for 3-5 min after addition of 10 mL of 6 mol ·L^-1 HCl to reduce Se(Ⅵ) completely to Se(Ⅳ). An aliquot of the sample solution was taken for the HG-AFS determination after addition of Ka Fe(CN)6. Hydride generation was performed in 5 g ·L^-1 KOH medium with 20 g ·L^-1 of KBH4. Standard curve with mass concentration of Se(Ⅳ) in the range within 60μg · L^-1 was used for the determination. Detection limit (3s/k) found was 0. 26 μg · L^-1. The proposed method was used to analyze a CRM of wheat powder (GBW 085036), giving the analytical result of Se 0. 046μg · L^-1, which is in consistency with the certified value (0. 049±0. 014) μg · L^-1 and the value of RSD (n=6) found was 2.1 %.
关 键 词:氢化物发生-原子荧光光谱法 硒 香菇
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