微波消解样品-氢化物发生-原子荧光光谱法测定海贝中硒  

HG-AFS Determination of Selenium in Sea Shellfish with Microwave Assisted Sample Digestion

作　　者：张晓[1] 郎春燕[1] 赖晨焕[1] 张安琪[1] 

机构地区：[1]中铁二院工程集团有限责任公司工程测试中心,成都610059

出　　处：《理化检验（化学分册）》2011年第7期823-825,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：海贝样品经硝酸和过氧化氢微波加热消解,用氢化物发生-原子荧光光谱法测定其中硒的含量。使用溶于5g·L^(-1)氢氧化钾溶液中的10g·L^(-1)硼氢化钾溶液与溶液中硒离子反应生成氢化物。试样溶液中加入抗坏血酸消除硝酸的干扰。在优化的试验条件下,硒的质量浓度在600μg·L^(-1)以内与其荧光强度呈线性关系;方法检出限(3s/k)为0.076μg·L^(-1)。对2μg·L^(-1)硒标准溶液进行11次测定,相对标准偏差为1.6%。方法用于4种的海贝样品分析,加标回收率在86.0%～116.0%之间。The sample of sea shellfish was digested with HNO_3 and H_2O_2 with microwave assisted heating, and the content of Se in sample solution was determined by HG-AFS.Hydride of Se ion was generated by reacting with 10 g·L^（-1） KBH_4 solution（dissolved in 5 g·L^（-1） KOH solution）.The interference of HNO_3 was eliminated by adding ascorbic acid.Under the optimized experimental conditions,linear relationship between the fluorescence intensity and mass concentration of Se was kept in the range within 600μg·L^（-1）,with detection limit（3s/k） of 0.076μg·L^（-1）.Test for precision was performed with 2μg·L^（-1） Se standard solution,the value of RSD（n=11） found was 1.6%.The proposed method was applied to the analysis of 4 substantial samples,giving values of recovery found by standard addition method in the range of 86.0%-116.0%.

关 键 词：氢化物发生-原子荧光光谱法 微波消解样品 海贝 硒 

分 类 号：O657.31[理学—分析化学]