微波消解ICP-MS法测定广西北部湾海鸭蛋中硒和锗的含量

摘要

以硝酸-过氧化氢(体积比为5∶3)混合溶液为消解剂,微波消解法处理海鸭蛋样品,采用电感耦合等离子体质谱法测定样品溶液中的硒和锗的含量.选择适合的同位素元素,运用碰撞室技术(CCT)降低多原子离子对元素硒、锗的干扰,用钇作为在线内标.硒、锗工作曲线的线性范围均为0.0～100.0 ng/mL,相关系数r=0.9996；硒、锗的检出限分别为1.1,0.15 ng/mL,测定结果的相对标准偏差分别为4.78％,5.70％(n=6),加标回收率为92.2％～104.0％.用该法测定国家标准物质黄鱼(GBW 08573)中硒的含量,测定值在标称值范围内.%The sea duck egg sample was dissolved with mixed solution of HNO3-H2O2 ( volum ratio was 5 : 3 ) by using microwave digestion, and the Se, Ge in the sample solution were determined by ICP-MS. The appropriate isotopes were selected, the polyatomic ions causing interference were eliminated by collision cell technology(CCT), and Y was used as internal standard. The liner range of calibration curves for Se and Ge was 0.0-100.0 ng/tnL with regression coefficient of 0.999 6. Detection limits of Se and Ge were 1,1,0,15 ng/mL respectively, the relative standard deviations of detection results were 4.78%,5.70%(n=6) respectively, and the recovery ranged from 92,2% to 104%. The method was used in determination of Se in national standard sample (yellow croak GBW08573), the result was in conformity with standard value.