Korea Research Institute of Standards and Science, Daejeon, Republic of Korea.
Anal Chem. 2011 May 1;83(9):3493-8. doi: 10.1021/ac200158e. Epub 2011 Apr 5.
An accurate and precise measurement of selenium in Standard Reference Material (SRM) 3149, a primary calibration standard for the quantitative determination of selenium, has been accomplished by instrumental neutron activation analysis (INAA) in order to resolve a question arising during the certification process of the standard. Each limiting factor of the uncertainty in the activation analysis, including the sample preparation, irradiation, and γ-ray spectrometry steps, has been carefully monitored to minimize the uncertainty in the determined mass fraction. Neutron and γ-ray self-shielding within the elemental selenium INAA standards contributed most significantly to the uncertainty of the measurement. An empirical model compensating for neutron self-shielding and reducing the self-shielding uncertainty was successfully applied to these selenium standards. The mass fraction of selenium in the new lot of SRM 3149 was determined with a relative standard uncertainty of 0.6%.
为了解决标准认证过程中出现的问题,采用仪器中子活化分析(INAA)方法,对作为硒定量测定一级校准标准的标准参考物质(SRM)3149 中的硒进行了精确测量。仔细监测了活化分析中不确定度的每个限制因素,包括样品制备、辐照和γ射线谱测量步骤,以将测定的质量分数的不确定度降到最小。元素硒 INAA 标准内的中子和γ射线自屏蔽对测量的不确定度影响最大。成功地为这些硒标准应用了一个补偿中子自屏蔽并降低自屏蔽不确定度的经验模型。新一批 SRM 3149 中硒的质量分数的相对标准不确定度为 0.6%。