Hocquellet P, Candillier M P
Institut Municipal de Recherches sur l'Alimentation Humaine et Animale, Laboratoire Municipal, Bordeaux, France.
Analyst. 1991 May;116(5):505-9. doi: 10.1039/an9911600505.
A sensitive method for the accurate determination of Se in agricultural products at sub-ppm levels is described. The proposed procedure involves the wet oxidation of samples by using a mixture of nitric, sulphuric and perchloric acids, co-extraction of Se and added Pd with diethylammonium N,N-diethyldithiocarbamate in chloroform, and electrothermal atomic absorption spectrometric determination of Se in the organic extract. Atomization and extraction conditions are discussed. Special attention is given to the wet oxidation step, and its advantages in speed and simplicity over conventional heating have been evaluated using an automated microwave digestion system. The results reported, obtained from several reference materials, confirm the accuracy of the method with which a detection limit of 0.002 micrograms g-1 of Se can be achieved.
描述了一种用于准确测定农产品中亚ppm水平硒的灵敏方法。所提出的程序包括用硝酸、硫酸和高氯酸的混合物对样品进行湿式氧化,用二乙铵N,N-二乙基二硫代氨基甲酸盐在氯仿中对硒和添加的钯进行共萃取,以及用电热原子吸收光谱法测定有机萃取物中的硒。讨论了原子化和萃取条件。特别关注湿式氧化步骤,并使用自动微波消解系统评估了其在速度和简便性方面优于传统加热的优点。从几种参考物质获得的报告结果证实了该方法的准确性,该方法的检测限可达0.002微克 g-1的硒。