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采用标样法,研究微波消解条件下,王水加辅助酸(双氧水、高氯酸、氢氟酸)消解土壤,氢化物原子化-原子荧光法测定土壤全As、全Se的最佳消解酸体系和方法.含HF或氟化物的消解液对As和Se的测定有强烈的非原子荧光干扰;加HClO_4处理,因在正常的微波消解和赶酸条件下均无法完全去除,其残留物可能对待测元素的还原—氢化物生成过程发生阻碍而产生严重干扰;而王水加H_2O_2辅助氧化处理,既保证土壤矿物完全被打开,又能彻底氧化有机质,同时也避免了氧化剂残留对后续还原反应的干扰,采用土壤标样做回收率测定,As、Se的回收率分别为102%、112%,标准偏差和变异系数均满足土壤微量元素测定要求.
The standard method was used to study the digestion of soil with aqua regia and azo acids (hydrogen peroxide, perchloric acid and hydrofluoric acid) under microwave digestion conditions. The best digestion acid was determined by atomic fluorescence spectrometry and atomic fluorescence spectrometry. System and method.H2F or fluoride-containing digestion solution has strong non-atomic fluorescence interference to the determination of As and Se.If HClO_4 treatment can not be completely removed under normal microwave digestion and acid catalysis, the residue may The reduction of the analyte element - hydride generation process hindered serious interference; and aqua regia plus H_2O_2 auxiliary oxidation, both to ensure that soil minerals are fully opened, but also completely oxidized organic matter, but also to avoid the oxidant residues on the subsequent reduction reaction The recoveries of As and Se were 102% and 112%, respectively. The standard deviation and coefficient of variation all met the requirements of soil trace element determination.