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建立了电感耦合等离子体质谱法(ICP-MS)测定痕量U价态分析方法。利用邻菲罗啉掩蔽Fe(Ⅱ)防止U(Ⅵ)被还原,硫酸羟胺防止U(Ⅳ)被氧化,HF溶解硅酸盐并与U(Ⅳ)形成UF4沉淀,硫酸铈铵和CaCO_3作为共沉淀剂混合载体,沉淀后离心分离。分别溶解上清液和沉淀,用ICP-MS进行测定。通过一系列条件优化,获得U(Ⅳ)和U(Ⅵ)的RSD分别为2.2%和1.9%,检出限为1.37μg/g。对实际样品进行测定,样品回收率均在65.5%~97.0%。
Inductively coupled plasma mass spectrometry (ICP-MS) was established for the determination of trace U valences. The use of o-phenanthroline to mask Fe (II) prevents the reduction of U (VI), hydroxylamine sulfate to prevent U (IV) from being oxidized, HF dissolves silicate and UF4 precipitates with U (IV), cerium ammonium sulfate and CaCO3 Precipitant mixed carrier, centrifuged after precipitation. Supernatants and pellets were separately lysed and assayed by ICP-MS. Through a series of conditional optimization, the RSDs of U (Ⅳ) and U (Ⅵ) were 2.2% and 1.9%, respectively. The detection limit was 1.37μg / g. The actual samples were measured, the sample recovery rates were 65.5% ~ 97.0%.