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叙述了四水硫酸钚中22种杂质元素的分配色谱分离-光谱测定法。方法采用磷酸三丁酯和三异辛胺(1:1)混合萃取剂作固定相,聚偏氟乙烯粉作支持体,5mol/L硝酸作流动相的柱分配色谱法,从50mg四水硫酸钚中分离出待测杂质元素,使它们全部收集在1mL接收液中,其中含钚量甚低不于扰测定。采用铟作外加基体,铟和钇为内标元素。以电弧溶液于渣法在ИСЛ-28型和ИСЛ-51型摄谱仪上联合测定铝、铍、硼、镉、铬、铁、锰、镁、镍、磷、铅、硅、钙、铜、钴、钪、钛、钒、锌、锂、钠、钾等22种杂质元素。各杂质的测定范围在3×10~(-6)至2×10~(-2)％之间不等,方法的回收率为83％至120％,精密度在±26％以内。吸附在柱上的钚可用4mol/L HCOOH或0.2mol/L H_2SO_4-0.1mol/LHNO_3混合酸作解吸剂。
Describes the chromatographic separation of 22 kinds of impurity elements in plutonium tetrahydrate sulfate - spectrometry. Methods Column chromatography with 5 mol / L nitric acid as mobile phase was carried out using tributyl phosphate and triisooctylamine (1: 1) mixed extractant as the stationary phase, polyvinylidene fluoride powder as the support, and 50 mg / Plutonium in the separation of impurities to be tested elements, so that they all collected in 1mL receiving solution, which contains very low content of plutonium is not determined. Indium is used as an additional matrix, indium and yttrium as internal standard elements. The determination of aluminum, beryllium, boron, cadmium, chromium, iron, manganese, magnesium, nickel, phosphorus, lead, silicon, calcium, copper, Cobalt, scandium, titanium, vanadium, zinc, lithium, sodium, potassium and other 22 kinds of impurity elements. The determination range of each impurity ranged from 3 × 10 -6 to 2 × 10 -2%. The recoveries were 83% to 120% and the precision was within ± 26%. Plutonium adsorbed on the column can be 4mol / L HCOOH or 0.2mol / L H_2SO_4-0.1mol / LHNO_3 mixed acid as desorbent.