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本文叙述了二氧化钚中29种杂质元素的分配色谱分离-光谱测定法。配制了一套带磁力搅拌的溶样装置。采用高沸点油浴溶样,对30毫克二氧化钚约20分钟即可完全溶解。 方法采用磷酸三丁醋和三异辛胺(1:1)混合萃取剂作固定相,聚三氟氯乙烯粉作支持体,3.5N硝酸作流动相的柱分配色谱法,从30毫克二氧化钚中分离出待测杂质元素,使它们全部收集在1毫升接收液中,其中含钚量甚低不干扰测定。采用铟作外加基体,铟和钇为内标元素。以高压火花溶液干渣法在ИСП-28型和ИСП-51型摄谱仪上联合测定镉、钡、铍、铁、钻、硅、硼、镓、钪、磷、锰、铬、钨、镁、钼、铅、镍、铝、钛、镧、钙、钒、铈、铜、银、锌、锂、钠、钾等29种杂质元素。各杂质的测定范围在3×10~(-6)—3×10~(-2)％之间不等,方法的回收率为83—120％,精密度在±28％以内。吸附在柱上的钚可用4N甲酸作解吸剂,30毫克二氧化钚用2毫升解吸即可定量解吸。
This paper describes the chromatographic separation of 29 impurity elements in plutonium dioxide - spectrometry. A magnetic stirring device was prepared. High-boiling oil bath dissolved sample, 30 mg of plutonium dioxide about 20 minutes to completely dissolve. Methods The column was chromatographed with 3.5 N nitric acid as mobile phase using tributyl phosphate and triisooctylamine (1: 1) mixed extractant as stationary phase, polychlorotrifluoroethylene powder as support and 30 mg of dioxan Plutonium was isolated from the detection of impurity elements, so that they all collected in 1 ml of the receiving solution, containing very low levels of plutonium does not interfere with the determination. Indium is used as an additional matrix, indium and yttrium as internal standard elements. Determination of cadmium, barium, beryllium, iron, diamond, silicon, boron, gallium, scandium, phosphorus, manganese, chromium, tungsten and magnesium in ИСП-28 and ИСП-51 spectrographs by high-pressure sparking solution dry-slag method 29 kinds of impurity elements such as molybdenum, lead, nickel, aluminum, titanium, lanthanum, calcium, vanadium, cerium, copper, silver, zinc, lithium, sodium and potassium. The measurement range of each impurity ranged from 3 × 10 -6 to -3 × 10 -2%. The recoveries were 83-120% and the precision was within ± 28%. Adsorbed on the column of plutonium available 4N formic acid as a desorbent, 30 mg of plutonium dioxide desorption with 2 ml to quantitative desorption.