液-液萃取分离和α谱法顺序测定环境样品中的钚和镅。
Liquid-liquid extraction separation and sequential determination of plutonium and americium in environmental samples by alpha-spectrometry.
机构信息
Environmental Research Laboratory II, Japan Atomic Energy Research Institute, Tokai-mura, Ibaraki-ken 319-11, Japan.
出版信息
Talanta. 1987 Jun;34(6):567-70. doi: 10.1016/0039-9140(87)80190-x.
A procedure is described by which plutonium and americium can be determined in environmental samples. The sample is leached with nitric acid and hydrogen peroxide, and the two elements are co-precipitated with ferric hydroxide and calcium oxalate. The calcium oxalate is incinerated at 450 degrees and the ash is dissolved in nitric acid. Plutonium is extracted with tri-n-octylamine solution in xylene from 4M nitric acid and stripped with ammonium iodide/hydrochloric acid. Americium is extracted with thenoyltrifluoroacetone solution in xylene at pH 4 together with rare-earth elements and stripped with 1M nitric acid. Americium and the rare-earth elements thus separated are sorbed on Dowex 1 x 4 resin from 1M nitric acid in 93% methanol, the rare-earth elements are eluted with 0.1M hydrochloric acid/0.5M ammonium thiocyanate/80% methanol and the americium is finally eluted with 1.5M hydrochloric acid in 86% methanol. Plutonium and americium in each fraction are electro-deposited and determined by alpha-spectrometry. Overall average recoveries are 81% for plutonium and 59% for americium.
介绍了一种从环境样品中同时测定钚和镅的方法。样品用硝酸和过氧化氢浸取，两种元素与氢氧化铁和草酸钙共沉淀。草酸钙在 450°C 下灼烧，灰分用硝酸溶解。在 4M 硝酸中用三正辛胺-二甲苯溶液萃取钚，用碘化铵/盐酸反萃取。在 pH 4 时，用三氟乙酰丙酮-二甲苯溶液从 4M 硝酸中萃取镅和稀土元素，用 1M 硝酸反萃取。分离出来的镅和稀土元素从 1M 硝酸在 93%甲醇中用 Dowex 1 x 4 树脂吸附，用 0.1M 盐酸/0.5M 硫氰酸铵/80%甲醇洗脱稀土元素，最后用 86%甲醇中的 1.5M 盐酸洗脱镅。各馏分中的钚和镅用电沉积法沉积并通过α谱法测定。钚的总平均回收率为 81%，镅的为 59%。
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