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使用双硫腙和碳粉对铜(II)和汞(II)进行预富集,随后进行中子活化分析(作者译)

[Preconcentration of copper (II) and mercury (II) using dithizone and carbon powder followed by neutron activation analysis (author's transl)].

作者信息

Akaiwa H, Kawamoto H, Ogura K, Koizumi T

出版信息

Radioisotopes. 1981 Oct;30(10):535-8.

PMID:7335886
Abstract

A combined method of dithizone-extraction and carbon powder column adsorption was applied to concentrate trace amounts of copper (II) and mercury (II) in natural water samples before neutron activation analysis. The sample solution was adjusted to pH 1.0 with nitric acid, an aliquot of which as taken in a 500 cm3 separating funnel and then 5.0 cm3 of 0.01% dithizone-benzene and 25 cm3 of n-hexane wee added. The mixture was shaken for 10 min and stood for 30 min. After the aqueous phase was discarded, another aliquot of the sample solution was added. The above procedure was repeated until the treatment of the sample solution (1.00 dm3) was completed. The organic phase was then flown through the column (6mm phi x 50 mmh) containing carbon powder, and the resulting column was dried. The monitor containing 10 micrograms of mercury or copper was also prepared according to the above procedure. The samples and monitors were irradiated together in a pneumatic tube of JRR-3. After cooling, copper and mercury were determined by gamma-spectrometry using 64Cu, 197Hg, respectively. The recovery of trace metal ions obtained by this method was more than 99%, and the present method was found to be applicable to the preconcentration of copper (II) and mercury (II) in natural water samples.

摘要

在进行中子活化分析之前,采用双硫腙萃取和碳粉柱吸附相结合的方法对天然水样中的痕量铜(II)和汞(II)进行富集。用硝酸将样品溶液的pH值调至1.0,取一份等分试样置于500 cm3分液漏斗中,然后加入5.0 cm3 0.01%双硫腙苯溶液和25 cm3正己烷。将混合物振荡10分钟,静置30分钟。弃去水相后,再加入一份等分试样溶液。重复上述步骤,直至完成对1.00 dm3样品溶液的处理。然后使有机相流经装有碳粉的柱(内径6mm×高50mm),将所得柱子干燥。按照上述步骤还制备了含10微克汞或铜的监测样品。样品和监测样品在JRR - 3的气动管中一起辐照。冷却后,分别使用64Cu、197Hg通过γ能谱法测定铜和汞。该方法获得的痕量金属离子回收率超过99%,发现本方法适用于天然水样中铜(II)和汞(II)的预富集。

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