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http://dx.doi.org/10.5806/AST.2010.23.1.045

Separation of chlorine in a uranium compound by pyrohydrolysis and steam distillation, and its determination by ion chromatography  

Kim, Jung-Suk (Nuclear Chemistry Research Division, KAERI)
Lee, Chang-Hun (Nuclear Chemistry Research Division, KAERI)
Park, Soon-Dal (Nuclear Chemistry Research Division, KAERI)
Han, Sun-Ho (Nuclear Chemistry Research Division, KAERI)
Song, Kyu-Seok (Nuclear Chemistry Research Division, KAERI)
Publication Information
Analytical Science and Technology / v.23, no.1, 2010 , pp. 45-53 More about this Journal
Abstract
For the determination of chlorine in uranium compound, analytical methods by using a steam distillation and a pyrohydrolysis have been developed. The steam distillation apparatus was composed of steam generator, distilling flask and condenser etc. The samples were prepared with an aliquot of LiCl standard solution and a simulated spent nuclear fuel. A sample aliquot was mixed with a solution containing 0.2 M ferrous ammonium sulfate-0.5 M sulfamic acid 3 mL, phosphoric acid 6 mL and sulfuric acid 15 mL. The chloride was then distilled by steam at the temperature of $140^{\circ}C$ until a volume of $90{\pm}5\;mL$ is collected. The pyrohydrolysis equipment was composed of air introduction system, water supply, quartz reaction tube, combustion tube furnace, combustion boat and absorption vessel. The chloride was separated from powdered sample which is added with $U_3O_8$ accelerator, by pyrohydrolysis at the temperature of $950^{\circ}C$ for 1 hour in a quartz tube with a stream of air of 1 mL/min supplied from the water reservoir at $80^{\circ}C$. The chlorides collected in each absorption solution by two methods was diluted to 100 mL and measured with ion chromatography to determine the recovery yield. For the ion chromatographic determination of chlorine in molten salt retained in a metal ingot, the chlorine was separated by means of pyrohydrolysis after air and dry oxidation, and grinding for the sample.
Keywords
chlorine; steam distillation; pyrohydrolysis; ion chromatography; uranium compound;
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