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KMID : 0385520100230010045
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Analytical Science & Technology
2010 Volume.23 No. 1 p.45 ~ p.53
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Separation of chlorine in a uranium compound by pyrohydrolysis and steam distillation, and its determination by ion chromatography
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Kim Jung-Suk
Lee Chang Heon
Park Soon-Dal
Han Sun-Ho
Song Kyu-Seok
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Abstract
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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 ℃ until a volume of 90±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 U₃O? accelerator, by pyrohydrolysis at the temperature of 950 ℃ for 1 hour in a quartz tube with a stream of air of 1 mL/min supplied from the water reservoir at 80 ℃. 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.
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KEYWORD
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chlorine, steam distillation, pyrohydrolysis, ion chromatography, uranium compound
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