• Analytical Science and Technology
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• v.23 no.1
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• pp.45-53
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• 2010

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.

• Proceedings of the Korean Nuclear Society Conference
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• 2001.05a
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• pp.388.1-388
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• 2001

• Journal of Soil and Groundwater Environment
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• v.18 no.1
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• pp.112-122
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• 2013

Current status of soil contamination with fluorine and its source were investigated. The basic principles and procedures of various techniques for the analysis of fluorine contents in soil and solid phase samples were summarized in this review. Analysis of fluorine in solid matrices can be achieved by two types of techniques: (i) UV/Vis spectrophotometer or ion selective electrode (ISE) analysis after performing appropriate extraction steps and (ii) direct solid analysis. As the former cases, the standard method of Korean ministry of environment, alkali fusion-ISE method, pyrohydrolysis, oxygen bomb combustion, aqua regia digestion-automatic analysis, and sequential extraction-ISE method were introduced. In addition, direct analysis methods (i.e., X-ray fluorescence spectrometry and proton induced gamma-ray emission spectrometry) and atomic spectrometry combining with the equipment for introducing solid phase sample were also reviewed. Fluorine analysis techniques can be reasonably selected through site-specific information such as matrix condition, contamination level, the amount of samples and the principles of various methods for the analysis of fluorine presented in this review.

• Analytical Science and Technology
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• v.13 no.6
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• pp.712-721
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• 2000

$LiF-BeF_2-ZrF_4$(63-30-7 mol%) molten salt was dissolved up to 0.02g in 1ml of distilled water at room temperature. $ZrO_2$ oxide made from $ZrF_4$ through pyrohydrolysis was recovered by leaching in distilled water with $LiF-BeF_2-ZrF_4$molten salt including it at room temperature. The crystalline sharpness of recovered $ZrO_2$ oxide was not damaged.