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Separation of chlorine in a uranium compound by pyrohydrolysis and steam distillation, and its determination by ion chromatography
Analytical Science and Technology / Analytical Science and Technology, (P)1225-0163; (E)2288-8985
2010, v.23 no.1, pp.45-53
https://doi.org/10.5806/AST.2010.23.1.045
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(2010). Separation of chlorine in a uranium compound by pyrohydrolysis and steam distillation, and its determination by ion chromatography. Analytical Science and Technology, 23(1), 45-53, https://doi.org/10.5806/AST.2010.23.1.045
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Abstract
우라늄 화합물 중에 함유된 염소를 정량하기 위하여 수증기증류 및 열가수분해를 이용한 미량염소의 분리 및 정량법을 개발하였다. 수증기 증류에 의한 시료 중의 염소를 분리하기 위하여 수증기 발생장치, 증류플라스크 및 냉각기 등으로 구성된 장치를 제작 설치하였다. LiCl 표준용액과 모의사용후핵연료 일정량을 혼합하여 만든 우라늄 화합물 시료 중의 염소를 분리하기 위하여 혼산(0.2 M ferrous ammonium sulfate-0.5M sulfamic acid 3 mL + phosphoric acid 6 mL + sulfuric acid 15 mL)을 이용하여140 oC로 증류시키고 90±5 mL를 수집하였다. 열가수분해에 의한 시료 중의 염소를 분리하기 위하여 공기공급장치, 온수공급장치, 석영반응관, 연소로 및 연소보트, 그리고 휘발 염소 흡수장치로 구성된 열가수분해장치를 제작 설치하였다. 일정량의 우라늄 화합물 시료에 반응촉진제(U3O8)를 가하고 1 mL/min의공기유속과 80℃의 공급수 온도를 유지하고 950℃에서 1시간 반응시켜 시료 중의 염소를 분리하였다. 두 방법에 의하여 수집된 각 흡수용액은 일정부피로 희석하고 이온크로마토그래피로 정량하여 회수율을측정하였다. 금속전환체 잔류 용융염 중의 미량 염소를 이온크로마토그래피로 정량하기 위하여 시료를공기 및 건조 산화시키고 분쇄한 후 열가수분해하여 염소를 회수하였다.
- keywords
- chlorine, steam distillation, pyrohydrolysis, ion chromatography, uranium compound
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