Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
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Determination of Free Acid in U(VI)-Al(III) Solutions by Gran Plot Titration

Gran Plot 적정법을 이용한 U(VI)-AI(III) 용액의 자유산 농도 측정

  • Suh, Moo-Yul (Nuclear Chemistry Research Team, Korea Atomic Energy Research Institute) ;
  • Lee, Chang-Heon (Nuclear Chemistry Research Team, Korea Atomic Energy Research Institute) ;
  • Sohn, Se-Chul (Nuclear Chemistry Research Team, Korea Atomic Energy Research Institute) ;
  • Kim, Jung-Suk (Nuclear Chemistry Research Team, Korea Atomic Energy Research Institute) ;
  • Kim, Won-Ho (Nuclear Chemistry Research Team, Korea Atomic Energy Research Institute) ;
  • Eom, Tae-Yoon (Nuclear Chemistry Research Team, Korea Atomic Energy Research Institute)
  • Received : 1998.12.28
  • Published : 1999.06.25
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Abstract

The determination method of free acid in spent U-Al nuclear fuel solutions by Gran plot titration was described. Effect of U(VI) and Al(III) on the alkalimetric titration of nitric acid was investigated in oxalate complexing media as well as in noncomplexing media. Positive biases were observed in both titration media when the end-point was estimated by the Gran plot method. It was found that the cause of the bias was U(VI) in the oxalate complexing media, but Al(III) in the noncomplexing media. The relative error was less than 1% in the titration of 0.1 M $HNO_3$ at a U(VI) : Al(III) : $H^+$ mole ratio of up to 2:12:1 as long as the pH of the oxalate titration media was sustained to be below 5.0 at the beginning of titration. The method was successfully applied to the determination of nitric acid in a solution of HANARO reactor fuel with U:Al mole ratio of 1:6.

사용후 U-Al 핵연료 용해용액의 자유산 농도 측정에 이용할 수 있는 Gran plot적정법을 개발하였다. 질산을 염기로 적정할 때 미치는 U(VI)과 Al(III)의 영향을 옥살산칼륨 착화제가 함유된 적정매질과 함유되지 않은 적정매질에서 조사하였다. Gran plot방법으로 종말점을 구할 경우 두 가지 매질에서 모두 양의 오차가 있었으며, 착화제가 함유된 매질에서는 U(VI)이 그리고 착화제가 없는 매질에서는 Al(III)이 오차의 원인이었다. 옥살산칼륨 적정매질에 첨가하는 시료량을 조절하여 pH 5.0 이하에서 적정을 시작함으로써 오차를 줄일 수 있었으며, 질산 농도가 0.1 M이고 U(VI) : Al(III) : $H^+$의 몰비율이 2:12:1인 시료의 질산 농도 측정오차는 1%이하였다. 이 방법으로 U:Al의 몰비율이 1:6인 하나로핵연료 용해용액의 질산 농도를 정확하게 측정할 수 있었다.

Keywords

Acknowledgement

Supported by : 과학기술부

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