Determination of Tributyl Phosphate Degradation Products by Ion Chromatography

Tributyl phosphate(TBP) is used in solvent extraction process for radioactive waste. This compound may be degraded to dibutyl phosphate($DBP^-$), monobutyl phosphate($MBP^{2-}$) and ${PO_4}^{3-}$ by radioactive material. Amount of $DBP^-$ and $MBP^{2-}$ in TBP must be monitored because they production of these compounds means degradation of which leads to a decrease in the extraction yield. Retention behavior for $DBP^-$, $MBP^{2-}$, $F^-$, $Cl^-$, ${NO_2}^-$, ${NO_3}^-$, ${SO_4}^{2-}$ and ${PO_4}^{3-}$ are studied with AS4A-SC(Dionex) analytical column and $Na_2CO_3$/NaOH eluent by Ion chromatography. Optimum condition for these anions is 2 mM $Na_2CO_3$/1 mM NaOH eluent. All anions by this condition is well separated within 15min. Dynamic range is $10{\mu}g/mL$ - $100{\mu}g/mL$ for DBP and $5{\mu}g/mL$ - $50{\mu}g/mL$ for $MBP^{2-}$, respectively. The Detection limit for AS4A-SC are $1{\mu}g/mL$ for $DBP^-$ and $0.5{\mu}g/mL$ for $MBP^{2-}$ in this system with a $25{\mu}L$ sample loop.

이온크로마토그래피에 의한 Tributyl Phosphate(TBP) 분해산물의 정량

TBP 내의 분해산물인 $DBP^-$ 및 $MBP^{2-}$의 정량을 위하여 이온크로마토그래피를 이용하였으며, AS4A-SC(Dionex) 분리관과 $Na_2CO_3$/NaOH 용리액을 사용하여 $DBP^-$, $MBP^{2-}$, $F^-$, $Cl^-$, ${NO_2}^-$, ${NO_3}^-$, ${SO_4}^{2-}$ 및 ${PO_4}^{3-}$의 머무름거동을 살펴보았다. 2 mM $Na_2CO_3$/1 mM NaOH 용리액에서 이들의 분리가 가장 효율적이었으며, 15분 이내에 분리되었다. $5{\mu}g/mL$ - $100{\mu}g/mL$의 농도범위가 측정에 적합하였으며, 이 범위에서 검량곡선은 $r^2$=0.999로 좋은 상관관계를 보여주었다. 시료량 $25{\mu}L$를 취할경우 $DBP^-$의 검출한계는 $1{\mu}g/mL$이고, $MBP^{2-}$의 검출한계는 $0.5{\mu}g/mL$ 이었다.