• 분석과학
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• 제20권3호
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• pp.246-250
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• 2007

The quantitative determination of chromium(VI) by separation from chromium(III) complex of 8-hydroxyquinoline using solvent extraction has been studied. The reaction conditions for chromium(III) complex of 8-hydroxyquinoline and the solvent extraction of complex were investigated in detail. The chromium(III) complex was extracted with organic solvent (n-hexane) and residual chromium(VI) was determined by ICP-AES in aqueous layer. This technique is quantitative in the pH range of 8-9 and the limitations such as interfering ions were discussed.

• 대한환경공학회지
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• 제27권6호
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• pp.590-598
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• 2005

본 연구에서는 HPLC와 DRC ICP-MS를 연결하여 수중의 Cr(III)와 Cr(VI) 측정을 위한 최적의 분석조건을 설정하고, 서울시 6개 취수장 원수에서의 Cr(III)와 Cr(VI)의 분포 특성을 조사하였다. 크롬 종(species) 분리를 위한 HPLC 이동상으로는 tetrabutylammonium phosphate monobasic(1.0 mM TBAP), ethylenediaminetetraacetic acid(0.6 mM EDTA) 그리고 2% v/v 메탄올을 사용하였으며, flushing solvent로는 5% v/v 메탄올을 사용하였다. 또한 크롬 종 분리 시 방해물질인 $ArC^+$의 제거를 위한 반응가스로 암모니아($NH_3$) 가스를 사용하였으며, Cr(III)와 Cr(VI)의 최적의 분리를 위해 이동상의 solvent ratio, pH 유속 및 시료 주입량의 변화에 따른 시험을 실시하였다. 외국의 경우 Cr(III)가 Cr(VI)보다 분석 감도가 우수한 것으로 보고되고 있으나 본 연구 결과 반응가스($NH_3$)를 사용할 경우, Cr(III)에 비해 Cr(VI)의 분석 감도가 더 우수한 것으로 나타났으며, 검출한계는 Cr(III)와 Cr(VI)에 대해 각각 $0.061\;{\mu}g/L$, $0.052\;{\mu}g/L$로 분석시간은 3분 이내로 나타났다. 서울시 6개 취수장 원수에서의 Cr(III)는 $0.048{\sim}0.064\;{\mu}g/L$(평균 $0.054\;{\mu}g/L$), Cr(VI)는 $0.014{\sim}0.023\;{\mu}g/L$(평균 $0.019\;{\mu}g/L$)의 농도 범위로 검출되었다. 회수율은 $90.1{\sim}94.1%$ 범위로 우수하게 나타났으며, Cr(III)가 Cr(VI)에 비해 $2{\sim}3$배 정도 높은 농도로 나타났다.

• Bulletin of the Korean Chemical Society
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• 제31권10호
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• pp.2813-2818
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• 2010

A novel method was developed for the speciation of chromium in natural water samples based on homogeneous liquid-liquid extraction and determination by flame atomic absorption spectrometry (FAAS). In this method, Cr(III) reacts with a new Schiff's base ligand to form the hydrophobic complex, which is subsequently entrapped in the sediment phase, whereas Cr(VI) remained in aqueous phase. The Cr(VI) assay is based on its reduction to Cr(III) by the addition of sodium sulfite to the sample solution. Thus, separation of Cr(III) and Cr(VI) could be realized. Homogeneous liquid-liquid extraction based on the pH-independent phase-separation process was investigated using a ternary solvent system (water-tetrabutylammonium ion ($TBA^+$)-chloroform) for the preconcentration of chromium. The phase separation phenomenon occurred by an ion-pair formation of TBA and perchlorate ion. Then sedimented phase was separated using a $100\;{\mu}L$ micro-syringe and diluted to 1.0 mL with ethanol. The sample was introduced into the flame by conventional aspiration. After the optimization of complexation and extraction conditions such as pH = 9.5, [ligand] = $1.0{\times}10^{-4}\;M$, [$TBA^+$] = $2.0{\times}10^{-2}\;M$, [$CHCl_3$] = $100.0\;{\mu}L$ and [$ClO_4$] = $2.0{\times}10{-2}\;M$, a preconcentration factor (Va/Vs) of 100 was obtained for only 10 mL of the sample. The relative standard deviation was 2.8% (n = 10). The limit of detection was sufficiently low and lie at ppb level. The proposed method was applied for the extraction and determination of chromium in natural water samples with satisfactory results.

• 분석과학
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• 제7권2호
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• pp.205-211
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• 1994

아세트산과 숙신산이 결합된 폴리아민-폴리우레아(CPPI와 SAPPI) 수지는 폴리에틸렌이민-폴리메틸렌폴리페닐렌 이소시안에이트(PPI) 고분자와 클로로 아세트산 또는 클로로 숙신산의 반응으로 각각 합성되었다. 이 수지들은 적외선 분광광도법 및 원소분석법으로 구조를 확인하였다. 이 수지들에 대한 3가와 6가 크롬의 흡착특성은 용액의 pH를 변화시키면서 뱃치법에 의하여 분포계수($K_d$)를 측정하여 조사하였다. 3가와 6가 크롬은 이온교환반응으로 폴리아민-폴리우레아 수지에 흡착되는 것으로 생각되었다. 이들의 최적 분리조건을 발견하고, 단지 pH를 변화시키는 단계적 용리법에 의하여 이들의 SAPPI 수지관(내경 0.6cm, 길이 10cm)으로 분리하였다. 또한 6가 크롬은 CPPI 수지관에 의하여 50배의 농축인자로 농축할 수 있다.

• Bulletin of the Korean Chemical Society
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• 제27권5호
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• pp.694-698
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• 2006

A method has been described for the chemical speciation, preconcentration and determination of Cr(III) and Cr(VI) species in filtered tannery waste waters by flame atomic absorption spectrometry using ion-exchange resins. Amberlite IR-120($H^+$) strongly acidic cation exchanger and Amberlite IRA-410($CI ^-$) strongly basic anion exchanger resins were used for the separation and preconcentration of Cr(III) and Cr(VI) species, respectively. Optimum condition for preconcentration and speciation was obtained by testing pH of sample and eluent, flow rates of sample and eluent, amount of resins, volume of sample and eluents, and effect of foreign ions. The recommended method has been successfully applied for the preconcentration and determination of chromium species in the dissolved phase of waste water samples collected from a tannery waste water treatment plant in Kayseri, Turkey. The detection limits achieved were 0.73 $\mu$g/L for Cr(III) and 0.81 $\mu$g/L for Cr(VI). Recovery studies showed 99% for Cr(III) and 98% for Cr(VI), for samples spiked with single species.