• Bulletin of the Korean Chemical Society
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• 제29권1호
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• pp.99-103
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• 2008

Solvent extraction using salphen as a ligand has been investigated for the selective separation and determination of trace Fe(II) and Fe(III). A salphen ligand was synthesized, and solvent extraction variables, such as solution pH, the concentration of salphen, the type of organic solvent, auxiliary agents, oxidants and the effect of interference were optimized. Salphen is stable at pH 3-4, and Fe(III)-salphen complexes can be selectively extracted into an MIBK(4-methyl-2-pentanone) phase from an aqueous solution within this pH range. For the determination of the total amount of iron in 100 mL of aqueous solution, Fe(II) ions were completely oxidized using 0.05 mL of 3.5% H2O2 without side reactions. To evaluate its applicability, the proposed method was applied to determine trace Fe(II) and Fe(III) in several kinds of water samples. Reproducible results were obtained with RSD of less than 3.0%, and the recoveries for this reliability were obtained with 91-112%.

• 약학회지
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• 제13권1호
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• pp.28-32
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• 1969

For the colorimetric determination of Sulfa-drugs by means of solvent extraction, the sample solutions were added into dimethylglyoxime-Fe(II) complex solution, and extracted with pyridine-chloroform mixture (1:50) is a range of pH 7.5-8.5. The extracted solution shows stability and maximum absorption at 402m${\mu}$.

• 분석과학
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• 제24권3호
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• pp.231-235
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• 2011

A spectrofluorimetric method for the determination of EDTA in real samples such as mayonnaise, powder detergent and cleansing cream with tiron (4,5-dihydroxy-1,3-benzenedisulfonic acid) as a fluorimetric reporter was developed. When tiron is chelated with Cu(II), the fluorescent intensity is decreased by a quenching effect. However, when Cu(II)-tiron chelate reacts with EDTA, fluorescent intensity is increased as tiron is released. Several experimental conditions such as pH of the sample solution, the amount of Cu(II), the amount of tiron, heating temperature and heating time were optimized. Fe(III) interfered more seriously than any other ions, interference of Fe(III) could be disregarded, because Fe(III) was scarcely contained in selected real samples. The linear range of EDTA was from $8.0{\times}106{-8}\;M$ to $2.0{\times}10^{-6}\;M$. With this proposed method, the detection limit of Fe(III) was $5.2{\times}10^{-8}\;M$. Recovery yields of 92.7~99.3% were obtained. Based on experimental results, it is proposed that this technique can be applied to the practical determination of EDTA.

• 약학회지
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• 제16권4호
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• pp.180-185
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• 1972

A new spectrophotometric method was established for the determination of undecylenic acid. The method is based on the solvent extraction into nitrobenzene of the ion pair formed between tris(1,10-phenanthroline)Fe(II) chelate and the anion of undecylenic acid. The maximum absorbance of the extract in the organic phase was at 518nm. A maximum extraction was obtained at pH 9-11, when excess of at least 50-fold(molar) of the phenanthroline-Fe(II) chelate to undecylenic acid was present. The color intensity of the extracted species remained constant at room temperature for the several hours after separation of the organic layer. A linear relationship was obtained over the tested range of 5-20${\gamma}$/ml of undecylenic acid. The effect of several other fungicids on this method was investigated. The method was applied to the determination of undecylenic acid in preparations and the results were in good agreement with those added amounts.

• 약학회지
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• 제13권1호
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• pp.22-27
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• 1969

Nicotinamide Complex Compound was not formed in simple alkaline solution under two to one molar ratio of dimethyglyoxime and Fe (II), but it was formed with ammonia or pyridine under the same molar ratio. Based on this fact, nicotinamide solution was added into dimethyglyoxime-Fe (II) complex solution, and the chelation product was extracted with chloroform. The extraction was Completed in a range of pH 8.4-11.0. The chloroform solution shows stability and maximum absorption at 516 m${\mu}$.

• 응용화학
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• 제15권2호
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• pp.113-116
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• 2011

A sensitive and selective determination method of Fe(II) ion by luminol-H₂O₂ system using a chelating reagent has been presented. A metal ion-chelating ligand complex such as Fe(II)-diethylenetriamine pentaacetic acid (DTPA) produced higher chemiluminescence (CL) intensity as well as longer lifetime in luminol-H₂O₂ system than metal exist as free ions. Furthermore, the catalytic activity of Cu(II) and Pb (II) complexes with chelating reagents in luminol-H₂O₂ system was lost since chelating reagents act as a masking agent although free Cu(II) and Pb(II) ions have high catalytic activity. On the optimized conditions, the calibration curve of Fe(II) ion was linear over the range from 1.0×10^-7 to 2.0×10^-5 M with correlation coefficient of 0.996. The detection limit was calculated to be 4.0×10^-8 M.

• 대한화학회지
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• 제47권2호
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• pp.115-120
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• 2003

Perfluorinated sulfonated polymer(Nafion)-ethylenediamine(en)이 화학수식된 유리탄소전극으로 Fe(II) 이온의 정량에 대해 연구하였다. Fe(II) 이온의 착화제인 en을 nafion에 고정시켜 유리탄소전극 표면에 수식하면 이 수식전극의 en은 Fe(II) 이온과 $[Fe(en)_3]^{+2}$의 착물을 형성한다. Nafion-en이 화학수식된 유리탄소전극에서 시차펄스전압전류법에 의한 Fe(II) 이온의 산화봉우리전위는 0.340${\pm}$0.015 V(vs. Ag/AgCl), 측정범위는 $5{\times}10^{-6}{\sim}0.2{\times}10^{-3} M(0.28{\sim}11.17 mg/L)$, 검출한계(3s)는 $1.89{\times}10^{-5}$M(1.056 mg/L)이었다.

• 대한화학회지
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• 제46권6호
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• pp.509-514
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• 2002

정지흐름분석법을 이용하여 화학발광법으로 수용액 중의 Fe(II)와 Fe(III)을 분리 정량하는 방법에 대하여 연구하였다. 이 방법은 lucegenin과 $H_2O_2$ 혼합용액에 Fe(III)이온을 첨가하였을 때 화학발광의 세기가 증가하는 것을 기초로 하였다. KO H, $H_2O_2$ 및 Fe(III)의 가리움제로 이용한 citric acid의 농도와 시료의 주입속도가 화학발광의 세기에 미치는 영향을 조사하였다. 전체 철의 정량을 위하여 구한 [$H_2O_2$], [KOH] 및 흐름속도의 죄적조건은 각각 4.0M, 2.0M, 및 3.5mL/min 이었고, 이러한 최적조건 하에서 얻은 검정곡선에서 직선성이 성립하는 범위는 1.0${\times}10^{-6}$M에 서 1.0${\times}10^{-4}$M이었고, 상관계수는 0.996, 검출한계는 1.0${\times}10^{-7}$M이었다. Fe(III)이온의 정량을 위하여 구한 [$H_2O_2$], [KOH], [citric acid] 및 흐름속도의 최적조건은 각각 4.0M, 2.0M, 0.01M 및 3.5mL/min이었고 이러한 최적조건 하에서 얻은 검정곡선에서 직선성이 성립하는 범위는 1.0${\times}10^{-6}$M에서 1.0${\times}10^{-4}$M이었고, 상관관계수는 0.997, 검출한계는 5.0${\times}10^{-7}$M이었다.

• 대한화학회지
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• 제46권5호
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• pp.419-437
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• 2002

산성조건에서 $H_2O_2$에 의한 $Fe^{2+}$ 이온의 산화($Fe^{2+}{\to}Fe^{3+}$)반응과 $Fe^{3+}$이온과 $SCN^-$이온이 결합하여 붉은색 Fe$(SCN)^{3-x}_x$ 이온을 형성하는 착화반응을 도입한 흐름주입분석기법을 사용하여 $Fe^{2+}$이온과 $Fe^{2+}$이온이 공존하는 시료용액 중 각 이온들의 동시정량을 위한 분석법을 개발하였다. 이 분석법은 개별 이온들에 대한 정량단계에 앞서 혼합시료의 전처리($Fe^{2+}$이온의 예비산화 혹은 $Fe^{2+}$이온의 예비환원)단계를 거쳐야 하는 기존의 분석법들과는 달리 두가지 단계들을 동시에 수행할 수있다는 장점을 가진다. 이 분석법의 측정한계는 [$Fe^{2+}$]=6.00${\times}10^{-7}$M 이었다.

• 분석과학
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• 제12권6호
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• pp.515-520
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• 1999

Al(III)-thorin 착물에 대한 분광학적 정량 방법을 연구하였다. pH, 리간드와 계면활성제의 농도 및 안정화 시간에 대한 최적 조건을 결정하였다. thorin 리간드는 Fe(III), Ni(II), Cu(II), Pb(II) 그리고 Co(II)를 포함한 시료용액으로부터 Al(III)을 선택적으로 분리할 수 있도록 해준다. 여러 계면활성제중에서 비이온성인 Triton X-100에서 가장 안정한 상태를 나타냈고 수용액 중에서 Al(III)-Thorin-Triton X-100 착물은 526 nm에서 최대 흡광도를 가진다. 이 방법은 혼합된 시료용액에서 Al(III)을 정량하는데 이용되었다. 그리고, 분리 및 예비농축과정은 resoreinol-fermaldehyde 수지로 채워진 컬럼을 이용하였다. 컬럼 단계에서 수지의 흡착 능력은 pH변화에 매우 민감하기 때문에 pH를 조절하는 것이 필수적이다. 분리과정은 0.2 M acetic acid-sodium acetate 완충용액 (pH 4.5)와 1.0 M $HNO_3$용액으로 이루어졌다.