• Journal of Pharmaceutical Investigation
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• 제4권1_2호
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• pp.46-54
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• 1974

A new spectrophotemetric method was estalished for the determination of oleic acid. This method is based on the 1,2-dichloroe-thane extraction of the ion-pair formed between methylene blue and oleic acid. But the absorbance of an ion-pair in the 1,2-dichloroe-thane layer was variable with the temperature, the ion-pair was extracted back into a diluted hydrochloric acid solution. The maximum absorbance of the acid extract observed at $660m{\mu}$ and a lineal relationship was observed from the initial amount over the range of $50-800{\gamma}/ml$ of oleic acid in the aqueous phase. The composition ratio of the ion-pair formed between methylene blue and oleic acid was determined to be 2 : 1 by both the mole ratio and continuous variation methods.

• 한국대기환경학회지
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• 제6권2호
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• pp.147-154
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• 1990

A sensitive method for the determination of total selenium in aerosol particles is described. The method involves dissolution of aerosol particles by $HNO_3-HClO_4$ mixed acids, pre-reduction of Se (VI) to Se (IV) by boiling hydrochloric acid, and hydride generation followed by atomic absorption detection. Dissolved Se (IV) in 4M hydrochloric acid is reacted with $NaBH_4$ to form $H_2Se$, which is subsequently collected in an U-tube cooled in liquid nitrogen. Upon the completion of $H_2Se$ generation, the collected $H_2Se$ is rapidly vaporized into a quartz cuvette burner by removing the U-tube from liquid nitrogen, atomized, and then detected by an atomic absorption spectrophotometer. The absolute sensitivity of the method is 0.49 ng/0.0044 Abs. The accuracy of the method evaluated by analyzing standard reference materials for urban aerosol is better than 10%. Analytical results for urban and rural aerosol particles are reported.

• Preventive Nutrition and Food Science
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• 제5권1호
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• pp.7-9
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• 2000

Variouss concentrationss of free malonaldehyde were prepared from 1,1,3,3-tetraethoxy propane (TEP). Spectrophoto-metric determination and HPLC analysis of free malonaldehyde instead of malonaldehyde-thiobaribituric acid (MA-TBA) complex were conducted. Malonaldehyde was well separated on a $\mu$Bondapak C18 column. The absorbances at 254 nm and the HPLC peak areas of free malonaldehyde increased with the increase in its concentration. The correlation coefficient between absorbances and peak areas was 0.998. The total time elapsed to conduct the whole procedure was less than 15 minutes. This method directly measured the amount of free malonaldehyde in a short period of time successfully. This procedure is expected to be used as a rapid, accurate and specific means to de-termine the development of lipid oxidation in food.

• Bulletin of the Korean Chemical Society
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• 제27권11호
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• pp.1780-1784
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• 2006

Cloud point extraction was used to extract mefenamic acid (MF) from human urine, and spectrofluorimetry and spectrophotometry were used to analyze extracted MF. The variables affecting extraction and phase separation, i.e. HCl and Triton X-114 concentration, temperature and time of equilibration, were optimized. Under the experimental conditions used the limit of detection for extraction of 25 mL of sample was 0.006 and 0.045 mg $L^{-1}$, with relative standard deviations of 2.52 and 1.45% (n = 5) for spectrofluorimetric or spectrophotometric methods, respectively. Good recoveries in the range of 95-107% were obtained for spiked samples. The proposed methods were applied to the determination of MF in human urine.

• 분석과학
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• 제7권4호
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• pp.555-561
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• 1994

A method was described for the graphite furnace atomic absorption spectrophotometric determination of trace cadmium, copper, chromium and lead in urine samples. The elements were directly determined without any other treatments. The ash temperature was intensively optimized to improve the large background by the removal of organic materials and alkali and alkali earth metals in urine samples. Two kinds of standard solutions were used to plot calibration curves. From the recovery data, it could be confirmed that the analytical results with the synthetic urine matrix similar to real urine were more accurate than with a deionized water matrix.

• Bulletin of the Korean Chemical Society
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• 제21권11호
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• pp.1090-1094
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• 2000

A reaction between germanium (Ge) and the ligand, o-chlorophenylfluorone (o-CPF) has been carried out. The reaction sensitive at pH 4.5 in the presence of triton x-100 was selective in the presence of EDTA. The spectral correction technique was ap plied to the analysis of the reaction instead of single wavelength spectrophotometry because the absorption of excess of o-CPF was not negligible. An updated determination of the properties of the Ge(IV)-o-CPF complex is given, which involved the complex ratio, stepwise absorptivity and stability constant of the complex. In present work, the results show that the complex $Ge(o-CPF)_3was$ formed and its cumulative stability constant was 1.09 ${\times}$1016 . For sample analysis, the detection limit of germanium was 0.01 mg/L, and the recoveries were between 96.4% and 102%, with relative standard deviations of less than 6.5%.

• Bulletin of the Korean Chemical Society
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• 제17권4호
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• pp.338-342
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• 1996

A sensitive method for the determination of trace cadmium after the preconcentration by extracting its 8-hydroxyquinoline complex into a molten benzophenone was developed. Several experimental conditions such as the pH of solution, the amounts of 8-hydroxyquinoline and benzophenone, stirring time, and standing time were optimized. Trace cadmium in 100 mL water sample was chelated with 2.5 mL of 0.001 M 8-hydroxyquinoline at pH 8.0. After 0.07 g benzophenone was added, the solution was heated to about 70 ℃ and stirred vigorously for 1 minute to dissolve the complex quantitatively in a molten benzophenone, and stood for 30 minutes to reproduce the microcrystalline benzophenone. The benzophenone containing Cd-8-hydroxyquinoline complex was filtered and dissolved in acetone. Cadmium was determined by a flame atomic absorption spectrophotometry. The interfering effects of diverse concomitant ions were investigated and eliminated. This method could be applied to natural water samples and the recovery of more than 90% was obtained in the real samples.

• 분석과학
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• 제9권3호
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• pp.244-252
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• 1996

라탄족(III) 이온과 methylthymol blue 및 cetyltrimethylammonium bromide의 삼성 분계에 라탄족(III)-methylthymol blue 착물의 분광학적 특성을 조사하고 이를 토대로 흐름주입법에 의하여 라탄족(III) 이온들을 정량하였다. pH 5.8인 cetyltrimethylammonium bromide 용액에서 라탄족(III)-methylthymol blue 착물의 최대 흡수 파장은 대략 635nm 영역이며, 몰흡광계수는 $^{64}Gd$(III)로부터 $^{70}Yb$(III)에 대해 $4.51{\sim}6.11{\times}10^4Lmol^{-1}cm^{-l}$였다. Cetyltrimethyl-ammonium bromide 존재하에서, 이들 착물의 조성비는 1:2였다. 흐름주입법에 의한 란탄족(III) 이온의 검정곡선은 0.1~0.4ppm 범위에서 Beer의 법칙에 따른다. 시료의 분석속도는 약 60개 $hr^{-1}$이었다. 여러 양이온과 음이온의 영향을 조사한 결과 tartrate나 citrate 같은 리간드 음이온과 대부분 전이원소, 희토류 원소들에 의해 방해를 받았으며, 이들 양이온들은 란탄족(III) 이온을 정량하기 전에 사전 제거가 필요하다.

• 대한화학회지
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• 제35권5호
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• pp.534-538
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• 1991

흡착 분리 방법을 이용하여 고순도 삼염화실란(TCS) 중의 미량 붕소 농도를 분광광도법적으로 측정하는 방법을 제안하였다. TCS중의 붕소 화합물과 복합체를 잘 형성하고 황산-quinalizarin계 발색 시약에 잘 녹으며 측정시 간섭 효과를 나타내지 않는 Lewis 염기성 물질로 NaCl이 선택되었다. 이러한 흡착 분리 방법을 통해 TCS분석 도중에 실리카겔 및 기포가 생성되는 문제를 방지할 수 있었는데, 반도체급 TCS중의 붕소 농도는 ${\pm}$20%의 표준편차 범위내에서 6.1 ${\mu}$g/l로 측정되었다. 반면 NaCl로 붕소화합물을 제거시킨 정제된 TCS 중의 붕소 농도는 0.2 ${\mu}$g/l이어서 NaCl의 우수한 흡착 성능을 확인할 수 있었다. 또한 NaCl이 TCS 정제 중 붕소 제거에 효과적임을 다른 잘 알려진 흡착제들과 비교 분석하였다.

• 분석과학
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• 제6권1호
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• pp.57-63
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• 1993

흐름주입법에 의하여 분광광도 방법으로 코발트를 정량하였다. $NH_3-NH_4Cl$ 완충용액(pH 10.5)에서 2-(5-bromo-2-pyridylazo)-5-(N-propyl-N-sulfopropylamino)aniline은 코발트와 수용성 착물을 형성한다. 이 착물의 최대흡수 파장은 545nm이고, 몰흡광계수는 $58000L\;mol^{-1}\;cm^{-1}$이다. 코발트의 검정곡선은 0.1~0.6ppm 범위에서 직선관계를 보였고, 검출한계는 25ppb였다. 상대표준편차는 0.5ppm에 대하여 ${\pm}0.72%$였고, 시료의 채취속도는 $60samples\;hr^{-1}$였다. 여러 가지 양이온과 음이온의 방해효과를 조사한 결과, NI(II), Cu(II), Fe(III) 및 $CN^-$이 많은 방해를 하였다. 그러나 운반체흐름에 $1.0{\times}10^{-3}M$ EDTA 용액을 넣음으로써 금속이온들의 방해를 감소시킬 수 있었다.