• Bulletin of the Korean Chemical Society
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• 제32권2호
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• pp.673-680
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• 2011

The compound 3-(2-Mercaptopyridine)phthalonitrile has been synthesized and characterized by IR, UV-vis, and X-ray single-crystal determination. The molecular geometry from X-ray determination of the title compound in the ground state has been compared using the Hartree-Fock (HF) and density functional theory (DFT) with the 6-31G(d) basis set. The calculated results show that the DFT and HF can well reproduce the structure of the title compound. The energetic behavior of the title compound in solvent media was examined using the B3LYP method with the 6-31G(d) basis set by applying the Onsager and polarizable continuum model. Using the TD-DFT and TD-HF methods, electronic absorption spectra of the title compound have been predicted and good agreement with the TD-DFT method and the experimental determination was found. The predicted nonlinear optical properties of the title compound are much greater than those of urea. Besides, molecular electrostatic potential of the title compound were investigated by theoretical calculations. The thermodynamic properties of the compound at different temperatures have been calculated and corresponding relations between the properties and temperature have also been obtained.

• Bulletin of the Korean Chemical Society
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• 제28권3호
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• pp.369-372
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• 2007

A fast and simple high-performance liquid chromatography (HPLC) method for the simultaneous determination of four pesticides having fungicide properties has been proposed for Panax ginseng, C. A. Meyer grown for 4, 5, or 6 years. Analytical separation was performed on C18 columns using ultraviolet detector under gradient conditions. Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination. The HPLC response for all pesticides was linear, with determination coefficients > 0.9986. The average rate of recovery for pesticides spiked with 2 fortification levels was > 72% with relative standard deviations < 9%. The limits of quantification (LOQ) ranged from 0.03 to 0.16 ppm. These LOQs were lower than the respective maximum residue limits (MRL) established by the Korean Food and Drug Administration (KFDA), except for cyazofamid. The proposed method was used to determine pesticide residue levels in samples of ginseng obtained from Jeonnam Province (Republic of Korea). None of the pesticides were found in ginseng samples grown for 4, 5, or 6 years.

• Bulletin of the Korean Chemical Society
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• 제28권3호
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• pp.373-378
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• 2007

A micro organism Agrobacterium tumifacient as an immobilized cell on a solid support was presented as a new biosorbent in a simple and sensitive spectrophotometry determination of Ni(II) in various samples using 4-hydroxy benzaldehyde-4-bromophenyl hydrazone as a color developing agent (λmax 497 nm) at pH 4.0 ± 0.2. Beer's law was obeyed over the range of 0.01-0.1 μg L-1. The molar absorptivity and Sandell's sensitivity were 1.285 × 105 L mol-1cm-1 and 0.007245 μg cm-2 respectively. Under these conditions, the preconcentration factor obtained was 82, and the detection limit achieved was 0.05 μg L-1. The detailed study of various interfering ions made the method more sensitive and selective. The recovery of Ni(II) from various samples range from 97.75 to 99.35%. The present method was successfully applied for the determination of Ni(II) in spiked, natural water and alloy samples. The proposed method was compared with reported methods in terms of Student's ‘t'-test and Variance ratio ‘f'-test which indicates that there is no significant difference between proposed and literature method at 95% confidence level.

• 대한화학회지
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• 제33권3호
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• pp.315-320
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• 1989

철광석 중에 존재하는 미량 금속원소들을 분석하는 방법을 제시하였다. 분석방법은 ammonium pyrrolidinedithiocarbamate(APDC)-methyl isobutyl ketone(MIBK) 추출계와 원자흡수 분광법(AA)를 이용하였다. 철이 유기층으로 추출되는 것을 막기 위하여 가리움제로서 코발트, 니켈 및 구리의 분석시에는 pH $8{\sim}10$에서 citrate를, 그리고 망간 및 구리의 분석시에는 pH 6{\sim}7$에서 tiron을 가하였다. MIBK의 물에 대한 용해도를 줄이기 위해 NaCl을 염석제로 가하였다. 금속 추출용액의 안정도를 증가시키기 위한 방안으로 MIBK 금속 추출물을 질산 수용액으로 역추출하는 것을 검토하였다.

• Bulletin of the Korean Chemical Society
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• 제35권1호
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• pp.211-217
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• 2014

A new needle-based device for headspace wire coated in-needle microextraction (HS-WC-INME) was fabricated using a nichrome wire coated with poly(ethylene glycol) (PEG) and poly(dimethylsiloxane) (PDMS) mixture. The proposed needle device was applied for the determination of volatile compounds in lavender and lavandin essential oils by gas chromatography. Fundamental parameters such as needle design, conditions of extraction and desorption were optimized along with the validation of the extraction and desorption efficiency. The optimal conditions were 30 min extraction at $50^{\circ}C$ and 2 min desorption at $240^{\circ}C$. The calibration curves showed good linearity with the suitable values of the coefficients of determination ($r^2$) greater than 0.99. The limits of detection for linalyl acetate, ${\beta}$-caryophyllene, linalool and (+)-limonene were 7.15, 9.04, 10.79 and 22.26 ng, respectively. Analytical recoveries were acceptable in the test samples, varying from 86.7% to 108.0%. The values of relative standard deviations for run to run showed range less than 0.9% while 3.9% through 7.2% for needle to needle. The proposed PEG-PDMS coating could be more suitable than PDMS coating to extract particular polar groups such as alcohols.

• Bulletin of the Korean Chemical Society
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• 제35권1호
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• pp.197-203
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• 2014

A rapid, accurate and precise method for the determination of 22 amino acids in Isatidis Radix by Hydrophilic Interaction Ultra-High-Performance Liquid Chromatography Coupled with Triple-Quadrupole Mass Spectrometry (HILIC-UPLC-MS/MS) was established. Chromatographic separation was carried out on a Acquity UPLC BEH Amide column ($2.1mm{\times}100mm$, $1.7{\mu}m$) with gradient elution of acetonitrile (containing 0.05% formic acid and 2 mM ammonium formate) and water (containing 0.15% formic acid and 10 mM ammonium formate) at a flow rate of 0.4 mL/min; Waters Xevo$^{TM}$ TQ worked in multiple reaction monitoring mode. All components were separated in 17 min. All calibration curves were linear ($R^2$ > 0.991) over the tested ranges. The limits of detection (LOD) and limits of quantitation (LOQ) for these compounds were 0.21-79.55 and 0.72-294.23 ng/mL, respectively. The average recoveries were in the range of 93.75-104.16% with RSD value less than 6.56%. Therefore, this method could be an alternative assay for the determination of 22 amino acids in Isatidis Radix due to its rapidness, sensitivity, less sample and solvent consumption.

• Bulletin of the Korean Chemical Society
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• 제34권11호
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• pp.3206-3210
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• 2013

This study focused on the matrix interference for the qualitative and quantitative analysis of inorganic arsenic species in seaweed by ion chromatography (IC) combined with inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The matrix of seaweed has a significant effect on the determination of inorganic arsenic species. In particular, the retention times of inorganic arsenic species in the in the standard solution were different from those in seaweed because of the matrix interference. Thus, it was not suitable to use the chromatographic method for the determination of the arsenic species in seaweed. We investigated an alternative method for the determination of inorganic arsenic species in seaweed. The method was applied for the seaweed samples such as laver, green laver, sea tangle and sea mustard. The sample extraction methods of the arsenic species were also investigated in this study.

• Bulletin of the Korean Chemical Society
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• 제23권6호
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• pp.861-865
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• 2002

A sensitive method for the determination of trace copper(II) after the preconcentration by adsorbing its cupferron complex onto microcrystalline benzophenone was developed.Several experimental conditions such as the pH of sample solution,concentration of cupferron, amount of benzophenone and atirring time were optimized. Trace compper(II) in 100mL solution was chelated with $3.0\;{\times}\;10^3$ M cupferron at pH 5.0. After 0.20g benzophenone, The benzophenone adsorbing Cu-cupferron complex was filtered and then Cu-cupferron complex was desorbed in 10 mL ethanol. Copper was determined by a flame atomic absorption spectrophotomethry. The interfering effects of diverse concomitant ions were investigated. Fe(III) interfered seriously with, but the interference by Fe(III) was completely eliminated by adjusting the concentration of copferron to $5.0\;{\times}\;10^3$ M. The detection limit of this method was 8.6${\times}$10 M(5.5 ngmL$^1$). Recoveries of 97% and 96% were obtained for Cu(II) in a stream water and a brass sample, respectively. Based on the results from the experiment. this proposed technique could be applied to the determination of copper(II) in real samples.

• Bulletin of the Korean Chemical Society
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• 제29권7호
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• pp.1323-1325
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• 2008

The acetylene black (AB) was dispersed into water in the presence of dihexadecyl hydrogen phosphate (DHP) via ultrasonication, resulting in a stable and well-distributed AB/DHP suspension. After evaporation of water, an AB/DHP composite film-modified electrode was prepared. The electrochemical responses of $K_3$[Fe$(CN)_6$] at the unmodified electrode, DHP film-modified electrode and AB/DHP film-modified electrode were investigated. It is found that the AB/DHP film-modified electrode possesses larger surface area and electron transfer rate constant. Furthermore, the electrochemical behaviors of 1-naphthylacetic acid (NAA) were examined. At the AB/DHP film-modified electrode, the oxidation peak current of NAA remarkably increases. Based on this, a sensitive and convenient electrochemical method was proposed for the determination of NAA. The linear range is in the range from $4.0 {\times} 10^{-8}\;to\;5.0 {\times} 10^{-6}$ mol $L^{-1}$, and the detection limit is $1.0 {\times} 10^{-8}$ mol $L^{-1}$. Finally, this new sensing method was employed to determine NAA in several soil samples.

• Bulletin of the Korean Chemical Society
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• 제25권8호
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• pp.1133-1136
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• 2004

The need for highly reliable methods for the determination of trace metals is recognized in analytical chemistry and environmental science. A method based on the cloud-point extraction (CPE) technique for the trace analysis of Pb and Cu in water samples is described in this study. The analytes in the initial aqueous solution are complexed with pyrogallol, and 0.1%(w/v) Triton X-114 is added as surfactant. Following phase separation at $50^{\circ}C$, based on the cloud point of the mixture and dilution of the surfactant-rich phase with acidified methanolic solution, the enriched analytes are determined by flame atomic absorption spectrometry. After optimization of the complexation and extraction conditions, the enrichment factors of Pb and Cu were found to be 72 and 85, respectively. Under optimum conditions, the preconcentration of 60 mL of samples in the presence of 0.1%(w/v) Triton X-114 permitted the detection of 0.4 ${\mu}gL^{?1}$ of Pb and 0.05 ${\mu}gL^{?1}$ of Cu. The proposed method was applied successfully to the determination of Pb and Cu in water samples.