• Bulletin of the Korean Chemical Society
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• v.24 no.12
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• pp.1731-1736
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• 2003

The reaction of ${\alpha}$-Benzilmonoxime with palladium(II) produces a green complex in triton X-100 micellar media. Palladium has been determined using zero and first derivative spectrophotometric methods. The absorbances of Pd(II)- ${\alpha}$--benzilmonoxime complex at 441.8 and 677.0 nm in 0.10 M perchloric acid solution were monitored and linear working ranges of 0.3-12.0 and 0.7-20 ${\mu}$g mL$^{-1}$ with detection limits of 0.07 and 0.10 ${\mu}$g $mL^-1$ were obtained, respectively. Also, recoveries in the range of 92.8 to 100.1% and relative standard deviations in the range of 0.4 to 7.1% were obtained. First derivative spectrophotometry has also been applied for palladium determination under the optimum condition. The linear dynamic range of 0.2-24.0 ${\mu}$g $mL^{-1}$ palladium with relative standard deviations of 0.6-6.9% and recoveries in the range of 94.9-102.5% has been obtained by first derivative spectrophotometry. The method shows high selectivity because of the high concentration of acid used, which prevents formation of complexes of ${\alpha}$--benzilmonoxime with the other cations. The palladium complex formed was stable at least one day. The method was successfully applied to the determination of palladium in some synthetic palladium alloys and palladium-charcoal powder.

• Bulletin of the Korean Chemical Society
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• v.24 no.1
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• pp.27-31
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• 2003

A Polythiophene-quinoline/glassy carbon (PTQ/GC) modified electrode was developed for the determination of trace mercury in industrial waste water, natural water, soil, and other media. The electrode was prepared by the cyclic voltammetric polymerization of thiophene and quinoline on glassy carbon (GC) electrode by the potential application from -0.6 V to +2.0 V (50 mV/sec) in a solution of 0.1 M thiophene, quinoline and tetrabutyl ammonium perchlorate (TBAP) in acetonitrile. Optimum thickness of the polymer membrane on the GC electrode was obtained with 20 repeated potential cyclings. The redox behavior of Cu(Ⅱ) and Hg(Ⅱ) were almost identical on this electrode. The addition of 4-(2-pyridylazo)resorcinol (PAR) to the solution containing Cu(Ⅱ) and Hg(Ⅱ) allowed the separation of the components due to the formation of the Cu(Ⅱ)-PAR complex reduced at -0.8V, which was different from the Hg(Ⅱ) reduced at -0.5 V on a saturated calomel electrode (SCE). The calibration graph of Hg(Ⅱ) shows good linear relationship with the correlation factor of 0.9995 and the concentration gradient of 0.33 ㎂/㎠/ppb down to 0.4 ppb Hg. The method developed was successfully applied to the determination of mercury in samples such as river, waste water, and sea water.

• Bulletin of the Korean Chemical Society
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• v.25 no.12
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• pp.1877-1880
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• 2004

The simple and convenient determination of trace Hg(II) with its 2-mercaptobenzothiazole (MBT) complex in cetyltrimethylammonium bromide (CTAB) media has been studied. The UV-visible spectrum of Hg(II)-MBT complex in CTAB media had a good sensitivity and reproducibility. The Hg(II)-MBT complex in CTAB solution was very stable at pH 10.0 and could be quantitatively complexed if MBT were added to the sample solution more than 10 equivalent of Hg(II). The optimum concentration of CTAB was 0.001%. The calibration curve of Hg(II)-MBT complex with good linearity ($R^2$ = 0.9985) was obtained at the concentration range between $1.0{\times}10^-7$ and $1.0{\times}10^-5$ M in 0.001% CTAB media. The detection limit was $3.1{\times}10^-8$ M (6.2 ng m$L^{-1}$). Hg(II) in the synthetic samples and in the wastewater of the university's wastewater tank and the industrial wastewater tank could also be determined. Based on the experimental results, this proposed technique could be applied to the simple and convenient determination of trace Hg(II) in real samples.

• Bulletin of the Korean Chemical Society
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• v.32 no.10
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• pp.3561-3565
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• 2011

A rapid and inexpensive method was developed for the determination of trace silver in geological samples by using sulfhydryl cotton coupled with ICP-MS. The interferences such as $^{90}Zr$, $^{92}Mo$ and $^{93}Nb$ on silver were investigated in detail. Sulfhydryl cotton was found to be an effective adsorbent for separation of interferences for Ag in the solutions. Excellent agreements with the certified values were obtained for all the certified reference materials. The memory effects of Ag by ICP-MS were examined by using different agents, including water, nitric acid, and HCl-thiourea to all standards/samples. The agents also acted as cleansing solutions. A combination of HCl with thiourea gave the minimum memory effect. For comparison of results, a proposed Chinese Geology Survey procedure DC-ARC-AES and a direct determination pretreatment method of ICP-MS (water bath- auqa regia digestion) were studied. Under optimal conditions, the detection limits of our method for $^{107}Ag$ and $^{109}Ag$ were 1.2 ng/g and 1.3 ng/g, which offered much better accuracy for some difficult analysis geological samples such as GBW07604, GBW07605.

• Bulletin of the Korean Chemical Society
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• v.31 no.4
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• pp.845-849
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• 2010

A gold nanoparticles modified carbon paste electrode (GN-CPE) has been used for the determination of atenolol (ATN) in drug formulations by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and chronocoulometric methods. The results revealed that the modified electrode shows an electrocatalytic activity toward the anodic oxidation of atenolol by a marked enhancement in the current response in buffered solution at pH 10.0. The anodic peak potential shifts by -80.0 mV when compared with the potential using bare carbon paste electrde. A linear analytical curve was observed in the range of $1.96\;{\times}\;10^{-6}$ to $9.09\;{\times}\;10^{-4}\;mol\;L^{-1}$. The detection limit for this method is $7.3\;{\times}\;10^{-8}\;mol\;L^{-1}$. The method was then successfully applied to the determination of atenolol in tablets and human urine. The percent recoveries in urine ranged from 92.0 to 110.0%.

• Bulletin of the Korean Chemical Society
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• v.30 no.7
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• pp.1516-1520
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• 2009

A sensitive technique for the determination of trace Co(II) in various samples after column preconcentration by adsorbing onto silica gel loaded with 1-nitroso-2-naphthol was developed. Several experimental conditions, such as pH of sample solution, the amount of silica gel loaded with 1-nitroso-2-naphthol, the flow rate for adsorption and so forth, were optimized. The interfering effects of diverse concomitant ions were investigated. Fe(III) interfered with more than any other ions, but the interference by Fe(III) was completely eliminated by adjusting the amount of silica gel loaded with 1-nitroso-2-naphthol to 0.30 g. The dynamic range, the correlation coefficient ($R^2$), and the detection limit obtained by the proposed technique were 3.0-140.0 ng m$L^{-1}$, 0.9942, and 1.81 ng m$L^{-1}$, respectively. For validating the technique, the aqueous samples (tap water, reservoir water, stream water, and wastewater) and the plastic samples were used as real samples. Recovery yields of 93.0-107.0% were obtained. These measured data were not different from ICP-MS data at the 95% confidence level by F test. Based on the results of the experiment, it has been found that the proposed technique can be applied to the determination of Co(II) in various real samples.

• Bulletin of the Korean Chemical Society
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• v.28 no.2
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• pp.183-187
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• 2007

A simple and sensitive extractive spectrophotometric method has been described for the determination of buprenorphine either in raw material or in pharmaceutical formulations. The developed method is based on the formation of a colored ion-pair complex (1 : 1 drug/dye) of buprenorphine and bromocresol green (BCG) in buffer pH 3 and extracting in chloroform. The extracted complex shows absorbance maxima at 415 nm. Beer's law is obeyed in the concentration range of 1.32-100.81 μ g mL-1. The proposed method has been applied successfully for the determination of drug in commercial sublingual tablets and injectable dosage form. No significant interference was observed from the excipients commonly used as pharmaceutical aids with the assay procedure.

• Bulletin of the Korean Chemical Society
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• v.28 no.2
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• pp.246-250
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• 2007

The crude extract of kohlrabi (Brassica oleracea gongylodes) was prepared as a rich source of peroxidase and its enzymatic and specific activities in the presence of cross-linked polyvinylpyrrolidone as a stabilizer were determined. This extract was used to catalyze the oxidation of thiamine in the presence of hydrogen peroxide to thiochrome at pH 8.0. Thiochrome shows strong fluorescence at 436 nm with excitation at 370 nm. Based on the obtained results, a sensitive and simple spectrofluorimetric method was developed for the determination of thiamine. In the optimum conditions, the calibration graph was linear from 2 × 10-7 to 1 × 10-4 mol L-1, with a detection limit of 6.2 × 10-8 mol L-1. The relative standard deviation (RSD) was 1.2% for 5 × 10-6 mol L-1 thiamine. The method was successfully applied to the determination of thiamine in vitamin B1 and vitamin B complex tablets and vitamin B complex syrup.

• Bulletin of the Korean Chemical Society
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• v.29 no.9
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• pp.1774-1780
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• 2008

New PVC based polymeric membrane electrodes (PME) and coated glassy carbon electrodes (CGCE) based on synthesized Schiff base complexes of Co(III); [Co(Salen)$(PBu_3)_2$]$ClO_4$, [Co($Me_2$Salen)$(PBu_3)_2$]$ClO_4$, [Co(Salen)$(PBu_3)H_2O$]$ClO_4$; as anion carriers for potentiometric determination of $ClO_4\;^-$were studied. The PME and also CGCE electrodes prepared with [Co(Me2Salen)$(PBu_3)_2$]$ClO_4$ showed excellent response characteristics to perchlorate ions. The electrodes exhibited Nernstian responses to $ClO_4\;^-$ ions over a wide concentration range with low detection limits ($1.0 {\times} 10^{-6}\;mol\;L^{-1}$ for PME and $9.0 {\times} 10^{-7}\;mol\;L^{-1}$ for CGCE). The electrodes possess fast response time, satisfactory reproducibility, appropriate lifetime and, most importantly, good selectivity toward $ClO_4\;^-$ relative to a variety of other common inorganic anions. The potentiometric response of the electrodes is independent of the pH in the pH range 2.5-8.5. The proposed sensors were used in potentiometric determination of perchlorate ions in mineral water and urine samples. The interaction of the ionophore with perchlorate ions was shown by UV/Vis spectroscopy.

• Bulletin of the Korean Chemical Society
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• v.33 no.6
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• pp.1967-1971
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• 2012

A hexavalent chromium (Cr (VI)) is one of the hazardous substances regulated by the RoHS. The determination of Cr (VI) in various polymers and printed circuit board (PCB) has been very important. In this study, the three different analytical methods were investigated for the determination of a hexavalent chromium in Acrylonitrile Butadiene Styrene copolymer (ABS) and PCB. The results by three analytical methods were obtained and compared. An analytical method by UV-Visible spectrometer has been generally used for the determination of Cr (VI) in a sample, but a hexavalent chromium should complex with diphenylcarbazide for the detection in the method. The complexation did make an adverse effect on the quantitative analysis of Cr (VI) in ABS. The analytical method using diphenylcarbazide was also not applicable to printed circuit board (PCB) because PCB contained lots of irons. The irons interfered with the analysis of hexavalent chromium because those also could complex with diphenylcarbazide. In this study, hexavalent chromiums in PCB have been separated by ion chromatography (IC), then directly and selectively detected by inductively coupled plasma atomic emission spectrometry (ICP-AES). The quantity of Cr (VI) in PCB was 0.1 mg/kg.