• Journal of the Korean Chemical Society
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• v.10 no.1
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• pp.4-10
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• 1966

A new method of cobalt determination has been developed by employing ethylenediamine tetrabutyl acetate(EDTA-butyl ester) synthesized from EDTA and Butyl alcohol. The synthesized EDTA ester dissolved in butyl alcohol extracts various metal ions from aqueous solutions. Cobaltous ion extracted into organic phase containing EDTA ester to form Co (II)-EDTA butyl ester complex is back extracted into alkaline aqueous phase forming a stable pink colored complex of Co (III). The optimum condition for spectrophotometric determination of cobalt via the new complex has been established. The absorption peak occurs at 540$m{\mu}$ and Beer's law was obeyed over the concentration range of 0∼50 ${\mu}g/ml$ of cobalt.

• Proceedings of the Korean Vacuum Society Conference
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• 2016.02a
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• pp.427-427
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• 2016

Organic-inorganic hybrid perovskite have attracted significant attention as a new revolutionary light absorber for photovoltaic device due to its remarkable characteristics such as long charge diffusion lengths (100-1000nm), low recombination rate, and high extinction coefficient. Recently, power conversion efficiency of perovskite solar cell is above 20% that is approached to crystalline silicon solar cells. Planar heterojunction perovskite solar cells have simple device structure and can be fabricated low temperature process due to absence of mesoporous scaffold that should be annealed over 500 oC. However, in the planar structure, controlling perovskite film qualities such as crystallinity and coverage is important for high performances. Those controlling methods in one-step deposition have been reported such as adding additive, solvent-engineering, using anti-solvent, for pin-hole free perovskite layer to reduce shunting paths connecting between electron transport layer and hole transport layer. Here, we studied the effect of alkali metal halide to control the fabrication process of perovskite film. During the morphology determination step, alkali metal halides can affect film morphologies by intercalating with PbI2 layer and reducing $CH3NH3PbI3{\cdot}DMF$ intermediate phase resulting in needle shape morphology. As types of alkali metal ions, the diverse grain sizes of film were observed due to different crystallization rate depending on the size of alkali metal ions. The pin-hole free perovskite film was obtained with this method, and the resulting perovskite solar cells showed higher performance as > 10% of power conversion efficiency in large size perovskite solar cell as $5{\times}5cm$. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and inductively coupled plasma optical emission spectrometry (ICP-OES) are analyzed to prove the mechanism of perovskite film formation with alkali metal halides.

• Bulletin of the Korean Chemical Society
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• v.22 no.8
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• pp.821-826
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• 2001

Solvent sublation has been studied for the separation and determination of trace Zn(Ⅱ) and Pb(Ⅱ) in water samples. A synergy producing method was utilized to improve the efficiency of extraction in the sublation using an ion-pair of metal-naphth oate {M-(Nph)3- } complexes and tetra-n-butylammonium (TBA+ ) ion. After the M-(Nph)3- complexes were formed by adding 1-naphthoic acid to the sample solution, tetra-n-butylammonium bromide was added in the solution to form the ion-pair. And sodium lauryl sulfate (SLS) was added to make the ion-pair hydrophobic. The ion-pairs of the metal complexes were floated and extracted into methylisobutyl ketone (MIBK) from the aqueous solution by bubbling with nitrogen gas in a flotation cell. Metal ions in MIBK solution were measured by graphite furnace-AAS. Experimental conditions were optimized as follow so. After the pH of a 1.0 L water sample was adjusted to 5.0, 6.0 mL of 0.1 M 1-HNph and 10 mL of 0.03 M TBA-bromide were added to the sample to form ion-pairs, and 2.0 mL of 0.2%(w/v) SLS was added to make the ion-pairs hydrophobic. The solution was bubbled with 30 mL/min N2 gas for 5 minutes in a flotation cell. Linear calibration curves were obtained for the determination of Zn(Ⅱ) and Pb(Ⅱ) in several water samples. Reproducible results of showing a relative standard deviation of < 10% and recoveries of 80-100% could be obtained.

• Bulletin of the Korean Chemical Society
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• v.28 no.4
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• pp.553-556
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• 2007

We previously reported a 27.12 MHz inductively coupled plasma source at atmospheric pressure for atomic emission spectrometry based on polymer microchip plasma technology. For the PDMS polymer microchip plasma, molecular emission was observed, but no metallic detection was done. In this experiment, a lab-made electrothermal vaporizer (ETV) with tantalum coil was connected to the microchip plasma for aqueous sample introduction to detect metal ions. The electrode geometry of this microchip plasma was redesigned for better stability and easy monitoring of emission. The plasma was operated at an rf power of 30-70 W using argon gas at 300 mL/min. Gas kinetic temperatures between 800-3200 K were obtained by measuring OH emission band. Limits of detection of about 20 ng/mL, 96.1 ng/mL, and 1.01 μ g/mL were obtained for alkali metals, Zn, and Pb, respectively, when 10 μ L samples in 0.1% nitric acid were injected into the ETV.

• Analytical Science and Technology
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• v.20 no.6
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• pp.496-501
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• 2007

The 242.795 nm on ICP-AES for the gold analysis was the most sensitive wavelength which was also interfered severely by the spectra of other metal ions such as manganese, chromium, cobalt, and iron. In order to analyze the gold in ore, the gold must be separated from the interfering ions. The best solvent for separation of gold in ore solution was 10 % n-hexane contained MIBK mixed solvent. The gold recovery was 97.5 % from mixed metal solution contained about 2 M $HNO_3$ and 0.5 M HCl.

• Analytical Science and Technology
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• v.36 no.1
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• pp.1-11
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• 2023

A new, sensitive, and reliable flow injection methodology was investigated for the determination of lead ion (II) in vegetables' samples using a laboratory-prepared reagent 2-[(6-methoxy-2-benzothiazoly)azo]-4-methoxy phenol (6-MBTAMP). Infrared spectroscopy, UV-visible spectrophotometry, Energy dispersive X-ray spectroscopy (EDX), Elemental Analysis (CHN), nuclear magnetic resonance spectroscopy ¹HNMR, and ¹³CNMR techniques were used to characterize the reagent and lead (II) complex. The method is based on lead ion (II) reacting with the reagent (6-MBTAMP) in a neutral solution to produce a green-red complex with a maximum absorbance at 670 nm. The optimum conditions, such as flow rate, lead ion (II) volume, reagent volume, medium pH, reagent concentration, and reaction coil length were thoroughly examined. The limits of detection (LOD) and quantification (LOQ) were determined to be 0.621 mg·L^-1 and 2.069 mg·L^-1 , respectively, while Sandell's sensitivity was determined to be 0.345 ㎍·cm^-2.

• Analytical Science and Technology
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• v.24 no.4
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• pp.243-248
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• 2011

A selective determination method of mercury (II) ion in aqueous solution by luminol-based chemiluminescence system (luminol CL system) has been developed. Determination of metal ions such as copper (II), iron (III), chromium (III) ion in solution by the luminol CL system using its catalytic role in the reaction of luminol and hydrogen peroxide has been reported by several groups. In this study, the catalytic activity of mercury (II) ion in the reaction of luminol and hydrogen peroxide was observed by the enhanced CL intensity of the luminol CL system. Based on this phenomenon, experimental conditions of the luminol CL system were investigated and optimized to determine mercury (II) ion in aqueous solution. While mercury (II) ion in mixed sample solution containing mercury (I) and (II) ions highly enhanced the CL intensity of the luminol CL system, the mercury (I) ion could not enhanced the CL intensity. Thus selective determination of the mercury (II) ions in a mixture containing mercury (I) and (II) ions could be achieved. Each concentration of mercury (I) and (II) ions in aqueous solution can be obtained from the results of the CL method that give the concentration of only mercury (II) ion and the inductively coupled plasma (ICP) method that give the total concentration of mercury ions. On the optimized conditions, the calibration curve of mercury (II) ion was linear over the range from $1.25{\times}10^{-5}$ to $2.50{\times}10^{-3}M$ with correlation coefficient of 0.991. The detection limit of mercury (II) ion in aqueous solution was calculated to be $1.25{\times}10^{-7}M$.

• Applied Chemistry
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• v.15 no.2
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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.

• Bulletin of the Korean Chemical Society
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• v.23 no.10
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• pp.1381-1391
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• 2002

The solvent sublation using ion pairs of metal-2-naphthoate(2-HNph) and tetrabutyl ammonium ($TBA^+$) ion has been studied for the concentration and determination of ultra trace Bi(III), In(III) and Tl(Ⅲ) ions in water samples. The partition coefficients ($K_p$) and the extraction percentages of 2-HNph and the ion pairs to methyl isobutyl ketone (MIBK) were obtained as basic data. After the ion pair $TBA^+$·M$(Nph)_4^-$ was formed in water samples, the analytes were concentrated by the solvent sublation and the elements were determined by GF-AAS. The pH of the sample solution, the amount of the ligand and counter ion added and stirring time were optimized for the efficient formation of the ion pair. The type and amount of optimum surfactant, bubbling time with nitrogen and the type of solvent were investigated for the solvent sublation as well. 10.0 mL of 0.1 M 2-HNph and 2.0 mL of 0.1 M $TBA^+$ were added to a 1.0 L sample solution at pH 5.0. After 2.0 mL of 0.2%(w/v) Triton X-100 was added, the ion pairs were extracted into 20.0 mL MIBK in a flotation cell by bubbling. The analytes were determined by a calibration curve method with measured absorbances in MIBK, and the recovery was 80-120%.

• Bulletin of the Korean Chemical Society
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• v.15 no.12
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• pp.1035-1037
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• 1994

An ultrasensitive and selective stripping voltammetric scheme for the determination of rhodium is described. By the use of combined accumulation and catalytic effects in formaldehyde-hydrochloric acid medium, substantial improvement in the limit of detection can be obtained. Optimal experimental conditions were found to be 0.42 M hydrochloric acid solution containing 0.008${\%}$ formaldehyde, an accumulation potential of -0.70 V (vs. Ag/AgCl) and an accumulation time of 20 s. The stripping mode was differential pulse voltammetry. In these conditions the limit of detection lies at 2 ${\times}$ l0$^{-12}$ M (0.21 ppt). The relative standard deviation at 5 ${\times}$ l0$^{-11}$ M was 4.9${\%}$ (n=5). There were no serious interferences from other platinum group metal ions being the tolerable amounts more than 500 times that of rhodium.