• Korean Chemical Engineering Research
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• v.60 no.2
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• pp.237-242
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• 2022

In this study, a drying method that can effectively remove residual solvent from (+)-dihydromyricetin was developed. Residual acetone concentration was efficiently removed below ICH-specified value (5,000 ppm) by simple rotary evaporation with ethanol pretreatment. In addition, the residual ethanol met the ICH-specified value (5,000 ppm) by simple rotary evaporation through the addition of water, and the residual moisture also met the specified value (<4%) for active pharmaceutical ingredients. At all the drying temperature (35, 45, and 55 ℃), a large amount of the residual solvent was initially removed during the drying, and the drying efficiency increased when increasing the drying temperature. Removal of residual solvent by ethanol pretreatment was shown to be related to high vapor pressure of acetone-ethanol mixture and hydrogen bonding between acetone and ethanol.

• Bulletin of the Korean Chemical Society
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• v.16 no.4
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• pp.326-331
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• 1995

Poly(enaryloxynitriles) containing Schiff bases were prepared from p-bis(1-chloro-2,2-dicyanovinyl)benzene (2) and various aromatic diols having Schiff base moiety by interfacial polymerization. The chemical structure of the polymers was confirmed through synthesis of their corresponding model compounds. All the polymers were soluble in polar aprotic solvents and their brittle films were cast from DMF solution. They showed a large exotherm around 340 ℃ attributable to the chemical change of dicyanovinyl group. Especially, curing of azomethine group was observed to occur at 390 ℃ by differential scanning calorimetry. According to the thermogravimetric analyses, they exhibited excellent thermal stability with 60-90% residual weight at 500 ℃ in nitrogen.

• Proceedings of the PSK Conference
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• 2002.04a
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• pp.212.2-212.2
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• 2002

• Analytical Science and Technology
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• v.30 no.5
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• pp.226-233
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• 2017

In general, quantitative chemical analysis in various areas including food, the environment, in vitro diagnostics, etc., requires traceability in order to increase the reliability of the measurements. Measurement traceability is a property of an unbroken chain of comparisons relating an instrument's measurements to SI units. Purity analysis is the first process for establishing traceability to SI units in chemical measurements. The purpose of this study is to develop and validate a method of purity assignment for establishing the traceability of $17{\beta}$-estradiol measurements in an in vitro diagnostics field. The establishment of this method is very important as it can be applied to the development of CRM and to the analysis of the purity of other hormones. The method of assignment of the purity of $17{\beta}$-estradiol was developed using the mass balance method and was validated through participation in an International comparison. In the mass balance method, impurities are categorized into four classes as follows: total related structure impurities, water, residual organic solvents, and nonvolatiles/inorganics. In this study, total related structure impurities were characterized by a gas chromatography-flame ionization detector (GC-FID) and a high-performance liquid chromatography-ultraviolet (HPLC-UV) detector, water content was determined by a Karl-Fisher coulometer, and total residual solvents and nonvolatiles/inorganics were checked simultaneously by thermogravimetric analysis (TGA). The purity of the $17{\beta}$-estradiol was 985.6 mg/g and the expanded uncertainty was 2.1 mg/g at 95% confidence. The developed method can be applied to the development of certified reference materials, which play a critical role in traceability.

• Bulletin of the Korean Chemical Society
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• v.34 no.2
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• pp.531-538
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• 2013

A mass balance method established in this laboratory was applied to determine the purity of an endosulfan-II pure substance. Gas chromatography-flame ionization detector (GC-FID) was used to measure organic impurities. Total of 10 structurally related organic impurities were detected by GC-FID in the material. Water content was determined to be 0.187% by Karl-Fischer (K-F) coulometry with an oven-drying method. Non-volatile residual impurities was not detected by Thermal gravimetric analysis (TGA) within the detection limit of 0.04% (0.7 ${\mu}g$ in absolute amount). Residual solvents within the substance were determined to be 0.007% in the Endosulfan-II pure substance by running GC-FID after dissolving it with two solvents. The purity of the endosulfan-II was finally assigned to be ($99.17{\pm}0.14$)%. Details of the mass balance method including interpretation and evaluating uncertainties of results from each individual methods and the finally assayed purity were also described.

• Polymer(Korea)
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• v.38 no.5
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• pp.645-649
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• 2014

The causes of residual stress in an injection molded part are high temperature variation and shear stress during molding process. Chemical cracking test is one of the methods of measuring residual stress and cracks are developed according to the degree of residual stress. In this study, the relationship between chemical cracking and exerted stress have been investigated. Deformation jig was designed and used to give a stress through deformation in a specimen. Specimens were molded by a hot press using polycarbonate (PC) and annealed to remove residual stresses in the specimens. Specimens were fixed in the deformation jig and immersed into the solvent to create cracks in the specimens. Solvents were prepared by using tetrahydrofuran and methyl alcohol. As stress accordance with the deformation in the specimen increased, the frequency and density of cracks in the specimen also increased. The results of this study can be used for the measurement of residual stress quantitatively in an injection molded PC product using a chemical cracking method.

• Carbon letters
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• v.18
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• pp.24-29
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• 2016

High pollutant-loading capacities (up to 319 times its own weight) are achieved by three-dimensional (3D) macroporous, slightly reduced graphene oxide (srGO) sorbents, which are prepared through ice-templating and consecutive thermal reduction. The reduction of the srGO is readily controlled by heating time under a mild condition (at 1 10⁻² Torr and 200℃). The saturated sorption capacity of the hydrophilic srGO sorbent (thermally reduced for 1 h) could not be improved further even though the samples were reduced for 10 h to achieve the hydrophobic surface. The large meso- and macroporosity of the srGO sorbent, which is achieved by removing the residual water and the hydroxyl groups, is crucial for achieving the enhanced capacity. In particular, a systematic study on absorption parameters indicates that the open porosity of the 3D srGO sorbents significantly contributes to the physical loading of oils and organic solvents on the hydrophilic surface. Therefore, this study provides insight into the absorption behavior of highly macroporous graphene-based macrostructures and hence paves the way to development of promising next-generation sorbents for removal of oils and organic solvent pollutants.

• Nuclear Medicine and Molecular Imaging
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• v.41 no.6
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• pp.566-569
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• 2007

Purpose: Analysis of volatile organic solvents in 2-deoxy-2-$[^{18}F]$ fluoro-D-glucose ($[^{18}F]$FDG) preparations was performed by gas chromatography (GC), in accordance with USP. Materials and Methods: Analyses were carried out on a Hewlett-Packard 6890 gas chromatography equipped with an FID. Results: We determined the amounts of ethanol and acetonitrile on every batch of our routine $[^{18}F]$FDG preparations, ranging between 5000 ppm and 100 ppm. In our routine preparation of $[^{18}F]$FDG, the amount of acetonitrile and ethanol in the final product were well below the maximum allowable limit described in the USP. Conclusion: Our $[^{18}F]$FDG preparations were in accordance with the suggested USP maximum allowable levels of the quality control analysis of volatile organic compounds.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.22 no.11
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• pp.961-968
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• 2009

In this work, transparent conductive oxide(TCO) films such as $In_2O_3-SnO_2$(ITO) and $In_2O_3-ZnO$(IZO) were prepared on polyethylene naphthalene(PEN) and glass substrates by using rf-magnetron sputtering system. The TCO films deposited on PEN substrate show very poor conductivity as compared to that of the TCO films deposited on glass substrates. From the results of the residual gas analysis(RGA) test, this poor stability of plastic substrate is presumed to be caused by the deteriorated adhesion between the TCO films and the plastic substrate due to outgassing from the plastic substrate during deposition of TCO films. From our experiment, it is found that the vaporization of some defects in the plastic substrates deteriorate the adhesion of the TCO films to the plastic substrate, because the most plastic substrates containing the water vapor and/or other adsorbed particles such as organic solvents. Mixing of these gases vaporized in the sputtering process will also affect the electrical property of the deposited TCO films. Inorganic thin composite $(SiO_2)_{40}(ZnO)_{60}$ film as a gas barrier layer is coated on the PEN substrate to protecting the diffusion of vapors from the substrate, so that the TCO films with an improved quality can be obtained.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.02a
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• pp.561-561
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• 2012

Graphene, two dimensional single layer of carbon atoms, has tremendous attention due to its superior property such as fast electron mobility, high thermal conductivity and optical transparency, and also found many applications such as field-effect transistors (FET), energy storage and conversion, optoelectronic device, electromechanical resonators and chemical sensors. Several techniques have been developed to form the graphene. Especially chemical vapor deposition (CVD) is a promising process for the large area graphene. For the electrically isolated devices, the graphene should be transfer to insulated substrate from Cu or Ni. However, transferred graphene has serious drawback due to remaining polymeric residue during transfer process which induces the poor device characteristics by impurity scattering and it interrupts the surface functionalization for the sensor application. In this study, we demonstrate the characteristics of solution-gated FET depending on the removal of polymeric residues. The solution-gated FET is operated by the modulation of the channel conductance by applying a gate potential from a reference electrode via the electrolyte, and it can be used as a chemical sensor. The removal process was achieved by several solvents during the transfer of CVD graphene from a copper foil to a substrate and additional annealing process with H2/Ar environments was carried out. We compare the properties of graphene by Raman spectroscopy, atomic force microscopy(AFM), and X-ray Photoelectron Spectroscopy (XPS) measurements. Effects of residual polymeric materials on the device performance of graphene FET will be discussed in detail.