• Korean Chemical Engineering Research
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• 제60권2호
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• pp.237-242
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• 2022

본 연구에서는 정제된(+)-dihydromyricetin로부터 잔류 용매를 효과적으로 제거할 수 있는 건조 방법을 개발하였다. 에탄올 전 처리를 통한 회전 증발(rotary evaporation)에 의해 잔류 아세톤 농도를 ICH 규정치(5,000 ppm) 이하로 효율적으로 제거하였다. 또한 잔류 에탄올 역시 물 첨가를 통한 회전 증발로 ICH 규정치(5,000 ppm)를 충족시켰으며 잔류 수분 함량은 4% 이내였다. 모든 건조 온도(35, 45, 55 ℃)에서 잔류 용매는 건조 초기에 급격히 제거되었으며 건조 효율은 건조 온도가 높을수록 증가하였다. 건조 메커니즘 조사 결과, 에탄올 전 처리에 의한 잔류 용매 제거는 아세톤-에탄올 혼합물의 높은 증기압과 아세톤-에탄올 간의 수소 결합과 연관됨을 알 수 있었다.

• Bulletin of the Korean Chemical Society
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• 제16권4호
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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.

• 대한약학회:학술대회논문집
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• 대한약학회 2002년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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• pp.212.2-212.2
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• 2002

• 분석과학
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• 제30권5호
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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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• 제34권2호
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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.

• 폴리머
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• 제38권5호
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• pp.645-649
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• 2014

사출성형품의 잔류응력 형성의 원인은 사출성형공정 중 재료가 받는 높은 온도변화와 전단응력이다. 케미컬 크랙킹 테스트는 잔류응력을 측정하는 방법 중의 하나이며 크랙은 잔류응력의 크기에 따라 형성된다. 본 연구에서는 시편이 받고있는 응력과 케미컬 크랙킹과의 관계를 연구하였다. 변형지그를 설계하고 이를 이용하여 시편에 변형을 주어 응력을 가하였다. 시편은 폴리카보네이트를 이용하여 핫 프레스로 제작하였고 시편의 제작 중에 형성된 잔류응력을 제거하기 위해 어닐링을 하였다. 시편을 변형지그에 고정시키고 시편에 크랙을 유도하기 위해 이를 솔벤트에 담궜다. 솔벤트는 tetrahydrofuran과 methyl alcohol을 이용하여 제조하였다. 시편에서 변형에 따라 응력이 증가할수록 크랙의 빈도수와 밀도가 증가하였다. 본 연구의 결과는 케미컬 크랙킹 방법으로 폴리카보네이트 사출성형품의 잔류응력을 정량적으로 측정하는데 활용될 수 있다.

• Carbon letters
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• 제18권
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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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• 제41권6호
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• pp.566-569
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• 2007

목적: 의약품의 FDA 개정에 따라 $[^{18}F]$FDG에 휘발성 유기 용매의 분석을 GC로 수행하였다. $[^{18}F]$FDG 주사액은 약 3개월에 걸쳐 생산하면서 정도관리를 수행하였다. 대상 및 방법: $[^{18}F]$FDG 주사액에 존재하는 잔류유기용매의 종류를 줄이기 위해 $[^{18}F]$FDG자동합성장치를 ethanol을 이용해 세정하였다. $[^{18}F]$FDG주사액은 FID가 장착된 Hewlett-Packard 6890 Gas Chromatograph로 분석을 수행하였다. 생산된 $[^{18}F]$FDG의 시료는 상온에서 밀봉된 Vial에 보관하였고 일주일 내에 분석하였다. 결과: $[^{18}F]$FDG 생성물에서 ethanol의 양은 $16.8\sim2762.8ppm$이 검출 되었고 acetonitrile의 양은 $2.3\sim327.6ppm$이 검출 되었다. 결론: 약 3개월간 생산한 $[^{18}F]$FDG 주사액 중에 ethanol과 acetonitrile잔류 용매를 측정해본 결과 USP 허용기준인 ethanol 5000 ppm과 acetonitrile 400 ppm 이하가 유지됨을 확인하였다.

• 한국전기전자재료학회논문지
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• 제22권11호
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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.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2012년도 제42회 동계 정기 학술대회 초록집
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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.