• Title/Summary/Keyword: gravimetric preparation method #3

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Preparation and Characteristics of Heat-releasing Sheet Containing AlN(alunimum nitride) Powder (AlN 분말을 이용한 방열 Sheet의 제조와 그 특성)

  • Kim, Sang-Mun;Lee, Seok-Moon
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.25 no.6
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    • pp.431-434
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    • 2012
  • In this paper, heat-releasing sheets made of AlN powder and acryl binder as thermoset were prepared using tape casting method. The crystal structure and morphology, the thermal properties as nonvolatile solid content and thermal conductivity, and the surface resistance of heat-releasing sheet were measured by using X-ray diffractometer, field emission-scanning electron microscopy, thermo gravimetric analyzer and laser flash instrument, and surface resistance meter. It was proved that thermal conductivity is greatly affected by the content of binder in heat-releasing sheet. Superior thermal conductivity above 3.5 W/mK and suface resistance were obtained at heat-releasing sheet with above 90% of AlN powder.

Development of analysis method for high purity nitrogen using GC-FID/Methanizer (GC-FID/Methanizer를 이용한 고순도 질소의 순도분석법 개발)

  • Jei, You;Jin Bok, Lee;Jin Seog, Kim;Woonjung, Kim;Kiryong, Hong
    • Analytical Science and Technology
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    • v.35 no.6
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    • pp.249-255
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    • 2022
  • In this study, a new method for the analysis of high-purity nitrogen was developed. A gas chromatography-flame ionization detector (GC-FID) was used for purity analysis. Certified reference materials (CRMs) at a level of 3 µmol/mol of carbon monoxide (CO), carbon dioxide (CO2), and methane (CH4), which may exist in high-purity nitrogen, were prepared using the gravimetric method, and these CRMs were used for purity analysis. In this new method, ultra-high-purity and high-purity nitrogen were used as carrier gases. The impurities in high-purity nitrogen were quantitatively analyzed by comparing the differences in the area values of the GC chromatograms of the prepared CRMs. We purchased liquid nitrogen and three bottles of nitrogen gas, which were produced by three different manufacturers, using high-purity nitrogen. Furthermore, to validate the developed purity analysis method, the fraction of impurities in high-purity nitrogen was compared with the results of the typical purity analysis method. The comparison results were consistent within the expanded uncertainties (k = 2).

Study on Isolative Determination Methylephedrine Hydrochloride and Ephedrine Hydrochloride in the Mixed Preparation (혼합제제중 Methylephedrine Hydrochloride와 Ephedrine Hydrochloride의 분리정량에 관한 연구)

  • Ko, In-Suk
    • Korean Journal of Pharmacognosy
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    • v.1 no.3
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    • pp.93-99
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    • 1970
  • There have been reported by several workers for the isolation and determination of the amine derivatives as Metbylephedrine Hydrochloride and Ephedrine Hydrochloride adopting neutralization method, steam distillation method, non-aqous titration method, ion-exchange resin method, titration method after acetylation, colorimetric method, gravimetric method, iodine titration method and gas chromatography. Those methods mentioned in above, can be practically applied for the sample which is not mixed one mith the other amine compounds. Presently, it has not shown on the isolative determination of the mixed sample of amine derivatives. In this paper, it is discussed on the isolative determination of Methylephedrine Hydrochloride as the tertiary amine compound and Ephedrine Hydrochloride as the secondary amine compound. According to the results of the experiment, it could be summarized as follows: 1. There is no time-variation on the color reaction of Methylephedrine Hydrochloride and Ephedrine Hydrochloride with the color reagent, bromcresolgreen. And Methylephedrine Hydrochloride and Ephedrine Hydrochloride, respectively, can be determined spectrophotometrically by means oft his color reaction. 2. For the isolation of Methylephedrine Hydrochloride and Ephedrine Hydrochloride from the mixed sample, Methylephedrine Hydrochloride can be eluted by chloroform, while Ephedrine Hydrochloride by the mixed solvent of chloroform and ethylalcohol (2:1), from the celite column adsorbed at pH6.4 followed by extraction with ether undersodium hydroxide alkali re action. 3. When the sample is mixed with quinine hydrochloride, dihydrocodeine bitartate, and noscapine, these mixed compounds can be eliminated by means of stram distillation. 4. When the sample is mixed with chlorpheniramine maleate, dextromethorphan hydrobromide and diphenhydramine hydrochloride, the mixed compounds can be eliminated by means of steam distillation and celite adsorption column chromatography, In conclusion, the isolative determination method for Methylephedrine Hydrochloride and Ephedrine Hydrochloride studied in this paper, indicates with the excellent reproducibility and accuracy.

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Preparation of a Bi$_{4}$Ti$_{3}$O$_{12}$ Thin Film and Its Electrical Properties (Bi$_{4}$Ti$_{3}$O$_{12}$ 박막의 제작과 그 특성에 관한 연구)

  • Gang, Seong-Jun;Jang, Dong-Hun;Min, Gyeong-Jin;Kim, Seong-Jin;Jeong, Yang-Hui;Yun, Yeong-Seop
    • Journal of the Institute of Electronics Engineers of Korea SD
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    • v.37 no.4
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    • pp.7-14
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    • 2000
  • A Bi$_{4}$Ti$_{3}$O$_{12}$ (BIT) thin film is prepared by sol-gel method using acetate precursors and evaluated whether it could be applied to NVFRAM (Non-Volatile Ferroelectric RAM). The drying and the annealing temperature are 40$0^{\circ}C$ and $650^{\circ}C$, respectively and they are determined from the DT-TG (Differential Thermal-Thermal Gravimetric) analysis. The BIT thin film deposited on Pt/Ta/SiO$_{2}$/Si substrate shows orthorhombic perovskite phase. The grain size and the surface roughness are about 100 nm and 70.2$\AA$, respectively. The dielectric constant and the loss tangent at 10 KHz are 176 and 0.038, respectively, and the leakage current density at 100 ㎸/cm is 4.71 $mutextrm{A}$/$\textrm{cm}^2$. In the results of hysteresis loops measured at $\pm$250 ㎸/cm, the remanent polarization (Pt) and the coercive field (Ec) are 5.92 $\mu$C/$\textrm{cm}^2$ and 86.3 ㎸/cm, respectively. After applying 10$^{9}$ square pulses of $\pm$5V, the remanent polarization of the BIT thin film decreases as much as about 33% from 5.92 $\mu$C/$\textrm{cm}^2$ of initial state to 3.95 $\mu$C/$\textrm{cm}^2$.

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Preparation of Anatase TiO2 Thin Films with (OiPr)2Ti(CH3COCHCONEt2)2 Precursor by MOCVD

  • Bae, Byoung-Jae;Lee, Kwang-Yeol;Seo, Won-Seok;Miah, Md. Arzu;Kim, Keun-Chong;Park, Joon T.
    • Bulletin of the Korean Chemical Society
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    • v.25 no.11
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    • pp.1661-1666
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    • 2004
  • The reaction of titanium tetraisopropoxide with 2 equiv of N,N-diethyl acetoacetamide affords Ti($O^iPr)_2(CH_3COCHCONEt_2)_2$ (1) as colorless crystals in 80% yield. Compound 1 is characterized by spectroscopic (Mass and $^1H/^{13}C$ NMR) and microanalytical data. Molecular structure of 1 has been determined by a single crystal X-ray diffraction study, which reveals that it is a monomeric, cis-diisopropoxide and contains a six coordinate Ti(IV) atom with a cis($CONEt_2$), trans($COCH_3$) configuration (1a) in a distorted octahedral environment. Variable-temperature $^1H$ NMR spectra of 1 indicate that it exists as an equilibrium mixture of cis, trans (1a) and cis, cis (1b) isomers in a 0.57 : 0.43 ratio at -20$^{\circ}C$ in toluene-$d_8$ solution. Thermal properties of 1 as a MOCVD precursor for titanium dioxide films have been evaluated by thermal gravimetric analysis and vapor pressure measurement. Thin films of pure anatase titanium dioxide (after annealing above 500$^{\circ}C$ under oxygen) have been grown on Si(100) with precursor 1 in the substrate temperature range of 350- 500$^{\circ}$ using a bubbler-based MOCVD method.

Development of Primary Standard Gas Mixtures for Monitoring Monoterpenes (α-pinene, 3-carene, R-(+)-limonene, 1,8-cineole) Ambient Levels (at 2 nmol/mol) (대기 중 모노테르펜 (α-피넨, 3-카렌, R-리모넨, 1,8-시네올) 측정을 위한 혼합표준가스개발)

  • Kang, Ji Hwan;Kim, Mi Eon;Kim, Young Doo;Rhee, Young Woo;Lee, Sangil
    • Journal of Korean Society for Atmospheric Environment
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    • v.32 no.3
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    • pp.320-328
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    • 2016
  • Among biogenic volatile organic compounds (BVOCs) in the natural ecosystem, monoterpenes, along with isoprene, play important roles in atmospheric chemistry and make significant impacts on air pollution and climate change, especially due to their contribution to secondary organic aerosol production and photochemical ozone formation. It is essential to measure monoterpene concentrations accurately for understanding their oxidation processes, emission processes and estimation, and interactions between biosphere and atmosphere. Thus, traceable calibration standards are crucial for the accurate measurement of monoterpenes at ambient levels. However, there are limited information about developing calibrations standards for monoterpenes in pressured cylinders. This study describes about developing primary standard gas mixtures (PSMs) for monoterpenes at about 2 nmol/mol, near ambient levels. The micro-gravimetric method was applied to prepare monoterpene (${\alpha}$-pinene, 3-carene, R-(+)-limonene, 1,8-cineole) PSMs at $10{\mu}mol/mol$ and then the PSMs were further diluted to 2 nmol/mol level. To select an optimal cylinder for the development of monoterpene PSMs, three different kinds of cylinders were used for the preparation and were evaluated for uncertainty sources including long-term stability. Results showed that aluminum cylinders with a special internal surface treatment (Experis) had little adsorption loss on the cylinder internal surface and good long-term stability compared to two other cylinder types with no treatment and a special treatment (Aculife). Results from uncertainty estimation suggested that monoterpene PSMs can be prepared in pressured cylinders with a special treatment (Experis) at 2 nmol/mol level with an uncertainty of less than 4%.

Development of standard gas mixtures of hydrocarbons in methane contained in aluminum cylinders (알루미늄 실린더에서 혼합 탄화수소(C6-C10) 표준가스 개발)

  • Kim, Yong-Doo;Bae, Hyun-Kil;Woo, Jin-Chun;Lee, Sangil;Oh, Sang-Hyub;Lee, Jin Hong
    • Analytical Science and Technology
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    • v.30 no.5
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    • pp.287-294
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    • 2017
  • As the demand for natural gas increases with industrial development, the supply of natural gas is expected to become unstable with a shortage of imported natural gas. It is hence necessary to meet this demand by introducing and developing various types of natural gas, such as pipeline natural gas (PNG) and substituted natural gas (SNG), in addition to liquefied natural gas (LNG). The components included in PNG as well as their concentrations must be measured accurately, and a standard gas should be developed to accurately measure hydrocarbons ($C_6-C_{10}$), which are trace components included in natural gas. The components in the primary standard gas mixtures (PSMs) developed in the present study were hexane, heptane, octane, nonane, and decane with concentrations of $10-30{\mu}mol/mol$ with methane as the balance gas. Standard hydrocarbon ($C_6-C_{10}$) gas mixtures were prepared in aluminum cylinders by a gravimetric method with traceability following ISO 6142 with raw material gases, for which the purity of each component was analyzed completely. The prepared standard gas mixtures were analyzed by to evaluate the preparation consistency between the standard gas mixtures, the adsorbability of the cylinders, the variation of the stability, and the uncertainty. The results showed that aluminum cylinders have little adsorptive loss on their internal surfaces with excellent long-term stability. The developed standard gas mixture, containing hexane, heptane, octane, nonane, and decane with concentrations of $10-30{\mu}mol/mol$, showed an uncertainty in a range of 0.79 % - 1.63 %.