• 제목/요약/키워드: gravimetric preparation method #3

검색결과 7건 처리시간 0.021초

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

  • 김상문;이석문
    • 한국전기전자재료학회논문지
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    • 제25권6호
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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.

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

  • 유제이;이진복;김진석;김운중;홍기룡
    • 분석과학
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    • 제35권6호
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    • pp.249-255
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    • 2022
  • 본 연구에서는 기체 크로마토그래피-불꽃이온화검출기(GC-FID)를 이용한 고순도 질소의 새로운 순도분석법을 개발하였다. 고순도 질소에 존재할 수 있는 불순물인 일산화탄소(CO), 이산화탄소(CO2), 및 메탄(CH4)에 대한 3 µmol/mol 수준의 인증표준물질(Certified reference material, CRM)을 중량법을 이용하여 제조하였고, 이를 순도분석에 활용하였다. 개발된 순도분석법에서는 운반가스로 초고순도 질소와 순도분석 대상 질소를 사용하여, 제조된 인증표준물질의 기체 크로마토그래피에서 얻어지는 크로마토그램의 면적 값 차이를 비교함으로써 순도분석 대상 질소의 불순물을 정량 분석하였다. 순도분석 대상 질소로는 액체질소 및 제조사가 각기 다른 3곳의 고순도 질소를 사용하였다. 또한, 개발된 순도분석법의 유효성을 평가하기 위하여 순도분석 대상 질소 내 불순물의 물질량 분율을 기존 순도분석법과 비교하였다. 두 가지 순도분석법을 이용하였을 때 대상 질소 내 불순물의 물질량 분율이 불확도 (k = 2) 내에서 서로 일치함을 확인함으로써, 개발된 순도분석법이 유효함을 확인하였다.

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

  • 고인석
    • 생약학회지
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    • 제1권3호
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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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Bi$_{4}$Ti$_{3}$O$_{12}$ 박막의 제작과 그 특성에 관한 연구 (Preparation of a Bi$_{4}$Ti$_{3}$O$_{12}$ Thin Film and Its Electrical Properties)

  • 강성준;장동훈;민경진;김성진;정양희;윤영섭
    • 대한전자공학회논문지SD
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    • 제37권4호
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    • pp.7-14
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    • 2000
  • Bi/sub 4/Ti/sub 3/O/sub 12/ (BIT) 박막을 acetate 계 precursor 를 이용한 sol-gel 법으로 제작한 후, 구조적 및 전기적 특성을 조사하여 NVFRAM (Won-Volatile Ferroelectric RAM)으로의 응용가능성을 조사하였다. DT-TG (Differential Thermal-Thermal Gravimetric) 분석으로 drying 온도와 annealing 온도가 각각 400℃ 와 650℃ 인 BIT 박막의 열처리조건을 확립하였다. Pt/Ta/Sio/sub 2//Si 기판 위에 제작된 BIT 박막은 완전한 orthorhombic perovskite상을 가지며, 입자크기가 약 100nm 이고 표면 거칠기는 약 70.2Å 으로 비교적 치밀한 형상을 나타내었다. 10㎑ 의 주파수에서 비유전률과 유전손실은 각각 176 과 0.038 이었으며, 100 ㎸/cm 의 전기장에서 누설전류밀도는 4.71㎂/㎠ 이었다. ±250㎸/㎝ 에서 이력곡선을 측정한 결과, 잔류분극 (Pr)과 항전계 (Ec)는 각각 5.92μC/㎠ 과 86.3㎸/㎝ 이었다. BIT 박막에 ±5V 의 사각펄스를 인가하여 피로특성을 측정한 결과, 잔류분극은 초기값 5.92μC/㎠ 에서 10/sup 9/회에서는 3.95μC/㎠ 로 약 33% 감소하였다.

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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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    • 제25권11호
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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.

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

  • 강지환;김미언;김용두;이영우;이상일
    • 한국대기환경학회지
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    • 제32권3호
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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%.

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

  • 김용두;배현길;우진춘;이상일;오상협;이진홍
    • 분석과학
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    • 제30권5호
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    • pp.287-294
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    • 2017
  • 천연가스는 산업의 발전으로 인하여 수요가 계속 증가하고 있어 도입물량 부족 현상이 일어나 수급이 점차 불안정해질 것으로 예상된다. 액화천연가스 외에 파이프라인 천연가스 및 대체 천연가스등 다양한 형태의 가스 도입과 개발로 수요를 충당해야 할 필요성이 있다. 도입된 PNG의 성분과 농도를 정확하게 측정해야 한다. 이에 따른 천연가스 내에 있는 미량 성분인 탄화수소류($C_6-C_{10}$)의 정확한 측정이 요구되어 표준가스의 개발이 필수적이다. 이 연구에서 개발한 일차 표준물질에 대한 조성과 농도는 $10-30{\mu}mol/mol$의 헥산, 헵탄, 옥탄, 노난, 데칸이며 바탕가스는 메탄이다. 탄화수소류($C_6-C_{10}$)의 표준가스 제조는 각 성분 원료가스에 대한 순도분석이 완료된 가스를 ISO 6142에 근거하여 소급성이 있는 중량법으로 알루미늄 실린더에 제조하였다. 제조된 표준가스는 분석기로 표준가스간의 제조일치성, 실린더의 흡착성, 안정성 변화 및 불확도 평가를 하였다. 결과는 알루미늄 실린더에서 내부표면의 흡착 손실이 적고 장기 안정성이 매우 우수하다는 것을 알 수 있었고, 헥산, 헵탄, 옥탄, 노난, 데칸의 농도 $10-30{\mu}mol/mol$ 수준에서 불확도 0.79-1.63 %이내의 표준가스를 개발하였다.