• Title/Summary/Keyword: NMR 분석

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Comparative analysis of glycerin in cosmetics by LC/MS and 1H NMR (LC/MS와 1H NMR을 이용한 화장품속의 글리세린 비교분석)

  • Park, Gyo-Beom;Park, Chan Jo;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.20 no.5
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    • pp.400-405
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    • 2007
  • The comparative analysis of glycerin in cosmetic samples was carried out by LC/MS and $^1H$ NMR spectrometry. For the LC/MS analysis, aqueous solution was controlled in strong basic condition with sodium hydroxide, and benzoyl chloride was added to the solution for the derivatization of glycerin. The derivative was extracted using pentane and analyzed by the LC/MS. For the $^1H$ NMR analysis, sample was directly dissolved in $D_2O$ solvent without pretreatment. The quantitative analysis of glycerin was done by $^1H$ NMR ERETIC method. The analysis results of LC/MS and $^1H$ NMR showed that the calibration curves were a good linearity with $r^2=0.9991$ in the range of 0.1 to $10{\mu}g/mL$ and $r^2=1$ in the range of 25 to $500{\mu}g/mL$, respectively.

Analytical Study for an Acrylic Coating (아크릴 코팅의 성분 분석 연구)

  • Kim, Seog-Jun
    • Analytical Science and Technology
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    • v.17 no.2
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    • pp.98-107
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    • 2004
  • In this study, $^1H$ NMR spectroscopy and HPLC were used to identify the type and quantity of each component in an acrylic coating materials applied for an automotive part. By the $^1H$ NMR analysis, it was found that this acrylic coating contained about 88.40 wt% of poly methyl methacrylate (PMMA), 7.05 wt% of methyl methacrylate (MMA), and 2.36 wt% of allyl methacrylate. Polymer additives such as a benzotriazole light stabilizer (Hisorb 328), an oxanilide light stabilizer, butylated hydroxy toluene (BHT), and dimethyl phthalate (DMP) were also identified and measured quantitatively from the $^1H$ NMR spectra. However, only two light stabilizers were identified by reverse phase (RP) HPLC analysis using Bondapak C18 column, methanol mobile phase, and a PDA (Photodiode array) detector. The contents of two light stabilizers in the acrylic coating were measured by a quantitative analysis through UV-Vis spectroscopy and compared with the NMR data. The analytical informations from $^1H$ NMR spetra were better than those from HPLC-PDA plot.

새로운 분석법으로서의 2D NMR 분광법에 관한 이론적 배경 및 고찰

  • Kim, Taek-Je;Jeong, Min-Hwan;Lee, Gang-Bong
    • Analytical Science and Technology
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    • v.5 no.2
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    • pp.1096-1113
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    • 1992
  • 분자구조, 동력학, 그리고 분자들의 화학분응에 관한 정확한 지식은 분자들의 기능과 성질을 이해하는 데 중요한 정보를 제공한다. 2D NMR 분광법의 개발은 용액상의 분자들에 관한 이러한 의문을 해결하는 데 결정적인 역할을 하게 되었다. 그동안 아주 다양한 NMR기술들이 개발되어 왔으며 현재 그들에 대한 이용이 활발하게 진행되고 있다. 그러나 성공적인 2D NMR 분광법의 적용을 위해서는 적당한 기계뿐만 아니라 실험실의 정확한 선택 및 최적 조건의 변수들을 선택해야 하며 스펙트럼의 세밀하고도 정확한 해석을 필요로 한다. 곱연산자 방식(product operator formalism)의 도입은 펄스 FT NMR 분광학을 정성, 정량적으로 이해하도록 하는 것을 가능케 했으며, 이번 해설은 연속적으로 주어지는 펄스의 이해를 위해서 필요로 하는 상의 순환(phase cycle) 및 곱연산자 방식을 이용하여 다양한 2D NMR 기술의 이해를 돕고, 분석기기로서 2D NMR 분광법이 널리 사용 및 활용되어지고자 하는 데 목적이 있다.

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Investigation of Gas Hydrate Crystallization and Structure Analysis by $^{13}C$ NMR with Surfactant (계면활성제 첨가에 따른 가스하이드레이트 생성 결정과 $^{13}C$ NMR 구조 분석 고찰)

  • Cho, Byoung-Hak;Lee, Young-Chul;Shin, Myung-Uk;Lee, Sung-Han
    • 한국신재생에너지학회:학술대회논문집
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    • 2006.06a
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    • pp.395-398
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    • 2006
  • 동일한 조건에서 순수한 물과 계면활성제인 DBS(dodecyl bezebe sulfonic acid) 25ppm을 첨가한 물에 대해 천연가스 하이드레이트를 제조시 가스의 함유량은 각각 80배와 160배로 2배의 차이가 발생한다. 이에 대해 본 연구에서는 결정 생성 형태의 관찰 및 $^{13}C$ NMR을 사용한 분광학적 구조 분석으로부터 이의 원인을 찾고자 하였다. 순수한 물과 DBS를 미량 함유한 물을 사용하여 whiskery 결정을 생성시킨 결과, 순수한 물을 사용한 경우보다 섬유 다발 형태가 매우 활발한 형태의 결정 형태로 가스하이드 레이트가 생성됨을 알 수 있었다. 또한 400MHz의 NMR을 사용한 분광학적 구조 분석으로부터 천연가스하이드레이트는 구조-I과 구조-II가 혼재된 결정 구조를 이루고 있음을 알 수 있었다. 또한 DBS를 함유한 물에 의해 제조된 천연가스하이드레이트는 arge cage를 많이 생성시키는 역할을 하는 분석 결과를 보였고 이것이 가스 함유량을 증대시키는 원인 중의 하나임을 알 수 있었다.

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FT-NMR as an analytical tool for identification of inert materials in crop protection products (농약제품분석의 정성분석도구로서 FT-NMR)

  • Choi, Dal-Soon;Kyung, Suk-Hun;Hong, Su-Myeong;Jin, Yong-Duk;Lee, Hea-Keun;Kim, Jin-Hwa;Ryu, Gab-Hee
    • The Korean Journal of Pesticide Science
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    • v.8 no.2
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    • pp.88-94
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    • 2004
  • In order to evaluate NMR spectrometer as the analytical tool for identification of individual adjuvant in crop protection products, the standard sample of individual adjuvant was analyzed by NMR spectrometer and then the formulation of crop protection products was also analyzed. Almost polymer system of surfactant was a co-polymer and there was an excess of ethylene. The most intense signal comes from long polyethylene blocks, 70.5 ppm. The carbonyl groups of ester group resonate at 173.5 ppm. Analytical sample was prepared in NMR tube without extraction, cleanup, concentration, or chromatographic separation. Identification of individual adjuvant in crop protection products was conducted by comparison of sample and reference spectra. NMR spectrometer was useful to analyze adjuvant in crop protection products without preparation process.

Application of Deuterium NMR Analysis for the Differentiation of Korean and Foreign Liquors (중수소 핵자기 공명을 이용한 외국 술과 국산 술의 비교 분석)

  • Han, Gee-Chung;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.13 no.1
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    • pp.127-129
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    • 2000
  • The $^2H$ NMR analysis was used to determine the relative deuterium contents at the position of methyl and methylene in ethyl alcohols. Four different liquors manufactured in Korea clearly showed different R values from those of foreign liquors. These R values for the Korean liquors could be used to distinguish adulteration.

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Determination of phosphorous in lubricating oil by XRF and NMR methods (XRF 및 NMR 법에 의한 윤활유 중의 인 함량 비교분석 연구)

  • Lim, Heon-Sung;Han, Gee-Chung;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.18 no.2
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    • pp.168-172
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    • 2005
  • A comparison study of XRF and $^{31}P$-NMR method for the analysis of phosphorous in lubricating oil has been described. Pure oil and water were used for the observation of matrices effect variation by different analytical methods. Quantitative analysis was carried out by XRF and $^{31}P$-NMR using real samples. Significant difference is observed from the slopes on the calibration curves by the XRF due to the matrices (water: 124.0, oil: 276.6). While the result obtained from XRF showed a large matrix effect, the slopes obtained from $^{31}P$-NMR results of two different matrices, however, are in good agreement ranged of ${\pm}9%$ (water: 4.9, oil: 5.3).

Synthesis and Analysis of 6,6-dichlorobicyclo[3, 1, 0]hexane-3-carboxylic acid (6,6-Dichlorobicyclo[3, 1, 0]hexane-3-carboxylic acid의 합성과 분석)

  • Lee, Kwang-Soo;Yang, Jae-Kun
    • Analytical Science and Technology
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    • v.14 no.1
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    • pp.1-7
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    • 2001
  • 6,6-Dichlorobicyclo[3, 1, 0]hexane-3carboxylic acid was synthesized by dichlorocarbene addition into 3-cyclopentenecarboxylic acid using BTEA.Cl as phase transfer catalyst. $^1H$ NMR $^{13}C$ NMR data analyst showed that this compound had boat-like conformation and carboxyl group existed as trans form.

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$A^{13}$ CNMR Determination of Monomer Composition in EP Copolymers, EPB and EPDM Terpolymers (EP 공중합체, EPB 및 EPDM 삼중합체의 단량체조성에 관한 $^{13}C$-NMR 분석)

  • Lee, Kang-Bong;An, Seong-Uk;Rhee, Jae-Seong;Kweon, Jeehye;Choi, Young-Sang
    • Analytical Science and Technology
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    • v.7 no.1
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    • pp.91-102
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    • 1994
  • The monomer compositions in a series of propylene heterophasic copolymer, propylene random copolymer, propylene random terpolymer and ethylene-propylene-ENB terpolymer have been determined from $^{13}C-NMR$ spectra. The simplified and highly resolved $^{13}C-NMR$ spectra made it possible to assign unambiguousely and calculate the monomer composition. A complete sets of NMR chemical shift assignments and the way to measure the quantity of monomer are newly given in diverse polymers. Furthermore complete dyad, triad, tetrad and pentad distributions have been able to be determined. These NMR quantitative analytical results for monomer compostition have consistent with those from Infrared spectral data.

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