• Title/Summary/Keyword: NMR spectrometer

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The Synthesis of Green-Sensitizing Dye for Photographic Emulsion (사진유제용 Green-Sensitizing Dye의 합성)

  • Kim, Yeoung-Chan
    • Journal of the Korean Applied Science and Technology
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    • v.14 no.2
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    • pp.57-64
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    • 1997
  • The symmetric naphthothiazolo carbocyanine is of industrial importance as green-sensitizing dye in the spectral sensitization of emulsion microcrystals in negative film-making. In this study, green-sensitizing dye was prepared by the reaction of 2-methyl-3-sulfopropyl-5-phenyl-benzoxazolium(inner salt) with triethyl orthoacetate in the presence of triethylamine. The product was identified by using various analytical tools such as Elemental analyzer, IR spectrophotometer, UV-Vis spectrophotometer, $^1H$-NMR spectrometer, TGA and DSC. The maximum absorption peak in methanol solvent was 502nm. Therefore, it was concluded that benzoxazolo carbocyanine dye can be used as green-sensitizing dye for the spectral sensitization of photographic emulsion.

Screening of Inhibitory Effect of Edible Mushrooms on Tyrosinase and Isolation of Active Component (한국산 식용버섯류의 Tyrosinase 활성 저해 검색 및 그 유효성분 분리)

  • 박영현;장성근
    • Journal of Food Hygiene and Safety
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    • v.12 no.3
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    • pp.195-199
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    • 1997
  • For the purpose of isolation and screening of tyrosinase inhibitory activity from edible mushrooms, Pleurotus ostreatus, Auricularia auricula-Judae, Umbilicaria esculenta, Agaricus bisporus, Flammuline velutipes, Lentinus edodes, Ganoderma lucidum, and Coriouls versicolor were examined by tracing inhibitory activities against tyrosinase, utilizing L-3,4-dihydroxyphenylalanine (L-DOPA) as a substrate. Among the eight edible mushrooms tested, Umbilicaria esculenta showed potent enzyme inhibitory activities above 7804% against tyrosinase in ethylacetate (EtOAc) extracts. Ganoderma lucidum and Agaricus bisporus showed inhibitory activities of 67.3% and 51.5% in water extracts. EtOAc extracts of Umbilicaria esculenta was fractionated from silicagel column chromatography and one fraction showed the most inhibitory activity of 60.9%. The three bands (Rf=0.38, 0.27, 0.19) were isolated from preparative TLC of the fraction for purification and identified as mixtures of orsellinate, methyl orsellinate, methyl lecanorate, and methyl gyrophorate by high pressure liquid chromatography (HPLC), ultravisible spectrophotometer (UV), mass spectrophotometer (Mass), nuclear magnetic resonance spectrometer (NMR).

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Synthesis of 9-Phenyl-5,5'-Diphenyl-3,3'-Bis(3-Sulfopropyl)-Benzoxazolo Carbocyanine Triethyl Ammonium Salt (9-Phenyl-5,5'-Diphenyl-3,3'-Bis(3-Sulfopropyl)-Benzoxazolo Carbocyanine Triethyl Ammonium Salt의 합성)

  • Kim, Yeoung-Chan
    • Journal of the Korean Applied Science and Technology
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    • v.25 no.2
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    • pp.226-231
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    • 2008
  • In this study, benzoxazolo carbocyanine is of industrial importance as green-sensitizing dye in the spectral sensitization. Sensitizing dye was prepared by the reaction of 2-methyl-3-sulfopropyl-4,5-benzoxazolium (inner salt) with triethyl orthobenzoate in the presence of triethylamine. The product was identified by using various analytical tools such as elemental analyzer, IR spectrophotometer, UV-Vis spectrophotometer, $^1H$-NMR spectrometer, TGA and DSC. The maximum absorption peak in methanol solvent was 507 nm. Therefore, it was concluded that benzoxazolo carbocyanine dye can be used as sensitizing dye for the spectral sensitization of photographic emulsion and color cosmetics.

Synthesis of 9-Ethyl-3,3'-Bis(3-sulfopropyl)-4,5,4'5'-Naphthothiazolo Carbocyanine Triethyl Ammonium Salt (9-Ethyl-3,3'-Bis(3-sulfopropyl)-4,5,4'5'-Naphthothiazolo Carbocyanine Triethyl Ammonium Salt의 합성)

  • Kim, Yeoung-Chan
    • Journal of the Korean Applied Science and Technology
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    • v.31 no.3
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    • pp.416-421
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    • 2014
  • Naphthothiazolo carbocyanine is of industrial importance as red-sensitizing dye in the spectral sensitization. Sensitizing dye was prepared by the reaction of 2-methyl-3-sulfopropyl-4,5-naphthothiazolium (inner salt) with triethyl orthopropionate in the presence of triethylamine. The product was identified by using various analytical tools such as elemental analyzer, IR spectrophotometer, UV-Vis spectrophotometer, $^1H$-NMR spectrometer, TGA and DSC. The maximum absorption peak in methanol solvent was 578nm. Therefore, it was concluded that naphthothiazolo carbocyanine dye can be used as sensitizing dye for the spectral sensitization of photographic emulsion and color cosmetics.

$^{17}O$ NMR Study On Water Excharge Rate of Paramagnetic Contrast Agents ($^{17}O$ NMR 기법을 이용한 상자성 자기공명조영제의 물분자 교환에 관한 연구)

  • Yongmin Chang;Sung Wook Hong;Moon Jung Hwang;Il Soo Rhee;Duk-Sik Kang
    • Investigative Magnetic Resonance Imaging
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    • v.5 no.1
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    • pp.33-37
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    • 2001
  • Purpose : The water exchange rate between bulk water and bound water is an important parameter in deciding the efficiency of paramagnetic contrast agents. In this study, we evaluated the water exchange rates of various Gd-chelates using oxygen-17 NMR technique. Material and Methods : The samples (Gd-DTPA, Gd-DTPA-BMA, Gd-DOTA, Gd-EOB-DTPA) were prepared by mixing 5% $^{17}O-enriched$ water (Isotech, USA). The pH of the samples was adjusted to physiological value [pH=7.0] by buffer solution. The variable temperature $^{17}O-NMR$ measurements were performed using Bruker-600 (14.1 T, 81.3 MHz) spectrometer. Bruker VT-1000 temperature control units were used to stabilize the temperature. The $^{17}O$ spin-spin relaxation times (T2) were measured using Carr-Purcell-Meiboom-Gill (CPMG)I pulse sequence with 24 echo trains. The variable temperature T2 relaxation data were then fitted into Solomon-Bloembergen equations using least square fit algorithm to estimate the water exchange times. Results : From the measured $^{17}O-NMR$ relaxation rates, the determined water exchange rates at 300K are $0.42{\;}{\mu}s$ for Gd-DTPA, $1.99{\;}{\mu}s$ for Gd-DTPA-BMA, $0.27{\;}{\mu}s$ for Gd-DOTA, and $0.11{\;}{\mu}s$ for Gd-EOB-DTPA. The Gd-DTPA-BMA showed slowest exchange whereas Gd-EOB-DTPA had fastest water exchange rate. In addition, it was found that the water exchange rates (${\tau}_m$) of all samples had exponential temperature dependence with different decay constant. Conclusion : $^{17}O-NMR$ relaxation rate measurements, when combined with variable temperature technique, provide a solid tool for studying water exchange rate, which is very important in investigating the detailed mechanism of relaxation enhancement effect of the paramagnetic contrast agents.

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The Dispersibility and Adsorption Behaviour of Cement Paste with Molecular Structures of Polycarboxylates (폴리카복실레이트 분자 구조에 따른 시멘트페이스트의 분산 및 흡착 특성 연구)

  • Shin, Jin-Yong;Hong, Ji-Sook;Suh, Jeong-Kwon;Lee, Young-Seok;Hwang, Eui-Hwan
    • Journal of the Korea Concrete Institute
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    • v.18 no.4 s.94
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    • pp.489-496
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    • 2006
  • Graft copolymerized polycarboxylate(PC)-type superplasticizers which have carboxylic acid with $\pi$ bond among the molecular structure and polyethyleneglycol methyl ether methacrylate(PMEM) were synthesized by free radical reaction. To investigate their chemical structures and molecular weights, PCs were analyzed by FT-IR(fourier transform spectrometer), C-NMR(nuclear magnetic resonance spectrometer) and GPC(gel permeation chromatograpy). When types of carboxylic acids(methacrylic acid, acrylic acid, maleic anhydride, and itaconic acid) and molar ratios of carboxylic acid/PMEM) were varied, adsorptive and fluid characteristics in cement paste were discussed. As the molar ratio of carboxylic acid/PMEM) was higher, amount adsorbed on the cement particles and the fluidity of cement paste by mini-slump spread testing method were increased. When main chain of PC was methacrylic acid, a larger amount was adsorbed on the cement particles. PCs with acrylic acid as main chain showed higher dispersing power. However, it was confirmed that PCs with dicarboxylic acids(maleic anhydride, itaconic acid) didn't have good adsorption and dispersibility.

Synthesis of Subphthalocyanine Compound Derivatives and Their Properties (Subphthalocyanine 화합물 유도체들의 합성 및 특성 비교)

  • Kim, Jae Hwan;Heo, Jin;Lee, Yun-Yi;Kim, Bo Hyun;Lee, Geun-Dae;Hong, Seong-Soo;Park, Seong Soo
    • Applied Chemistry for Engineering
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    • v.20 no.1
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    • pp.46-51
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    • 2009
  • Subphthalocyanine (SubPc) derivatives consisting of the different kinds and positions of substitute group were successfully synthesized using various types of the precursor as the intermediate compound. The chemical structure of precursor and product was determined by the means of $^{1}H-NMR$ and FT-IR spectrometer. Also, spectroscopic and crystalline properties were determined by means of UV-Vis spectrometer and XRD, respectively. It was found that SubPc derivatives absorbed selectively visible light ranging from 560 to 600 nm, their solubility was enhanced by introducing substitute groups, and their maximum absorbing wavelength was shifted by changing the kind and position of substitute groups.

CORRELATION BETWEEN BIS-GMA : TEGDMA RATIO AND DEGREE OF CONVERSION IN VARIOUS LAYERS OF COMPOSITE AFTER ADDITIONAL HEAT CURING (수종 복합레진 내의 bis-GMA와 TEGDMA의 구성비가 레진 인레이 법에 의한 부가적 열처리시 복합레진의 표면 및 내부의 중합률 변화에 미치는 영향)

  • Park, Seong-Ho;Chung, Chan-Moon
    • Restorative Dentistry and Endodontics
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    • v.21 no.2
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    • pp.642-651
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    • 1996
  • The purpose of this study was to evaluate the relationship between monomer compositions and the changes in the degree of conversion in the various layers of composites after additional heat curing. Four types of composites and 3 types of inlay ovens were used in this study. Composite was placed in a 4-mm thick teflon mold, and light cured from the top for 60 seconds. Ten samples were prepared for each composite ; 5 of these were additionally heat cured in an inlay oven as the manufacturer recommended. After light curing or light and heat curing, the samples were sectioned into four parts and assigned to groups A, B, C, or D according to their distance from the light source. These sections were then thinned to 50-$70{\mu}m$, and these wafers were analyzed with a Fourier Transform Infrared Spectrometer(FI-IR) to determine the degree of conversion. A standard baseline technique was used to calculate the degree of conversion. $^{13}C$ NMR spectra of bis-GMA, TEGDMA and bis-EMA, were acquired using a Varian Gemini spectrometer operated at 200 MHz. $CDCl_3$ solvent was used for qualitative analysis. The degree of conversion was affected by bis-GMA : TEGDMA ratio but it seemed to be also affected by other factors. When the composites were heat cured, significant increases in the degree of conversion were noted throughout the samples, but the amount of increase differed between materials. Thus, clinical performance of a heat-treated composite inlay may be different depending on materials.

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Identification of Antioxidative Components from Ethanol Extracts of Dalbergia odorifera T.CHEN (강진향(Dalbergia odorifera T.CHEN) 에탄올 추출물로부터 항산화 활성물질의 구조동정)

  • Choi, Ung;Kim, In-Won;Baek, Nam-In;Shin, Dong-Hwa
    • Korean Journal of Food Science and Technology
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    • v.34 no.5
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    • pp.893-897
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    • 2002
  • The chloroform layer from 75% ethanol extract of Dalbergia odorifera T.CHEN showed strong antioxidative activity on lard and palm oil as tested by Rancimat method. Antioxidative active compound isolated and identified by silica gel column chromatography, thin layer chromatography, mass spectrophotometer, $^1H-NMR$ and $^{13}C-NMR$ was identified as mucronulatol (3(R&S)-3,7-Dihydroxy-2',4-dimethoxyisoflavan). Results of Rancimat method revealed the induction period of Mucronulatol increased longer than those of synthetic antioxidant, BHA and BHT, at the same concentration. Mucronulatol combined with ${\delta}-tocopherol(200ppm)$, and with ascorbic acid (200 ppm) and citric acid (200 ppm) on lard and palm oil, respectively, showed strong synergistic effects.

Identification of Antioxidative Components from Ethanol Extract of Rhus verniciflua STOKES (옻나무 에탄올 추출물로부터 항산화 활성 물질의 구조동정)

  • Kim, In-Won;Shin, Dong-Hwa;Baek, Nam-In
    • Korean Journal of Food Science and Technology
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    • v.31 no.6
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    • pp.1654-1660
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    • 1999
  • The free phenolic acid fraction of the chloroform extract from 75% ethanol extract of Rhus verniciflua STOKES (RCF) showed stronger antioxidative activity than BHT, BHA and ${\delta}-tocopherol$ at the same concentration. RCF components were isolated and identified by silica gel column chromatography, thin layer chromatography, mass spectrometer and $^1H-NMR\;and\;^{13}C-NMR$. The antioxidative activity was confirmed by electron donating activity, Rancimat method and thiobarbituric acid test in liposome system. RCF-11 could be further separated into three fractions. The antioxidative active compounds were purified and identified as gallic acid, butin and butein. The RCF-13 was purified and identified as sulfuretin.

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