• Title/Summary/Keyword: FT-NMR

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Preparation and Characterization of Poly(Arylene Ether) Having Heterocyclic Quaternary Ammonium Functional Groups for Anion Exchange Membranes (음이온교환막용 헤테로고리형 4차 암모늄 작용기를 갖는 폴리(아릴렌 이써)의 제조 및 특성 분석)

  • LEE, SANG HYEOK;YOO, DONG JIN
    • Transactions of the Korean hydrogen and new energy society
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    • v.33 no.4
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    • pp.372-382
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    • 2022
  • In this study, anion exchange membranes were prepared by synthesizing the main chain into a poly(arylene ether) (PAE) structure, and the structures capable of improving the physical and chemical stability of the membrane by introducing a heterocyclic quaternary ammonium functional groups were studied. The chemical structure and thermal properties of the prepared polymer were confirmed by 1H-NMR, FT-IR, TGA, and DSC, and surface analysis was performed through AFM measurement. Additionally, dimensional stability and chemical properties was studied by measuring water uptake and swelling ratio, IEC and ionic conductivity. At 90℃, the quaternized poly(arylene ether) (QPAE)/1-methylpiperidine (MP) membrane exhibited the highest ionic conductivity of 27.2 mS cm-1, while the QPAE/1-methylimidazole (MI) membrane and QPAE/1-methylmorpholine (MM) membrane exhibited values of 14.5 mS cm-1 and 11.5 mS cm-1, respectively. In addition, the prepared anion exchange membrane exhibited high chemical stability in alkaline solution.

Poly(vinyl alcohol)의 합성과 유변학적 성질

  • Lee, Jeong Kyung;Lee, Hyang Aee;Kim, Keyn Gyi
    • Journal of the Korean Chemical Society
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    • v.45 no.6
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    • pp.555-561
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    • 2001
  • Vinyl acetate usually used in PVA resin preparation was converted to PVAc by bulk polymerization using AIBN as a initiator and PVA was synthesized by changing the concentration of NaOH added for saponification subsequently. As a result of estimating molecular weight using GPC, molecular weight increased as the NaOH concentration increased to 2.5 N, 5.0 N, 7.5 N and 10.0 N and polydispersity had similar values of 2.1~2.3, however, showed slightly decreasing tendency. In addition, PVA saponificated by 10.0 N-NaOH showed high syndiotacticity in observation of tacticity using NMR spectroscopy. From this fact, the degree of tacticity was predicted to be high and it was in good agreement with the tendency of polydispersity by GPC. Also, from the result of FT-IR spectroscopy, it might be known that hydrolysis was more promoted in the PVA with 10.0 N-NaOH than other NaOH concentration. Intrinsic viscosity measured using Ubbelohde viscometer, which increased as the concentration of NaOH added for saponification increased. The change of shear strength with the change of shear rate was investigated using Brookfield viscometer, in consequence, viscosity of PVA synthesized decreased as shear rate increased. PVA solution confirmed to show the shear thining behavior by Casson plot and PVA with 10.0 N-NaOH had the largest yield value. DSC measurement was performed to know the thermal properties of PVA. Tp had nearly constant value of 214$^{\circ}C$ in all cases except for adding 2.5 N-NaOH and $\Delta$H was increased as the concentration of NaOH increased. From this properties, it was concluded that the degree of hydrogen bonding was proportional to the added concentration of NaOH and the increase of the degree of hydrogen bonding and hydrophobic interaction could affect the rheological and thermal properties of title compound.

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Enzymological Evaluation of Oral Inflammation inhibitory activity by Aloe vera peel extract (Aloe vera peel 추출물에 의한 구강염증 저해 효과의 효소학적 평가)

  • Pack, Chung-Sun;Ryu, Il-Hwan;Lee, Kap-Sang
    • Korean Journal of Food Science and Technology
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    • v.33 no.6
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    • pp.753-759
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    • 2001
  • To evaluate antiinflammation of Aloe vera peel, antiimflammation substances were extracted from Aloe vera peel and identified, and we investigated the effect of the its substance the inhibitory effect on the activity of hyaluoronidase, elastase, collagenase and prostaglandin endoperoxide synthase. The water extract from Aloe vera peel were successfully purified with solvent fractionation, silica gel column chromatography, preparative thin layer chromatography and UV spectrometer. Two purified active substances were identified as aloe-emodin and barbaloin by Mass Spectrometer, $^1H-NMR$ and FT-IR. Aloe-emodin and barbaloin. $IC_{50}$ values of aloe-emodin and barbaloin against hyaluronidase activity were 40 and $70\;{\mu}g/mL$, respectively. Leuckocyte elastase, which is related to the destruction of various tissue, $IC_{50}$ values of them were 50 and $60\;{\mu}g/mL$, respectively. $IC_{50}$ values of aloe-emodin and barbaloin against collagenase activity were 40 and $60\;{\mu}g/mL$, respectively. and $IC_{50}$ values of aloe-emodin and barbaloin aganist the prostaglandin endoperoxide synthase, which play an important role in inflammatory reactions, were 40 and $70\;{\mu}g/mL$, respectively. Inhibitory effects of aloe-emodin, barbaloin and aspirin against carrageenan paw edema were 74.9, 52.9 and 51.9% as inhibiton percentage, respectively, at dose of 100 mg/kg and that of indomethancin was 49.7 at dose of 10 mg/kg. Cell cytotoxicity of barbaloin against human gingival cells was lower than that of aloe-emodin. Aloe-emodin and barbaloin did not show cytotoxicity against human gingival cells at concentration of 1.0 and $5.0\;{\mu}g/mL$, However, aloe-emodin and barbaloin showed less cytotoxicity than chlorhexidine, which usually have been used as the agent of anticaries and antiinflammation. These results suggested that aloe-emodin and barbaloin from Aloe vera peel have the effect of anticaries and antiinflammation.

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Etherification of n-Butanol to Di-n-Butyl Ether over H3+xPW12-xNbxO40 (x=0, 1, 2, 3) Keggin and H6+xP2W18-xNbxO62 (x=0, 1, 2, 3) Wells-Dawson Heteropolyacid Catalysts (Keggin형 H3+xPW12-xNbxO40 (x=0, 1, 2, 3) 및 Wells-Dawson형 H6+xP2W18-xNbxO62 (x=0, 1, 2, 3) 헤테로폴리산 촉매를 이용한 n-Butanol로부터 Di-n-Butyl Ether의 제조)

  • Kim, Jeong Kwon;Choi, Jung Ho;Yi, Jongheop;Song, In Kyu
    • Korean Chemical Engineering Research
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    • v.50 no.2
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    • pp.251-256
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    • 2012
  • Etherification of n-butanol to di-n-Butyl Ether was carried out over Keggin $H_{3+x}PW_{12-x}Nb_xO_{40}$ (x=0, 1, 2, 3) and $H_{6+x}P_2W_{18-x}Nb_xO_{62}$ (x=0, 1, 2, 3) Wells-Dawson heteropolyacid catalysts. Niobium-substituted Keggin and Wells-Dawson heteropolyacid catalysts with different niobium content were prepared. Successful preparation of the catalysts was confirmed by FT-IR, ICP-AES, and $^{31}P$ NMR analyses. Their acid properties were determined by $NH_3$-TPD (Temperature-Programmed Desorption) measurements. Heteropolyacid catalysts showed different acid properties depending on niobium content in both series. The correlation between acid properties of heteropolyacid catalysts and catalytic activity was then established. Acidity of Keggin and Wells-Dawson heteropolyacid catalysts decreased with increasing niobium content, and conversion of n-butanol and yield for di-n-butyl ether increased with increasing acidity of the catalysts, regardless of the identity of heteropolyacid catalysts (without heteropolyacid structural sensitivity). Thus, acidity of heteropolyacid catalysts served as an important factor determining the catalytic performance in the etherification of n-butanol to di-n-Butyl Ether.

Synthesis and Lubricating Properties of Succinic Acid Alkyl Ester Derivatives (숙신산 알킬 에스테르 유도체의 합성 및 윤활특성)

  • Baek, Seung-Yeob;Kim, Young-Wun;Chung, Keun-Wo;Yoo, Seung-Hyun;Park, Su-Jin
    • Applied Chemistry for Engineering
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    • v.22 no.2
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    • pp.196-202
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    • 2011
  • In this paper, a series of alkyl succinic acid esters for base oil were synthesized by condensation reaction of succinic anhydride and fatty alcohol. The structures of the synthesized esters were confirmed by $^1H-NMR$, FT-IR spectrum and GC analysis. Basic properties of esters such as kinematic viscosity (KV), refractive index (RI), total acid number (TAN) and pour points were measured and lubricating properties such as SRV wear scar diameter (SRV WSD), fraction coefficient (COF) and 4-ball wear (4-ball WSD) were also evaluated. As the results of basic properties, KV, RI and pour point of synthetic esters increased as the carbon chain of the esters increased. Measurement value of total acid number (TAN) was indicated between 0.2~4 mgKOH/g, and that metal working fluids and pressure working oils are acceptable to use as base oil. Also, lubricating properties of the esters showed as follows: 0.391~0.689 mm of SRV WSD, 0.110~0.138 of SRV COF and 0.49~0.55 mm of 4-ball WSD depended on the structure of the esters. In a comparison on the lubrication capacity of the SRV test based on polyester TMPTO, SRV WSD result showed that a better performance caused by the alkyl group. On the other hand, SRV COF test was not influenced of the alkyl group which the capacity of the lubricant was sightly diminished than the comparison material, regardless of the alkyl group.

Mineralogical Studies of the Tourmaline for Medicinal Applications by Production Localities (본초 광물로서의 활용을 위한 산지별 전기석의 광물학적 연구)

  • Jie, Yan;Kim, Seon-ok;Park, Hee Yul;Park, Maeng-Eon
    • Economic and Environmental Geology
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    • v.51 no.4
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    • pp.345-358
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    • 2018
  • In this study, we have performed electron probe micro analyzer (EPMA), X-ray differaction (XRD), inductively coupled plasma spectroscopy (ICP), Fourier transform Raman spectroscopy (FT-Raman), far-infrared (FIR), nuclear magnetic resonance (NMR), and pH-DO Analyses for characterizing medicinal mineralogy aspect of the black tourmaline (Shantung, china), black and pink tourmaline (Minas Geraris, Brazil), black touemaline (Daeyu mine, Korea). In addition, heating effects of the tourmaline sauna as well as the effects of tourmaline powder-added soap on skin troubles have been investigated. It has been revealed that chemical composition of the tourmaline is either high in Fe-, Al-, B-rich types. Ratio of the K-Ca, Na-K, and Fe-B reflects the component change property of solid solution. $CaO/CaO+Na_2O$ and MgO/FeO+MgO ratio show high positive correlation. When tourmaline reacts with distilled water, extended reaction time DO values approximately decrease and it stabilizes at DO = 10. Otherwise, pH values increase until 6 hours and it stabilizes at pH = 8 after 24 hours. Distilled water changes to alkaline when it reacts with tourmaline powder and particles. Tourmaline showed lower absorption spectrum strength and transmittance at short wave, where absorption spectrum wavelength and strength were determined by the content of the composition elements and characteristics of crystallography. Increase of the Fe content has been confirmed to be the cause for the reduction of irradiation. For the chemical composition and spectral property of the tourmaline particle samples, it has been found that Si and Fe contents show positive correlation with Far-Infrared irradiation, while Al and Mg contents show negative correlation. For tourmaline powder, it has been confirmed that $^{17}O-NMR$ FWHM (full width at half maximum) decreases when reacts with distilled water. Tourmaline sauna (approximately $100^{\circ}C$) was found to increase $0.5-1.5^{\circ}C$ of body temperature, average of 12 heartbeat, and 10mg Hg of blood pressure. Tourmaline soap had very good aesthetic effect to skin and was confirmed to have above the average improvements to skin troubles (e.g., allergy or atopy).

Preparation and Characterization of O-Carboxymethyl Chitosan Ion-complexed Poly(L-Lysine) for Drug and Gene Delivery System (약물 및 유전자 전달체로 응용하기 위한 Poly(L-Lysine)이 결합된 O-Carboxymethyl Chitosan PEG의 제조와 특성)

  • Nam, Joung-Pyo;Kim, Young-Min;Park, Jin-Su;Lee, Eung-Jae;Choi, Chang-Yong;Jang, Mi-Kyeong;Nah, Jae-Woon
    • Applied Chemistry for Engineering
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    • v.21 no.6
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    • pp.643-647
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    • 2010
  • O-carboxymethyl water-soluble chitosan (OCMCh) prepared for enhance the application of chitosan was modified with mthoxy polyethyleneglycol (mPEG) by ion-complex for long circulation in the blood. OCMCh-PEG-PLLs was prepared by forming ion-complex with OCMCh-PEG and Poly(L-Lysine) (PLL) for drug and gene delivery system. The physicochemcal characterisitcs of OCMCh-PEG-PLLs were investigated by FT-IR, $^1H$-NMR. These results showed that CMCh-PEG-PLLs were successfully syntehsized by ion-complex. Particle size distribution and zeta potential of the OCMCh-PEG-PLLs were determined using dynamic light scattering technique. Transmission electron microscopy (TEM) was also used to observe the morphology of the OCMCh-PEG-PLLs. OCMCh-PEG-PLLs have spherical shapes with particle size 290∼390 nm. OCMCh-PEG-PLLs were showed when the feeding amount of mPEG ratio was increased, particle size and zeta potential were decreased. Based on these results, it is possible to introduction of the OCMCh-PEG-PLLs into various biomedical fields such as drug and gene delivery system.

Biosurfactant as a microbial pesticide

  • Lee, Baek-Seok;Choi, Sung-Won;Choi, Ki-Hyun;Lee, Jae-Ho;Kim, Eun-Ki
    • 한국생물공학회:학술대회논문집
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    • 2003.04a
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    • pp.40-44
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    • 2003
  • Soil-borne infectious disease including Pythium aphanidermatum and Rhizoctonia solani causes severe damage to plants, such as cucumber. This soil-borne infectious disease was not controlled effectively by chemical pesticide. Since these diseases spread through the soil, chemical agents are usually ineffective. Instead, biological control, including antagonistic microbe can be used as a preferred control method. An efficient method was developed to select an antagonistic strain to be used as a biological control agent strain. In this new method, surface tension reduction potential of an isolate was included in the ‘decision factor’ in addition to the other factors, such as growth rate, and pathogen inhibition rate. Considering these 3 decision factors by a statistical method, an isolate from soil was selected and was identified as Bacillus sp. GB16. In the pot test, this strain showed the best performance among the isolated strains. The lowest disease incidence rate and fastest seed growth was observed when Bacillus sp. GB16 was used. Therefore this strain was considered as plant growth promoting rhizobacteria (PGPR). The action of surface tension reducing component was deduced as the enhancement of wetting, spreading, and residing of antagonistic strain in the rhizosphere. This result showed that new selection method was significantly effective in selecting the best antagonistic strain for biological control of soil-borne infectious plant pathogen. The antifungal substances against P. aphanidermatum and R. solani were partially purified from the culture filtrates of Bacillus sp. GB16. In this study, lipopeptide possessing antifungal activity was isolated from Bacillus sp. GB16 cultures by various purification procedures and was identified as a surfactin-like lipopeptide based on the Fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR), high performance liquid chromatography mass spectroscopy (HPLC-MS), and quadrupole time-of-flight (Q-TOF) ESI-MS/MS data. The lipopeptide, named GB16-BS, completely inhibited the growth of Pythium aphanidermatum, Rhizoctonia solani, Penicillium sp., and Botrytis cineria at concentrations of 10 and 50 mg/L, respectively. A novel method to prevent the foaming and to provide oxygen was developed. During the production of surface active agent, such as lipopeptide (surfactin), large amount of foam was produced by aeration. This resulted in the carryover of cells to the outside of the fermentor, which leads to the significant loss of cells. Instead of using cell-toxic antifoaming agents, low amount of hydrogen peroxide was added. Catalase produced by cells converted hydrogen peroxide into oxygen and water. Also addition of corn oil as an oxygen vector as well as antifoaming agent was attempted. In addition, Ca-stearate, a metal soap, was added to enhance the antifoam activity of com oil. These methods could prevent the foaming significantly and maintained high dissolved oxygen in spite of lower aeration and agitation. Using these methods, high cell density, could be achieved with increased lipopeptide productivity. In conclusion to produce an effective biological control agent for soil-borne infectious disease, following strategies were attempted i) effective screening of antagonist by including surface tension as an important decision factor ii) identification of antifungal compound produced from the isolated strain iii) novel oxygenation by $H_2O_2-catalase$ with vegetable oil for antifungal lipopeptide production.

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Purification and Structure of Antioxidative Substance Derived from Tetraselmis suecica (Tetraselmis suecica유래의 항산화성 물질의 정제 및 구조)

  • Kim Se Kwon;Byun Hee Guk;Park Pyo Jam;Adachi Kyoko
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.35 no.2
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    • pp.155-161
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    • 2002
  • Tetraselmis suecica (T. suecica) of Prasinophyta was selected because the growth rate is comparatively higher and the culturing is also easy. In order to investigate antioxidative activity, the soluble elements of T. suecica were fractionated using water and organic solvents such as methanol, hexane, chloroform, ethylacetate and butanol. The chloroform fraction of T. suecica showed strong antioxidative activity. The potential antioxidative activity was detected in hexane: ethylacetate (1:5) once used the fractions by different mixtures of organic solvents. This fraction was further purified by preparative thin layer chromatography (PTLC) and repeated reverse-phase HPLC. On the basis of chemical and spectroscopic evidences obtained by UV, FT-IR, FAB-MS and NMR, the compound purified from T. suecica was identified as pheophorbide-a. The antioxidative activity of the compound was comparable to that of $\alpha$-tocopherol and could be act as an antioxidant in foods.

Synthesis and Characterization of Polymers with Azobenzene and Hexamethylene Groups in Main Chain (주사슬에 아조벤젠기와 헥사메틸렌기를 갖는 고분자의 합성 및 특성)

  • Gu, Su-Jin;Lee, Eung-Jae;Bang, Moon-Soo
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.4
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    • pp.86-92
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    • 2019
  • Polymers with various compositions of azobenzene and hexamethylene groups in the main chain were synthesized by a Schotten-Baumann reaction and their properties were investigated. The chemical structures and physical properties of the synthesized polymers were investigated by Fourier transform infrared spectroscopy, proton nuclear magnetic resonance spectroscopy, differential scanning calorimetry, thermogravimetric analysis, polarized optical microscopy, and x-ray diffraction. The polymers showed an inherent viscosity of 1.28-1.36 dl/g and were relatively insoluble in most organic solvents. The melt transition temperature increased rapidly with increasing number of azobenzene groups in the polymer. When the azobenzene monomer content was more than 50 mol%, no melting transition occurred below the decomposition temperature. Among the polymers with a melt transition temperature, the MP-A3C7 and MP-A5C5 polymers were liquid crystalline materials and exhibited a nematic phase with weak liquid crystallinity over a wide liquid crystal temperature range. This difference in the properties of the synthesized polymers is likely due to the changes in intermolecular forces resulting from the linearity and polarity of the trans-form of azobenzene.