• Title/Summary/Keyword: GPC method

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Synthesis and Characterization of High Molecular Weight Biodegradable Polyoxalate (고분자량 생분해성 폴리옥살레이트의 합성과 특성분석)

  • Kim, Se-Ho;Yoo, Han-Na;Khang, Gil-Son;Lee, Dong-Won
    • Polymer(Korea)
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    • v.34 no.6
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    • pp.547-552
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    • 2010
  • Biodegradable polymers have gained enormous attentions in the pharmaceutical and biomedical applications, especially in drug delivery. In this work, we report the synthesis and characteristics of high molecular weight polyoxalate with ~75000 Da. Hydrolytic degradation kinetics and degradation products were characterized by nuclear magnetic resonance and gel permeation chromatography. Polyoxalate is a semicrystalline and thermally stable polymer with a glass transition temperature of ${\sim}35^{\circ}C$, which is suitable for drug delivery applications. The hydrophobic nature of polyoxalate allows it to be formulated into nanoparticles and encapsulate drugs using a conventional oil-in-water emulsion/solvent displacement method. Polyoxalate nanoparticles also exhibited excellent cytotoxicity profiles. It can be suggested that polyoxalate has great potential for numerous biomedical and pharmaceutical applications.

Influence of Initial Molar Ratios on the Performance of Low Molar Ratio Urea-Formaldehyde Resin Adhesives

  • LUBIS, Muhammad Adly Rahandi;PARK, Byung-Dae
    • Journal of the Korean Wood Science and Technology
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    • v.48 no.2
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    • pp.136-153
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    • 2020
  • In this paper, the influence of initial formaldehyde/urea (F/U) molar ratios on the performance of low molar ratio (1.0) urea-formaldehyde (UF) resin adhesives has been investigated. Two initial F/U molar ratios, i.e., the first and second initial molar ratios were used for the alkaline addition reaction. Three levels of the first initial F/U molar ratios (2.0, 3.0, and 4.0) and two levels of the second initial molar ratios (2.0 and 1.7) were employed to prepare a total of six UF resins with an identical final molar ratio (1.0). The basis properties, functional groups, molecular weight, crystallinity, and thermal curing properties of the UF resins were characterized in detail. Higher levels (3.0 and 4.0) of the first initial F/U molar ratio provided the UF resins with better properties (non-volatile solids content, viscosity, gelation time, pH, and specific gravity) than those of the resins prepared with the conventional level F/U molar ratio of 2.0. Statistical analysis suggested that combining the first and second initial molar ratio of 4.0 with 1.7 would result in UF resins with greater adhesion strength and lower formaldehyde emission than those of the resins prepared with other molar ratios. The results showed that higher levels of the first initial molar ratio resulted in a more branched structure, as indicated by GPC, FTIR, DSC, XRD, and greater adhesion strength than those of the other UF resins with an identical final molar ratio of 1.0.

Chemoenzymatic Synthesis of H-shaped Amphiphilic Pentablock Copolymer and Its Self-assembly Behavior (H-형태 양친매성 펜타블록 공중합체의 화학효소적 합성과 자기회합거동 평가)

  • Chen, Peng;Li, Ya-Peng;Li, Cai-Jin;Meng, Xin-Lei;Zhang, Bao;Zhu, Ming;Liu, Yan-Jing;Wang, Jing-Yuan
    • Polymer(Korea)
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    • v.37 no.3
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    • pp.332-341
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    • 2013
  • H-shaped amphiphilic pentablock copolymers $(PSt)_2-b-PCL-b-PEO-b-PCL-b-(PSt)_2$ was synthesized via chemoenzymatic method by combining enzyme-catalyzed ring-opening polymerization (eROP) of ${\varepsilon}$-caprolactone (${\varepsilon}$-CL) and atom transfer radical polymerization (ATRP) of styrene. By this process, we obtained copolymers with controlled molecular weight and low polydispersity. The structure and composition of the obtained copolymers were characterized by nuclear magnetic resonance (NMR), gel permeation chromatography (GPC) and infrared spectroscopy analysis (IR). The crystallization behavior of the copolymers was analyzed by differential scanning calorimetry (DSC) and X-ray diffraction (XRD). The crystallization behavior of the H-shaped block copolymers demonstrated a PCL dominate crystallization. The self-assembly behavior of the copolymers was investigated in aqueous media. The hydrodynamic diameters of the copolymer micelles in aqueous solution were measured by dynamic light scattering (DLS). The morphology of the copolymer micelles was observed by atomic force microscopy (AFM) and transmission electron microscopy (TEM). The hydrodynamic diameters of spherical micelles declined gradually with the increase of the hydrophobic chain lengths of the copolymers. The critical micelle concentration (CMC) values were determined from fluorescence emission, and it was found that the CMCs decreased with an increase of PSt hydrophobic block lengths.

Synthesis and Characterization of Thiophene-Based Copolymers Containing Urethane and Alkyl Functional Side Chains for Hybrid Bulk Heterojunction Photovoltaic Cell Applications

  • Im, Min-Joung;Kim, Chul-Hyun;Song, Myung-Kwan;Park, Jin-Su;Lee, Jae-Wook;Gal, Yeong-Soon;Lee, Jun-Hee;Jin, Sung-Ho
    • Bulletin of the Korean Chemical Society
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    • v.32 no.2
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    • pp.559-565
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    • 2011
  • The following noble series of statistical copolymers, poly[(2-(3-thienyl)ethanol n-butoxycarbonylmethylurethane)-co-3-hexylthiophene] (PURET-co-P3HT), were synthesized by the chemical dehydrogenation method using anhydrous $FeCl_3$. The structure and electro-optical properties of these copolymers were characterized using $^1H$-NMR, UV-visible spectroscopy, elemental analysis, GPC, DSC, TGA, photoluminescence (PL), and cyclic voltammetry (CV). The statistical copolymers, PURET-co-P3HT (1:0, 2:1, 1:1, 1:2, 1:3), were soluble in common organic solvents and easily spin coated onto indium-tin oxide (ITO) coated glass substrates. Hybrid bulk heterojunction photovoltaic cells with an ITO/G-PEDOT/PURET-co-P3HT:PCBM:Ag nanowires/$TiO_x$/Al configuration were fabricated, and the photovoltaic cells using PURET-co-P3HT (1:2) showed the best photovoltaic performance compared with those using PURET-co-P3HT (1:0, 2:1, 1:1, 1:3). The optimal hybrid bulk heterojunction photovoltaic cell exhibits a power conversion efficiency (PCE) of 1.58% ($V_{oc}$ = 0.82 V, $J_{sc}$ = 5.58, FF = 0.35) with PURET-co-P3HT (1:2) measured by using an AM 1.5 G irradiation (100 mW/$cm^2$) on an Oriel Xenon solar simulator (Oriel 300 W).

Formaldehyde Free Cross-linking Agents Based on Maleic Anhydride Copolymers

  • Yoon, Kee-Jong;Woo, Jong-Hyung;Seo, Young-Sam
    • Fibers and Polymers
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    • v.4 no.4
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    • pp.182-187
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    • 2003
  • Low molecular weight copolymers of maleic anhydride and vinyl acetate were prepared to develop formaldehyde free cross-linking agents. Since lower molecular weight is favorable for efficient penetration of the finishing agent into the cotton fibers in the padding process, the concentration of the initiator, chain transfer agent and the monomer ratios were varied to obtain copolymers of low molecular weights. The prepared polymers were characterized by GPC, $^1{H-NMR}$, FTIR, DSC and TGA. Copolymers of molecular weights of 2 000 to 10 000 were obtained and it was found that the most efficient method of controlling the molecular weight was by varying the monomer ratios. Poly(maleic anhydride-co-vinyl acetate) did not dissolve in water, but the maleic anhydride residue hydrolyzed within a few minutes to form poly(maleic acid-co-vinyl acetate) and dissolved in water. However, the maleic acid units undergo dehydration to form anhydride groups on heating above ${160}^{\circ}C$ to some extent even in the absence of catalysts. The possibility of using the copolymers as durable press finishing agent for cotton fabric was investigated. Lower molecular weight poly(maleic anhydride-co-vinyl acetate) copolymers were more efficient in introducing crease resistance, which appears to be due to the more efficient penetration of the cross-linking agent into cotton fabrics. The wrinkle recovery angles of cotton fabrics treated with poly(maleic anhydride-co-vinyl acetate) copolymers were slightly lower than those treated with DMDHEU and were higher when higher curing temperatures or higher concentrations of copolymer were used, and when catalyst, $NaH_2$$PO_2$, was added. The strength retention of the poly(maleic anhydride-co-vinyl acetate) treated cotton fabrics was excellent.

Studies on the Constituents of Korean Edible Oils and Fats -Part 3. Studies on the oil soluble constituents of sunflower seed- (한국산(韓國産) 식물식용유지(植物食用油脂)의 성분(成分)에 관(關)한 연구(硏究) -제3보(第3報) 해바라기 종자(種子)의 유성성분(油性成分)에 대하여-)

  • Choi, Kee-Young;Ko, Young-Su
    • Journal of Nutrition and Health
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    • v.12 no.2
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    • pp.75-85
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    • 1979
  • The Korean origin sunflower (Helianthus Annus Linn.) seed of netural lipid were analysed by thinchrography, High performance liquid chromatography, preparative Thinlayer and Gas liquid chromatography. 1) The seed oil triglyceride components were conveniently separated based on their degree of unsaturation by employing the chromatography on silica gel sintered rod impregnated with 12.5% silver nitrate. Sunflower seed oil was composed of triglyceride, especially trilinolein 57. 74% triolein 25.28%, tripalmitin 7 55% ana tristearin 9.43% by a thinctrography. 2) The fatty acid compositions of seed oil have been determined by a high performance liquid chromatographic analysis using a ALC/GPC 244 type from Waters Association (Japan) with ${\mu}$ Bondapak FFAA column. It contained stearic acid 8.59%, oleic acid 27. 19%, palmitic acid 7.50% and linoleic acid 56.72% respectively. 3) The composition of sterols were determined by a preparative Thinlayer and Gas liquid chromatographic analysis. It was noted that sitosterol was the major sterol in the Korean sunflower seed. The results showed that contents of sterols were cholesterol trace, campesterol $13_.^{22\sim}13.9%$, stigmasterol $13.8{\sim}14.1%$, If, sitosterol $58.4{\sim}60.7%$, ${\vartriangle}^7$-stigmastenol $10.2{\sim}10.5%$ and ${\vartriangle}^{7,24(25)}$-stigmastenol $3.6{\sim}3.8%$ by method of planimetry and triangulation.

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Polymerization of Polystyrene Latex using Ultrasound Energy Effect (초음파 에너지를 이용한 Polystyrene Latex의 중합 특성)

  • Kim, Hyung Jin;Kim, Won II;Lee, Seung Bum;Hong, In Kwon
    • Applied Chemistry for Engineering
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    • v.8 no.6
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    • pp.886-892
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    • 1997
  • There are many methods to synthesize polystyrene latex. Emulsion polymerization technique is commonly used commercially, but it requires a new technology to replace a traditional polymerization method because of the disadvantage of chemical initiator for environmental pollution. Since free radicals can be produced by ultrasound energy effect, polystyrene latex was synthesized using ultrasound energy instead of chemical initiator. As the ultrasonic irradiation time was increased, average molecular weight was increased and polydispersity was decreased. The degree of polymerization was increased with the concentration of SDS and maximum degree of polymerization was shown at 2wt.% SDS concentration and the reaction temperature of $40^{\circ}C$. During the course of polymerization, molecular weight was repeatedly fluctuated because of occurrence of depolymerization. Narrow molecular weight distribution polystyrene latex having controlled molecular weight was synthesized by controlling ultrasonic irradiation time and the concentration of SDS.

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A Study on the molecular structure and molecular weight control of styrene films by plasma polymerization (플라즈마 중합법에 의한 스티렌 박막의 분자 구조 및 분자량 제어에 관한 연구)

  • 김종택;최충양;박종관;박응춘;이덕출
    • Journal of the Korean Vacuum Society
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    • v.6 no.3
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    • pp.213-219
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    • 1997
  • The plasma polymerized styrene films were prepared by using an inter-electrode capacitively coupled gas-flow-type reactor, and the effects of plasma polymerization condition on the molecular weight distribution were investigated by Fourier Transform Infrared (FT-IR), Pyrolysis Gas Chromatography(PyGC), Differential Scanning Calorimetry(DSC) and Gel Permeation Chromatography(GPC). From the above results, the very cross-linked films different from chemical characteristics of the starting monomer were taken out, and it is realized that the molecular structure, cross linking density, and molecular weight distribution could be controlled by changing the parameters such as deposition pressure, deposition power and gas flow rate. Accordingly, it is suggested that plasma polymerization method performed by inter-electrode capacitively coupled gas-flow-type reactor has good characteristics for manufacturing the functional organic thin films which can be applied in sensors, opto-electric device, photo-resist by changing the polymerization parameters.

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Preparation and Characterization of BICND-loaded Multi-Layer PLGA Wafer Containing Glycolide Monomer (글리콜라이드 단량체를 함유한 BICNU 함유 다중층 PLGA웨이퍼의 제조 및 특성결정)

  • 채강수;이진수;정제교;조선행;이해방;강길선
    • Polymer(Korea)
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    • v.28 no.4
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    • pp.335-343
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    • 2004
  • Carmustine (l,3-bis(2-chloroethyI)-1-nitrosourea, BICNU) used as antineoplastic drug for the treatment of brain tumor is not appropriate for the long term delivery, because it has short biological half life. Therefore, poly(D,L-lactide-co-glycolide) (PLGA) is useful as drug carrier for the long term delivery due to bulk erosion property. Glycolide monomer is applied to release of BICNU owing to non-toxic and monomeric components after biodegradation of PLGA. In this study, BICNU-loaded PLGA wafers with or without glycolide monomer were fabricated by conventional direct compression method for the sustained release of BICNU. These wafers were observed for their release profiles of BICNU and degradation rates by SEM, NMR, and GPC. Furthermore, we make multi-layer wafers and compare them with release profiles of conventional wafer. From these results, drug release of BICNU-loaded PLGA wafers was increased with increasing the glycolid monomer contents. We confirmed that glycolide monomer and BICNU contents in barrier-layer influenced the drug release profiles and degradation rate.

A novel preparation of polyaniline in presence electric and magnetic fields

  • Hosseini, Seyed Hossein;Gohari, S. Jamal
    • Advances in materials Research
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    • v.2 no.4
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    • pp.209-219
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    • 2013
  • We have described primary studies on conductivity and molecular weight of polyaniline separately in the electric and magnetic fields when it is used in a field effect experimental configuration. We report further studies on doped in-situ deposited polyaniline. First we have chemically synthesized polyaniline by ammonium peroxodisulfate in acidic aques and organic solutions at different times. Then we measured mass and conductivity and obtained the best time of polymerizations. In continue, we repeated these reactions separately under different electric and magnetic fields in constant time and measured mass and conductivity. The polyaniline is characterized by gel permeation chromatography (GPC), UV-Visible spectroscopy and electrical conductivity. High molecular weight polyanilines are synthesized under electric field, $M_w$ = 520000-680000 g/mol, with $M_w/M_n$ = 2-2.5. The UV-Visible spectra of polyanilines oxidized by ammonium peroxodisulfate and protonated with dodecylbenzenesulfonic acid (PANi-DBSA), in N-methylpyrolidone (NMP), show a smeared polaron peak shifted into the visible. Electrical conductivity of polyanilines has been studied by four-probe method. The conductivity of the films of emeraldine protonated by DBSA cast from NMP are higher than 500 and 25 S/cm under 10 KV/m of potential) electric field and 0.1 T magnetic field, respectively. It shows an enhanced resistance to ageing too. By the next steps, we carried chemical polymerization at the best electric and magnetic fields at different times. Finally, resulted in finding the best time and amount of the fields. The longer polymerization time and the higher magnetic field can lead to degradation of polyaniline films and decrease conductivity and molecular mass.