• Title/Summary/Keyword: Polydispersity

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Synthesis and Properties of Oligomers Containing 3-Triethylsilyl-1-silacyclopent-3-ene and Borane Derivatives via Polyaddition Reaction

  • Lee, Jung-Hwan;Park, Young-Tae
    • Bulletin of the Korean Chemical Society
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    • v.25 no.6
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    • pp.889-894
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    • 2004
  • Polyaddition reactions of 1,1-diethynyl-3-triethylsilyl-1-silacyclopent-3-ene with several organoborane derivatives have afforded the oligomeric materials containing organosilacyclic group and organoboron moiety along the oligomer main chains. All of these materials are soluble in THF as well as chloroform, and their molecular weights are in the range of 1,990/1,190-21,950/7,050 ($M_w/M_n$) with the polydispersity indexes of 1.67-3.43. The prepared oligomers are characterized by several spectroscopic methods such as $^1H,\;^{13}C, \;^{29}Si,\;^{11}B$ NMR and FTIR spectra along with elemental analysis. FTIR spectra of all the oligomers show that the new strong C=C stretching frequencies appear at 1599-1712 $cm^{-1}$, in particular. The UV-vis absorption spectra of the materials in THF solution exhibit the strong absorption bands at the ${\lambda}_{max}$ of 268-275 nm. The oligomeric materials show that the strong excitation peaks appear at the ${\lambda}_{max}$ of 255-279 nm and the strong fluorescence emission bands at the ${\lambda}_{max}$ of 306-370 nm. All the spectroscopic data suggest that the obtained materials contain both the organoboron ${\pi}$-conjugation moiety of C=C-B-C=C and the organosilacyclic group of 3-triethylsilyl-1-silacyclopent-3-ene along the oligomer main chains. The oligomers are thermally stable up to 162-200 $^{\circ}C$ under nitrogen.

Synthesis and Thermal Property of Poly(styrene-g-caprolactone) with Well-defined Structure (분자구조가 제어된 Poly(styrene-g-caprolactone)의 합성 및 그라프트 공중합체의 열적 성질)

  • 오병석;안성국;조창기
    • Polymer(Korea)
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    • v.24 no.3
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    • pp.306-313
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    • 2000
  • Polycaprolactone (PCL) macromer containing terminal methacrylate group was synthesized by ring-opening polymerization. The number average molecular weight of PCL macromer was 11600 g/mole and polydispersity index was 1.09. The synthesized PCL macromer was copolymerized with styrene by stable free radical polymerization using 2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO), benzoyl peroxide, and well-defined poly(styrene-g-caprolactone)s were synthesized. The synthesized copolymers was characterized by $^1$H-NMR and gel permeation chromatography equipped with multiangle laser light scattering detector. Thermal properties of graft copolymers were investigated by DSC.

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Application of Image Processing to Determine Size Distribution of Magnetic Nanoparticles

  • Phromsuwan, U.;Sirisathitkul, C.;Sirisathitkul, Y.;Uyyanonvara, B.;Muneesawang, P.
    • Journal of Magnetics
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    • v.18 no.3
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    • pp.311-316
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    • 2013
  • Digital image processing has increasingly been implemented in nanostructural analysis and would be an ideal tool to characterize the morphology and position of self-assembled magnetic nanoparticles for high density recording. In this work, magnetic nanoparticles were synthesized by the modified polyol process using $Fe(acac)_3$ and $Pt(acac)_2$ as starting materials. Transmission electron microscope (TEM) images of as-synthesized products were inspected using an image processing procedure. Grayscale images ($800{\times}800$ pixels, 72 dot per inch) were converted to binary images by using Otsu's thresholding. Each particle was then detected by using the closing algorithm with disk structuring elements of 2 pixels, the Canny edge detection, and edge linking algorithm. Their centroid, diameter and area were subsequently evaluated. The degree of polydispersity of magnetic nanoparticles can then be compared using the size distribution from this image processing procedure.

Preparation and Evaluation of Ketoconazole-loaded Solid-SNEDDS (Self-Nanoemulsifying Drug Delivery System) using Various Solidification Carriers (다양한 분말화 담체를 이용한 케토코나졸 함유 자가미세유화약물전달시스템의 제조 및 평가)

  • Da Young Song;Kyeong Soo Kim
    • Journal of Powder Materials
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    • v.30 no.6
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    • pp.493-501
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    • 2023
  • This study aimed to develop a solid self-nanoemulsifying drug delivery system (solid-SNEDDS) to enhance the formulation of ketoconazole (KTZ), a BCS Class II drug with poor solubility. Ketoconazole, which is insoluble above pH 3, requires solubilization for effective delivery. This SNEDDS comprises oil, surfactant, and co-surfactant, which spontaneously emulsify in the gastrointestinal tract environment to form nanoemulsions with droplet sizes less than 100 nm. The optimal SNE-vehicle composition of oleic acid, TPGS, and PEG 400 at a 10:80:10 weight ratio was determined based on the smallest droplet size achieved. This composition was used to prepare liquid SNEDDS containing ketoconazole. The droplet size and polydispersity index (PDI) of the resulting liquid SNEDDS were analyzed. Subsequently, solid-SNEDDS was fabricated using a spray-drying method with solidifying carriers such as silicon dioxide, crospovidone, and magnesium alumetasilicate. The physicochemical properties of the solid-SNEDDS were characterized by scanning electron microscopy and powder X-ray diffraction, and its solubility, droplet size, and PDI were evaluated. In particular, the solid-SNEDDS containing ketoconazole and crospovidone in a 2:1 weight ratio exhibited significantly enhanced solubility, highlighting its potential for improved medication adherence and dissolution rates.

Synthesis, Characterization, and Thermal Degradation of Oligo-2-[(pyridin-4-yl-)methyleneamino]pyridine-3-ol and Oligomer-Metal Complexes (올리고피리디닐메틸렌아미노피리딘올과 금속 착화물의 합성, 분석 및 열분해 특성 연구)

  • Kaya, Ismet;Gul, Murat
    • Polymer(Korea)
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    • v.32 no.4
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    • pp.295-304
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    • 2008
  • This study examined the oxidative polycondensation reaction of 2-[(pyridin-4-yl-) methyleneamino] pyridine-3-ol (2-PMAP) using air $O_2$ and NaOCl oxidants at various temperatures and times in aqueous alkaline and acidic media. Under these reactions, the optimum reaction conditions using air $O_2$ and NaOCl oxidants were determined for 2-PMAP. The number-average molecular weight ($M_n$), weight average molecular weight ($M_w$), and polydispersity index (PDI) values of O-2-PMAP synthesized in aqueous alkaline media were found to be 960, 1230, and $1.281\;g\;mol^{-1}$ using NaOCl, and 1030, 1520, and $1.476\;g\;mol^{-1}$ using air $O_2$, respectively. At the optimum reaction conditions, the yield of O-2-PMAP in aqueous alkaline media was 92.50% and 85.70% for air $O_2$ and NaOCl oxidants, respectively. The yield of O-2-PMAP in aqueous acidic media was 88.5% and 88.0% for NaOCl and air $O_2$ oxidants, respectively. O-2-PMAP was characterized by $^1H-$, $^{13}C$-NMR, FT-IR, UV-vis, SEC, and elemental analysis. TGA-DTA analysis revealed O-2-PMAP and its oligomer metal complex compounds, such as $Co^{+2}$, $Ni^{+2}$, and $Cu^{+2}$, to be stable against thermal decomposition and their weight losses at $1000^{\circ}C$ were found to be 73.0, 58.0, 53.5%, and 50.0%, respectively. In addition, the antimicrobial activities of the monomer and oligomer were tested against E. Coli (ATCC 25922), E. Faecelis (ATCC 29212), P. Auroginasa (ATCC 27853), and S. Aureus (ATCC 25923).

Synthesis and Characterization of Polyacrylate Derivatives Baying Protected Isocyanate Groups and fluorinated Alkyl Groups (보호된 이소시아네이트기와 불소화 알킬기를 가지는 아크릴계 고분자의 합성과 특성)

  • 김우식;김민우;정은천;백창훈;박이순;강인규;박수영
    • Polymer(Korea)
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    • v.27 no.4
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    • pp.364-369
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    • 2003
  • The copolymerizations of 2-fluorohexylethyl acrylate (FA) with 2-(o-(1'-methylpropylidenamino)carboxyl amino)ethyl methacrylate(MEM) with different molar ratios of the two monomers were carried out in methyl ethyl ketone using ${\alpha}$,${\alpha}$'-azobisisobutyronitrile as an initiator to synthesize water repellent polyacrylate derivatives with protected isocyanate groups. The contents of FA and MEM in the copolymers were analyzed by NMR. The monomer reactivity ratios of MEM (1) and FA (2) were determined by Kelen-Tudos plot as follows : r$\_$1/=1.59 and r$\_$2/=0.50. The number-average molecular weights of the copolymers were in the range of 39400 to 72400 and the polydispersity indexes were about 1.5. The protected isocyanate groups in the copolymers were converted into isocyanate groups above 150$^{\circ}C$. The contact angle of the copolymer with 65 ㏖% of FA fur water was about 95$^{\circ}$.

Formation and Characterization of Casein Phosphopeptide/Chitosan Oligosaccharide NanoComplex (케이신 포스포펩티드/키토올리고당 나노 복합체 형성과 특성 연구)

  • Baek, Yun-Seo;Ha, Ho-Kyung;Lee, Ji-Hong;Lee, Mee-Ryung;Lee, Won-Jae
    • Journal of Dairy Science and Biotechnology
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    • v.36 no.3
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    • pp.164-170
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    • 2018
  • The objectives of this study were to manufacture casein phosphopeptide (CPP)/chitosan oligosaccharide (CSO) nanocomplexes and to investigate the impacts of manufacturing variables, such as CPP concentration and pH, on their morphological and physicochemical characteristics. Transmission electron microscopy (TEM) and particle size analysis were used to assess the morphological and physicochemical properties of the CPP/CSO nano-complexes, respectively. Based on the images obtained by TEM, the spherical shapes of the CPP/CSO nanocomplexes ranged from 50 to 150 nm. As the concentration of CPP was increased and the pH was decreased, the average particle size of the nanocomplexes significantly (p<0.05) increased. The CPP/CSO nanocomplexes had a highly uniform distribution with a polydispersity index value of less than 0.3. In addition, they had a negative surface charge with a zeta-potential value between -17 and -26 mV. The CPP/CSO nanocomplexes showed good stability during the freeze-drying process. In conclusion, CPP/CSO nanocomplexes were successfully manufactured, and the CPP concentration and pH were found to be key factors that affected their morphological and physicochemical properties.

Synthesis of Poly(alkylene carbonate) from Carbon Dioxide (이산화탄소로부터 Poly(alkylene carbonate)의 합성)

  • Lee, Yoon-Bae;Choi, Jeong-Hyun
    • Applied Chemistry for Engineering
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    • v.7 no.5
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    • pp.813-822
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    • 1996
  • In order to reduce carbon dioxide, one of the major greenhouse gases, a new type of copolymer, poly(alkylene carbonate) has been synthesized. The alternating copolymers have been obtained from carbon dioxide and various epoxides with zinc carboxylate as a catalyst. The number-average molecular weight of the polymer is about 50,000 and polydispersity is rather broad(5~10). The polymers are amorphous, and glass-clear materials that exhibit unusually facile and clean thermal decomposition behavior. Complete decomposition with no carbon residue is observed at elevated temperature even in an inert atmosphere. Terpolymers with bulkier epoxides improve the physical properties of the copolymer with simple epoxides. The decomposition properties of the polymer provide versatile applications such as ceramic, metal, and electronic binders and lost-foam casting. Further application of the polymer for the barrier film or the plasticizer will be investigated.

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Evaluation of Granular Activated Carbon Process Focusing on Molar mass and size distribution of DOM (DOM의 분자량과 크기분포에 따른 입상활성탄 공정의 평가)

  • Chae, Seon H.;Lee, Kyung H .
    • Journal of Korean Society of Water and Wastewater
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    • v.22 no.1
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    • pp.31-38
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    • 2008
  • The primary objective of this study was to evaluate the variation of the molecular size distribution by granular activated carbon (GAC) adsorption. GAC adsorption was assessed by using the rapid small-scale column test (RSSCT) and high-performance size-exclusion chromatography (HPSEC) was used to analyze the molecular size distribution (MSD) in the effluent of GAC column. RSSCT study suggested that GAC adsorption exhibited excellent interrelationship between dissolved organic carbon (DOC) breakthrough and MSD as function of bed volumes passed. After GAC treatment, the nonadsorbable fraction which was about 25percents of influent DOC corresponded to the hydrophilic (HPI) natural organic carbon (NOM) of NOM fractions and was composed entirely of <300 molecular weight (MW) in the HPSEC at the initial stage of the RSSCT operation. The dominant MW fraction in the source water was 1,000~5,000daltons. At the bed volumes 2,500, MW <500 of GAC treated water was risen rather than it of source water. After the bed volumes 7,300 of operation, the MW 1,000~3,000 fraction was closed to about 80percents of DOC found in the GAC influent. The Number-average molecular weight (Mn) value determined using HPSEC for the effluent of GAC column was gently increased as DOC breakthrough progress. The quotient p(Mw/Mn) can be used to estimate the degree of polydispersity was shown greatest value for the GAC effluent at the initial stage of the RSSCT operation.

Measurement of Molecular Weights of Melamine-Urea-Formaldehyde Resins and Their Influences to Properties of Medium Density Fiberboards

  • Jeong, Bora;Park, Byung-Dae
    • Journal of the Korean Wood Science and Technology
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    • v.44 no.6
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    • pp.913-922
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    • 2016
  • This study attempted to measure molecular weight (MW) of melamine-urea-formaldehyde (MUF) resins prepared by two different synthesis methods: the one-step MUF resins were synthesized in one batch procedure, while the two-step MUF resins were prepared by a physical mixing of urea-formaldehyde (UF) resin with melamine-formaldehyde (MF) resin that had been synthesized in a separate procedure. The properties of medium density fiberboard (MDF) panels bonded with two types of MUF resins were also investigated. MWs of these MUF resins were measured using gel permeation chromatography (GPC). In addition, this study measured the MWs of one-step MUF resin during its synthesis procedure. The performance of two types of MUF resins was evaluated by determining properties of MDF panels prepared in laboratory. As the synthesis procedure progressed, both number average MW ($M_n$) and weight average MW ($M_w$) of one-step MUF resin gradually increased, while the polydispersity index (PDI) decreased. And low Mw species of the resin predominantly decreased as the synthesis step progressed. The one-step MUF resin showed greater $M_n$ and $M_w$ than those of the two-step ones even though the PDI values of both resins were very similar each other. As expected, the one-step MUF resin resulted in better properties of MDF panels than those of two-step resins. In particular, the one-step MUF resin provided better internal bond (IB) strength and thickness swelling (TS) with MDF panels than those of two-step ones, indicating better water resistance of the one-step resin. These results suggest that the preparation method of MUF resins have a great impact on the MW and final panel properties.