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Gravimetric Analysis (gravimetric + analysis)
Kinds of Gravimetric Analysis Selected AbstractsGrowth of tetrakis thiourea potassium iodide as new second order optical materialCRYSTAL RESEARCH AND TECHNOLOGY, Issue 4 2008J. Thomas Joseph Prakash Abstract A novel organometallic nonlinear optical (NLO) crystal, namely thiourea complex of tetrakis thiourea potassium iodide (TTPI), has been grown by slow evaporation solution growth technique. The harvested crystal is large in size. To our knowledge there is no report is available for the bulk size single crystal of TTPI. This material has a positive temperature coefficient and has been grown by slow evaporation solution growth technique. The grown crystal have been characterized by employing several techniques such as single crystal and powder X-ray diffraction, FTIR, UV-Vis-NIR spectra, thermo gravimetric analyses respectively. Etching studies have also been carried out in order to know the surface defects on the as grown specimen of TTPI. The relative second harmonic generation efficiency have been tested by using Nd:YAG laser as source. (© 2008 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Synthesis of mordenite from diatomite: a case of zeolite synthesis from natural materialJOURNAL OF CHEMICAL TECHNOLOGY & BIOTECHNOLOGY, Issue 5 2003Vilma Sanhueza Abstract A high mordenite product was obtained from a natural raw material, diatomite, either with or without the presence of diethanolamine. The synthesis process took 2 days, and was carried out under hydrothermal conditions, at autogenic pressure, and at a temperature of 180 °C. The resulting crystals were identified as mordenite by X-ray diffraction and characterized by scanning electron microscopy, and differential thermal and gravimetric analyses. Copyright © 2003 Society of Chemical Industry [source] Antibacterial, spectral and thermal aspects of drug based-Cu(II) mixed ligand complexesAPPLIED ORGANOMETALLIC CHEMISTRY, Issue 10 2009G. J. Kharadi Abstract The antibiotic agent clioquinol is well known for its drug design and coordinating ability towards metal ions. Copper(II) mixed-ligand complexes of clioquinol with various uninegative bidentate ligands were prepared. The structure of the synthesized complexes was characterized using elemental analyses, infrared spectra, 1H-NMR spectra, electronic spectra, magnetic measurements, FAB mass spectrum and thermo gravimetric analyses. The kinetic parameters such as order of reaction (n) and the energy of activation (Ea) are reported using the Freeman,Carroll method. The pre-exponential factor (A), the activation entropy (,S#), the activation enthalpy (,H#) and the free energy of activation (,G#) were calculated. Complexes were also screened for their in vitro antibacterial activity against a range of Gram-positive and Gram-negative bacteria in order to set the precursors for anti-tumourigenic agent. Copyright © 2009 John Wiley & Sons, Ltd. [source] Powder second harmonic generation measurement and thermal decomposition mechanisms of a new organometallic compound [(18C6)Li][Cd(SCN)3]CRYSTAL RESEARCH AND TECHNOLOGY, Issue 9 2009J. J. Zhang Abstract Single crystals of a novel nonlinear optical organometallic compound CLTC, ([(18C6)Li][Cd(SCN)3]), were grown from aqueous solutions via evaporation technique and characterized by IR spectroscopy, thermal gravimetric analysis and X-ray single-crystal diffraction. By X-ray single-crystal structural analysis it is revealed that the compound crystallized in a noncentrosymmetric space group Cmc21 of orthorhombic system with cell parameter a = 14.767(3) Å, b = 15.454(3) Å, c = 10.644(2) Å, V = 2429.0(8) Å3 and Z = 4. The thermal stability and thermal decomposition of CLTC crystal were investigated by means of thermogravimetry and differential thermal analysis. The second harmonic generation (SHG) efficiency was measured using the Kurtz and Perry powder technique. It was shown that the value of the SHG efficiency of CLCT powder was about 2 times higher than that of potassium dihydrogen phosphate (KDP). (© 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Transition-Metal (MnII and CoII) Complexes with the Heteropolymolybdate Fragment [AsVMo9O33]7,: Crystal Structures, Electrochemical and Magnetic PropertiesEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 17 2007Yanyan Yang Abstract Two novel heteropolymolybdates, [(CH3)4N]8n[M(H2O)5]2n(H3O)2n[{M(H2O)5}2(MAsVMo9O33)2]n[M(H2O)4(MAsVMo9O33)2]n·20nH2O (M = Mn2+, 1; M = Co2+, 2), constructed from the new fragment (AsVMo9O33)7, and a transition metal have been synthesized in aqueous solution and characterized by elemental analysis, IR spectroscopy, thermal gravimetric analysis, and single-crystal X-ray diffraction. Structurally the title complexes resemble a sandwich-type complex because they involve the coordination of two transition metals to two [AsVMo9O33]7, fragments, which derive from the well-known B -, - Keggin structure. Compounds 1 and 2 exhibit a one-dimensional chain-like framework [M(H2O)4(MAsVMo9O33)2]8n, with isolated {[M(H2O)5]2(MAsVMo9O33)2}6, units residing among the chains. The magnetic properties of the two complexes were investigated to indicate typical antiferromagnetic interactions through the MnII,O,MnII bridge unit for complex 1 and the CoII,O,CoII bridge unit for complex 2. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007) [source] Graft copolymerization modification of silk fabric with an organophosphorus flame retardantFIRE AND MATERIALS, Issue 5 2010Guan Jinping Abstract This paper mainly deals with flame retardance of a silk fabric treated with a vinyl phosphate dimethyl 2-(methacryloyloxyethyl) phosphate (DMMEP) onto silk fabric by a graft copolymerization technique. This paper also explores the relationship between limiting oxygen index (LOI) and weight gain of DMMEP treated silk fabric. The paper also investigates the whiteness, handle, tensile strength and laundering durability of treated silk fabric. Microscale combustion calorimetry (MCC) is applied to test the heat release rate of silk fabric. Thermal gravimetric analysis (TG) and differential thermal analysis (DTA) are carried out to investigate the thermal decomposition behavior of DMMEP treated silk fabric. The kinetic parameters, activation energy and pre-exponential factor are determined using the Kissenger method. Copyright © 2009 John Wiley & Sons, Ltd. [source] Covalent-Ionically Cross-linked Poly(Etheretherketone)-Basic Polysulfone Blend Ionomer MembranesFUEL CELLS, Issue 3-4 2006J. Kerres Abstract Sulfinated-sulfonated PEEK was synthesized via partial reduction of sulfochlorinated PEEK with aqueous Na2SO3. From these polymers, covalent-ionically cross-linked ionomer blend membranes were prepared by mixing the sulfinated-sulfonated PEEK with different base-modified polysulfones (PSU-base), followed by cross-linking with 1,4-diiodobutane. These membranes have been compared with covalently cross-linked membranes which were obtained by the cross-linking of sulfinated-sulfonated PEEK and with ionically cross-linked membranes obtained by mixing sulfonated PEEK with different PSU bases. The membranes have been characterized in terms of thermal stability by means of thermogravimetry (TGA) and coupled TGA-FTIR, in terms of cross-linking extent by extraction experiments, in terms of proton conductivity by impedance spectroscopy, and finally, in terms of water uptake by gravimetric analysis. [source] Preparation of bimodal porous copolymer containing ,-cyclodextrin and its inclusion adsorption behaviorJOURNAL OF APPLIED POLYMER SCIENCE, Issue 4 2010Zhao-Yang Sun Abstract A novel insoluble bimodal porous polymer containing ,-cyclodextrin (,-CD) was prepared to adsorb aromatic amine compound. The process involved copolymerization of styrene and methyl methacrylate with a maleic acid derivative of ,-CD, subsequently, above formed copolymer was foamed by supercritical CO2. The chemical properties and physical structure of obtained copolymer was analyzed using Fourier transform infrared spectra, Thermal gravimetric analysis, X-ray diffraction, scanning electron microscope, and N2 adsorption techniques. The inclusion adsorption of aromatic amine compounds on ,-CD copolymer was carried out in a batch system. The quantities of aromatic amine compounds adsorbed on ,-CD copolymer reached equilibrium within 60 min. The adsorption kinetic could be fitted to a pseudo-second-order kinetic equation, and the linear correlation coefficients varied from 0.9828 to 0.9935. With the influence of molecular structure and hydrophobicity of the aromatic amine compound, the sequence of quantity of aromatic amine compounds adsorbed on ,-CD copolymer is p -toluidine > aniline > benzidine > o -toluidine. The adsorption equilibrium data of aromatic amine compound adsorbed on ,-CD copolymer were fitted to Freundlich and Langmuir models, respectively. The linear correlation coefficients of Langmuir model varied from 0.9516 to 0.9940, and the linear correlation coefficients of Freundlich varied from 0.9752 to 0.9976. It is concluded that Freundlich model fits better than Langmuir model, because the adsorption of aromatic amine compound on ,-CD copolymer is a chemical process. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010 [source] Evaluation of the potential of polymeric carriers based on chitosan- grafted -polyacrylonitrile in the formulation of drug delivery systemsJOURNAL OF APPLIED POLYMER SCIENCE, Issue 3 2010A. A. Sarhan Abstract Graft copolymerization of chitosan with acrylonitrile (AN) was carried out by free radical polymerization using KMnO4 and oxalic acid as a combined redox initiator system. Graft copolymerization was confirmed by Fourier transform infrared spectra (FTIR), proton nuclear magnetic resonance spectra (1H-NMR), thermal gravimetric analysis (TGA) measurements, and wide angle X-ray diffraction (WAXD). In addition, further modification of the cyano groups of the grafted copolymers was performed by partial hydrolysis into carboxylic function groups with various extents. The extent of hydrolysis was monitored using FTIR spectroscopy. The potential of the hydrolyzed and unhydrolyzed grafted copolymers as polymeric carriers for drug delivery systems was extensively studied by preparation of tablets incorporated with methyl orange (MO) as a drug model. In vitro drug release was carried out in simulated gastric and intestinal conditions. The effects of grafting percentage (GP) and the extent of hydrolysis on the release kinetics were evaluated. Release continued up to 24 h for both hydrolyzed and unhydrolysed chitosan- g -PAN copolymers. The nature of drug transport through the polymer matrices was studied by comparing with power law or Kormeyer-Peppas equation. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010 [source] Characterization of acrylic acid grafted poly(ethylene terephthalate) fabricJOURNAL OF APPLIED POLYMER SCIENCE, Issue 6 2010Navdeep Grover Abstract The preirradiation grafting of acrylic acid (AA) onto poly(ethylene terephthalate) (PET) had been found to affect the thermal and physical characteristics of fabric. The grafted fabrics with various graft levels were characterized by thermal gravimetric analysis (TGA), ATR-FTIR spectroscopy, contact angle, differential scanning calorimetry (DSC), X-ray diffraction (XRD), atomic force microscopy (AFM), and scanning electron microscopy (SEM). The initial decomposition temperature and T50 were increased with the increase in degree of grafting. The percentage crystallinity was decreased as the degree of grafting increases. The detailed elemental analysis was done by X-ray photoelectron spectroscopy (XPS). The atomic ratio (O1s/C1s) was found to increase significantly with increasing the degree of grafting and reached 0.64 at 14.5% grafting from 0.38 for virgin PET. The surface topography and morphology was strongly influenced as the degree of grafting was increased. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010 [source] Mechanochemical preparation of a novel polymeric photostabilizer for poly(vinyl chloride)JOURNAL OF APPLIED POLYMER SCIENCE, Issue 5 2010Xiaofei Zhang Abstract The preparation of a novel polymeric photostabilizer was carried out via the vibromilling of poly(vinyl chloride) (PVC) powder, a reactive light stabilizer (r-LS), and a peroxide initiator in ball-containing jars with a planetary ball mill for a certain time. The effects of the initiator content, milling time, and temperature on the grafting ratio were studied with gravimetric analysis and intrinsic viscosity measurements. Fourier transform infrared and ultraviolet,visible spectra were used to investigate the structural development of the mixture of the r-LS and PVC during vibromilling. The results showed that the r-LS was grafted onto PVC chains successfully, and the aforementioned factors had a significant effect on the grafting ratio. The optimum preparation conditions were 0.5 wt % initiator, 8 h, and 20°C. A grafting mechanism is proposed. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010 [source] Polypropylene nanocomposite film: A critical evaluation on the effect of nanoclay on the mechanical, thermal, and morphological behaviorJOURNAL OF APPLIED POLYMER SCIENCE, Issue 6 2010S. K. Sharma Abstract Polypropylene (PP)/clay nanocomposites prepared by melt blending technique using different percentages of clay with and without maleic anhydride grafted PP (MA-PP) were studied. The intercalated and exfoliated structure of nanocomposites was characterized by X-Ray Diffraction (XRD) and transmission electron microscopy (TEM). Because of the typical intercalated and exfoliated structure, the tensile modulus of the nanocomposites were improved significantly as compared to virgin PP. The viscoelastic behavior of the nanocomposites was studied by dynamical mechanical analysis (DMA) and the results showed that with the addition of treated clay to PP there was substantial improvement in storage modulus increases. The thermal stability and crystallization of the PP nanocomposites as studied by differential scanning calorimeter (DSC) and thermo gravimetric analysis (TGA) were also improved significantly compared to PP. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010 [source] Preparation and characterization of epoxidate poly(1,2-butadiene),toughened diglycidyl ether bisphenol-A epoxy compositesJOURNAL OF APPLIED POLYMER SCIENCE, Issue 5 2009Jie He Abstract By the oxidation of liquid poly(1,2-butadiene) (LPB) with H2O2/HCOOH, epoxidate poly(1,2-butadiene) (ELPB) was obtained as a toughening agent to prepare diglycidyl ether bisphenol-A (DGEBA) epoxy composites by using V115 polyamide(PA) as a cross-linking agent. DGEBA, ELPB, and the composites were effectively cured by PA at 100°C for 2 h followed by postcuring at 170°C for 1 h. Thermal gravimetric analysis results in air and nitrogen atmosphere showed that the thermal stability of composites could be improved by the addition of ELPB. Compared with DGEBA/PA, the composites exhibited a decrease in strength at yield but an increase in strain at break with the increase in ELPB amount. The composite with 10% ELPB exhibited both thermal stability and tenacity superior to those of DGEBA/PA and composites with 5 and 20% ELPB, respectively. The improvements in thermal and mechanical properties of composites depended on the formation of Inter Penetrating Networks (IPN) among DGEBA/PA/ELPB and their distributions in the matrix. At an appropriate ELPB amount, the IPN, mostly made of DGEBA/PA/ELPB, may be distributed more evenly in the matrix; less ELPB resulted in the formation of IPN mainly made of DGEBA/PA; excessive addition of ELPB resulted in the local aggregation of ELPB/PA and phase separations. The toughening mechanism was changed from chemically forming IPN made of DGEBA/PA/ELPB to physically reinforcing DGEBA/PA by ELPB/PA with the increase in ELPB addition. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009 [source] Properties of styrene-methyl methacrylate grafted DPNR latex at different monomer concentrationsJOURNAL OF APPLIED POLYMER SCIENCE, Issue 1 2008Siti Hajjar Che Man Abstract The graft copolymerization of styrene and methyl methacrylate (MMA) on to deproteinized natural rubber (DPNR) latex was carried out. The effect of monomer concentrations on grafting efficiency, thermal and mechanical properties was studied. The synthesized graft copolymers were characterized by proton nuclear magnetic resonance (1H NMR) and the highest grafting efficiency was found at 20 wt % monomer concentration. At low monomer concentration (10 wt %) the grafting was not significant and at 30 wt %, the grafting efficiency was slightly decreased. The thermal properties of graft copolymers were analyzed using differential scanning calorimeter (DSC) and thermal gravimetric analysis (TGA). The degradation temperature (Tdeg) of the graft copolymer was increased with the increase in monomer concentration which indicates the improvement in thermal stability. The DSC result showed improvement in miscibility between the components as the monomer concentration increased. The mechanical properties of gum and filled modified NR were also investigated in terms of tensile strength, tensile modulus and elongation at break. The tensile strength and elongation at break decreased with an increase in monomer concentration while tensile modulus increased as the monomer concentration increased. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008 [source] Synthesis, characterization, and electrical properties of diazophenylene bridged Co, Ni, Cu, Ce, and Er phthalocyanine polymersJOURNAL OF APPLIED POLYMER SCIENCE, Issue 1 2007Cemil Alkan Abstract In this research, diazophenylene bridged metal-phthalocyanine (Pc) polymers were produced from diazonium salt of 1,4-diaminophenylene and presynthesized 1,8,15,22-tetraamino metal-Pcs. 1,8,15,22-Tetraamino metal-Pc complexes of Co, Ni, Cu, Ce, and Er were obtained by reducing 1,8,15,22-tetranitro metal-Pc complexes synthesized from 3-nitrophthalic anhydride, urea, metal salt, and ammonium molybdate catalyst. Complexes and polymers were characterized by Fourier transform infrared (FTIR), ultraviolet,visible (UV,vis), and X-ray powder diffraction spectroscopes. X-ray analysis of the polymers showed that there were short-range orientations in the polymers. Thermal analysis of the complexes and the polymers were done by differential scanning calorimeter (DSC) and thermal gravimetric analysis (TGA) at a heating rate of 10°C min,1 under nitrogen atmosphere. Ash analysis was performed to determine the metal content of the polymers. Viscosimetry and ebullioscopy measurements of the soluble part of the polymers were done for molecular weight analysis of the soluble part in tetrahydrofuran (THF) at 25°C. Four-probe conductivity measurements on isothermal conditions revealed that the polymer samples showed 104 fold increases in their electrical conductivities when doped with iodine. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007 [source] Synthesis and characterization of conducting polyaniline-activated carbon nanocompositesJOURNAL OF APPLIED POLYMER SCIENCE, Issue 3 2007Mohammad Rezaul Karim Abstract Conducting polyaniline (PAni)/activated carbon (AC) nanocomposites were synthesized by the in situ chemical polymerization method. The resultant shell,core PAni,AC nanocomposites were characterized by elemental analysis, Fourier transform infrared, scanning electron microscopy, thermal gravimetric analysis, X-ray diffraction, and transmission electron microscopy. We did not observe any significant chemical interaction between the PAni and AC, only core,shell coupling between the AC and the tightly coated polymer chain was revealed. Measurement of the physical properties showed that the incorporation of conducting PAni on to AC particles during chemical synthesis increased electrical conductivity and thermal stability by several orders of magnitude to that of the pristine PAni powders. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 1973,1977, 2007 [source] Pervaporation of tertiary butanol/water mixtures through chitosan membranes cross-linked with toluylene diisocyanate,JOURNAL OF CHEMICAL TECHNOLOGY & BIOTECHNOLOGY, Issue 12 2005Smitha Biduru Abstract Membranes made from 84% deacetylated chitosan biopolymer were cross-linked by a novel method using 2,4-toluylene diisocyanate (TDI) and tested for the separation of t -butanol/water mixtures by pervaporation. The unmodified and cross-linked membranes were characterized by Fourier transform infra red (FTIR) spectroscopy, X-ray diffraction (XRD) studies and sorption studies in order to understand the polymer,liquid interactions and separation mechanisms. Thermal stability was analyzed by differential scanning calorimetry (DSC) and thermo gravimetric analysis (TGA) while tensile strength measurement was carried out to assess mechanical strength. The membrane appears to have good potential for breaking the aqueous azeotrope of 88.2 wt% t -butanol by giving a high selectivity of 620 and substantial water flux (0.38 kg m,2 hr,1). The effects of operating parameters such as feed composition, membrane thickness and permeate pressure on membrane performance were evaluated. Copyright © 2005 Society of Chemical Industry [source] A bi-order kinetic model for poly(methyl methacrylate) decomposition in HNO3 using microwave irradiationAICHE JOURNAL, Issue 8 2009Chun-Chih Lin Abstract In this study, a novel bi-order model combined with zero- and first-order kinetics was proposed for the decomposition of PMMA (MW = 120,000 g/mol) in concentrated HNO3 by microwave irradiation. To develop and validate this model, Fourier Transform Infrared spectroscopy, scanning electron microscopy, fractional-life method, the gravimetric analysis and Newton's method were utilized. Rate constants, activation energies, the pre-exponential factors and the weight fractions (,) via main-chain scission for the decomposition at 423,453 K were derived from this model. The zero-order reaction was observed dominant at 423,443 K, while the first-order reaction dominated at 453 K and 473 K. The digestion efficiency increased as HNO3 was increased to >3 mL at 423 K,443 K. At 473 K, the digestion was almost 100% when HNO3 volume was >3 mL. The estimated , values increased with HNO3 volume at 423 and 443 K, but varied insignificantly at 453 and 473 K. © 2009 American Institute of Chemical Engineers AIChE J, 2009 [source] Synthesis and characterization of high molecular weight hexafluoroisopropylidene-containing polybenzimidazole for high-temperature polymer electrolyte membrane fuel cellsJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 16 2009Guoqing Qian Abstract A high molecular weight, thermally and chemical stable hexafluoroisopropylidene containing polybenzimidazole (6F-PBI) was synthesized from 3,3,-diaminobenzidine (TAB) and 2,2-bis(4-carboxyphenyl) hexafluoropropane (6F-diacid) using polyphosphoric acid (PPA) as both the polycondensation agent and the polymerization solvent. Investigation of polymerization conditions to achieve high molecular weight polymers was explored via stepwise temperature control, monomer concentration in PPA, and final polymerization temperature. The polymer characterization included inherent viscosity (I.V.) measurement and GPC as a determination of polymer molecular weight, thermal and chemical stability assessment via thermo gravimetric analysis and Fenton test, respectively. The resulting high molecular weight polymer showed excellent thermal and chemical stability. Phosphoric acid doped 6F-PBI membranes were prepared using the PPA process. The physiochemical properties of phosphoric acid doped membranes were characterized by measuring the phosphoric acid doping level, mechanical properties, and proton conductivity. These membranes showed higher phosphoric acid doping levels and higher proton conductivities than the membranes prepared by the conventional membrane fabrication processes. These membranes had sufficient mechanical properties to be easily fabricated into membrane electrode assemblies (MEA) and the prepared MEAs were tested in single cell fuel cells under various conditions, with a focus on the high temperature performance and fuel impurity tolerance. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 47: 4064,4073, 2009 [source] Synthesis and characterization of organic/inorganic hybrid star polymers of 2,2,3,4,4,4-hexafluorobutyl methacrylate and octa(aminophenyl)silsesquioxane nano-cage made via atom transfer radical polymerizationJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 22 2008H. Hussain Abstract Well-defined organic/inorganic hybrid fluorinated star polymers were synthesized via atom transfer radical polymerization (ATRP) of 2,2,3,4,4,4-hexafluorobutyl methacrylate (HFBMA) using octa(aminophenyl)silsesquioxane (OAPS) nano-cage as initiator. For this purpose, OAPS was transformed into ATRP initiator by reacting with 2-bromoisobutyrylbromide. ATR polymerization of HFBMA was carried out in trifluorotoluene at 75 °C using CuCl/2,2-bipyridine or N,N,N,,N,,N,-pentamethyldiethylenetriamine as catalyst system. GPC and 1H NMR data confirmed the synthesis of OAPS/PHFBMA hybrid star polymer. Kinetics of the ATR polymerization of HFBMA using OAPS nano-cage initiator was also investigated. The OAPS/PHFBMA hybrid stars were found to be molecularly dispersed in solution (THF); however, TEM micrographs revealed the formation of spherical particles of , 120,180 nm by the OAPS/PHFBMA hybrid star polymer after solvent evaporation. Thermal characterization of the nanocomposites by differential scanning calorimetry (DSC) revealed a slightly higher glass transition temperature (Tg) (when compared with the linear PHFBMA) of higher molecular weight OAPS/PHFBMA hybrid star polymers. In contrast, lower Tg than the linear PHFBMA was observed for OAPS/PHFBMA of relatively lower molecular weight (but higher than the linear PHFBMA). Thermal gravimetric analysis (TGA) showed a significant retardation (by ,60 °C) in thermal decomposition of nanocomposites when compared with the linear PHFBMA. Additionally, surface properties were evaluated by measuring the contact angles of water on polymer surfaces. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 7287,7298, 2008 [source] Multi-walled carbon nanotubes encapsulated with polyurethane and its nanocompositesJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 14 2008Xiao Wang Abstract Poly(acryloyl chloride) (PACl) was employed to enhance the surface of multi-walled carbon nanotubes (MWCNTs). MWCNTs were first acid treated to generate hydroxyl groups on the surface, which was reacted with PACl to obtain an encapsulation. The numerous acryloyl chloride groups on the out layer were esterified with a proper amount of ethylene glycol (EG). Subsequently, 4,4,-methylenebis (phenylisocyanate) (MDI) and 1,4-butanediol (BDO) were introduced into the system, and a polyurethane (PU) layer was formed in situ. The formation of PU layers on MWCNTs was confirmed by Fourier transform infrared spectrometer (FTIR) and X-ray photoelectron spectroscope (XPS). The morphology of encapsulated MWCNTs was observed by transmission electron microscope (TEM) and scanning electron microscope (SEM). Thermo gravimetric analysis (TGA) showed the grafted polymer fraction was up to 90%. On introducing the modified MWCNTs into a PU matrix, an increase in tensile strength by 60.6% and improvement in modulus by 6.3% over neat PU was observed. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 4857,4865, 2008 [source] Functionalization of multiwalled carbon nanotube via surface reversible addition fragmentation chain transfer polymerization and as lubricant additivesJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 9 2008Xiaowei Pei Abstract Polymer-grafted multiwalled carbon nanotube (MWCNT) hybrid composite which possess a hard backbone of MWCNT and a soft shell of brush-like polystyrene (PSt) were synthesized. The reversible addition fragmentation chain transfer (RAFT) agents were successfully immobilized onto the surface of MWCNT first, and PSt chains were subsequently grafted from sidewall of MWCNT via RAFT polymerization. Chemical structure of resulting product and the quantities of grafted polymer were determined by Fourier transform infrared, thermal gravimetric analysis, nuclear magnetic resonance, and X-ray photoelectron spectra. Transmission electron microscopy and field emission scanning electron microscopy images clearly indicate that the nanotubes were coated with a polymer layer. Furthermore, the functionalized MWCNT as additives was added to base lubricant and the tribological property of resultant MWCNT lubricant was investigated with four-ball machines. The results indicate that the functionalization led to an improvement in the dispersion of MWCNT and as additives it amended the tribological property of base lubricant. The mechanism of the significant improvements on the tribological properties of the functionalized MWCNT as additives was discussed. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 3014,3023, 2008 [source] A Diels-Alder/retro Diels-Alder strategy to synthesize polymers bearing maleimide side chainsJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 20 2007Tugba Dispinar Abstract Polymers containing thiol-reactive maleimide groups on their side chains have been synthesized by utilization of a novel methacrylate monomer containing a masked maleimide. Diels-Alder reaction between furan and maleimide was adapted for the protection of the reactive maleimide double bond prior to polymerization. AIBN initiated free radical polymerization was utilized for synthesis of copolymers containing masked maleimide groups. No unmasking of the maleimide group was evident under the polymerization conditions. The maleimide groups in the side chain of the polymers were unmasked into their reactive form by utilization of retro Diels-Alder reaction. This cycloreversion was monitored by thermo gravimetric analysis (TGA), differential scanning calorimetry (DSC), and 1H and 13C NMR spectroscopy. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 4545,4551, 2007 [source] Controlled-release systems based on the intercalation of polymeric metribuzin onto montmorilloniteJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 14 2002Ahmed Rehab Abstract A series of polymer,clay composites carrying metribuzin as herbicide moieties were prepared. Linear copolymers containing metribuzin via an imide linkage were prepared by the free-radical polymerization of metribuzin monomer (N,N -diacryloyl metribuzin) with different comonomers. The intercalation of the copolymers onto montmorillonite through a cationic exchange process was carried out and yielded metribuzin composite products. The prepared materials were characterized with a wide variety of analytical techniques, including gel permeation chromatography, NMR, IR, elemental microanalysis, gravimetric analysis (calcination), and swelling measurements. The release rates for the prepared materials were investigated in media of different pHs with an ultraviolet spectrophotometer. Also, these compounds were studied for the control of herb growth. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 2513,2525, 2002 [source] Effect of pH on the Carbonate Incorporation into the Hydroxyapatite Prepared by an Oxidative Decomposition of Calcium,EDTA ChelateJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 1 2008Yusuf Yusufoglu In this study, the carbonate incorporation into the hydroxyapatite (HAp) lattice under various pH conditions was investigated. Crystalline-sodium and carbonate-containing calcium HAp (NaCO3HAp) powders were prepared using an oxidative decomposition of calcium,EDTA chelates in a sodium phosphate solution with hydrogen peroxide. The powders obtained were characterized by X-ray diffraction, infrared spectroscopy, thermal gravimetric analysis, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and elemental analysis. Depending on pH, spherical particles approximately 3.5 ,m in diameter or hexagonal prismatic particles measuring 3,9 ,m in length were obtained. Various characterization techniques showed that the precipitates were a single-phase NaCO3HAp. The carbonate content and the lattice parameters of the HAp were a function of solution pH. Maximum carbonate incorporated into the HAp lattice was at pH=10, corresponding to lattice parameters of a=0.93880 nm and c=0.69070 nm. Furthermore, spectroscopic analyses indicate that the as-prepared samples are B-type carbonated HAp, in which carbonate ions occupy the phosphate sites. After heat treatment at 965°C, most of the carbonate is removed from the HAp lattice. [source] Termination Rate Coefficients for Radical Homopolymerization of Methyl Methacrylate and Styrene at Low Conversion,MACROMOLECULAR CHEMISTRY AND PHYSICS, Issue 5 2010David R. Taylor Abstract A comprehensive and systematic study of overall termination rate coefficients, kt, in low-conversion radical (homo)polymerization of methyl methacrylate and styrene is presented. Values of kt were determined by gravimetric analysis of steady-state experiments, employing 2,2,-azoisobutyronitrile as initiator. The values delivered by this simple method were found to be in qualitative and quantitative agreement with those from more modern and sophisticated techniques for measuring kt. Accordingly, correlations for bulk, low-conversion kt as a function of temperature are given for each monomer. The effects of initiator concentration, cI, and temperature on bulk kt were studied in a controlled way for both monomers. Additionally, ethyl benzene was used as solvent in order to investigate rigorously the effect of monomer concentration, cM, on styrene kt. The trends found by these systematic studies were considered in the light of what is known about the chain-length dependence of termination. Styrene's behavior was always found to be qualitatively in accord with expectation, although the variations of kt with cI and cM were not as strong as should be the case. However its activation energy, 15,kJ,·,mol,1, is shown to be almost perfectly in agreement with theory. Methyl methacrylate, on the other hand, is recalcitrant in that its overall kt does not make manifest the chain-length dependent termination that has been directly measured by other techniques. Possible reasons for these discrepancies are discussed, as are reasons for the difference in values between kt for the two monomers. On the latter topic it is concluded likely that the chain-length dependence of termination at short chain lengths is primarily responsible for styrene having kt that is higher by a factor of about 3, with there also being a contribution that arises from styrene's slower propagation. [source] Synthesis and Characterization of Organic/Inorganic Polyrotaxanes from Polyhedral Oligomeric Silsesquioxane and Poly(ethylene oxide)/, -Cyclodextrin Polypseudorotaxanes via Click ChemistryMACROMOLECULAR CHEMISTRY AND PHYSICS, Issue 9 2009Ke Zeng Abstract Organic/inorganic polyrotaxanes were synthesized via Huisgen 1,3-dipolar cycloaddition between 3-azidapropylhepta(3,3,3-trifluoropropyl) POSS and dialkyne-terminated PEO/, -cyclodextrin polypseudorotaxanes. The organic/inorganic hybrid polyrotaxanes were characterized by means of 1H NMR spectroscopy and WAXRD. It was found that the nanosized POSS blocking agents significantly affected the crystal structures of polyrotaxanes. Thermal gravimetric analysis showed that the organic/inorganic hybrid polyrotaxanes exhibited enhanced thermal stability compared to their parent polypseudorotaxanes, in terms of rate of thermal degradation and the summation of char and ceramic yields. [source] Architecturally and Chemically Modified Poly(1,3-cyclohexadiene),MACROMOLECULAR CHEMISTRY AND PHYSICS, Issue 3 2008Tianzi Huang Abstract Star-shaped, star- block -linear, and hyperbranched poly(1,3-cyclohexadiene) (PCHD) (co)polymers were synthesized through a convergent living anionic polymerization process or via addition of divinylbenzene. Chemical modification of star-shaped PCHDs, including aromatization, hydrogenation, fluorination, and sulfonation, was carried out in order to manipulate the physical and thermal properties of these materials. The obtained (co)polymers were characterized by gel permeation chromatography, 1H NMR, DSC, and thermal gravimetric analysis in order to elucidate their molecular weights, molecular weight distributions, chemical nature, and physical and thermal properties. The synthetic approaches described herein offer routes to novel structure and functionality in PCHD-based materials. [source] Polystyrene/Montmorillonite Nanocomposites Prepared by In Situ Intercalative Polymerization: Influence of the Surfactant TypeMACROMOLECULAR CHEMISTRY AND PHYSICS, Issue 17 2004Hisham A. Essawy Abstract Summary: Na-montmorillonite (MMT) with a cation exchange capacity (CEC) of 90 meq/100 g was converted to MMT-CTAB and MMT-CPC by the intercalation of cetyltrimethylammonium bromide (CTAB) and cetylpyridinium chloride (CPC), respectively. The intercalation of CPC onto the basal space of the montmorillonite expanded the basal space from 12.19 to 21.47 Å, whereas in the case of CTAB, the spacing was only expanded to 19.35 Å. The MMT-CPC and MMT-CTAB forms were subsequently used as hosts for the preparation of polystyrene nanocomposites via intercalative free-radical polymerization of styrene. Different structures were obtained by varying the preparation conditions; the exfoliated and intercalated nanocomposites were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), thermal gravimetric analysis (TGA), and differential scanning calorimeter (DSC). The produced nanocomposites exhibited improved thermal stability in comparison with that of pure polystyrene above 400,°C especially in the case of the nanocomposites based on the MMT-CPC, in which intercalation exists. A glass transition temperature (Tg) could not be detected for the prepared nanocomposites using DSC; this was assumed to result from the restricted molecular motion of the polymer chains. XRD pattern of PS nanocomposites prepared by intercalative polymerization. [source] Use of the Surfmer 11-(Methacryloyloxy) undecanylsulfate MET as a Comonomer in Polystyrene and Poly(methyl methacrylate)MACROMOLECULAR SYMPOSIA, Issue 1 2004P.C. Hartmann Abstract The polymerizable surfactant sodium 11-(methacryloyloxy) undecanylsulfate (MET) has been synthesized with high purity, and its thermal stability and phase transitions have been studied by thermo gravimetric analysis (TGA) and differential scanning calorimetry (DSC), respectively. MET has been copolymerized in solution with methylmethacrylate (MMA) or styrene (S), initiated by azo-bis-isobutyronitrile (AIBN). The copolymers thus obtained have been studied by Gel Permeation Chromatography (GPC), Transmission Electron Microscopy (TEM), and DSC. Due to the incompatibility between the polar head of the MET units and the non polar S or MMA units, MET units organize in the amorphous polymer matrix and arrange in lamellar structures. [source] | |||||||||||||||||||