171 resultados para Two-phase experiments


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Differential scanning calorimeter (DSC), wide-angle X-ray diffraction (WAXD), small-angle X-ray scattering (SAXS), and density techniques have been used to investigate the structural parameters of the solid state of Nylon 11 annealed at different temperatures. The equilibrium heat of fusion Delta H-m(0) and equilibrium melting temperature T-m(0) were estimated to be 189.05 J g(-1) and 202.85 degrees C respectively by using the Hoffman-Weeks approach. The degree of crystallinity (W-c,W-x) ranged approximately 24-42% was calculated by WAXD and compared with those by calorimetry (W-c,W-h) and density (W-c,W-d) measurements. The radius of gyration R-g, crystalline thickness L-c, noncrystalline thickness L-a, long period L, semiaxes of the particles (a, b), electron-density difference between the crystalline and noncrystalline regions eta(c) - eta(a), and the invariant Q increased with increasing annealing temperature. The analysis of the SAXS data was based upon the particle characteristic function and the one-dimensional electron-density correlation function. An interphase region existed between the crystalline and noncrystalline region with a clear dimension of about 2 nm for semicrystalline Nylon 11. Instead of the traditional two-phase model, a three-phase model has been proposed to explain these results by means of SAXS.

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Polyaniline (PANI), a member of the intrinsically conducting polymer (ICPs) family, was blended with polyamide-11 (polyco-aminoundecanoyle) in concentrated sulfuric acid. The above solution was used to spin conductive PANI/polyamide-11 fibers by wet-spinning technology. Scanning electron microscope (SEM) and transmission electron microscope (TEM) were employed to study the two-phase morphology of the conductive PANI/polyamide-11 fibers. The micrographs of the cross-section, the axial section and the surface of the monofilament demonstrated that the two blend components were incompatible. The morphology of PANI in the fibers was of fibrillar form, which was valuable for producing conducting channels. The electrical conductivity of the fibers was from 10(-6) to 10(-1) S/cm with the different PANI fraction and the percolation threshold was about 5 wt.%. By comparing the two blend systems of PANI/Polyamide-11 fibers and carbon black filled poly(ethylene terephthalate) (PET) fibers, it was shown that the morphology of the conductive component had an influence on electrical conductivity, The former had higher conductivity and lower percolation threshold than the latter. (C) 2001 Elsevier Science B.V. All rights reserved.

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In this work some basic constants of extractant Sec-Octylphenoxy acetic acid (CA-12) such as solubility (S) in water, dissociation constant (K-a) in aqueous solution, dimerization constant( K-2) and distribution constant (K-d) between water and haptane have been determined by two phase titration method. The results are as follows: S = 1.40 x 10(-4) mol/L, K-a = 3.02 x 10(-4), K-2 = 3.56 x 10(2), K-d = 4.06 x 10(2) (25 +/-0.5 degreesC).

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The interface thickness in two-component interpenetrating polymer networks (IPN) system based on polyacrylate and epoxy were determined using small-angle X-ray scattering (SAXS) in terms of the theory proposed by Ruland. The thickness was found to be nonexistent for the samples at various compositions and synthesized at variable conditions-temperature and initiator concentration. By viewing the system as a two-phase system with a sharp boundary, the roughness of the interface was described by fractal dimension, D, which slightly varies with composition and synthesis condition. Length scales in which surface fractals are proved to be correct exist for each sample and range from 0.02 to 0.4 Angstrom(-1). The interface in the present IPN system was treated as fractal, which reasonably explained the differences between Pored's law and experimental data, and gained an insight into the interaction between different segments on the interface. (C) 1997 Elsevier Science Ltd.

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Blends of a poly(ether sulfone) (PES) and a polycarbonate (PC) were prepared by melt-mixing and were studied by tensile tests, differential scanning calorimetry, dynamic mechanical analysis, density measurements and transmission electron microscopy (TEM). The blends were found to be two-phase systems and an interfacial layer was presumed to be formed between two phases, which was verified by TEM. A synergism of elongation at break and tensile modulus was shown in PES/PC blends. The effects of the crosshead speed on the mechanical properties were discussed for blends with different PES/PC weight ratios.

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The blend polyamide 1010/N,N'-(diphenylmethane-4,4'-diyl)bismaleimide (PA1010/ BMI) has been investigated by means of WAXD and SAXS. The results obtained with the help of the Ruland, variance and 1D EDCF analysis showed that the degree of crystallinity (W-c,W-x), crystallite size (L(hikl)), long period (L) and thickness of average crystal lamellae (d) decrease with BMI content. Experimental and calculated density values (rho(c)) are in good agreement. Addition of BMT to PA1010 causes an increase in structural distortion. The results from SAXS analysis also supported that a crystalline amorphous interphase exists in the lamellae of semicrystalline polymers, so that a three-phase model instead of the traditional two-phase model should be used.

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The estimate formulas for the two-phase structure seminvariants (TPSSs) in the presence of anomalous scattering are obtained from the estimate of the two-phase structure invariants [Hauptman (1982). Acta Cryst. A38, 632-641; Giacovazzo (1983). Acta Cryst.

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Blends of poly[3,3-bis(chloromethyl)oxetane] (Penton) with poly(vinyl acetate) were prepared. Compatibility, morphology, thermal behavior, and mechanical properties of blends with various compositions were studied using differential scanning calorimetry (DSC), dynamic mechanical measurements (DMA), tensile tests, and scanning electron microscopy (SEM). DMA study showed that the blends have two glass transition temperatures (T(g)). The T(g) of the PVAc rich phase shifts significantly to lower temperatures with increasing Penton content, suggesting that a considerable amount of Penton dissolves in the PVAc rich phase, but that the Penton rich phase contains little PVAc. The Penton/PVAc blends are partially compatible. DSC results suggest that PVAc can act as a beta-nucleator for Penton in the blend. Marked negative deviations from simple additivity were observed for the tensile strength at break over the entire composition range. The Young's modulus curve appeared to be S-shaped, implying that the blends are heterogeneous and have a two-phase structure. This was confirmed by SEM observations.

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The low-frequency Raman spectrum of n-decylammonium chloride was measured as a function of temperature in the temperature range from 290 to 340K, and the longitudinal acoustical mode vibration band was assigned. The results showed that there are two phase transitions at 313K and 321K, respectively. The phase transition at 313K is mainly induced by change of hydrocarbon chain conformations, while that at 321K is mainly induced by change of order degree of molecular packing. The results suggest low-frequency Raman spectroscopy is a useful probe of structural phase transition for long-chain compounds.

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Polyoxypropylene glycol (PPG) (or castor oil) and toluene diisocyanate (TDI) were mixed, and the prepolymer polyurethane (PU) (I) was formed. Vinyl-terminated polyurethane (II) was prepared from (I), and hydroxyethyl acrylate, AB crosslinked polymers (ABCPs) were synthesized from (II) and vinyl monomers such as styrene, methyl methacrylate, vinyl acetate, etc. The dynamic mechanical properties and morphology of ABCPs were measured. The ABCPs based on PPG have double glass transition temperatures (T(g)) on the sigma-vs. temperature curves. They display a two-phase morphology with plastic components forming the continous phase and PU-rich domains forming the separated phase on the electron micrographs. Irregular shapes and a highly polydisperse distribution of PU-rich domain sizes were observed. The crosslink density of ABCPs has a notable effect on the morphology and properties. The average diameter of the PU-rich domains depends on the molecular weight of prepolymer PPG. The highly crosslinked structures will produce large numbers of very small domains. ABCPs based on castor oil show a single T(g) relaxation on the dynamic mechanical spectra. The compatibility between the two components is much better in ABCPs based on castor oil than in those based on PPG, because there is a high crosslink density in the former. Comparison of the dynamic mechanical spectra of ABCP and interpenetrating networks (IPN) based on castor oil with similar crosslink density and composition imply that the two components in ABCP are compatible whereas microphase separation occurs in IPN. An improvement in the compatibility is achieved by the crosslinking between the two networks.

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The properties of miscible phenolphthalein poly(ether ether ketone)/phenoxy (PEK-C/phenoxy) blends have been measured by dynamic mechanical analysis and tensile testing. The blends were found to have single glass transition temperatures (T(g)) that vary continuously with composition. The tensile moduli exhibit positive deviations from simple additivity. Marked positive deviations were also observed for tensile strength. The tensile strengths of the 90/10 and 75/25 PEK-C/phenoxy blends are higher than those of both the pure components. Embrittlement, or transition from the brittle to the ductile mode of failure, occurs in the composition range of 50-25 wt% PEK-C. These observations suggest that mixing on the segmental level has occurred and that there is enough interaction between the components to decrease its internal mobility significantly. PEK-C was also found to be miscible with the epoxy monomer, diglycidyl ether of bisphenol A (DGEBA), as shown by the existence of a single glass transition temperature (T(g)) within the whole composition range. Miscibility between PEK-C and DGEBA could be considered to be due mainly to entropy. However, PEK-C was judged to be immiscible with the diaminodiphenylmethane-curved epoxy resin (DDM-cured ER). It was observed that the PEK-C/ER blends have two T(g), which remain invariant with composition and are almost the same as those of the pure components, respectively. Scanning electron microscopy showed that the PEK-C/ER blends have a two-phase structure. The different miscibility with PEK-C between DGEBA and the DDM-cured ER is considered to be due to the dramatic change in the chemical and physical nature of ER after curing.

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Satellite and in situ observations in the equatorial Atlantic Ocean during 2002-03 show dominant spectral peaks at 40-60 days and secondary peaks at 10-40 days in sea level and thermocline within the intraseasonal period band (10-80 days). A detailed investigation of the dynamics of the intraseasonal variations is carried out using an ocean general circulation model, namely, the Hybrid Coordinate Ocean Model (HYCOM). Two parallel experiments are performed in the tropical Atlantic Ocean basin for the period 2000-03: one is forced by daily scatterometer winds from the Quick Scatterometer (QuikSCAT) satellite together with other forcing fields, and the other is forced by the low-passed 80-day version of the above fields. To help in understanding the role played by the wind-driven equatorial waves, a linear continuously stratified ocean model is also used. Within 3 degrees S-3 degrees N of the equatorial region, the strong 40-60-day sea surface height anomaly (SSHA) and thermocline variability result mainly from the first and second baroclinic modes equatorial Kelvin waves that are forced by intraseasonal zonal winds, with the second baroclinic mode playing a more important role. Sharp 40-50-day peaks of zonal and meridional winds appear in both the QuikSCAT and Pilot Research Moored Array in the Tropical Atlantic (PIRATA) data for the period 2002-03, and they are especially strong in 2002. Zonal wind anomaly in the central-western equatorial basin for the period 2000-06 is significantly correlated with SSHA across the equatorial basin, with simultaneous/ lag correlation ranging from-0.62 to 0.74 above 95% significance. Away from the equator (3 degrees-5 degrees N), however, sea level and thermocline variations in the 40-60-day band are caused largely by tropical instability waves (TIWs). On 10-40-day time scales and west of 10 degrees W, the spectral power of sea level and thermocline appears to be dominated by TIWs within 5 degrees S-5 degrees N of the equatorial region. The wind-driven circulation, however, also provides a significant contribution. Interestingly, east of 10 W, SSHA and thermocline variations at 10 40- day periods result almost entirely from wind-driven equatorial waves. During the boreal spring of 2002 when TIWs are weak, Kelvin waves dominate the SSHA across the equatorial basin (2 degrees S-2 degrees N). The observed quasi-biweekly Yanai waves are excited mainly by the quasi-biweekly meridional winds, and they contribute significantly to the SSHA and thermocline variations in 1 degrees-5 degrees N and 1 degrees-5 degrees S regions.

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Distribution of dimethylsulfide (DMS) and/or particulate dimethylsulfoniopropionate (DMSPp) concentrations in the Jiaozhou Bay, Zhifu Bay and East China Sea were investigated during the period of 1994 - 1998. Both DMS and DMSPp levels showed remarkable temporal and spatial variations. High values occurred in the coastal or shelf waters and low values in the offshore waters. The highest levels were observed in spring or summer and lowest in autumn. DMS or DMSPp distribution patterns were associated with water mass on a large geographical scale, while biological and chemical factors were more likely influential on smaller-scale variations. Diatoms could play an important role in total DMS or DMSPp abundance in coastal waters. Nitrate was found to have a two-phase relationship with DMSPp concentrations: positive when nitrate concentration was lower than 1 mumol/L, and negative when it was above. Anthropogenic factors such as sewage input and aquaculture also showed influences on DMS or DMSPp concentration.

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Supercritical fluid extraction (SFE) was used to extract homoisoflavonoids from Ophiopogon japonicus (Thunb.) Ker-Gawler. The optimization of parameters was carried out using an orthogonal test L-9 (3)(4) including pressure, temperature, dynamic extraction time and the amount of modifier. The process was then scaled up by 100 times with a preparative SFE system under the optimized conditions of 25 MPa, 55 degrees C, 4.0 h and 25% methanol as a modifier. Then crude extracts were separated and purified by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of n-hexane/ethyl acetate/methanol/ACN/water (1.8:1.0:1.0:1.2:1.0 v/v). There three homoisoflavonoidal compounds including methylophiopogonanone A 6-aldehydo-isoophiopogonone A, and 6-formyl-isoophiopogonanone A, were successfully isolated and purified in one step. The collected fractions were analyzed by HPLC. In each operation, 140 mg crude extracts was separated and yielded 15.3 mg of methylophiopogonanone A (96.9% purity), 4.1 mg of 6-aldehydo-isoophiopogonone A (98.3% purity) and 13.5 mg of 6-formyl-isoophiopogonanone A (97.3% purity) respectively. The chemical structure of the three homoisoflavonoids are identified by means of ESI-MS and NMR analysis.

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High-speed counter-current chromatography (HSCCC) technique in semi-preparative scale has been successfully applied to the separation of bioactive flavonoid compounds, liquiritigenin and isoliquiritigenin in one step from the crude extract of Glycyrrhiza uralensis Risch. The HSCCC was performed using a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-acetonitrile-water (2:2:1:0.6:2, v/v). Yields of liquiritigenin (98.9% purity) and isoliquiritigenin (98.3% purity) obtained were 0.52% and 0.32%. Chemical structures of the purified liquiritigenin and isoliquiritigenin were identified by electrospray ionization-MS (ESI-MS) and NMR analysis. (c) 2005 Published by Elsevier B.V.