Melting and Crystallization of Poly(oxyethylene) Mixtures

1995 ◽  
Vol 60 (11) ◽  
pp. 1855-1868 ◽  
Author(s):  
Ivo Lapeš ◽  
Josef Baldrian ◽  
Ján Biroš ◽  
Julius Pouchlý ◽  
Hanes Mio

Solid-liquid eutectic phase diagrams of mixtures of poly(oxyethylene) (M.w. 2 000) with hydroxy and methoxy endgroups, crystallizing in extended-chain macroconformation only, with glutaric acid, benzoic acid or 1,2-diphenylethane are given. The composition dependence of the melting temperature can be fitted by the Flory-Huggins equation. Interaction parameters X and interaction energy densities B evaluated from the diluent branch of the phase diagram are consistent with those obtained from the polymer branch provided the calorimetric value of enthalpy of polymer fusion is used in the latter computation. Measurements of small- and wide-angle X-ray scatterings showed a stacked lamellar structure of POE. Below the eutectic melting point, the long period of the polymer is almost independent of the diluent concentration. On raising temperature gradually from this melting point to the melting point of pure polymer, the increasing long period indicates the penetration of the diluent between the lamellae. As follows from SAXS measurements, the crystallinity of poly(oxyethylene) in the mixtures remains unchanged compared to that of the pure polymer.

2012 ◽  
Vol 191 ◽  
pp. 159-168 ◽  
Author(s):  
Roman Przeliorz ◽  
Jaroslaw Piątkowski

The aim of the studies was to determine the oxidation kinetics of two magnesium alloys, i.e. WE43 and MSR-B, in CO2 atmosphere with and without the addition of 2 vol.% H2O. The rate of oxidation was measured by thermogravimetry in the temperature range of 530-580°C, i.e. below and above the eutectic melting point. The melting point of the eutectic mixture was determined by differential scanning calorimetry (DSC). The corrosion products were analysed by scanning electron microscopy (SEM) and X-ray microanalysis combined with EDS. Studies showed that on the WE43 alloy, a two-layer scale was formed, in which the outer part was composed of yttrium and magnesium oxides, while the inner part contained only yttrium oxide. The scale was found to preserve its good protective properties even above the eutectic temperature. Analysis of the results showed that on the MSR-B alloy, under a thin, uneven layer of scale, the process of internal oxidation occurred, and at a temperature of 580°C, the alloy underwent partial melting


Author(s):  
Noriyuki Kuwano ◽  
Masaru Itakura ◽  
Kensuke Oki

Pd-Ce alloys exhibit various anomalies in physical properties due to mixed valences of Ce, and the anomalies are thought to be strongly related with the crystal structures. Since Pd and Ce are both heavy elements, relative magnitudes of (fcc-fpd) are so small compared with <f> that superlattice reflections, even if any, sometimes cannot be detected in conventional x-ray powder patterns, where fee and fpd are atomic scattering factors of Ce and Pd, and <f> the mean value in the crystal. However, superlattices in Pd-Ce alloys can be analyzed by electron microscopy, thanks to the high detectability of electron diffraction. In this work, we investigated modulated superstructures in alloys with 12.5 and 15.0 at.%Ce.Ingots of Pd-Ce alloys were prepared in an arc furnace under atmosphere of ultra high purity argon. The disc specimens cut out from the ingots were heat-treated in vacuum and electrothinned to electron transparency by a jet method.


1999 ◽  
Vol 82 (08) ◽  
pp. 271-276 ◽  
Author(s):  
Glen Spraggon ◽  
Stephen Everse ◽  
Russell Doolittle

IntroductionAfter a long period of anticipation,1 the last two years have witnessed the first high-resolution x-ray structures of fragments from fibrinogen and fibrin.2-7 The results confirmed many aspects of fibrinogen structure and function that had previously been inferred from electron microscopy and biochemistry and revealed some unexpected features. Several matters have remained stubbornly unsettled, however, and much more work remains to be done. Here, we review several of the most significant findings that have accompanied the new x-ray structures and discuss some of the problems of the fibrinogen-fibrin conversion that remain unresolved. * Abbreviations: GPR—Gly-Pro-Arg-derivatives; GPRPam—Gly-Pro-Arg-Pro-amide; GHRPam—Gly-His-Arg-Pro-amide


Processes ◽  
2021 ◽  
Vol 9 (2) ◽  
pp. 217
Author(s):  
Marin Ugrina ◽  
Martin Gaberšek ◽  
Aleksandra Daković ◽  
Ivona Nuić

Sulfur-impregnated zeolite has been obtained from the natural zeolite clinoptilolite by chemical modification with Na2S at 150 °C. The purpose of zeolite impregnation was to enhance the sorption of Hg(II) from aqueous solutions. Chemical analysis, acid and basic properties determined by Bohem’s method, chemical behavior at different pHo values, zeta potential, cation-exchange capacity (CEC), specific surface area, X-ray powder diffraction (XRPD), scanning electron microscopy with energy-dispersive X-ray analysis (SEM-EDS), Fourier transform infrared spectroscopy (FTIR), as well as thermogravimetry with derivative thermogravimetry (TG-DTG) were used for detailed comparative mineralogical and physico-chemical characterization of natural and sulfur-impregnated zeolites. Results revealed that the surface of the natural zeolite was successfully impregnated with sulfur species in the form of FeS and CaS. Chemical modification caused an increase in basicity and the net negative surface charge due to an increase in oxygen-containing functional groups as well as a decrease in specific surface area and crystallinity due to the formation of sulfur-containing clusters at the zeolite surface. The sorption of Hg(II) species onto the sulfur-impregnated zeolite was affected by the pH, solid/liquid ratio, initial Hg(II) concentration, and contact time. The optimal sorption conditions were determined as pH 2, a solid/liquid ratio of 10 g/L, and a contact time of 800 min. The maximum obtained sorption capacity of the sulfur-impregnated zeolite toward Hg(II) was 1.02 mmol/g. The sorption mechanism of Hg(II) onto the sulfur-impregnated zeolite involves electrostatic attraction, ion exchange, and surface complexation, accompanied by co-precipitation of Hg(II) in the form of HgS. It was found that sulfur-impregnation enhanced the sorption of Hg(II) by 3.6 times compared to the natural zeolite. The leaching test indicated the retention of Hg(II) in the zeolite structure over a wide pH range, making this sulfur-impregnated sorbent a promising material for the remediation of a mercury-polluted environment.


1991 ◽  
Vol 239 ◽  
Author(s):  
J.-M. Baribeau ◽  
D. J. Lockwood

ABSTRACTStrain shift coefficient measurements for longitudinal optical phonons in molecular beam epitaxy grown metastable pseudomorphic Si1−xGex layers on (100) Si (0 < x < 0.35) and Ge (0.80 < x < 1) are reported. Strain in partially relaxed annealed specimens was obtained by double-crystal x-ray diffractometry and the corresponding strain phonon shift was measured by Raman scattering spectroscopy. For epilayers grown on Si it was found that the epilayer Si-Si phonon frequency varies linearly with strain. The magnitude of the strain shift coefficient b however showed a small composition dependence varying from b ≈ -700 cm-1 at x = 0 to b ≈ -950 cm-1 at x = 0.35, corresponding to a stress factor τ = 0.40 + 0.57x: + 0.13x2 cm-1/kbar. For the Ge-Ge vibration mode in epilayers grown on Ge, b decreased from ∼-425 cm-1 at x = 1 to ∼-500 cm-1 at x = 0.8, corresponding to a stress factor τ ≈ 0.52 – 0.14x - 0.08x2 cm-1/kbar.


1989 ◽  
Vol 03 (04) ◽  
pp. 307-311 ◽  
Author(s):  
N. CAO ◽  
J.Q. ZHENG ◽  
X.Y. SHAO ◽  
X.S. CHEN ◽  
W.Y. GUAN

The composition dependence of superconductivity and crystal structure in La ( Ba 1−x Ca x)2 Cu 3 O 7−y system was determined by the resistivity measurements and X-ray diffraction analysis. The superconducting transition temperature is raised with the increase of Ca content till x=0.6, at which the zero resistance temperature of the sample is 81.5 K. In the meanwhile, the crystal structure of the sample changed from tetragonal (x=0) to orthorhombic structure (x=0.2, 0.4, 0.6). With further increase of Ca content, the superconductivity decrease for the sample of x=0.8 with mixed phases including the orthorhombic oxygen-deficient perovskite-like (ODP) structure and no superconducting transition is found at 4.2 K for the sample of x=1 without the ODP structure. A possible explanation of these experimental results is given.


1992 ◽  
Vol 7 (7) ◽  
pp. 1751-1761 ◽  
Author(s):  
J. Eckert ◽  
J.C. Holzer ◽  
C.E. Krill ◽  
W.L. Johnson

Nanocrystalline fcc metals have been synthesized by mechanical attrition. The crystal refinement and the development of the microstructure have been investigated in detail by x-ray diffraction, differential scanning calorimetry, and transmission electron microscopy. The deformation process causes a decrease of the grain size of the fcc metals to 6–22 nm for the different elements. The final grain size scales with the melting point and the bulk modulus of the respective metal: the higher the melting point and the bulk modulus, the smaller the final grain size of the powder. Thus, the ultimate grain size achievable by this technique is determined by the competition between the heavy mechanical deformation introduced during milling and the recovery behavior of the metal. X-ray diffraction and thermal analysis of the nanocrystalline powders reveal that the crystal size refinement is accompanied by an increase in atomic-level strain and in the mechanically stored enthalpy in comparison to the undeformed state. The excess stored enthalpies of 10–40% of the heat of fusion exceed by far the values known for conventional deformation processes. The contributions of the atomic-level strain and the excess enthalpy of the grain boundaries to the stored enthalpies are critically assessed. The kinetics of grain growth in the nanocrystalline fcc metals are investigated by thermal analysis. The activation energy for grain boundary migration is derived from a modified Kissinger analysis, and estimates of the grain boundary enthalpy are given.


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