Differential scanning calorimetry has been used to study glassy indomethacin aged at 0 and -10 degrees C for periods of time up to 109 and 210 days, respectively. The results demonstrate the emergence of a small melting peak of the alpha-polymorph after aging for 69 days at 0 degrees C and for 147 days at -10 degrees C (i.e., approximately 55 degrees C below the glass-transition temperature) that provides evidence of nucleation occurring in the temperature region of the beta-relaxation. The evolution of an endothermic recovery peak temperature features a plateau at longer annealing times that suggests that the glass has made significant progress toward reaching the supercooled liquid state. It has been found that the melting peaks become detectable after the recovery peak has reached the plateau. The results highlight the importance of studying physical aging in the temperature region of the beta-relaxation as a means of evaluating the physical stability of amorphous pharmaceutical materials. 相似文献
Summary: Thermogravimetry and differential scanning calorimetry have been used to study the thermal and thermo‐oxidative degradation of polystyrene (PS) and a PS–clay nanocomposite. An advanced isoconversional method has been applied for kinetic analysis. Introduction of the clay phase increases the activation energy and affects the total heat of degradation, which suggests a change in the reaction mechanism. The obtained kinetic data permit a comparative assessment of the fire resistance of the studied materials.
The change in activation energy for the degradation of PS and the PS–clay nanocomposite with the extent of polymer conversion. 相似文献
Staudinger Reactions with Bornanylene(dimethylphosphino)methylimine. Phosphorylation of the Trimethylsilylphosphine Imide formed with Diorganochlorophosphines: unexpected Formation of Compounds with P=N–P–P Units Phosphinimido derivatives of the chiral bornanylene(dimethylphosphino)methyl imine have been obtained from its reactions with trimethylsilyl-, phenyl- and 4-nitrobenzoyl azide. A single crystal X-ray structure determination has been conducted on the 4-nitro-benzoylphosphinimido derivative of bornanylene(dimethylphosphino)methyl imine. The compound was found to crystallize with two independent molecules in the chiral monoclinic space group P21. The trimethylsilylphosphinimido derivative of bornanylene(dimethylphosphino)methyl imine was allowed to react with diorgano-chlorophosphines, with unexpected formation of compounds with PP-bonded RR′2P=N–P(+)R″2–PR″2 groups. The 31P-NMR spectra of two representative compounds are simulated and discussed. 相似文献
Proton transverse relaxation, deuterium and oxygen-17 NMR measurements on functional animal heart muscle were employed to study the distribution and exchange of water protons in the heart. Our nonlinear regression analysis of such data showed the presence of three proton transverse relaxation components that are likely to correspond, respectively, to two major types of water compartments in the heart muscle and the heart muscle matrix. A deuterium exchange study was undertaken to obtain additional information concerning the chemical exchange of water protons/deuterium within these two water compartments, and the effects of proton intermolecular dipolar interactions on the transverse relaxation of water protons. Our results are likely to influence the analysis and interpretation of MRI data for myocardium since it provides details of the microscopic water distribution in the myocardium which is important to the heart function. 相似文献
Pulsed laser deposition (PLD) method was used to obtain bioglass (BG) thin film coatings on titanium substrates. An UV excimer laser KrF* (λ = 248 nm, τ = 25 ns) was used for the multi-pulse irradiation of the BG targets with 57 or 61 wt.% SiO2 content (and Na2O-K2O-CaO-MgO-P2O5 oxides). The depositions were performed in oxygen atmosphere at 13 Pa and for substrates temperature of 400 °C. The PLD films displayed typical BG of 2-5 μm particulates nucleated on the film surface or embedded in. The PLD films stoichiometry was found to be the same as the targets. XRD spectra have shown, the glass coatings obtained, had an amorphous structure. One set of samples, deposited in the same conditions, were dipped in simulated body fluids (SBFs) and subsequently extracted one by one after several time intervals 1, 3, 7, 14 and 21 days. After washing in deionized water and drying, the surface morphology of the samples and theirs composition were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), IR spectroscopy (FTIR) and energy dispersive X-ray analysis (EDX). After 3-7 days the Si content substantially decreases in the coatings and PO43− maxima start to increase in FTIR spectra. The XRD spectra also confirm this evolution. After 14-21 days the XRD peaks show a crystallized fraction of the carbonated hydroxyapatite (HAP). The SEM micrographs show also significant changes of the films surface morphology. The coalescence of the BG droplets can be seen. The dissolution and growth processes could be assigned to the ionic exchange between BG and SBFs. 相似文献
Rotaviruses are the leading cause of diarrhoea in infants around the globe and, under certain conditions they can be present in drinking water sources and systems. Ingestion of 10–100 viral particles is enough to cause disease, emphasizing the need for sensitive diagnostic methods. In this study we have optimized the concentration of rotavirus particles using methacrylate monolithic chromatographic supports. Different surface chemistries and mobile phases were tested. A strong anion exchanger and phosphate buffer (pH 7) resulted in the highest recoveries after elution of the bound virus with 1 M NaCl. Using this approach, rotavirus particles spiked in 1 l volumes of tap or river water were efficiently concentrated. The developed concentration method in combination with a real time quantitative polymerase chain reaction assay detected rotavirus concentrations as low as 100 rotavirus particles/ml. 相似文献
Reaction of the copper precursor [Cu(MeOsaltn)(H2O)] (H2MeOsaltn = N,N′-bis(3-methoxysalicylidene)-1,3-diaminopropane) with Ln(NO3)3·6H2O (Ln = Sm and Tb) and pyrazine-2,3-dicarboxylic acid (H2pyrdic) results in the formation of 1D zigzag chains with the general formula of [Cu(MeOsaltn)Ln(NO3)(pyrdic)]n·nDMF. X-ray crystal structures reveal that the samarium and terbium compounds are isostructural and crystalize in the orthorhombic space group Pbcn. The chains are composed of heterodinuclear copper–lanthanide building blocks which are linked by the pyrazine-2,3-dicarboxylate bridging units. Temperature-dependent susceptibility measurements indicate antiferromagnetic exchange interactions for the samarium–copper chain whereas for the terbium–copper compound ferromagnetic interactions are observed. 相似文献