Thermodynamic study of ibuprofen by adiabatic calorimetry and thermal analysis

Molar heat capacities of ibuprofen were precisely measured with a small sample precision automated adiabatic calorimeter over the temperature range from 80 to 400 K. The polynomial functions of C-p,C-m (J K-1 mol(-1)) versus T were established on the heat capacity measurements by means of the least fitting square method. The functions are as follows: for solid ibuprofen, at the temperature range of 79.105 K less than or equal to T less than or equal to 333.297 K, C-p,C-m = 144.27 + 77.046X + 3.5171X(2) + 10.925X(3) + 11.224X(4), where X = (T - 206.201)/127.096; for liquid ibuprofen, at the temperature range of 353.406 K less than or equal to T less than or equal to 378.785 K, C-p,C-m = 325.79 + 8.9696X - 1.6073X(2) - 1.5145 X-3, where X = (T - 366.095)/12.690. A fusion transition at T = 348.02 K was found from the C-p-T curve. The molar enthalpy and entropy of the fusion transition were determined to be 26.65 kJ mol(-1) and 76.58 J mol(-1) K-1, respectively. The thermodynamic functions on the base of the reference temperature of 298.15 K, (H-T - H-298.15) and (S-T - S-298.15), were derived. Thermal characteristic of ibuprofen was studied by thermo-gravimetric analysis (TG-DTG) and differential scanning calorimeter (DSC). The temperature of fusion, the molar enthalpy and entropy of fusion obtained by DSC were well consistent with those obtained by adiabatic calorimeter. The evaporation process of ibuprofen was investigated further by TG and DTG, and the activation energy of the evaporation process was determined to be 80.3 +/- 1.4 kJ mol(-1). (C) 2003 Elsevier B.V. All rights reserved.

Stratigraphic Model Predictions of Geoacoustic Properties

Geoacoustic properties of the seabed have a controlling role in the propagation and reverberation of sound in shallow-water environments. Several techniques are available to quantify the important properties but are usually unable to adequately sample the region of interest. In this paper, we explore the potential for obtaining geotechnical properties from a process-based stratigraphic model. Grain-size predictions from the stratigraphic model are combined with two acoustic models to estimate sound speed with distance across the New Jersey continental shelf and with depth below the seabed. Model predictions are compared to two independent sets of data: 1) Surficial sound speeds obtained through direct measurement using in situ compressional wave probes, and 2) sound speed as a function of depth obtained through inversion of seabed reflection measurements. In water depths less than 100 m, the model predictions produce a trend of decreasing grain-size and sound speed with increasing water depth as similarly observed in the measured surficial data. In water depths between 100 and 130 m, the model predictions exhibit an increase in sound speed that was not observed in the measured surficial data. A closer comparison indicates that the grain-sizes predicted for the surficial sediments are generally too small producing sound speeds that are too slow. The predicted sound speeds also tend to be too slow for sediments 0.5-20 m below the seabed in water depths greater than 100 m. However, in water depths less than 100 m, the sound speeds between 0.5-20-m subbottom depth are generally too fast. There are several reasons for the discrepancies including the stratigraphic model was limited to two dimensions, the model was unable to simulate biologic processes responsible for the high sound-speed shell material common in the model area, and incomplete geological records necessary to accurately predict grain-size

The research of rheology and thermodynamics of organic-inorganic hybrid membrane during the membrane formation

To clarify the mechanism of organic-inorganic hybrid membrane formation by phase-inversion method, the thermodynamical and theological properties of PSF/TiO2 casting solution were investigated by the viscosity measurement and the triangle phase diagram, respectively. TiO2 introduction decreased the non-solvent tolerance of casting solution with non-solvent 20% ethanol aqueous solution, which caused thermodynamic enhancement of phase separation, and also resulted in the change of theological properties from Newtonian fluid to non-Newtonian fluid and the viscosity increase of casting solution, which induced rheological hindrance in demixing process

Failure of the plasma-sprayed coating of lanthanum hexaluminate

Lanthanum magnesium hexaluminate (LaMgAl11O19, LMA) is an attractive material for thermal barrier coatings (TBCs), and the failure of its coating was studied in this work by thermal cycling, X-ray diffraction, dilatometric measurement and thermal gravimetric-differential thermal analysis. The dilatometric measurement indicates that even though the bulk material of LMA has a higher sintering-resistance than the typical TBC material, i.e. yttria-stabilized zirconia (YSZ), the plasma sprayed coating of LMA has two serious contractions due to the re-crystallization of LMA and phase transitions of alumina.

catena-Poly[diammonium [diaquabis(pyridine-2,4-dicarboxylato-kappa N-2,O-2)cuprate(II)] [[diaquacopper(II)]-mu-pyridine-2,4-dicarboxylato-kappa N-3,O-2:O-2 '-[tetraaquacadmium(II)]-mu-pyridine-2,4-dicarboxylato-kappa O-3(2):N,O-2 '] hexahydrate]

The title mixed-metal complex, {(NH4)(2)[Cu(C7H3NO4)(2)(H2O)(2)][CdCu(C7H3NO4)(2)(H2O)(6)]center dot 6H(2)O}(n), contains one octahedrally coordinated Cd-II center and two octahedrally coordinated Cu-II centers, each lying on an inversion center. The two Cu-II atoms are each coordinated by two O atoms and two N atoms from two 2,4-pydc (2,4-H(2)pydc = pyridine-2,4-dicarboxylic acid) ligands in the equatorial plane and two water molecules at the axial sites, thus producing two crystallographically independent [Cu(2,4-pydc)(2)(H2O)(2)](2-) metalloligands. One metalloligand exists as a discrete anion and the other connects the Cd(H2O)(4) units, forming a neutral chain.

A polymorph of diaquabis(pyrazine-2-carboxylato-kappa N-2(1),O)copper(II)

The title compound, [Cu(C5H3N2O2)(2)(H2O)(2)], is a new polymorph of the previously reported compound [Klein et al. (1982). Inorg. Chem. 21, 1891-1897]. The Cu-II atom, lying on an inversion center, is coordinated by two N atoms and two O atoms from two pyrazine-2-carboxylate ligands and by two water molecules in a distorted octahedral geometry with the water molecules occupying the axial sites. Intermolecular O-H center dot center dot center dot O, O-H center dot center dot center dot N and C-H center dot center dot center dot O hydrogen bonds connect the complex molecules into a two-dimensional layer parallel to (10 (1) over bar), whereas the previously reported polymorph exhibits a three-dimensional hydrogen-bonded network.

The Surface Modification of Hydroxyapatite Nanoparticles by the Ring Opening Polymerization of gamma-Benzyl-L-glutamate N-carboxyanhydride

The surface modification of hydroxyapatite (HA) nanoparticles by the ring opening polymerization (ROP) of gamma-benzyl-L-glutamate N-carboxyanhydride (BLG-NCA) was proposed to prepare the poly(gamma-benzyl-L-glutamate) (PBLG)-grafted HA nanoparticles (PBLG-g-HA) for the first time. HA nanoparticles were firstly treated by 3-aminopropylthriethoxysilane (APS) and then the terminal amino groups of the modified HA particles initiated the ROP of BLG-NCA to obtain PBLG-g-HA. The process was monitored by XPS and FT-IR. The surface grafting amounts of PBLG on HA ranging from 12.1 to 43.1% were characterized by thermal gravimetric analysis (TGA). The powder X-ray diffraction (XRD) analysis confirmed that the ROP only underwent on the surface of HA nanoparticles without changing its bulk properties. The SEM measurement showed that the PBLG-g-HA hybrid could form an interpenetrating net structure in the self-assembly process.

Hydrothermal Synthesis and Luminescence of Eu-Doped Ba0.92Y2.15F8.29 Submicrospheres

The nonstoichimetric Ba0.92Y2.15F8.29 submicrospheres that piled up by nanoparticles have been prepared via a solution-based method in a hydrothermal environment. The size distribution of the submicrospheres could be tuned by varying the amount of BaCl2. The fluoride source NaBF4 plays an important role in the formation of the submicrospheres. The chelator ethylenediaminetetraacetic acid regulates the growth of the primary nanoparticles as well as the aggregated submicrospheres. The photoluminescence properties of different concentrations of Eu3+-doped Ba0.92Y2.15F8.29 were investigated and the results revealed that the 8% concentration of Eu3+ ions is the optimum doping concentration and the Y3+ ions occupy the site of inversion symmetry.

Deposition of GdVO4 : Eu3+ nanoparticles on silica nanospheres by a simple sol-gel method

The deposition and coating of GdVO4: Eu3+ nanoparticles on spherical silica was carried out using a simple sol - gel method at low temperature. The GdVO4: Eu3+-coated silica composites obtained were characterized by differential thermal analysis (DTA), thermogravimetric (TG) analysis, x-ray diffraction (XRD), Fourier-transform IR spectroscopy (FT-IR), transmission electron microscopy (TEM), x-ray photoelectron spectroscopy (XPS), photoluminescence spectra, and kinetic decay. It is found that the similar to 5 nm GdVO4: Eu3+ nanoparticles coating the silica spheres are crystal in the as-prepared samples and the crystallinity increases with increasing annealing temperature. The composites obtained are spherical in shape with an average size of 100 nm. The GdVO4: Eu3+ nanoparticles are linked with silica cores by a chemical bond. The photoluminescence spectra of the obtained GdVO4: Eu3+-coated silica composites are similar to those of the bulk GdVO4: Eu3+ phosphors. The strongest peak is near 617 nm, which indicates that Eu3+ is located in the low symmetry site with non-inversion centre.

Charge ordering induced metal-semiconductor transition in Ag2BiO3: A first-principles study

Accurate ab initio density-functional calculations are performed to investigate the relationship of the ground-state crystal structures and electronic properties of Ag2BiO3 compound. The results indicate that Ag2BiO3 in Pnna phase, in which the bismuth atoms occupy the same Wyckoff positions, exhibits metallic conductivity, while in Pnn2 and Pn phases, Ag2BiO3 exhibits semiconducting character, which is in agreement with the experimental results. Charge ordering is indeed induced by the crystal inversion twin in the Pnn2 phase compared with the Pnna phase. In the low temperature phase Pn, the charge ordering is similar to that of Pnn2 phase although it is more distorted in Pn phase. In addition, the calculation indicates that the charge ordering is caused in the 6s electron rearrangement.

Preparation of nano-hydroxyapatite/poly(L-lactide) biocomposite microspheres

Nano-hydroxyapatite (HA)/poly(L-lactide) (PLLA) composite microspheres with relatively uniform size distribution were prepared by a solid-in-oil-in-water (s/o/w) emusion solvent evaporation method. The encapsulation of the HA nanopaticles in microshperes was significantly improved by grafting PLLA on the surface of the HA nanoparticles (p-HA) during emulsion process. This procedure gave a possibility to obtain p-HA/PLLA composite microspheres with uniform morphology and the encapsulated p-HA nanoparticle loading reached up to 40 wt% (33 wt% of pure HA) in the p-HA/PLLA composite microspheres. The microstructure of composite microspheres from core-shell to single phase changed with the variation of p-HA to PLLA ratios. p-HA/PLLA composite microspheres with the diameter range of 2-3 mu m were obtained. The entrapment efficiency of p-HA in microspheres could high up to 90 wt% and that of HA was only 13 wt%. Surface and bulk characterizations of the composite microspheres were performed by measurements such as wide angle X-ray diffraction (WAXD), thermal gravimetric analysis (TGA), environmental scanning electron microscope (ESEM) and transmission electron microscopy (TEM).

Structural analysis of PEKEKK(T/I) using WAXD, imaging plates and SAXS

Structures and crystal form transition of the novel aryl ether ketone polymer containing meta-phenylene linkage: PEKEKK(T/I) were investigated by wide angle X-ray diffraction (WAXD), imaging plates (IPs) and small angle X-ray scattering (SAXS). The energy of activation of the decomposition reaction and degree of crystallinity of PEKEKK(T/I) were determined by WAXD and thermo-gravimetric analysis (TGA), respectively. Results obtained from WAXD and IPs show that crystal forms I and II coexist in the PEKEKK(T/I) samples isothermally cold crystallized in the temperature range from 180degreesC to 240degreesC and only form I occurs in PEKEKK(T/I) samples isothermally cold crystallized at 270degreesC. The radius of gyration (Rg), thickness of microregions with electron-density fluctuations (E) and distribution of particle sizes were investigated by SAXS.

In situ circular dichroic electrochemical study of bilirubin and bovine serum albumin complex

The electrooxidation of bilirubin (BR) and bovine serum albumin (BSA) complexes was studied by in situ circular dichroism (CD) spectroelectrochemistry. The result showed that the mechanism of the whole electrooxidation process of this complex corresponded to electrochemical processes (EE mechanism) in aqueous solution. Some parameters of the process were obtained by double logarithm method, differential method and nonlinear regression method. In visible region, CD spectra of the two enantiomeric components of the complex and their fraction distribution against applied potentials were obtained by singular value decomposition least-square (SVDLS) method. Meanwhile, the distribution of the five components of secondary structure was also obtained by the same method in far-UV region. The peak potential gotten from EE mechanism corresponds to a turning point for the component transition, beyond which the whole reaction reaches a new equilibrium. Under applied positive potentials, the enantiomeric equilibrium between M and P form is broken and M form transfers to its enantiomer of P, while the fraction of alpha-helix increases and that improves the transition to P form.

Thermal mechanical and dynamic mechanical property of biphenyl polyimide fibers

High-performance polyimide fibers possess man), excellent properties, e.g., outstanding thermal stability and mechanical properties and excellent radiation resistant and electrical properties. However, the preparation of fibers with good mechanical properties is very difficult. In this report, a biphenvl polyimide from 3,3',4,4'-biphenyltetracarboxylic dianhydride and 4,4'-oxydianiline is synthesized in p-chlorophenol by one-step polymerization. The solution is spun into a coagulation bath of water and alcohol via dry-jet wet-spinning technology. Then, the fibers are drawn in two heating tubes. Thermal gravimetric analysis, thermal mechanical analysis, and dynamic mechanical analysis (DMA) are performed to study the properties of the fibers. The results show that the fibers have a good thermal stability at a temperature of more than 400degreesC. The linear coefficient of thermal expansion is negative in the solid state and the glass transition temperature is about 265degreesC. DMA spectra indicate that the tandelta of the fibers has three transition peaks, namely, alpha, beta, and gamma transition. The alpha and gamma transition temperature, corresponding to the end-group motion and glass transition, respectively, extensively depends on the applied frequency, while the beta transition does not.

Grafting polymerization of L-lactide on the surface of hydroxyapatite nano-crystals

A novel method of grafting ring-opening polymerization of L-lactide (LLA) onto the surface of hydroxyapatite nano-particles (n-HAP) was developed. PLLA was directly connected onto the HAP surface through a chemical linkage. The PLLA-g-HAP particles could be stably dispersed in organic solvent such as chloroform for several weeks. The n-HAP particles still retained the original dimension and shape after the grafting of PLLA. Compared with the P-31 MAS-NMR spectrum of pure HAP powders, there appeared a downfield displacement of 1.2 ppm in the spectrum of PLLA-g-HAP. Fourier transformation infrared (FT-IR) spectra further confirmed the existence of PLLA on the surface of PLLA-g-HAP. The amount of grafted polymer determined by thermal gravimetric analysis (TGA) was about 6% in weight. The tensile strength and elongation at break of the PLLA/PLLA-g-HAP composite containing 8 wt% of PLLA-g-HAP were 55 MPa and about 10-13%, respectively, while those of the PLLA/n-HAP composites were 40 MPa and 3-5%, respectively.