FTIR, XRD, SEM and solid state NMR investigations of carbonate-containing hydroxyapatite nano-particles synthesized by hydroxide-gel technique

Nano-crystalline hydroxyapatite (HA), Ca₁₀(PO₄)₆(OH)₂ has been synthesized by a precipitate conversion technique using hydroxide gel at lower temperatures, e.g. 80 °C. HA crystallizes in hexagonal structure (space group: P6₃/m) having lattice parameters: and and around 17 nm in crystallite-size for the 80 °C-heated sample. SEM micrographs show hexagonal crystallites of average particle dimensions approximately 50×20 nm for 80 °C heated sample. The structure analysis by XRD, FTIR, ¹H and ³¹P MAS NMR show the existence of structural disorder at the particle surface that either does not form hydrogen bonding due to lack of adequate bonding parameters or forms a very weak dipolar bonding. The structural disorder has been explained as a result of chemical interactions between the phosphate groups either with the surface adsorbed water or the hydroxyl groups at the surface of the nano-particles.     

Isolation and characterization of kallosin A,a novel rearranged pseudopterane diterpenoid from the Caribbean sea plume Pseudopterogorgia kallos (Bielschowsky)

The Caribbean alcyonacean Pseudopterogorgia kallos is shown to contain a novel rearranged pseudopterane diterpene, kallosin A (1), possessing several unusual structural features. In addition to having two distinct 2(3H)- and 2(5H)-furanone moieties, kallosin A is based on a new carbon skeleton. The structural assignment of 1 was based mainly on 1D and 2D NMR spectral data and was further supported by accurate mass measurement and single-crystal X-ray diffraction analysis.     

Pre-equilibrium dipole strength in charge asymmetric peripheral heavy-ion reactions

We report on the results obtained from the study of the ³²S + ⁶⁴Ni and ³²S + ⁵⁸Ni peripheral reactions at incident energies E _lab = 288 MeV and E _lab = 320 MeV, respectively. High-energy γ-rays were detected in an array of 8 seven-pack BaF₂ clusters. Coincidence with complex fragments detected in 12 three-stage telescopes ensured the selection of peripheral reaction events. All of the relevant reaction parameters were kept constant with the exception of the different initial dipole moment caused by the different entrance channel charge asymmetry. While for quasi-elastic events no N/Z effect was observed in the differential γ-ray multiplicities of the two reactions, for deep-inelastic events a larger dipole γ-ray emission occurs during the more N/Z asymmetric reaction. A theoretical interpretation based on a collective Bremsstrahlung analysis of the reaction dynamics is presented. Received: 26 September 2002 / Accepted: 13 November 2002 / Published online: 6 March 2003 RID="a" ID="a"e-mail: pierroutsakou@na.infn.it RID="b" ID="b"Present address: INFN, Laboratori Nazionali di Legnaro, Padova, Italy. Communicated by C. Signorini     

Neutron diffraction structure of Y2V10O28·24H2O at 297 and 60 K

The structure of yttrium-decavanadate-24-hydrate, [Y₂V₁₀O₂₈·24H₂O], was determined by neutron diffraction at temperatures of 297 and 60 K. Space group P-1, triclinic, Z = 2; at 297 K : a = 9.36(1), b = 9.86(1), c = 23.53(3) Å, = 98.79(2), = 98.15(2), = 89.30(2), V = 2123(5); at 60 K : a = 9.19(3), b = 9.85(3), c = 23.31(12) Å, = 99.03(3), = 98.99(6), = 89.39(6)°, V = 2058(13). Final R factors of 10 and 9.4% were obtained using 1955 and 1100 observed structure factors at both temperatures, respectively. The position of the 24 water molecules was determined and the characteristics of the hydrogen bonds were analyzed at both temperatures.     

Magnetic properties of aerugite Co<Subscript>10</Subscript>Ge<Subscript>3</Subscript>O<Subscript>16</Subscript>

This paper reports on the first study of the temperature and field dependences of the magnetization, heat capacity, and electrical properties of synthesized polycrystalline samples of aerugite Co₁₀Ge₃O₁₆, as well as on x-ray diffraction analysis of this compound. It is shown that the cobalt ions in this compound occupy three nonequivalent positions. The results of the experimental and theoretical studies suggest that aerugite is a ferrimagnet with two uncompensated magnetic moments of the cobalt atom per formula unit.     

Syntheses and optoelectronic properties of quinoxaline polymers: The effect of donor unit

Tuning the bandgap of electrochromic polymers is one of the important research topics in electrochromism. To understand clearly the effect of donor unit in donor–acceptor–donor‐type polymers, 2,3‐bis(4‐tert‐butylphenyl)‐5,8‐di(thiophen‐2‐yl)quinoxaline and 2,3‐bis(4‐tert‐butylphenyl)‐5‐(2,3‐dihydrothieno[3,4‐b][1,4]dioxin‐ 5‐yl)‐8‐(thiophen‐2‐yl)quinoxaline were synthesized and polymerized potentiodynamically. Their electrochemical and spectroelectrochemical studies were performed, and the results were compared with those of poly(2,3‐bis(4‐tert‐butylphenyl)‐5,8‐bis(2,3‐dihydrothieno[3,4‐b][1,4]dioxin‐5‐yl)quinoxaline) (Gunbas et al., Adv Mater 2008, 20, 691–695). A blue shift in the polymer π–π* transitions revealed that the bandgap of such polymers with the same acceptor unit is related to the electron density of donor units. © 2011 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2011     

An efficient catalytic method for the Beckmann rearrangement of ketoximes to amides and aldoximes to nitriles mediated by propylphosphonic anhydride (T3P®)

An efficient method for the Beckmann rearrangement of ketoximes to amides mediated by a catalytic amount (15 mol %) of propylphosphonic anhydride (T3P®) is described. Aldoximes underwent second order Beckmann rearrangement to provide the corresponding nitriles in excellent yields on reacting with T3P (15 mol %) at room temperature. The main advantages of this environmentally friendly protocol include procedural simplicity, and particularly ease of isolation of the products.     

Calculation of geometrical coupling coefficients for the hyperspherical harmonics approach

An elegant and fast method for the calculation of geometrical structure coefficients needed for an expansion of a few-body wavefunction and interaction in hyperspherical harmonics has been proposed. A sum rule for the GSC has also been derived, which is useful for an independent check of the coefficients. The proposed method of computation is many orders of magnitude faster than conventional methods.     

An HPTLC Method for the Simultaneous Analysis of Compactin and Citrinin in Penicillium citrinum Fermentation Broth

JPC – Journal of Planar Chromatography – Modern TLC - A simple and precise high-performance thin-layer chromatographic (HPTLC) method has been established for simultaneous analysis of...