Morphology and structure of poly(di-n-butylsilane) single crystals prepared by controlling kinetic process of solvent evaporation

The silicon backbone conformation in poly(di-n-butylsilane) (PDBS) has been shown to be a 7/3 helix at ambient conditions, which is in marked contrast to the near-planar conformation of its homologous polymers with side chain lengths of one to three or six to eight carbon atoms. In this work, both the 7/3 helical and near-planar chain conformations are achieved by controlling the solvent evaporation rate around room temperature. The chain conformation and crystal structure obtained in this method have been correlated to the crystal morphology by wide-angle X-ray diffraction, transmission electron microscopy, electron diffraction, optical microscopy, atomic force microscopy, and UV absorption spectrum. The lath-shaped single crystals obtained at 12 degreesC correspond to an orthorhombic form with near-planar chain conformation whereas the lozenge-shaped single crystals obtained at 30 degreesC (in coexistence with the lath-shaped crystals) are orthohexagonal with a 7/3 helix.

Morphology-controllable synthesis and characterization of single-crystal molybdenum trioxide

Molybdenum trioxide nanobelts and prism-like particles with good crystallinity and high surface areas have been prepared by a facile hydrothermal method, and the morphology could be controlled by using different inorganic salts, such as KNO3, Ca(NO3)(2), La(NO3)(3), etc. The possible growth mechanism of molybdenum trioxide prism-like particles is discussed on the basis of the presence of HI and the modification of metal cations. The as-prepared nanomaterials are characterized by means of powder X-ray diffraction (PXRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), Fourier transformation infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and ultraviolet and visible spectroscopy (UV-vis). TEM and HRTEM micrographs show that the molybdenum trioxide nanobelts and prism-like particles have a relatively high degree of crystallinity and uniformity. BET specific surface areas of the as-prepared molybdenum trioxide nanocrystals are 67-79 m(2)g(-1). XPS analysis indicates that the hexavalent molybdenum is predominant in the nanocrystals. UV-vis spectra reveal that the direct band gap energy of the annealed molybdenum trioxide prism-like particles shows a pronounced blue shift compared to that of bulk MoO3 powder.

An one-pot epitaxial growth method to synthesize cactus-like ZnO

In this work, we have developed a one-pot, morphology controlled epitaxial growth method to synthesize novel cactus-like ZnO in solution. Utilizing zinc acetate and hexamethylenetetramine as the precursors, ZnO nanorods synthesized in the first step remained in the solution, without any separation, served directly as the matrix for the epitaxial growth in the second step. Control experiments revealed that a proper mass of precursors added in the second step was crucial to form cactus-like ZnO. The as-synthesized ZnO was single crystalline and possessed three photoluminescence emissions centered at 390, 425 and 490 run. Finally, a possible mechanism for the epitaxial growth ZnO was proposed and discussed.

Growth and vibrational spectra of doped KMgF3 single crystal

The different ions doped KMgF3 single crystals are prepared by the vertical Bridgman method. The near-infrared absorption spectra for different parts of all as-growth crystals indicate that there is the best transparency in middle part. The correlation between the vibronic frequencies of Eu2+ and the site displacement of Cu+ co-doped ions is firstly studied, which indicates that Cu+ ions replace the site of the Mg2+ ions. The co-doped Eu2+ counteracts the charge misfit causing by the replacement of Mg2+ with Cu+. The overlapping of the emission spectra of the Eu2+ and the excitation spectra of the Cu+ results in the energy transfer from Eu2+ to Cu+.

Study of color centers and trace oxygen in KMgF3 : Eu single crystal

Using the Bridgeman-Stockbarger method, the KMgF3:EU2+ single crystal was grown. The color centers in unirradiated KMgF3:Eu crystal were studied. By thermal annealing, we confirmed the 422-nm emission resulted from color centers and oxygen centers, and we proved the energy transfer from EU2+ to color centers. From spectra, the relative oxygen content in crystal was calculated, and the relationships of oxygen displacing fluorine were studied.

Investigating mechanical response of single chain polystyrene particles by scanning probe techniques

Single chain polystyrene particles were obtained by dilute solution casting method. The sample with both single chain polystyrene particles and multi-chain (more than 1000 molecular chains) polystyrene particles was obtained by a little more concentrate solution. Force modulation technique showed that single chain polystyrene particles were softer than multichain polystyrene particles. On the other hand, nanoindentation experiments on multi-chain particles and bulk polystyrene manifested that the elastic modulus of multi-chain polystyrene particles was very close to that of bulk polystyrene. Therefore, it was concluded that single chain polystyrene particles were softer than bulk polystyrene,which indicated that the density of intrachain entanglement points in the single chain polystyrene particles was not as large as that of the interchain entanglement points in the bulk state.

Estimation of individual phases from the four-phase structure invariants in the single isomorphous replacement case

The probability distribution of the four-phase invariants in the case of single isomorphous replacement has been developed to estimate some individual phases. An example of its application to obtain the phases having special values of 0, pi or +/-pi /2 is given for a known protein structure in space group P2(1)2(1)2(1). The phasing procedure includes the determination of starting phases and an iterative calculation. The initial values of starting phases, which are required by the formula, can be obtained from the estimate of one-phase seminvariants and by specifying the origin and enantiomorph. In addition, the calculations lead to two sets of possible phases for each type of reflection by assigning arbitrarily an initial phase value. The present method provides a possibility for the multisolution technique to increase greatly the number of known phases while keeping the number of the trials quite small.

High resolution electron microscopy study of single chain single crystals of gutta percha

Single chain single crystals (SCSC) of gutta percha (GP) were prepared by a dilute-solution spraying method. Electron diffraction (ED) patterns revealed that the single chain single crystal was of a new crystalline modification, the delta form. The images of SCSC of GP obtained with a high resolution electron microscope (HREM) showed a two dimensional periodic structure. Most of the images consisted of lattice fringes derived from the (001) zone. This is the first time that the single chain single crystal images of GP have been observed at a molecular level. Micrographs were image processed using optical filtering methods to improve the signal-to-noise ratio, and were compared with computer-generated simulations of the images. From the viewpoint of the defects seen in high resolution images, the crystal formation and melting processes are discussed. (C) 1998 Elsevier Science Ltd. All rights reserved.

A novel electrochemical method for simultaneously measuring diffusion coefficient and ion transference number

This paper introduces a new method to estimate the diffusion coefficient and transference number of a salt or an electroactive ion in a solution with little or no supporting electrolyte. The above two parameters can be obtained from a single potential step experiment without previous knowledge of either one. It would appear that the method could also be used in the study of ion transport in a high viscosity solvent or a solid electrolyte. (C) 1998 Elsevier Science S.A.

ESTIMATION OF THE ONE-PHASE STRUCTURE SEMINVARIANTS IN THE SINGLE ISOMORPHOUS REPLACEMENT CASE - AN APPLICATION OF HAUPTMANS DISTRIBUTION

A method for estimating the one-phase structure seminvariants (OPSSs) having values of 0 or pi has been proposed on the basis of the probabilistic theory of the three-phase structure invariants for a pair of isomorphous structures [Hauptman (1982). Acta Cryst. A38, 289-294]. The test calculations using error-free diffraction data of protein cytochrome c(550) and its PtCl42- derivative show that reliable estimates of a number of the OPSSs can be obtained. The reliability of the estimation increases with the increase of the differences between diffraction intensities of the native protein and its heavy-atom derivative. A means to estimate the parameters of the distribution from the diffraction ratio is suggested.

LUMINESCENCE AND ENERGY-TRANSFER IN GDP5O14-EU3+,SM3+ SINGLE-CRYSTALS

In this paper we report on the luminescence and energy transfer in GdP4O14:Eu3+,Sm3+ (GdPP:Eu,Sm) in single crystals grown by the hydrothermal method. The room temperature excitation, emission, absorption and IR spectra of the crystals have been measured and analysed. The energy transfer from Gd3+ and Sm3+ to Eu3+ ions in GPP:Eu,Sm crystals is also discussed.

DETERMINATION OF PARAMETERS OF FAST CHEMICAL REACTION OF ALIZARIN RED S BY SPECTROELECTROCHEMICAL METHOD WITH LOPTLC

The rate constant of very fast chemical reaction generally can be measured by electrochemical methods, but can not by the thin layer electrochemical methods because of the influence of diffusion effect. Long optical path length thin layer cell (LOPTLC) with large ratio of electrode area to solution volume can be used to monitor the fist chemical reaction in situ with high sensitivity and accuracy. It enable the adsorption spectra to be measured without the influence of diffusion effect. In the present paper, a fast chemical reaction of Alizarin Red S (ARS) with its oxidative state has been studied. The reaction equilibrium constant (K) under different potentials can be determined by single step potential-absorption spectra in LOPTLC. An equilibrium constant of 7.94 x 10(5) l.mol(-1) for the chemical reaction has been obtained from the plot of lgK vs. (E - E-1(0)'). Rate constant (k) under different potentials can be measured by single step potential-chronoabsorptiometry. A rate constant of 426.6 l.mol(-1).s(-1) for the chemical reaction has been obtained from the plot of lgK vs. (E - E-1(0)') with (E - E-1(0)') = 0.

Method for large-scale isolation and purification of R-phycoerythrin from red alga Polysiphonia urceolata Grev

R-phycoerythrin was isolated and purified from a red alga, Polysiphonia urceolata Grev, using Streamline column combined with ion-exchange chromatography or hydroxyapatite chromatography. The purity of R-phycoerythrin isolated by Streamline column was up to 1.66 and the yield of R-phycoerythrin could be as high as 0.68 mg/g frozen P. urceolata. All the eluates from Streamline column were divided into two equivalent parts, respectively. One part was pumped into the ion-exchange column loaded with Q-Sepharose and the other was applied to the adsorption column loaded with hydroxyapatite. The purities of R-phycoerythrin purified using these two methods were both up to 3.26, more than 3.2 the commonly accepted criterion. The yield of purified R-phycoerythrin from the ion-exchange chromatography was 0.40 mg/g frozen P. urceolata and that from the hydroxyapatite chromatography could reach 0.34 mg/g frozen P. urceolata. The purified protein had three absorption peaks at 498, 535, and 565 nm and displayed a fluorescence maximum at 580 nm, which was consistent with the typical spectrum of R-phycoerythrin. The purified R-PE was also identified with electrophoresis. Only one single protein band appeared on native-PAGE with silver staining. SDS-PAGE demonstrated the presence of one 20 kDa major subunit, and one low intensity band corresponding to 33 kDa subunit. The results indicate that using the expanded bed adsorption combined with ion-exchange chromatography or hydroxyapatite chromatography, R-phycoerythrin can be purified from frozen P. urceolata on large scale. (c) 2006 Elsevier Inc. All rights reserved.

Mining expressed sequences for single nucleotide polymorphisms in Pacific abalone Haliotis discus hannai

Although single nucleotide polymorphisms (SNPs) are important resources for population genetics, pedigree analysis and genomic mapping, such loci have not been reported in Pacific abalone so far. In this study, a bioinformatics strategy was adopted to discover SNPs within the expressed sequences (ESTs) of Pacific abalone, Haliotis discus hannai, and furthermore, polymerase chain reaction direct sequencing (PCR-DS) and allele-specific PCR (AS-PCR) were used for SNPs detection and genotype scoring respectively. A total of 5893 ESTs were assembled and 302 putative SNPs were identified. The average density of SNPs in ESTs was 1%. Fifty-two sets of sequencing primers were designed from SNPs flanking ESTs to amplify the genomic DNA, and 13 could generate products of expected size. Polymerase chain reaction direct sequencing of the amplification products from pooled DNA samples revealed 40 polymorphic SNP loci. Using a modified tetra-primer AS-PCR, seven mitochondrial and six nuclear SNPs were typed and characterized among 37 wild abalones. In conclusion, it is feasible to discover SNPs from number limited ESTs and the AS-PCR as a simple, robust and reliable assay could be a primary method for small- and medium-scale SNPs detection in abalones as well as other non-model organisms.

Total analytical method for Radix astragali extract using two-binary multi-segment gradient elution liquid chromatography

There is an urgent need for thorough analysis of Radix astragali, a widely used Chinese herb, for quality control purposes. This paper describes the development of a total analytical method for Radix astragali extract, a multi-component complex mixture. Twenty-four components were separated step by step from the extract using a series of isocratic isopropanol-methanol elutions, and then 42 components were separated similarly using methanol-water elutions. Based on the log k(w) and -S of the 66 components obtained from the above procedure and the optimization software developed in our laboratory, an optimum elution program consisting of seven methanol-water segments and four isopropanol-methanol segments was developed to finish the task of analyzing the total components in a single run. Under optimized gradient conditions, the sample of Radix astragali extract was analyzed. As expected, most of the components were well separated and the experimental chromatogram was in a good agreement with the predicted one.