Detailed analysis of α,ω-bis(4-hydroxybutyl) poly(dimethylsiloxane) using GPC-MALDI TOF mass spectrometry

In this study the prepolymer alpha,omega-bis(4-hydroxybutyl) poly(dimethylsiloxane), used in the formulation of oxygen permeable films, is evaluated by gel permeation chromatography (GPC) combined with matrix assisted laser desorption ionization (MALDI) time of flight (TOF) mass spectrometry (MS). Two unexpected mass distributions are observed in the mass spectra. Reaction schemes for the formation of these distributions are proposed. A solution phase trimethylsilane end group modification was performed on the prepolymer to determine whether the unexpected mass distributions occur as impurities from synthesis or as artifacts from the MS process. Evaluation of the TMS modified prepolymer indicates the unexpected mass distributions indeed occur as impurities from the synthetic procedure. Average molecular weight values are determined by traditional GPC, direct MALDI-TOF MS, and GPC-MALDI-TOF MS methods and the results are compared.     

Studies on the thermotropic liquid crystalline polymer. XII. Synthesis and properties of crosslinkable thermotropic liquid crystalline homo- and copoly(ether-ester)s

A series of crosslinkable thermotropic liquid crystalline poly(ether-ester)s and copoly(ether-ester)s was prepared. All of the polymers were crosslinked by thermal treatment or photo-irradiation upon heating. The thermal stability and thermal crosslinking reaction of these polymers were investigated. These polymers also could be crosslinked by copolymerization with vinyl monomers, such as styrene or methyl methacrylate. The crosslinked polymers exhibited thermotropic liquid crystalline behavior after softening by heating. The phase behavior of linear polymers and crosslinked polymers was studied by differential scanning calorimetry (DSC) and an optical polarizing microscope equipped with a heating stage. © 1995 John Wiley & Sons, Inc.     

离子注入修饰电极检测硝基苯

离子注入是一种新技术，可按人们的意愿和需要，将不同的离子注入不同的基本电极表面，制成具有催化活性强，稳定性高，重现性好等特点的修饰电极。作者研究了离子注入钴和注入镍的玻碳电极在０．１ｍｏｌ／ＬＨＡｃ－ＮａＡｃ缓冲溶液中硝基苯的行为及测定。     

采用Seemann－Bohlin准聚焦X射线衍射仪测量薄膜厚度的误差理论分析

本文从理论上分析了衍射强度比偏差Δ（Ｉ／Ｉ∞）和衍射峰位偏差Δ２θ对Ｓｅｅｍａｎｎ－Ｂｏｈｌｉｎ准聚焦Ｘ射线衍射仪测量表面单层薄膜厚度误差的影响。分析结果表明，降低Δ（Ｉ／Ｉ∞）可提高膜厚的测量精度，在Δ（Ｉ／Ｉ∞）－定的情况下，按μρｔ［Ｓｉｎ（－１）γ＋Ｓｉｎ（－１）（２θ－γ）］＝１选择靶辐射和衍射晶面可使由Δ（Ｉ／Ｉ∞）导致的膜厚测量误差具有极小值；选择高角度衍射线有助于减小试样离焦引起的衍射峰位偏差，亦可降低因衍射角测量偏差导致的膜厚测量误差，当衍射线处于薄膜的法向２θ＝γ＋π／２时，角度项误差（Δｔ／ｔ）（２θ）完全消除。     

Chromatographic characterization of molecularly imprinted microspheres for the separation and determination of trimethoprim in aqueous buffers

Molecularly imprinted microspheres (MIMs) against trimethoprim (TMP), prepared by aqueous microsuspension polymerization, bound strongly to TMP, by electrostatic and other non-covalent interactions. The effects of pH, kind and ionic strength (I) of buffer on capacity factors (k') have been discussed in detail. The capacity factors for TMP increased with increasing pH of both acetate and phosphate buffers. The effects of ionic strength on capacity factors were very substantial and the linear relationship between logk' and logI was described by the equation logk'=0.3162-0.4420logI with R=-0.9995. The results showed that pH 3.5 acetate buffer (0.05 mol L(-1)) containing 0.1 mol L(-1) sodium chloride and a 1:9 ratio of buffer to methanol were the optimum conditions for separation and determination of TMP. The calibration plot of peak area against concentration was linear with R=0.9979.     

A unique spherical molecular host with D2d symmetry. A novel intramolecular kinetic equilibrium in metal ion complexation between two crown ethers

[formula: see text] A spherical host with D2d symmetry consisting of a tetrathia[3.3.3.3]paracyclophane and two 18-crown-6 moieties was synthesized. Its crystal structure shows a central cavity with a diameter of 1.96 A and a depth of 6.75 A. A Na+ ion could rest in the cavity center but prefers core binding to external binding in one of the crown units. An intramolecular kinetic equilibrium was reached with the Na+ ion switching between the two crown units with an energy barrier of 14.1 +/- 3 kcal/mol.     

Synthesis and Electrochemical Studies of Spinel LiNi1−xMnxVO4

Spinel compound LiNi_1−xMn_xVO₄ (0≤x≤0.4) had been prepared by using the moist chemical method. X-ray diffraction spectra showed that the lattice constant increased with x in the LiNi_1−xMn_xVO₄, XPS spectra indicating that Li1s had a chemical shift towards lesser binding energy, and manganese in LiNi_1−xMn_xVO₄ existing as the mixed valence of Mn²⁺ and Mn³⁺. The electrochemical charge and discharge testing at a current density of 0.1 mA/cm² between the potentials of 4.0 and 3.0 V vs Li/Li⁺ in 1 mol/dm³ LiPF₆/EC+DEC (1:1 by volume) at 25°C showed that LiNi_1−xMn_xVO₄ cell has a better rechargeability, but a lower cell voltage of 4.0 V vs Li/Li⁺ than that without the doping sample, and the capacity and the cycle efficiency of the Li/LiNi_1−xMn_xVO₄ cells increased with x in the LiNi_1−xMn_xVO₄.     

RNA Methylation m6A: A New Code and Drug Target?

The m⁶A‐RNA modification is a dynamic and reversible process, which has emerged as a new RNA code for the regulation of gene expression. The functional network of methyltransferases (writers), demethylases (erasers), and binding proteins (readers) modulate the level of m⁶A modification. Dysfunction of RNA methylation has been associated with various fundamental biological processes and human diseases. Herein, we briefly introduce an understanding‐enabled manipulation on m⁶A‐RNA modification with an emphasis on the use of small‐molecule intervention.      

Synthesis and photopolymerization of monomers bearing isopropenylphenoxy groups

The synthesis of a series of monomers containing isopropenylphenoxy groups was carried out. On irradiation with UV light in the presence of onium salt photoacid generators, these monomers undergo a chain extension reaction consisting of a dimerization followed by a Friedel-Crafts ring closure which results in the formation of polymers with indane groups in the backbone. Aryl imide-containing monomers bearing isopropenylphenoxy groups were also shown to undergo facile photoinduced cationic polymerization. The resulting polymers displayed excellent thermal stability. © 1995 John Wiley & Sons, Inc.     

Diffraction techniques for nonlamellar phases of phospholipids

A neutron diffraction method applicable to nonlamellar phases of substrate-supported lipid membranes is described and validated. When prepared on a flat substrate, the resulting nonlamellar phases have layered symmetry which provides some advantages over powder diffraction for detailed structure determination. This approach recently led to the detection of a rhombohedral phase and a distorted hexagonal phase of lipids. Here the determination of intensity and phase information for such phases is demonstrated by application to the hexagonal phase of diphytanoyl phosphatidylcholine (DPhPC). The hexagonal symmetry is used to verify the data reduction procedure for the intensities of the diffraction peaks. Diffraction intensities measured while varying the D2O/H2O ratio in the relative humidity was used to solve the phase problem. The neutron scattering length density distribution of the hexagonal phase was constructed and analyzed to elucidate the packing of the lipid molecules. The structure of DPhPC in the hexagonal phase is of interest in connection with its stalk structure in the rhombohedral phase. We also found that the incorporation of tetradecane into the DPhPC hexagonal phase is limited, similar to the case for dioleoyl phosphatidylethanolamine.