Effect of the premelting temperature and sample thickness on the polymorphic behavior of syndiotactic polystyrene/clay nanocomposites

X‐ray diffraction methods and differential scanning calorimetry thermal analysis have been used to investigate the structural changes of syndiotactic polystyrene (sPS)/clay nanocomposites. sPS/clay nanocomposites have been prepared by the mixing of sPS polymer solutions with organically modified montmorillonite. X‐ray diffraction data and differential scanning calorimetry results indicate that the dominating crystal forms and their relative fractions in sPS and sPS/clay nanocomposites are different for various premelting temperatures (T_max's). Higher T_max's favor the formation of the thermodynamically more stable β‐crystalline form, and its relative fraction has been obtained from the X‐ray diffraction data in the range of 11.5–13°. The intensity of the X‐ray diffraction data in the range of 11.5–13° decreases as the thickness of sPS/clay nanocomposites decreases from 150 to 20 μm. At the same time, the intensity of the X‐ray data in the range of 6–7° becomes sharper as the thickness of sPS/clay nanocomposites decreases. The calculation ratio based on the peak intensities at 6.2 and 6.8° for sPS/clay nanocomposites of equal thickness and crystallinity in the pure β and α forms has also been determined in this study. © 2003 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 41: 1730–1738, 2003     

Studies on the Ion Exchange Separation of Aspirin,Salicylic Acid and Acetic Acid

The liquid chromatography of aspirin, salicylic acid and acetic acid using cation exchange resins with aqueous alcohol and water as eluent was described. The results indicated that acetic acid could be separated from aspirin and salicylic acid by hydrogen form cation exchange resin with 25% ethanol or water as eluent. The possibility of using this method to determine the degree of hydrolysis of aspirin was discussed.     

Measurements of crack growth in a solid at elevated temperature by holographic interferometry

Real-time holographic interferometry was used to follow the crack-opening displacement (COD) of a compact tension specimen of zirconium 2.5-percent niobium subjected to a constant tensile load at 120°C for a period of 860 h. This was made possible by a dimensionally stable invar plate placed beside the specimen as the reference for the alignment of holograms. A finite-element elasto-plastic stress-analysis code and measurements on a duplicate specimen with a clip gage were used to correlate the measured COD and the corresponding crack growth.     

广义M?bius反演及其在积分方程与插值过程上的应用——纪念华罗庚教授

The object of this expository paper is to establish a kind of generalized M?bius-Rota inversion formula by the aid of non-standard analysis. Certain constructive applications to Volterra type integral equations and to equidistant smooth interpolation process are expounded in some detail. Moreover, some of our earlier results (cf. [1] ,[2] ,[4]) are refined and improved.     

Polymorphic behavior in syndiotactic polystyrene/clay nanocomposites

X‐ray diffraction methods were used in an investigation of the structural changes in syndiotactic polystyrene (sPS)/clay nanocomposites. sPS/clay was prepared by the intercalation of sPS polymer into layered montmorillonite. Both X‐ray diffraction data and transmission electron microscopy micrographs of sPS/clay nanocomposites indicated that most of the swellable silicate layers were exfoliated and randomly dispersed in the sPS matrix. The X‐ray diffraction data also showed the presence of polymorphism in the sPS/clay nanocomposites. This polymorphic behavior was strongly dependent on the thermal history of the sPS/clay nanocomposites from the melt and on the content of clay in the sPS/clay nanocomposites. Quenching from the melt induced crystallization into the α‐crystalline form, and the addition of montmorillonite probably increased heterophase nucleation of the α‐crystalline form. The effect of the melt crystallization of sPS and sPS/clay nanocomposites at different temperatures on the crystalline phases was also examined. © 2002 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 40: 736–746, 2002     

Air-stable Pd(II) catalysts with cryptand-22 ligand for convenient and efficient Suzuki cross-coupling reactions

Air-stable Pd(II) catalysts with cryptand-22 ligand was easily handled in atm air at room temperature for Suzuki cross-coupling reactions of aryl bromides with arylboronic acids both containing electron-withdrawing and electron-donating groups. Generally, reactions proceeded fast to completion in 2 h to give high product yields. Our Pd(OAc)₂/cryptand-22 catalyst is unique, since the reaction solution remained yellow during reaction period and air-stable without formation of Pd black as usually observed for ordinary simple amine ligands.     

α-Nitro carbonyl compounds in the synthesis of 2,3-dihydrofurans

A new method for the synthesis of 2,3-dihydrofurans from readily available starting enones and α-nitro carbonyl compounds has been developed. This protocol can provide a novel and effective methodology for the preparation of 2,3-dihydrofurans in a stereoselective fashion. With 1,4-dien-3-ones, 2,3-dihydrofurans and cyclohexenecarboxylates were produced and high chemoselectivity was observed in different solvents.