Determination of the degree of cure under dynamic and isothermal curing conditions with electrical impedance spectroscopy

This article presents a new methodology for the quantitative determination of the progress of the curing reaction of a thermosetting resin, using the results of electrical impedance spectroscopy. The method is an extension of the use of the imaginary impedance maximum as a reaction progress indicator and is based on the demonstration of a close correlation between the reaction rate, as measured by conventional differential scanning calorimetry, and the rate of change of the value of the imaginary impedance spectrum maximum. Tests on a commercial aerospace epoxy resin under both isothermal and dynamic heating conditions with calorimetry and impedance spectroscopy have demonstrated the validity of the method and set the accuracy limits involved. This technique can be used as a real-time online control tool for thermoset composite manufacturing. © 2003 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 42: 146–154, 2004     

Classification of Raman spectra using the correlation kernel

The classification of Raman spectra can be very useful in a wide range of diagnostic applications including bacterial identification. Before any form of classification can be carried out on the Raman spectra, some form of pre‐processing is commonly applied. This pre‐processing greatly affects the accuracy of the results and introduces user bias and over‐fitting effects. In this paper, we propose using support vector machines with the correlation kernel. The use of the correlation kernel on Raman spectra has not been presented before in any published work. Our results illustrate that the correlation kernel is ‘self‐normalizing’ and produces superior classification performance with minimal pre‐processing, even on highly noisy data obtained using inexpensive equipment. Such effective classification approaches can lead to clinically valuable diagnostic applications of Raman Spectroscopy. Copyright © 2010 John Wiley & Sons, Ltd.     

A polarization-/angle-insensitive, bandwidth-optimized, metamaterial absorber in the microwave regime

An enhanced metamaterial absorber based on the circumscribed-cross resonator is introduced in this paper. The new structure is polarization-independent, due to the symmetry of its unit cell, and is proven efficient for the attenuation of obliquely incident waves. The absorption mechanism is thoroughly investigated and is found to be mainly related to the losses of the dielectric substrate. Furthermore, by exploiting the scalability property of metamaterials, the operational bandwidth of our design can be drastically improved by placing unit cells with properly scaled resonators adjacent to each other. In this context, various combinations of three, four, and nine unit cells that can increase the full width at half maximum up to as much as 11.18?%, are developed. The overall performance of the proposed configurations is deemed promising for the realization of microwave metamaterial absorbers for several practical applications.     

Accessing the structural diversity of pyridone alkaloids: concise total synthesis of rac-citridone A

A unique route to the structural diversity of pyridone alkaloids is described based on the concept of a common synthetic strategy. Three different core structure analogues corresponding to akanthomycin, septoriamycin A, and citridone A have been prepared by using a highly selective and novel carbocyclization reaction.     

PMMA/organomodified montmorillonite nanocomposites prepared by in situ bulk polymerization

Kinetics of the in situ bulk polymerization of methyl methacrylate in the presence of organomodified montmorillonite (MMT) was investigated using differential scanning calorimetry (DSC) and gravimetrically. Different amount and types of MMT under the trade names Cloisite were employed. Using DSC, the amount of heat released versus time, under isothermal conditions, was recorded, and eventually, the time evolution of polymerization rate and monomer conversion was calculated. Results on the variation of monomer conversion with reaction time were in good agreement to corresponding from the gravimetric measurements. The nanocomposites prepared were characterized with WAXD, TEM and FTIR, and their glass transition temperature, T _g, was measured with DSC. Depending on the added amount of nano-MMT, either exfoliated or intercalated structures were obtained. An enhancement of the polymerization rate with the presence of the nanoparticles was observed especially in the gel effect region. This was accompanied by a higher T _g and average molecular weight, as measured by GPC, of all nanocomposites compared to neat PMMA.     

Investigation of confined ionic liquid in nanostructured materials by a combination of SANS, contrast-matching SANS, and nitrogen adsorption

Small-angle neutron scattering (SANS), contrast-matching SANS, and nitrogen adsorption have been utilized to investigate the confined ionic liquid (IL) [bmim][PF(6)] phase in ordered mesoporous silica MCM-41 and SBA-15. The results suggest that the pores of SBA-15 are completely filled with IL whereas a small fraction of the pore volume, the pore "core", of MCM-41 is empty. The contrast-matching SANS measurements confirm the enhanced solubility of water in IL. In addition, they provide strong evidence that water does not enter the empty pore core of MCM-41, possibly because of the preferred orientation of the IL molecules in the adsorbed layer.     

Adsorption of block copolymers in nanoporous alumina

We have studied the adsorption of end-attaching block copolymer chains inside the cylindrical pores of nanoporous alumina. Highly asymmetric PS-PEO block copolymers, with a small PEO anchoring block and a long PS dangling block, were allowed to adsorb onto porous alumina substrates with an average pore diameter of ∼200 nm from toluene solution. The adsorption process was monitored using FTIR spectroscopy, whereas depth profile analysis was performed by means of XPS and Ar⁺ ion sputtering. It is found that the PS-PEO adsorption kinetics in porous alumina are ∼4 orders of magnitude slower than the corresponding case of a flat alumina substrate. It appears that chains adsorbed near the pore entrance early on tend to form a barrier for chains entering the pore at later times, thereby slowing down the adsorption process significantly. This effect is much more pronounced for large chains whose dimensions are comparable with the pore diameter. The equilibrium adsorbance value is also affected by chain size due to the additional entropic penalty associated with chain confinement, the adsorbance falling substantially when the chain dimensions become comparable with the pore diameter. © 2010 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 48: 1676–1682, 2010     

A convenient synthesis of 2-C-methyl-d-erythritol 4-phosphate and isotopomers of its precursor

A new synthetic approach toward 2-C-methyl-d-erythritol 4-phosphate (MEP), a key intermediate in the mevalonate-independent biosynthetic pathway for isoprenoids, and deuterated analogues of its precursor, 2-C-methyl-d-erythritol acetonide, is described. This procedure uses 2-C-methyl-d-erythrose acetonide as starting material and delivers, through a mono-protection strategy, the target compounds in a short way and in high yield.     

Optimizing Melt‐Processing Conditions for the Preparation of iPP/Fumed Silica Nanocomposites: Morphology,Mechanical and Gas Permeability Properties

A series of iPP/SiO₂ nanocomposites, containing 1, 2.5, 5, 7.5, and 10 wt.‐% fumed silica nanoparticles, were prepared by melt mixing in a twin screw co‐rotating extruder. The effect of different extrusion parameters was evaluated. The size of aggregates increased with increase in SiO₂ content and repetition of the mixing process improved the filler's dispersion. A similar effect was also exhibited by either increasing the rotor speed or the mixing temperature, with the latter being more pronounced at the ranges studied. The mechanical properties of the prepared nanocomposites were evaluated and various models used to explain the observed enhancements. However, only the three‐phase model could provide some correlation with the experimental results. All nanocomposites displayed lower permeability to gases.

     

A short and efficient synthesis of (+)-disparlure and its enantiomer

A short and highly efficient approach was applied for the total synthesis of the gypsy moth sex pheromone (+)-disparlure and its enantiomer from isopropylidene D- and L-erythrose, using a common strategy.