The ring transformations of 1,2,3,4-diepoxybutane (2,2′-bioxirane) catalysed by various aluminosilicates

The transformations of a molecule containing two adjacent epoxide rings, 2,2-bioxirane that is, were studied over various acidic aluminosilicates (HZSM-5, HY-FAU, AlMCM-41), for the first time, In the 373–473 K temperature range, in a pulse reactor, a ring-opening–ring-enlargment reaction producing furan only occured over the zeolites and it was the predominant reaction on AlMCM-41 as well. The driving force of this transformation route is water formation via elimination from 2,2-bioxirane. Suprising is the lack of the mono- or dialdehyde, the would-be products of the cleavage of the sterically more hindered C–O bonds – an acid-catalysed reaction typical for alkyl-substituted oxiranes.     

Rheological and morphological properties of high‐density polyethylene and poly(ethylene–octene) blends

The rheological and morphological properties of blends based on high‐density polyethylene (HDPE) and a commercial ethylene–octene copolymer (EOC) produced by metallocene technology were investigated. The rheological properties were evaluated in steady and dynamic shear experiments at 190°C in shear rates ranging from 90 s^?1 to 1500 s^?1 and frequency range between 10^?1 rad/s and 10² rad/s, respectively. These blends presented a high level of homogeneity in the molten state and rheological behavior was generally intermediate to those of the pure components. Scanning electron microscopy (SEM) showed that the blends exhibit dispersed morphologies with EOC domains distributed homogeneously and with particle size inferior to 2 μm. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 2240–2246, 2002     

Classification of vegetable oils by high-resolution <Superscript>13</Superscript>C NMR spectroscopy using chromatographically obtained oil fractions

¹³C NMR spectra of oil fractions obtained chromatographically from 109 vegetable oils were obtained and analyzed to evaluate the potential use of those fractions in the classification of vegetable oils and to compare the results with the NMR analysis of complete oils. The oils included the following: virgin olive oils from different cultivars and regions of Europe and north Africa; “lampante” olive, refined olive, refined olive pomace, hazelnut, rapeseed, high-oleic sunflower, corn, grapeseed, soybean, and sunflower oils; and mixtures of virgin olive oils from different geographical origins. Oils were divided into two sets of samples. The training set (98 samples) was employed to select the variables that resulted in significant discrimination among the different oil classes. By using stepwise discriminant analysis, more than 98% of correct validated assignments were obtained; these results were confirmed when applied to the test set (11 blind samples). Results suggest that the use of oil fractions considerably increases the discriminating power of NMR in the analysis of vegetable oils.     

Fatty acid composition of spanish shortenings with special emphasis on <Emphasis Type="Italic">trans</Emphasis> unsaturation content as determined by fourier transform infrared spectroscopy and gas chromatography

A Fourier transform infrared spectroscopic procedure was used to analyze 34 edible fats (22 shortenings and 12 vegetable margarines) as neat fats (IR_NF) to determine their total trans fatty acid (TFA) content. The sloping baseline was corrected with a reference spectrum based on a nonprocessed olive oil. The calibration was done using seven partially hydrogenated fats with an individual TFA content previously determined by the combination of gas chromatography (GC) with argentation thin-layer chromatography. Taking into account the different absorptivities of various trans isomers, different correction factors were calculated using the calibration standards (0.83 and 1.71 for single trans bonds in both diethylene and triethylene and for trans, trans-diethylene fatty acids, respectively) and applied to calculate the total TFA of samples. Moreover, the samples were converted to their methyl esters and reanalyzed following the same procedure (IR_FAME). Differences in TFA content of fats were not found when a t-test was used to compare the results obtained by IR_NF vs. either IR_FAME or GC, suggesting that IR of neat fats could be used, thus avoiding the need to prepare sample solutions in organic solvents and to prepare fatty acid methyl esters. The mean TFA content (determined by IR_NF) of a representative group of Spanish shortenings (22 samples) that varied widely in terms of fat sources, processes, and purposes (bakery, sandwiches, ice cream, coatings, chocolate coverings) was 6.55±11.40%, although more than 54% contained <3% of TFA. Fatty acid composition of shortenings by direct GC using a 100-m polar cyanopolysiloxane capillary column indicated that the mean trans-18∶2 isomer content was 0.58%, ranging from 0.9 to 3.4%. Small amounts of trans-18∶3 isomers (<0.3%) were observed in 18 of the 22 shortenings studied; the maximal value was <2%. The mean value of the fraction saturated+TFA of shortenings was high (59.95±12.73%), including two values higher than 83%.     

Enhancing thermal and dynamic-mechanical properties of epoxy reinforced by amino-functionalized microcrystalline cellulose

In this study, microcrystalline cellulose (MCC) was chemically modified with 3-(aminopropyl)triethoxysilane and added to epoxy to improve chemical, thermal and dynamic-mechanical characteristics of the composites. The composites were manufactured aided by sonication with 1.0%, 2.5%, or 5.0% wt/wt of untreated MCC or amino-functionalized MCC (MCC-Si). The epoxy/MCC-Si composites showed a decrease in the ─OH band by Fourier-transform infrared spectroscopy, and X-ray diffraction analysis indicated better dispersion. The incorporation of MCC-Si in epoxy resin decreased the heat of reaction, increased activation energy values (E_a) and pre-exponential factor (A), and did not affect thermal degradation. All conversion degree (α) versus temperature curves for the composites showed a sigmoidal shape. MCC-Si composites showed better dynamic-mechanical properties than the MCC counterparts, and the functionalization effect was evidenced in storage modulus (E') and loss modulus (E"). At 2.5% wt/wt of MCC-Si content an increase of 119% in E' at the glassy region, 127% in E' at the rubbery region and 173% in E" was observed compared to the neat resin, whereas the T_g barely changed among samples. Good adhesion between the amino-functionalized MCC and the epoxy matrix was observed at the fracture surface, evidencing that surface modification of MCC improves their chemical interaction.     

Rheological,thermal, and morphological properties of blends based on poly(propylene), ethylene propylene rubber,and ethylene-1-octene copolymer that could result from end of life vehicles: Effect of maleic anhydride grafted poly(propylene)

The objective of this work is to study the properties of blends that could result from the recycling of end-of-life vehicles (ELV). While ethylene propylene rubber (EPR) and ethylene propylene diene monomer (EPDM) have been used extensively as elastomeric additives in poly(propylene) (PP), they can be substituted by ethylene-1-octene copolymer (EOC). As a consequence, the matter resulting from the sorting of ELV might be more complex and made of PP, EPR, and EOC. The effect of incorporating EOC [that is a polyethylene elastomer (PEE)] and maleic anhydride grafted polypropylene (PP-g-MAH) on the rheological, thermal, and morphological properties of PP/EPR blends has been investigated. Blends of various compositions (with and without compatibilizer) were prepared using a corotating twin-screw extruder. The results were compared to the ones presented by a commercial (PP/EPR) blend. The EPR phase is dispersed in the form of spherical particles in (PP/EPR). The EOC phase is dispersed in the form of aggregated particles. Dynamic viscoelastic and differential scanning calorimetry properties of (PP/EPR)/EOC blends shows the incompatibility of the components even in presence of PP-g-MAH copolymer. POLYM. ENG. SCI., 47:1009–1015, 2007. © 2007 Society of Plastics Engineers     

Sintering-driven effects on the band gap of (Pb,La)(Ti,Ni)O3 photovoltaic ceramics

In this work, the influence of the sintering temperature on the physical properties of (Pb_0.8La_0.2)(Ti_0.9Ni_0.1)O₃ (PLT-Ni) ceramics is reported. The experimental data revealed that the energy band gap of PLT-Ni ceramics could be tailored from approximately 2.7 to 2.0 eV by changing the sintering temperature from 1100°C to 1250°C. It is demonstrated that the simple substitution of Ti⁴⁺ by Ni²⁺ cations is effective to decrease the intrinsic band gap while increasing the tetragonality factor and the spontaneous polarization. However, the additional red-shift observed in the absorption edge of the PLT-Ni with increasing the sintering temperature was associated with a continuous increase in the oxygen vacancies () amount. It is believed that the impact of the creation of these thermally induced is manifold. The presence of and Ni²⁺ ions generate the Ni²⁺- defect-pairs that promoted both a decrease in the intrinsic band gap and an additional increase of the tetragonality factor, consequently, increasing the spontaneous polarization. The creation of Ni²⁺- defects also changed the local symmetry of Ni²⁺ ions from octahedral to a square pyramid, thus lifting the degeneracy of the Ni²⁺ 3d orbitals. With the increase in the sintering temperature, lower-energy absorbing intraband states were also formed due to an excess of , being responsible for an add-on shoulder in the absorption edge, extending the light absorption curve to longer wavelengths and leading to an additional absorption in “all investigated” spectrum as well.     

Boundary scan test,test methodology,and fault modeling

The test technique called boundary scan test (BST) offers new opportunities in testing but confronts users with new problems too. The implementation of BST in a chip has become an IEEE standard and users on board level are the next group to begin thinking about using the new possibilities. This article addresses some of the questions about changes in board-level testing and fault diagnosis. The fault model itself is also affected by using BST. Trivial items are extended with more sophisticated details in order to complete the fault model. Finally, BST appears to be a test technique that offers a high degree of detectability on board level, but for diagnosis, some additional effort has to be made.     

Capture device identification from digital images using Kullback-Leibler divergence

Multimedia Tools and Applications - It is proposed a forensic method for the capture device identification from digital images, which requires two elements: i) a digital image subject to...     

Twin-image suppression in digital in-line holography based on wave-front filtering

Pattern Analysis and Applications - Digital holography is an imaging process able to recreate three-dimensional representations of objects from recording pattern interference among distinct waves....