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.     

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     

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.     

The effect of aging and natural organic matter on the Th(OH)4 solubility

The solution chemistry of actinides, particularly hydrolysis, is of major importance in the design of nuclear waste repositories and in relation to nuclear fuel reprocessing cycles. In this study the formation and solubility of the Th(OH)₄ solid phase has been investigated as a function of the aging time and the presence of natural organic matter (e.g. humic acid) in 0.1 M NaClO₄, at weak acid pH and under normal atmospheric conditions. Th(OH)₄ has been prepared by alkaline precipitation and characterized by TGA, ATR–FTIR, XRD, and solubility measurements. According to the experimental data Th(OH)₄ is stable and remains the solubility limiting solid phase even in the presence of increased humic acid concentration in solution. Increasing humic acid concentration doesn’t affect the crystallite size and the solubility product of Th(OH)₄. Th(OH)₄ solubility is basically pH depended and governed by the presence of colloidal species. However, solid phase aging, which in absence of humic acid favors crystallinity, affects significantly the Th(OH)₄ solubility.     

Americium and samarium determination in aqueous solutions after separation by cation-exchange

The concentration of trivalent americium and samarium in aqueous samples has been determined by means of alpha-radiometry and UV–Vis photometry, respectively, after chemical separation and pre-concentration of the elements by cation-exchange using Chelex-100 resin. Method calibration was performed using americium (²⁴¹Am) and samarium standard solutions and resulted in a high chemical recovery for cation-exchange. Regarding, the effect of physicochemical parameters (e.g. pH, salinity, competitive cations and colloidal species) on the separation recovery of the trivalent elements from aqueous solutions by cation-exchange has also been investigated. The investigation was performed to evaluate the applicability of cation-exchange as separation and pre-concentration method prior to the quantitative analysis of trivalent f-elements in water samples, and has shown that the method could be successfully applied to waters with relatively low dissolved solid content.     

Development of a Wine Metabolomics Approach for the Authenticity Assessment of Selected Greek Red Wines

Wine metabolomics constitutes a powerful discipline towards wine authenticity assessment through the simultaneous exploration of multiple classes of compounds in the wine matrix. Over the last decades, wines from autochthonous Greek grape varieties have become increasingly popular among wine connoisseurs, attracting great interest for their authentication and chemical characterization. In this work, 46 red wine samples from Agiorgitiko and Xinomavro grape varieties were collected from wineries in two important winemaking regions of Greece during two consecutive vintages and analyzed using ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QToF-MS). A targeted metabolomics methodology was developed, including the determination and quantification of 28 phenolic compounds from different classes (hydroxycinnamic acids, hydroxybenzoic acids, stilbenes and flavonoids). Moreover, 86 compounds were detected and tentatively identified via a robust suspect screening workflow using an in-house database of 420 wine related compounds. Supervised chemometric techniques were employed to build an accurate and robust model to discriminate between two varieties.     

A highly efficient synthesis of [1-C, O]- and [1-C, H2]-glycerol for the elucidation of biosynthetic pathways

Labeled glycerol is a widely used biochemical probe to investigate biosynthetic pathways. A highly efficient synthesis of [1-¹³C, ¹⁸O]- and [1-¹³C, ²H₂]-glycerol is described in which the ¹³C label is introduced using cyanide. The ¹⁸O label was introduced by a Pinner synthesis and reduction of the ester 5 allowed incorporation of the ²H labels.     

An adaptive way for improving noise reduction using local geometric projection

We propose an adaptive way to improve noise reduction by local geometric projection. From the neighborhood of each candidate point in phase space, we identify the best subspace that the point will be orthogonally projected to. The signal subspace is formed by the most significant eigendirections of the neighborhood, while the less significant ones define the noise subspace. We provide a simple criterion to separate the most significant eigendirections from the less significant ones. This criterion is based on the maximum logarithmic difference between the neighborhood eigendirection lengths, and the assumption that there is at least one eigendirection that corresponds to the noise subspace. In this way, we take into account the special characteristics of each neighborhood and introduce a more successful noise reduction technique. Results are presented for a chaotic time series of the Henon map and Ikeda map, as well as on the Nasdaq Composite index.     

Preparation of hydroxyapatite via microemulsion route

Hydroxyapatite (HAp) was prepared using a microemulsion route in combination with the pH-shock wave method. The samples as received consisted of amorphous aggregated particles, which had remarkable mesoporosity with a narrow pore size distribution. After being heated at 650 degrees C, the A-type carbonate hydroxyapatite was crystallized at 635 degrees C in particles of similar size (40--120 nm) with no internal porosity. At a higher temperature (900 degrees C) a sintering process took place, resulting in network of a larger particles, consisting of HAp and beta-tricalcium phosphate (beta-TCP). The crystallization of HAp occurs at 635 degrees C with an activation energy of 62.7--72.2 kcalmol(-1).