Impact of high pressure treatment on the structure of montmorillonite

The modification of sodium montmorillonite after a high pressure pasteurization treatment was followed by X-ray diffraction, FTIR spectroscopy and thermogravimetric analysis. Regardless of the treatment intensity (300 and 800 MPa), the structure of montmorillonite was clearly modified. Such changes should be taken into consideration when binging montmorillonite–polymer nanocomposites into contact with food.     

Toward a continuous synthesis of porous carbon xerogel beads

A continuous process for producing porous carbon xerogel beads has been developed. It consists in injecting a pre‐cured aqueous solution of resorcinol and formaldehyde on top of a column filled with hot oleic acid. The latter is pumped on the top of the column and fed at the bottom, generating an upward flow that can be adjusted to match the terminal velocity of the settling beads. Thus, the bead residence time in the column can be adjusted to match the gelation time, allowing the beads to solidify before reaching the bottom of the vessel. The obtained beads are subsequently dried and pyrolyzed. The developed experimental setup proved the continuous synthesis of porous carbon beads is possible. Nevertheless, the shaping process caused various texture changes of the porous carbon, which mainly yields macropores instead of micro and mesopores. This process also leads to the build‐up of a denser skin around the beads. © 2018 American Institute of Chemical Engineers AIChE J, 64: 1049–1058, 2018     

Tetrahydroindoles as Multipurpose Screening Compounds and Novel Sirtuin Inhibitors

Indoles are privileged structures in medicinal and bioorganic chemistry that are particularly well suited to serve as platforms for diversity. Among many other therapeutic areas, the indole scaffold has been used to design aromatic compounds useful to interfere with enzymes engaged in the regulation of substrate acylation status, such as sirtuins. However, the planarity of the indole ring is not necessarily optimal for all target enzymes, especially when functionalization with aromatic side chains is required. Replacement of flat scaffolds by nonplanar molecular cores dominated by sp³ hybridization is a common strategy to avoid the disadvantages associated with poor solubility and high promiscuity, while covering less-well-explored areas of chemical space. Thus, we synthesized fragment-like tetrahydroindoles suitable for fragment-based drug discovery as well as a well-characterized small library intended as multipurpose screening compounds. For proof of principle, these compounds were screened against sirtuins 1–3, enzymes known to be addressable by indoles. We found that 2,6,6-trimethyl-4-oxo-4,5,6,7-tetrahydro-1H-indole-3-carboxamides are potent and selective SIRT2 inhibitors. Compound 16 t displayed an IC₅₀ value of 0.98 μm and could serve as exquisite starting point for hit-to-lead profiling.     

Near-Field Electron Energy Loss Spectroscopy in Porous Silicon

First results of an Electron Energy Loss Spectroscopy in the Near Field (NFEELS) mode of n⁺ porous silicon are described here. Sequences of EELS spectra in the low loss energy range (0–30 eV) were recorded, using a scanning transmission electron microscope, as the e-beam was scanned across a nano-hole surrounded by Si platelets. This technique is shown to be very sensitive to spectral and spatial changes in the electromagnetic field distribution outside the surface of nanoparticles, governed by their local nature and shape.     

Concomitant use of liquid–liquid batch and continuous plug flow reactors for kinetic model discrimination. Application to the Rh/TPPTS catalysed reduction of the C–C double bond in dimethylitaconate

The biphasic catalytic reduction of the C–C double bond of dimethylitaconate with a water soluble rhodium/triphenylphosphinetrisulphonated sodium salt (TPPTS) complex is investigated. Kinetic studies in a well-mixed batch reactor provide kinetics parameters and an activation energy of 71 kJ mol⁻¹ but cannot discriminate between a first order or a complex kinetic model within the range of substrate concentration where the approximation of linear liquid/liquid partition is respected. Catalytic tests in the centrifugal partition chromatograph (CPC) reactor under steady-state operations in chemical regime and plug flow mode allow discriminating the kinetic models, the complex kinetic rate law being preferred.     

Cold Compaction and Solid-State Sintering of WC-Co-Based Structures: Experiments and Modeling

Cold compaction (200-1900 MPa) and sintering (1250°-1350°C) of cermets based on WC-Co were experimentally studied using die compaction, cold isostatic pressing, sintering, and creep tests. Two different-sized WC powders were used. The cobalt content varied over a range of 10-30 wt%. Cold-compaction behavior has been described by using a Cam-Clay model. Die-wall friction was measured by using green powder compacts that had different aspect ratios. Friction coefficients were 0.28-0.85, depending on the WC particle size and cobalt content. Simple constitutive equations have been used to model the high-temperature behavior (sintering and creep). The constitutive equations were implemented in a finite-element program to model the compaction, ejection, and sintering of bilayer structures that had different cobalt contents. The model can represent the effect of die-wall friction on the average density, as well as deformation inside the green compact. Density gradients were generated; they were revealed during sintering, because the compact does not deform homogeneously. Simulation also can be used to evaluate deformations that are induced by sintering.     

Chemometric analysis of combined NIR and MIR spectra to characterize French olives

Chemometric treatment of near‐infrared (NIR) and mid‐infrared (MIR) combined spectra was used firstly to predict oil and water contents in fresh olive fruit samples (n = 223) and secondly to classify these samples into five principal French cultivar origins (Aglandau, Cailletier, Olivière, Salonenque, and Tanche). The study was carried out during four crop years (2005/2006 to 2008/2009) to take into account the seasonal variations. The comparison of the results obtained in the combined range (REP = 2.6% for the water content and 3.5% for the oil content) provides an obvious advantage compared to the NIR and MIR techniques used separately. Fresh olive fruit cultivars were satisfactorily classified with the partial least squares‐discriminant analysis (PLS‐DA) method in the combined range. After use of the K‐means clustering on the PLS‐DA scores, all the samples were well classified into their five groups of origin. The use of infrared combined spectra allows a considerable improvement in estimating olive fruit quality (oil and water contents, varietal origins).     

Variable energy positron beam study of Xe-implanted uranium oxide

Doppler broadening of annihilation gamma-line combined with a slow positron beam was used to measure the momentum density distribution of annihilating pair in a set of sintered UO₂ samples. The influence of surface polishing, of implantation with 800-keV ¹³⁶Xe²⁺ at fluences of 1 × 10¹⁵ and 1 × 10¹⁶ Xe cm^?2, and of annealing were studied by following the changes of the momentum distribution shape by means of S and W parameters. The program used for this purpose was VEPFIT. At the two fluences in the stoichiometric as-implanted UO₂, formation of Xe bubbles was not detected. The post-implantation annealing and over-stoichiometry in the as-implanted sample caused Xe precipitation and formation of Xe bubbles.     

NARP-HPLC/MS and silver cationization fingerprinting of triacylglycerols in wild and cultivar Tunisian peanut kernels

A simple strategy to identify triacylglycerols (TAGs) in wild and cultivar peanuts was performed using on line coupling of non-aqueous reversed phase chromatography-electrospray ionization–mass spectrometry (NARP-LC-ESI–MS) with silver nitrate (AgNO₃) as a post-column additive. The combination of the structural information given by MS with chromatographic retention laws led to the determination of the structure of TAGs in wild and cultivar peanut oil. In addition, by using the MS⁵ method, the regio-specificity of the TAGs was determined. It was also demonstrated that in Tunisian peanut oil, the saturates have a preference for the sn-1/sn-3 position for the arachidonic and behenic acids. In the wild variety fatty acids with odd numbers of carbons were found and more TAGs were identified in comparison to the cultivar peanut oil.