Synthesis and characterization of decyl phosphonic acid,applications in emulsion polymerization and anti-corrosion coating

Alkyl phosphonic acids are amphiphilic structures consisting of non-polar organic hydrophobic groups and anionic inorganic hydrophilic groups, which makes them be able to behave as surfactants as well as smart corrosion inhibitors. A simple and high yield (up to 87%) pathway for synthesizing decyl phosphonic acid (DPA) is described. ¹H and ¹³C-NMR) as well as FTIR spectroscopy were used to characterize chemical structures and purity of the obtained product. Thermal properties and crystal structure of DPA were investigated using differential scanning calorimetry analysis (DSC) and thermogravimetric analysis (TGA). The stability of DPA in Oil-in-Water (O/W) and Water-in-Oil (W/O) emulsions was improved in the presence of ammonium persulfate (APS), which allowed us to measure their specific characteristics such as particle size and zeta potential (ξ) of micelles. Both emulsions were used for synthesizing polyaniline (PANI) by emulsion polymerization. Wettability of DPA on the mild steel surface was examined using contact angle measurements. Moreover, corrosion-inhibition properties studied by using electrochemical impedance spectroscopy (EIS) technique and salt spray test results revealed that DPA can be an efficient ingredient for anti-corrosion coating.     

Analyzing the nanoindentation response of carbon black filled elastomers

Carbon black (CB) filled elastomers are structurally complex materials that offer unique properties at different length scales. They have tremendous potential applications in a number of fields including the automotive and aerospace industries and for designing innovative smart materials such as artificial muscles but their applications remain limited primarily due to inadequate understanding of their unique mechanical properties. Here, using the Berkovich technique to probe the surface mechanical properties at different scales the nanoindentation response of a series of composites made by homogeneously dispersed CB nanoparticles inside a semicrystalline copolymer matrix has been explored. While the measured loading part of the force–displacement curves is well described by Meyer's empirical power relation, the inverted methodology (IM) approach to deal with the unloading part has been considered and its outcome has been compared with that obtained from the standard Oliver–Pharr's method. The results were consistent with the observed increase of hardness when the applied displacement decreases for all composite samples over a large range of CB volume fraction. Zhang and Xu's model is demonstrated to produce experimentally consistent explanation of this indentation size effect. X-ray photoelectron spectroscopy (XPS) spectra also show composition gradients with depth up to 100 nm. Furthermore, the effect of CB content, surface features, and length scale-dependent deformation on the hardness–displacement behavior have been considered. These findings highlight the possibility of attaining a diverse set of mechanical properties by a better understanding of the nanoindentation response of CB filled elastomers which can be useful for material selection and design improvements in a number of practical applications.     

Mass Spectrometry-Based Proteomics Reveal Alcohol Dehydrogenase 1B as a Blood Biomarker Candidate to Monitor Acetaminophen-Induced Liver Injury

Acute liver injury (ALI) is a severe disorder resulting from excessive hepatocyte cell death, and frequently caused by acetaminophen intoxication. Clinical management of ALI progression is hampered by the dearth of blood biomarkers available. In this study, a bioinformatics workflow was developed to screen omics databases and identify potential biomarkers for hepatocyte cell death. Then, discovery proteomics was harnessed to select from among these candidates those that were specifically detected in the blood of acetaminophen-induced ALI patients. Among these candidates, the isoenzyme alcohol dehydrogenase 1B (ADH1B) was massively leaked into the blood. To evaluate ADH1B, we developed a targeted proteomics assay and quantified ADH1B in serum samples collected at different times from 17 patients admitted for acetaminophen-induced ALI. Serum ADH1B concentrations increased markedly during the acute phase of the disease, and dropped to undetectable levels during recovery. In contrast to alanine aminotransferase activity, the rapid drop in circulating ADH1B concentrations was followed by an improvement in the international normalized ratio (INR) within 10–48 h, and was associated with favorable outcomes. In conclusion, the combination of omics data exploration and proteomics revealed ADH1B as a new blood biomarker candidate that could be useful for the monitoring of acetaminophen-induced ALI.     

High‐Pressure High‐Temperature Transparent Fixed‐Bed Reactor for Operando Gas‐Liquid Reaction Follow‐up

A 3‐MPa, 350 °C fixed‐bed reactor was designed to follow‐up gas‐liquid‐solid reactions on a millimetric size heterogeneous catalyst with Raman spectroscopy. The transparent reactor is a quartz cylinder enclosed in a Joule effect heated stainless‐steel tube. A methodology to determine how to focus the microscope for liquid and solid phase characterization is presented. The setup was validated by performing diesel hydrodesulfurization on a CoMo/alumina extrudate catalyst with a conversion very close to expected values along with the acquisition of Raman spectra of the solid catalyst showing an evolution of the catalyst phase during sulfidation.     

Design of a General‐Purpose European Compound Screening Library for EU‐OPENSCREEN

This work describes a collaborative effort to define and apply a protocol for the rational selection of a general‐purpose screening library, to be used by the screening platforms affiliated with the EU‐OPENSCREEN initiative. It is designed as a standard source of compounds for primary screening against novel biological targets, at the request of research partners. Given the general nature of the potential applications of this compound collection, the focus of the selection strategy lies on ensuring chemical stability, absence of reactive compounds, screening‐compliant physicochemical properties, loose compliance to drug‐likeness criteria (as drug design is a major, but not exclusive application), and maximal diversity/coverage of chemical space, aimed at providing hits for a wide spectrum of drugable targets. Finally, practical availability/cost issues cannot be avoided. The main goal of this publication is to inform potential future users of this library about its conception, sources, and characteristics. The outline of the selection procedure, notably of the filtering rules designed by a large committee of European medicinal chemists and chemoinformaticians, may be of general methodological interest for the screening/medicinal chemistry community. The selection task of 200K molecules out of a pre‐filtered set of 1.4M candidates was shared by five independent European research groups, each picking a subset of 40K compounds according to their own in‐house methodology and expertise. An in‐depth analysis of chemical space coverage of the library serves not only to characterize the collection, but also to compare the various chemoinformatics‐driven selection procedures of maximal diversity sets. Compound selections contributed by various participating groups were mapped onto general‐purpose self‐organizing maps (SOMs) built on the basis of marketed drugs and bioactive reference molecules. In this way, the occupancy of chemical space by the EU‐OPENSCREEN library could be directly compared with distributions of known bioactives of various classes. This mapping highlights the relevance of the selection and shows how the consensus reached by merging the five different 40K selections contributes to achieve this relevance. The approach also allows one to readily identify subsets of target‐ or target‐class‐oriented compounds from the EU‐OPENSCREEN library to suit the needs of the diverse range of potential users. The final EU‐OPENSCREEN library, assembled by merging five independent selections of 40K compounds from various expert groups, represents an excellent example of a Europe‐wide collaborative effort toward the common objective of building best‐in‐class European open screening platforms.     

Effect of environmental pressure on the microstructure of YSZ thermal barrier coating via suspension plasma spraying

Suspension plasma spraying (SPS) as a potential technique to prepare thermal barrier coatings (TBCs) has been attracting more and more attention. However, most reports on SPS were carried out in the atmosphere. Given the unique features of in-flight particles and plasma jets under low pressure, the resulting coatings are expected to be different from those under atmospheric pressure. In this article, yttria-stabilized zirconia (YSZ) thermal barrier coatings were prepared using suspension plasma spraying under different environmental pressures. The results show that as the environmental pressure decreased, the column-like structural coating turned into a vertical crack segmented structure, as well as a dramatic decrease in surface roughness. More nanoparticle agglomerates were formed in the coating under lower environmental pressures. The real porosity of the coating increased with a decrease in environmental pressure.     

Imbibition test in a clay powder (MX-80 bentonite)

The MX-80 bentonite is a reference material for studies in clay barriers. This paper aims to present an investigation of the behaviour of such a material during an infiltration test from the bottom in oedometric conditions. Using dual-energy γ radiation technique, time variations of moisture content are measured at various locations along the clay sample. The transport of water occurring in this experiment can be described by the classical diffusion equation in terms of the Boltzmann variable. A parameter of hydraulic diffusivity is obtained with the Matano's method.Two fluid transport mechanisms govern the phenomena: imbibition of the microporosity in the clay grains and capillary imbibition in the mesoporosity around the grains. The competition between these two mechanisms will be put into relief by modelling the distribution of the water between and inside the bentonite grains. A clogging behaviour of the mesopores during the imbibition process will allow to explain the surprising decrease in hydraulic diffusivity.     

Influence of the amorphous phase molecular mobility on impact and tensile properties of polyamide 6,6

In this work, the relationship between molecular mobility of polyamide 6,6 amorphous phase and mechanical properties is studied. PA66 formulations having different glass transition temperatures (T_g) obtained by additivation, chemical modification of the polyamide chains, and/or water conditioning at different hygrometry levels, are considered. The main emphasis is put on the impact strength, as measured by instrumented Charpy impact tests over a broad temperature range. It is observed that the brittle‐tough transition temperature T_B/T is closely correlated with the T_g of the samples rather than to the β secondary relaxation. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43457.     

Al0.3Ga0.7As-GaAs microwave resonant tunneling oscillator

We describe the design of a microwave oscillator using resonant tunneling diodes. The devices are fabricated from Al_0.3Ga_0.7As-GaAs double barrier hetero-structures grown by molecular beam epitaxy. Design criteria improving current drivability are established from a theoretical study of tunneling transmission probabilities. Very high peak current densities up to 3.10⁴ A/cm², favorable for high frequency operation as an oscillator, have been achieved experimentally. The devices exhibit stable oscillations at liquid nitrogen temperature and at room temperature when the tunnel diode oscillator is constructed with a stabilizing network.