Novel Aerosol-Based Approach toward Mesoporous Silica Nanoparticles

This study introduces a novel gas-phase method for the synthesis of mesoporous silica nanoparticles (MSNs). The method is a two-step templating approach by first forming silicon-coated carbon structures in a hybrid microwave-plasma/hot-wall reactor followed by an annealing step to produce mesoporous silica with distinct nanostructure and porosity. Two different (sacrificial) carbonaceous templates have been prepared (plasma reactor) and coated (hot-wall reactor), 2D few-layer graphene (FLG) flakes and soot-like fractal aggregates. Results show that the wall thickness of the porous silica structures can be adjusted by changing the concentration of the silicon precursor (monosilane). High monosilane concentrations, however, result in solid silica particles after annealing. Using soot-like particle templates permitted to control of the shell thickness of the hollow porous particles, while the FLG template results in ultrathin silica sheets after heat treatment. The pore volume and specific surface area increase up to 263 m² g⁻¹ and 0.6 cm³ g⁻¹, respectively, by the formation of hollow porous particles. An adsorption study on carbamazepine reveals up to ≈86% removal. The gas-phase aerosol-based template method presented here offers scalability and versatility, and it is capable of producing MSNs with a controlled structure and porosity by modifying the carbonaceous templates.     

Rotary Blanking ‐ a New Manufacturing Process

Rotary blanking is a method of blanking and punching with rotating tools whereby the cutting tools are fixed to a pair of rollers performing a continuous blanking operation on a strip of sheet metal. The purpose of this paper is to outline the determining conditions under which the rotary blanking process takes place and to discuss advantages, restrictions, applications and optimization of this technology.     

Solubilization of fish muscle proteins with buffers containing sodium dodecyl sulfate

Summary The extraction of fish muscle protein using SDS containing solubilization buffers was studied varying the time and the temperature of solubilization, as well as pH and SDS concentration of the buffer. At pH < 6 the myofbrillar proteins were incompletely solubilized; temperatures of 80-100 °C resulted in protein degradation observable in the SDS-PAGE.Samples of fish muscle containing high amounts of formaldehyde (50 mmoles FA/kg wet weight) could only be solubilised at 100 °C; on the other hand it was possible to solubilize cooked and/or canned products under mild conditions (2% SDS, 1% 2-ME, pH 8.9, shaking for 2 h at 60 °C).

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Solubilisierung von Fischmuskelproteinen durch Natriumdodecylsulfathaltige Puffer

Zusammenfassung Der Einfluß von Solubilisierungszeit und -temperatur, des pH-Wertes und der SDS-Konzentration des Solubilisierungspuffers auf die Extraktion von Fischmuskelproteinen wurde überprüft. Bei pH-Werten < 6 wurden die myofbrillären Proteine nur unvollständig gelöst; Solubilisierungstemperaturen von 80 bis 100 °C führten zu einem in der SDS-PAGE sichtbaren Proteinabbau. Fischmuskelproben mit hohem Formaldehydgehalt (50 mmole FA/kg Feuchtgewicht) ließen sich nur bei 100 °C vollständig solubilisieren; demgegenüber gelang die weitgehende Solubilisierung gegarter und/oder sterilisierter Produkte unter milden Bedingungen (2% SDS, 1% 2-ME, pH 8,9; 2stündiges Schütteln bei 60 °C).

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Abbreviations FA formaldehyde - IEF isoelectric focusing - 2-ME 2-mercaptoethanol - PA polyacrylamide - PAGE polyacrylamide gel electrophoresis - pI isoelectric point - SDS sodium dodecyl sulfate - TMAO trimethylamine oxide - Tris Tris (hydroxymethyl)methylamine     

Combination of nuclear magnetic resonance spectroscopy and nonlinear methods to analyze the copolymerization of phosphonic acid derivatives

We demonstrate in this study that the combination of modern inline monitoring methods [here: inline nuclear magnetic resonance (NMR)] with simulations gains more exact and profound kinetic results than previously used methods like linearization without that combination. The ¹H-NMR spectroscopic data (more than 100 data points) are used to construct the copolymerization diagram. The reactivity ratios are obtained applying the van Herks nonlinear least square method. The examination of the radical copolymerization of 2-hydroxyethyl methacrylate (HEMA) with (2-{[2-(ethoxycarbonyl)prop-2-en-1-yl]oxy}ethyl) phosphonic acid (ECPPA) as important adhesive monomer used in dentistry yields reactivity ratios of r_HEMA = 1.83; r_ECPPA = 0.42. The copolymerization diagram reflects nonideal, non-azeotropic copolymerization. The sequence distribution of the obtained by Monte Carlo simulation indicates the generation of statistical copolymers. As an important finding, it is demonstrated that the repeating units responsible for etching and adhesion are arranged over the whole polymer chain, which is necessary to achieve proper functionality. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 48256.     

High resolution STEM/EDX spectral imaging to resolve metal distributions within ∼100 nm combustion generated ash particles

Ultrafine ash particles play an important role in establishing a sticky inner deposit layer on heat transfer surface for power plants, but it is still unclear whether a thin surface alkali coating on these ultrafine particles might control this deposition behavior. In this research, we used a high resolution FE-TEM/STEM equipped with twin SDD EDX detectors for high X-ray detection efficiency, to determine the presence and absence of surface enrichment of alkali metals on ultrafine solid fuel ash samples that had low bulk alkali compositions but high deposition rates. Results from two types of combustion generated nano-sized ash particles are presented. One was from the oxy-combustion of pulverized bituminous coal, the other from oxy-combustion of pulverized rice husks, both being burned in a 100?kW rated down-flow laboratory combustor. Elemental mapping results from STEM/EDX uncovered some surface enrichment of alkali metals in ultrafine ash particles, where it existed, as it did for combustion of rice husks. However, it was not able to discern similar alkali metal surface enrichment for the bituminous coal ultrafines that had resulted in even higher deposition rates. Since deposition rates from both of these cases lie on the same correlation with PM₁, one can conclude that although surface enrichment of alkali metals is present for some ～100?nm particles, it is not a prerequisite to achieve high inner surface deposition rates. This is in contrast to prevailing theories that point to alkali metals as “bad actors” as far as the sticky inner deposition rate is concerned.

Copyright © 2019 American Association for Aerosol Research     

Konformation und Rotationsbarrieren substituierter Glyoxylsäureamide

Conformation and Rotation Barriers of Substituted Glyoxylic Acid Amides Semiempirical calculations predict an orthogonal orientation of the carbonyl groups in tertiary glyoxylic acid amides, which is in good agreement with an X-ray structure analysis of 5 . Due to the influence of the α-carbonyl group, the rotation barrier in the substituted glyoxylic acid amides 2a–d, 3a, 3b , and 4–6 (ΔG^#_c = 84–92 kJ mol⁻¹) is about 10 kJ/mol higher than in simple acid amides, as was found by dynamic NMR line shape analysis.     

Synthesis,characterization, and properties of new siloxane grafted copolyimides

Three new siloxane containing grafted copolyimides have been prepared by one‐pot solution imidization technique. The polymers are made by the reaction of 4,4′‐(4,4′‐isopropylidenediphenoxy)bis(phthalic anhydride) (BPADA) with commercially available diamine 4,4′‐oxydianiline (ODA) with variation of silicon containing diamine, namely 3,5‐diaminobenzoate terminated polydimethylsiloxane (DBPDMS), as a comonomer to 10, 20, and 30 wt %. The films of the polymers were prepared by casting the polymer solution in dichloromethane. The polymers have been well‐characterized by GPC, IR, and NMR techniques. Thermal stabilities and decomposition behavior of the copolyimides were studied by DSC and TGA. The water contact angle values of the films indicate hydrophobic nature of the polymers. Thermal, flame retardant, mechanical, and surface properties of these polymers have been compared with the homopolyimide and with polyimides where polysiloxane is incorporated in the main chain. DSC revealed melting of the grafted siloxane chain at sub‐ambient temperature and a glass transition corresponding to the main polymer chain above 200°C. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Ubiquitin C-Terminal Hydrolase L1: Biochemical and Cellular Characterization of a Covalent Cyanopyrrolidine-Based Inhibitor

The deubiquitinase (DUB) ubiquitin C-terminal hydrolase L1 (UCHL1) is expressed primarily in the central nervous system under normal physiological conditions. However, UCHL1 is overexpressed in various aggressive forms of cancer with strong evidence supporting UCHL1 as an oncogene in lung, glioma, and blood cancers. In particular, the level of UCHL1 expression in these cancers correlates with increased invasiveness and metastatic behavior, as well as poor patient prognosis. Although UCHL1 is considered an oncogene with potential as a therapeutic target, there remains a significant lack of useful small-molecule probes to pharmacologically validate in vivo targeting of the enzyme. Herein, we describe the characterization of a new covalent cyanopyrrolidine-based UCHL1 inhibitory scaffold in biochemical and cellular studies to better understand the utility of this inhibitor in elucidating the role of UCHL1 in cancer biology.     

Potential of the Electronic Nose for the Detection of Respiratory Diseases with and without Infection

Respiratory tract infections are common, and when affecting the lower airways and lungs, can result in significant morbidity and mortality. There is an unfilled need for simple, non-invasive tools that can be used to screen for such infections at the clinical point of care. The electronic nose (eNose) is a novel technology that detects volatile organic compounds (VOCs). Early studies have shown that certain diseases and infections can result in characteristic changes in VOC profiles in the exhaled breath. This review summarizes current knowledge on breath analysis by the electronic nose and its potential for the detection of respiratory diseases with and without infection.