A study on the spectral,microstructural, and magnetic properties of Eu–Nd double-substituted Ba0.5Sr0.5Fe12O19 hexaferrites synthesized by an ultrasonic-assisted approach

In this study, an examination on the spectral, microstructural, and magnetic characteristics of Eu–Nd double-substituted Ba_0.5Sr_0.5Fe₁₂O₁₉ hexaferrites (Ba_0.5Sr_0.5Nd_xEu_xFe_12−2xO₁₉ (x = 0.00–0.05) HFs) fabricated by an ultrasonic-assisted approach has been presented. An UZ SONOPULS HD 2070 ultrasonic homogenizer with frequency of 20 kHz and power of 70 W was used. The chemical bonding, structure and the morphology of the products were evaluated by Fourier-Transform Infrared (FT-IR) Spectroscopy, XRD (X-ray diffraction), scanning and transmission electron microscopy and techniques. The textural properties of the prepared nanomaterials were examined by using the Brunauer-Emmett-Teller (BET) method. The magnetic properties were studied using a vibrating sample magnetometer (VSM) at room temperature (RT) and low temperature 10 K. The magnitudes of various magnetic parameters including M_s (saturation magnetization), M_r (remanence) and H_c (coercivity) were estimated and evaluated. The M-H loops revealed the hard ferrimagnetic nature for all products at both temperatures. The M_s and M_r values showed a decreasing tendency with increasing degree of Eu³⁺ and Nd³⁺ substitutions whereas H_c values displayed an increasing trend. At RT, M_s, M_r and H_c values lie in the ranges of 63.0–68.8 emu·g⁻¹, 24.6–39.2 emu·g⁻¹ and 2252.4–2782.1 Oe, respectively. At 10 K, the values of M_s, M_r and H_c lie between 87.5–97.1 emu·g⁻¹, 33.5–40.1 emu·g⁻¹ and 2060.6–2417.2 Oe, respectively. The observed magnetic properties make the prepared products promising candidates to be applied in the recording media.     

Enantioselective Approach for Expanding the Three-Dimensional Space of Tetrahydroquinoline to Develop BET Bromodomain Inhibitors**

The pharmaceutical industry has a pervasive need for chiral specific molecules with optimal affinity for their biological targets. However, the mass production of such compounds is currently limited by conventional chemical routes, that are costly and have an environmental impact. Here, we propose an easy access to obtain new tetrahydroquinolines, a motif found in many bioactive compounds, that is rapid and cost effective. Starting from simple raw materials, the procedure uses a proline-catalyzed Mannich reaction followed by the addition of BF₃ ⋅ OEt₂, which generates a highly electrophilic aza-ortho-quinone methide intermediate capable of reacting with different nucleophiles to form the diversely functionalized tetrahydroquinoline. Moreover, this enantioselective one-pot process provides access for the first time to tetrahydroquinolines with a cis-2,3 and trans-3,4 configuration. As proof of concept, we demonstrate that a three-step reaction sequence, from simple and inexpensive starting compounds and catalysts, can generate a BD2-selective BET bromodomain inhibitor with anti-inflammatory effect.     

Novel sponge-like molecularly imprinted mesoporous silica material for selective isolation of bisphenol A and its analogues from sediment extracts

Bisphenol A (BPA) imprinted sponge mesoporous silica was synthesized using a combination of semi-covalent molecular imprinting and simple self-assembly process. The molecularly imprinted sponge mesoporous silica (MISMS) material obtained was characterized by FT-IR, scanning electron microscopy, transmission electron microscopy, and nitrogen adsorption–desorption measurements. The results show that the MISMS possessed a large specific surface area (850.55 m² g⁻¹) and a highly interconnected 3-D porous network. As a result, the MISMS demonstrated a superior specific adsorption capacity of 169.22 μmol g⁻¹ and fast adsorption kinetics (reaching equilibrium within 3 min) for BPA. Good class selectivity for BPA and its analogues (bisphenol F, bisphenol B, bisphenol E and bisphenol AF) was also demonstrated by the sorption experiment. The MISMS as solid-phase extraction (SPE) material was then evaluated for isolation and clean-up of these bisphenols (BPs) from sediment samples. An accurate and sensitive analytical method based on the MISMS–SPE coupled with HPLC–DAD has been successfully established for simultaneous determination of five BPs in river sediments with detection limits of 0.43–0.71 ng g⁻¹ dry weight (dw). The recoveries of BPs for lyophilizated sediment samples at two spiking levels (50 and 500 ng g⁻¹ dw for each BP) were in the range of 75.5–105.5% with RSD values below 7.5%.     

适用于本科教学的BET比表面测定实验

采用自组装的流动吸附仪建立了基于BET吸附原理的快速测定固体比表面积的实验方法(单点法),对同一活性炭样品,在多功能气体吸附系统上进行对照实验(多点法)。实验结果表明,采用流动吸附仪测定比表面积方便易行,数据稳定可靠,实验教学效果良好。本文介绍这一特色实验,期望对从事物理化学实验教学的同行有所助益。     

Atomistic insights into the selective therapeutic activity of 6-(2,4-difluorophenoxy)-5-((ethylmethyl)pyridine-3-yl)-8-methylpyrrolo[1,2-a]pyrazin-1(2H)-one towards bromodomain-containing proteins

Cross-target effect has been one of the major mechanisms of drug toxicity, this has necessitated the design of inhibitors that are specifically tailored to target particular biomolecules. 6-(2,4-difluorophenoxy)-5-((ethylmethyl)pyridine-3-yl)-8-methylpyrrolo[1,2-a] pyrazin-1(2H)-one (Cpd38) is an inhibitor possessing high inhibition rate and tailored specificity towards bromodomain-containing protein 4 (BRD4). In this research, we used an array of computational techniques to provide insight at the atomistic level the specific targeting of BRD4 by Cpd38 relative to the binding of Cpd38 with E1A binding protein P300 (EP300); another bromodomain-containing protein (BCP). Comparatively, binding of Cpd38 improved the conformational stability and compactness of BRD4 protein when compared to the Cpd38 bound EP300. Also, Cpd38 induced a conformational change in the active site of BRD4 that facilitated a complementary pose between Cpd38 and BRD4 suitable for effective atomistic interactions. Expectedly, thermodynamic calculations revealed that the Cpd38-BRD4 system had higher binding energy (−36.11 Kcal/mol) than the Cpd38-EP300 system with a free binding energy of −15.86 Kcal/mol. Noteworthy is the opposing role Trp81 (acting as hydrogen bond acceptor) and Pro1074 (acting as hydrogen bond donor) found on the WPF and LPF loops respectively play in maintaining Cpd38 stability. Furthermore, the hydrogen bond acceptor/donator ratio was approximately 4:1 in Cpd38-BRD4 system compared with 2:1 in Cpd38-EP300 system. Taken together, atomistic insights and structural perspectives detailed in this report supplements the experimental report supporting the improved selectivity of Cpd38 for BRD4 ahead of other BCPs while providing leeway for the future design of BET selective agents with better pharmacological profile.     

α-Al_2O_3比表面积标准物质的研制

选择市售α-Al2O3粉体作为比表面积标准物质候选材料,采用交叉缩分方法对标准物质样品进行分装。检验结果表明α-Al2O3标准物质样品具有良好的均匀性和稳定性(18个月)。采用国际公认的氮气物理吸附BET方法,联合测量能力经过确认的8家实验室对α-Al2O3标准物质样品进行定值,标准值比表面积为5.47 m2/g,不确定度为0.22 m2/g(k=2)。     

Fibrinogen adsorption onto 316L stainless steel, Nitinol and titanium

Fibrinogen adsorption onto mechanically polished biomedical grade 316L stainless steel (316LSS), nickel titanium alloy (Nitinol) and commercially pure titanium (CpTi) surfaces were studied by measurements of adsorption isotherms and adsorption kinetics using an ex-situ wavelength dispersive spectroscopy technique (WDS). Surface composition, roughness and wettability of these materials were characterized by X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and water contact angle (WCA) measurements. Adsorption isotherm results showed that surface protein concentration on these materials increased with increasing concentration of fibrinogen in phosphate buffer solution. The fibrinogen adsorption isotherms were modeled by both the monolayer Langmuir isotherm and the multilayer Brunauer-Emmett-Teller (BET) isotherm. The results strongly suggest that fibrinogen forms multilayer structures on these materials when the concentration in solution is high. Complementary measurements on the absorbed fibrinogen films by spectroscopic ellipsometry (SE) support this view.     

单分散SiO_2无孔微球比表面积标准物质的研究进展

从单分散二氧化硅(SiO_2)微球的合成方法、粒度表征、定值及其组装体几何比表面积的计算等几个方面对SiO_2比表面积标准物质的合成进行了总结.这种类型比表面积标准物质的合成不仅可以扩展我国比表面积标准物质的种类,而且将有助于加深人们对物质真实比表面积的进一步认识.     

Electrorheological effect of carbonaceous materials with hierarchical porous structures

Carbonaceous materials with different hierarchical porous structures for electrorheological (ER) dispersed phase have been synthesized by carbonization of as-prepared starch/silica precurser at different temperatures. The N₂ adsorption isotherms show that Cmeso-700 and Cmeso-500 particles have the BET surface areas of 1028 and 603 m² g⁻¹, respectively. They both have the mesoporous pores with size of about 4.6 nm and the microporous pores (1.1 and 1.5 nm, respectively). The BET surface areas and C/O atomic ratio of porous carbon materials can be increased with the carbonization temperatures. The rheological measurements indicate that the Cmeso-700 and Cmeso-500 ERF have the better ER effect resulted from their hierarchical porous structures. The shear stress of Cmeso-700 ERF is 900 Pa at 1000 s⁻¹ under 3 kV mm⁻¹, which is almost 4.5 times larger than that of Cmicro-350 ERF. The mesoporous carbon ERFs also show the better sedimentation stability than microporous carbon ERFs. The different ER effect of carbonaceous particles may derive from their different dielectric polarization property induced by the hierarchical porous structures.     

Basic study of the gelation of dimethacrylate‐type crosslinking agents

An investigation was made of the gelation of dimethacrylate‐type crosslinking agents in view of an application for separation media. The study mainly centered on a crosslinking agent, glycerol dimethacrylate (GDMA), which is relatively hydrophilic because of a hydroxyl group in the middle of its structure. The gelation of GDMA was compared with that of other hydrophobic crosslinking agents such as ethylene glycol dimethacrylate and 1,6‐hexanediol dimethacrylate. The diluents used in the study were toluene, toluene with methanol, and cyclohexanol. The gelation was observed in real time with a charge coupled device camera and dynamic light scattering (DLS). Also, the separated dry gels were extensively characterized with scanning electron microscopy, BET (N₂ absorption and desorption isotherm), and Fourier transform infrared. DLS analysis showed a stronger molecular interaction of GDMA gelation in toluene, whereas this interaction was much weaker in an alcoholic solvent such as toluene with methanol or cyclohexanol. This indicated that GDMA gelation might proceed through hydrogen bonding as well as a crosslinking reaction of vinyl groups. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 949–958, 2006