Thermal Degradation Kinetics and Modeling Study of Ultra High Molecular Weight Polyethylene (UHMWP)/Graphene Nanocomposite

The incorporation of nanofillers such as graphene into polymers has shown significant improvements in mechanical characteristics, thermal stability, and conductivity of resulting polymeric nanocomposites. To this aim, the influence of incorporation of graphene nanosheets into ultra-high molecular weight polyethylene (UHMWPE) on the thermal behavior and degradation kinetics of UHMWPE/graphene nanocomposites was investigated. Scanning electron microscopy (SEM) analysis revealed that graphene nanosheets were uniformly spread throughout the UHMWPE’s molecular chains. X-Ray Diffraction (XRD) data posited that the morphology of dispersed graphene sheets in UHMWPE was exfoliated. Non-isothermal differential scanning calorimetry (DSC) studies identified a more pronounced increase in melting temperatures and latent heat of fusions in nanocomposites compared to UHMWPE at lower concentrations of graphene. Thermogravimetric analysis (TGA) and derivative thermogravimetric (DTG) revealed that UHMWPE’s thermal stability has been improved via incorporating graphene nanosheets. Further, degradation kinetics of neat polymer and nanocomposites have been modeled using equations such as Friedman, Ozawa–Flynn–Wall (OFW), Kissinger, and Augis and Bennett’s. The "Model-Fitting Method” showed that the auto-catalytic nth-order mechanism provided a highly consistent and appropriate fit to describe the degradation mechanism of UHMWPE and its graphene nanocomposites. In addition, the calculated activation energy (E_a) of thermal degradation was enhanced by an increase in graphene concentration up to 2.1 wt.%, followed by a decrease in higher graphene content.     

Direct syntheses,characterization and optical analysis of PbX2 (X = I,Br and Cl) nanoparticles without any additives

Lead iodide, bromide and chloride nanoparticles (NP-PbX₂, X = I, Br and Cl) with various morphologies were successfully prepared through a simple hydrothermal method without any additives or stabilizers. By treating the PbX₂ in EtOH/CH₂Cl₂ solution at 170 °C for 12 h, the corresponding PbX₂ nanoparticles were synthesized. The average sizes of PbX₂ nanoparticles were between 30 and 80 nm. The structure, morphology, surface and size of PbX₂ nanoparticles were determined by X-ray diffraction powder, Scanning Electron Microscopy, solid state Photo Luminescent, BET surface area and solid state UV.     

Trends in the bioanalytical applications of microfluidic electrocapture

Downscaled analytical tools for sample preparation have offered benefits such as higher throughput, easier automation and lower sample/reagent consumption. Microfluidic electrocapture, which is a newly developed sample preparation/manipulation system, uses an electric field to trap and separate charged species without using any solid sorbent. The feasibility of using microfluidic electrocapture is reported for separation, clean-up, concentration, microreactions and complexation studies of proteins, peptides and other biologically important biomolecules. The instrumentation and applications of microfluidic electrocapture are reviewed and an overview is provided of future perspectives offered by the current and envisaged platforms.     

Application of QR Decomposition Algorithm for Multivariate Calibration in High Overlapping Systems

An accurate and stable algorithm, QR Decomposition Algorithm (QRDA) is initially presented into the chemistry field. The basic principle of QR Multivariate Calibration Algorithm (QRMCA) is investigated, and the complexes system of sodium tripolyphosphate (STPP), sodium sulfate (SS), and sodium Carbonate (SC) with serious overlapping absorption peaks is analyzed by QRMCA. According to our survey, QRDA can avoid matrix inverting, reduce the orders of matrixes, and speed up the operation of matrices. So, it has bright prospects in chemometrics. The process of the QR Decomposition Algorithm (QRDA) was implemented by an orthogonal and upper triangular matrix decomposition that is robust and convenient. Then it was applied to overcome the problem of overlapping spectra of different components in detergent-washing powder.     

Synthesis and characterization of nanocrystalline α-Al2O3 using Al and Fe2O3 (hematite) through mechanical alloying

In this present work, the synthesis of nanocrystalline α-Al₂O₃ using pure aluminum (Al) and Fe₂O₃ (hematite) as the precursors by mechanical alloying technique has been studied. The formation of α-Al₂O₃ nanocrystallites occurs during the solid-state reaction and through the reduction treatment. Also in this paper, effects of milling time on particle size and the lattice strain nanocrystalline α-Al₂O₃ have been investigated. Obtained powders were evaluated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), differential thermal analysis (DTA), thermal gravimetric analysis (TGA) and X-ray diffraction (XRD). The obtained results indicated that a reduction reaction was completed after 2 h milling in a planetary mill. The crystallite size of obtained α-alumina (α-Al₂O₃) was in general about 12 nm. Finally, the results showed appropriate homogeneity and dispersion of related nanocrystalline.     

A novel technique based on diffuse reflectance near-infrared spectrometry and back-propagation artificial neural network for estimation of particle size in TiO2 nano particle samples

Determination of particle size is one of the critical parameters in nanotechnology. The relationship between particle size and diffuse reflectance (DR) spectra in near-infrared region has been applied to introduce a method for estimation of particle size. Back-propagation artificial neural network (BP-ANN) as a nonlinear model was applied to estimate average particle size based on near-infrared diffuse reflectance spectra. Thirty five different nano TiO₂ samples with different particle size were analyzed by DR-FTNIR spectrometry and the obtained data were processed by BP-ANN. The network was trained by 30 samples and was evaluated by the remaining 5 samples. In order to establish whether the new method is applicable for estimation of particle size of nano structured samples, the optimized model was applied to analyze 44 nano TiO₂ samples. It was observed that ANN using the back-propagation algorithm is capable of generalization and could correctly predict the average particle size of nano-sized particles.     

A biocompatible composite based on poly(ε‐caprolactone fumarate) and hydroxyapatite

Fabrication of biodegradable composites applicable as hard tissue substitutes consisting of poly(ε‐caprolactone fumarate) (PCLF), methacrylic acid (MAA), and hydroxyapatite (HA) was investigated. PCLF macromers were synthesized by reaction of PCL diol with fumaryl chloride in the presence of propylene oxide and characterized by gel permeation chromatography, FTIR, and ¹H NMR spectroscopy. Composites were fabricated by incorporating HA as inorganic filler in PCLF matrix which followed by thermal curing of the composition using benzoyl peroxide and MAA as a free radical initiator and reactive diluent, respectively. Uniform distribution of the fine ceramic phase in the polymer matrix was elucidated by scanning electron microscopy. The effects of the initial macromer molecular weight and the filler volume fraction on mechanical properties and cytotoxicity of the composites were also examined. Significant enhancement in the mechanical properties was observed upon increasing HA content and/or initial PCLF molecular weight. The biocompatibility of the specimens was also improved with increasing ceramic phase. Copyright © 2010 John Wiley & Sons, Ltd.     

Synthesis of molecularly imprinted polypyrrole as an adsorbent for solid‐phase extraction of warfarin from human plasma and urine

The aim of this work was to develop a method for the clean‐up and preconcentration of warfarin from biological sample employing a new molecularly imprinted polymer (MIP) as a selective adsorbent for solid‐phase extraction (SPE). This MIP was synthesized using warfarin as a template, pyrrole as a functional monomer and vinyl triethoxysilane as a cross‐linker. The molar ratio of 1:4:20 (template–functional monomer–cross‐linker) showed the best results. Nonimprinted polymers (NIPs) were prepared and treated with the same method, but in the absence of warfarin. The prepared polymer was characterized by Fourier transmission infrared spectrometry and scanning electron microscopy. An adsorption process (SPE) for the removal of warfarin using the fabricated MIPs and NIPs was evaluated under various conditions. Effective parameters on warfarin extraction, for example, type and volume of elution solvent, pH of sample solution, breakthrough volume and maximum loading capacity, were studied. The limits of detection were in the range of 0.0035–0.0050 µg mL^?1. Linearity of the method was determined in the range of 0.0165–10.0000 µg mL^?1 for plasma and 0.0115–10.0000 µg mL^?1 for urine with coefficients of determination (R²) ranging from 0.9975 to 0.9985. The recoveries for plasma and urine samples were >95%. Copyright © 2015 John Wiley & Sons, Ltd.