Synthesis of high-modulus thermoset PUs of PCL-PTMG/CNW biomaterials with different soft domain architecture and composition for high shape memory performance

Cellulose - In this research work, a series of thermoset polyurethane (tPU) nanocomposites and a thermoplastic PU (TPPU) were synthesized using semi-crystalline polyols. Poly(ε-caprolactone)...     

Cold column trapping-cloud point extraction coupled to high performance liquid chromatography for preconcentration and determination of curcumin in human urine

A cold column trapping-cloud point extraction (CCT-CPE) method coupled to high performance liquid chromatography (HPLC) was developed for preconcentration and determination of curcumin in human urine. A nonionic surfactant, Triton X-100, was used as the extraction medium. In the proposed method, a low surfactant concentration of 0.4% v/v and a short heating time of only 2 min at 70 °C were sufficient for quantitative extraction of the analyte. For the separation of the extraction phase, the resulted cloudy solution was passed through a packed trapping column that was cooled to 0 °C. The temperature of the CCT column was then increased to 25 °C and the surfactant rich phase was desorbed with 400 μL ethanol to be directly injected into HPLC for the analysis. The effects of different variables such as pH, surfactant concentration, cloud point temperature and time were investigated and optimum conditions were established by a central composite design (response surface) method. A limit of detection of 0.066 mg L⁻¹ curcumin and a linear range of 0.22–100 mg L⁻¹ with a determination coefficient of 0.9998 were obtained for the method. The average recovery and relative standard deviation for six replicated analysis were 101.0% and 2.77%, respectively. The CCT-CPE technique was faster than a conventional CPE method requiring a lower concentration of the surfactant and lower temperatures with no need for the centrifugation. The proposed method was successfully applied to the analysis of curcumin in human urine samples.     

Application of copolymer coated frits for solid-phase extraction of poly cyclic aromatic hydrocarbons in water samples

A conducting copolymer of pyrrole and phenol was electrochemically synthesized on steel frits as a sorbent. The applicability of the frit was assessed for the solid-phase extraction of trace amounts of polycyclic aromatic hydrocarbons (PAHs) in aqueous samples followed by HPLC–UV. The coating produced was very adherent and the scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and FTIR spectrum for the coated frit were studied. The effects of various parameters on the efficiency of the solid-phase extraction process, such as the sample loading rate, elution solvent type, salt effect, volume and flow rate of sample and elution solvent were investigated. Under the optimal conditions, the calibration curves were obtained in the range of 0.1–500 ng mL⁻¹ (r² > 0.98) and the LODs (S/N = 3) were obtained in the range of 0.01–0.08 ng mL⁻¹. Relative standard deviations (RSDs) for intra- and inter-day precision were 2.7–10.2% and 3.6–11.4%, respectively. The recoveries (8 and 40 ng mL⁻¹) ranged from 79% to 115%. The simplicity of experimental procedure, short sample analysis, high extraction efficiency, and the use of low-cost adsorbent show the potential of this method for routine analysis of PAHs in real samples.     

Ultracompact and fabrication-tolerant integrated polarization splitter

Design and fabrication of a 2×2 two-mode interference (TMI) coupler based on-chip polarization splitter is presented. By changing the angle between the access waveguides, one can tune the effective TMI length for the mode with less optical confinement (transverse magnetic, TM) to coincide with the target TMI length for a desired transmission of the mode with higher optical confinement (transverse electric, TE). The fabricated 0.94?μm long 2×2 TMI splits the input power into TM (bar) and TE (cross) outputs with splitting ratio over 15?dB over 50?nm bandwidth. Fabrication tolerance analysis shows that the device is tolerant to fabrication errors as large as 60?nm.     

Preparation of a trihydrazinotriazine-functionalized core-shell nanocatalyst as an extremely efficient catalyst for the synthesis of benzoxanthenes

In recent years, there is a high demand on utilizing heterogeneous nanocatalysts in organic synthetic routes because of their green approach, facile purification of the products, and reusability of the catalyst. Herein, we introduced trihydrazinotriazine (THDT)-coated Fe₃O₄@SiO₂ as a novel amino-functionalized magnetic nanocompostie. We fully characterized the nanocatalyst and proved the morphology and magnetic property of the nanoparticles by using essential analyses. The basic attribute of the amino-rich porous surface of the nanocomposite provides a desirable environment for enhancing various reaction conditions. To examine the applicability of the nanocatalyst in organic reactions, we synthesized several benzoxanthenes using Fe₃O₄@SiO₂-THDT nanocatalysts. The nanocomposite successfully improved the reaction conditions and provided the benzoxanthenes in an environmentally friendly procedure, which afforded product in excellent yields (80–96%) and reduced time. The nanomagnetic catalyst was easily recovered after each trial by using an external magnet. After six successive runs, the loss of catalytic activity of the nanocomposite was negligible. Finally, we propounded a plausible mechanism for the preparation of the benzoxanthenes derivatives using the THDT-functionalized core-shell magnetic nanocatalyst.     

Surfactant-Free Hydrothermal Synthesis of Mesoporous Niobia Samples and Their Photoinduced Decomposition of Terephthalic Acid (TPA)

This study introduces a low temperature surfactant-free hydrothermal method to synthesize mesoporous Nb₂O₅ photocatalysts using NbCl₅ and H₂O₂ as precursors that are subsequently calcinated at 300, 400 and 450 °C and are assigned as mNb₂O₅-300, mNb₂O₅-400 and mNb₂O₅-450, respectively. Commercial niobia sample was used as reference sample for comparison purpose. All of materials were characterized by XRD, SEM, UV–Vis DRS, FTIR, TG/DTG and BET techniques. The synthesized Nb₂O₅ particles especially mNb₂O₅-300 sample shows a high surface area (240 m²/g), a large pore volume (0.21 cm³/g) and an identifying morphology of these features. Photocatalytic decomposition of terephthalic acid was evaluated using UV–Vis spectrophotometer. The photocatalytic reactions followed pseudo-first-order kinetics with an apparent rate constant of k = 105 × 10^?3 min^?1 for mNb₂O₅-300 sample with the highest activity among all samples at natural pH (pH = 6). Meanwhile, it was observed that optimum pH of 4 resulted in fast photocatalytic reaction for mNb₂O₅-300 sample.     

Comparison Between Surface and Near-Surface Residual Stress Measurement Techniques Using a Standard Four-Point-Bend Specimen

Background

Determination of near-surface residual stresses is challenging for the available measurement techniques due to their limitations. These are often either beyond reach or associated with significant uncertainties.

Objective

This study describes a critical comparison between three methods of surface and near-surface residual stress measurements, including x-ray diffraction (XRD) and two incremental central hole-drilling techniques one based on strain-gauge rosette and the other based on electronic speckle pattern interferometry (ESPI).

Methods

These measurements were performed on standard four-point-bend beams of steel loaded to known nominal stresses, according to the ASTM standard. These were to evaluate the sensitivity of different techniques to the variation in the nominal stress, and their associated uncertainties.

Results

The XRD data showed very good correlations with the surface nominal stress, and with superb repeatability and small uncertainties. The results of the ESPI based hole-drilling technique were also in a good agreement with the XRD data and the expected nominal stress. However, those obtained by the strain gauge rosette based hole-drilling technique were not matching well with the data obtained by the other techniques nor with the nominal stress. This was found to be due to the generation of extensive compressive residual stress during surface preparation for strain gauge installation.

Conclusion

The ESPI method is proven to be the most suitable hole-drilling technique for measuring near-surface residual stresses within distances close to the surface that are beyond the penetration depth of x-ray and below the resolution of the strain gauge rosette based hole-drilling method.

     

A Simple Synthesis of 2‐{(Arylmethylidene)hydrazinylidene]‐3‐hydroxy‐4H‐furo[3,2‐c]pyran‐4(3H)‐ones

A simple synthesis of 2‐hydrazinylidene‐3‐hydroxy‐4H‐furo[3,2‐c]pyran‐4‐ones is described. A mixture of (isocyanoimino)(triphenyl)phosphorane, an aromatic aldehyde, and dehydroacetic acid (=3‐acetyl‐2‐hydroxy‐6‐methyl‐4H‐pyran‐4‐one) undergo a 1 : 1 : 1 addition reaction under mild conditions to afford the title compounds in excellent yields.     

Frame properties of wave packet systems in L^2({\mathbb R}^d)

Extending work by Hernandez, Labate and Weiss, we present a sufficent condition for a generalized shift-invariant system to be a Bessel sequence or even a frame for . In particular, this leads to a sufficient condition for a wave packet system to form a frame. On the other hand, we show that certain natural conditions on the parameters of such a system exclude the frame property.      

Molecular simulation of protein dynamics in nanopores. I. Stability and folding

Discontinuous molecular dynamics simulations, together with the protein intermediate resolution model, an intermediate-resolution model of proteins, are used to carry out several microsecond-long simulations and study folding transition and stability of alpha-de novo-designed proteins in slit nanopores. Both attractive and repulsive interaction potentials between the proteins and the pore walls are considered. Near the folding temperature T(f) and in the presence of the attractive potential, the proteins undergo a repeating sequence of folding/partially folding/unfolding transitions, with T(f) decreasing with decreasing pore sizes. The unfolded states may even be completely adsorbed on the pore's walls with a negative potential energy. In such pores the energetic effects dominate the entropic effects. As a result, the unfolded state is stabilized, with a folding temperature T(f) which is lower than its value in the bulk and that, compared with the bulk, the folding rate decreases. The opposite is true in the presence of a repulsive interaction potential between the proteins and the walls. Moreover, for short proteins in very tight pores with attractive walls, there exists an unfolded state with only one alpha-helical hydrogen bond and an energy nearly equal to that of the folded state. The proteins have, however, high entropies, implying that they cannot fold onto their native structure, whereas in the presence of repulsive walls the proteins do attain their native structure. There is a pronounced asymmetry between the two termini of the protein with respect to their interaction with the pore walls. The effect of a variety of factors, including the pore size and the proteins' length, as well as the temperature, is studied in detail.