Three-dimensional Pd/Pt bimetallic nanodendrites on a highly porous copper foam fiber for headspace solid-phase microextraction of BTEX prior to their quantification by GC-FID

The preparation of bimetallic Pd/Pt nanofoam for use in fiber based solid-phase microextraction (SPME) is described. First, a highly porous copper foam was prepared on the surface of an unbreakable copper wire by an electrochemical method. Then, the substrate was covered with metallic Pd and Pt using galvanic replacement of the Cu nanofoam substrate by applying a mixture of Pd(II) and Pt(IV) ions. The procedure provided an efficient route to modify Pd/Pt nanofoams with large specific surface and low loading with expensive noble metals. The fiber was applied to headspace SPME of benzene, toluene, ethylbenzene and xylene (BTEX) (as the model compounds) in various spiked water and wastewater samples. It was followed by gas chromatography-flame ionization detection (GC-FID). A Plackett-Burman design was performed for screening the experimental factors prior to Box-Behnken design. Compared with the commercial PDMS SPME fiber (100 μm), it had higher extraction efficiency for BTEX. Under the optimum conditions, the method has low limits of detection (0.16–0.35 μg L^?1), a wide linear range (1–200 μg L^?1), relative standard deviations between 5.8 and 10.5%, and good recoveries (>85% from spiked samples).

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Graphical abstract Schematic presentation of a three-dimensional Pd/Pt bimetallic nanodendrites supported on a highly porous copper foam fiber for use in headspace solid phase microextraction of BTEX. They were then quantified by gas chromatography–flame ionization detector.

     

Magnetic solid-phase extraction of warfarin and gemfibrozil in biological samples using polydopamine-coated magnetic nanoparticles via core-shell nanostructure

Herein, polydopamine-coated Fe₃O₄ spheres were synthesized using a very simple, easy, cost-effective, efficient, and fast method. First, magnetic nanoparticles (Fe₃O₄) were synthesized and were followed by accommodating polydopamine on the surface of the prepared Fe₃O₄. The prepared polydopamine-coated Fe₃O₄ spheres were utilized as a sorbent in magnetic solid phase extraction of gemfibrozil and warfarin (as the model analytes). The extracted model analytes were desorbed by a suitable organic solvent and were analyzed by high-performance liquid chromatography. Under optimized condition, the linearity of the method was in the range of 0.1–200.0 μg/L for the selected analytes in water. The limits of detection were calculated to be in the range of 0.026–0.055 μg/L for warfarin and gemfibrozil, respectively. The limits of quantification were calculated to be in the range of 0.089–0.185 μg/L. The inter-day and intra-day relative standard deviations were determined to be in the range of 1.4%–3.3% in three concentrations in order to calculate the method precision. Furthermore, the enrichment factors were found to be 78 and 81 for warfarin and gemfibrozil, respectively. Moreover, the calculated absolute recoveries were between 78% and 81%. The obtained recoveries indicated that the method was useful and applicable in complicated real samples.     

Adsorption Kinetics,Equilibrium, and Thermodynamics of Copper From Aqueous Solutions using Silicon Carbide Derived from Rice Waste

Adsorption of Cu(II) from aqueous solution on a novel adsorbent, silicon carbide ash (SiC ash), was studied using batch technique. The adsorbent was prepared by pyrolysis of Egyptian rice waste (rice straw and rice husk) and was characterized by scanning electron microscopy (SEM), energy-dispersive x-ray (EDX), Fourier-transform infrared (FTIR) spectroscopy, x-ray diffraction (XRD), and surface area analysis by Brunauer-Emmett-Teller (BET) Theory. The influence of pH, contact time, initial Cu(II) concentration, adsorbent dose, agitation speed, and temperature was investigated. Adsorption kinetics was analyzed using the pseudo-first-order, the pseudo-second-order, and intraparticular diffusion model. The adsorption process was found to follow a pseudo-second-order rate mechanism. The adsorption isotherm data could be well described by the Langmuir and Freundlich than the Dubinin–Radushkevich adsorption model. The adsorption capacity of 22.06 mg g^?1for SiC ash was obtained at pH = 5 and temperature of 298 K. Thermodynamic parameters, change in the free energy (ΔG°), the enthalpy (ΔH°), and the entropy (ΔS°), were also calculated. The overall adsorption process was exothermic, spontaneous in nature, and proceeds with decreased randomness as the entropy is negative value. Adsorption process was successfully applied to remove Cu(II) from an industrial wastewater sample.     

Computational Design,Synthesis and Application of a New Selective Molecularly Imprinted Polymer for Electrochemical Detection

A computational approach was developed to find a suitable functional monomer to design a new molecularly imprinted polymer (MIP), based on which methacyrlic acid (MAA) was selected as a functional monomer to synthesize the molecular imprinted and non‐imprinted polymers. All calculations were carried out using Gaussian 03 software based on the application of Hartree?Fock (HF) method with 6‐31G (d) basis set. The performance of the MIPs prepared with different ratios of MAA was then evaluated using equilibrium rebinding assays. The MIP with the highest binding capacity was chosen as recognition material for the fabrication of new PVC sensors and their responses were compared with each other and with previously reported modifiers in literature. The addition of the ionic surfactant (TFPB) was found to have a synergistic effect on the response mechanism of the electrodes. The results of the MIP modified sensors show that they provide an improved electrode slope, wider pH range and a highly extended life time reaching 7 months compared to 2–4 weeks in case of traditional ion‐exchangers reported in literature, besides, being successfully applied for measurements in biological samples.     

QuEChERS method combined with GC‒MS for pesticide residues determination in water

A miniaturized, QuEChERS based, liquid–liquid extraction method followed by gas chromatography–mass spectrometry was developed and validated for pesticide residues determination in water. Malathion, chlorpyrifos, profenofos, chlorfenapyr, pyriproxyfen, λ-cyhalothrin, coumaphos and α-cypermethrin were selected for this study. The accuracy, precision, specificity, linearity, limit of detection and limit of quantification were evaluated. The recovery ranged from 85.3 to 107% with RSD ranging from 1.8 to 15.4%. The linearity showed reliable range (0.995–0.999). The limit of detection ranged from 0.3 to 4 μg/L. Matrix effect was evaluated. The obtained results meet the European Commission standard legislations, implying that our method can be considered accurate and reproducible. The validated method was used to analyze river and well water samples. No residues of the investigated pesticides were detected in all collected water samples.     

Cardinality enrichment of flexible cross correlation (FCC) code for SAC-OCDMA system by alleviation interference scheme (AIS)

In this paper, we propose an alleviation interference scheme (AIS) for spectral amplitude coding (SAC) – optical code division multiple access (OCDMA) coding system approaches. The AIS SAC-OCDMA systems is demonstrated by utilizing the new flexible cross correlation (FCC) code. The FCC code has advantages, such as flexibility in-phase cross-correlation at any given number of users and weights, as well as effectively reduces the impacts of phase-induced intensity noise (PIIN) and has the multiple-access interference (MAI) cancelation property. The results indicated good performance whereas the FCC (W = 4, K = 150) AIS SAC-OCDMA coding system offers 66%, 172%, 650% and 900% percentage of cardinality enrichments as a contrast to DCS (W = 4, K = 90), MDW (W = 4, K = 55), MFH (W = 4, K = 20) and Hadamard (W = 8, K = 15) codes, respectively. Finally, the FCC AIS SAC-OCDMA coding system has low effective receive power Psr = −21 dBm which is expected to be more significant for future SAC-OCDMA coding systems without requiring any amplification at the receiving plant.     

Investigation of the intracavity frequency doubling of a gain-switched InGaAs/GaAs pulsed diode laser

A mathematical model describing the dynamic emission of the intracavity frequency doubling (IFD) of a gain-switched two-section InGaAs/GaAs diode laser has been presented. One section is electrically pumped to provide gain, while the second section is unpumped (reverse biased) to provide a saturable absorber. The three-dimensional physical problem is reduced to one-dimensional model using adiabatic approximation, which allows the separation of the wavefunction. The suggested model in this paper allows studying the impact of the variations of the input InGaAs/GaAs/KTP diode laser parameters on the output pulsation characteristics. The proposed mathematical model is solved numerically using fourth-order Runge-Kutta method. The numerical calculations reflect the influence of the variation of the applied gain current and saturable bias current on the output laser pulse characteristics. The numerical results show good consistency with the available experimental data in references.     

Electrophoretic deposited MWCNT composite graphite pencils and its uses to determine hyperin

A simple, fast, and effective method of fabricating electrochemical sensors using composite pencil graphite (CPG) lead modified with carboxylic multiwalled carbon nanotube (c-MWCNT) via electrophoretic deposition (EPD) has been developed. The EPD of c-MWCNT film on the CPG electrode (CPGE) was carried out at a constant applied potential of 25?V and deposition time of 1?min. The electrochemical performances of the modified CPGE, i.e., c-MWCNT/CPGE, in Fe(CN) ₆ ^4?/3? has been studied by cyclic voltammetry and electrochemical impedance spectroscopy (EIS). The c-MWCNT/CPGE has better current density, onset potentials, and charge transfer resistances than the CPGE. The c-MWCNT/CPGE has been successfully used to analyze hyperin in dry fruits of Acanthopanax sessiliflorus.