Preconcentration of trace metals on Amberlite XAD-4 resin coated with dithiocarbamates and determination by inductively coupled plasma-atomic emission spectrometry in saline matrices

Preconcentration of Cd(II), Cu(II), Mn(II), Ni(II), Pb(II) and Zn(II) in saline matrices on Amberlite XAD-4 resins coated with ammonium pyrrolidine dithiocarbamate (APDC) and piperidine dithiocarbamate (pipDTC) and subsequent determination by inductively coupled plasma atomic emission spectrometry were studied. Parameters such as effect of pH, effect of HNO(3) concentration on elution of metals from resin were studied. The results show that Amberlite XAD-4 coated with APDC was more efficient in the recovery of metal ions compared with Amberlite XAD-4 coated with pipDTC, in the concentration range of 0.1-200 mug l(-1), for 1 g of Amberlite XAD-4 coated resin. The detection limits for Cd(II), Cu(II), Mn(II), Ni(II), Pb(II), Zn(II) are 0.1, 0.4, 0.3, 0.4, 0.6, 0.5 mug l(-1), respectively, for resin coated with APDC and 0.7, 1.0, 0.8, 0.9, 1.7 and 1.2 mug l(-1) for resin coated with pipDTC. The effect of diverse ions on the determination of aforesaid metals was studied. The method was applied for the determination of trace metal ions in artificial sea water and natural water samples. The results were compared with extraction AAS method.     

Liquid chromatography–tandem mass spectrometry method for simultaneous quantification of urapidil and aripiprazole in human plasma and its application to human pharmacokinetic study

A sensitive and selective liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for simultaneous determination of urapidil and aripiprazole in human plasma. A simple liquid–liquid extraction with ethyl acetate was used for the sample preparation. Chromatographic separation was achieved on a Phenomenex C₁₈ (4.6 × 50 mm, 5 µm) column with 0.1% formic acid–acetonitrile (10:90, v/v) as the mobile phase with flow rate of 0.6 mL/min. The quantitation of the target compounds was determined in a positive ion multiple reaction monitoring mode. Calibration plots were linear over the range of 2.0–2503.95 ng/mL for urapidil and 1.0–500.19 ng/mL for aripiprazole. The lower limit of quantitation for urapidil and aripiprazole was 2.0 and 1.0 ng/mL, respectively. Mean recovery was in the range of 69.94–75.62% for both analytes and internal standards. Intra‐day and inter‐day precisions of the assay at three concentrations were 2.56–5.89% with accuracy of 92.31–97.83% for urapidil, and 3.14–6.84% with accuracy of 91.38–94.42% for aripiprazole. The method was successfully applied to human pharmacokinetic study of urapidil and aripiprazole in healthy human male volunteers. Copyright © 2013 John Wiley & Sons, Ltd.     

Synthesis of VO2 (B) nanorods for Li battery application

Vanadium dioxide nanorods were synthesized through a hydrothermal reaction from V₂O₅ xerogel, poly(vinyl pyrrolidone) (PVP) and lithium perchlorate (LiClO₄). The prepared samples were characterized by X-ray diffraction, infrared spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electrochemical discharge–charge cycling in lithium battery. SEM images reveal the nanorods to have dimensions on the order of 1–3 μm in length and 10–50 nm in diameter. The measured initial discharge capacity of the lithium battery with a cathode made of VO₂ (B) nanorods was 152 mA h/g.     

Characterization of MoO3 nanorods for lithium battery using PVP as a surfactant

We synthesized MoO₃ nanorods using poly (vinyl pyrrolidone) (PVP) as a surfactant through the hydrothermal route for making a cathode for a lithium battery. Scanning electron microscopy images reveal the structures to have dimensions on the order of 1–10 μm in length and 50–200 nm in diameter. Analytical techniques such as X-ray diffractometry, Fourier transformation infrared spectroscopy, thermogravimetric analysis, and cyclic voltammetry were used to characterize the nanorods. The measured specific charge of MoO₃ nanorods prepared through a 15-day hydrothermal reaction was 156 mAhg⁻¹ during the initial discharge process.     

Characterization of SBA-15 doped (PEO + LiClO4) polymer electrolytes for electrochemical applications

SBA-15 mesoporous material was prepared by the simple hydrothermal process and added to poly(ethylene oxide) (PEO) and lithium percholorate (LiClO₄) as a filler. X-ray Diffractometry (XRD), Differential Scanning Calorimetry (DSC) and Scanning Electron Microscopy (SEM) were used to determine the characteristics of the composite polymer electrolyte. The SEM of the electrolyte containing 10 wt% of SBA-15 confirms the highest miscibility and amorphous nature. SBA-15 doped (PEO + LiClO₄) polymer electrolytes have shown improved conductivity over the pure PEO and (PEO + LiClO₄) electrolyte. The mesoporous SBA-15 acted as crystal cores and fined the crystallites thus decreasing the crystallinity, which provided a much more continuous amorphous domain for Li⁺ ions to move easily in the (PEO + LiClO₄) electrolyte.     

Functionalization of cross linked chitosan with 2-aminopyridine-3-carboxylic acid for solid phase extraction of cadmium and zinc ions and their determination by atomic absorption spectrometry

We have developed a new method for solid phase extraction (SPE) and preconcentration of trace amounts of cadmium and zinc using cross linked chitosan that was functionalized with 2-aminopyridine-3-carboxy acid. Analytical parameters, sample pH, effect of flow rate, sample volume, and concentration of eluent on column SPE were investigated. The effect of matrix ions on the recovery of cadmium and zinc has been investigated and were found not to interfere with preconcentration. Under the optimum experimental conditions, the preconcentration factors for Cd(II) and Zn(II) were found to be 90. The two elements were quantified via atomic absorption spectrometry. The detection limits for cadmium and zinc are 21 and 65?ng?L^?1, respectively. The method was evaluated by analyzing a certified reference material (NIST 1643e; water) and has been successfully applied to the analysis of cadmium and zinc in environmental water samples.

Morphological and mechanical behavior of montmorillonite grafted block copolymer brushes

Here we report the phase behavior of a family of montmorillonite (MMT) block copolymer brushes (MBBs), a novel class of polymer nanocomposites. MBBs are comprised of discrete MMT platelets encapsulated with block copolymer brushes. These MBBs were synthesized via surface-initiated atom transfer radical polymerization using halogenated alkylammonium surfactants to localize initiation sites on the clay surfaces. Two styreninc MBB systems—poly(styrene-b-n-butyl acrylate) and poly(styrene-b-t-butyl acrylate)—were prepared varying the composition and total 80–250 kDa. MBB materials were compared with their non-clay bulk block copolymer counterparts via electron microscopy and a host of mechanical tests in both the solid and melt states. Notably, MBBs have similar melt-state rheological properties compared to neat block copolymers and are thus amenable to current processing techniques. MBBs were found to self-assemble into single grain morphologies across incredibly large areas (>3 μm) which resulted in extremely well-ordered, defect-free lamellar structures with applications in microelectronics. © 2015 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2016, 54, 353–361     

Synthesis,spectral characterization,docking studies and biological activity of urea,thiourea, sulfonamide and carbamate derivatives of imatinib intermediate

Molecular Diversity - A series of new urea/thiourea derivatives 3a–j were synthesized by simple addition reaction of functionalized phenyl isocyanates/isothiocyanates 2a–j with...