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A capillary zone electrophoresis method was developed for the determination of NiII(3-OMe-salophene), a substance with anticancer activity in vitro. A fused silica capillary (56 cm × 100 µm) was used for this purpose. The method was optimized in terms of parameters affecting the electrophoretic conditions in order to optimize separation efficiency and total time of migration. The analysis was best performed using an operating buffer of 50 mM borate, adjusted to pH 9.3, mixed with acetonitrile (50%, v/v) as organic modifier. Injections were performed hydrodynamically by applying a pressure of 50 mbar for 8 s, and a 30 kV separation voltage was selected at 25 °C. Detection was carried out at 250 nm using diode array detector (DAD). The method allowed the separation of NiII(3-OMe-salophene) from four other structurally related impurities in a total migration time (tm) of 8 min. Peak identification was achieved using the standard reference of individual impurities. The purity of the migrated NiII(3-OMe-salophene) was confirmed by Ultra-violet (UV) scan overlay depending on DAD. The linear ranges for the determination of NiII(3-OMe-salophene) was 400–20,000 ng mL−1 with limit of detection (LOD) of 120 ng mL−1. Acceptable intra-day and inter-day precisions were achieved (%relative standard deviation (RSD) results were less than 0.76% and 0.30%, respectively). The proposed method was assessed for greenness and compared to reported methodologies to prove superiority.

(E)-5-(Methoxyimino)-1,3,4,5-tetrahydro-2H-benzo[b]azepin-2-one was prepared by a condensation reaction from 3,4-dihydro-1H-benzo[b]azepin-2,5-dione and O-methylhydroxylamine. The configuration at the C=N double bond was determined by X-ray crystallography.

Chondroitin sulfate A was covalently immobilized onto a monolithic silica epoxy column involving a Schiff base formation in the presence of ethylenediamine as a spacer and evaluated in terms of its selectivity in enantioseparation. The obtained column was utilized as a chiral stationary phase in enantioseparation of amlodipine and verapamil using a mobile phase consisting of 50 mM phosphate buffer pH 3.5 and UV detection. Sample dilution by organic solvents (preferably 25% v/v acetonitrile-aqueous solution) was applied to achieve baseline enantioresolution (Rs &gt, 3.0) of the individual drug models within 7 min, an excellent linearity (R2 = 0.999) and an interday repeatability of 1.1% to 1.8% RSD. The performance of the immobilized column for quantification of racemate in commercial tablets showed a recovery of 86&ndash, 98% from tablet matrices. Computational modeling by molecular docking was employed to investigate the feasible complexes between enantiomers and the chiral selector.

Gold amalgam microelectrodes (GAMEs) have been characterized and successfully calibrated to measure &gt, 1.5 mM (30 mg L&minus, 1) sulfide in artificial wastewater (AWW) using cathodic stripping voltammetry (CSV). Microbial sulfide generation in two types of AWW was traced. Artificial wastewater type 1 (AWW1) held the potential for almost 50% conversion of sulfur compounds at a maximum rate of ~4.3 &plusmn, 0.5 &micro, M h&minus, 1 while AWW 2 held a potential for 75&ndash, 100% conversion at a rate of 165 &micro, 1. In addition, the GAMEs were thoroughly examined during fabrication, maturation, and aging. An earlier described plating method was found to result in varying electrode surfaces due to excess mercury deposition and, therefore, deviating stripping signals. The limited shelf life of GAMEs has been proposed previously. This study shows the extent of electrode surface changes during amalgam formation and the wear and tear of application. As a result, suggestions to optimize fabrication and application are discussed to provide reliable measurements and proceed toward a future commercialization.

Water pollution caused by industrial wastes containing heavy metals and dyes is a major environmental problem. This study reports on the synthesis, characterization, and utilizations of Polyaniline (PANI) and its composites with Fe3O4 for the removal of hexavalent chromium Cr(VI) and divalent nickel Ni(II) ions from water. The adsorption data were fitted in Freudlich, Langmuir, Tempkin, Dubbanin&ndash, Ruddishkawich (D&ndash, R), and Elovich adsorption isotherms. The Freundlich isotherm fits more closely to the adsorption data with R2 values of 0.9472, 0.9890, and 0.9684 for adsorption of Cr(VI) on Fe3O4, PANI, and PANI/Fe3O4 composites, respectively, while for adsorption of Ni(II) these values were 0.9366, 0.9232, and 0.9307 respectively. The effects of solution pH, initial concentration, contact time, ionic strength, and adsorbent dosage on adsorption behavior were investigated. The adsorption ability of composites was compared with pristine PANI and Fe3O4 particles. Activation energy and other thermodynamic properties such as changes in enthalpy, entropy, and Gibbs free energy indicated spontaneous and exothermic adsorption.

An eco-friendly solid-state symmetric ultracapacitor (Uc) device was fabricated using a polyaniline graphene oxide composite co-doped with sulfuric acid (H2SO4) and dodecyl benzene sulfonic acid (DBSA) or camphor sulfonic acid (CSA), as electrode material utilizing gold sheets as current collectors. The device showed specific capacitance value of 150 F/g at 1 A/g current density, with a capacitance retention value of 93.33% at higher current density (10 A/g), indicating a high rate capability. An energy density of 15.30 Whkg−1 with a power density of 1716 Wkg−1 was obtained at the current density of 1 A/g. The values of areal capacitance, power density, and energy density, achieved at the current density of 5 mAcm−2, were 97.38 mFcm−2, 9.93 mWhcm−2, and 1.1 Wcm−2, respectively. Additionally, the device showed very low solution and charge transfer resistance (0.885 Ω and 0.475 Ω, respectively). A device was also fabricated utilizing copper as current collector; however, a lower value of specific capacitance (82 F/g) was observed in this case.

The cost effective synthesis of electroactive polyaniline (PANI) while retaining its desirable properties is one of the most debatable and challenging tasks for researchers in the field. Herein, we report a cost effective inverse emulsion polymerization pathway for the synthesis of soluble and processable PANI salt by using diesel as a novel dispersion medium. Different reaction parameters and their effects on the properties and yield of polyaniline were optimized. The polymer exhibited a highly porous morphology and was found to be stable up to 417 °C. The PANI salt showed good solubility in common solvents, such as chloroform, N-Methyl-2-pyrrolidone (NMP), dimethyl sulphoxide (DMSO) and in a 1:3 mixtures by volume of 2-propanol and toluene. The coating of the synthesized PANI salt on stainless steel has shown good corrosion resistant behavior in marine water by reducing the corrosion rate to 67.9% as compared to uncoated stainless steel.

Alkynyl functionalized boron compounds are versatile intermediates in the areas of medicinal chemistry, materials science, and optical materials. In particular, alkynyl boronate esters [R1−C≡C−B(OR2)2] are of interest since they provide reactivity at both the alkyne entity, with retention of the B−C bond or alkyne transfer to electrophilic substrates with scission of the latter. The boron atom is commonly well stabilized due to (i) the extraordinary strength of two B−O bonds, and (ii) the chelate effect exerted by a bifunctional alcohol. We reasoned that the replacement of a B−O for a B−S bond would lead to higher reactivity and post-functionalization in the resulting alkynyl boronate thioesters [R1−C≡C−B(S2X)]. Access to this poorly investigated class of compounds starts form chloro dithioborolane cyclo-Cl−B(S2C2H4) as a representative example. Whereas syntheses of three coordinate alkynyl boronate thioesters [R1−C≡C−B(S2X)] proved to be ineffective, the reactions of NHC-adducts (NHC = N-heterocyclic carbene) of cyclo-Cl-B(S2C2H4) afforded the alkyne substituted thioboronate esters in good yield. The products NHC−B(S2C2H4)(C≡C-R1) are remarkably stable towards water and air, which suggests their use as boron-based building blocks for applications akin to oxygen-based boronate esters.

Although current desalination technologies are mature enough and advanced, the shortage of freshwater is still considered as one of the most pressing global issues. Therefore, there is a strong incentive to explore and investigate new potential methods with low energy consumption. We have previously reported that reversible thermally induced sorption/desorption process using polymeric hydrogels hold promise for water desalination with further development. In order to develop a more effective hydrogels architecture, polyelectrolyte moieties were introduced in this work as pendent chains and a thermally responsive polymer as network backbone using reversible addition-fragmentation chain transfer (RAFT) polymerisation. The ability of the comb-type polymeric hydrogels to desalinate water was evaluated. These hydrogels were proved to absorb water with low salinity from brine solution of 2 g L − 1 NaCl and release the absorbed water at relatively low temperature conditions of 50 ∘ C. The fraction of the grafted polyacrylic acid and the comb-chain length were varied to understand their influence on the swelling/deswelling behaviour for these hydrogels. The ionic fraction in the hydrogels and the resulting hydrophilic/hydrophobic balance are crucial for the proposed desalination process. In contrast, the comb-chain length impacted the swelling behaviour of hydrogels but showed relatively little influence on the dewatering process.

Molecules : a journal of synthetic chemistry and natural product chemistry / Molecular Diversity Preservation International 23(2), 64 (2018). doi:10.3390/molecules23020064, Published by MDPI, Basel