Comparison of selectivity and sensitivity of various ferric selective electrodes prepared using N-((bis(dimethyl amino)methylene)carbamothioyl)benzamide.

N-((Bis(dimethyl amino)methylene)carbamothioyl)benzamide (NBMCB) was synthesized, characterized, and used as an ionophore for producing three novel ion-selective potentiometric sensors for Fe(III) determination. Firstly, using the molecular mechanic-based MMFF94 method, the most stable NBMCB's conformer and its isosteric complexes with various cations were determined. According to the Gibbs free energy results of the reaction, the thermodynamic complexation reactivity of Fe(III) and the ligand was acceptable. These results were obtained using the B3LYP approach and the 6-31G(d,p) basis set that was substituted for heavy metals by the LanL2DZ basis set. We used UV-visible spectrophotometry to confirm the tendency of NBMCB to react with Fe(III). Generally, three diverse liquid membrane ferric selective electrodes were obtained by the use of the specified ligand: classic with a liquid internal electrolyte-ferric selective electrode (LIE-FSE), solid state-FSE (SS-FSE), and coated wire-FSE (CW-FSE). The reactions exhibited Nernstian behavior across all electrodes. The limit of detection was enhanced for the SS-FSE (3 × 10-9 M) and the CW-FSE (3 × 10-7 M) in comparison with that of the LIE-FSE (7 × 10-7 M). The lifetime of the LIE-FSE was 8 weeks, while it was 10 weeks for the SS-FSE and the CW-FSE. Elimination of the internal solution reduced the limit of detection and prolonged the lifespan of the sensors. Also, the three electrodes all had a short response time of around 5-7 s. The sensors were utilized as indicator electrodes during the potentiometric titration of Fe(III) using ethylenediaminetetraacetic acid.

Fast chromium determination in pharmaceutical tablets by using electrochemical sensors: Preparation and comparison.

In the present paper, three electrodes were prepared with the aim of detecting chromium (III) in pharmaceutical tablets and comparing their capabilities and efficiency. At first, N-(pyridine-2-ylcarbamothioyl) benzamide (NP2YCTB) was synthesized and characterized by 1H NMR, FTIR, and 13C NMR spectroscopy methods. Then, it is used as a sensing material to prepare three types of chromium potentiometry sensors including solid-state electrodes (SSE), coated wire electrodes (CWE) as asymmetric electrodes, and liquid membrane electrodes (LME) as symmetric electrodes. The responses of all electrodes were Nernstian. Field-emission scanning electron microscopy was utilized to investigate the liquid membrane morphology. The presence of chromium (III) in the membrane was proved using Energy-dispersive X-ray spectroscopy and the coordination of NP2YCTB heteroatoms with chromium (III) was confirmed by Fourier transform infrared spectroscopy. The limit of detection for SSE (3 × 10-9 mol/L) was enhanced compared with LME (7 × 10-6 mol/L) and CWE (3 × 10-7 mol/L). The response time of electrodes was very short so it was about 5-6 s for LME and CWE and 5-8 s for SSE. The sensors were used for the potentiometric determination of chromium (III) in pharmaceutical tablets and in the potentiometric titration of it with EDTA.

Chromium measurement in pharmaceutical samples: a comparative study of three new membrane electrodes with different electron-ion exchangers.

The present study deals with synthesis of N-(thiazol-2-ylcarbamothioyl) benzamide. It was utilized as a neutral ionophore for designing three types of chromium(III) sensors including coated wire ion selective electrodes (CW-ISEs), ion selective electrodes with liquid internal electrolyte (LIE-ISEs), and solid-state ion selective electrodes (SS-ISEs). UV-visible spectrophotometry was used to confirm the affinity of N-(thiazol-2-ylcarbamothioyl) benzamide to chromium(III). It was found that a membrane with a composition of 2% NaTPB, 8% ionophore, 60% DBP, and 30% PVC showed the best performance and a Nernstian slope of 21.6 mV per decade. Scanning electron microscopy was used to assess the PVC membrane morphology. The existence of chromium(III) in the liquid membrane matrix was proved by energy-dispersive X-ray spectroscopy. Detection limits for SS-ISE (1 × 10-6 M) and CW-ISE (1 × 10-6 M) were enhanced relative to LIE-ISE (1 × 10-5 M). All three electrodes showed a response time of about 5 s. The sensors' applicable pH range was 4.0-6.0. Fourier transform infrared spectra recorded through the electrode membrane showed that chromium(III) ion can interact with sulfur, nitrogen and oxygen atoms of N-(thiazol-2-ylcarbamothioyl) benzamide. The sensors were utilized as indicator electrodes in chromium(III) potentiometric titration with ethylenediaminetetraacetic acid and for directly measuring chromium(III) in some pharmaceutical samples.

Bio-Fe3O4 Magnetic Nanoparticles Promoted Green Synthesis of thioxo- 1,3-Oxazole Derivatives: Study of Antimicrobial and Antioxidant Activity.

AIMS AND OBJECTIVE: In this work, 1,3-oxazoles were generated using the multicomponent reaction of α-bromo ketones, alkyl (aryl) isothiocyanates, sodium hydride and Fe3O4 MNPs in the water at room temperature in good yields. The nanoparticles generated via the biosynthesis method have potential value in different purposes, such as organic synthesis. MATERIALS AND METHODS: To study the antioxidant ability of some synthesized thioxo-1,3-oxazoles, diphenyl-picrylhydrazine (DPPH) radical trapping and power of ferric reduction testes are employed. Among the studied thioxo-1,3-oxazoles, compound 4b have good power for radical trapping and reduction activity than the standard antioxidants such as BHT and TBHQ. In addition, the antimicrobial activity of some thioxo-1,3-oxazoles was studied, employing the disk diffusion test on Gram-positive bacteria and Gram-negative bacteria. The results of the disk diffusion test showed that compounds 4a, 4b, 4d and 4f prevented bacterial growth. RESULTS: Without employing catalyst, these reactions have low yield and busy mixture. The synthesis of compound 4a as sample reaction has a similar yield in the presence of ZnO-NPs and Fe3O4 MNPs (entry 20 and entry 30), but the removal of catalyst from the mixture of reaction after the completion of the reaction is comfortable in the presence of Fe3O4 MNPs. Structures of compound 4a-4i are confirmed by IR, 1H NMR and 13C NMR mass spectra. CONCLUSION: The reaction of α-bromo ketones, isothiocyanate and sodium hydride in the presence of the catalytic amount of Fe3O4 MNPs in water generates 1,3-oxazole derivatives in good yields. Some of the advantages of performing these reactions with the present procedure are to carry out these reactions in water as a green solvent and simple removal of catalyst.

CuO nanostructures: optical properties and morphology control by pyridinium-based ionic liquids.

Copper oxide nanostructures have been synthesized by a simple reflux method in aqueous medium of pyridinium based ionic liquids. The structural and optical properties of CuO nanostructures were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), photoluminescence spectroscopy (PL) and UV-visible. The morphologies of the nanostructures can be controlled by changing the amount of NaOH and ionic liquids. The results show that the use identical pyridinium based ionic liquids in ratio of 4:1 NaOH/Cu(OAc)2⋅H2O yield minor differences in morphology of CuO nanostructures. Different morphologies of CuO nanostructures were obtained by changing the ratio NaOH/Cu(OAc)2⋅H2O to 2:1. Ionic liquids play an important role on optical properties of CuO nanostructures. The results of optical measurements of the CuO nanostructures illustrate that band gaps are estimated to be 1.67-1.85 eV. PL patterns studies show that the ionic liquids can be effect on PL patterns of the samples. The reasons of these phenomena are discussed.