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.

Intercalated chitosan-ionic liquid ionogel in SnO nanoplate: band gap narrow and adsorption-photodegradation process.

Ionogels are a category of hybrid material containing ionic liquid stabilized by polymeric network. These composites have some applications in solid-state, energy storage devices and environmental studies. In this research, chitosan (CS), ethyl pyridinium iodide ionic liquid (IL), and ionogel (IG) consisting of chitosan and ionic liquid were used in the preparation of a SnO nanoplate (SnO-IL, SnO-CS and SnO-IG). For the preparation of the ethyl pyridinium iodide, a mixture of pyridine and iodoethane (1: 2 molar ratio) was refluxed for 24 hours. The ionogel was formed using ethyl pyridinium iodide ionic liquid in chitosan that was dissolved in acetic acid (1 % v/v). By increasing NH3∙H2O, the pH of the ionogel reached 7-8. Then, the resultant IG was mixed with SnO in an ultrasonic bath for 1 h. The microstructure of the ionogel was involved as assembled unit via π-π, electrostatic and hydrogen bonding interactions to be three-dimensional networks. The intercalated ionic liquid and chitosan influenced the stability of the SnO nanoplates and improved band gap values. When chitosan was contained as the interlayer space of the SnO nanostructure, the resulting biocomposite formed a well-ordered flower-like SnO structure. These hybrid material structures were characterized by FT-IR, XRD, SEM, TGA, DSC, BET, and DRS techniques. The changes in the band gap values for photocatalysis applications were investigated. In the case of SnO, SnO-IL, SnO-CS, and SnO-IG, the band gap energy was 3.9, 3.6, 3.2, and 2.8 eV, respectively. The dye removal efficiency of SnO-IG was 98.5, 98.8, 97.9, and 98.4 % via the second-order kinetic model for Reactive Red 141, Reactive Red 195, Reactive Red 198, and Reactive Yellow 18, respectively. The maximum adsorption capacity of SnO-IG was 540.5, 584.7, 1501.5, and 1100.1 mg/g for Red 141, Red 195, Red 198, and Yellow 18 dyes, respectively. Also, an acceptable result (96.47 % dye removal) was obtained with the prepared SnO-IG biocomposite for dye removal from textile wastewater.

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.

A comparative study on selectivity and sensitivity of new chromium and copper electrodes.

4-Methylcoumarin-7-yloxy-N-phenyl acetamide and 4-methylcoumarin-7-yloxy-N-4-nitrophenyl acetamide were synthesized and used as new ionophores in the carbon paste matrix to produce two novel potentiometric modified electrodes. The selectivity of the electrode changed from copper (II) to chromium (III) with the addition of a nitro group to the phenyl ring of the ionophore. The ionophores' tendency to ions was confirmed by UV-visible spectrophotometry. Both electrodes were modified by multi-walled carbon nanotubes (MWCNTs) as an excellent modifier of carbon paste electrode (CPE). The best sensor response in the case of copper (II) selective CPE was obtained by 5% ionophore, 65% graphite powder, 5% MWCNT, and 25% paraffin oil. In addition, in the case of chromium (III) selective CPE, these conditions are 20% ionophore, 50% graphite powder, 5% MWCNT, and 25% paraffin oil. The copper (II) selective CPE showed a Nernstian slope of 32.15 mV/decade within the concentration range of 1.0 × 10-10-1.0 × 10-1 mol L-1, while chromium (III) selective CPE showed a Nernstian slope of 19.28 mV/decade over the concentration range of 1.0 × 10-10-7.0 × 10-3 mol L-1. The electrodes have short response time of less than 5 s and were used successfully to determine copper (II) in wastewater and to speciation of chromium (III) and chromium (VI).

Dichlorido(di-2-pyridylamine)mercury(II).

In the mol-ecule of the title compound, [HgCl(2)(C(10)H(9)N(3))], the Hg(II) atom is four-coordinated in a distorted tetra-hedral configuration by two N atoms from the chelating di-2-pyridylamine ligand and by two Cl atoms. In the crystal structure, inter-molecular N-H⋯Cl hydrogen bonds link the mol-ecules into centrosymmetric dimers. There is a π-π contact between the pyridine rings [centroid-centroid distance = 3.896 (5) Å].