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.

Hydrogen bond-mediated self-assembly of Tin (II) oxide wrapped with Chitosan/[BzPy]Cl network: An effective bionanocomposite for textile wastewater remediation.

A novel and efficient bionanocomposite was synthesized by incorporating SnO into chitosan (Ch) and a room-temperature ionic liquid (RTIL). The bionanocomposite was synthesized in benzoyl pyridinium chloride [BzPy]Cl to maintain the unique properties of SnO, chitosan, and the ionic liquid. Adsorption and photodegradation processes were applied to evaluate the bionanocomposite for removing azo and anthraquinone dyes and textile wastewater. SnO/[BzPy]Cl and SnO/[BzPy]Cl/Ch samples were prepared and characterized using various techniques, including FT-IR, SEM, XRD, EDAX, XPS, DSC, TGA, nitrogen adsorption/desorption isotherm, and DRS analysis. SEM analysis revealed a hierarchical roughened rose flower-like morphology for the biocomposite. The band gap energies of SnO/[BzPy]Cl and SnO/[BzPy]Cl/chitosan were found to be 3.9 and 3.3 eV, respectively, indicating a reduction in the band gap energy with the introduction of [BzPy]Cl and chitosan. SnO/[BzPy]Cl/Ch showed high removal rates (92-95 %) for Fast Red, Blue 15, Red 120, Blue 94, Yellow 160, and Acid Orange 7 dyes. The adsorption kinetics followed a pseudo-second-order model. In addition, the effect of different photodegradation parameters such as solution pH, dye concentrations, contact time, and amount of photocatalyst, was studied. Given the optimal results obtained in removing azo and anthraquinone dyes, the SnO/[BzPy]Cl/Ch nanocomposite was used as an efficient nanocomposite for removing dyes from textile wastewater. The highest removal efficiency was found to be 95.8 %, obtained under ultraviolet and visible light. Furthermore, BOD and COD reduction analysis showed significant reductions, indicating the excellent performance of the photocatalyst.

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).

Heavy metals determination in water and food samples after preconcentration by a new nanoporous adsorbent.

In this work, SBA-15 mesoporous silica has been chemically functionalized with guanidin groups. The resulting material has been characterised and employed as solid phase extractant for preconcentration of Pb(2+), Cu(2+), Zn(2+) and Cd(2+) ions. The ions were identified by flame atomic absorption spectrometry (FAAS). The enrichment factor of the proposed method was 100 and detection limits were found to be 4.5, 0.6, 0.2 and 0.5 ng mL(-1) for Pb(2+), Cu(2+), Zn(2+) and Cd(2+) respectively. The time and the optimum amount of the sorbent, pH and minimum amount of acid for stripping and break through volume were investigated. The maximum capacity the adsorbent was found to be 89.1 (±1.7) µg, 57.2 (±1.6) µg, 26.8 (±1.6) µg and 36.0 (±0.6) µg of Pb(2+), Cu(2+), Zn(2+) and Cd(2+) per mg functionalized SBA-15, respectively. Guanidin functionalized SBA-15 was successfully applied as a new solid extractant for the simultaneous preconcentration of Pb(2+), Cu(2+), Zn(2+) and Cd(2+) ions in water and food samples.

Aminobenzenesulfonamide functionalized SBA-15 nanoporous molecular sieve: a new and promising adsorbent for preconcentration of lead and copper ions.

A rapid method for the extraction and monitoring of nanogram level of Pb2+ and Cu2+ ions using uniform silanized mesopor (SBA-15) functionalized with aminobenzenesulfonamide groups and flame atomic absorption spectrometry (FAAS) is presented. Aminobenzenesulfonamide functionalized SBA-15 was synthesized according to procedure in the literature and the presence of organic groups in the silica framework was demonstrated by FT-IR spectra. The functionalized product showed the BET surface area 110 m2/g and pore diameter 5.1 nm, based on adsorption-desorption of N2 at 77 K. The effect of several variables such as (amount of adsorbent, stirring time, pH and presence of other ions in the medium) has been studied. Lead and copper were completely extracted at pH greater than 3 after stirring for 10 min. The maximum capacity of the adsorbent was found to be 191.3 +/- 1.4 and 155.0 +/- 1.0 microg of lead and copper ions/mg functionalized SBA-15, respectively. The preconcentration factor of the method was found to be 200. The detection limit of the technique was 3.4 and 0.4 ng/mL for Pb2+ and Cu2+, respectively. The applications of this methodology for real samples were examined by various water type, black tea and pepper samples.