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1.
Molecules ; 28(18)2023 Sep 20.
Artigo em Inglês | MEDLINE | ID: mdl-37764499

RESUMO

Two new vanadium (V) complexes involving 6-hexyl-4-(2-thiazolylazo)resorcinol (HTAR) and tetrazolium cation were studied. The following commercially available tetrazolium salts were used as the cation source: tetrazolium red (2,3,5-triphenyltetrazol-2-ium;chloride, TTC) and neotetrazolium chloride (2-[4-[4-(3,5-diphenyltetrazol-2-ium-2-yl)phenyl]phenyl]-3,5-diphenyltetrazol-2-ium;dichloride, NTC). The cations (abbreviated as TT+ and NTC+) impart high hydrophobicity to the ternary complexes, allowing vanadium to be easily extracted and preconcentrated in one step. The complexes have different stoichiometry. The V(V)-HTAR-TTC complex dimerizes in the organic phase (chloroform) and can be represented by the formula [(TT+)[VO2(HTAR)]]2. The other complex is monomeric (NTC+)[VO2(HTAR)]. The cation has a +1 charge because one of the two chloride ions remains undissociated: NTC+ = (NT2+Cl-)+. The ground-state equilibrium geometries of the constituent cations and final complexes were optimized at the B3LYP and HF levels of theory. The dimer [(TT+)[VO2(HTAR)]]2 is more suitable for practical applications due to its better extraction characteristics and wider pH interval of formation and extraction. It was used for cheap and reliable extraction-spectrophotometric determination of V(V) traces in real samples. The absorption maximum, molar absorptivity coefficient, limit of detection, and linear working range were 549 nm, 5.2 × 104 L mol-1 cm-1, 4.6 ng mL-1, and 0.015-2.0 µg mL-1, respectively.

2.
Molecules ; 27(15)2022 Jul 24.
Artigo em Inglês | MEDLINE | ID: mdl-35897901

RESUMO

The hydrophobic azo dye 6-hexyl-4-(2-thiazolylazo)resorcinol (HTAR, H2L) was studied as part of a system for the centrifuge-less cloud point extraction (CL-CPE) and spectrophotometric determination of traces of cobalt. The extracted 1:2 (Co:HTAR) complex, [CoIII(HL-)(L2-)]0, shows an absorption maximum at 553 nm and contains HTAR in two different acid-base forms. Optimum conditions for its formation and CL-CPE were found as follows: 1 × 10-5 mol L-1 of HTAR, 1.64% of Triton X-114, pH of 7.8, incubation time of 20 min at ca. 50 °C, and cooling time of 30 min at ca. -20 °C. The linear range, limit of detection, and apparent molar absorptivity coefficient were 5.4-189 ng mL-1, 1.64 ng mL-1, and 2.63 × 105 L mol-1 cm-1, respectively. The developed procedure does not use any organic solvents and can be described as simple, cheap, sensitive, convenient, and environmentally friendly. It was successfully applied to the analysis of artificial mixtures and real samples, such as steel, dental alloy, rainwater, ampoules of vitamin B12, and saline solution for intravenous infusion.


Assuntos
Compostos Azo , Cobalto , Compostos Azo/química , Cobalto/análise , Solventes/química , Espectrofotometria/métodos
3.
Spectrochim Acta A Mol Biomol Spectrosc ; 262: 120106, 2021 Dec 05.
Artigo em Inglês | MEDLINE | ID: mdl-34214740

RESUMO

A simple, cheap, and environmentally friendly centrifuge-less cloud point extraction procedure was developed for the preconcentration of traces of Cu(II) before its spectrophotometric determination. It is based on a complexation reaction with the hydrophobic azo reagent 6-hexyl-4-(2-thiazolylazo)resorcinol (HTAR), in which a complex with a stoichiometric ratio of 1:1 and an absorption maximum at 535 nm is formed. The experimental conditions for Cu(II) determination were found: HTAR concentration (8 × 10-6 mol mL-1), mass fraction of the surfactant Triton X-114 (2.2%), pH (5.9, ammonium acetate buffer), and incubation time (10 min at 60 °C). The linear range, limit of detection, molar absorption coefficient and preconcentration factor were calculated to be 4.5-254 ng mL-1, 1.34 ng mL-1, 2.54 × 105 L mol-1 cm-1, and 10, respectively. The effect of foreign ions was studied, and the proposed procedure was applied to the analysis of water samples and a saline solution for intravenous infusion.


Assuntos
Cobre , Polietilenoglicóis , Compostos Azo , Resorcinóis , Espectrofotometria
4.
Acta Chim Slov ; 61(4): 813-8, 2014.
Artigo em Inglês | MEDLINE | ID: mdl-25551721

RESUMO

The formation of ternary ion-association complexes of Co(II) with 4-(2-pyridylazo)resorcinol (PAR) and tetrazolium salts (TS) - (3-(4,5-dimethylThiazol-2-yl)-2,5-diphenyl-2H-tetrazolium bromide (MTT) and 3-(2-naphtyl)-2,5-diphenyl-2H-tetrazolium chloride (TV) - were investigated with the aid of the extraction-spectrophotometric method. The optimum conditions for the extraction of Co(II) were found. On the basis of the experimental data and their mathematical treatment the association process in aqueous phase and extraction process was investigated quantitatively. The molar ratios of the components in the associates were determined. The results show that the extracted species could be represented with the general formula (TS)[CoH(PAR)(2)]. The following key constants were calculated: association constant, distribution constant, extraction constant and recovery factor. The validity of Beer's law was checked and some analytical characteristics were calculated.

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