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.
A new liquid—liquid extraction system for molybdenum(VI) was studied. It contains 4-nitrocatechol (4NC) as a complexing chromogenic reagent and benzalkonium chloride (BZC) as a source of heavy cations (BZ+), which are prone to form chloroform-extractable ion-association complexes. The optimum conditions for the determination of trace molybdenum(VI) were found: concentrations of 4NC and BZC (7.5 × 10−4 mol dm−3 and 1.9 × 10−4 mol dm−3, respectively), acidity (3.75 × 10−2 mol dm−3 H2SO4), extraction time (3 min), and wavelength (439 nm). The molar absorptivity, limit of detection, and linear working range were 5.5 × 104 dm3 mol−1 cm−1, 5.6 ng cm−3, and 18.6–3100 μg cm−3, respectively. The effect of foreign ions was examined, and the developed procedure was applied to the analysis of synthetic mixtures and real samples (potable waters and steels). The composition of the extracted complex was 1:1:2 (Mo:4NC:BZ). Three possible structures of its anionic part [MoVI(4NC)O2(OH)2]2− were discussed based on optimizations at the B3LYP/3-21G level of theory, and simulated UV/Vis absorption spectra were obtained with the TD Hamiltonian.
Complex formation between Ga(III) and 6-hexyl-4-(2-thiazolylazo)resorcinol (HTAR, H2L) was studied in a water-chloroform medium, in the presence or absence of xylometazoline hydrochloride (XMH). Optimum conditions for the extraction of Ga(III) were found. In the presence of XMH, the extracted ion-associate has the formula (XMH +)[Ga III L2], where HTAR is in its deprotonated form L 2-. Some key extractionspectrophotometric characteristics were determined: absorption maximum (521 nm), apparent molar absorptivity (5.8 × 10 4 dm 3 mol-1 cm-1), limit of detection (18 ng cm-3), limit of quantitation (60 ng cm-3), extraction constant (LogK = 4.44), distribution ratio (LogD = 2.2) and fraction extracted (99.3 %). In the absence of XMH, the extracted chelate contains one deprotonated and one monoprotonated HTAR: [Ga III (HL-)(L 2-)]. It has an absorption maximum at 523 nm and a shoulder at 580-590 nm. The pKa of HTAR (H2L ⇄ H + + HLequilibrium) was calculated (5.4) and the effect of foreign ions was studied.
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