An inexpensive and fast vanadium [(IV), (V)] speciation method was performed by using optical chemical sensor that incorporates lipophilized calmagite (Cal) with cetyl pyridinium chloride (CPC) as a suitable ligand on triacetylcellulose membrane in aqueous solutions prior to UV-Vis spectrometric determination. Absorbance decrease of the optode in pH 6 at 490 nm depended on the V(V) ion concentration. The V(IV) content was found after oxidation to V(V) at the mentioned conditions. Two aliquots of sample were used for speciative determination of V(V) and V(V) + V(IV) mixture. With the optimized proposed sensor V(V) and V(IV) can be assayed with detection limits of 0.002 and 0.003 nmol L−1, respectively. The optode was tested by analysing several mixtures containing different ratios of V(V) + V(IV) and was found to be highly reproducible. The validity of the method was checked via spiked water samples with total relative standard error less than 4%.

Este trabalho apresenta um novo sensor químico óptico, simples e de baixo custo, para a determinação de íon mercúrio (II) em solução aquosa. A membrana sensível a mercúrio foi preparada pela incorporação de triazina ((E)-1-(2-etoxifenil)-3-(4-nitrofenil) triazol-1-ene como um ligante adequado para Hg(II) sobre uma membrana de triacetilcelulose. O estudo espectrofotométrico do complexo formado entre o ligante triazene (L) e íons Hg2+ em solução de dimetilformamida (DMF) mostrou uma grande constante de estabilidade para o íon mercúrio complexado. A membrana responde ao íon mercúrio pela troca reversível da cor de laranja para verde em solução tamponada em pH 3,0. Uma relação linear foi observada entre a absorbância da membrana em 405 nm, na faixa de 7 a 90 µg mL-1, com um limite de detecção de 64 ng mL-1 em soluções aquosas, em pH 3,0. O sensor óptico for aplicado com sucesso na determinação de mercúrio em amostras de água enriquecidas com o analito.

A new simple and inexpensive optical chemical sensor for mercury(II) ion in aqueous solutions is presented. The mercury sensing membrane was prepared by incorporating of triazene ((E)-1-(2-ethoxyphenyl)-3-(4-nitrophenyl) triaze-1-ene) (L) as a suitable ligand for Hg(II) on triacetylcellulose membrane. Spectrophotometric study of complex formation between the triazene ligand L and Hg2+ in dimethyl formamide solution indicated a large stability constant for the mercury ion complex. The membrane responds to mercury ion by changing color reversibly from orange to green in buffer solution at pH 3.0. A linear relationship was observed between the membrane absorbance at 405 nm in a range from 7 to 90 µg mL-1 with a limit of detection of 64 ng mL-1 in aqueous solutions at pH 3.0. The optical sensor was successfully applied to the determination of mercury in spiked water samples.

A simple and fast approach for solid phase extraction is herein described, and used to determine trace amounts of Pb2+ and Cu2+ metal ions. The solid phase support is sodium dodecyl sulfate (SDS)-coated γ-alumina modified with bis(2-hydroxy acetophenone)-1,6-hexanediimine (BHAH) ligand. The adsorbed ions were stripped from the solid phase by 6 mL of 4 M nitric acid as eluent. The eluting solution was analyzed by flame atomic absorption spectrometry (FAAS). The sorption recovery of metal ions was investigated with regard to the effects of pH, amount of ligand, γ-alumina and surfactant and the amount and type of eluent. Complexation of BHAH with Pb2+ or Cu2+ ions was examined via spectrophotometry using the HypSpec program. The detection limit for Cu2+ was 7.9 µg L-1 with a relative standard deviation of 1.67%, while that for Pb2+ was 6.4 µg L-1 with a relative standard deviation of 1.64%. A preconcentration factor of 100 was achieved for these ions. The method was successfully applied to determine analyte concentrations in samples of liver, parsley, cabbage, and water.

A very simple cloud point extraction (CPE) methodology for the preconcentration of trace amounts of silver and magnesium as a prior step for their determination by flame atomic absorption spectrometry (FAAS) has been developed. The method is based on the extraction of silver and magnesium at pH 10 by using non-ionic surfactant Triton X-114 and 4 methyl-3-((1-H-Indol-3-iyl) (phenyl) methyl)) -1-H-Indol (MPBIM) as a complexing agent. Several important variables that affect the CPE efficiency and FAAS signal were investigated and optimized. The calibration curves, using the preconcentration system, were linear in the range of 0.007-0.200 μg mL-1 with a correlation coefficient of 0.999. The lower limits of detection (3s) obtained in the optimal conditions were 1.47 ng mL-1 and 3.00 ng mL-1 for Mg²+ and Ag+ ions, respectively. The relative standard deviation for five replicate determinations of magnesium and silver at 0.133 μg mL-1 concentration level, were 1.17 and 0.97, respectively. The proposed method was successfully applied to the ultra-trace determination of silver and magnesium in various water samples, blood serum, urine, and radiology film samples.