Flame AAS determination of metal ions in fuel ethanol after preconcentration on acid carboxymethylcellulose (CMCH)

This paper describes the preparation of acid carboxymethylcellulose (CMCH), and the results of a study on the adsorption and preconcentration (using batch and flow-through column methods) of Cd(II), Cu(II), Cr(III), Fe(III), Ni(II) and Zn(II) in ethanol medium. The adsorption capacities for each metallic ion were (in mmol g(-1)) Cd(II) = 0.92; Cu(II) = 1.45; Cr(III) = 1.70; Fe(III) = 1.60; Ni(II) = 1.30; and Zn(II) = 1.10. By means of the flow-through method, a recovery of ca. 100% of the metallic ions adsorbed in a column packed with 2 g of CMCH was found when 5.0 mL of 1.0 mol L-1 hydrochloric acid were used as eluent. An enrichment factor of 20 (100 mt solution containing 50 mu g L-1 of the metallic ions, concentrated to 5.0 mt) was obtained by this preconcentration procedure. The sorption-desorption procedure applied allowed the development of a preconcentration and Flame AAS quantification method of metallic ions in fuel ethanol at trace levels.

Determination of metal ions in natural waters by flame-AAS after preconcentration on a 5-amino-1,3,4-thiadiazole-2-thiol modified silica gel.

5-amino-1,3,4-thiadiazole-2-thiol groups attached on a silica gel surface have been used for adsorption of Cd(II), Co(II), Cu(II), Fe(III), Ni(II), Pb(II) and Zn(II) from aqueous solutions. The adsorption capacities for each metal ion were (in mmol.g(-1)): Cd(II)= 0.35, Co(II)= 0.10, Cu(II)= 0.15, Fe(III)= 0.20, Hg(Il)= 0.46, Ni(II)= 0.16, Pb(II)= 0.13 and Zn(II)= 0.15. The modified silica gel was applied in the preconcentration and quantification of trace level metal ions present in water samples (river, and bog water).

Initiating structural studies of Lys49-PLA2 homologues complexed with an anionic detergent, a fatty acid and a natural lipid

Lys49-Phospholipase A(2) (Lys49-PLA(2) - EC 3.1.1.4) homologues damage membranes by a Ca2+-independent mechanism which does not involve catalytic activity. Both MjTX-II from Bothrops moojeni and BthTX-I from Bothrops jararacussu are dimeric in solution and in the crystalline states, and a model for the Ca2+-independent membrane damaging mechanism has been suggested in which flexibility at the dimer interface region pert-nits quaternary structural transitions between open and closed membrane bound dimer conformations which results in the perturbation of membrane phospholipids and disruption of the bilayer structure [1]. With the aim of gaining insights into the structural determinants involved in protein/lipid association, we report here the crystallization and preliminary X-ray analysis of the (i) MjTX-II/SDS complex at a resolution of 2.78Angstrom, (ii) MjTX-II/STE complex at a resolution of 1.8 Angstrom and (W) BthTX-I/DMPC complex at 2.72Angstrom. These complexes were crystallized by the hanging drop vapour-diffusion technique in (i) HEPES buffer (pH 7.5) 1.8M ammonium sulfate with 2% (w/v) polyethyleneglycol 400, in (ii) 0.6-0.8 M sodium citrate as the precipitant (pH 6.0-6.5) and in (iii) sodium citrate buffer (pH 5.8) and PEG 4000 and 20% isopropanol, respectively. Single crystals of these complexes have been obtained and X-ray diffraction data have been collected at room temperature using a R-AXIS IV imaging plate system and graphite monochromated Cu Kalpha X-ray radiation generated by a Rigaku RU300 rotating anode generator for (i) and (W) and using using a Synchrotron Radiation Source (Laboratorio Nacional de Luz Sincrotron, LNLS, Campinas, Brazil) for (ii).

Corrosion of dental amalgams: electrochemical study of Ag-Hg, Ag-Sn and Sn-Hg phases

Dental amalgams, formed by reaction of mercury with a powder alloy containing mainly Ag, Sn, Cu and Zn, have a complex metallurgical structure which can contain up to six phases. Their observed corrosion is thus a complex process, which involves contributions from each of the phases present as well as intergranular corrosion. It is thus of interest to investigate the corrosion of individual phases present in dental amalgams. In this work the corrosion behaviour in 0.9% NaCl solution of Ag-Hg, Ag-Sn and Sn-Hg phase components of dental amalgams was investigated by electrochemical methods. The corrosion resistance was found to decrease in the order gamma (1)-Ag2\Hg3, gamma -Ag3Sn and gamma (2)-Sn7Hg. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

Determinação do íon ferro em preparações farmacêuticas através da cromatografia planar e espectrofotometria

Os autores estudaram o comportamento cromatográfico de preparações farmacêuticas comerciais contendo o íon Fe (II). Utilizando celulose microcristalina/Propanol: ácido clorídrico 4 N: ácido acético concentrado: ácido nítrico concentrado: clorofórmio (40: 5: 5: 10: 10), como sistema cromatográfico e alizarina como reagente de detecção, Fe (II), Mn (II), Mg (II), Cu (II), Zn (II) e Ca (II) foram separados e identificados pela Cromatografia Planar. O Fe (II) foi determinado pela reação com a ortofenantrolina, resultando em solução adequada para quantificação colorimétrica.

Synthesis, characterization and thermal behaviour of solid 2-methoxycinnamylidenepyruvate of some bivalent metal ions in CO2 and N2 atmospheres

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Sorption and preconcentration of metal ions on silica gel modified with 2,5-dimercapto-1,3,4-thiadiazole

Silica gel, chemically modified with 2,5-dimercapto-1,3,4-thiadiazole [=Si(CH2)(3)-NC2HNS3], abbreviated as SiB, was used to adsorb metal ions from ethanol by both batch and column techniques. Elution of Cu(II) was done with a solvent mixture of acetone and hydrochloric acid (9:1 v/v). Zn(II), Cd(II), Ni(II), Pb(II), Co(II) and Fe(III) were eluted with 0.5 mol l(-1) HC1 in ethanol solution. The modified silica was applied in the preconcentration of metal ions from commercial ethanol, normally used as engine fuel. The method is suitable for quantifying these metals at low mu g l(-1) levels.

Synthesis, characterization and electrochemical study of layered double hydroxides intercalated with 2-thiophenecarboxylate anions

The synthesis, characterization, and electrochemical study of the Zn(II)-Al(III) and Zn(II)-Cr(III) Layered Double Hydroxides (LDHs) containing 2-thiopenecarboxylate as the interlayer anions are described. The LDHs were prepared by the constant pH coprecipitation technique followed by hydrothermal treatment for 72 h. The materials were analyzed by PXRD, FT-IR, C-13 CP-MAS, EDX, TEM, and CV. The presence of the organic heterocyclic anions was confirmed by FT-IR and the related solid-state C-13 NMR data strongly suggested that these were dimerised during coprecipitation. Accordingly, the basal spacing found by the X-ray technique was similar to 15.3 Angstrom, a distance coincident with the formation of bilayers of the intercalated anions. The structural organization of all the new materials was greatly enhanced by hydrothermal treatment, as shown by PXRD. The improved organization of the bilayered structures had a strong influence in the electrochemical behaviour of clay-modified electrodes produced with these materials, such as the diminished resistance to the ionic flow through the LDHs films. (C) 2003 Elsevier Ltd. All rights reserved.

Thermal behaviour of malonic acid, sodium malonate and its compounds with some bivalent transition metal ions

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Thermal and spectroscopic data to investigate the oxamic acid, sodium oxamate and its compounds with some bivalent transition metal ions

Synthesis, characterization, and thermal behavior of transition metal oxamates, M(NH(2)C(2)O(3))(2)center dot nH(2)O (M = Mn(II), Fe(II), Co(II), Ni(II), Cu(II), Zn(II)), as well as the thermal behavior of oxamic acid and its sodium salt (NaNH(2)C(2)O(3)) were investigated employing simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC), experimental and theoretical infrared spectroscopy, TG-DSC coupled to FTIR, elemental analysis and complexometry. The results led to information about the composition, dehydration, thermal stability, thermal decomposition, as well as of the gaseous products evolved during the thermal decomposition of these compounds in dynamic air and N(2) atmospheres.

Thermal behaviour of succinic acid, sodium succinate and its compounds with some bivalent transition metal ions

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Thermal behaviour of mandelic acid, sodium mandelate and its compounds with some bivalent transition metal ions

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

2-Mercaptobenzothiazole clay as matrix for sorption and preconcentration of some heavy metals from aqueous solution

2-Mercaptobenzothiazole loaded on previously polystyrene treated clay was prepared, characterized and used for sorption and preconcentration of Hg(II) Pb(II), Zn(II) and Cd(II) from an aqueous solution. The support used was a natural clay previously treated with sulphuric acid solution. Adsorptiou isotherms of metal ions from aqueous solutions as function of pH were studied at 298 K. Conditions for quantitative retention and elution were established for each metal by batch and column methods. The chemically treated clay was very selective to Hg(II) in solution in which Zn(II), Cd(II), Pb(II) and some transition metal ions were also present.

Sorption and preconcentration of some heavy metals by 2-mercaptobenzothiazole-clay

2-Mercaptobenzothiazole loaded on previously treated clay was prepared, characterized and used for sorption and preconcentration of Hg(II), Pb(II), Zn(II), Cd(II), Cu(II) and Mn(II) from an aqueous solution. The support used was a natural clay previously treated with sulphuric acid solution. Adsorption isotherms of metal ions from aqueous solutions as function of pH were studied at 298 K. Conditions for quantitative retention and elution were established for each metal by batch and column methods. The chemically treated clay was very selective to Hg(II) in solution in which Zn(II), Cd(II), Pb(II), Cu(II) and Mn(II) were also present. © 1995.

Thermal decomposition of the magnesium, zinc, lead and niobium chelates derived from 8-quinolinol

Solid M-Ox compounds, where M represents Mg(II), Zn(II), Pb(II) and NbO(III), and Ox is 8-quinolinol, have been prepared. Thermogravimetry, derivative thermogravimetry (TG, DTG), differential scanning calorimetry (DSC), nuclear magnetic resonance (NMR) and infrared absorption spectra (IR) have been used to characterize and to study the thermal stability and thermal decomposition of these compounds. © 1997 Akadémiai Kiadó.