Flow injection spectrophotometric determination of adrenaline using a solid-phase reactor containing triiodide ions immobilized in an anion-exchange resin

A flow injection spectrophotometric procedure with on-line solid-phase reactor containing ion triiodide immobilized in an anion-exchange resin is proposed for the determination of adrenaline (epinephrine) in pharmaceutical products. Adrenaline is oxidized by triiodide ion immobilized in an anionic-exchange resin yielding adrenochrome which is transported by the carrier solution and detected at a wavelength of 488 nm. Adrenaline was determined in three pharmaceutical products in the 6.4 x 10-6 to 3.0 x 10-4 mol L-1 concentration range with a detection limit of 4.8 x 10-7 mol L-1. The recovery of this analyte in three samples ranged from 96.0 to 105 %. The analytical frequency was 80 determinations per hour and the RSDs were less than 1 % for adrenaline concentrations of 6.4 x 10-5 and 2.0 x 10-4 mol L-1 (n=10). A paired t-test showed that all results obtained for adrenaline in commercial formulations using the proposed flow injection procedure and a spectrophotometric batch procedure agree at the 95% confidence level.

Synthesis, characterization and thermal studies of solid state 4-methylbenzylidenepyruvate of some trivalent metal ions

Solid state compounds of 4-methylbenzylidenepyruvate with Al(III), Ga(III), In(III) and Sc(III) have been synthesized. Complexometry, X-ray powder diffractometry, infrared spectroscopy and simultaneous thermogravimetry-differential thermal analysis (TG-DTA) have been used to characterize and to study the thermal behavior of these compounds. The results provided information concerning the stoichiometry, crystallinity, thermal stability and thermal decomposition of these compounds.

Synthesis, characterization and thermal studies on solid 3-methoxybenzoate of some bivalent transition metal ions

Solid-state M-3-MeO-Bz compounds, where M stands for bivalent Mn, Co, Ni, Cu and Zn and 3-MeO-Bz is 3-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, and chemical analysis were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds.

Synthesis, characterization and thermal behaviour of solid-state compounds of 2-methoxybenzoate with some bivalent transition metal ions

Solid-state M-2-MeO-Bz compounds, where M stands for bivalent Mn, Co, Ni, Cu and Zn and 2-MeO-Bz is 2-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry-differential thermal analysis (TG-DTA), thermogravimetry, derivative thermogravimetry (TG/DTG), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to have information about the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds.

Ascorbic acid determination using a carbon paste electrode modified with iron(III) ions adsorbed on humic acid

An amperometric sensor was constructed, by using humic acids to immobilize Fe3+ ions on a carbon paste electrode (CPE-HA-Fe), and used for ascorbic acid (H2A) determination. The cyclic voltammogram of the electrode showed electrochemical response due to the Fe3+/Fe2+ couple at E1/2=+0.78 V vs SCE, using 0.5 mol L-1 KCl and 0.2 mol L-1 acetate/0.020 mol L-1 phosphate buffer, at pH = 5.4, as supporting electrolyte. When H2A is added to the electrolyte solution it is observed an oxidation process. The oxidation current, obtained by chronoamperommetry at +0.87 V vs SCE, is proportional to the concentration, represented by the equation I(µA) = 7.6286 [H2A] (mmol L-1) + 1.9583, r = 0.9996, for concentrations between 0.0 and 1.4 mmol L-1. The electrode showed high stability and was used for H2A determination in a natural orange juice.

Adsorption isotherm studies of Cd (II), Pb (II) and Zn (II) ions bioremediation from aqueous solution using unmodified and EDTA-modified maize cob

The need to clean-up heavy metal contaminated environment can not be over emphasized. This paper describes the adsorption isotherm studies of Cd (II), Pb (II) and Zn (II) ions from aqueous solution using unmodified and EDTA-modified maize cob. Maize cob was found to be an excellent adsorbent for the removal of these metal ions. The amount of metal ions adsorbed increased as the initial concentration increased. Also, EDTA - modification enhanced the adsorption capacity of maize cob probably due to the chelating ability of EDTA. Among the three adsorption isotherm tested, Dubinin-Radushkevich gave the best fit with R² value ranging from 0.9539 to 0.9973 and an average value of 0.9819. This is followed by Freundlich isotherm (Ave. 0.9783) and then the Langmuir isotherm (Ave. 0.7637). The sorption process was found to be a physiosorption process as seen from the apparent energy of adsorption which ranged from 2.05KJ\mol to 4.56KJ\mol. Therefore, this study demonstrates that maize cob which is an environmental pollutant could be used to adsorb heavy metals and achieve cleanliness thereby abating environmental nuisance caused by the maize cob.

Biheterocyclic ligands: synthesis, characterization and coordinating properties of bis(4-amino-5-mercapto-1,2,4-triazol-3-yl) alkanes with transition metal ions and their thermokinetic and biological studies

The Co(II), Ni(II) and Cu(II) metal ions complexes of Bis(4-amino-5-mercapto-1,2,4-triazol-3-yl) alkanes (BATs) have been prepared and characterized by elemental analysis, conductivity measurements infrared, magnetic susceptibility, the electronic spectral data and thermal studies. Based on spectral and magnetic results, the ligands are tetradentate coordinating through the N and S-atoms of BATs; six-coordinated octahedral or distorted octahedral and some times four-coordinated square planar were proposed for these complexes. Activation energies computed for the thermal decomposition steps were compared. The ligands and their metal complexes were tested in vitro for their biological effects. Their activities against two gram-positive, two gram-negative bacteria and two fungal species were found to vary from moderate to very strong.

Synthesis, characterization and thermal behaviour on solid pyruvates of some bivalent metal ions

Solid state M-L compounds, were M stands for bivalent Mn, Fe, Co, Ni, Cu, Zn and L is pyruvate, have been synthesized. Thermogravimetry and derivative thermogravimetry (TG/DTG), differential scanning calorimetry (DSC), X-Ray powder diffractometry, infrared spectroscopy, elemental analysis, and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, ligand denticity, and thermal decomposition of the isolated compounds.

Comparison of the dehydration kinetics of solid state compounds of 2-methoxybenzylidenepyruvate with some divalent metal ions

Divalent metal complexes of ligand 2-methoxybenzylidenepyruvate with Fe, Co, Ni, Cu and Zn as well as sodium salt were synthesized and investigated in the solid state. TG curves of these compounds were obtained with masses sample of 1 and 5mg under nitrogen atmosphere. Different heating rates were used to characterize and study these compounds from the kinetic point of view. The activation energy and pre-exponential factor were obtained applying the Wall-Flynn-Ozawa method to the TG curves. The obtained data were evaluated and the values of activation energy (Ea / kJ mol-1) was plotted in function of the conversion degree (α). The results show that due to mass sample, different activation energies were obtained. The results are discussed mainly taking into account the linear dependence between the activation energy and the pre exponential factor, where was verified the effect of kinetic compensation (KCE) and possible linear relations between the dehydrations steps of these compounds.

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

Solid State M-2-MeO-CP compounds, where M stands for bivalent metals (Mn, Fe, Co, Ni, Cu and Zn) and 2-MeO-CP is 2-methoxycinnamylidenepyruvate, were synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), elemental analysis and complexometry were used to establish the stoichiometry and to study the thermal behaviour of these compounds in CO2 and N2 atmospheres. The results were consistent with the general formula: M(L)2∙H2O. In both atmospheres (CO2, N2) the thermal decomposition occurs in consecutive steps which are characteristic of each compound. For CO2 atmosphere the final residues were: Mn3O4, Fe3O4, Co3O4, NiO, Cu2O and ZnO, while under N2 atmosphere the thermal decomposition is still observed at 1000 º C.

Thermal behaviour of succinic acid, sodium succinate and its compounds with some bivalent transitions metal ions in dynamic N2 and CO2 atmospheres

Thermal stability and thermal decomposition of succinic acid, sodium succinate and its compounds with Mn(II), Fe(II), Co(II), Ni(II), Cu(II) and Zn(II) were investigated employing simultaneous thermogravimetry and differential thermal analysis (TG-DTA) in nitrogen and carbon dioxide atmospheres and TG-FTIR in nitrogen atmosphere. On heating, in both atmospheres the succinic acid melt and evaporate, while for the sodium succinate the thermal decomposition occurs with the formation of sodium carbonate. For the transition metal succinates the final residue up to 1180 ºC in N2 atmosphere was a mixture of metal and metal oxide in no simple stoichiometric relation, except for Zn compound, where the residue was a small quantity of carbonaceous residue. For the CO2 atmosphere the final residue up to 980 ºC was: MnO, Fe3O4, CoO, ZnO and mixtures of Ni, NiO and Cu, Cu2O.

Temperature effect in potassium and nitrate ions in soil transport

When doing researches on solute dynamics in porous medium, the knowledge of medium characteristics and percolating liquids, as well as of external factors is very important. An important external factor is temperature and, in this sense, our purpose was determining potassium and nitrate transport parameters for different values of temperature, in miscible displacement experiments. Evaluated parameters were retardation factor (R), diffusion/dispersion coefficient (D) and dispersivity, at ambient temperature (25 up to 28 ºC), 40 ºC and 50 ºC. Salts used were potassium nitrate and potassium chlorate, prepared in a solution made up of 5 ppm nitrate and 2.000 ppm potassium, with Red-Yellow Latosol porous medium. Temperature exhibited a positive influence upon porous medium solution and upon dispersion coefficient.

Sorption of metal ions to wood, pulp and bark materials

Ett huvudmål med denna avhandling var att erhålla ny information om växelverkan mellan metalljoner i vattenfas och träbaserade material såsom olika pappersmassor, ved och bark. Material av gran, tall och björk har studerats. En ny känslig kolonnkromatografisk metod utvecklades för bestämning av affinitetsordningar för 17 olika metalljoner. Av dessa bands trevärt järn och de mycket toxiska tungmetallerna bly, koppar och kadmium starkast till de studerade materialen. Växelverkan i dessa tvåfas system sker som jonbyte, huvudsakligen via komplexbildning av metalljoner till funktionella grupper i den fasta fasen. Vattenfasens pH är den viktigaste parametern som bestämmer totala halten av metalljoner som binds till materialen. Resultatet i denna avhandling kan delvis betraktas som grundforskning. En ny kunskap om metalljoners förekomst och kemiska reaktioner i dessa system är även av stor ekonomisk och ekologisk, betydelse, när man strävar till allt mera slutna system i moderna massafabriker. Avhandlingen visar också att trädbark har stor potential för biosorption av tungmetaller t.ex. från avfallsvatten. Trädbark har nästan lika stor bindningskapacitet som dyra syntetiska jonbytare.

Control of the phosphorylation of the astrocyte marker glial fibrillary acidic protein (GFAP) in the immature rat hippocampus by glutamate and calcium ions: possible key factor in astrocytic plasticity

The present review describes recent research on the regulation by glutamate and Ca2+ of the phosphorylation state of the intermediate filament protein of the astrocytic cytoskeleton, glial fibrillary acidic protein (GFAP), in immature hippocampal slices. The results of this research are discussed against a background of modern knowledge of the functional importance of astrocytes in the brain and of the structure and dynamic properties of intermediate filament proteins. Astrocytes are now recognized as partners with neurons in many aspects of brain function with important roles in neural plasticity. Site-specific phosphorylation of intermediate filament proteins, including GFAP, has been shown to regulate the dynamic equilibrium between the polymerized and depolymerized state of the filaments and to play a fundamental role in mitosis. Glutamate was found to increase the phosphorylation state of GFAP in hippocampal slices from rats in the post-natal age range of 12-16 days in a reaction that was dependent on external Ca2+. The lack of external Ca2+ in the absence of glutamate also increased GFAP phosphorylation to the same extent. These effects of glutamate and Ca2+ were absent in adult hippocampal slices, where the phosphorylation of GFAP was completely Ca2+-dependent. Studies using specific agonists of glutamate receptors showed that the glutamate response was mediated by a G protein-linked group II metabotropic glutamate receptor (mGluR). Since group II mGluRs do not act by liberating Ca2+ from internal stores, it is proposed that activation of the receptor by glutamate inhibits Ca2+ entry into the astrocytes and consequently down-regulates a Ca2+-dependent dephosphorylation cascade regulating the phosphorylation state of GFAP. The functional significance of these results may be related to the narrow developmental window when the glutamate response is present. In the rat brain this window corresponds to the period of massive synaptogenesis during which astrocytes are known to proliferate. Possibly, glutamate liberated from developing synapses during this period may signal an increase in the phosphorylation

Modulation of staphylokinase-dependent plasminogen activation by mono- and divalent ions

The effect of several ions (Cl-, Na+, K+, Ca2+) on the rate of plasminogen (Pg) activation by recombinant staphylokinase (rSTA) is reported. Both monovalent and divalent ions affect the rate at which Pg is activated by rSTA, in a concentration-dependent manner (range 0-100 mM). In almost all cases, a decrease of the initial velocity of activation was observed. Cl- showed the most striking inhibitory effect at low concentrations (64% at 10 mM). However, in the presence of a fibrin surface, this inhibition was attenuated to 38%. Surprisingly, 10 mM Ca2+ enhanced the Pg activation rate 21% when a polymerized fibrin matrix was present. These data support the idea that ions can modulate the rate of Pg activation through a mechanism that may be associated with changes in the molecular conformation of the zymogen. This effect is strongly dependent on the presence of a fibrin clot.