Ionic medium effects on equilibrium constants .2. Binary systems comprising some bivalent cations and monocarboxylates in aqueous solution

Simple equations were derived relating stoichiometric protonation constants of several monocarboxylates and formation constants associated with 1:1 complexes involving some bivalent cations and selected monocarboxylates, in aqueous sodium perchlorate media, at 25 degrees C, as a function of ionic strength (I), allowing the interconversion of parameters from one ionic strength to another, up to I = 3.00 M. In addition, thermodynamic formation constants as well as activity coefficients of the species involved in the equilibria were estimated. The results show that the proposed calculation procedure is very consistent with critically selected experimental data

Spectrophotometric determination of formaldehyde with chromotropic acid in phosphoric acid medium assisted by microwave oven

In the present study. a spectrophotometric method for the determination of formaldehyde by using chromotropic acid was devised. in which the use of potentially hazardous and corrosive concentrated sulfuric acid was eliminated and advantageously C replaced by a mixture of H, concentrated H3PO4 and H2O2. The reaction between formaldehyde and chromotropic acid (CA) in a cone phosphoric acid medium was accelerate by irradiating the mixture with microwave energy for 35 s (1100 W), producing a violetred compound (lambda(max)=570 nm). Beer's Law is obeyed in a concentration range of 0.8-4.8 mg 1(-1) of formaldehyde with a good correlation coefficient (r = 0.9968). The proposed method was applied in the analysis of formaldehyde in commercial disinfectants. Recoveries were within 98.0-100.4%, with standard deviations ranging from 0.03 to 0.13%. (C) 2003 Elsevier B.V All rights reserved

Otimização de ELISA empregando a proteína Tc85-11 e planejamento fatorial

A doença de Chagas é causada pelo Trypanosoma cruzi (T. cruzi) e a detecção de anticorpos anti-T. cruzi no soro é um método para diagnosticar a doença. Neste trabalho, ELISA indireto foi otimizado para a detecção de anticorpos no soro de pacientes com doença de Chagas empregando a proteína Tc85-11 (Ag) da superfície do parasita tripomastigota. Na otimização das condições experimentais foi aplicado planejamento fatorial completo para os parâmetros tempo de incubação, diluições do Ag (0,08 mg mL-1), anticorpo primário (Ac) e anti-IgG conjugada com a peroxidase (Ac*). Os melhores resultados foram obtidos nas seguintes condições: 0,14 mg Ag/poço, 60 min para o tempo de incubação, diluições de 1:35 e 1:1000 para Ac e Ac*, respectivamente. O valor do limiar de reatividade (cut off) foi A450nm = 0,371. O ELISA indireto foi aplicado em amostras de soros de pacientes infectados com doença de Chagas e pacientes com diferentes doenças sistêmicas. A proteína Tc85-11, a qual está envolvida com a adesão do parasita na célula hospedeira, é também apropriada para o diagnóstico sorológico da doença de Chagas.Chagas' disease is caused by the Trypanosoma cruzi (T. cruzi) and the detection of anti-T. cruzi antibodies in the serum is a method for diagnosis of the disease. In this work, indirect ELISA was optimized for detection of antibodies in patients' sera with Chagas' disease using Tc85-11 protein (Ag) from the trypomastigote surface of the parasite. The full factorial design for optimization of the experimental conditions was carried out for the incubation time, dilutions of Ag (0.08 mg mL-1), primary antibody (Ac) and anti-IgG conjugated with peroxidase (Ac*) parameters. The best results were obtained with the following conditions: 0.14 mg Ag/well, 60 min incubation time, dilutions of 1:35 and 1:1000 for Ac and Ac*, respectively. The cut off value was A450nm = 0.371. The indirect ELISA was applied to sera Chagas' disease infected patients samples and patients with different systemic diseases. Tc85-11 protein, which is involved in the adhesion of the parasite to host cell, is also suitable for serological diagnosis of Chagas' disease.Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP

Estrógenos em água: otimização da extração em fase sólida utilizando ferramentas quimiométricas

Muitos métodos analíticos estão sendo desenvolvidos visando à determinação de contaminantes orgânicos, especialmente alteradores endócrinos. Tais métodos baseiam-se geralmente na extração em fase sólida (SPE) seguida por determinação cromatográfica (CG ou HPLC). No presente trabalho utilizou-se ferramentas quimiométricas no processo de SPE para avaliar os principais fatores que influenciam tal processo e as interações entre os mesmos. Foram analisadas matrizes de água subterrânea fortificada com hormônios (17 b estradiol, estrona e 17 b etinilestradiol) e a determinação analítica foi feita por HPLC/Fluorescência. Um planejamento fatorial completo foi utilizado. Os fatores escolhidos incluíram: condicionamento da fase sólida, concentração dos analitos, volume da amostra e solvente de eluição. As melhores condições obtidas foram: 500 mL da amostra, condicionamento da fase sólida (C18) com acetona (4mL), metanol (6 mL) e água pH 3(10 mL), e eluição dos analitos com 4 mL de acetona.Several analytical methods have been proposed for organic pollutants determination in water, specially endocrine disrupters. These methods are frequently based in solid phase extraction (SPE) followed by chromatographic determination (GC or HPLC). In this work it was used chemometric tools on experimental design and experimental data treatment to evaluate the principal factors in SPE process and their interactions. It was used water matrices fortified with hormones (17 b estradiol, estrone and 17 b ethinylestradiol) and HPLC/Fluorescence did analytical determination. It was used a factorial complete design. The choosed factors included: solid phase type, analytes concentration, sample volumen, eluent composition, analytes concentration and solvents to solid phase conditioning. The best condition obtained in this initial procedure included: 500 mL sample, conditioning SPE cartridge with acetone (4mL), methanol (6 mL) and water pH 3(10 mL), and analytes elution with acetone

A new approach for determining stability constants of metal ion complexes in aquatic systems based on flow injection-ion exchange-flame atomic absorption spectrometry coupling

A method based an ion exchange(IE)-atomic absorption spectrometry(AAS) coupled by flow techniques, allowing the determination of formation constants of, at least, the first species of complex systems, in aqueous solution, was developed.The IE-AAS coupling reduces significantly the number of experimental steps in comparison with IE batch methods, resulting in an important increase in analytical rate. The method is simple both from experimental and computational points of view, making possible its utilization by workers without special expertise in the field of complex equilibria in solution. on the other hand, taking into account mainly the amount of hollow cathode lamps available to date, the developed procedure may be applied, within certain limitations, to the study of many systems whose features prevent the use of traditional approaches

Environmental coordination chemistry: Binary systems comprising some bivalent cations and monocarboxylates in aqueous solution. Ionic medium effects on equilibrium constants

The molar single activity coefficients associated with propionate ion (Pr) have been determined at 25 degrees C and ionic strengths comprised between 0.300 and 3.00 M, adjusted with NaClO4, as background electrolyte. The investigation was carried out potentiometrically by using a second class Hg/Hg2Pr2 electrode. It was found that the dependence of propionate activity coefficients as a function of ionic strength (I) can be assessed through the following empirical equation: log y(Pr) = -0.185 I-3/2 + 0.104 I-2. Next, simple equations relating stoichiometric protonation constants of several monocarboxylates and formation constants associated with 1:1 complexes involving some bivalent cations and selected monocarboxylates, in aqueous solution, at 25 degrees C, as a function of ionic strength were derived, allowing the interconversion of parameters from one ionic strength to another, up to I = 3.00 M. In addition, thermodynamic formation constants as well as parameters associated with activity coefficients of the complex species in the equilibria are estimated. The body of results shows that the proposed calculation procedure is very consistent with critically selected experimental data