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11.
The present work describes a selective, rapid and economical method for the determination of cobalt using the 2-(2-benzothiazolylazo)-p-cresol (BTAC) as a spectrophotometric reagent associated with a solid extraction on polyurethane foam. The BTAC reacts with Co(II) in the presence of Triton-X100 surfactant forming a green complex with maximum absorption at 615 nm. The reaction is used for cobalt determination within a pH range of 6.50-7.50, with an apparent molar absorptivity of 1.62 x 10(4) L mol(-1) cm(-1). Beer's Law is obeyed for a concentration of at least 1.60 microg ml(-1). A selective procedure is proposed for cobalt determination in the presence of Fe(II), Hg(II), Zn(II) and Cu(II) up to milligram levels using masking agents. Polyurethane foam is used for the preconcentration and separation of cobalt from thiocyanate media and this procedure is applied to its determination in nickel salts and steel alloys. 相似文献
12.
Lisardo Núñez F. Fraga A. Castro L. Fraga 《Journal of Thermal Analysis and Calorimetry》1998,52(3):1013-1022
The influence of the resin/diamine ratio on the properties of the system diglycidyl ether of bisphenol A (BADGE n=0/m-xylylenediamine)
(m-XDA) was studied. Variation of this ratio resulted in significant effects on the cure kinetics and final dynamic mechanical
properties of the product material.
The study was made in terms of storage modulus (E′), vss modulus (E″) and molecular mass between cross-links (Mc) at different ratios. Two geometries (cylindrical and rectangular) were considered. The influence of temperature was studied
through the activation energy (Ea>), which depends on the epoxy/amine ratio and the geometry of the samples. Glass transition temperatures (Tg>) and glass transition temperatures for thermosets with null degree of conversion (Tgo>) were determined by DSC. Tg> decreases when amounts of curing agent greatly in excess of the stoichiometric composition were used.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
13.
14.
Multivariate calibration methods that use fluorescence data for the simultaneous determination of furosemide and triamterene were developed. One of the most salient advantages of them is that the vast amount of information provided by the whole spectrum of the sample is not required. This makes analyses simple and fast. The methods require selecting chemometric parameters such as the specific spectral region and number of factors to be used. Both spectral region and number of factors are selected, simultaneously, by minimising the prediction residual error sum of squares (PRESS).The proposed methods were used for the simultaneous determination of the two drugs in real samples (pharmaceutical preparations) with no excipient separation pre-treatment, with furosemide and triamterene contents of 1.68E−3 to 4.31E−2 and 1.03E−3 to 3.12E−2 μg ml−1, respectively; as well as that of triamterene at concentrations of 5.00E−4 to 5.80E−3 μg ml−1 in urine samples. The ability to construct the calibration validation sets directly from the urine samples itself avoids the need to consider matrix interferences or to pre-treat the sample and/or separate some analytes The results were quite good in all cases. 相似文献
15.
As shown in this paper, multivariate calibration in general and principal component regression (PCR) in particular allow the determination of Captopril by differential pulse polarography (DPP) in the presence of oxygen despite the overlap between their polarographic bands. Electrochemical parameters (pulse amplitude, pulse delay and drop time) are optimized from response surfaces using PCR to determine the relationship between the variables to be optimized and the relative square error of prediction (RSEP), which was adopted as the parameter to be minimized. The proposed method is quite fast and inexpensive as a result of the decreased analysis times and sparing use of the inert gas. It was applied to the determination of Captopril in synthetic samples and a commercially available pharmaceutical preparation, with relative errors and confidence intervals <2.5% and 2.0%, respectively. It should be noted that the sample can be analysed directly following dissolution in water without the need to remove the excipients. 相似文献
16.
Serafin Fraga 《International journal of quantum chemistry》1988,34(6):505-507
The quantity ? = (Φ||(H ? E)Φ|) gives a measure of the error in the approximate solution, Φ (with corresponding energy expectation value E), to an eigenfunction of the Hamiltonian operator H of the system under consideration; this quantity vanishes for the exact function ψ. In a percentage scale (with 0% error for the exact function and 100% for a reference, approximate function), the error of Φ may be expressed as 100(?/?r), where ?r corresponds to the reference function (e.g., obtained with a minimal basis set). This approach eliminates the need of knowing beforehand the exact solution in order to have an estimate of the error of an approximate solution. 相似文献
17.
Núñez Lisardo Fraga L. Núñez M. R. Villanueva M. Rial B. 《Journal of Thermal Analysis and Calorimetry》2002,70(1):9-17
Curing reactions of the epoxy system consisting of a diglycidyl ether of bisphenol A (BADGE n=0) and m-xylylenediamine (m-XDA) were studied to calculate time-temperature-transformation (TTT) isothermal cure diagram for this system. Gel times were
measured as a function of temperature using solubility test. Differential scanning calorimetry (DSC) was used to calculate
the vitrification times. DSC data show a one-to-one relationship between T
g and fractional conversion, a independent of cure temperature. As a consequence, T
g can be used as a measure of conversion. The activation energy for the polymerization overall reaction was calculated from
the gel times obtained using the solubility test (41.5 kJ mol-1). This value is similar to the results obtained for other similar epoxy systems. Isoconversion contours were calculated by
numerical integration of the best fitting kinetic model.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
18.
19.
Núñez Lisardo Villaneuva M. Rial B Núñez M. R. Fraga L. 《Journal of Thermal Analysis and Calorimetry》2002,70(1):75-84
The thermal degradation of the epoxy system diglycidyl ether of bisphenol A (BADGE n=0)/1,2-diamine cyclohexane (DCH) containing different concentrations of an epoxy reactive diluent was studied by thermogravimetric
analysis in order to determine the reaction mechanism of the degradation process and to compare it with the results for the
same system without diluent. The value of the activation energy, necessary for this study, was calculated using various integral
and differential methods. Values obtained using the different methods were compared to the value obtained by the Flynn-Wall-Ozawa"s
method (between 193-240 kJ mol-1 depending on the diluent concentration) with does not require a knowledge of the nth order reaction mechanism. All the experimental
results were compared to master curves in the range of Doyle"s approximation (20-35% of conversion). Analysis of the results
suggests that the reaction mechanism could be F2, F3, or A2 type.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
20.
Dehydroluciferyl-coenzyme A (L-CoA) was chemically synthesized and characterized by MS, UV-vis spectrometry and RP-HPLC. The identity of the chemically synthesized compound with the one that was produced by firefly luciferase was confirmed. Moreover, the reversibility of the enzymatic conversion of dehydroluciferin ? dehydroluciferyl-adenylate ? L-CoA was also confirmed. The chemical synthesis of L-CoA, described here, may help the clarification of the activator effect of CoA on luciferase bioluminescent assays, in which the enzyme catalyzed formation of L-CoA and the consequent destruction of L-AMP is one of the possible explanations for that effect. 相似文献