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101.
Elisana Afonso Moura Lidiane Pinto Correia Márcia Ferraz Pinto José Valdilânio Virgulino Procópio Fábio Santos de Souza Rui Oliveira Macedo 《Journal of Thermal Analysis and Calorimetry》2010,100(1):289-293
This article had studied the thermal characterization of the raw material and different fluconazole crystals, obtained through
recrystallization with different solvents using thermoanalytical techniques (TG, DTA, DSC-50, DSC Photovisual, DSC-60) and
Pyr-GC/MS. The results confirmed that the fluconazole volatilizes without decomposition until 250 °C. Pyr-GC/MS showed hexachlorobenzene
like impurities in fluconazole raw material. 相似文献
102.
Simas ER Gehlen MH Pinto MF Siqueira J Misoguti L 《The journal of physical chemistry. A》2010,114(47):12384-12390
Polyfluorene end-capped with N-(2-benzothiazole)-1,8-naphthalimide (PF-BNI) is a highly fluorescent material with fluorescence emission modulated by solvent polarity. Its low energy excited state is assigned as a mixed configuration state between the singlet S(1) of the fluorene backbone (F) with the charge transfer (CT) of the end group BNI. The triexponential fluorescence decays of PF-BNI were associated with fast energy migration to form an intrachain charge-transfer (ICCT) state, polyfluorene backbone decay, and ICCT deactivation. Time-resolved fluorescence anisotropy exhibited biexponential relaxation with a fast component of 12-16 ps in addition to a slow one in the range 0.8-1.4 ns depending on the solvent, showing that depolarization occurs from two different processes: energy migration to form the ICCT state and slow rotational diffusion motion of end segments at a longer time. Results from femtosecond transient absorption measurements agreed with anisotropy decay and showed a decay component of about 16 ps at 605 nm in PF-BNI ascribed to the conversion of S(1) to the ICCT excited state. From the ratio of asymptotic and initial amplitudes of the transient absorption measurement, the efficiency of intrachain ICCT formation is estimated in 0.5, which means that, on average, half of the excited state formed in a BNI-(F)(n)-BNI chain with n = 32 is converted to its low energy intrachain charge-transfer (ICCT) state. 相似文献
103.
Amit Katiyar Stephen W. Thiel Vadim V. GuliantsNeville G. Pinto 《Journal of chromatography. A》2010,1217(10):1583-1588
The adsorption of bovine serum albumin (BSA) and lysozyme (LYS) on siliceous SBA-15 with 24 nm pores was studied using flow microcalorimetry; this is the first attempt to understand the thermodynamics of protein adsorption on SBA-15 using flow microcalorimetry. The adsorption mechanism is a strong function of protein structure. Exothermic events were observed when protein–surface interactions were attractive. Entropy-driven endothermic events were also observed in some cases, resulting from lateral protein–protein interactions and conformational changes in the adsorbed protein. The magnitudes of the enthalpies of adsorption for primary protein–surface interactions decrease with increased surface coverage, indicating the possibility of increased repulsion between adsorbed protein molecules. Secondary exothermic events were observed for BSA adsorption, presumably due to secondary adsorption made possible by conformational changes in the soft BSA protein. These secondary adsorption events were not observed for lysozyme, which is structurally robust. The results of this study emphasize the influence of solution conditions and protein structure on conformational changes of the adsorbed protein and the value of calorimetry in understanding protein–surface interactions. 相似文献
104.
Fátima C.M. Portugal Moisés L. Pinto João Pires J.M.F. Nogueira 《Journal of chromatography. A》2010,1217(23):3707-3710
Polyurethane (PU) foams were applied for stir bar sorptive extraction of five triazinic metabolites (desethyl-2-hydroxyatrazine, desisopropylatrazine, desethylatrazine, 2-hydroxyatrazine and desethylterbuthylazine) in water matrices, followed by liquid desorption and high performance liquid chromatography with diode array detection (SBSE(PU)-LD/HPLC-DAD). The optimum conditions for SBSE(PU)-LD were 5 h of extraction (1000 rpm) and 5% (v/v) of methanol for the analysis of desethyl-2-hydroxyatrazine and 2-hydroxyatrazine, 15% (w/v) of sodium chloride for the remaining compounds and acetonitrile as back-extraction solvent (5 mL) under ultrasonic treatment (60 min). The methodology provided recoveries up to 26.3%, remarkable precision (RSD < 2.4%), excellent linear dynamic ranges between 5.0 and 122.1 μg/L (r2 > 0.9993) and convenient detection limits (0.4-1.3 μg/L). The proposed method was applied in the analysis of triazinic metabolites in tap, river and ground waters, with remarkable performance and negligible matrix effects. The comparison of the recoveries obtained by PU and commercial stir bars was also performed, where the yields achieved with the former were up to ten times higher proving that PU is appropriate for analysis at trace level of this type of polar compounds in water matrices. 相似文献
105.
The wavelet transform has been shown to be a useful tool for multivariate calibration. However, the choice of wavelet transform settings (wavelet family, length and number of decomposition levels) for a given application is still an open problem. The present paper proposes an alternative approach, which consists of generating an ensemble model by combining individual models obtained with different wavelet transform settings. The advantages of the proposed method are demonstrated in two analytical problems, namely the determination of moisture and protein in wheat by near infrared spectroscopy and the determination of specific mass and three distillation temperatures (T10, T50, T90) in gasoline by middle infrared spectroscopy. In these problems, the results varied considerably among individual models, which underlines the risk associated to an inadequate choice of wavelet transform settings. In contrast, the ensemble model always provided adequate results in terms of prediction error and noise sensitivity. The proposed method can be seen as an advantageous alternative for multivariate calibration in the wavelet domain, as it frees the analyst from the need to choose a particular configuration for the wavelet transform. 相似文献
106.
The generation of two idler waves inside a high birefringent (HiBi) optical fiber through three four-wave mixing (FWM) processes is studied theoretically. The coupled-equations for the field amplitudes are derived and analytically solved, in the co-polarized and orthogonal polarization schemes. The obtained solutions take into account the delayed Raman response of the medium. The polarization sensitivity of the generation of the idler waves is analyzed. Results show that the stimulated Raman scattering does not change the efficiency of the idler wave generation in the co-polarized scheme, whereas in the orthogonal polarization scheme that nonlinear process decreases the efficiency of the four-wave mixing processes. Results also show that this set of multiple four-wave mixing processes is physically quite different from the typical single or dual pump four-wave mixing configurations. Findings show that the power transfer from the pumps to the idler fields can lead to a monotonous growth, or a periodic evolution of the sidebands along the fiber. Results show that the process efficiency varies greatly with the angle between the two pump polarizations. 相似文献
107.
108.
In this paper, two-dimensional convolutional codes constituted by sequences in $(\mathbb F ^n)^{\mathbb{Z }^{2}}$ where $\mathbb F $ is a finite field, are considered. In particular, we restrict to codes with rate $\frac{1}{n}$ and we investigate the problem of minimal dimension for realizations of such codes by separable Roesser models. The encoders which allow to obtain such minimal realizations, called R-minimal encoders, are characterized. 相似文献
109.
110.