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41.
Jone Omar Asier Vallejo Maitane Olivares Aresatz Usobiaga Olatz Zuloaga Nestor Etxebarria 《Journal of Chemometrics》2015,29(4):237-244
The interest in the analysis of alkylphenols (APs) has widely increased in the last decades because of the endocrine disrupting features of these phenol derivatives. However, the isolation and identification of many of the multiple chemical structures of all APs is a very challenging task because of their similar physicochemical properties. In this work, the co‐elution of the isomers present in technical mixtures and using comprehensive two‐dimensional gas chromatography coupled to quadrupole mass spectrometry was resolved using multivariate curve resolution‐alternating least squares algorithm. The mass spectrum of each resolved compound was compared with the theoretical mass spectrum obtained from the literature, in order to assign the appropriate identification of each isomer. Two commercial mixtures were studied; in one of them, 34 compounds were resolved, and in the second mixture, 40 compounds were resolved. The relative abundances of the compounds were also calculated in both mixtures. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
42.
Karl R. Whittle Gregory R. Lumpkin Robert D. Aughterson Nestor J. Zaluzec 《Journal of solid state chemistry》2010,183(10):2416-2420
Thin crystals of La2O3, LaAlO3, La2/3TiO3, La2TiO5, and La2Ti2O7 have been irradiated in situ using 1 MeV Kr2+ ions at the Intermediate Voltage Electron Microscope-Tandem User Facility (IVEM-Tandem), Argonne National Laboratory (ANL). We observed that La2O3 remained crystalline to a fluence greater than 3.1×1016 ions cm−2 at a temperature of 50 K. The four binary oxide compounds in the two systems were observed through the crystalline-amorphous transition as a function of ion fluence and temperature. Results from the ion irradiations give critical temperatures for amorphisation (Tc) of 647 K for LaAlO3, 840 K for La2Ti2O7, 865 K for La2/3TiO3, and 1027 K for La2TiO5. The Tc values observed in this study, together with previous data for Al2O3 and TiO2, are discussed with reference to the melting points for the La2O3-Al2O3 and La2O3-TiO2 systems and the different local environments within the four crystal structures. Results suggest that there is an observable inverse correlation between Tc and melting temperature (Tm) in the two systems. More complex relationships exist between Tc and crystal structure, with the stoichiometric perovskite LaAlO3 being the most resistant to amorphisation. 相似文献
43.
44.
Patricia Navarro Luis Bartolomé Juan Carlos Raposo Olatz Zuloaga Gorka Arana Nestor Etxebarria 《Analytica chimica acta》2010,675(1):91-96
Due to high cost of certified reference materials (CRMs), reference materials (RMs) are preferred to check the method performance in environmental analysis. In this work, a laboratory reference material (LRM) was prepared and characterised to carry out the quality control in monitoring analysis of eight polycyclic aromatic hydrocarbons (PAHs) and nine trace metals in mussel tissue. Mussels were collected in a naturally polluted area. Before the reference material was bottled, the mussel tissue was stabilised by freeze-drying, ground and sieved. For the material characterisation, several statistical tests were applied to check the homogeneity of the analytes in the tissue, and a stability test was performed to study the effect of the storage temperature in the analyte concentration. Other characteristics such as specific density, moisture and lipid contents as well as particle size distribution of the material were determined. Although the LRM had a homogeneous distribution for all PAHs and almost all metals, the stability study showed different results at both storage temperatures studied. For both PAHs and trace metals, the material was suitable to assure the quality control of the analysis. 相似文献
45.
Julius P. Neumeyer James I. Wadsworth Nestor B. Knoepfler Charles H. Mack 《Thermochimica Acta》1976,16(2):133-148
Polyester/cotton fabric swith blend ratios of 0/100, 11/89, 20/80, 30/70, 50/50, and 65/35 were investigated via thermogravimetric analysis in both nitrogen and air atmospheres. The samples were heated from ambient to 750°C at a heating rate of 5°C min?1. The same fabrics were analyzed after treatment with tetrakis (hydroxymethyl) phosphonium chloride-urea-poly(vinyl bromide) (Thpc-urea-PVBr) flame retardant.Weight losses observed during pyrolysis were assigned to the cotton and polyester portions of the blends. Both cotton and polyester thermally decompose to yield gases and solid char byproducts. In nitrogen the 100% cotton fabric undergoes one major weight loss between 270 and 370°C, with the maximum rate of weight loss, 0.15 mg/min-mg occurring at 346°C. Thermal decomposition of the 100% polyester occurs over a range of 335–470°C, with the peak rate of weight loss, 0.11 mg/min-mg, measured at 416°C. In an air atmosphere, both volatile gases and solid char by- products of pyrolysis undergo combustion. The combustion reactions are associated with measured weight losses. The maximum rate of weight loss for the cotton portion increases to 0.25 mg/min-mg and occurs at 317°C. The maximum rate of polyester decomposition remains the same in both air and nitrogen, but the temperature decreases to 405°C. 相似文献
46.
Efstathios Laskos Pygmalion S. Lianis Nestor A. Rodios 《Journal of heterocyclic chemistry》1994,31(2):425-430
The title compounds 2 are prepared from the reaction of 1-(N, N-diaroyl)amino-5-bromomethyl-1,2,3-triazoles with aromatic amines. The fragmentation pattern upon electron impact at 70 eV of compounds 2 is studied. The molecular ion peak is present in all the spectra examined. Besides the [M-28]++, there is also a more abundant [M-29]+ peak, corresponding to a N2H loss of the molecular ion. The ion Ar2NH = CH2 is the base or the most prominent peak. 相似文献
47.
Baranda AB Etxebarria N Jiménez RM Alonso RM 《Journal of chromatographic science》2005,43(10):505-512
A high-performance liquid chromatographic method with diode array detection has been developed and optimized for the separation of five calcium channel blockers belonging to the 1,4-dihydropyridine subgroup (nifedipine and related drugs). The possibility of the simultaneous drug analysis allows a decrease of time during the assay as well as a saving of reagents and solvents. In this work, the effect of four experimental parameters (organic modifier percentage, pH value, concentration of the buffer in the mobile phase, and column temperature) on the chromatographic resolution are investigated by experimental design in order to optimize the chromatographic separation of five 1,4-dihydropyridines (amlodipine, nitrendipine, felodipine, lacidipine, and lercanidipine). Fractional factorial design, central composite design, and finally the Multisimplex program are used to establish the optimal conditions in terms of resolution and minimum analysis time. Optimal separation of the five compounds under study is achieved in less than 12 min using a Sulpecosil LC-ABZ+Plus C18 column, a composition of mobile phase of acetonitrile-10mM acetic acid acetate buffer pH 5 (72:28, v/v) at a flow rate of 1 mL/min, a column temperature of 30 degrees C +/- 0.1 degrees C, and a detection wavelength of 238 nm. 相似文献
48.
1-(N-Phenacylidene)amino-1,2,3-triazoles 3 react with propionylchloride and phenoxyacetylchloride in the presence of triethylamine to give trans- ( 5 ) and cis- ( 6 ) 1-(1,2,3-triazol-1-yl)-4-aroylaztidin-2-ones in a 1:1 ratio, on the contrary to the 1-(N-arylidene)amino-1,2,3-triazoles, which do not give any reaction product with the same acid chlorides. The spectroscopic characteristics of these new N-triazolyl-β-lactams are also discussed. 相似文献
49.
Joaquim J. Moura Ramos Joo F. Mano David Lacey G. Nestor 《Journal of Polymer Science.Polymer Physics》1996,34(12):2067-2075
The molecular relaxation mechanisms in the glass transition region and in the liquid crystalline phase exhibited by two side-chain liquid crystalline polysiloxanes have been studied by Thermally Stimulated Discharge Currents. These results were compared with those previously obtained by dielectric relaxation spectroscopy. It was observed that two relaxation mechanisms were present in the liquid crystalline phase, and we suggest that these might correspond to the motions of the mesogenic moieties in the liquid crystalline phase. © 1996 John Wiley & Sons, Inc. 相似文献
50.
Carlos García Gorka Arana Nestor Etxebarria Luis A. Fernández 《Mikrochimica acta》2001,136(1-2):15-21
The analysis of mixtures of four phenolic compounds in an on-line system using UV-visible measurements with a fibre optic
probe is discussed in this work. The aim of this system is to provide accurate real time concentration profiles in order to
monitor the transport of phenols across a solid supported liquid membrane in both the feed and stripping phases. Different
calibration models are taking into account the pH of the solution, using experimental designs and the first derivative in
combination with different multivariate approaches like multiple linear regression (MLR), inverted least squares (ILS) and
partial least squares regression (PLS). The comparison of all these combinations is carried out by means of the predictive
residual error sum of squares (PRESS) evaluated from an independent set of spectra. From this comparison it is concluded that
a PLS model using first derivative spectra offers the most accurate and robust prediction in the permeation experiments. Additionally,
the stability of the model and the figures of merit obtained are also discussed.
Received July 22, 1999. Revision October 23, 2000. 相似文献