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81.
Luisa Célia Melo Djenaine De Souza Pedro de Lima‐Neto Adriana Nunes Correia 《Electroanalysis》2010,22(21):2502-2510
The highly boron‐doped diamond electrode (HBDD) combined with square wave voltammetry (SWV) was used in the development of an analytical procedure for diquat determination in potato and sugar cane samples and lemon, orange, tangerine and pineapple juices. Preliminary experiments realised in a medium of 0.05 mol L?1 Na2B4O7 showed the presence of two voltammetric peaks around ?0.6 V and around ?1.0 V vs. Ag/AgCl/Cl? 3.0 mol L?1, where the first peak could be successfully used for analytical proposes due the facility in the electrode surface renovation. After the experimental and voltammetric optimisation, the calculated detection and quantification limits were 1.6×10?10 mol L?1 and 5.3×10?10 mol L?1 (0.057 µg L?1 and 0.192 µg L?1, respectively), which are lower than the maximum residue limit established for fresh food samples by the Brazilian Sanitary Vigilance Agency. The proposed methodology was used to determine diquat residues in potato and sugar cane samples and lemon, orange, tangerine and pineapple juices and the calculated recovery efficiencies indicated that the proposed procedure presents higher robustness, stability and sensitivity, good reproducibility, and is very adequate for diquat determination in complex samples. 相似文献
82.
Pavlo Solokha Serena De Negri Bernhard Eck Adriana Saccone 《Journal of solid state chemistry》2010,183(12):2995-3001
The crystal structures of two new ternary phases, La4Ag10Mg3 and La4Ag10.3Mg12, were refined from X-ray single crystal diffraction data. La4Ag10Mg3 crystallizes in the Ca4Au10In3 structure type, an ordered variant of the binary Zr7Ni10 compound: orthorhombic, Cmce, oS68, a=14.173(5), b=10.266(3), c=10.354(3) Å, Z=4, wR2=0.0826, 676 F2 values, 50 variables. La4Ag10.3Mg12 represents a new structure type: orthorhombic, Cmmm, oS116-10.32, a=9.6130(3), b=24.9663(8), c=9.6333(2) Å, Z=4, wR2=0.0403, 1185 F2 values, 101 variables. The structural analysis of both compounds, highlighting a significant contraction of the Ag-Mg distances, suggests the existence of three-dimensional [Ag-Mg] networks hosting La atoms. LMTO calculations applied to La4Ag10Mg3 indicate that the strongest bonds occur for Ag-Ag and Ag-Mg interactions, and confirm the presence of a 3D∞[Ag10Mg3]δ− polyanionic framework balanced by positively charged La atoms. 相似文献
83.
Noemí Andrade-López Tracy A. Hanna José G. Alvarado-Rodríguez Adriana Luqueño-Reyes Bernat A. Martínez-Ortega Daniel Mendoza-Espinosa 《Polyhedron》2010
Cis-diaquobis{di-(2-pyridyl)-N-ethylimine}nickel(II) chloride (2) was obtained from the reaction of di-(2-pyridyl)-N-ethylimine (1) and [NiCl2dppe] [dppe = cis-1,2-bis(diphenylphosphino)ethylene] in a 2:1 ratio in hot acetonitrile. Cis-dichloro{di-(2-pyridyl)-N-ethylimine}palladium(II) (3) and cis-dichloro{di-(2-pyridyl)-N-ethylimine}platinum(II) (4) complexes were obtained from the reaction of MCl2 (M = Pd, Pt) and (1) in equimolar ratio in hot acetonitrile. Compounds 1–4 were characterized by IR spectroscopy, elemental analysis, and mass spectrometry; the complexes 3 and 4 were characterized in solution by NMR. In addition, solid state structures of compounds 1–4 were determined using single crystal X-ray diffraction analyses. X-ray diffraction data of the complexes 3 and 4 showed a distorted square planar local geometry at palladium and platinum atoms with the chlorine atoms in a cis-coordination; in 2 a local octahedral geometry at nickel atom was observed. Complexes 3 and 4 are arranged as dimers with a M?M distance of 3.4567(4) Å (M = Pd) and 3.4221(4) Å (M = Pt), respectively; 2 consists of units linked by intermolecular hydrogen bonding. 相似文献
84.
Benedetto Bozzini Andreas Bund Bertrand Busson Christophe Humbert Adriana Ispas Claudio Mele Abderrahmane Tadjeddine 《Electrochemistry communications》2010,12(1):56-60
In this paper we report an SFG/DFG investigation of the adsorption of CN? – used as a probe molecule to study the electrochemical double-layer structure – at a polycrystalline Au electrode in 1-butyl-1-methyl-pyrrolidinium bis(trifluoromethylsulfonyl) amide ([BMP][TFSA]) room-temperature ionic liquid (RTIL). The adsorption of CN? yielded single SFG and DFG bands in the range from ca. 2125 to 2135 cm?1, exhibiting a Stark tuning of ca. 3 cm?1 V?1. Vibrational resonances – corresponding to modes of the RTIL coadsorbed with CN?, were found in the range from ca. 1200 to 1500 cm?1. The study of the double-layer structure was complemented by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) measurements, from which the differential double-layer capacity (CDL) was estimated. 相似文献
85.
86.
A new, simple and highly sensitive method for spectrofluorimetric determination of amiloride (AMI) and furosemide (FUR) in pharmaceuticals is presented. The proposed method is based on the separation of AMI from FUR by solid-phase extraction using a nylon membrane, followed by spectrofluorimetric determination of both drugs, on the solid surface and the filtered aqueous solution, respectively. AMI shows low native fluorescence, but its separation-preconcentration by immobilization (solid-phase extraction) on nylon membrane surface provides a considerable enhancement in fluorescence intensity. The fluorescence determination is carried out at λex = 237, λem = 415 nm for FUR; and λex = 365, λem = 406 nm for AMI. The calibration graphs are linear in the range 3.20 × 10−4 to 0.8 μg mL−1and 1.33 × 10−3 to 4.0 μg mL−1, for AMI and FUR, respectively, with a detection limit of 9.62 × 10−5 and 4.01 × 10−4 μg mL−1 (S/N = 3). The commonly found excipients in commercial pharmaceutical formulations do not interfere. The developed method is successfully applied to the determination of both drugs in pharmaceutical formulations. 相似文献
87.
88.
89.
Ambalangodage C. Jayasuriya Adriana Schirokauer Jerry I. Scheinbeim 《Journal of Polymer Science.Polymer Physics》2001,39(22):2793-2799
The electroactive properties of two random copolymers of vinylidene fluoride (VDF) and hexafluoropropylene (HFP) were studied. The compositions were 95/5 and 85/15 mol % P(VDF/HFP). For each composition, three different film‐preparation methods were used—solvent casting, melt‐pressed quenched, and melt‐pressed slow‐cooled. The ferroelectric properties observed were strongly dependent on the preparation methods of the films as well as the HFP molar content of the samples. The highest remanent polarizations (Pr) obtained from electric displacement versus electric field (D‐E) hysteresis data are 80 and 50 mC/m2 for the 5 and 15% HFP solvent‐cast samples, respectively. The slow‐cooled samples do not exhibit any ferroelectric behavior for either the 5 or 15% HFP copolymers. It was also observed that both the 5 and 15% HFP slow‐cooled samples have a smaller electrostrictive response relative to the other two types of samples. Wide‐angle X‐ray diffraction and DSC results suggest that the 5% HFP sample has a higher crystallinity relative to the 15% HFP sample for each preparation method. In addition, different crystal phases form in the samples resulting from the different preparation methods. Fourier transform infrared results suggest that the slow‐cooled samples are in the nonpolar α phase, whereas the quenched and solvent‐cast samples are more likely in the polar β phase. The slow‐cooled samples do not show a switching peak in their nonpolar α‐phase crystalline state. © 2001 John Wiley & Sons, Inc. J Polym Sci Part B: Polym Phys 39: 2793–2799, 2001 相似文献
90.
Bogdan Tiţa Eleonora Marian Adriana Fuliaş Tunde Jurca Dumitru Tiţa 《Journal of Thermal Analysis and Calorimetry》2013,112(1):367-374
The application of thermal method is of great importance regarding the pharmaceutical problems such as the control of raw materials, the determination of purity, the qualitative and quantitative analysis of drug formulation, tests of thermal stability and compatibility and the determination of kinetic parameters etc. The purpose of a kinetic investigation is to calculate the kinetic parameters and the determination of the kinetic model for the studied process. The results are further used to predict the system’s behaviour in various circumstances. A kinetic study regarding the piroxicam—active substance’s thermal decomposition was performed under isothermal conditions and nitrogen atmosphere, for the temperature steps: 200, 205, 210, 215 and 220 °C. The TG/DTG data were processed by three differential methods: isothermal—isoconversional, Friedman’s isothermal isoconversional and isothermal model-fitting. The obtained results are in good accord between them, as well as with those obtained under non-isothermal conditions from a previous work and confirm the necessity of the kinetic parameters determining in different thermal conditions, by the adequate calculation methods. 相似文献