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991.
High Sensitive Microsensor Based on Organic‐Inorganic Composite for Two‐Dimensional Mapping of H2O2 by SECM
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Danielle Diniz Justino Isabel Lourenço Torres Rita de Cássia Silva Luz Flavio Santos Damos 《Electroanalysis》2015,27(5):1202-1209
The present work describes the development of a selective, sensitive and stable sensing microsensor for scanning electrochemical microscopy (SECM) to measure H2O2 during electrochemical reduction of oxygen. The microsensor is based on graphene and Poly(3,4‐ethylenedioxythiophene) composite as support to iron (III) hexacyanoferrate (II) (PEDOT/graphene/FeIII4[FeII(CN)6]3 microsensor). The electrochemical properties of the PEDOT/graphene/FeIII4[FeII(CN)6]3 microsensor were investigated by cyclic voltammetry (CV) and scanning electrochemical microscopy (SECM). The PEDOT/graphene/FeIII4[FeII(CN)6]3 microsensor showed an excellent electrocatalytic activity toward hydrogen peroxide (H2O2) reduction with a diminution of the overpotential of about 500 mV in comparison to the process at a bare gold microelectrode. The microsensor presented excellent performance for two dimensional mapping of H2O2 by SECM in 0.1 mol L?1 phosphate buffer solution (pH 7.0). Under optimized conditions, a linear response range from 1 up to 1000 µmol L?1 was obtained with a sensitivity of 0.08 nA L µmol?1 and limit of detection of 0.5 µmol L?1. 相似文献
992.
MALDI‐MS of flavonoids: a systematic investigation of ionization and in‐source dissociation mechanisms
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Matrix assisted laser desorption ionization (MALDI) is a technique widely employed in the analysis of proteins and peptides, and nowadays it has also been applied to small molecules. There is little significant information regarding the in‐source dissociation processes on MALDI for natural products. Twenty‐six flavonoids (flavanones, flavones and flavonols) were analyzed by MALDI using different methods (with different matrices) and without matrix to comprehend the in‐source reactions and establish good analysis methods for these compounds. Depending on the class, structure and the laser intensity applied, methoxylated flavonoid aglycones can eliminate methyl radicals (˙CH3) in the source, such as flavonols, but lithium 2,4‐dihydroxybenzoate matrix suppresses the ˙CH3 eliminations and retro‐Diels–Alder cleavages in the source. All of the flavonoid O‐glycosides evaluated herein eliminated the sugar in source, even in the presence of the matrix, and its product radical ions ([M‐H‐sugar]?˙) were observed in the negative mode. The flavone C‐glycosides suffered intense dissociation, which was reduced by the addition of a matrix and the application of low laser intensity, mainly in the negative mode. Depending on the hydroxyl substituents, the [M‐H‐H]?˙ ion was observed with variable relative intensity in the spectra. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
993.
994.
Suellen Christtine da Costa Sanches Flávio de Vasconcelos Carlos Emmerson Ferreira da Costa Patrícia Santana Barbosa Marinho Marcos R. Guilherme Eraldo José Madureira Tavares José Antônio Picanço Diniz Júnior José Otávio Carréra Silva Júnior Roseane Maria Ribeiro-Costa 《Journal of Thermal Analysis and Calorimetry》2015,120(1):991-999
995.
996.
997.
Tavane A. Alvarenga Camila S. Bertanha Pollyanna F. de Oliveira Denise C. Tavares Valéria M.M. Gimenez Márcio L.A. Silva 《Natural product research》2015,29(11):1083-1086
This work evaluated the in vitro inhibitory activity of the crude ethanolic extract from the aerial parts of Cuspidaria pulchra (Cham.) L.G. Lohmann against 15-lipoxygenase (15-LOX). The bioassay-guided fractionation of the n-butanol fraction, which displayed the highest activity, led to the isolation of three compounds: caffeoylcalleryanin (1), verbascoside (2) and 6-hydroxyluteolin-7-O-β-glucoside (3). Assessment of the ability of the isolated compounds to inhibit 15-LOX revealed that compounds 1, 2 and 3 exerted strong 15-LOX inhibitory activity; IC50 values were 1.59, 1.76 and 2.35 μM respectively. The XTT assay showed that none of the isolated compounds seemed to be significantly toxic. 相似文献
998.
Combination of hollow‐fiber‐supported liquid membrane and dispersive liquid–liquid microextraction as a fast and sensitive technique for the extraction of pesticides from grape juice followed by high‐performance liquid chromatography
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![点击此处可从《Journal of separation science》网站下载免费的PDF全文](/ch/ext_images/free.gif)
Vanessa Dutra Silva Vanessa Simão Adriana Neves Dias Jeferson Schneider Carletto Eduardo Carasek 《Journal of separation science》2015,38(11):1959-1968
The simultaneous use of a hollow‐fiber‐supported liquid membrane and dispersive liquid–liquid microextraction for the determination of pesticides directly in grape juice was investigated. The detection and quantification were performed by liquid chromatography with diode array detection. The optimum extraction condition was reached by filling the pores of the membrane wall with dodecanol and using hexane/acetone as extraction/dispersion solvents. Salt addition had a highly negative effect on the extraction efficiency and the optimum extraction time was 60 min. The volume of hexane/acetone mixture and the sample pH did not affect the signal at the levels studied. Therefore, an intermediate amount of these solvents (250 μL; 1:7.5 v/v) and pH 6 were selected. The optimum desorption condition was obtained with acetonitrile and 10 min of desorption time. The linear working range varied from 58 to 500 μg/L (parathion‐methyl), 62–500 μg/L (difenoconazole) and 107–500 μg/L (chlorpyrifos), with correlation coefficients ranging from 0.9980–0.9942. The limits of detection and quantification found were, respectively, 17 and 58 μg/L for parathion‐methyl, 19 and 62 μg/L for difenoconazole and 32 and 107 μg/L for chlorpyrifos. The relative standard deviation ranged between 3.5 and 11.2%. 相似文献
999.
1000.
Vianney O. Santos Isabela R. Leite Alexandre G. Brolo Joel C. Rubim 《Journal of Raman spectroscopy : JRS》2016,47(6):674-680
The electrochemical conversion of CO2 into value‐added products using room temperature ionic liquids as solvent/electrolyte has been proposed as an alternative to minimize the environmental effects of CO2 emissions. A key issue in the design of electrochemical systems for the reduction of CO2 is the in situ identification of intermediate surface species as well as reaction products. Copper electrodes, besides being used as cathodes in the electrochemical reduction of CO2, present surface‐enhanced Raman scattering (SERS) when properly activated. In this sense, the electrochemical reduction of CO2 over a copper electrode in the room temperature ionic liquids 1‐n‐butyl‐3‐methyl imidazolium tetrafluoroborate (BMI.BF4) was investigated by cyclic voltammetry and by in situ SERS. The cyclic voltammetries have shown that the presence of CO2 on the BMI.BF4 anticipates the reduction of BMI+ to the corresponding carbene. Fourier‐transform‐SERS spectra excited at 1064 nm and SERS spectra excited at 632.8 nm have shown vibrational signals from adsorbed CO. These SERS results indicated that CO adsorbs on the copper surface at two different surface sites. The observation of a 2275 cm−1 vibration in the SERS spectra also confirmed the presence of chemically adsorbed CO2. Other products of CO2 reduction in BMI.BF4, besides CO, were identified, including BMI carbene and the BMI‐CO2 adduct. The SERS results also suggest that the presence of a thin film of Cu2O on the copper surface anticipates the reduction of CO2 to CO, an important component of syngas. Copyright © 2016 John Wiley & Sons, Ltd. 相似文献