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131.
132.
Lívia Riberti Rodrigues Diogo Noin de Oliveira Mônica Siqueira Ferreira Rodrigo Ramos Catharino 《Analytica chimica acta》2014
The analysis of impurities and degradation products in pharmaceutical preparations are usually performed by chromatographic techniques such as high-performance liquid chromatography (HPLC). This approach demands extensive analysis time, mostly due to extraction and separation phases. These steps must be carried out in samples in order to adapt them to the requirements of the analytical method of choice. In the present contribution, matrix-assisted laser desorption/ionization mass spectrometry imaging (MALDI-MSI) was employed to quantify an important degradation product in atorvastatin calcium 80 mg tablets: the atorvastatin lactone. Through the standard of the impurity, it was possible to perform quantitative analysis directly on the drug tablet, using a quick and novel approach, suitable for quality control processes in the pharmaceutical industry. 相似文献
133.
Synthesis and Structure Elucidation of New Regioisomeric 2‐Alkylamino‐6‐aryl‐8,9‐dihydropyrimido[4,5‐b][1,4]diazepin‐4(7H)‐ones
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Braulio Insuasty Fabián Orozco Jairo Quiroga Rodrigo Abonía Manuel Nogueras Justo Cobo 《Journal of heterocyclic chemistry》2014,51(1):196-202
Novel 2‐Alkylamino‐6‐aryl‐8,9‐dihydropyrimido[4,5‐b][1,4]diazepin‐4(7H)‐ones 5a , 5b , 5c , 5d , 5e , 5f , 5g , 5h , 5i , 5j , 5k , 5l , 5m , 5n , 5o were prepared regioselectively by the reaction of 2‐alkylamino‐5,6‐diaminopyrimidin‐4(3H)‐ones 3a , 3b , 3c and dimethylamino propiophenones (Mannich bases) 4a , 4b , 4c , 4d , 4e , 4f . The combination of conventional heating and microwave irradiation approaches provided the possibility of working with both stable and sensitive diaminopyrimidines by controlling parameters such as reaction rates, temperature, and power of irradiation. All products were fully characterized by detailed NMR measurements. 相似文献
134.
Galiote NA Camargo MN Iost RM Crespilho F Huguenin F 《Langmuir : the ACS journal of surfaces and colloids》2011,27(19):12209-12217
Self-assembled materials consisting of V(2)O(5), polyallylamine (PAH) and silver nanoparticles (AgNPs) were obtained by the layer-by-layer (LbL) method, aiming at their application as electrodes for lithium-ion batteries and electrochromic devices. The method employed herein allowed for linear growth of visually homogeneous films composed of V(2)O(5), V(2)O(5)/PAH, and V(2)O(5)/PAH/AgNP with 15 bilayers. According to the Fourier transform infrared spectra, interaction between the oxygen atom of the vanadyl group and the amino group should be responsible for the growth of these films. This interaction also enabled establishment of an electrostatic shield between the lithium ions and the sites with higher negative charge, thereby raising the ionic mobility and consequently increasing the energy storage capacity and reducing the response time. According to the site-saturation model and the electrochemical and spectroelectrochemical results, the presence of PAH in the self-assembled host matrix decreased the number of V(2)O(5) electroactive sites. Thus, AgNPs were stabilized in PAH and inserted into the nanoarchitecture, so as to enhance the specific capacity. This should provide new conducting pathways and connect isolated V(2)O(5) particles in the host matrix. Therefore, new nanoarchitectures for specific interactions were formed spontaneously and chosen as examples in this work, aiming to demonstrate the potentiality of the adopted self-assembled method for enhancing the charge transport rate into the host matrices. The obtained materials displayed suitable properties for use as electrodes in lithium batteries and electrochromic devices. 相似文献
135.
de Oliveira RJ Brown P Correia GB Rogers SE Heenan R Grillo I Galembeck A Eastoe J 《Langmuir : the ACS journal of surfaces and colloids》2011,27(15):9277-9284
A new class of photoreactive surfactants (PRSs) is presented here, consisting of amphiphiles that can also act as reagents in photochemical reactions. An example PRS is cobalt 2-ethylhexanoate (Co(EH)(2)), which forms reverse micelles (RMs) in a hydrocarbon solvent, as well as mixed reversed micelles with the standard surfactant Aerosol-OT (AOT). Small-angle neutron scattering (SANS) data show that mixed AOT/PRS RMs have a spherical structure and size similar to that of pure AOT micelles. Excitation of the ligand-to-metal charge transfer (LMCT) band in the PRSs promotes electron transfer from PRS to associated metal counterions, leading to the generation of metal and metal-oxide nanoparticles inside the RMs. This work presents proof of concept for employing PRSs as precursors to obtain nearly monodisperse inorganic nanoparticles: here both Co(3)O(4) and Bi nanoparticles have been synthesized at high metal concentration (10(-2) M) by simply irradiating the RMs. These results point toward a new approach of photoreactive self-assembly, which represents a clean and straightforward route to the generation of nanomaterials. 相似文献
136.
Cormanich RA Moreira MA Freitas MP Ramalho TC Anconi CP Rittner R Contreras RH Tormena CF 《Magnetic resonance in chemistry : MRC》2011,49(12):763-767
The present study shows that a hydrogen bond between the OH group and the fluorine atom is not involved in the (1h)J(FH) spin-spin coupling transmission either for 4-bromo-2-fluorophenol or 2-fluorophenol. In fact, according to a quantum theory of atoms in molecules analysis, no bond critical point is found between O-H and F moieties. The nature of the transmission mechanism of the Fermi contact term of the (1h)J(FH) spin-spin coupling is studied by analyzing canonical molecular orbitals (see J. Phys. Chem. A 2010, 114, 1044), and it is observed that virtual orbitals play only a quite minor role in its transmission. This is typical of a Fermi contact term transmitted mainly through exchange interactions owing to the overlap of proximate electronic clouds; therefore, it is suggested to identify them as (nTS)J(FH) coupling where n stands for the number of formal bonds separating the coupling nuclei. In the cases studied in this work is n = 4. Results presented in this work could provide an interesting rationalization for different experimental signs known in the current literature for proximate J(FH) couplings. 相似文献
137.
Di?go P. Bezerra Ronan S. Oliveira Rodrigo S. Vieira Célio L. Cavalcante Diana C. S. Azevedo 《Adsorption》2011,17(1):235-246
Adsorption may be a potentially attractive alternative to capturing CO2 from stationary sources in the context of Carbon Capture and Sequestration (CCS) technologies. Activated carbon and zeolites
are state-of-art adsorbents which may be used for CO2 adsorption, however physisorption alone tends to be insignificant at high temperatures. In the present work, commercial adsorbents
have been impregnated with monoethanolamine (MEA) and triethanolamine (TEA) in order to investigate the effect of the modified
surface chemistry on CO2 adsorption, especially above room temperature. Adsorption isotherms for CO2, N2 and CH4 were measured in a gravimetrically system in the pressure range of UHV to 10 bar, at 298 and 348 K for activated carbon and
zeolite 13X supports. The adsorbed concentration of CO2 was significantly higher than those of CH4 and N2 for both adsorbents in the whole pressure range studied, zeolite 13X showing a remarkable affinity for CO2 at very low pressures. However, at 348 K, the adsorbed concentration of CO2 decreases significantly. The supports impregnated with concentrated amine solutions and dried in air suffered a detrimental
effect on the textural properties, although CO2 uptake became much less susceptible to temperature increase. Impregnations carried out with dilute solution followed by drying
in inert atmosphere yielded materials with very similar textural characteristics as compared to the parent support. CO2 isotherms in such materials showed a significant change with similar capacities at 348 K as compared to the original support
at 298 K in the case of activated carbons. The impregnated zeolite showed a decrease in adsorbed phase concentration in low
pressures for a given temperature, but the adsorbed amount also seemed to be less affected by temperature. These results are
promising and indicate that CO2 adsorption may be enhanced despite high process temperatures (e.g. 348 K), if convenient impregnation and drying methods
are applied. 相似文献
138.
A sensitive procedure is presented for the voltammetric determination of nickel. The procedure involves an adsorptive accumulation of nickel 1-nitroso-2-napthol (NN) complex on a bismuth film electrode prepared ex situ by electrodeposition. The most suitable operating conditions and parameters such as pH, ligand concentration (CNN), adsorptive potential (Eads), adsorptive time (tads), scan rate and others were selected and the determination of nickel in aqueous solutions using the standard addition method was possible. The adsorbed Ni-NN complex gives a well defined cathodic stripping peak current at −0.70 V, which was used for the determination of nickel in the concentration range of 10.0-70.0 μg L−1 (pH 7.5; CNN 6.5 μmol L−1; Eads −0.30 V; tads 60 s) with a detection limit of 0.1 μg L−1. The relative standard deviation for a solution containing 10.0 μg L−1 of Ni(II) was 3.5% (n = 4). The proposed method was validated determining Ni(II) in certified reference waste water (SPS-WW1) and Certified Reference Water for Trace Elements (TMDA 51.3) with satisfactory results. Then lake water samples were analyzed. 相似文献
139.
Adsorption of CO2, N2, CH4 and H2 on triamine-grafted pore-expanded MCM-41 mesoporous silica (TRI-PE-MCM-41) was investigated at room temperature in a wide
range of pressure (up to 25 bar) using gravimetric measurements. The material was found to exhibit high affinity toward CO2 in comparison to the other species over the whole range of pressure. Column-breakthrough dynamic measurements of CO2-containing mixtures showed very high selectivity toward CO2 over N2, CH4 and H2 at CO2 concentrations within the range of 5 to 50%. These conditions are suitable for effective removal of CO2 at room temperature from syngas, flue gas and biogas using temperature swing (TS) or temperature-pressure swing (TPS) regeneration
mode. Moreover, TRI-PE-MCM-41 was found to be highly stable over hundreds of adsorption-desorption cycles using TPS as regeneration
mode. 相似文献
140.