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941.
J. del-Castillo A. C. Yanes J. Méndez-Ramos V. K. Tikhomirov V. V. Moshchalkov V. D. Rodríguez 《Journal of Sol-Gel Science and Technology》2010,53(3):509-514
89.5(SiO2)10(PbF2)0.5(REF3) silicate glasses have been prepared using room temperature sol–gel processing of Si(OCH2CH3)4, Pb(CH3COO)2·3H2O, RE(CH3COO)3·nH2O and trifluoroacetic acid as a fluorinating agent, where RE stands for rare-earth ions, such as Yb3+, Er3+, Ho3+, Tm3+, or combinations of those ions. On heat treatment of these glasses at about 300–400 °C, the rare-earth doped spherical PbF2 nanocrystals precipitate within SiO2 glass matrix providing transparent nano-structured glass–ceramics, while the diameter of the nanocrystals can be set in the range from 5 to 25 nm by varying time and temperature of the heat
treatment. The structural and photoluminescence studies confirm the incorporation of rare-earth ions into the PbF2 nanocrystals and white and tuneable colour up-conversion luminescence has been detected in case of Yb3+-Er3+-Tm3+ and Yb3+-Ho3+-Tm3+ co-doped nanocrystals by varying dopant ratio and pump power. 相似文献
942.
D. García-Rodríguez A. M. Carro R. Cela R. A. Lorenzo 《Analytical and bioanalytical chemistry》2010,398(2):1005-1016
A microwave-assisted extraction method followed by clean-up with solid-phase extraction (SPE) combined with large-volume injection
gas chromatography–tandem mass spectrometry (LVI-GC-MS/MS) for the analysis of 17 pesticides in wild and aquaculture edible
seaweeds has been developed. An experimental central composite design was employed to evaluate the effects of the main variables
potentially affecting the extraction (temperature, time, and solvent volume) and to optimize the process. The most effective
microwave extraction conditions were achieved at 125 °C and 12 min with 24 mL of hexane/ethyl acetate (80:20). SPE clean-up
of the extracts with graphitized carbon and Florisil, optimized by means of the experimental design, proved to be efficient
in the removal of matrix interferences. The analytical recoveries were close to 100% for all the analytes, with relative standard
deviations lower than 13%. The limits of detection ranged from 0.3 to 23.1 pg g−1 and the limits of quantification were between 2.3 and 76.9 pg g−1, far below the maximum residue levels established by the European Union for pesticides in seaweed. The results obtained prove
the suitability of the microwave-assisted extraction for the routine analysis of pesticides in aquaculture and wild seaweed
samples. 相似文献
943.
Sonia Herranz Markéta Bocková María Dolores Marazuela Ji?í Homola María Cruz Moreno-Bondi 《Analytical and bioanalytical chemistry》2010,398(6):2625-2634
A surface plasmon resonance (SPR) biosensor for the detection of microcystins (MCs) in drinking water has been developed.
Several assay formats have been evaluated. The selected format is based on a competitive inhibition assay, in which microcystin-LR
(MCLR) has been covalently immobilized onto the surface of an SPR chip functionalized with a self-assembled monolayer. The
influence of several factors affecting sensor performance, such as the nature and concentration of the antibody, the composition
of the carrier buffer, and the blocking and regeneration solutions, has been evaluated. The optimized SPR biosensor provides
an IC50 0.67 ± 0.09 μg L−1, a detection limit of 73 ± 8 ng L−1, and a dynamic range from 0.2 to 2.0 μg L−1 for MCLR. Cross-reactivity to other related MCs, such as microcystin-RR (88%) and microcystin-YR (94%), has also been measured.
The SPR biosensor can perform four simultaneous determinations in 60 min, and each SPR chip can be reused for at least 40
assay–regeneration cycles without significant binding capacity loss. The biosensor has been successfully applied to the direct
analysis of MCLR in drinking water samples, below the provisional guideline value of 1 μg L−1 established by the World Health Organization for drinking water. 相似文献
944.
José Luis Martínez-Hernández Marco Arnulfo Mata-Gómez Cristóbal Noé Aguilar-González Anna Ilyina 《Applied biochemistry and biotechnology》2010,160(7):2045-2053
The production of extracellular and mycelia-associated penicillin G acylase (maPGA) with Mucor griseocyanus H/55.1.1 by surface-adhesion fermentation using Opuntia imbricata, a cactus, as a natural immobilization support was studied. Enzyme activity to form 6-aminopencillanic acid (6-APA) from
penicillin G was assayed spectrophotometrically. The penicillin G hydrolysis to 6-APA was evaluated at six different times
using PGA samples recovered from the skim milk medium at five different incubation times. Additionally, the effect of varying
the penicillin G substrate concentration level on the PGA enzyme activity was also studied. The maximum reaction rate, V
max, and the Michaelis constant, K
M, were determined using the Michaelis–Menten model. The maximum levels for maPGA and extracellular activity were found to
be 2,126.50 international unit per liter (IU/l; equal to 997.83 IU/g of support) at 48 h and 755.33 IU/l at 60 h, respectively.
Kinetics of biomass production for total biomass showed a maximum growth at 60 h of 3.36 and 2.55 g/l (equal to 0.012 g of
biomass per gram of support) for the immobilized M. griseocyanus biomass. The maPGA was employed for the hydrolysis of penicillin G to obtain 6-APA in a batch reactor. The highest quantity
of 6-APA obtained was 226.16 mg/l after 40-min reaction. The effect of substrate concentration on maPGA activity was evaluated
at different concentrations of penicillin G (0–10 mM). K
M and V
max were determined to be 3.0 × 10−3 M and 4.4 × 10−3 mM/min, respectively. 相似文献
945.
Jaime G. Mayoral Francisco J. Alarcón Tomás F. Martínez Pablo Barranco F. Noriega 《Applied biochemistry and biotechnology》2010,160(1):1-8
A novel end-point fluorimetric procedure based on the use of rhodamine-110-labeled specific substrate was developed to determine
trypsin activities in biological samples. We evaluated the ability of trichloroacetic acid and acetic acid to stop the enzymatic
reaction without hindering the detection of the fluorescence of rhodamine-110 released into the reaction mixture from the
specific substrate (CBZ-l-alanyl-l-arginine)2-rhodamine-110. Trichloroacetic acid decreased markedly the fluorescence of rhodamine-110, even at low concentrations. On
the other hand, the addition of 50 mmol/l acetic acid inactivated efficiently trypsin activity, causing minor effects on rhodamine-110
fluorescence. The proposed procedure was more sensitive than the spectrophotometric end-point method using N-α-benzoyl-dl-arginine-p-nitroanilide as substrate. The possibility of carrying out end-point fluorimetric assays improves the performance of monocell
fluorimeters by setting specific conditions optimal for each enzyme activity independently of the fluorimeter. This method
also allows replicate assays to be conducted simultaneously, resulting in considerable time saving and in increased performance
of low-cost equipment. 相似文献
946.
Rocío García-Villalba Alegría Carrasco-Pancorbo Ekaterina Nevedomskaya Oleg A. Mayboroda André M. Deelder Antonio Segura-Carretero Alberto Fernández-Gutiérrez 《Analytical and bioanalytical chemistry》2010,398(1):463-475
Olive oil polyphenols have important biological properties which closely depend on their bioavailability; it is, therefore,
essential to understand how polyphenols are absorbed, metabolized, and eliminated from the body. An analytical method based
on rapid-resolution liquid chromatography (RRLC) coupled with mass spectrometric detection with a time-of-flight analyzer
(RRLC–ESI-TOF MS) has been developed for analysis of the main olive oil phenolic compounds and their metabolites in human
urine. Urine samples from ten healthy volunteers were collected before and 2, 4, and 6 h after intake of 50 mL extra-virgin
olive oil. The proposed method includes liquid–liquid extraction with ethyl acetate, which provides extraction recoveries
of the phenolic compounds studied between 35 and 75% from spiked urine samples. Good repeatability was obtained—the relative
standard deviations (RSDs) of peak areas in intra-day and inter-day studies were 4.3 and 6.5%, respectively. Statistical studies
enabled us to discriminate between urine samples before and after intake, and facilitated the search for m/z values enabling this discrimination. Based on the very accurate mass information and the isotopic pattern provided by the
TOF MS analyzer, together with other available information, ten of these biomarkers and more than 50 metabolites, obtained
through phase I and phase II biotransformation reactions, were tentatively identified. Additionally, kinetic studies were
conducted on the metabolites identified as possible biomarkers; for most of the compounds concentrations were maximum in the
first two hours. 相似文献
947.
The Becke3LYP density functional was used to study structural and thermodynamic parameters of bivalent zinc cation complexes
with selected substrates and ACE inhibitors (H2O/OH−, neutral forms of captopril, zofenoprilat, omapatrilat, CH3CONHCH3, and N-terminal anions of captopril, zofenoprilat, omapatrilat, enalaprilat, perindoprilat, trandolaprilat, and fosinoprilat). The
combination of DFT and the conductor-like polarizable continuum model (CPCM) were employed to compute the Gibbs interaction
energies (ΔG) between Zn2+ and the selected ACE inhibitors for dielectric media with ɛ = 5 (to simulate the protein environment) and for water media (ɛ = 78.39) for comparison purposes. The results show that ΔG is sensitive to the dielectric constant of the environment and that lower dielectric medium favors the binding of inhibitors
to the zinc cation. 相似文献
948.
Boris Remenec Silvia Dulanská Ľubomír Mátel Ján Bilohuščin 《Journal of Radioanalytical and Nuclear Chemistry》2014,302(1):117-122
The behaviour of 95Zr and 95Nb isotopes on TEVA® resin column was studied. The influence of hydrofluoric, hydrochloric, oxalic and sulphuric acids on the separation and chemical yield of zirconium and niobium was tested. The method is suitable for the separation of 93Zr and 94Nb isotopes from hydrofluoric, hydrochloric and sulphuric acid by using different concentrations of the acid for the load or elutes solutions. Samples from reactor and fuel assemblies such as the control-rod connection rod, shielding/absorber parts of fuel rods, neutron in-core measurement channels, pressure vessel basic construction material and internal cladding, core barrel and reactor protection tube unit were analysed. 相似文献
949.
950.
Juan Sanz García Martial Boggio-Pasqua Ilaria Ciofini Marco Campetella 《Journal of computational chemistry》2019,40(14):1420-1428
The ability to locate minima on electronic excited states (ESs) potential energy surfaces both in the case of bright and dark states is crucial for a full understanding of photochemical reactions. This task has become a standard practice for small- to medium-sized organic chromophores thanks to the constant developments in the field of computational photochemistry. However, this remains a very challenging effort when it comes to the optimization of ESs of transition metal complexes (TMCs), not only due to the presence of several electronic ESs close in energy, but also due to the complex nature of the ESs involved. In this article, we present a simple yet powerful method to follow an ES of interest during a structural optimization in the case of TMCs, based on the use of a compact hole-particle representation of the electronic transition, namely the natural transition orbitals (NTOs). State tracking using NTOs is unambiguously accomplished by computing the mono-electronic wave function overlap between consecutive steps of the optimization. Here, we demonstrate that this simple but robust procedure works not only in the case of the cytosine but also in the case of the ES optimization of a ruthenium nitrosyl complex which is very problematic with standard approaches. © 2019 The Authors. Journal of Computational Chemistry published by Wiley Periodicals, Inc. 相似文献