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961.
Barluenga J Fernández-Rodríguez MA García-García P Aguilar E Merino I 《Chemistry (Weinheim an der Bergstrasse, Germany)》2005,12(1):303-313
The reaction of electron-deficient alkenes with alkoxyalkynyl Fischer carbene complexes (FCCs) represents a straightforward route to a new type of captodative (donor-acceptor) alkynylcyclopropanes, which have been prepared in moderate to high yields and in a diastereoselective manner. Some studies regarding the employment of additives to facilitate the recovery of the metal moiety after the reaction are also described. Finally, the first example of a cyclopropanation reaction through employing Fischer carbene complexes under microwave irradiation is presented; this method proved to be an advantageous alternative to the thermal reaction. 相似文献
962.
Martínez-Pla JJ Martín-Biosca Y Sagrado S Villanueva-Camañas RM Medina-Hernández MJ 《Journal of chromatography. A》2004,1048(1):111-118
Capillary electrophoresis (CE) is a powerful technique for enantiomer separations due to its intrinsic high separation efficiencies, speed of analysis, low reagent consumption and small sample requirements. However, some chiral selectors present strong background UV absorption providing high detection limits. The present paper deals with the application of the partial-filling technique to the separation of bupivacaine enantiomers by capillary electrophoresis using human serum albumin (HSA) as chiral selector. In this procedure the cationic surfactant cetyltrimethylammonium bromide (CTAB) was used as a dinamic capillary coating in order to reduce the electro-osmotic flow and detect both bupivacaine enantiomers out of the chiral selector plug. Several experimental conditions such as CTAB concentration, pH, HSA concentration and plug length, background electrolyte concentration, temperature and voltage were studied. Under the selected conditions it is possible to detect the separated enantiomers out of the HSA plug in less than 4 min using 50 mM Tris pH 8 as background electrolyte with 50 microM CTAB, at 30 degrees C and using a separation voltage of 25 kV. The proposed methodology was then validated for analytical purposes and applied to the analysis of pharmaceutical preparations commercially available. The results obtained with the proposed methodology were in good agreement with those declared by the manufacturers. The simplicity, sample throughput, accuracy, reproducibility and low cost of the proposed method make it suitable for the control of the enantiomeric composition of bupivacaine in pharmaceuticals. 相似文献
963.
Batistoni DA Garavaglia RN Rodríguez RE 《Fresenius' Journal of Analytical Chemistry》2000,366(3):221-227
The simultaneous injection of volatile hydride species and hydrogen gas, originating in reagent decomposition, was monitored during the operation of a continuous hydride generation manifold employed for the determination of trace arsenic by HG-ICP-AES. Line and background intensities as well as the FWHM of the hydrogen Hgamma and Hdelta lines were measured, and electron number densities (ne) estimated from Stark broadening of the line profiles. Results were compared with those obtained by conventional pneumatic injection of aqueous solutions. Overlapping with atomic nitrogen lines at 410 nm and 411 nm tends to distort the Hdelta line profile for the hydrogen-seeded plasma, rendering unreliable results. The N I lines seem to be quenched by the presence of water aerosol. More consistent results were obtained with the Hgamma line. When no solutions are pumped through the hydride generation manifold ("dry" plasma), the measured ne value was (1.57 +/- 0.22) x 10(15)cm(-3). Conversely, when the reducing reagent flow was replaced by pure water (corresponding to the injection of water vapor in equilibrium that is swept by the argon carrier gas passing through the phase separator), the electron concentration is 25% higher. In that case the ne value agrees between the experimental error with that obtained for a plasma in which a water aerosol is introduced at a flow rate of 1 mL/min. An enhancement of 52% relative is observed in ne when the system is operated under optimized conditions for arsine generation, employing sodium tetrahydroborate in acidic medium as reducing agent (i.e. hydrogen seeded plasma). It was also observed that the continuum emission near 410 nm for the hydrogen containing plasma correlates with the measured electron number density, suggesting that the background enhancement under hydride generation conditions may respond to the ion-electron recombination mechanism. 相似文献
964.
Pilar De Miguel Nazario Martín Miguel F. Braa 《Journal of heterocyclic chemistry》1994,31(5):1235-1239
Novel tetrahydroimidazo[1,5-b]-β-carbolines derivatives 6 bearing complex basic chains as substituents on the imidic nitrogen have been prepared in a one-pot reaction. This simple experimental procedure overcomes the direct handle of isocyanates which can be favorably generated “in situ” from carbonyldiimidazole (CDI) and different amines. The stereochemistry of the novel compounds was determined by nmr experiments. 相似文献
965.
S. M. Bardavid G. C. Pedrosa M. Katz M. A. Postigo P. García 《Journal of solution chemistry》1996,25(11):1125-1135
Exces molar volumes, and excess viscosities of then-hexane+dichloromethane+tetrahydrofuran system have been determined at 25°C by measuring densities and viscosities. Different expressions exist in the literature to predict these excess properties from binary data. The empirical correlation of Cibulka is shown to be the best in this system. 相似文献
966.
Romero R Bagur MG Sánchez-Viñas M Gázquez D 《Analytical and bioanalytical chemistry》2003,376(2):162-167
Biogenic amines, as dabsyl derivatives, were determined in beer samples, intermediate products, and raw materials (malt and maize) by HPLC. A procedure for the extraction of the amines from malt and maize with diluted hydrochloric acid was optimised by combining a Response Surface Methodology with a Simultaneous Decision Making Approach. The results of the analysis indicate that, in brewing, technology and hygiene are the decisive factors that determine the amine concentrations in the final product. 相似文献
967.
Paterson I Aceña JL Bach J Chen DY Coster MJ 《Chemical communications (Cambridge, England)》2003,(4):462-463
Simplified analogues of the potent antimitotic marine macrolide spongistatin 1/altohyrtin A were synthesised and evaluated as growth inhibitory agents against a range of human tumour cell lines, including Taxol-resistant strains, revealing that E-ring dehydration leads to enhanced cytotoxicity at the low picomolar level while truncation of the side-chain at C46 results in a drastic decrease in activity. 相似文献
968.
P. Vaňura V. Jedináková-Křížová M. Vobecký 《Journal of Radioanalytical and Nuclear Chemistry》2006,267(2):501-503
Summary An extraction technique for the separation of 90Sr from a high excess of90Y has been developed. This procedure can be used for the determination of trace amounts of90Sr in90Y prepared by a radiochemical90Y/90Sr generator by liquid scintillation. 相似文献
969.
Izaskun Bustero García Ainara Obieta Isabel Muñoz Roberto Rincón Inés Arteche Amaya 《Mikrochimica acta》2006,152(3-4):239-247
Interest in carbon nanotubes (CNT) has grown at a very rapid rate in the last decade. Their interesting physical and chemical
properties open attractive possibilities in many application areas. These properties depend on the process conditions during
synthesis and on subsequent purification steps. Recent studies have demonstrated that CNT can promote the electron transfer
of biomolecules. These exceptional properties make them attractive for use in electrochemical biosensors.
Multi walled nanotubes have been synthesized by the Chemical Vapor Deposition (CVD) method using methane as a carbon source
and Ni–Al2O3–SiO2 as the catalyst. The influence of the variation of certain reaction parameters such as feed gas composition, catalyst mass,
temperature and reaction time in the yield of the CVD process has been established. In addition, the structural and chemical
characteristics of the CNTs have been studied and a purification process to eliminate the catalyst and amorphous carbon has
been developed that involves a gaseous oxidative process and acid treatment. The efficiency of the purification step has been
determined by analytical techniques.
Atomic force microscopy, Raman scattering, thermogravimetric analysis, inductively coupled plasma atomic spectroscopy are
the characterization techniques employed in this work. 相似文献
970.
Yingyongnarongkul BE How SE Díaz-Mochón JJ Muzerelle M Bradley M 《Combinatorial chemistry & high throughput screening》2003,6(7):577-587
Advances in high throughput screening (HTS), together with the rapid progress in combinatorial chemistry, genomic and proteomic sciences have dramatically stimulated the development of a variety tools to enable the drug discovery process to become more efficient. Major future challenges in HTS include obtaining high density and good quality data based on assays that are rapid, reliable, inexpensive, sensitive, simple and miniaturised. This paper reviews the development and role of bead-based assays for HTS including DNA and single nucleotide polymorphism (SNP) assays, particularly from a multiplex perspective and evaluating the recent advances in bead-based arrays. The encoding strategies that are commonly used in bead-based assays are highlighted, while the importance of magnetic beads in genomic and proteomic purifications is discussed. In conclusion, bead-based assays offer a powerful promising approach for many aspects of drug discovery. 相似文献