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11.
Arsenic compounds including arsenous acid (As(III)), arsenic acid (As(V)), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) were separated by high-performance liquid chromatography (HPLC) and detected by inductively coupled plasma mass spectrometry (ICP-MS). A Hamilton PRX-100 anionic-exchange column and a pH 8.5 K2HPO4/KH2PO4 5.0 × 10−3 mol L−1 mobile phase were used to achieve arsenic speciation. The separation of arsenic species provided peaks of As(III) at 2.75 min, DMA at 3.33 min, MMA at 5.17 min and As(V) at 12.5 min. The detection limits, defined as three times the standard deviation of the lowest standard measurements, were found to be 0.2, 0.2, 0.3 and 0.5 ng mL−1 for As(III), DMA, MMA and As(V), respectively. The relative standard deviation values for a solution containing 5.0 μg L−1 of As(III), DMA, MMA and As(V) were 1.2, 2.1, 2.5 and 3.0%, respectively. This analytical procedure was applied to the speciation of arsenic compounds in drinking (soft drink, beer, juice) samples. The validation of the procedure was achieved through the analysis of arsenic compounds in water and sediment certified reference materials. 相似文献
12.
In this communication we report a stereoselective total synthesis of N-Boc-dolaproine (Dap), an amino acid residue of the antineoplastic pentapeptide Dolastatin 10. Our strategy is based on a Baylis-Hillman reaction between N-Boc-prolinal and methyl acrylate, followed by a diastereoselective double bond hydrogenation and hydrolysis of the ester function. 相似文献
13.
Luiz A. F. Coelho Jos V. Oliveira Saul G. D'vila Janete H. Y. Vilegas Fernando M. Lanas 《Journal of separation science》1997,20(8):431-436
The effects of temperature and solvent density on the characteristics of the extracts obtained from supercritical fluid extraction (SFE) of the volatile compounds from Brazilian rosemary (Rosamarinus officianalis L., Labiatae) using carbon dioxide (CO2) as solvent were investigated. The experiments were performed in a semi-batch laboratory scale home-made unit at two temperatures, viz. 310.15 and 320.15 K, over the pressure range of 100-160 bar. This study allowed to determine the crossover point and the maximum solubility of the oil. The products were analyzed by HRGC-MS, and compounds grouped in three different classes according to their molecular mass distribution in order to evaluate the influence of the variables studied on the characteristics of the extracts. The model proposed by Sovová was adopted in an attempt to interpret the mass transfer phenomena in the extraction process. 相似文献
14.
Nívia Maria Melo Coelho Edmar Isaías de Melo Hélen Cristine de Rezende Ana Graci Brito-Madurro João Marcos Madurro 《Journal of Solid State Electrochemistry》2012,16(3):945-951
In this work, carbon electrodes modified with aminophenols were developed for the production of pesticides biosensors based
on acetylcholinesterase. The polymers were potentiodynamically deposited on a graphite electrode surface by the oxidation
of monomers, 2-aminophenol, 3-aminophenol and 4-aminophenol. The electrochemical behaviour and surface analysis of the electrodes
modified by polyaminophenols non-immobilized and immobilized on acetylcholinesterase were studied by cyclic voltammetry, electrochemical
impedance spectroscopy and atomic force microscopy. Roughness values obtained for graphite electrodes modified with poly(4-aminophenol)
and poly(4-aminophenol)/acetylcholinesterase were 174 and 86 nm, respectively. The acetylcholinesterase enzyme was immobilized
on a graphite and a graphite modified with poly(4-aminophenol), and these electrodes were coupled in the flow system. Potentiometric
response due to hydrogen ions generated by an enzymatic system in the presence of acetylcholine chloride substrate was evaluated.
The results showed that the graphite/poly(4-aminhophenol) sensor presents high sensitivity to hydrogen ions when compared
with other graphite/polyaminophenols sensors. The biosensor coupled in a continuous flow system was employed for the detection
of dichlorvos. The detection and quantification limits were 0.8 and 2.4 μmol L−1 dichlorvos, respectively. This sensor reveals an efficient and promising material for biomolecules immobilization. 相似文献
15.
16.
C. García-Astrain A. Gandini D. Coelho I. Mondragon A. Retegi A. Eceiza M.A. Corcuera N. Gabilondo 《European Polymer Journal》2013
This study describes an environmentally friendly and green synthetic approach for the preparation of poly(aminoethylmethacrylate)-based hydrogels crosslinked through Diels–Alder (DA) reaction in water. This “click” reaction offers the possibility of preparing chemically crosslinked hydrogels in the absence of any catalyst, initiator or coupling agent, thus preserving the biocompatibility of the material. The suitable furan diene was obtained by modifying a methacrylate polymer by its reaction with furfural, a first generation compound derived from renewable resources. Methacrylate-based complementary polymeric dienophiles were also prepared by introducing maleimide groups into the structure. The products obtained at different steps were characterized by FTIR, NMR and TGA techniques. The study of the rheological properties of the hydrogels proved the success of this green “click” synthetic strategy confirming the formation of chemically crosslinked networks by the use of the Diels–Alder reaction. Furthermore, SEM studies revealed promising morphological properties of the ensuing hydrogels in terms of biomedical applications. 相似文献
17.
Easily prepared choline iodide is an active catalyst for the synthesis of cyclic carbonates through the coupling reaction of CO2 and epoxides using low pressure (1 MPa), moderate temperature (85 ºC) and green solvents (ethanol and propan-2-ol). The effects of reaction temperature, pressure, reaction time and amount of catalyst used were also investigated. The results showed moderate to high yields and excellent selectivities of cyclic carbonates with vinyl or acrylate groups under mild reaction conditions. The heterogenization of choline over a Merrifield resin gives access to a supported catalyst with good recyclability and reactivity that can be extended to a variety of terminal epoxide substrates. 相似文献
18.
Thiago Henrique Napoleão Teodomiro Gomes dos Santos-Filho Emmanuel Viana Pontual Rodrigo da Silva Ferreira Luana Cassandra Breitenbach Barroso Coelho Patrícia Maria Guedes Paiva 《Applied biochemistry and biotechnology》2013,171(3):744-755
This work reports the use of matrices containing Cratylia mollis lectins (Cramoll 1,2,3-Sepharose and Cramoll 3-Sepharose) for isolation of glycoproteins from fetal bovine serum, human colostrum, hen egg white, and human blood plasma. Cramoll 1,2,3-Sepharose was able to bind a glycoprotein from fetal bovine serum which showed the same fetuin electrophoretic profile. The data indicate that this protein adsorbed to the matrix by interaction with Cramoll 3. Cramoll 1,2,3-Sepharose was not efficient to retain glycoproteins from human colostrum or commercial ovalbumin. Cramoll 3-Sepharose bound ovalbumin, and the support retained protein from hen egg white. Protein peaks eluted from the column with 1.0 M NaCl or 0.3 M galactose showed apparent molecular mass of ovalbumin. Two main proteins from blood plasma with apparent molecular mass 67 (similar to albumin) and 50 kDa (similar to fetuin) adsorbed on Cramoll 3-Sepharose and were eluted with 1.0 M NaCl as a single peak. Elution of adsorbed plasma proteins with 0.3 M galactose was less selective than with 1.0 M NaCl as revealed by SDS-PAGE. In conclusion, the Cramoll 1,2,3-Sepharose and Cramoll 3-Sepharose matrices were useful to separate glycoproteins from complex protein mixtures, and the adsorption phenomena was a carbohydrate-dependent event. 相似文献
19.
Martina Palomba Italo Franco Coelho Dias Ornelio Rosati Francesca Marini 《Molecules (Basel, Switzerland)》2021,26(11)
In recent years, vinyl selenones were rediscovered as useful building blocks for new synthetic transformations. This review will highlight these advances in the field of multiple-bond-forming reactions, one-pot synthesis of carbo- and heterocycles, enantioselective construction of densely functionalized molecules, and total synthesis of natural products. 相似文献
20.
Exploring the Molecular Structure of Imidazolium–Silica‐Based Nanoparticle Networks by Combining Solid‐State NMR Spectroscopy and First‐Principles Calculations 下载免费PDF全文
Dr. Marie‐Alexandra Neouze Martin Kronstein Dr. Marco Litschauer Dr. Michael Puchberger Dr. Cristina Coelho Prof. Christian Bonhomme Prof. Christel Gervais Dr. Frederik Tielens 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(46):15188-15196
A DFT‐based molecular model for imidazolium–silica‐based nanoparticle networks (INNs) is presented. The INNs were synthesized and characterized by using small‐angle X‐ray scattering (SAXS), NMR spectroscopy, and theoretical ab initio calculations. 11B and 31P HETCOR CP MAS experiments were recorded. Calculated 19F NMR spectroscopy results, combined with the calculated anion–imidazolium (IM) distances, predicted the IM chain density in the INN, which was also confirmed from thermogravimetric analysis/mass spectrometry results. The presence of water molecules trapped between the nanoparticles is also suggested. First considerations on possible π–π stacking between the IM rings are presented. The predicted electronic properties confirm the photoluminescence emissions in the correct spectral domain. 相似文献