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951.
952.
Zanolari B Wolfender JL Guilet D Marston A Queiroz EF Paulo MQ Hostettmann K 《Journal of chromatography. A》2003,1020(1):75-89
The bark of catuaba (Erythroxylum vacciniifolium Martius, Erythroxylaceae), a tree native to the northern part of Brazil, was investigated for its alkaloid content. With the aim of obtaining preliminary structure information on-line, the alkaloid extract was analysed by high-performance liquid chromatography coupled to diode array UV detection, to mass spectrometry and to nuclear magnetic resonance. Interpretation of on-line spectroscopic data obtained from this extract led to structural elucidation of six new alkaloids and partial identification of 18 potentially original alkaloids bearing the same tropane skeleton esterified in positions 3 and 6 by 1-methyl-1H-pyrrol-2-carboxylic acid and/or 4-hydroxy-3,5-dimethoxybenzoic acid. 相似文献
953.
顺磁性聚酯金属配合物的合成及其驰豫性能的研究 总被引:2,自引:0,他引:2
本文通过二乙三胺五乙酸(DTPA)或乙二胺四乙酸(EDTA)的双酸酐与二元醇或二元酚进行聚合反应,制备了两个系列共15种新的聚酯型大分子配体及其顺磁性金属配合物,用核磁、红外光谱以及元素分析表征了配体和配合物的结构。初步试验结果表明,与相应的小分子金属配合物相比,聚酯金属配合物具有较高的弛豫性能。 相似文献
954.
955.
Fedushkin I. L. Kurskii Yu. A. Nevodchikov V. I. Bochkarev M. N. Müchle S. Schumann H. 《Russian Chemical Bulletin》2002,51(1):160-169
ansa-Metallocenes (5:5-C24H16)M(THF)2 (M = Sm (1), Yb (2), Ca (3)) and (5:5-C24H16)MI(THF) (M = Dy (8), Er (9), Tm (10), Lu (11)) were prepared in 50—90% yields by the in situ reactions of two equivalents of potassium acenaphthylenide K+C12H8
– with MI2 or MI3, respectively. Complexes 2 and 3 were also obtained by direct reduction of acenaphthylene with ytterbium and calcium naphthalenides, respectively. An ESR signal of the acenaphthylene radical anion, which was observed upon dissolution of compound 2 in THF, indicates that the [C24H16]2–
ansa-ligand dissociated into two [C12H8]·– radical anions. Hydrolysis of complex 2 in benzene afforded 1,1",3,3"-tetrahydro-3,3"-biacenaphthylene (4) and 3,3",4,4"-tetrahydro-3,3"-biacenaphthylene (5). The reaction of complex 2 with ZrCl4 and the reaction of compound 3 with Me3SiCl proceeded with the cleavage of the C—C bond between two acenaphthylene fragments of the [C24H16]2–
ansa-ligand to produce (2-C12H8)ZrCl2(THF)3 (6) and bis(trimethylsilyl)acenaphthene (Me3Si)2C12H8 (7), respectively. Compounds 1—3, 6, 7, and 11 were characterized by 1H and 13C NMR spectroscopy. The temperature dependence of the 1H NMR spectrum of compound 11 in tetrahydrofuran is indicative of the dynamic exchange of the solvent molecules in the coordination sphere of the Lu atom. After cooling of the solution to 210 K, the dynamic process was terminated as evidenced by the nonequivalence of the 1H signals of two acenaphthylene fragments. According to the X-ray diffraction data for complex 11, dimerization of two acenaphthylene radical anions at the Lu atom gave rise to the rac-ansa-metallocene structure. In compound 11, the Lu atom is 5-coordinated by two five-membered rings of the acenaphthylene ligands and also by the I atom and the THF molecule. The coordination environment about the Lu atom is a distorted tetrahedron. The average distance between the lutetium atom and the carbon atoms of the five-membered rings is 2.623 . 相似文献
956.
The Molecule S?GeCl2. Matrix IR Investigation and Ab initio SCF Calculation Molecular S?GeCl2 is found in a matrix reaction between the high-temperature molecule Ge?S and Cl2. A structure analog to that of phosgene can be derived from the isotopical shifts (70Ge/72Ge/73Ge/74Ge/76Ge and 35Cl/37Cl) within the IR spectra. The normal coordinate analysis results for the Ge?S force constant a value of 4.21 mdyn/Å. The spectroscopic results are confirmed by ab initio SCF calculations. 相似文献
957.
The comparison of a pure electrostatic approximation and complete supermolecule SCF ab initio computations on the hydration scheme of uracil and cytosine shows that the electrostatic procedure is capable to reproduce the general aspects of the results of the supermolecule treatment provided that different distances of shortest approach be adopted for the distances between the oxygen of water and the nitrogen of NH2 or NH groups or the oxygen of C-O groups on the one hand and the oxygen of water and pyridine-type nitrogens on the other hand. 相似文献
958.
The thermodynamics of the conversion of aqueous glucose to fructose has been investigated using both heat conduction microcalorimetry
and high pressure liquid chromatography (HPLC). The reaction was carried out in both aqueous Tris/HCl buffer and in aqueous
phosphate buffer in the pH range 7–8 using the enzyme glucose isomerase and the cofactors CoCl2 and MgSO4. The temperature range over which this reaction was investigated was 298.15–358.15 K. We have found that the enthalpy of
reaction is independent of pH over the range investigated. A combined analysis of both the HPLC and microcalorimetric data
leads to the following results at 298 15 K:ΔG° = 349 ± 53 J mol-1, ΔH° = 2.78 ± 0.20 kJ mol-1, and ΔC
p
°
= 76 ± 30 J mol-1 K-1. The stated uncertainties are based upon an analysis of both the random and systematic errors inherent in the measurements.
Comparisons are made with literature data. The percent conversion of glucose to fructose has been calculated for the temperature
range 300–373.15 K. 相似文献
959.
Karen L. Kindle 《Applied biochemistry and biotechnology》1983,8(2):153-170
Thermostable α-amylases have application in a variety of industrial processes and enzymes from a substantial number of thermophilic
bacteria and fungi have been screened and characterized to varying degrees. The characteristics of these enzymes are summarized
in this review. The genetics of α-amylase production inBacillus subtilis is reviewed and classical and recombinant DNA approaches to increasing α-amylase production are discussed. 相似文献
960.
Immobilized sulfhydryl groups were prepared by partial thiolation of NH2-glass beads. The microenvironment of the immobilized SH groups was varied by different chemical modifications of neighboring
NH2 groups. Introduction of a strong charge in the surroundings of immobilized sulfhydryls results in their dramatic stabilization
against autooxidation. This effect is due to the salting of O2 from the surface microlayer of the thiolated beads. 相似文献