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101.
Marimganti S Yasmeen S Fischer D Maier ME 《Chemistry (Weinheim an der Bergstrasse, Germany)》2005,11(22):6687-6700
The synthesis of the omega-amino acid 4 is described utilizing a two-dimensional synthesis strategy combined with an enzymatic differentiation of homotopic ester groups. The amino acid 4 features two non-bonded interactions that result in conformational constraints on a cyclic construct. This amino acid was incorporated into the four macrolactams 17, 22, 31, and 37. The ring in 17 and 22 is 18-membered, whereas 31 and 37 have a 19-membered ring. The pairs with the same ring size differ in a N-methyl group. For the larger macrolactams (31 and 37) conformational analysis showed that the macrocyclic rings are somewhat more rigid than in the natural lead, the depsipeptide jasplakinolide. Nevertheless, their conformations are comparable to the natural product. There are no intramolecular hydrogen bonds, neither is the cis-rotamer populated in the N-methyl compound 37. Due to the increased flexibility of the smaller macrolactams 17 and 22 and signal overlap, a distinct solution structure could not be obtained for these compounds. The amino acid 4 should be useful for restricting the conformation of other small peptides. 相似文献
102.
An oxidation method (sulfone method) for the determination of polycyclic aromatic sulfur heterocycles (PASH) in diesel fuel is presented. The aromatic fraction of a diesel fuel, isolated by solid phase extraction, is oxidized under controlled conditions with hydrogen peroxide. The oxidation products, mainly methylated dibenzosulfone, are determined and quantified directly, without further clean-up, by HPLC with photodiode-array detection. 相似文献
103.
The addition of C6H5? to the NN' ligand (NN' = Schiff base of pyridine carbaldehyde-(2) and (S)-(—)-α-phenylethylamine) in [C5H5 Mo(CO)2 NN'] PF6 occurs stereospecific from the side opposite to the C5H5-ring. 相似文献
104.
C. G. van der Paauw A. M. J. Rietveld H. Maarse B. Griepink E. A. Maier 《Fresenius' Journal of Analytical Chemistry》1992,344(7-8):297-300
Summary A pork fat sample was prepared and tested as candidate reference material for 10 organochlorine pesticides and metabolites (OCPs): hexachlorobenzene, -, - and -HCH, -heptachlor epoxide, dieldrin, endrin, p,p'-DDT, p,p'-TDE and p,p'-DDE. Preparation and testing for homogeneity and stability of the OCPs in the pork fat are discussed. The coefficient of variation of pesticide determinations carried out to test the between-ampoule homogeneity ranged from 2.4–5.8% and was found to be very similar to that for the analytical method (2.5–4.9%). This means that the homogeneity is very good. Stability data over 12 months do not show any trends that suggest lack of stability. 相似文献
105.
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107.
NMR spectroscopy plays an important part in the determination of the structures of organic compounds. The parameters of importance here are the chemical shifts of the 1H and 13C nuclei and the spin-spin interactions both between 1H nuclei and between 1H and 13C nuclei. Couplings between 13C nuclei were almost completely neglected until a few years ago, since they were extremely difficult to observe because of the low natural abundance of 13C. However, it is these couplings which afford information directly on the carbon-carbon connectivities in the molecule. It is now possible to use a special NMR pulse sequence to make these couplings more readily visible: the result of using this sequence is a 13C-NMR spectrum from which the carbon skeleton concerned can be directly read off. Two-dimensional spectra in particular are very easy to evaluate. The pulse sequence involved, which bears the somewhat puzzling name INADEQUATE, produces double-quantum coherences from which the NMR signals of the coupled carbon nuclei can be obtained. In this article the principle of double-quantum coherence is described and a number of examples for the application of the INADEQUATE pulse sequences to problems in synthetic organic chemistry, biosynthesis and natural products chemistry are presented; in addition, the possibility of applying the INADEQUATE method to other nuclei is considered. 相似文献
108.
The thermodynamics of water incorporation into Fe-doped SrTiO(3) was investigated by thermogravimetric measurements. Changes in valence states of redox-active dopant ions (Fe(3+)/Fe(4+)) with water vapor pressure were taken into account in the defect chemical analysis. The proton solubility was significantly enhanced by the presence of the redox centers. The hydration enthalpies and entropies were -60 kJ mol(-1) and -122 J mol(-1) K(-1). The defect chemical model was applied to describe the water vapor dependence of the electrical conductivity in mixed ionic and electronic conducting Fe-doped SrTiO(3) single crystals. 相似文献
109.
Water concentrations in dichloroacetic acid in the range of 0<C <1 % (C = percent by weight) can be determined directly by photometry at 1425 nm. The absorbance A at this maximum is described by the function A=1.267×C0.93 (cell path d=5 cm, correlation coefficient r=0.997). The variation coefficient for water concentrations of ≈0.06% was found to be V=6.5%. 相似文献
110.
Bicyclo[2.2.1]-2,5-heptadiene complexes of transition metal carbonyls have been treated with organometallic phosphines, to give the disubstituted compounds [(R3M′)3P]2M(CO)4 [R = CH3; M′ = Ge, Sn; M = Cr, Mo, W] by exchange of ligands. The chemical and spectroscopic properties of the new compounds are reported. 相似文献