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Unusual odd-electron fragments from even-electron protonated prodiginine precursors using positive-ion electrospray tandem mass spectrometry 总被引:1,自引:0,他引:1
Chen K Rannulu NS Cai Y Lane P Liebl AL Rees BB Corre C Challis GL Cole RB 《Journal of the American Society for Mass Spectrometry》2008,19(12):1856-1866
Reports of anticancer and immunosuppressive properties have spurred recent interest in the bacterially produced prodiginines. We use electrospray tandem mass spectrometry (ES-MS/MS) to investigate prodigiosin, undecylprodiginine, and streptorubin B (butyl-meta-cycloheptylprodiginine) and to explore their fragmentation pathways to explain the unusual methyl radical loss and consecutive fragment ions that dominate low-energy collision-induced dissociation (CID) mass spectra. The competition between the formation of even-electron ions and radical ions is examined in detail. Theoretical calculations are used to optimize the structures and calculate the energies of both reactants and products using the Gaussian 03 program. Results indicate that protonation occurs on the nitrogen atom that initially held no hydrogen, thus allowing formation of a pseudo-seven-membered ring that constitutes the most stable ground state [M + H](+) structure. From this precursor, experimental data show that methyl radical loss has the lowest apparent threshold but, alternatively, even-electron fragment ions can be formed by loss of a methanol molecule. Computational modeling indicates that methyl radical loss is the more endothermic process in this competition, but the lower apparent threshold associated with methyl radical loss points to a lower kinetic barrier. Additionally, this characteristic and unusual loss of methyl radical (in combination with weaker methanol loss) from each prodiginine is useful for performing constant neutral loss scans to quickly and efficiently identify all prodiginines in a complex biological mixture without any clean-up or purification. The feasibility of this approach has been proven through the identification of a new, low-abundance prodigiosin analog arising from Hahella chejuensis. 相似文献
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P R Levison S E Badger D W Toome M L Koscielny L Lane E T Butts 《Journal of chromatography. A》1992,590(1):49-58
The scale-up of the separation of hen egg-white proteins has been investigated using Whatman DE92 anion-exchange cellulose. Having developed suitable chromatographic conditions, a maximum binding capacity of 100 mg protein/ml packed DE92 was determined in a 25-ml column. The process was scaled up 1000-fold and the influence of batch and column techniques on the chromatographic step assessed. Data indicate column processes to be more efficient than batch in the adsorptive stage. 相似文献
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We present a sum rule which related the inclusive cross section for high-energy neutrino scattering on polarized proton targets to the axial-vector coupling constant. The derivation of the sum rule rests on the equal-time algebra of the time-components of the weak currents. The sum rule also provides a discriminatory test of unified models of weak and electromagnetic interactions based on spontaneously-broken gauge symmetry. 相似文献
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For a state in a single-particle potential we derive simple expressions that the eigenvalue behavior and normalization integral properties near threshold. For the square-well, the various parameters in these expressions can be derived analytically. For the more realistic Saxon-Woods well-shape, we have made numerical calculations for s- and p-states and obtained values of these parameters and give rules for their evaluation. We show that those parameters determining the negative energy eigenvalues are also involved in determining the positive energy behavior, and the normalization properties. These studies have direct relevance to recent theories of some types of (d, p) and (n, γ) reactions which critically involve threshold behavior. 相似文献
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Stephen A. Wise Michele M. Schantz Bruce A. Benner Jr. Reenie M. Parris Richard E. Rebbert Lane C. Sander Barbara J. Koster Stephen N. Chesler Willie E. May 《Fresenius' Journal of Analytical Chemistry》1993,345(2-4):325-329
Summary Recent activities at the National Institute of Standards and Technology (NIST) related to the development of standard reference materials (SRMs) for the determination of polycyclic aromatic hydrocarbons (PAHs) are described. These activities include: (1) the development of four new calibration solution SRMs, a marine sediment SRM, and a frozen mussel tissue SRM; (2) noncertified measurements of PAHs for two additional sediment SRMs; and (3) the establishment of reference Ames bioassay mutagenicity values on three existing SRMs. Activities in progress include the recertification of the existing air particulate and diesel particulate SRMs and the preparation of a new diesel particulate extract SRM. 相似文献
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