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31.
Wall DB Berger SJ Finch JW Cohen SA Richardson K Chapman R Drabble D Brown J Gostick D 《Electrophoresis》2002,23(18):3193-3204
Peptide mass fingerprinting by matrix-assisted laser desorption/ionization (MALDI)-mass spectrometry (MS) is one of the standard high-throughput methods for protein identification today. Traditionally this method has been based on spotting peptide mixtures onto MALDI targets. While this method works well for more abundant proteins, low-abundance proteins mixed with high-abundance proteins tend to go undetected due to ion suppression effects, instrumental dynamic range limitations and chemical noise interference. We present an alternative approach where liquid chromatography (LC) effluent is continuously collected as linear tracks on a MALDI target. In this manner the chromatographic separation is spatially preserved on the target, which enables generation of off-line LC-MS and LC-MS/MS data by MALDI. LC-MALDI sample collection provides improved sensitivity and dynamic range, spatial resolution of peptides along the sample track, and permits peptide mass mapping of low-abundance proteins in mixtures containing high-abundance proteins. In this work, standard and ribosomal protein digests are resolved and captured using LC-MALDI sample collection and analyzed by MALDI-TOF-MS. 相似文献
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Robert A. Tromans Soumen K. Samanta Andy M. Chapman Anthony P. Davis 《Chemical science》2020,11(12):3223
Glucose is a key biomedical analyte, especially relevant to the management of diabetes. Current methods for glucose determination rely on the enzyme glucose oxidase, requiring specialist instrumentation and suffering from redox-active interferents. In a new approach, a powerful and highly selective achiral glucose receptor is mixed with a sample, l-glucose is added, and the induced CD spectrum is measured. The CD signal results from competition between the enantiomers, and is used to determine the d-glucose content. The involvement of l-glucose doubles the signal range from the CD spectrometer and allows sensitivity to be adjusted over a wide dynamic range. It also negates medium effects, which must be equal for both enantiomers. The method has been demonstrated with human serum, pre-filtered to remove proteins, giving results which closely match the standard biochemical procedures, as well as a cell culture medium and a beer sample containing high (70 mM) and low (0.4 mM) glucose concentrations respectively.A highly selective receptor, circular dichroism and chiral competition are combined in this versatile method for d-glucose analysis. 相似文献
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MgBr2 · OEt2 efficiently catalyzes the O- and N-tert-butoxycarbonylation of functionalized phenols and amines. The presented procedure is operationally simple and done under solvent-free conditions. 相似文献
35.
Henry N. Chapman 《Synchrotron Radiation News》2015,28(6):20-24
X-ray free-electron lasers produce brief flashes of X-rays that are of about a billion times higher peak brightness than achievable from storage ring sources. Such a tremendous jump in X-ray source capabilities, which came in 2009 when the Linac Coherent Light Source began operations, was unprecedented in the history of X-ray science. Protein structure determination through the method of macromolecular crystallography has consistently benefited from the many increases in source performance from rotating anodes to all generations of synchrotron facilities. But when confronted with the prospects of such bright beams for structural biology, enthusiastic proposals were tempered by trepidation of the effects of such beams on samples and challenges to record data [1]. A decade after these discussions (and others in the USA) on the applications of X-ray FELs for biology, the first experiments took place at LCLS, giving results that fulfilled many of the dreams of the early visionaries. In particular, the concept that diffraction representing the pristine object could be recorded before the X-ray pulse completely vaporizes the object was validated [2], confirming predictions [3] that established dose limits could be vastly exceeded using femtosecond-duration pulses. The first experiments illuminated a path to achieve room-temperature structures free of radiation damage, from samples too small to provide useful data at synchrotron facilities, as well as providing the means to carry out time-resolved crystallography at femtoseconds to milliseconds. In the five years since, progress has been substantial and rapid, invigorating the field of macromolecular crystallography [4, 5]. This phase of development is far from over, but with both the LCLS and the SPring-8 Ångström Compact Free-electron Laser (SACLA) providing facilities for measurements, the benefits of X-ray FELs are already being translated into new biological insights. 相似文献
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Development and application of sub‐2‐μm particle CO2‐based chromatography coupled to mass spectrometry for comprehensive analysis of lipids in cottonseed extracts 下载免费PDF全文
37.
The mechanical behavior of a system of parallel fibrils, capable of a phase change and embedded in a matrix, is analyzed by considering a simplified model. The model consists of a single infinitely long isolated fibril together with its associated matrix. Furthermore, it is assumed that slippage cannot occur at the fibril-matrix interface but that the matrix deforms in both tension and in shear. The phase change occurring in the fibrils gives rise to large discontinuous local strains in the fibril and is characterized by a “critical stress” and an “equilibrium stress.” Analysis of the model shows that distinct zones of the secondary phase will form consecutively along the fibril length when the system is extended. These zones are mobile and the stress fields in the matrix associated with each zone result in the mutual repulsion of adjacent zones. Stress-strain curves for both extension and recovery are calculated using linear and nonlinear forms of the system parameters. It is suggested that the model studied is relevant to the mechanical behavior of keratin fibers. 相似文献
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Dizaji RM Chapman NR Kirlin RL 《The Journal of the Acoustical Society of America》2002,111(2):800-808
An inversion method based on the concept of back wave propagation (BWP) is described in this paper for estimation of geoacoustic parameters from acoustic field data. A phase-regulation technique is introduced to increase the sensitivity of the method for geoacoustic model parameters having low sensitivity. The case of data consisting of signal plus additive noise is also addressed. It is shown theoretically that the sensitivity can be increased by a factor alpha using the phase regulation procedure, and that the spatial resolution of signal energy that is concentrated by BWP at the known source position is increased when a increases. This result suggests an effective criterion for use in the inversion, based on the spatial distribution of signal energy around the true source location. The basis for the criterion is the spatial variance of the back-propagated pressure field in a window around the known source location. A multistep search process is proposed to avoid using a complicated multidimensional search process. Inversion results from both simulations and experimental data are given. The real data were taken from the Pacific Shelf experiment carried out in shallow water off the West Coast of Vancouver Island in the Northeast Pacific Ocean. 相似文献