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131.
A dual-layer ion-exchange latex-coated column was prepared and characterised for on-capillary preconcentration of cations using an open-tubular ion-exchange CEC format. After preconcentration, the analyte cations were eluted with a transient isotachophoretic gradient and separated by CE. The latex double layer was established by first coating the negatively charged wall of the capillary with a layer of cationic quaternary ammonium anion-exchange Dionex AS5A latex particles (60 nm diameter), and then coating a layer of anionic sulphonated cation-exchange Dionex CS3 latex particles (300 nm diameter) onto the underlying AS5A layer. The adhesion of layers is based on electrostatic attractions. Several dual-layer capillaries were characterised for their EOF and ion-exchange capacity and this showed that coatings could be prepared reproducibly by a simple flushing procedure. The dual-layer columns exhibited a moderate, pH-independent EOF (ca. 26 x 10(-9 )m2V(-1)s(-1)) and an ion-exchange capacity of 57 microequiv./g (or 2.69 nequiv./column). Using an 8 cm length of coated capillary combined with a 72 cm length of untreated capillary, a method for on-line preconcentration and separation of monovalent organic bases, alkali metal ions and alkaline earth metal ions by CE was developed. Recoveries for the preconcentration step were 48% for 4-methylbenzylammonium, 43% for benzylammonium, 30-32% for alkali metal ions and 71-75% for alkaline earth cations. In all cases, recoveries were reproducible with RSDs being less than 6.2%. The influences of the ion-exchange selectivity coefficient of the analyte and the sample-loading rate on analyte recovery were also examined. The proposed method was utilised for the determination of alkaline earth cations and low microM detection limits were obtained. 相似文献
132.
Hutchinson JP Hilder EF Macka M Avdalovic N Haddad PR 《Journal of chromatography. A》2006,1109(1):10-18
Silica monoliths coated with functionalised latex particles have been prepared for use in monolithic ion-exchange capillary electrochromatography (IE-CEC) for the separation of inorganic anions. The ion-exchange monoliths were prepared using 70 nm quaternary ammonium, anion-exchange latex particles, which were bound electrostatically to a monolithic silica skeleton synthesised in a fused silica capillary. The resulting stationary phases were characterised in terms of their chromatographic performance and capacity. The capacity of a 50 microm diameter 25 cm latex-coated silica monolith was found to be 0.342 nanoequivalents and 80,000 theoretical plates per column were typically achieved for weakly retained anions, with lower efficiency being observed for analytes exhibiting strong ion-exchange interaction with the stationary phase. The electroosmotic flow (EOF) was reversed after the latex-coating was applied (-25.96 m2 V(-1) s(-1), relative standard deviation (RSD) 2.8%) and resulted in anions being separated in the co-EOF mode. Ion-exchange interactions between the analytes and the stationary phase were manipulated by varying the ion-exchange selectivity coefficient and the concentration of a competing ion (phosphate or perchlorate) present in the electrolyte. Large concentrations of competing ion (greater than 1M phosphate or 200 mM perchlorate) were required to completely suppress ion-exchange interactions, which highlighted the significant retention effects that could be achieved using monolithic columns compared to open tubular columns, without the problems associated with particle-packed columns. The latex-coated silica monoliths were easily produced in bulk quantities and performed reproducibly in acidic electrolytes. The high permeability and beneficial phase ratio makes these columns ideal for micro-LC and preconcentration applications. 相似文献
133.
Hong B Haddad M Maley F Jensen JH Kohen A 《Journal of the American Chemical Society》2006,128(17):5636-5637
The nature of a H-transfer in the thymidylate synthase catalyzed reaction was investigated by comparison of the wild-type enzyme with the W80M mutant. The nature of the H-transfer was not affected, as indicated by intrinsic isotope effects and their temperature dependence. These findings support a single-step hydride transfer instead of a two-step radical transfer. 相似文献
134.
The separation of three selective serotonin reuptake inhibitors (SSRIs) by capillary electrophoresis (CE) with fully integrated solid-phase extraction (SPE) is described. Polymeric monolithic SPE modules were prepared in situ within a fused silica capillary from either butyl methacrylate-co-ethylene dimethacrylate or 3-sulfopropyl methacrylate-co-butyl methacrylate-co-ethylene dimethacrylate. Using a 1 cm SPE module placed at the inlet of the capillary, a mixture of sertraline, fluoxetine and fluvoxamine was extracted from aqueous solution by applying a simple pressure rinse. Under pressure-driven conditions, efficient elution was possible from both SPE materials investigated using 50 mM phosphate buffer, pH 3.5 in acetonitrile (20/80, v/v). Two different strategies were investigated for the efficient elution and subsequent CE separation. Injection of an aqueous sample plug directly into the non-aqueous elution/separation buffer was found to be unsuitable with poor elution profiles observed in the electrodriven mode. Alternatively, a sample plug equivalent to several capillary volumes could be injected by pressure followed by filling the capillary with the non-aqueous elution/separation buffer from the outlet end using a combination of pressure and electrodriven flow. Using a neutral monolith, efficient elution/separation was not possible due to an unstable electroosmotic flow (EOF), however, by adding the ionisable monomer, 3-sulfopropyl methacrylate to the SPE module to increase and stabilise the EOF, it was possible to achieve efficient elution from the SPE module, followed by baseline separation by CE using a 200 mM acetate buffer, pH 3.5 in acetonitrile (10/90, v/v). With enrichment factors of over 500 achieved for each of the analytes this demonstrates the potential of in-line SPE-CE for the sensitive analysis of these drugs. 相似文献
135.
136.
This paper focuses on semistability and finite-time semistability for discontinuous dynamical systems. Semistability is the property whereby the solutions of a dynamical system converge to Lyapunov stable equilibrium points determined by the system initial conditions. In this paper, we extend the theory of semistability to discontinuous autonomous dynamical systems. In particular, Lyapunov-based tests for strong and weak semistability as well as finite-time semistability for autonomous differential inclusions are established. Using these results we then develop a framework for designing semistable and finite-time semistable protocols for dynamical networks with switching topologies. Specifically, we present distributed nonlinear static and dynamic output feedback controller architectures for multiagent network consensus and rendezvous with dynamically changing communication topologies. 相似文献
137.
Omid Bozorg Haddad Mahsa Mirmomeni Mahboubeh Zarezadeh Mehrizi Miguel A. Mariño 《Computational Optimization and Applications》2010,47(1):97-128
Effective project management requires the development of a realistic plan and a clear communication of the plan from the beginning
to the end of the project. The critical path method (CPM) of scheduling is the fundamental tool used to develop and interconnect
project plans. Ensuring the integrity and transparency of those schedules is paramount for project success. The complex and
discrete nature of the solution domain for such problems causes failing of traditional and gradient-based methods in finding
the optimal or even feasible solution in some cases. The difficulties encountered in scheduling construction projects with
resource constraints are highlighted by means of a simplified bridge construction problem and a basic masonry construction
problem. The honey-bee mating optimization (HBMO) algorithm has been previously adopted to solve mathematical and engineering
problems and has proven to be efficient for searching optimal solutions in large-problem domains. This paper presents the
HBMO algorithm for scheduling projects with both constrained and unconstrained resources. Results show that the HBMO algorithm
is applicable to projects with or without resource constraints. Furthermore, results obtained are promising and compare well
with those of well-known heuristic approaches and gradient-based methods. 相似文献
138.
Arianne Soliven Gary R. Dennis Georges Guiochon Emily F. Hilder Paul R. Haddad R. Andrew Shalliker 《Journal of chromatography. A》2010,1217(39):6085-6091
This study investigates the synthesis and chromatographic behaviour of an analytical size cyanopropyl “cyano” bonded silica monolith. Surface modification was undertaken by treating a neat silica monolith with chloro(3-cyanopropyl)dimethyl silane in dry heptane over a two day period. The resulting monolith showed stability over the duration of the testing program that involved flushing the column with more than 2000 column volumes of mobile phase. Efficiency measurements before and after sylation verified that the integrity of the silica monolith itself was not affected by the modification process, the highest number of theoretical plates (N/m) using anisole was 81,650. A brief selectivity test was then undertaken to assess methylene selectivity and phenyl selectivity. Elemental analysis was used to determine the homogeneity of the carbon load throughout the monolithic bed, and was compared to two commercial C18 and one ‘self’ modified C18 silica monoliths. The development of the in situ modification is also discussed. 相似文献
139.
140.
Kenneth Berg David Gove Kamel Haddad 《Proceedings of the American Mathematical Society》1998,126(3):899-905
Enveloping semigroups of topological actions of semigroups on compact spaces are studied. For zero dimensional spaces, and under modest conditions on , the enveloping semigroup is shown to be the Stone-\v{C}ech compactification if and only if some Cartesian product has the two-shift as a factor. Examples are discussed showing that, unlike in the measure theory case, positive entropy does not imply the existence of such a factor even if the Cartesian product has large entropy.