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41.
Stratified materials are of great importance for many branches of modern industry, e.g. electronics or optics and for biomedical applications. Examination of chemical composition of individual layers and determination of their thickness helps to get information on their properties and function. A confocal 3D micro X‐ray fluorescence (3D µXRF) spectroscopy is an analytical method giving the possibility to investigate 3D distribution of chemical elements in a sample with spatial resolution in the micrometer regime in a non‐destructive way. Thin foils of Ti, Cu and Au, a bulk sample of Cu and a three‐layered sandwich sample, made of two thin Fe/Ni alloy foils, separated by polypropylene, were used as test samples. A Monte Carlo (MC) simulation code for the determination of elemental concentrations and thickness of individual layers in stratified materials with the use of confocal 3D µXRF spectroscopy was developed. The X‐ray intensity profiles versus the depth below surface, obtained from 3D µXRF experiments, MC simulation and an analytical approach were compared. Correlation coefficients between experimental versus simulated, and experimental versus analytical model X‐ray profiles were calculated. The correlation coefficients were comparable for both methods and exceeded 99%. The experimental X‐ray intensity profiles were deconvoluted with iterative MC simulation and by using analytical expression. The MC method produced slightly more accurate elemental concentrations and thickness of successive layers as compared to the results of the analytical approach. This MC code is a robust tool for simulation of scanning confocal 3D µXRF experiments on stratified materials and for quantitative interpretation of experimental results. Copyright © 2011 John Wiley & Sons, Ltd. 相似文献
42.
Summary We prove the existence of martingale solutions and of stationary solutions of stochastic Navier-Stokes equations under very general hypotheses on the diffusion term. The stationary martingale solutions yield the existence of invariant measures, when the transition semigroup is well defined. The results are obtained by a new method of compactness. 相似文献
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A new multiresidue method for the efficient screening, identification and quantification of over 160 pesticides belonging to different chemical classes in red, rose and white wines have been developed. The analysis was based on gas chromatographic-tandem quadrupole mass spectrometric determination (GC-QqQ-MS/MS). An optimization strategy involved the selection of buffering conditions and sorbents for dispersive-solid phase extraction (dispersive-SPE) in order to achieve acceptably high recoveries and reduce co-extractives in the final extracts. As a result, the optimized procedure allowed us to obtain consistent recoveries of the target pesticides including problematic ones such as captan, chlorothalonil, dichlofluanid, folpet and tolylfluanid. The attained recoveries were typically between 80 and 110% (89% on average) with RSD values typically lower than 10% (8% on average) at three spiking levels of 0.01, 0.05 and 0.2 mg kg−1. Linearity was studied in the range between 0.005 and 0.2 mg kg−1 using pesticide standards prepared both in pure solvent and in the presence of matrix, showing coefficients of determination (R2) higher than 0.99 for all the pesticides except for desmedipham, thiabendazole and thiamethoxam in pure solvent. The study of the ratio of the slopes obtained in solvent and in matrix provided information about the matrix effects, which was <10%, 10-20% and >20% for 33, 36 and 31% of the studied pesticides, respectively. To improve accuracy, matrix matched standards were always used for calculation of the quantification results. The expanded uncertainties were estimated by using a “top-down” approach as being 17% on average (coverage factor k = 2, confidence level 95%). Finally, the method was used with success to detect and quantify pesticide residues in commercial wines. 相似文献
46.
Cathodic stripping mechanism of an insoluble salt coupled with a homogenous chemical reaction is considered both theoretically and experimentally under conditions of square‐wave voltammetry. For the mercury electrode in aqueous solution, the electrode reaction is described as L(aq)+Hg(l)=HgL(s)+2e?, where L(aq) is the reactive ligand that forms a sparingly soluble compound HgL(s). The electrode reaction is coupled with a homogenous, first‐order chemical reaction, A(aq)=L(aq). Theoretical predictions are confirmed by experiments with 6‐mercaptopurine‐9‐D‐riboside in the presence of nickel(II) ions. 相似文献
47.
A GC/tandem quadrupole MS/MS method was developed and validated for the determination of the residues of 140 pesticides in fruits and vegetables. Pesticides were extracted from samples by using a miniaturized acetonitrile-based extraction technique known as the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. Validation studies were carried out on carrots, tomatoes, and strawberries. In order to reduce systematic errors due to a matrix-induced effect, quantification was carried out using matrix-matched standard calibration curves. The recovery and precision results satisfied the European Union criteria (i.e., average recoveries were in the range 70-120% with RSDs < or = 20%) for 125 of the 140 pesticides at a spiking level of 0.01 mg/kg. At the higher spiking levels, there were just two instances of overall average recovery < 70% (chlorothalonil and captan). The measurement uncertainty was estimated following a "top down" approach as being 21 and 35%, on average, based on validation and ongoing recovery data, respectively (coverage factor k = 2, confidence level 95%). Practical application to 541 samples of apples, tomatoes, strawberries, cucumbers, currants, mushrooms, carrots, peppers, pears, onions, and gooseberries under strict QC conditions demonstrated the ruggedness of the total procedure. 相似文献
48.
Ma?gorzata?Wi?niewskaEmail author Stanis?aw?Chibowski Teresa?Urban Dariusz?Sternik 《Journal of Thermal Analysis and Calorimetry》2011,103(1):329-337
The influence of solution pH on the structure of polyvinyl alcohol adsorption layer on the alumina surface was investigated.
The spectrophotometry, viscosimetry, thermogravimetry, potentiometric titration and microelectrophoresis were applied in experiments.
These methods enable determination of the following parameters: adsorbed amount of PVA, stability of suspension without and
with polymer, thickness of its adsorption layers, changes in thermal characteristics of Al2O3 surface with the adsorbed polymer, surface charge density and zeta potential of solid particles in the presence and absence
of PVA, respectively. All measurements were carried out in the pH range 3–9. The obtained results indicate that pH has a great
influence on the conformation of PVA chains adsorbed on the alumina surface. It is due to incomplete hydrolysis of acetate
groups of polyvinyl alcohol macromolecules (degree of hydrolysis 97.5%), which dissociate with the increasing pH. Moreover,
the polymer adsorption on the alumina surface causes changes in the course of thermogravimetric curves. The effect of weight
loss for Al2O3–PVA systems is smaller than that of Al2O3 without polymer. It is due to elimination of water molecules from the solid surface by adsorbed polymer. 相似文献
49.
Dariusz Gątarek 《Applied Mathematics and Optimization》1991,24(1):85-98
This paper deals with first-order quasi-variational inequalities with integral terms associated with impulsive and switching control of piecewise-deterministic processes. Two formulations of quasi-variational inequalities are studied, characteristic and viscosity, and the relations between them are discussed. As a tool we apply convex analysis methods. 相似文献
50.
We prove an existence result for topologically locally flat embeddings of 2-spheres in simply connected 4-manifolds. This topological result is deduced from a splitting theorem for pointed Hermitian modules over a cyclic group ring. A stability result for such modules is also proved. This applies to the isotopy classification of locally flat embeddings.Partially supported by the NSF. 相似文献