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941.
Advanced solvent signal suppression for the acquisition of 1D and 2D NMR spectra of Scotch Whisky
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Will Kew Nicholle G.A. Bell Ian Goodall Dušan Uhrín 《Magnetic resonance in chemistry : MRC》2017,55(9):785-796
A simple and robust solvent suppression technique that enables acquisition of high‐quality 1D 1H nuclear magnetic resonance (NMR) spectra of alcoholic beverages on cryoprobe instruments was developed and applied to acquire NMR spectra of Scotch Whisky. The method uses 3 channels to suppress signals of water and ethanol, including those of 13C satellites of ethanol. It is executed in automation allowing high throughput investigations of alcoholic beverages. On the basis of the well‐established 1D nuclear Overhauser spectroscopy (NOESY) solvent suppression technique, this method suppresses the solvent at the beginning of the pulse sequence, producing pure phase signals minimally affected by the relaxation. The developed solvent suppression procedure was integrated into several homocorrelated and heterocorrelated 2D NMR experiments, including 2D correlation spectroscopy (COSY), 2D total correlation spectroscopy (TOCSY), 2D band‐selective TOCSY, 2D J‐resolved spectroscopy, 2D 1H, 13C heteronuclear single‐quantum correlation spectroscopy (HSQC), 2D 1H, 13C HSQC‐TOCSY, and 2D 1H, 13C heteronuclear multiple‐bond correlation spectroscopy (HMBC). A 1D chemical‐shift‐selective TOCSY experiments was also modified. The wealth of information obtained by these experiments will assist in NMR structure elucidation of Scotch Whisky congeners and generally the composition of alcoholic beverages at the molecular level. 相似文献
942.
Jaromíra Chýlková Markéta Tomášková Lenka Janíková Renáta Šelešovská Tomáš Navrátil Petra Chudobová 《Chemical Papers》2017,71(6):1047-1054
A sensitive voltammetric method for the determination of pyrogallol (PY) was developed employing a boron-doped diamond electrode (BDDE). The composition of the supporting electrolyte was investigated during the development of the methodology. Linear sweep voltammetry (LSV) under the optimized experimental conditions was applied for PY determination with a limit of detection and limit of quantification of 0.85 and 2.82 μmol L?1, respectively. These values are satisfactory for application to real samples. The usability of this method for the quantification of pyrogallol was in range from 2.82 to 296.00 μmol L?1. Finally, the developed method was successfully used for the analysis of real samples of biodiesel produced from rapeseed oil and its blend with diesel fuel. Samples of biodiesel and biodiesel blends were analyzed directly in an electrochemical cell, while samples with very low concentrations of PY in biodiesel were extracted with water using the proposed simple and fast process. 相似文献
943.
944.
A. A. Chugunova M. B. Kralj O. V. Polyakova V. B. Artaev P. Trebše S. A. Pokryshkin A. T. Lebedev 《Journal of Analytical Chemistry》2017,72(14):1369-1374
Disinfection is an important step in the purification of drinking and swimming pool water. The most common procedure includes chlorination, which efficiently eliminates microorganisms. However, the reaction of active chlorine with dissolved organic matter produces numerous organochlorine compounds posing a hazard to the environment and human health. UV filters belong to emerging contaminants, as their application to skin protection from UV irradiation becomes increasingly popular all over the world. Certain components of UV filters were detected in swimming pools and result in the emergence of new ecotoxicants. In the present study, 40 compounds, including numerous brominated derivatives, which result from the chlorination of avobenzone in sea water, were identified by gas chromatography–high resolution mass spectrometry. In addition, the applicability of photocatalysis to the destruction of chlorination products was studied. The procedure was found to be rather efficient and allows a decrease in the total amount of avobenzone transformation products by a factor of 10. The only compound class demonstrating stability under the applied conditions is exemplified by halogenated acetophenone derivatives. 相似文献
945.
ABSTRACTInfluence of nine different solvents, either alone or in a mixture, on the retention behavior of ziprasidone and its five impurities were examined by normal-phase thin-layer chromatography. Migration distances of the examined compounds obtained under the examined chromatographic conditions were correlated with calculated mobile phase properties, such as Snyder polarity and Hansen solubility. Linear or second-order polynomial relationships with high correlation coefficients were established between investigated variables. The obtained mathematical functions and statistical results indicated that selected mobile phase properties can be used for the prediction of the retention behavior of ziprasidone and its five impurities. 相似文献
946.
Aleksandra Radoičić Radivoj Petronijević Filip Andrić Živoslav Tešić 《液相色谱法及相关技术杂志》2017,40(5-6):297-303
ABSTRACTA new method for the extraction and quantitative determination of amygdalin has been proposed. Accelerated solvent extraction was applied for the extraction, and reversed-phase high-performance thin-layer chromatography method was developed, validated, and applied for the determination of amygdalin in the extracts of apricot, plum, almond, and peach kernels. The chromatographic system used was RP-18 silica, as stationary phase and acetonitrile/water (50:50, v/v), as mobile phase. Densitometric scanning was performed at 210 nm. The method was validated with respect to specificity, linearity, precision, and accuracy. The results showed that the peak area responses were linear within the concentration range of 2.5–50.0 µg/spot (R2 = 0.9984). The limit of quantification was 4.28 µg/spot, and the detection limit 1.28 µg/spot. The intra-day and inter-day reproducibility, in terms of %RSD, were in the range of 0.81–1.15 and 1.32–1.89, respectively. The accuracy data were in the range from 99.98 to 100.56%. The method is linear, quantitative and reproducible, and could be used as an efficient and economical green chromatographic procedure for the determination of amygdalin in the fruit kernel. 相似文献
947.
Explaining the emergence of life is perhaps central and the most challenging question in modern science. Within this area of research, the emergence and evolution of the genetic code is supposed to be a critical transition in the evolution of modern organisms. The canonical genetic code is one of the most dominant aspects of life on this planet, and thus studying its origin is critical to understanding the evolution of life, including life’s emergence. In this sense it is possible to view the ribosome as a digital-to-analogue information converter. Why the translation apparatus evolved, is one of the enduring mysteries of molecular biology. Assuming the hypothesis that during the emergence of life evolution had to first involve autocatalytic systems, which only subsequently acquired the capacity of genetic heredity, in the present article we discuss some aspects and causes of the possible emergence of digital, discrete information arising from analogue information realized in the intra- and inter-molecular interactions throughout molecular evolution. How such reverse translation was achieved at a molecular level is still unclear. The results of such debates and investigations might shift current biological paradigms and might also have a momentous significance for modern philosophy in understanding our place in the universe. 相似文献
948.
In this study, we start from a multi-source variant of the two-stage capacitated facility location problem (TSCFLP) and propose a robust optimization model of the problem that involves the uncertainty of transportation costs. Since large dimensions of the robust TSCFLP could not be solved to optimality, we design a memetic algorithm (MA), which represents a combination of an evolutionary algorithm (EA) and a modified simulated annealing heuristic (SA) that uses a short-term memory of undesirable moves from previous iterations. A set of computational experiments is conducted to examine the impact of different protection levels on the deviation of the objective function value. We also investigate the impact of variations of transportation costs that may occur on both transhipment stages on the total cost for a fixed protection level. The obtained results may help in identifying a sustainable and efficient strategy for designing a two stage capacitated transportation network with uncertain transportation costs, and may be applicable in the design and management of similar transportation networks. 相似文献
949.
Jánošíková L’udmila Herda Miloš Haviar Michal 《Central European Journal of Operations Research》2017,25(3):651-664
Central European Journal of Operations Research - The paper suggests two ways of combining a genetic algorithm with integer programming to improve the quality of the problem solution. The... 相似文献
950.
Romana Cerc Korošec Silvija Renko Gregor Rep Peter Bukovec 《Journal of Thermal Analysis and Calorimetry》2017,130(3):1383-1390
Thermal modification is one of the environmental friendly wood preservation technologies. During this process, changes of the main woody cell wall components occur, which lead to improved dimensional stability, lower hygroscopicity and improvement in biological durability. Several chemical reactions which occur during thermal treatment of wood caused changes in wood properties. During TG measurements, thermal decomposition reactions, which was not completed during previous thermal modification process, continued in wood samples, meaning that more thermally treated samples exhibited lower mass losses in a certain or whole temperature range up to 600 °C. Therefore, mass loss, obtained within selected temperature range, could be used as a marker of previous thermal treatment. The aim of the present work is to evaluate suitability of a thermogravimetric method (TG) for determination of a degree of thermal treatment of beech wood. On the basis of thermally untreated sample and those which were thermally modified at 180, 190, 200, 210, 215 and 220 °C in the absence of oxygen, respectively, and with known values of mass loss during the modification processes, several calibration curves were constructed. They represent mass loss in a certain temperature range during TG measurement versus mass loss during previous thermal modification. In a temperature range from 130 to 300 °C and from 130 to 320 °C under nitrogen atmosphere, a linear dependence was observed; correlation coefficients R 2 were 0.87 and 0.91, respectively. In wider temperature range and under air atmosphere, lower correlation coefficients were obtained. High correlation coefficient, higher than 0.95, was observed in a temperature range from 25 to 130 °C under both atmospheres. In this region, dehydration due to rehydration of thermally modified samples occurs. The results of this work were compared with those obtained for Norway spruce. 相似文献