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951.
Summary Coupling of full adsorption-desorption and size-exclusion chromatography (FAD-SEC) has been applied to the separation and
molecular characterization of three- and four-component polymer blends. The method is based on the full adsorption of alln orn−1 components of the polymer blend in a specially designed FAD minicolumn. By appropriate eluent switching the adsorbed polymers
are desorbed stepwise from the FAD minicolumn into an on-line SEC column for molecular characterization. It is shown that
the desorption isotherms of particular blend components give valuable information about the appropriate displacer composition.
The exact position of the desorption isotherms depends, however, both on the amount of polymer adsorbed and in the presence
of other, chemically different, polymers within FAD column. The nature and composition of the displacer must, therfore, be
adjusted if the intervals between the desorption of particular blend components are to be large enough to prevent displacement
overlap.
Presented at: Balaton Symposium on High-Performance Separation Methods, Siófok, Hungary, September 3–5, 1997. 相似文献
952.
Summary The performance of injection valves with both curtain- and single-flow column couplings has been evaluated using reverse-phase octadecylsilane columns and a standard test mixture. The results are compared with those obtained from septum and stopped-flow syringe injections.Stopped-flow valve injection has been examined similarly. Configurations and couplings which give optimum efficiency and reproducibility are recommended. 相似文献
953.
954.
We have previously described [1] the design of a simple heart-cuttings device based on the Deans' principle of remote pressure switching [2]. Since that time, further work has been conducted to refine the design of the heart-cutting device and to develop complementary backflushing and cryofocusing units. This paper describes the results obtained from an intensive evaluation of the three modules in various combinations and considers parameters critical to the practical application of multidimensional gas chromatography (MDGC). 相似文献
955.
Summary A packed flow cell was used for fluorometric detection in micro high-performance liquid chromatography. The flow cell consisted of fused-silica tubing packed with the same material as the separation column. A focusing effect of the stationary phase on the signal intensity was observed, leading to an improvement of the mass detection limit, as achieved by on-column detection. 相似文献
956.
957.
The ideal way to prepare efficient, yet robust stationary phases for microanalytical high-resolution methods such as capillary chromatography and electrochromatography remains to be defined. In this contribution a one step sol-gel process is proposed for the production of monolithic, macroporous nanocomposite phases in fused silica capillaries, which require no additional derivatization, since they already bear the interactive (C8) moieties. The effect of the catalyst, the water content, the pH, as well as that of certain additives on monolith formation and porosity is investigated. Volume shrinkage and a tendency to crack were the major obstacles to overcome. Homogeneous stationary phases could be produced by applying a pH gradient during sol formation, thereby changing the catalytic principle from acidic (0.1 M HCl) to basic (gradual formation of OH– as a consequence of the hydrolysis of N-methylformamide). Gelation/coacervation of suchgels could be induced by the addition of N,N-diethylamine. The water content during sol formation was determined as decisive for pore formation, with 250% of the amount theoretically needed for complete hydrolysis of all precursors giving optimal results. The volume shrinkage problem during xerogel formation was resolved by integrating dialkyldialkoxysilane units (dimethyldiethoxysilane 35 mol%) into the silica network. 相似文献
958.
Joan Fraga-DubreuilJean Pierre Bazureau 《Tetrahedron》2003,59(32):6121-6130
The first report of the use of task-specific ionic liquid as synthetic equivalent of ionic liquid-phase matrice for the preparation of a small library of 4-thiazolidinones is reported in this paper. The starting (ethyleneglycol)ionic liquid-phase is functionalized in good yields with 4-(formylphenoxy)butyric acid by using usual esterification reaction conditions (DCC/DMAP as catalyst). The synthesis of the ionic liquid-phase bound 4-thiazolidinones was performed by a one-pot three-component condensation under microwave dielectric heating. The final cleavage under microwave/catalysis strategy provides the expected 4-thiazolidinones in high purity after flash-chromatography purification. According to the ionic liquid-phase organic synthesis (IoLiPOS) methodology, it was found that optimized reaction conditions were performed by standard analytical methods (NMR, TLC). The 1H, 13C NMR spectrum of some representative 4-thiazolidinones and ionic liquid-phase bound benzaldehyde are also reported. 相似文献
959.
高效液相色谱和热重分析在树形聚酰胺胺合成中的应用 总被引:2,自引:0,他引:2
优化了聚酰胺胺树形分子合成工艺条件,采用HPLC和热重分析(TG)相结合的方法对所合成的树形聚酰胺胺进行分析与表征;HPLC的分析表明,在各不同代的目标化合物中,均有反应物单体存在,在高代产物中除了含有少量反应物外,还有少量的低代数分子;TG分析表明,产物中小分子反应物占的比例很少,一般为2%-3%左右,如果将减压蒸馏后的产物重新进行真空干燥,对半代树形大分子,能进一步有效除去小分子反应物,而对于整数代树形大分子,则效果并不理想。 相似文献
960.
Vendeuvre C Bertoncini F Thiébaut D Martin M Hennion MC 《Journal of separation science》2005,28(11):1129-1136
Modeling the retention in comprehensive two-dimensional gas chromatography (GC x GC) was achieved using retention indices obtained in conventional GC. Predicted results were compared with experimental data obtained in the two-dimensional separation of a synthetic hydrocarbon mixture. This proved to be helpful in optimizing the operating conditions of GC x GC separation of a complex petroleum sample and in identifying chemical families. 相似文献