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51.
Quality by design: A systematic and rapid liquid chromatography and mass spectrometry method for eprosartan mesylate and its related impurities using a superficially porous particle column
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Pradipbhai D. Kalariya Murali V. N. Kumar Talluri Vinay D. Gaitonde Prashant S. Devrukhakar Ragampeta Srinivas 《Journal of separation science》2014,37(16):2160-2171
The present work describes the systematic development of a robust, precise, and rapid reversed‐phase liquid chromatography method for the simultaneous determination of eprosartan mesylate and its six impurities using quality‐by‐design principles. The method was developed in two phases, screening and optimization. During the screening phase, the most suitable stationary phase, organic modifier, and pH were identified. The optimization was performed for secondary influential parameters—column temperature, gradient time, and flow rate using eight experiments—to examine multifactorial effects of parameters on the critical resolution and generated design space representing the robust region. A verification experiment was performed within the working design space and the model was found to be accurate. This study also describes other operating features of the column packed with superficially porous particles that allow very fast separations at pressures available in most liquid chromatography instruments. Successful chromatographic separation was achieved in less than 7 min using a fused‐core C18 (100 mm × 2.1 mm, 2.6 μm) column with linear gradient elution of 10 mM ammonium formate (pH 3.0) and acetonitrile as the mobile phase. The method was validated for specificity, linearity, accuracy, precision, and robustness in compliance with the International Conference on Harmonization Q2 (R1) guidelines. The impurities were identified by liquid chromatography with mass spectrometry. 相似文献
52.
Kumar Gautam Mullick Prashansha Nandakumar Krishnadas Mutalik Srinivas Rao Chamallamudi Mallikarjuna 《Chromatographia》2022,85(7):629-642
Chromatographia - Stability-indicating reverse-phase HPLC analytical method for the quantification of Paclitaxel (PTX) in the bulk and cationic liposomes was developed. The optimized method was... 相似文献
53.
Chitra N. Chandrasekaran S. Srinivas C. Venkata Athmalingam S. Venkatraman B. 《Journal of Radioanalytical and Nuclear Chemistry》2022,331(6):2461-2468
Journal of Radioanalytical and Nuclear Chemistry - In this study, the thoron diffusion characteristic in soil is used as a tool to measure the porosity of the soil. The feasibility is demonstrated... 相似文献
54.
Effect of Temperature and Discharge Rate on Electrochemical Performance of Fiber Nickel–Cadmium Cell
Senthilkumar M. Satyavani T. V. S. L. Raman M. Venkat Sahoo P. K. Kumar A. Srinivas 《Russian Journal of Electrochemistry》2022,58(1):43-49
Russian Journal of Electrochemistry - The effect of temperature and discharge rate on the discharge capacity of nickel–cadmium (Ni?Cd) cell is investigated quantitatively. Ni–Cd... 相似文献
55.
Vladislav S. Krasnoukhov Prof. Dr. Valeriy N. Azyazov Prof. Dr. Alexander M. Mebel Dr. Srinivas Doddipatla Dr. Zhenghai Yang Shane Goettl Prof. Dr. Ralf I. Kaiser 《Chemphyschem》2021,22(14):1497-1504
The chemical dynamics of the elementary reaction of ground state atomic silicon (Si; 3P) with germane (GeH4; X1A1) were unraveled in the gas phase under single collision condition at a collision energy of 11.8±0.3 kJ mol−1 exploiting the crossed molecular beams technique contemplated with electronic structure calculations. The reaction follows indirect scattering dynamics and is initiated through an initial barrierless insertion of the silicon atom into one of the four chemically equivalent germanium-hydrogen bonds forming a triplet collision complex (HSiGeH3; 3 i1 ). This intermediate underwent facile intersystem crossing (ISC) to the singlet surface (HSiGeH3; 1 i1 ). The latter isomerized via at least three hydrogen atom migrations involving exotic, hydrogen bridged reaction intermediates eventually leading to the H3SiGeH isomer i5 . This intermediate could undergo unimolecular decomposition yielding the dibridged butterfly-structured isomer 1 p1 (Si(μ-H2)Ge) plus molecular hydrogen through a tight exit transition state. Alternatively, up to two subsequent hydrogen shifts to i6 and i7 , followed by fragmentation of each of these intermediates, could also form 1 p1 (Si(μ-H2)Ge) along with molecular hydrogen. The overall non-adiabatic reaction dynamics provide evidence on the existence of exotic dinuclear hydrides of main group XIV elements, whose carbon analog structures do not exist. 相似文献
56.
We study superconducting systems in the regime where superconductivity is destroyed by phase fluctuations. We find that the Nernst effect has a much sharper temperature decay than predicted by Gaussian fluctuations, with an onset temperature that tracks Tc rather than the pairing temperature. We find a close quantitative connection with diamagnetism--the ratio of magnetization to transverse thermoelectric conductivity reaches a fixed value at high temperatures. We interpret measurements on underdoped cuprates in terms of a dilute vortex liquid over a wide temperature range above Tc. 相似文献
57.
We demonstrate that a flowing liquid jet can be controllably split into two separate subfilaments through the application of a sufficiently strong tangential stress to the surface of the jet. In contrast, normal stresses can never split a liquid jet. We apply these results to observations of uncontrolled splitting of jets in electric fields. The experimental realization of controllable jet splitting would provide an entirely novel route for producing small polymeric fibers. 相似文献
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June Cyriac Justin Paulose Mathai George Marupaka Ramesh Ragampeta Srinivas Daryl Giblin Michael L. Gross 《Journal of the American Society for Mass Spectrometry》2014,25(3):398-409
ESI-protonated 1,5-bis-(2-methoxyphenyl)-1,4-pentadien-3-one (1) undergoes a gas-phase Nazarov cyclization and dissociates via expulsions of ketene and anisole. The dissociations of the [M + D]+ ions are accompanied by limited HD scrambling that supports the proposed cyclization. Solution cyclization of 1 was effected to yield the cyclic ketone, 2,3-bis-(2-methoxyphenyl)-cyclopent-2-ene-1-one, (2) on a time scale that is significantly shorter than the time for cyclization of dibenzalacetone. The dissociation characteristics of the ESI-generated [M + H]+ ion of the synthetic cyclic ketone closely resemble those of 1, suggesting that gas-phase and solution cyclization products are the same. Additional mechanistic studies by density functional theory (DFT) methods of the gas-phase reaction reveals that the initial cyclization is followed by two sequential 1,2-aryl migrations that account for the observed structure of the cyclic product in the gas phase and solution. Furthermore, the DFT calculations show that the methoxy group serves as a catalyst for the proton migrations necessary for both cyclization and fragmentation after aryl migration. An isomer formed by moving the 2-methoxy to the 4-position requires relatively higher collision energy for the elimination of anisole, as is consistent with DFT calculations. Replacement of the 2-methoxy group with an OH shows that the cyclization followed by aryl migration and elimination of phenol occurs from the [M + H]+ ion at low energy similar to that for 1. Figure
The role of methoxy group in the Nazarov cyclization of 1,5-bis-(2-methoxyphenyl)-1,4-pentadien-3-one in the gas-phase and condensed phase by June Cyriac, Justin Paulose, M. George, Department of Chemistry, Sacred Heart College, Thevara, Cochin, Kerala, India-682013., M. Ramesh, R. Srinivas, National center for Mass Spectrometry, IICT, Hyderabad, India. Daryl Giblin and Michael L. Gross, Department of Chemistry, Washington University in St.Louis, St.Louis, USA, MO 63130. 相似文献