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71.
A simple,rapid and reliable liquid chromatography–mass spectrometry method for determination of methotrexate in human plasma and its application to therapeutic drug monitoring 下载免费PDF全文
Dan Wu Yixuan Wang Yan Sun Nian Ouyang Jun Qian 《Biomedical chromatography : BMC》2015,29(8):1197-1202
A simple, rapid and reliable liquid chromatography–electrospray ionization tandem mass spectrometry method was established and validated for the determination of methotrexate in human plasma. After a straightforward protein precipitation by acetonitrile–water (70:30, v/v), methotrexate (MTX) and p‐aminoacetophenone (used as internal standard, IS) were separated on a Column C18 column (50 × 2.1 mm, 3 µm; Column Technology, Fremont, CA, USA) using a gradient elution with mobile phase of acetonitrile and 0.03% acetic acid aqueous solution at a flow rate of 0.5 mL/min. The total chromatographic runtime was 5 min for each injection. Quantification detection was performed in a triple‐quadruple tandem mass spectrometer under positive mode monitoring the following mass transitions: m/z 455.3 → 308.3 for MTX and m/z 136.1 → 94.4 for IS. The calibration curve was linear over the range of 0.05–25.0 µmol/L with a lower limit of quantification of 0.05 µmol/L. The intra‐ and interday precisions were <5.2%, the accuracy varied from ?4.1 to 4.5%. The recovery was >94%. The LC‐MS/MS method showed an excellent agreement with the existing HPLC‐UV method using Passing–Bablok regression and Bland–Altman difference plot analysis. The validated LC‐MS/MS can be successfully applied to the routine therapeutic drug monitoring of MTX in clinical laboratories. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
72.
Zhang Menghua Zhang Yongfeng Ouyang Huimin Ma Changhui Cheng Xingong 《Nonlinear dynamics》2020,99(4):2727-2741
Nonlinear Dynamics - An adaptive integral sliding mode control (AISMC) method with payload sway reduction is presented for 4-DOF tower cranes in this paper. The designed controller consists of... 相似文献
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The Dieudonn-Manin classification theorem on φ-modules (φ-isocrystals) over a perfect field plays a very important role in p-adic Hodge theory. In this note, in a more general setting we give a new proof of this result, and in the course of the proof, we also give an explicit construction of the Harder-Narasimhan filtration of a φ-module. 相似文献
75.
Formation and dissociation of protonated cytosine–cytosine base pairs in i-motifs by ab initio quantum chemical calculations 下载免费PDF全文
Formation and dissociation mechanisms of C-C+ base pairs in acidic and alkaline environments are investigated, employing ab initio quantum chemical calculations. Our calculations suggest that, in an acidic environment, a cytosine monomer is first protonated and then dimerized with an unprotonated cytosine monomer to form a C-C+ base pair; in an alkaline environment, a protonated cytosine dimer is first unprotonated and then dissociated into two cytosine monomers. In addition, the force for detaching a C-C+ base pair was found to be inversely proportional to the distance between the two cytosine monomers. These results provide a microscopic mechanism to qualitatively explain the experimentally observed reversible formation and dissociation of i-motifs. 相似文献
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77.
Solid phase microextraction (SPME), a simple, fast and promising sampling technique, has been widely used for complex sample analysis. However, complex matrices could modify the absorption property of coatings as well as the uptake kinetics of analytes, eventually biasing the quantification results. In the current study, we demonstrated the feasibility of a developed calibration method for the analysis of polycyclic aromatic hydrocarbons (PAHs) in complex milk samples. Effects of the complex matrices on the SPME sampling process and the sampling conditions were investigated. Results showed that short exposure time (pre-equilibrium SPME, PE-SPME) could increase the lifetime of coatings, and the complex matrices in milk samples could significantly influence the sampling kinetics of SPME. In addition, the optimized sampling time, temperature and dilution factor for PAHs were 10 min, 85 °C and 20, respectively. The obtained LODs and LOQs of all the PAHs were 0.1–0.8 ng/mL and 1.4–4.7 ng/mL, respectively. Furthermore, the accuracy of the proposed PE-SPME method for milk sampling was validated by the recoveries of the studied compounds in two concentration levels, which ranged from 75% to 110% for all the compounds. Finally, the proposed method was applied to the screening of PAHs in milk samples. 相似文献
78.
正The Chang'E-3(CE-3)mission began with a smooth countdown and flawless launch on the Long March 3B rocket from the Xichang satellite launch center at 01:30 CST on December 2,2013.It landed on the northeastern Imbrium basin(340.49°E,44.12°N)at 21:11 CST on December 14,2013,and the Yutu rover was deployed from the lander the next morning at 04:35.The lander was equipped with a number of remote-sensing 相似文献
79.
Sandilya Garimella Xiaoyu Zhou Zheng Ouyang 《Journal of the American Society for Mass Spectrometry》2013,24(12):1890-1899
The understanding of the gas dynamics of the atmospheric pressure interface is very important for the development of mass spectrometry systems with high sensitivity. While the gas flows at high pressure (>1 Torr) and low pressure (<10–3 Torr) stages are relatively well understood and could be modeled using continuum and molecular flows, respectively, the theoretical modeling or numeric simulation of gas flow through the transition pressure stage (1 to 10–3 Torr) remains challenging. In this study, we used the direct simulation Monte Carlo (DMSC) method to develop the gas dynamic simulations for the continuous and discontinuous atmospheric pressure interfaces (API), with different focuses on the ion transfer by gas flows through a skimmer or directly from the atmospheric pressure to a vacuum stage, respectively. The impacts by the skimmer location in the continuous API and the temporal evolvement of the gas flow with a discontinuous API were characterized, which provide a solid base for the instrument design and performance improvement. Figure
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80.
The detection of layer‐by‐layer self‐assembly multilayer films was carried out using low‐temperature plasma (LTP) mass spectrometry (MS) under ambient conditions. These multilayer films have been prepared on quartz plates through the alternate assembling of oppositely charged 4‐aminothiophenol (4‐ATP) capped Au particles and thioglycolic acid (TGA) capped Ag particles. An LTP probe was used for direct desorption and ionization of chemical components on the films. Without the complicated sample preparation, the structure information of 4‐ATP and TGA on films was studied by LTP‐MS. Characteristic ions of 4‐ATP (M) and TGA (F), including [M]+?, [M‐NH2]+, [M‐HCN‐H]+, and [F + H]+, [F‐H]+, [F‐OH]+, [F‐COOH]+ were recorded by LTP‐MS on the films. However, [M‐CS‐H]+ and [F‐SH]+ could not be observed on the film, which were detected in the neat sample. In addition, the semi‐quantitative analysis of chemical components on monolayer film was carried out, and the amounts of 4‐ATP and TGA on monolayer surface were 45 ng/mm2 and 54 ng/mm2, respectively. This resulted the ionization efficiencies of 72% for 4‐ATP and 54% for TGA. In order to evaluate the reliability of present LTP‐MS, the correlations between this approach and some traditional methods, such as UV–vis spectroscopy, atomic force microscope and X‐ray photoelectron spectroscopy were studied, which resulted the correlation coefficients of higher than 0.9776. The results indicated that this technique can be used for analyzing the films without any pretreatment, which possesses great potential in the studies of self‐assembly multilayer films. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献