首页 | 本学科首页   官方微博 | 高级检索  
文章检索
  按 检索   检索词:      
出版年份:   被引次数:   他引次数: 提示:输入*表示无穷大
  收费全文   917篇
  免费   29篇
  国内免费   7篇
化学   696篇
晶体学   14篇
力学   12篇
数学   47篇
物理学   184篇
  2024年   5篇
  2023年   10篇
  2022年   33篇
  2021年   46篇
  2020年   26篇
  2019年   30篇
  2018年   45篇
  2017年   25篇
  2016年   47篇
  2015年   24篇
  2014年   39篇
  2013年   64篇
  2012年   65篇
  2011年   62篇
  2010年   37篇
  2009年   36篇
  2008年   27篇
  2007年   33篇
  2006年   36篇
  2005年   38篇
  2004年   32篇
  2003年   26篇
  2002年   31篇
  2001年   6篇
  2000年   15篇
  1997年   2篇
  1996年   6篇
  1995年   5篇
  1993年   5篇
  1992年   11篇
  1991年   4篇
  1990年   6篇
  1989年   2篇
  1988年   2篇
  1986年   3篇
  1984年   3篇
  1983年   6篇
  1982年   2篇
  1981年   3篇
  1980年   2篇
  1979年   2篇
  1978年   11篇
  1977年   3篇
  1976年   4篇
  1975年   7篇
  1974年   4篇
  1972年   7篇
  1971年   5篇
  1967年   2篇
  1958年   1篇
排序方式: 共有953条查询结果,搜索用时 500 毫秒
91.
A versatile isocratic reversed-phase liquid chromatographic/ultraviolet–visible detection method for simultaneous determination of all-trans-retinol and α-tocopherol in human serum was developed and validated after optimization of various chromatographic conditions and other experimental parameters. Analytes were separated on a Kromasil 100 RP18 (150 × 4.6 mm, 5 μm) analytical column protected by a Perkin Elmer RP18 (30 × 4.6 mm, 10 μm) guard cartridge. The mobile phase, methanol–water (96:04 v/v) was pumped at a flow rate of 2.2 mL min?1 and the column eluents were monitored at the wavelength of 292 nm using retinyl acetate (1.0 μg mL?1) as the internal standard for both analytes. Sample preparation was based on protein precipitation and stabilization with 2,6-bis(1,1-dimethylethyl)-4-methylphenol/ethanol and a two step extraction process using n-hexane followed by dichloromethane as extraction solvents. Sample size was kept 20 μL and separation of analytes was achieved in less than 7 min. The present method demonstrated acceptable values for specificity/selectivity, linearity within the expected concentration range, recovery, precision, sensitivity, stability of solutions, robustness, and system suitability specifications and tests. The method was used for monitoring all-trans-retinol and α-tocopherol concentrations in human serum samples and could also be applied to other sample matrices such as brain slices and cosmetic products if attention is paid to the extraction procedure.  相似文献   
92.
Colloidal ZnS quantum dots (QDs) are prepared by passing H2S gas through a solution of Zn(CH3COO)2 in acetonitrile. Photophysical properties are investigated using UV?CVisible and photoluminescence (PL) spectroscopy. The spectrum shows an absorption shoulder at 271 nm representing a band gap of 4.6 eV. The doping of ZnS QDs with Co, Cu, and a mixture of Co and Cu not only increased the band gap to 0.2 eV but also turns these otherwise colorless QDs to blue in color due to cobalt, and green due to Cu. The observed emission in the visible region suggests that the dopants may have induced additional excited states to the ZnS QDs. This absorbance in the visible region can be utilized in the optoelectronic applications.  相似文献   
93.
 Fluoxetine hydrochloride reacts with benzoyl peroxide and potassium iodide, after heating for 1 min at 30 °C, to give a blue colour having maximum absorbance at 570 nm. The reaction is selective for fluoxetine with 0.01 mg/mL as visual limit of quantitation and provides a basis for a new spectrophotometric determination. The colour reaction obeys Beer’s law from 0.1 mg/10 mL to 2.0 mg/10 mL of fluoxetine and the relative standard deviation is 0.68%. The qualitative assessment of tolerable amounts of other drugs is also studied. Received September 21, 1998. Revision September 10, 1999.  相似文献   
94.
Cobalt(II) complexes 1 or 2, catalyses the epoxidation of alkenes in the presence of molecular oxygen and 2-methylpropanal in high yields.  相似文献   
95.
Cyclic voltammetric behavior of anthraquinone in aqueous medium has been studied in presence of a non-ionic surfactant, Triton X-100 (TX-100) using sodium salt of anthraquinone-2-sulphonic acid (AQS) as the electro-active species. When cathodic potential is applied, the anthraquinone (AQ) group of AQS is reduced to its dianion. In the reverse scan, the oxidation of AQ2− gives AQ. The electrochemical behavior shows a profound influence from the dissolved state of TX-100 in aqueous media. Spectrophotometric results indicate interaction between AQ and TX-100. A CEC (chemical–electrochemical–chemical) mechanism with the electrochemical reaction coupled with preceding interaction of AQS with TX-100 and following protonation reaction of reduced AQ has been proposed.  相似文献   
96.
Graft copolymerization of low‐density polyethylene (LDPE) with a maleic anhydride (MAH) was performed using intermeshing corotating twin‐screw extruder in the presence of benzoyl peroxide (BPO). The LDPE/polyamide 6 (PA6) and LDPE‐g‐MAH/PA6 blends were prepared in a corotating twin‐screw extruder. The melt viscosity of the grafted LDPE was measured by a capillary rheometer. The grafted copolymer was characterized by Fourier transform infrared spectroscopy (FTIR) and scanning electron microcopy (SEM). The influence of the variation in temperature, BPO and MAH concentration, and temperature on the grafting degree and on the melt viscosity was studied. The grafting degree increased appreciably up to about 0.45 phr and then decreased continuously with an increasing BPO concentration. According to the FTIR analysis, it was found that the amount of grafted MAH on the LDPE chains was ~5.1%. Thermal analysis showed that melting temperature of the graft copolymers decreases with increasing grafting degree. In addition to this, loss modulus (E″) of the copolymers first increased little with increasing grafting and then obviously decreased with increasing grafting degree. Furthermore, the results revealed that the tensile strength of the blends increased linearly with increasing PA6 content. The results of SEM and mechanical test showed that the blends have good interfacial adhesion and good stability of the phase structure, which is reflected in the mechanical properties. © 2009 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 48: 267–275, 2010  相似文献   
97.
The use of high‐performance liquid chromatography/mass spectrometry (HPLC/MS) and proton nuclear magnetic resonance (1H NMR) spectroscopy for the kinetic analysis of acyl glucuronide (AG) isomerisation and hydrolysis of the 1‐β‐O‐acyl glucuronides (1‐β‐O‐AG) of phenylacetic acid, (R)‐ and (S)‐α‐methylphenylacetic acid and α,α‐dimethylphenylacetic acid is described and compared. Each AG was incubated in both aqueous buffer, at pH 7.4, and control human plasma at 37°C. Aliquots of these incubations, taken throughout the reaction time‐course, were analysed by HPLC/MS and 1H NMR spectroscopy. In buffer, transacylation reactions predominated, with relatively little hydrolysis to the free aglycone observed. In human plasma incubations the calculated rates of reaction were much faster than for buffer and, in contrast to the observations in buffer, hydrolysis to the free aglycone was a significant contributor to the overall reaction. A diagnostic analytical methodology based on differential mass spectrometric fragmentation of 1‐β‐O‐AGs compared to the 2‐, 3‐ and 4‐positional isomers, which enables selective determination of the former, was confirmed and applied. These findings show that HPLC/MS offers a viable alternative to the more commonly used NMR spectroscopic approach for the determination of the transacylation and hydrolysis reactions of these AGs, with the major advantage of having the capability to do so in a complex biological matrix such as plasma. Copyright © 2010 John Wiley & Sons, Ltd.  相似文献   
98.
A new type of electrohydrodynamic instability originally reported in nematic liquid crystal mixtures with positive dielectric anisotropy and as moderately thick samples is further studied. The ability of homogeneously aligned nematics with positive dielectric anisotropy, in the presence of a magnetic field, to exhibit Williams domains as a threshold effect is numerically investigated. The variation of the threshold voltage for domain formation and dielectric alignment with dielectric anisotropy is calculated theoretically and compared with the experimental results as moderately thick and thin samples.  相似文献   
99.
Industrial units play a significant role in atmospheric pollution. Industrial exhausts deteriorate the atmospheric quality causing unhygienic environment for the people working in the vicinity. This work presents a study of the longitudinal distribution of trace elements of the Sheikhupura industrial area. Three kinds of distribution patterns were observed and are discussed in detail. The results are based on the neutron activation analysis of 16 trace elements.  相似文献   
100.
Asphalt binder was modified by low-density polyethylene (LDPE) and ethyl vinyl acetate (EVA) polymers to investigate the structure–property relationships of polymer-modified asphalt (PMA). The PMA was prepared in a high-shear blender at 160 °C. The optimum blending time (OBT) for each polymer was determined following a separate investigation. OBT was influenced by Mw, MWD, and polymer structure. The influence of Mw of LDPE and vinyl acetate (VA) content of EVA on PMAs was studied by rheological tools. Polymer modification improved the rheological properties of base asphalt. EVA–PMAs were found to be less temperature sensitive than LDPE-modified asphalts. LDPE modification increased flow activation energy (Ea) but EVA modification decreased Ea. Both VA content and Mw of LDPE have influenced the storage stability of PMAs. The low-temperature properties of PMAs and short ageing tests were not influenced by polymer type. On the other hand, the high-temperature properties of PMAs were strongly influenced by Mw of LDPE and VA content of EVA. Overall, EVA with low VA content showed the best temperature resistance to high- temperature deformations, the highest upper service temperature as well as the best storage stability.  相似文献   
设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号