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81.
Determination of forchlorfenuron residues in watermelon by solid-phase extraction and high-performance liquid chromatography 总被引:1,自引:0,他引:1
A method using solid-phase extraction for cleanup, followed by high-performance liquid chromatography with ultraviolet detection (HPLC/UV), was developed for the determination of forchlorfenuron residues in watermelon. The pesticide is extracted from the sample with acidic acetonitrile, and the extract is loaded onto a primary-secondary amine (PSA) column. The pesticide is eluted with acetone and determined by HPLC/UV. The PSA column was found to provide effective cleanup, removing the greatest number of sample matrix interferences. The acetonitrile extraction followed by the PSA cleanup provided recoveries of >95%, coefficients of variation (precision) of <10%, and sensitivity of 0.005 mg/kg, in agreement with the directives for method validation in residue analysis. The proposed method was successfully used to determine forchlorfenuron residue levels and dissipation rates in watermelon grown in an experimental greenhouse in Beijing, People's Republic of China. 相似文献
82.
During the past decade, the radial x-ray diffraction method using a diamond anvil cell (DAC) has been developed at the X17C beamline of the National Synchrotron Light Source. The detailed experimental procedure used with energy dispersive x-ray diffraction is described. The advantages and limitations of using the energy dispersive method for DAC radial diffraction studies are also discussed. The results for FeO at 135?GPa and other radial diffraction experiments performed at X17C are discussed in this report. 相似文献
83.
Identification of human brain structures in MR images comprises an area of increasing interest, which also presents numerous methodological challenges. Here we describe a new knowledge-based automated method designed to identify several major brain sulci and then to define the frontal lobes by using the identified sulci as landmarks. To identify brain sulci, sulcal images were generated by morphologic operations and then separated into different components based on connectivity analysis. Subsequently, the individual anatomic features were evaluated by using fuzzy membership functions. The crisp decisions, i.e., the identification of sulci, were made by taking the maximum of the summation of all the membership functions. The identification was designed in a hierarchical order. The longitudinal fissure was extracted first. The left and right central sulci were then identified based on the left and right hemispheres. Next, the lateral sulci were identified based on the central sulci and hemispheres. Finally, the left and right frontal lobes were defined from the two hemispheres. The method was evaluated by visual inspection, comparison with manual segmentation, and comparison with manually volumetric results in references. The average Jaccard similarities of left and right frontal lobes between the automated and manual segmentation were 0.89 and 0.91, respectively. The average Kappa indices of left and right frontal lobes between the automated and manual segmentation were 0.94 and 0.95, respectively. These results show relatively high accuracy of using this novel method for human frontal lobe identification and segmentation. 相似文献
84.
Pallambins A (1) and B (2), two novel 19-nor-7,8-secolabdane diterpenoids with unprecedented tetracyclo[4.4.0(3,5).0(2,8)]decane skeletons, along with a pair of structurally related isomers, pallambins C (3) and D (4), were isolated from the Chinese liverwort Pallavicinia ambigua. Their structures with absolute configurations were determined by means of NMR, X-ray diffraction, and CD analyses. Their preliminary cytotoxicity to human cancer cells was also tested. 相似文献
85.
The utility of Diels–Alder derivatization with 4-phenyl-1,2,4-triazoline-3,5-dione (PTAD) for liquid chromatography/electrospray
ionization tandem mass spectrometry of conjugated linoleic acids (CLAs) was examined. PTAD rapidly reacted with the CLAs,
and the resulting derivatives were highly responsive in electrospray ionization mass spectrometry operating in the positive-ion
mode. The derivatives produced characteristic product ions during tandem mass spectrometry, which enabled the sensitive detection
[limit of detection 18 fmol (signal-to-noise ratio of 5)] and the identification of the conjugated diene position. The PTAD
derivatization also significantly increased the reversed-phase liquid chromatography separation selectivity for the most biologically
active CLA isomers: cis-9,trans-11-CLA and trans-10,cis-12-CLA. The PTAD derivatization was applied to analyses of food and biological samples; the major CLAs in milk and beef fat
samples were successfully identified, and trace amounts of CLAs in human saliva were detected with a simple pretreatment and
short analysis time. 相似文献
86.
87.
Wang J Mei J Hu R Sun JZ Qin A Tang BZ 《Journal of the American Chemical Society》2012,134(24):9956-9966
It has been difficult to decipher the mechanistic issue whether E/Z isomerization is involved in the aggregation-induced emission (AIE) process of a tetraphenylethene (TPE) derivative, due to the difficulty in the synthesis of its pure E and Z conformers. In this work, pure stereoisomers of a TPE derivative named 1,2-bis{4-[1-(6-phenoxyhexyl)-4-(1,2,3-triazol)yl]phenyl}-1,2-diphenylethene (BPHTATPE) are successfully synthesized. Both isomers show remarkable AIE effect (α(AIE) ≥ 322) and high fluorescence quantum yield in the solid state (Φ(F) 100%). The conformers readily undergo E/Z isomerization upon exposure to a powerful UV light and treatment at a high temperature (>200 °C). Such conformational change, however, is not observed under normal fluorescence spectrum measurement conditions, excluding the involvement of the E/Z isomerization in the AIE process of the TPE-based luminogen. The molecules of (E)-BPHTATPE self-organize into ordered one-dimensional nanostructures such as microfibers and nanorods that show obvious optical waveguide effect. BPHTATPE shows rich chromic effects, including mechano-, piezo-, thermo-, vapo-, and chronochromisms. Its emission peak is bathochromically shifted by simple grinding and pressurization and the spectral change is reversed by fuming with a polar solvent, heating at a high temperature, or storing at room temperature for some time. The multiple chromic processes are all associated with changes in the modes of molecular packing. 相似文献
88.
Tetramethylpyrazine (TMP) is one of the most important active ingredients of a Chinese herb Ligusticum wallichii Franchat, which is widely used for the treatment of cardiovascular diseases. Several factors may affect TMP exposure after topical administration, resulting in large variability and demanding further elucidation of drug distribution. This paper describes a new efficient reliable LC‐MS/MS assay for the determination of TMP in dermal microdialysate, where TMP was separated on an Agilent C18 column (3.5 µm, 100 mm × 2.1 mm i.d.) using a mixture of methanol, water and acetic acid (50:50:0.6, v/v/v) at a flow‐rate of 0.3 mL/min. The retention time was 1.89 min for TMP and 1.17 min for the internal standard (caffeine). Histological analysis confirmed an inflammatory response to the microdialysis probes and the presence of a collagen capsule. The membrane extraction efficiency (percentage delivered to the tissue space) for TMP was not altered through the implant lifetime. The validation and sample analysis results showed that the method is precise, accurate and well suited to support dermal microdialysis experiments. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
89.
Ruzicka BA Werake LK Xu G Khurgin JB Sherman EY Wu JZ Zhao H 《Physical review letters》2012,108(7):077403
We demonstrate a new, nonlinear optical effect of electric currents. First, a steady current is generated by applying a voltage on a doped GaAs crystal. We demonstrate that this current induces second-harmonic generation of a probe laser pulse. Second, we optically inject a transient current in an undoped GaAs crystal by using a pair of ultrafast laser pulses and demonstrate that it induces the same second-harmonic generation. In both cases, the induced second-order nonlinear susceptibility is proportional to the current density. This effect can be used for nondestructive, noninvasive, and ultrafast imaging of currents. These advantages are illustrated by the real-time observations of a coherent plasma oscillation and spatial resolution of current distribution in a device. This new effect also provides a mechanism for electrical control of the optical response of materials. 相似文献
90.
Dávalos JZ Herrero R Chana A Guerrero A Jiménez P Santiuste JM 《The journal of physical chemistry. A》2012,116(9):2261-2267
We have studied the energetics and structural properties of trans-cinnamic acid (CA), o-, m-, and p-coumaric acids (2-, 3-, and 4-hydroxycinnamic acids), caffeic acid (3,4-dihydroxycinnamic acid), ferulic acid (4-hydroxy-3-methoxycinnamic acid), iso-ferulic acid (3-hydroxy-4-methoxycinnamic acid), and sinapic acid (3,5-dimethoxy-4-hydroxycinnamic acid). The experimental values of Δ(f)H(m)°(g), determined (in kJ·mol(-1)) for CA (-229.8 ± 1.9), p-coumaric acid (-408.0 ± 4.4), caffeic acid (-580.0 ± 5.9), and ferulic acid (-566.4 ± 5.7), allowed us to derive Δ(f)H(m)°(g) of o-coumaric acid (-405.6 ± 4.4), m-coumaric acid (-406.4 ± 4.4), iso-ferulic acid (-565.2 ± 5.7), and sinapic acid (-698.8 ± 4.1). From these values and by use of isodesmic/homodesmotic reactions, we studied the energetic effects of π-donor substituents (-OH and -OCH(3)) in cinnamic acid derivatives and in the respective benzene analogues. Our results indicate that the interaction between -OCH(3) and/or -OH groups in hydroxycinnamic acids takes place without significant influence of the propenoic fragment. 相似文献