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761.
Watchueng J Kamnaing P Gao JM Kiyota T Yeboah F Konishi Y 《Journal of chromatography. A》2011,1218(20):2929-2935
Paclitaxel was purified using high-performance displacement chromatography (HPDC) technique, but not by the mechanism of HPDC. On small scale, paclitaxel was extracted with methanol from dry needles of Taxus canadensis and was enriched by extracting with chloroform after removing water-soluble hydrophilic components and hexane-soluble hydrophobic components. Then, 93-99% purity of paclitaxel was obtained using the HPDC technique. On large scale, taxanes were enriched by solvent partitioning between acetic acid/MeOH/H(2)O and hexane and extracted with CH(2)Cl(2). Taxanes except paclitaxel were further removed by extracting with methanol-water-trifluoroacetic acid (1.0:98.9:0.1, v/v/v). Applying HPDC technique to water-insoluble substances is problematic as this method requires a highly aqueous solvent system. In order to overcome this incompatibility, a system was set up where paclitaxel, although in low concentration, was extracted by methanol-water-trifluoroacetic acid (10.0:89.9:0.1, v/v/v). Recycling the extracting solvent to ensure minimal volume, the extracted paclitaxel was adsorbed on a C(18) trap column. A C(18) column of 4.6mm internal diameter was then connected to the trap column. The HPDC technique was thus carried out using an isocratic acetonitrile-water-trifluoroacetic acid (30.0:69.9:0.1, v/v/v) mobile phase consisting of a displacer cetylpyridinium trifluoroacetate (3mg/mL). Paclitaxel was co-eluted with the displacer and spontaneously crystallized. The crystal (114mg) showed 99.4% purity and only 10% of paclitaxel in the starting crude extract was lost during the enrichment/purification processes. This large scale purification method was successfully applied to purify paclitaxel from Chinese yew in small scale, suggesting general applicability of the method. This is the first report of purifying a water-insoluble natural product using HPDC technique. 相似文献
762.
Dimethyl and bis[(trimethylsilyl)methyl] zirconium complexes ([OSSO]ZrR2) [4, R = Me; 5, R = CH2SiMe3] having [OSSO]-type bis(phenolato) ligand 1 based on the trans-1,2-cyclooctanediylbis(thio) core have been synthesized by the reactions of the corresponding dichloro zirconium complex 3 with 2 equiv. of MeMgBr and Me3SiCH2MgCl, respectively, in Et2O/toluene at −78 °C. The molecular structures of these complexes 3-5 were characterized by NMR spectroscopy, elemental analyses, and X-ray crystallography. 1H and 13C NMR data of complexes 3-5 exhibited that they took the C2-symmetry in solution in the NMR time scale. In the crystal structures of 3-5, each zirconium center lies at the center of a distorted octahedral coordination sphere with cis sulfur atoms and trans oxygen atoms, which adopts a cis-α [(Λ∗,S∗,S∗)] configuration. 相似文献
763.
Yutaka Mori Tomoya Yamauchi Masato Kanasaki Yusuke Maeda Keiji Oda Satoshi Kodaira Teruaki Konishi Nakahiro Yasuda Rémi Barillon 《Radiation measurements》2011,46(10):1147-1153
Chemical modification along ion tracks in PADC films has been studied by means of FT-IR spectrometry, which was exposed to proton and heavy ions of He, C, Ne, Ar, Fe, Kr and Xe with energies around the Bragg peaks. This study covers a wide region of the stopping power ranging from 10 to 10,000 keV/μm. Removal cross sections for the loss of ether and carbonate ester bonds are assessed for each ion, as a function of the stopping power. Chemical damage parameters like the damage density, the effective track core radius and the radiation chemical yields, G values (scissions/100 eV), for each bond are also derived. We have found anomalous dependence of these parameters on the stopping power. The G value for the loss of carbonate ester bond decreased from 20 for proton down to 5 for C and Ne ions, and then increased with atomic number of heavy ions up to 8 for Xe ion. Radial dose distribution for each ion has been also calculated. Results are discussed from the viewpoint of polymeric structure of PADC that consists of two parts with different radio-sensitivities. 相似文献
764.
Minoru Eto Toshiaki Fujimori Sven Bjarke Gudnason Kenichi Konishi Muneto Nitta Keisuke Ohashi Walter Vinci 《Physics letters. [Part B]》2008
We construct the general vortex solution in the color–flavor-locked vacuum of a non-Abelian gauge theory, where the gauge group is taken to be the product of an arbitrary simple group and U(1). Use of the holomorphic invariants allows us to extend the moduli-matrix method and to determine the vortex moduli space in all cases. Our approach provides a new framework for studying solitons of non-Abelian varieties with various possible applications in physics. 相似文献
765.
Isobe M Kuse M Tani N Fujii T Matsuda T 《Proceedings of the Japan Academy. Series B, Physical and biological sciences》2008,84(9):386-392
Symplectin is a photoprotein from a luminous squid, Symplectoteuthis oualaniensis. It has a luminous substrate, dehydrocoelenterazine (DCZ), linked through a thioether bond with a cysteine residue. We have proven the binding site of luminous substrate in symplectin by using an artificial analogue of DCZ, ortho-fluoro-DCZ (F-DCZ). F-DCZ-symplectin emitting strong blue light was reconstituted from apo-symplectin and F-DCZ. Proteolytic digestion of the reconstituted F-DCZ-symplectin afforded peptides including C(390)GLK-F-DCZ (amide), which was detected with a house assembled nano-LC-ESI-Q-TOF-MS. The chromo-peptide derived from the F-DCZ-symplectin after luminescence showed the lower molecular mass than that before the luminescence by 12 mass units, corresponding to the loss of one carbon atom upon emitting light. Thus, we have concluded that F-DCZ analogue binds to Cys390 in symplectin so as to emit light. 相似文献
766.
We theoretically study possible methods how to obtain imaging of magnetic atoms by use of photoelectron diffraction (PD). We propose a novel method to apply Daimon effect where PD peaks are rotated around forward focusing peaks. In usual circular dichroism, we simply use the difference of the PD intensities for different X-ray circular polarization. In contrast to this dichroism, we rather use the difference of the PD intensities for different circular polarizations but - is used for the – circular polarization only in the data handling. This technique allows us to obtain clear atomic image only of spin polarized atoms, and to distinguish magnetic atoms with up-spins from those with down spins. Some illustrative calculations demonstrate the potential use and also the limitation of this technique. 相似文献
767.
Dr. Yu Zhao Dr. Saikat Das Taishu Sekine Haruna Mabuchi Tsukasa Irie Jin Sakai Dan Wen Prof. Weidong Zhu Prof. Teng Ben Prof. Yuichi Negishi 《Angewandte Chemie (International ed. in English)》2023,62(13):e202300172
The unique structural characteristics of three-dimensional (3D) covalent organic frameworks (COFs) like high surface areas, interconnected pore system and readily accessible active sites render them promising platforms for a wide set of functional applications. Albeit promising, the reticular construction of 3D COFs with large pores is a very demanding task owing to the formation of interpenetrated frameworks. Herein we report the designed synthesis of a 3D non-interpenetrated stp net COF, namely TUS-64, with the largest pore size of all 3D COFs (47 Å) and record-low density (0.106 g cm−3) by reticulating a 6-connected triptycene-based linker with a 4-connected porphyrin-based linker. Characterized with a highly interconnected mesoporous scaffold and good stability, TUS-64 shows efficient drug loading and controlled release for five different drugs in simulated body fluid environment, demonstrating the competency of TUS-64 as drug nanocarriers. 相似文献