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971.
972.
Shi-Ji Xiao Xin-Xiang Lei Bing Xia Dan-Qing Xu Hong-Ping Xiao Hong-Xi Xu Fang Chen Li-Sheng Ding Yan Zhou 《Tetrahedron letters》2014
Two novel lignans, gymnothespirolignans A (1) and B (2), possessing a rare polycyclic spiro skeleton, were isolated from the endemic plant of Gymnotheca involucrata Pei. Their structures were determined by spectroscopic evidences and the absolute configurations were confirmed by single crystal X-ray diffraction analysis. Compounds 1 and 2 showed promising antiviral activities against RSV with an IC50 value of 31.87 and 17.51 μM, respectively. 相似文献
973.
A phosphine-mediated synthesis of trifluoromethyl substituted pyrrole derivatives was achieved. The method described here is very fast, operationally simple, and easily amenable to scale-up, and commercially available trifluoroacetic anhydride (TFAA) is used as the only trifluoromethyl source. A wide range of products were obtained with good yields under mild condition using this method. 相似文献
974.
Wen Zhou Xiao-Li Sun Lin Gu Fei-Fei Bao Xin-Xin Xu Chun-Yan Pang Zhi-Guo Gu Zaijun Li 《Journal of Radioanalytical and Nuclear Chemistry》2014,300(2):843-852
Three new mesoporous silica materials IL15SGs (HF15SG, TF15SG and DF15SG) doped with benzo-15-crown-5 and imidazolium based ionic liquids (C8mim+PF6 ?, C8mim+BF4 ? or C8mim+NTf 2 ? ) have been prepared by a simple approach to separating lithium isotopes. The formed mesoporous structures of silica gels have been confirmed by transmission electron microscopy image and N2 gas adsorption–desorption isotherm. Imidazolium ionic liquids acted as templates to prepare mesoporous materials, additives to stabilize extractant within silica gel, and synergetic agents to separate the lithium isotopes. Factors such as lithium salt concentration, initial pH, counter anion of lithium salt, extraction time, and temperature on the lithium isotopes separation were examined. Under optimized conditions, the extraction efficiency of HF15SG, TF15SG and DF15SG were found to be 11.43, 10.59 and 13.07 %, respectively. The heavier isotope 7Li was concentrated in the solution phase while the lighter isotope 6Li was enriched in the gel phase. The solid–liquid extraction maximum single-stage isotopes separation factor of 6Li–7Li in the solid–liquid extraction was up to 1.046 ± 0.002. X-ray crystal structure analysis indicated that the lithium salt was extracted into the solid phase with crown ether forming [(Li0.5)2(B15)2(H2O)]+ complexes. IL15SGs were also easily regenerated by stripping with 20 mmol L?1 HCl and reused in the consecutive removal of lithium ion in five cycles. 相似文献
975.
976.
Construction of a portable sample preparation device with a magnetic poly(methacrylic acid‐co‐ethylene dimethacrylate) monolith as the extraction medium and its application in the enrichment of UV filters in water samples 下载免费PDF全文
Jing Li Li Xu Qiong‐Wei Yu Zhi‐Guo Shi Ting Zhang Yan Liu 《Journal of separation science》2014,37(19):2732-2737
A portable sample preparation device with a magnetic polymer monolith as the extraction medium was constructed. The monolith was synthesized by polymerizing methacrylic acid and ethylene dimethacrylate around a cylindrical magnet. In this way, the monolith with a magnetic core could be readily attached to the extraction device by magnetism. The constructed device was evaluated for the enrichment of UV filters in water samples, followed by high‐performance liquid chromatographic analysis. The extraction efficiency for the targets was satisfactory with no matrix interference. Good linearities were obtained for the UV filters with the correlation coefficients >0.9986. The limits of detection and quantification for the UV filters were 0.3–0.8 and 1.0–2.4 ng/mL, respectively. The recoveries of the UV filters from the spiked water samples at the concentration of 100 ng/mL were 95.3–101.7%, with relative standard deviations <10%. Accordingly, the proposed portable device was demonstrated to be suitable for on‐site simultaneous sampling, purification, and preconcentration within a single step. 相似文献
977.
Peipei Qi Xiangyun Wang Xinquan Wang Hu Zhang Hao Xu Kezhi Jiang Qiang Wang 《Journal of separation science》2014,37(20):2955-2965
The computer‐assisted design and synthesis of molecularly imprinted polymers for the simultaneous capture of six carbamate pesticides from environmental water are reported in this work. The quantum mechanical computational approach was employed to design the molecularly imprinted polymers with carbofuran as template. The interaction energies between the template molecule and different functional monomers in various solvents were calculated to assist in the selection of the functional monomer and porogen. The optimised molecularly imprinted polymer was subsequently used as a class‐selective sorbent in solid‐phase extraction for pre‐concentration and determination of carbamates from environmental water. The parameters influencing the extraction efficiency of the molecularly imprinted solid‐phase extraction procedure were systematically investigated to facilitate the class‐selective extraction. For the proposed method, linearity was observed over the range of 2–500 ng/mL with the correlation coefficient ranging from 0.9760 to 1.000. The limits of detection ranged from 0.2 to 1.2 ng/mL, and the limit of quantification was 4 ng/mL. These results confirm that computer‐assisted design is an effective evaluation tool for molecularly imprinted polymers synthesis, and that molecularly imprinted solid‐phase extraction can be applied to the simultaneous analysis of carbamates in environmental water. 相似文献
978.
979.
Ming Xu Sandrine Frelon Olivier Simon Ryszard Lobinski Sandra Mounicou 《Analytical and bioanalytical chemistry》2014,406(4):1063-1072
A non-denaturating isoelectric focusing (ND-IEF) gel electrophoresis protocol has been developed to study and identify uranium (U)–protein complexes with laser ablation–inductively coupled plasma mass spectrometry (LA-ICP MS) and electrospray ionization mass spectrometry (ESI-MS). The ND-IEF-LA-ICP MS methodology set-up was initiated using in vitro U–protein complex standards (i.e., U–bovine serum albumin and U–transferrin) allowing the assessment of U recovery to 64.4?±?0.4 %. This methodology enabled the quantification of U–protein complexes at 9.03?±?0.23, 15.27?±?0.36, and 177.31?±?25.51 nmol U L?1 in digestive gland cytosols of the crayfish, Procambarus clarkii, exposed respectively to 0, 0.12, and 2.5 μmol of waterborne depleted U L?1 during 10 days. ND-IEF-LA-ICP MS limit of detection was 19.3 pmol U L?1. Elemental ICP MS signals obtained both in ND-IEF electropherograms and in size exclusion chromatograms of in vivo U–protein complexes revealed interactions between U- and Fe- and Cu-proteins. Moreover, three proteins (hemocyanin, pseudohemocyanin-2, and arginine kinase) out of 42 were identified as potential uranium targets in waterborne-exposed crayfish cytosols by microbore reversed phase chromatography coupled to molecular mass spectrometry (µRPC-ESI-MS/MS) after ND-IEF separation. Figure
The paper presents the development of a non-denaturating protocol for the separation of uranium-protein complexes by isoelectric focusing gel electrophoresis (ND-IEF) before their quantitative detection by Laser Ablation coupled to Inductively Coupled Plasma Mass Spectrometry. Potential protein targets of uranium are subsequently identified by liquid chromatography - electrospray mass spectrometry 相似文献
980.
Qi Zhang Yingxiang Du Jiaquan Chen Guangfu Xu Tao Yu Xiaoyi Hua Jinjing Zhang 《Analytical and bioanalytical chemistry》2014,406(5):1557-1566
Various chiral selectors have been utilized successfully in capillary electrophoresis (CE); however, the number of polysaccharides used as chiral selectors is still small and the mechanism of enantiorecognition has not been fully elucidated. Chondroitin sulfate D (CSD) and chondroitin sulfate E (CSE), belonging to the group of glycosaminoglycans, are linear, sulfated polysaccharides with large mass. In this paper, they were investigated for the first time for their potential as chiral selectors by CE. The effect of buffer composition and pH, chiral selector concentration, and applied voltage were systematically examined and optimized. A variety of drug enantiomers were resolved in the buffer pH range of 2.8–3.4 using 20 mM Tris/H3PO4 buffer with 5.0 % CSD or CSE and 20 kV applied voltage. A central composite design was used to validate the optimized separation parameters and satisfactory uniformity was obtained. As observed, CSE allowed satisfactory separation of the enantiomers of amlodipine, laudanosine, nefopam, sulconazole, and tryptophan methyl ester, as well as partial resolution of citalopram, duloxetine, and propranolol under the optimized conditions. CSD allowed partial or nearly baseline separation of amlodipine, laudanosine, nefopam, and sulconazole. The results indicated that CSE has a better enantiorecognition capability than CSD toward the tested drugs. Figure
Chiral separation of various drug enantiomers in CE with CSE (A) and CSD (B) as chiral selectors 相似文献