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991.
Xiao‐Hong Tian Chuan‐Feng Chen Prof. 《Chemistry (Weinheim an der Bergstrasse, Germany)》2010,16(27):8072-8079
Two pairs of novel triptycene‐derived calix[6]arenes 4 a , b and 5 a , b have been efficiently synthesized through both one‐pot and two‐step fragment‐coupling strategies starting from 2,7‐bis(hydroxymethyl)‐1,8‐dimethoxytriptycene 1 . Subsequent demethylation of 4 a , b and 5 a , b with BBr3 in dry dichloromethane gave the macrocyclic compounds 6 a , b and 7 a , b . Treatment of either 4 a or 6 a with AlCl3 resulted in the same debutylated product 8 , while 9 was similarly obtained from either 5 a or 7 a . Structural studies revealed that all of the macrocycles have well‐defined structures with fixed conformations both in solution and in the solid state owing to the introduction of the triptycene moiety with a rigid three‐dimensional (3D) structure, making them very different from their classical calix[6]arene counterparts. As a consequence, it was found that all of these the triptycene‐derived calix[6]arenes could encapsulate small neutral molecules in their cavities in the solid state. Moreover, it was also found that the macrocycles 4 b and 5 b showed highly efficient complexation abilities toward fullerenes C60 and C70, forming 1:1 complexes with association constants ranging from (5.22±0.20)×104 to (8.68±0.30)×104 M ?1. 相似文献
992.
993.
994.
In this paper a carbon ionic liquid electrode (CILE) was fabricated by using ionic liquid 1‐ethyl‐3‐methylimidazolium ethylsulphate ([EMIM]EtOSO3) as the modifier and further used as the working electrode for the sensitive anodic stripping voltammetric detection of Pb2+. The characteristics of the CILE were investigated by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). In pH 4.5 NaAc‐HAc buffer Pb2+ was accumulated on the surface of CILE due to the extraction effect of IL and reduced at a negative potential (‐1.20 V). Then the reduced Pb was oxidized by differential pulse anodic stripping voltammetry with an obvious stripping peak appeared at ?0.67 V. Under the optimal conditions Pb2+ could be detected in the concentration range from 1.0 × 10?8 mol/L to 1.0 × 10?6 mol/L with the linear regression equation as Ip(μA) = ?0.103 C (μmol/L) + 0.0376 (γ = 0.999) and the detection limit as 3.0 × l0?9 mol/L (3σ). Interferences from other metal ions were investigated and Cd2+ could be simultaneously detected in the mixture solution. The proposed method was further applied to the trace levels of Pb2+ detection in water samples with satisfactory results. 相似文献
995.
Zhi-Rong Tan Yao Chen Gan Zhou Shan Cao Xiang-Dong Peng Yi-Cheng Wang Xiu-Juan Peng Wei Zhang Hong-Hao Zhou 《Chromatographia》2010,72(11-12):1107-1113
A sensitive and specific liquid chromatography–electrospray ionization-tandem mass spectrometry method has been developed and validated for the identification and quantification of ursolic acid in human plasma using glycyrrhetic acid as an internal standard. The method involves extraction with methyl tert-butyl ether. The analyte was separated on a C18 column and analyzed in multiple reaction monitoring mode with a negative electrospray ionization interface using the [M–H]? ions, m/z 455.4 for ursolic acid and m/z 469.5 → m/z 425.5 for glycyrrhetic acid. The method was validated over the concentration range of 0.86–110.0 μg L?1. The intra- and inter-day precisions were less than 13.53% relative standard deviation (RSD) and the accuracy was within ?4.76% in terms of relative error (RE). The lower limit of quantification was 0.86 μg L?1 with acceptable precision and accuracy. There were almost no matrix effects. Recovery of ursolic acid from spiked drug-free plasma was higher than 68%. The method was used to study the pharmacokinetic profile of ursolic acid in human plasma after oral administration of Jieyu capsules. 相似文献
996.
The development of a two phase hollow fiber liquid-phase microextraction technique, followed by gas-chromatography-flame ionization detection (GC-FID) for the profiling of the fatty acids (FAs) (lauric, myristic, palmitic, stearic, palmitoleic, oleic, linoleic, linolenic and arachidic) in vegetable oils is described. Heptadecanoic acid methyl ester was used as the internal standard. The FAs were transesterified to their corresponding methyl esters prior to the extraction. Extraction parameters such as type of extracting solvent, temperature, extraction time, stirring speed and salt addition were studied and optimized. Recommended conditions were extraction solvent, n-tridecane; extraction time, 35 min; extraction temperature, ambient; without addition of salt. Enrichment factors varying from 37 to 115 were achieved. Calibration curves for the nine FAs were well correlated (r(2)>0.994) within the range of 10-5000 μg L(-1). The limit of detection (signal:noise, 3) was 4.73-13.21 ng L(-1). The method was successfully applied to the profiling of the FAs in palm oils (crude, olein, kernel, and carotino cooking oil) and other vegetable oils (soybean, olive, coconut, rice bran and pumpkin). The encouraging enrichments achieved offer an interesting option for the profiling of the minor and major FAs in palm and other vegetable oils. 相似文献
997.
Abstract
A 2D supramolecular compound [Co(phth)(phen) (H2O)3]·H2O has been synthysized by the reactions of Co(NO3)2·6H2O, 1, 10-phenanthroline(phen) and phthalate acid(H2phth) in NaOH solution with pH 7.0.The complex has been characterized by elemental analysis, IR, and single-crystal X-ray diffraction analysis which shows it belongs the monoclinic space group P2(1)/n, a = 7.571(2) ?, b = 13.737(3) ?, c = 20.015(4) ?, β = 95.56(1)°. V = 2071.9(8) ?3, Mr = 475.31, Dc = 1.524 g/cm−3, Z = 4, F(000) = 980, μ(MoKa) = 0.879 mm−1. The final R1 and wR2 are 0.0348 and 0.0711, respectively. The cobalt(II) ion is six-coordinated in a distorted octahedron to form a unit. Every unit is connected by hydrogen bonds forming 1D chain and 2D supramolecular network by π–π stacking interaction between adjoining chains. 相似文献998.
Syntheses,Structural Characterization and Thermoanalysis of Transition-Metal Compounds Derived from 3,5-Dinitropyridone 总被引:1,自引:0,他引:1
Rong Fan Qiu-Ping Zhou Guo-Fang Zhang Mei-Yu Cai Ping Li Li-Hua Gan Feng-Qi Zhao Ji-Zhen Li Xue-Zhong Fan Seik Weng Ng 《Journal of chemical crystallography》2010,40(3):266-271
Abstract
Nine metal compounds of Mn(II), Zn(II) and Cd(II) derived from dinitropyridone ligands (3,5-dinitropyrid-2-one, 2HDNP; 3,5-dinitropyrid-4-one, 4HDNP and 3,5-dinitropyrid-4-one-N- hydroxide, 4HDNPO) were characterized by elemental analysis, FT-IR and partly by TG-DSC. Three of which were further structurally characterized by X-ray single-crystal diffraction analysis. The structures of the three compounds, Mn(4DNP)2(H2O)4, 4, Zn(4DNPO)2(H2O)4, 8, and Cd(4DNPO)2(H2O)4, 9, crystallize in the monoclinic space group P2(1)/n and Z = 2, with a = 8.9281(9), b = 9.1053(9), c = 10.6881(11) Å, β = 97.9840(10)° for 4; a = 8.4154(7), b = 9.9806(8), c = 10.5695(8) Å, β = 97.3500(10)° for 8; a = 8.5072(7), b = 10.2254(8), c = 10.5075(8) Å, β = 96.6500(10)° for 9. All three complexes are octahedral consisting of four equatorial water molecules, and two nitrogen or oxygen donor ligands (DNP or DNPO). The abundant hydrogen-bonding and π-π stacking interactions seem to contribute to stabilization of the crystal structures of the compounds. The TG-DTG results revealed that the complexes showed a weight loss sequence corresponding to all coordinated water molecules, nitro groups, the breaking of the pyridine rings and finally the formation of metal oxides. 相似文献999.
1000.
A novel single-labeled fluorescent oligonucleotide (OND) probe for the detection of nanomolar mercury(II) ion in aqueous solution
is developed based on the inherent quenching of deoxyguanosines. The formation of hairpin structure of OND-Hg2+ complex brings deoxyguanosines close to dye, resulting in decreased dye fluorescence due to photoinduced electron transfer
from dye to deoxyguanosines. 相似文献