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61.
The reaction of [Cp*MoCl(4)] with an excess of LiBH(4), followed by thermolysis with tellurium powder in toluene, afforded a tricapped cubane cluster, [(Cp*Mo)(4)B(4)H(4)(μ(4)-BH)(3)] (1), which represents an unprecedented metal-rich metallaborane cluster with a cubane core containing 58 cluster valence electrons (cve) and three metal-metal bonds. 相似文献
62.
A high-resolution diode laser spectrum of the 882-cm?1 band of s-tetrazine has been obtained. A complete rotational analysis of this band, incorporating quartic and sextic centrifugal distortion coefficients, has been carried out. The rotational constants A, B, and C have been determined with an accuracy better than 10?5 cm?1. The analysis has shown the band to be A-type and, on this basis, the vibrational assignment of this band has been revised from ν12 to ν14. 相似文献
63.
Spectrophotometric Determination of Rhenium(IV) with Thiocyanate,TX-100 and N,N′-Diphenylbenzamidine
A spectrophotometric method to determine rhenium(IV) at trace level is based on the extraction of Re(IV)-SCN? complex in sulphuric acid media with N,N′-diphenylbenzamidine(DPBA) in presence of a non-ionic surfactant triton X-100 (TX-100) in chloroform. The complex shows maximum absorbance at 435 nm with amolar absorptivity value of 4.24 × 104 L mol?1 cm?1 at an acidity range 3.5-6.5 M H2SO4. The method followed Beer's Law for the system Re(IV)-SCN?(TX-100)-DPBA upto 4.0 μg Re(IV) mL?1. The detection limit of the method is 5 ppb. None of the tested foreign ions, except molybdenum(VI), interfere with the determination of rhenium. The interference due to molybdenum could effectively be removed by prior precipitation with oxine. The effect of various analytical parameters on the extraction of the metal are discussed. 相似文献
64.
Srinu Tothadi Balakrishna R. Bhogala Asha R. Gorantla Tejender S. Thakur Ram K. R. Jetti Gautam R. Desiraju 《化学:亚洲杂志》2012,7(2):330-342
The crystal polymorphism of the anthelmintic drug, triclabendazole ( TCB ), is described. Two anhydrates (Forms I and II), three solvates, and an amorphous form have been previously mentioned. This study reports the crystal structures of Forms I ( 1 ) and II ( 2 ). These structures illustrate the uncommon phenomenon of tautomeric polymorphism. TCB exists as two tautomers A and B. Form I (Z′=2) is composed of two molecules of tautomer A while Form II (Z′=1) contains a 1:1 mixture of A and B. The polymorphs are also characterized by using other solid‐state techniques (differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA), PXRD, FT‐IR, and NMR spectroscopy). Form I is the higher melting form (m.p.: 177 °C, ΔHf=≈105±4 J g?1) and is the more stable form at room temperature. Form II is the lower melting polymorph (m.p.: 166 °C, ΔHf=≈86±3 J g?1) and shows high kinetic stability on storage in comparison to the amorphous form but it transforms readily into Form I in a solution‐mediated process. Crystal structure analysis of co‐crystals 3 , 4 , 5 , 6 , 7 , 8 , 9 , 10 , 11 further confirms the existence of tautomeric polymorphism in TCB . In 3 and 11 , tautomer A is present whereas in 4 , 5 , 6 , 7 , 8 , 9 , 10 the TCB molecule exists wholly as tautomer B. The DFT calculations suggest that the optimized tautomers A and B have nearly the same energies. Single point energy calculations reveal that tautomer A (in Form I) exists in two low‐energy conformations, whereas in Form II both tautomers A and B exist in an unfavorable high‐energy conformation, stabilized by a five‐point dimer synthon. The structural and thermodynamic features of 1 , 2 , 3 , 4 , 5 , 6 , 7 , 8 , 9 , 10 , 11 are discussed in detail. Triclabendazole is an intriguing case in which tautomeric and conformational variations co‐exist in the polymorphs. 相似文献
65.
Das DD Mahapatra R Pradhan J Das SN Thakur RS 《Journal of colloid and interface science》2000,232(2):235-240
Removal of hexavalent chromium from aqueous medium by using activated cow dung carbon was studied. Cow dung was carbonized and activated by treating with concentrated H(2)SO(4) followed by heating for 24 h at 120 degrees C. The extent of adsorption was studied as a function of pH, contact time, amount of adsorbent, concentration of adsorbate, and temperature. At lower pH (<3.5), the prepared sorbent was capable of removing approximately 90% Cr(VI) at 5 ppm concentration from aqueous synthetic solution. The dynamics of migration of the sorbate ions from the bulk onto the sorbent surface was studied and the results obtained under various experimental conditions were found to follow standard adsorption isotherms. The reaction kinetics was found to be of first order. Copyright 2000 Academic Press. 相似文献
66.
[reaction: see text] A new synthetic procedure for aminohalogenation of olefins has been developed for the preparation of vicinal haloamine derivatives in high yields by using Cu, Mn, or V catalysts with p-toluenesulfonamide (TsNH(2)) and N-bromosuccinimide (NBS) as nitrogen and bromine sources, respectively. Unprecedented regio- and stereoselectivity (anti:syn > 99:1) toward the aminohalogenation process is shown for olefinic substrates as well as transition metal catalysts. 相似文献
67.
The stability constants and the associated thermodynamic parameters of formation for the 1:1 binary complexes of Am3+, Cm3+ and Eu3+ with N-(2-hydroxyethyl) ethylenediaminetriacetate (HEDTA) and their 1:1:1 ternary complexes with HEDTA + NTA (nitrilotriacate) were determined by distribution ratio measurements using solvent extraction in aqueous solutions of I=0.10?mol?L?1 (NaClO4) at temperatures of 0?C45?°C. Formation of these complexes is favored by both the enthalpy (exothermic) and the entropy (endothermic) terms. Luminescence lifetime measurements with Cm and Eu were used to study the coordination environment of these complexes over a range of concentrations and pH values. In the binary complexes M(HEDTA), HEDTA is a hexadentate ligand with three waters of hydration, while in the ternary complexes M(HEDTA)(NTA)3? we propose that the HEDTA retaines hexadentate coordination with NTA binding via three sites, depending on the pH of the solution, with the observation that the complex may contain a single water of hydration. 相似文献
68.
Agostic interactions and weak hydrogen bonds to metal acceptors, M, are chemically and geometrically distinct, and this distinction must be maintained in the classification of new C-H...M interactions. 相似文献
69.
Amar Singh Singha Bhanu Priya Thakur 《International Journal of Polymer Analysis and Characterization》2014,19(2):115-123
Grafting of methyl methacrylate (MMA) onto delignified Grewia optiva fiber using ascorbic acid/H2O2 as an initiator was carried out under microwave irradiation. The effects of varying the microwave power, exposure time, and concentration of initiator and monomer of graft polymerization were studied to obtain maximum grafting percentage (26.54%). The experimental results showed that the optimal conditions for grafting were: exposure time, 10min; microwave power, 110 W; ascorbic acid concentration, 3.74mol/L × 10?2; H2O2 concentration, 0.97mol/L × 10?1; monomer concentration, 1.87mol/L × 10?1. The graft copolymers were characterized by Fourier transform-infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), and thermogravimetric analysis (TGA). 相似文献
70.
Prof. Daniel W. Armstrong Dr. Mohsen Talebi Nimisha Thakur Dr. M. Farooq Wahab Dr. Alexander V. Mikhonin Matt T. Muckle Dr. Justin L. Neill 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2020,132(1):198-202
We designed and demonstrated the unique abilities of the first gas chromatography–molecular rotational resonance spectrometer (GC-MRR). While broadly and routinely applicable, its capabilities can exceed those of high-resolution MS and NMR spectroscopy in terms of selectivity, resolution, and compound identification. A series of 24 isotopologues and isotopomers of five organic compounds are separated, identified, and quantified in a single run. Natural isotopic abundances of mixtures of compounds containing chlorine, bromine, and sulfur heteroatoms are easily determined. MRR detection provides the added high specificity for these selective gas-phase separations. GC-MRR is shown to be ideal for compound-specific isotope analysis (CSIA). Different bacterial cultures and groundwater were shown to have contrasting isotopic selectivities for common organic compounds. The ease of such GC-MRR measurements may initiate a new era in biosynthetic/degradation and geochemical isotopic compound studies. 相似文献