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101.
Efficiency in HPLC can be enhanced by increasing the column length and/or decreasing the particle size. The use of high temperature in HPLC has emerged as a valuable tool to overcome the increase in column backpressure when using small packing particles, as it allows for reduction in mobile phase viscosity. In this study, high plate count was obtained by coupling sub-2 ??m columns at elevated temperature to reduce the viscosity of the mobile phase, thus reducing the column backpressure. At 80 °C, up to three columns of 15 cm × 4.6 mm I.D. packed with 1.8 ??m particles could be coupled generating ~84,000 theoretical plates for the last eluting compound. The number of theoretical plates was increased on average by a factor of ~3.6 when three columns were coupled at 80 °C compared with one column at 30 °C. The relationships between separation efficiency and column length were examined using Van Deemter plots constructed at 30 °C and 80 °C for different column lengths. The advantages of using coupled columns in combination with elevated temperature for the environmental analysis were illustrated using test mixtures comprised of eight sulfonamides separated on one column at 30 °C and three coupled columns at 80 °C by isocratic elution. Sample clean up was carried out by employing solid-phase extraction (SPE) using Oasis HLB cartridges. The method developed was validated based on parameters such as linearity, precision, accuracy, detection and quantification limits. Recoveries generally ranged from 71.7 to 99% (with the exception of sulfanilamide), with standard deviations not higher than 4.7%. The detection limits of the method ranged from 0.6?C2 ??g L?1, while limits of quantification were in the range 2?C6.7 ??g L?1 with UV detection. 相似文献
102.
Wojciech Jankowski Maria Gdaniec Tadeusz Pooski 《Acta Crystallographica. Section C, Structural Chemistry》2006,62(8):o492-o494
The crystal structure of the title compound, benzamide–2,3,4,5,6‐pentafluorobenzoic acid (2/1), 2C7H7NO·C7HF5O2, consists of centrosymmetric hexameric supermolecules composed of four amide and two carboxylic acid molecules connected via O—H⋯O and N—H⋯O hydrogen bonds. No phenyl–perfluorophenyl π–π stacking interactions are observed in this cocrystal. 相似文献
103.
Christian Albrecht Christoph Wagner Kurt Merzweiler Tadeusz Lis Dirk Steinborn 《应用有机金属化学》2005,19(11):1155-1163
The platina‐β‐diketone [Pt2{(COMe)2H}2(µ‐Cl)2] ( 1 ) was found to react with monodentate phosphines to yield acetyl(chloro)platinum(II) complexes trans‐[Pt(COMe)Cl(PR3)2] (PR3 = PPh3, 2a ; P(4‐FC6H4)3, 2b ; PMePh2, 2c ; PMe2Ph, 2d ; P(n‐Bu)3, 2e ; P(o‐tol)3, 2f ; P(m‐tol)3, 2g ; P(p‐tol)3, 2h ). In the reaction with P(o‐tol)3 the methyl(carbonyl)platinum(II) complex [Pt(Me)Cl(CO){P(o‐tol)3}] ( 3a ) was found to be an intermediate. On the other hand, treating 1 with P(C6F5)3 led to the formation of [Pt(Me)Cl(CO){P(C6F5)3}] ( 3b ), even in excess of the phosphine. Phosphine ligands with a lower donor capability in complexes 2 and the arsine ligand in trans‐[Pt(COMe)Cl(AsPh3)2] ( 2i ) proved to be subject to substitution by stronger donating phosphine ligands, thus forming complexes trans‐[Pt(COMe)Cl(L)L′] (L/L′ = AsPh3/PPh3, 4a ; PPh3/P(n‐Bu)3, 4b ) and cis‐[Pt(COMe)Cl(dppe)] ( 4c ). Furthermore, in boiling benzene, complexes 2a – 2c and 2i underwent decarbonylation yielding quantitatively methyl(chloro)platinum(II) complexes trans‐[Pt(Me)Cl(L)2] (L = PPh3, 5a ; P(4‐FC6H4)3, 5b ; PMePh2, 5c ; AsPh3, 5d ). The identities of all complexes were confirmed by 1H, 13C and 31P NMR spectroscopy. Single‐crystal X‐ray diffraction analyses of 2a ·2CHCl3, 2f and 5b showed that the platinum atom is square‐planar coordinated by two phosphine ligands (PPh3, 2a ; P(o‐tol)3, 2f ; P(4F‐C6H4)3, 5b ) in mutual trans position as well as by an acetyl ligand ( 2a, 2f ) and a methyl ligand ( 5b ), respectively, trans to a chloro ligand. Single‐crystal X‐ray diffraction analysis of 3b exhibited a square‐planar platinum complex with the two π‐acceptor ligands CO and P(C6F5)3 in mutual cis position (configuration index: SP‐4‐3). Copyright © 2005 John Wiley & Sons, Ltd. 相似文献
104.
Tadeusz Rzezuchowski 《Set-Valued Analysis》1997,5(2):181-193
The solutions of differential inclusions staying at the boundary of attained sets are investigated using the contingent cones to attained sets. The possibility of recovering the starting point and the time which elapsed since the beginning is shown when some fragments of an attained set are known. 相似文献
105.
An implementation of the p‐version of the finite element method for solving two‐dimensional linear elliptic problems on a shared‐memory parallel computer
is analyzed. The idea is to partition the problem among the available processors and perform computations corresponding to
different elements in parallel. The parallelization is based on a domain decomposition technique using the Lagrange multipliers.
The numerical experiments carried out on the Sequent system indicate very high performance of the mixed finite element algorithm
in terms of attained speedups.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
106.
A general equation for calculating the limit of the ligand interference region with the non-stoichiometric copper sulphide single-crystal electrode is described. The critical ligand concentration can be computed for a preselected maximal error in copper(II) ion determinations. The effect of the composition of the electrode material is discussed. The experimental results for the chloride interference show good agreement with theoretical predictions. 相似文献
107.
Quasiregular mappings in even dimensions 总被引:39,自引:0,他引:39
108.
Dilithium tetrabromonickelate (II) as a source of soft nucleophilic bromide : Reaction with epoxides
Dilithium tetrabromonickelate (II) in THF serves as a source of “soft” nucleophilic bromide and reacts regioselectively with epoxides to give bromohydrins in high yield. 相似文献
109.
An isomorphism is established between eertain compact and noncompact formulations of Abelian gauge theory on a lattice. For weak coupling, the mass gap predicted by the Higgs mechanism is then established. 相似文献
110.
Three types of porous polymers containing different functional groups were synthesized as stationary phases for gas chromatography. The influence of functional groups in the copolymer skeletons on their selectivities was studied. To determine the selectivities of these copolymers, two procedures were applied: the selectivity triangle and the general selectivity. As a reference phase Porapak Q which does not contain any functional groups was used. 相似文献