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991.
Dolores Bellido-Milla Anabel Oñate-Jaén Jose M. Palacios-Santander Dolores Palacios-Tejero María P. Hernández-Artiga 《Mikrochimica acta》2004,144(1-3):183-190
Many standard and official sample digestion procedures for trace metal determination are carried out in open vessels on hot plates. A new procedure for the determination of trace metals by flame atomic absorption spectrometry or inductively coupled plasmaatomic emission spectrometry in beer samples was developed to be performed in closed reactors assisted by microwaves. The results are compared with the ones obtained by other procedures by means of the analysis of the variance. The differences between the procedures are attributed to residual organic matter. Voltammetry, absorption molecular spectrophotometry and high pressure liquid chromatography with a photodiode array detector are used to study the nature of these residues. Nitrobenzoic acids, phenolic acids and other organic compounds are often present after digestion. The results obtained are related to the precision in metal determination by atomic spectrometry. The need for elaboration of certified reference materials for trace metals in beer is suggested. 相似文献
992.
The factors affecting host-guest complexation between the molecular container compound cucurbit[6]uril (CB6) and various guests in aqueous solution are studied, and a detailed complexation mechanism in the presence of cations is derived. The formation of the supramolecular complex is studied in detail for cyclohexylmethylammonium ion as guest. The kinetics and thermodynamics of complexation is monitored by NMR as a function of temperature, salt concentration, and cation size. The binding constants and the ingression rate constants decrease with increasing salt concentration and cation-binding constant, in agreement with a competitive binding of the ammonium site of the guest and the metal cation with the ureido carbonyl portals of CB6. Studies as a function of guest size indicate that the effective container volume of the CB6 cavity is approximately 105 A(3). It is suggested that larger guests are excluded for two reasons: a high activation barrier for ingression imposed by the tight CB6 portals and a destabilization of the complex due to steric repulsion inside. For example, in the case of the nearly spherical azoalkane homologues 2,3-diazabicyclo[2.2.1]hept-2-ene (DBH, volume ca. 96 A(3)) and 2,3-diazabicyclo[2.2.2]oct-2-ene (DBO, volume ca. 110 A(3)), the former forms the CB6 complex promptly with a sizable binding constant (1300 M(-1)), while the latter does not form a complex even after several months at optimized complexation conditions. Molecular mechanics calculations are performed for several CB6/guest complexes. A qualitative agreement is found between experimental and calculated activation energies for ingression as a function of both guest size and state of protonation. The potential role of constrictive binding by CB6 is discussed. 相似文献
993.
Concha-Graña E Turnes-Carou MI Muniategui-Lorenzo S López-Mahía P Fernández-Fernández E Prada-Rodríguez D 《Journal of chromatography. A》2004,1047(1):147-155
The scope of this work is the development of a rapid, reliable and sensitive method for the analysis of organochlorine pesticides from soils by pressurized liquid extraction (PLE). The effect of four parameters (temperature, pressure, static time and cell volume) on the extraction efficiency was studied. The great extracting power of the PLE causes the extraction of numerous interfering substances, so a more efficient purification of this extract was necessary. In this work several sorbents have also been assayed to carry out the purification of soil samples: Florisil, silica, alumina, carbon, as well as combinations of them. Finally, the proposed analytical method was validated using a certified reference soil material (CRM804-050) and the results were compared with those obtained by other extraction techniques (Soxhlet and microwave-assisted extraction). 相似文献
994.
Procedures are proposed for the determination of phosphorus and silicon in the ppM range, by extraction of phosphomolybdic and silicomolybdic acids with organic solvent, decomposition of the complex and spectrophotometric determination of its molybdenum content. 相似文献
995.
Summary There were studied the process of styrene polymerization in PVC swollen surface layer initiated by free radicals generated under the action of chemical potential gradient as an external force. It was found that conversion of styrene into the block copolymer is an diffusion controlled process.
Dedicated to ProfessorV. Kellö in celebration of his 60th birthday. 相似文献
Zusammenfassung Die Initiation des Prozesses der Polymerization von Styrol in den Oberflächenquellungsschichten von PVC wurde untersucht.Dabei wurde festgestellt, daß die freien Radikale, welche bei Zerreißung von spannungsbeanspruchten Bindungen, wie sie durch Einfluß von äußeren Kräften auf den Gradienten des chemischen Potentials des Quellungsmittels an Oberflächenquell bildungsmittel Polymer entstehen können, Polymerizationsprozesse des olefinischen Quellungsmittels initiieren können.
Dedicated to ProfessorV. Kellö in celebration of his 60th birthday. 相似文献
996.
The electronic spectra of tetrathiotetracene (TTT) and of its mono- and dipositive ions have been calculated by the Pariser-Parr-Pople (PPP) method. Furthermore, the band polarizations of the first two bands of TTT have been measured. A reasonable band assignment is given using a new set of PPP parameters based on spectral data of a naphthalene derivative containing similar typical weak S-S bond. Other physical parameters as ionization potential, disproportionation energy, S-S bond length and net π-charges are discussed. 相似文献
997.
An isotope analytical method for the simultaneous determination of35S and14C in double-labelled organic compounds by liquid scintillation counting is described. The sample is burned in a stream of
oxygen. Sulfur oxides are converted to sulfuric acid and separated from other combustion products, including carbon-14 dioxide,
on a heated quartz wool column previously wetted with hydrogen peroxide. Carbon dioxide is collected from the gas stream by
an absorbent suitable for liquid scintillation counting. The residual sulfuric acid is rinsed off the column with water and
the aqueous solution obtained is mixed with a liquid scintillation cocktail for radioactivity measurement. The final solutions
ready for counting are obtained in less than fifteen minutes, quantitative collection recovery is achieved and no cross contamination
occurs. 相似文献
998.
L. A. Sáenz-Carbonell I. E. Maldonado-Mendoza O. Moreno-Valenzula R. Clau-Uitz M. López-Meyer C. Oropeza V. M. Loyola-Vargas 《Applied biochemistry and biotechnology》1993,38(3):257-267
The release of alkaloids from root culturesDatura stramonium andCatharanthus roseus and thiophenes from root cultures ofTagetes patula was found to increase when the pH of the culture media (ranging from 4.8 to 7.0) was reduced to 3.5. The extent of the effect
was different in each type of culture. Increases ranged from 4- to 20-fold, which in some cases accounted for 75% of the total
secondary metabolite pool produced per flask. When the release of individual metabolites was measured, even larger increases,
were observed (nearly 400-fold for ajmalicine). Increased release of alkaloids fromC. roseus roots were also observed in cultures growing in a 14-L fermentor, when the medium pH was reduced. Reduction of the pH of
the media did not affect growth of the root cultures in subsequent subcultures. The importance of this treatment as a stategy
to improve the recovery of secondary metabolites from producing cultures is discussed. 相似文献
999.
Tomás Pérez-Ruiz Carmen Martínez-Lozano Virginia Tomás Antonio Sanz Jesús Martín 《Fresenius' Journal of Analytical Chemistry》1998,362(4):399-403
A flow-injection configuration is proposed for the fluorimetric determination of ethylenethiourea. The procedure is based
on the inhibitory effect of ethylenethiourea on the oxidation of thiamine to thiochrome by mercury(II). A linear calibration
graph was obtained between 0.1 and 2.0 μg mL–1, with a sampling rate of 40 samples per hour and a relative standard deviation of about 1.11%. The usefulness of the method
was tested for the determination of ethylenethiourea residues in water, milk, potatoes, pear, grape and apple.
Received: 26 January 1998 / Revised: 6 April 1998 / Accepted: 9 April 1998 相似文献
1000.
M. Pyldme é. Buzágh-Gere J. Pyldme M. Veiderma 《Journal of Thermal Analysis and Calorimetry》1976,10(2):195-204
The thermal reactions between Maardu (Estonia) phosphorite and acidic phosphates were investigated. TG, DTG and DTA of mixtures with H3PO4, Ca(H2PO4)2 · H2O, Ca2P2O7 and [Ca(PO3)2]n in different molar ratios showed a maximum mass loss when the CaO P2O5 value was 2. The main temperature ranges of the mass losses were determined. The probable reactions relating to the mass losses are given on the basis of the thermal curves and IR spectra.
Zusammenfassung Die thermische Reaktion zwischen Phosphorit aus Maardu (Estnien) und sauren Phosphaten wurde untersucht. TG, DTG und DTA von Gemischen mit H3PO4, Ca(H2PO4)2 · H2O, Ca2P2O7 und [Ca(PO3)2]n in verschiedenen molaren VerhÄltnissen zeigten den grö\ten Massenverlust bei dem VerhÄltnis von CaO P2O5=2. Die wichtigsten Temperaturbereiche der Massenverluste wurden bestimmt. Die den Massenverlusten zugeordneten wahrscheinlichen Reaktionen werden aus den erhaltenen thermischen Kurven und IR Spektren ermittelt.
Résumé Etude de l'effet thermique lié à la réaction entre la phosphorite de Maardu (Estonie) et les hydrogénophosphates. Etude par TG, TGD et ATD de mélanges de H3PO4 avec Ca(H2PO4)2 · 2 H2O, Ca2P2O7 et [Ca(PO3)2]n réalisés avec différents rapports molaires; mise en évidence d'une perte de masse maximale pour le rapport CaO P2O5 égal à deux. Détermination des principaux domaines de température où s'effectuent les pertes de masse. On donne les réactions probables correspondant aux pertes de masse en s'appuyant sur les courbes d'analyse thermique et spectres infrarouges.
() . TG, DTG DTA H3PO4, Cc(H2PO4)2. H2O, Ca2P2O7 [Ca(PO3)2] n , CaOP2O5 2. . , .相似文献