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981.
Three new thiosemicarbazides (1 a-c ) were prepared from N-[4-phenyl-5-(2-thienyl)-1,2,4-triazol-3-yl]mercaptoacetohydrazide. Reaction of (1 a-c) with the appropriate phenacyl bromide afforded thiazoline derivatives (2 a-i) whereas their reaction with chloroacetic acid or maleic anhydride gave the corresponding thiazolidine derivatives (3 a,b) and (4 a,b) . Cyclodesulfurization of (1 a-c) with DCCD in toluene yielded 5-substituted-amino-1,3,4-oxadiazoles (5 a,b) , while their dehydration with PPA gave the corresponding 5-substituted-amino-1,3,4-thiadiazoles (6 a-c) . Six representative compounds were tested for their in-vitro antimicrobial activity against some pathogenic microorganisms, some of them were proved to be active. 相似文献
982.
J. A. Navio M. Macias A. Justo C. Real 《Journal of Thermal Analysis and Calorimetry》1992,38(4):673-682
The thermal decomposition of sodium nitrite or nitrate pre-adsorbed upon TiO2 surfaces has been investigated by employing several techniques as infrared spectroscopy (IR) and temperature programmed desorption in conjunction with mass spectrometry analysis (TPD-MS) to study the features observed during these thermal decompositions. Differential thermal analysis (DTA) in combination with X-ray diffraction analysis (XRD) were used to investigate the possibility of a solid state chemical reaction between the solid products originated from the thermal decomposition of the pre-adsorbed species and the TiO2. On the basis of our results, various characteristic features of these thermal decomposition reactions will be discussed.This work was supported by JUNTA DE ANDALUCIA (financial support for research groups/1990). 相似文献
983.
An analytical method using alumina modified with water-soluble polyacrylic acid polymer for the simultaneous separation and
preconcentration of trace Cu and Cd in a column system, and their determination by flame atomic absorption spectrometry was
developed. The conditions for coating Al2O3 with polyacrylic acid were optimized, then the column was packed with 50 mg of this sorbent. Cd and Cu solution was passed
through a glass column at pH 4.5, and elution was carried out with 5 mL of 0.05 M HCl at a flow rate of 1 mL min−1. A sorption capacity of 10 mg Cu and 12 mg Cd was obtained for 1 g sorbent. The detection limit was calculated as 4.5 μg L−1 for Cu and 1.54 μg L−1 for Cd in the final solution. Enrichment factors of 300 for Cd and 400 for Cu were obtained. 相似文献
984.
M. J. Tiera V. A. De Oliveira H. D. Burrows M. Graça Miguel M. G. Neumann 《Colloid and polymer science》1998,276(3):206-212
The binding of the cations thallium(I), calcium(II) and terbium(III) to methyl methacrylate– methacrylic acid copolymers
with different fractions of acid groups (x) has been studied in aqueous solution at various pH values using the fluorescence of covalently bonded 9-vinyl anthracene
as a probe. In all cases, the extent of binding increases as a function of the charge of the polymer with either increasing
fraction of carboxylic acids or of pH. However, differences are observed in the behavior of the three cations. With Tl(I),
quenching of the anthracene group fluorescence is observed, indicating that the thallium(I) approaches the probe and suggesting
that the alkylanthracene is probably in a relatively polar region. Binding constants have been determined from anthracene
quenching data and from studies with the fluo-rescent-probe sodium pyrenetetra-sulfonate. Good agreement is obtained between
the two methods, and values for the binding constants increase from 250 to 950 M-1 as x increases from 0.39 to 1. It is suggested that the cation is held in the polyelectrolyte domain, partly by Debye–Hückel effects
and partly by more specific interactions. Stronger binding is found with calcium(II) and terbium(III), and in this case increases
in fluorescence intensity are observed on complexation due to the anthracene group being in a more hydrophobic region, probably
as a result of conformational changes in the polymer chain. In the former case the stoichiometry of the interaction was determined
from the fluorescence data to involve two carboxylate groups bound per calcium. Association constants were found using murexide
as an indicator of free calcium to vary from 8400 to 37 000 M-1 as x increases from 0.39 to 1. It is suggested that in this case specific calcium(II)–carboxylate interactions contribute to the
binding. With terbium(III), a greater increase in the probe fluorescence intensity was observed than with calcium, and it
is suggested that the interaction with the polymer is even stronger, leading to a more pronounced conformational change in
the polymer. It is proposed that the terbium(III) interacts with six carboxylic groups on the polymer chain, with three being
coordinated and three attracted by electrostatic interactions.
Received: 10 June 1997 Accepted: 24 October 1997 相似文献
985.
Marco Arfelli Giovanni Cossu Giulia Mattogno Carla Ferragina Maria Antonietta Massucci 《Journal of inclusion phenomena and macrocyclic chemistry》1990,9(2):161-170
X-ray photoelectron spectroscopy provides evidence that when [Cu(phen)2]2+(phen = 1,10-phenanthroline) is diffused between the layers of -zirconium phosphate, the complex species does not remain intact after intercalation, but some Cu-N bonds are broken, replaced with Cu-O bonds and the released nitrogen atoms can now interact with the PO3-OH groups of the host. XPS also provides evidence for coordination of the Cu2+ ions when they are diffused by ion exchange in the phenanthroline--zirconium phosphate intercalation compound. Although Cu2+ and phen are in a 1 : 1 molar ratio in the interlayer region of the host, so that a 1 : 1 coordination could be expected between the two species, the characteristic peaks of the uncoordinated phenanthroline, even though at a low intensity, are still present. The differences between the two Cu(II)-intercalation compounds are discussed. 相似文献
986.
987.
A. J. Berry D. E. Games I. C. Mylchreest J. R. Perkins S. Pleasance 《Journal of separation science》1988,11(1):61-64
A frit restrictor interface for capillary column supercritical fluid chromatography/mass spectrometry (SFC/MS) has been constructed and used for the analysis of high boiling point alkanes. Packed column SFC/MS is described using both a moving belt liquid chromatographic/mass spectrometric interface and a thermospray source in the filament-on mode. 相似文献
988.
I. I. Chuev S. M. Aldoshin E. G. Atovmyan D. B. Frolov A. N. Utenyshev 《Russian Chemical Bulletin》1996,45(4):851-855
N-Thenylidene- andN-(o-nitrobenzylidene)hydrazides of isonicotinic acid have been studied by X-ray structural analysis and IR spectroscopy. In the crystalline state, these molecules are linked through intermolecular N—H ... Npy hydrogen bonds. Carbonyl groups are not involved in intermolecular hydrogen bonds. However, it was found that the C=O group participates in an attractive interaction with the sulfur atom of the thiophene group. The energy of this interaction is comparable with the energies of intermolecular C=O ... H—N hydrogen bonds in amides.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 4, pp. 896–900, April, 1996. 相似文献
989.
Summary A gas chromatographic methodology with selective detection is presented for the analysis in wines and corks of pentachlorophenol residues, which are suspected to be the most likely precursors of some off-flavours described in several wine samples. After derivatisation, pentachlorophenol acetate residues were monitored by electrolytic conductivity detection and/or mass spectrometric detection in the selective ion mode at m/z 264 and 266. Recoveries varied from 80 to 96% for wine samples fortified with 5 to 100 g l–1 and from 83 to 91% for corks (fortified at 25 to 100 g kg–1). The proposed methodology allowed for a determination limit of g l–1 for wine and 10 g kg–1 for corks. 相似文献
990.
V. A. Saprykina V. I. Vinogradova R. F. Ambartsumova T. F. Ibragimov A. Sultankulov Kh. M. Shakhidoyatov 《Chemistry of Natural Compounds》2004,40(6):582-584
Several new derivatives were prepared by reaction of 3-alkylthio-5-chloroacetamido-1,2,4-thiadiazoles with cytisine.Translated from Khimiya Prirodnykh Soedinenii, No. 6, pp. 479–480, November–December, 2004.This revised version was published online in April 2005 with a corrected cover date. 相似文献