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91.
Natalini B Marinozzi M Sardella R Macchiarulo A Pellicciari R 《Journal of chromatography. A》2004,1033(2):363-367
The chromatographic resolution of enantiomeric amino acids is accomplished on a reversed phase column using aqueous mobile phase containing the chiral reagent N,N-dimethyl-S-phenylalanine-Cu(II). The separation is a result of the whole interaction between the diastereomeric complex surface and the mixed stationary phase realized by the dynamic coating of the RP-18 carbon chains layer. The elution order seems to be related to the different water coordination capability on copper ion in the formation of the mixed ternary complexes. 相似文献
92.
Nitro aromatic compound can be obtained in high yields via nitration of aromatic compound with wet carbon-based solid acid and NaNO_3 under solvent free oxidation at room temperature. 相似文献
93.
Effect of 1,10-phenanthroline on the extraction and separation of lithium(I), sodium(I) and potassium(I) with thenoyltrifluoroacetone 总被引:1,自引:0,他引:1
The extraction of Li+ with thenoyltrifluoroacetone (Htta) in the presence of 1,10-phenanthroline (phen) has been studied in various organic solvents. The remarkable enhancement of the extraction of Li+, that is a synergistic effect, was observed by the addition of phen, and the high extractability of Li+ was attained in toluene, benzene, chlorobenzene and o-dichlorobenzene. The extraction equilibrium of Li+, Na+ and K+ (denoted as M+) in the presence or absence of phen in chlorobenzene and the adduct formation reaction in the organic phase were studied in detail. The adduct of Li+ was Li(tta)(phen) in the wide concentration range of phen in the organic phase, while in Na+ and K+ M(tta)(phen)2 also exists in the high concentration region. The maximum value of the separation factor between Li+ and Na+ was observed in the present system and was larger than that in the Htta-trioctylphosphine oxide (TOPO)-benzene system reported previously. 相似文献
94.
Ramapanicker Ramesh 《Tetrahedron》2007,63(37):9153-9162
The base catalyzed cyclization of N-aryl and N-alkyl-O-propargyl carbamates is studied in detail. The effect of various bases and solvents on the efficacy of this cyclization reaction is analyzed and a new base-solvent system (LiOH in DMF) for effective cyclization of these carbamates is reported. A number of differentially substituted O-propargyl carbamates were cyclized to the corresponding 2-oxazolidinones under these conditions. The reaction conditions reported here are mild and no side reactions were observed in any of the substrates studied. A propargyl carbonate group was unaffected during the course of the cyclization of the O-propargyl carbamate group. The propargyl carbamates were prepared from the corresponding alkyl or aryl amines and the corresponding propargyl chloroformate, resulting in oxazolidinones diversely substituted at the nitrogen atom. N-Aryl-O-propargyl carbamates cyclized readily to the corresponding oxazolidinones with LiOH in DMF, whereas N-alkyl-O-propargyl carbamates reacted slowly under the same conditions. O-Propargyl carbamates substituted at the 1-position tend to cyclize faster whereas those substituted at 3-position cyclize considerably slower than the unsubstituted carbamates. 相似文献
95.
Summary In this study a new approach is presented for on-line radiometric detection in reversed phase LC of medium to low polarity
compounds labelled with14C.
The test compounds,14C-carbaryl and14C-parathion, are extracted post-column into a non-water miscible liquid scintillation cocktail. The segmented two-phase system
formed is introduced into the beta-detector without phase separation and collected in a capillary storage tube.
After completion of the LC separation and detection process, the direction of the flow in the storage system is reversed and
the segmented contents of the loop led at lower flow-rates through the beta-detector again. An enhanced signal, corresponding
to the increase in counting time is obtained without measurable peak broadening.
The lowest possible detection limit of the system is 9 counts per peak corresponding to subnanogram quantities of tested pesticides.
Calibration curves are linear over at least 2 orders of magnitude and have the expected theoretical slopes.
The reproducibility of the system is better than 4 % rel. S.D. An application to a recovery study of parathion shows the practical
potential of this technique.
Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984 相似文献
96.
Lämmerhofer M 《Journal of chromatography. A》2005,1068(1):3-30
Enantiomer separations by CE employing nonaqueous conditions are reviewed. The general focus of this article is directed towards solvent effects on chiral recognition and the separation mechanism. After a general discussion of solvent effects on the individual processes involved in CE enantiomer separation, specifics for various selector classes are discussed together with a few applications of enantioselective nonaqueous CE. 相似文献
97.
Solvent effects in a carbenoid N-H insertion route to triarylamines via 2-diazo-1,3-cyclohexanedione
Peter Livant 《Tetrahedron letters》2005,46(12):2113-2116
The Rh-carbenoid derived from 2-diazo-1,3-cyclohexanedione inserts into the N-H bond of arylalkylamines and diarylamines. A solvent for this reactive carbenoid is suggested. The insertion products undergo a Pd-mediated aromatization to afford alkyldiarylamines and triarylamines. 相似文献
98.
Ay?em Üzer 《Analytica chimica acta》2005,534(2):307-317
Contaminated land and groundwater remediation in military waste dumping sites often necessitates the use of simple, cost-effective, and rapid tests for detecting trinitrotoluene (TNT) residues in the field along with their dinitro-analogues. A simple, rapid, low-cost, and field-adaptable (on-site) colorimetric method was developed for quantifying TNT in the presence of RDX, PETN, picric acid, 2,4-DNT (dinitrotoluene), dinitrophenol, and dinitroaniline. Most commercialized methods for TNT assay-with the exception of Cold Regions Research and Engineering Laboratory of the U.S. Army (CRREL) method-use proprietary chemicals, and the color stability and intensity are highly dependent on the composition of the organic solution comprised of acetone or methanol. The developed colorimetric method is based on the extraction of TNT from water-acetone solution into an organic solvent mixture of dicyclohexylamine (DCHA)-isobutyl methyl ketone (IBMK) (10:1, v/v), filtration through a filter paper into a stoppered optical cell containing anhydrous sodium sulfate, and measurement of the absorbance of the organic extract at 531 nm after 5 min. The red-violet color of the extract was due to intermolecular charge-transfer (CT) between the electron attracting TNT and electron-donating DCHA, and the molar absorptivity for TNT in final organic solution was (1.16 ± 0.02) × 104 L mol−1 cm−1.The R.S.D. of the slope of calibration line was 0.7%. The LOD of the method in the final organic phase was 0.38 μM TNT, and LOD values expressed on the basis of original soil TNT content were 0.5, 1.3, and 1.5 ppm (μg g−1) for clay, loamy clay, and sandy soils, respectively. Unlike other spectrophotometric methods, the developed assay was basically tolerant to common cations and anions found in soil and water at 100-fold weight ratios, and to soil humic acids. Among a number of compounds that may be encountered in polynitro-explosive storage and waste reclaimation sites such as picric acid, dinitrophenol, 2,4-dinitrotoluene, dinitroaniline, RDX, PETN, and tetryl, only tetryl interfered with the developed TNT assay. Water tolerance and exploitability over a wide pH range were other superiorities over the CRREL method. The CT-complex was relatively stable, as the absorbance of the organic extract was not significantly influenced from the dilution of the water-acetone phase. Aside from the extractive-photometric procedure established for aqueous solutions, a simulated field colorimetric assay for TNT directly applicable to soil was also devised, based on direct color development in a 4:1 (v/v) acetone-dicyclohexylamine organic extract of soil at a liquid-to-solid ratio of 5 mL g−1. 相似文献
99.
Gerhard M. Schneider 《Angewandte Chemie (International ed. in English)》1978,17(10):716-727
The present review considers some physicochemical properties of fluid mixtures that are of importance for fluid extraction and supercitical fluid chromatography (SFC). Firstly, the important types of phase diagrams are treated, the occurrence of solid phases also being considered in some simple cases. Specific examples are given of mixtures of a highly volatile component I (e.g. CO2, C2H6) with a relatively involatile component II (e.g. squalane) of very different molecular size, shape, structure, and/or polarity, and it is shown how the rather complicated types of phase diagrams can be calculated and correlated. The importance of fluid mixtures extends far beyond the fields of science and technology reviewed. 相似文献
100.