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991.
Devendra Kumar Uday Razdan Alka D. Gupta 《Journal of polymer science. Part A, Polymer chemistry》1992,30(7):1477-1487
Various melt-polymerizable bisimido-bisphthalonitrile polymer precursors were synthesized by the reaction of 4-aminophthalonitrile (4-APN) with bis(3,4-dicarboxyphenyl) dimethylsilane dianhydride (SIDA), 4,4′-hexafluoroisopropylidene diphthalic anhydride (6FDA), bis(3,4-dicarboxyphenyl)ether dianhydride (ODPA), and 3,3′, 4,4′-tetracarboxylichenzophen+ne dianhydride (BTDA) in an aprotic solvent. The synthesized monomers showed crystalline melting at 269 and 271°C. Elemental analysis, differential thermal analysis (DTA), infrared (IR), nuclear magnetic resonance (1H-NMR) and mass spectral studies were carried out to characterize the synthesized monomers. Thermogravimetric analysis (TGA) of the synthesized monomers showed their thermal stability at 410–400°C. A detailed study and NMR investigation of the first step of condensation reaction was carried out and indicated the formation of a transient charge transfer complex. Thermal cyclization of the formed intermediate, however, gave the required monomers. A preliminary study demonstrated that melt-polymerization of the synthesized monomers gave thermallystable, tough polymers. 相似文献
992.
Reaction of 1,3-thiazolidine-2-thione with tellurium(IV) in hydrobromic acid medium gave the hexabromotellurate, [C6H9N2S3]22+[TeIVBr6]2− (3). Reaction of 1-methylimidazoline-2-(3H)-thione (L″) with tellurium(IV), in hydrobromic acid medium, gave the mixed-ligand tellurium(II) complex [TeIIL″3Br]+Br− (4). The structures of [C6H9N2S3]22+[TeIVBr6]2− (3) and [TeIIL″3Br]+Br− were determined by single crystal X-ray diffraction methods. In 3 the unit cell contains [TeBr6]2− anions and two [C6H9N2S3]+ cations. There is no direct bonding between the metal atom and the cations. In the anion only slight angular deviations from the perfect octahedral geometry are observed. The lone pair of electrons on tellurium(IV) is found to be stereochemically inert. In the cation the two five-membered heterocyclic rings adopt different conformations. In complex 4, in the solid state, the planar [TeIIL″3Br]+ cation and Br− anion are held together by ionic interactions. In the cation, L″ is bonded to the central tellurium atom through the sulphur atom. 相似文献
993.
Matthew J. Hills Irmgard Kiewitt Kumar D. Mukherjee 《Applied biochemistry and biotechnology》1991,27(2):123-129
Lipase from rape (Brassica napus L., immobilized onto celite, catalyzes esterification and transesterification reactions in hexane. The activity of the lipase is stimulated up to 35 fold by the addition of water (1.3% w/v). The activity of the lipase in hydrolysis is about 8 times higher than in the esterification reactions in hexane. Interesteri-fication reactions between mono- and diacylglycerols and transesterification reactions of mono- and diacylglycerols with alcohols were also catalyzed at relatively high rates but transesterification/esterification of these acylglycerols with fatty acids was comparatively slow. In transesterification reactions, triacylglycerols reacted rather slowly. 相似文献
994.
A simple and rapid alkalimetric method for the determination of mercaptans through trithiocarbonic acid formation is described. The mercaptans are titrated in tert.-butanol in the presence of carbon disulphide with standard aqueous sodium hydroxide, with phenolphthalein as indicator. The -SH group is smoothly, rapidly and quantitatively transformed into the group under the specified conditions. The method has been extended to the analysis of mercaptan-carboxylic acid and mercaptan-trithiocarbonate mixtures. 相似文献
995.
An amperometric titration method is described for the determination of 1-5 mg of organic isothiocyanates, based on their quantitative reaction with n-butylamine in dimethylfonnamide to form N,N-disubstituted thioureas which are then titrated amperometrically in aqueous ammonia-ammonium nitrate buffer with silver nitrate (dropping mercury electrode at -0.56V). The end-point corresponds to a silver:thiourea ratio of 2:1, with precipitation of silver sulphide. The method is simple, accurate, widely applicable, and gives reproducible results. 相似文献
996.
Summary Silver can be separated as its Bismuthiol II complex from OsO4
4
2–
, Os4+, Ir4+, Ru3+, Rh3+ with thiosulphate or complexone III as the masking agent at a pH between 5 and 9. Au3+ can be kept in solution only by thiosulphate at a pH 8–9 and cyanide complexes palladium at a PH of about 6. Separation from platinum in presence of a mixture of tartaric acid and complexone III is possible only to a limited extent.Part VI see Z. analyt. Chem. 155, 86 (1957) 相似文献
997.
Summary Copper has been determined gravimetrically as its bis-salicylaldehyde-ethylenediamine complex of the composition C16H14O2N2 · Cu, dried at 100–120° C. The complex is completely precipitated in theph range of 10.5–13.5, adjusted with ammonia or caustic alkali. It is stable in presence of excess ammonia, 0.1 N alkali, ammonium salts and complexing agents as tartrate, citrate, sodium-thiosulphate, fluoride, thiourea, triethanolamine and EDTA. In presence of tartrate and ammonia the ions of alkali metals, alkaline earths, Ag+, Tl+, Tl3+, Pb2+, Cd2+, Co2+, Mn2+, Pd2+, Al3+, Cr3+, La3+, Ce3+, Au3+, Pt4+, Ti4+, Zr4+, Th4+, UO2
2+ and anions as VO3
–, MoO4
2–, WO4
2–, CrO4
2–, PO4
3–, AsO4
3– do not interfere. Ni2+ and Hg2+ are masked by tartrate, EDTA and ammonia; As3+, Sb3+ and Sn2+ are separated using fluoride as the complexing agent; at an alkalinity of 0.1 N caustic alkali in presence of tartrate As3+, Sb3+, Sn2+, Bi3+, Zn2+ and Fe3+ are separated. Fe3+ can also be separated using triethanolamine as the masking agent at aph of about 13.0. Copper can be separated from almost all the ions, thus affording a highly selective method for the determination of copper.
Part I: Singh, B. R., and S. Kumar: Z. analyt. Chem. 185, 211 (1962). 相似文献
Zusammenfassung Es wird eine gravimetrische Methode zur Bestimmung von Kupfer beschrieben, die auf der Bildung des Bis-salicylaldehyd-äthylendiaminkomplexes beruht. Dieser hat die Zusammensetzung C16H14O2N2 · Cu. Die Fällung wird imph-Bereich 10,5–13,5 (mit Ammoniak oder Alkalilauge eingestellt) vorgenommen und der Niederschlag bei 100°–120° C getrocknet. Der Komplex ist beständig in Gegenwart von überschüssigem Ammoniak, 0,1 n Alkali, Ammoniumsalzen sowie Tartrat, Citrat, Natriumthiosulfat, Fluorid, Thioharnstoff, Triäthanolamin und ÄDTA. In Gegenwart von Tartrat und Ammoniak stören nicht: Alkalien, Erdalkalien, Ag+, Tl+, Tl3+, Pb2+, Cd2+, Co2+, Mn2+, Pd2+, Al3+, Cr3+, La3+, Ce3+, Au3+, Pt4+, Ti4+, Zr4+, Th4+, UO2 2+ sowie VO3 –, MoO4 2–, WO4 2–, CrO4 2–, PO4 3– und AsO4 3+. Ni2+ und Hg2+ können mit Tartrat, ÄDTA und Ammoniak maskiert werden, As3+, Sb3+ und Sn2+ mit Fluorid. In 0,1 n ätzalkalischer Lösung in Gegenwart von Tartrat können As3+, Sb3+, Sn2+, Bi3+, Zn2+ und Fe3+ abgetrennt werden. Fe3+ kann ebenfalls mit Triäthanolamin beiph 13,0 maskiert werden. Das beschriebene Verfahren erlaubt somit eine Abtrennung des Kupfers von fast allen anderen Ionen.
Part I: Singh, B. R., and S. Kumar: Z. analyt. Chem. 185, 211 (1962). 相似文献
998.
Abstract— Triplet-and singlet-related photoprocesses of pyrene-1-aldehyde (PA) in various solvents have been investigated in detail using 337.1 and 355 nm laser flash photolysis in conjunction with time-correlated determination of fluorescence lifetimes (τF ) and steady-state photochemical and absorption-emission spectral measurements. In benzene, the lowest triplet of PA (43 < ET < 46 kcal/mol) has a lifetime of about 50 µs (τT ) and displays the absorption maximum at 443 nm with a maximum extinction coefficient (εmax ) of 21000 M -1 cm-1 ; the corresponding ketyl radical has a sharp absorption maximum at 428 nm (εmax ≥ 25000 M -1 cm-1 ). The quantum yields (φT ) of lowest triplet occupation are high in nonprotic solvents (0.6–0.8), decrease in protic solvents (alcohols) as the polarity of the latter is increased, and maintain a complementary relationship with the quantum yields (φF ) of fluorescence. Quantum yields (φPC ) of loss of PA due to photoreactions in some solvents have also been determined under conditions of steady irradiation at 366 nm; φPC is in the range 0.1–0.2 in electron-rich olefinic solvents such as cyclohexene and tetramethylethylene. These results concerning τF , τT , φF . φT and φPC as well as the effects of 1,2,4-trimethoxybenzene and 2,5-dimethyl-2,4-hexadiene as quenchers for fluorescence, triplet yield, and photochemistry are discussed in the light of possible state orders for PA in polar and nonpolar environments. 相似文献
999.
Kondapi A. Kumar Pathaneni Sivaswaroop Kanuri Jaganmohana Rao Panuganti V. K. Rao 《Transition Metal Chemistry》1987,12(5):441-444
Summary The oxidation of MnII by S2O8
2– to MnVII in phosphoric acid medium proceeds via a stable MnIII and MnIV species. The reaction is catalysed by Ag+ and exhibits first order dependence on [S2O8
2–], [Ag+] and, is independent of [MnII]. The [H+] has no significant effect on the reaction. It is observed that the PO4
3– ion stabilises the transient manganese(III) and manganese(IV) species by forming a stable and soluble phosphato-complexes. The activation parameters for the two stages of oxidation, namely MnII MnIV and MnIVMnVII at 25° C are Ea=52 ±4 kJ mole–1, S*=–57±2 JK–1 mole–1 and Ea =56±4 kJ mole–1, S*=–44±2 JK–1 mole–1, respectively. A mechanism consistent with the experimental observations is proposed.Presented at the National Symposium on Reaction Kinetics and Mechanism, Department of Chemistry, University of Jodhpur, Jodhpur, India, Nov. 15–18, 1986. 相似文献
1000.
Sandeep Kumar Singh Balkishen Razdan 《Journal of Dispersion Science and Technology》2013,34(6):771-777
The dynamics of morphological transition in amphiphillic systems such as self-nanoemulsifying drug delivery system (SNEDDS) has become an increasingly active field of research in colloidal science. The present contribution deals with the morphological transition of selected optimized SNEDDS formulations of glibenclamide, carvedilol, and lovastatin on progressive aqueous dilution using transmission electron microscopy. The study emphasizes the structural aspects of the systems and stresses the effect of aqueous dilution under which the systems transform from water-in-oil (L2) phase into bicontinuous structure and, finally, in oil-in-water (L1) nanodroplets. 相似文献