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111.
    
Zusammenfassung Es wird gezeigt, daß sich -Tocopherol nach der Reaktion mit Eisen(III)-chlorid maßanalytisch durch Direkttitration des gebildeten Eisen(II) mit Dichlorphenolindophenol in Gegenwart von Metaphosphorsäure bestimmen läßt. Der Zusatz eines reaktionsbeschleunigenden Mehrstoffgemisches aus Bernsteinsäure, Cyclohexan und o-Nitrobenzoesäure stellt den quantitativen Ablauf der Tocopheroloxydation in Methanol sicher. Arbeitsvorschrift und 2 Analysenbeispiele für Vitamin E und sein Acetat werden gegeben, ferner Beispiele für die einfach zu messende Kinetik der -Tocopherol/Eisen(III)-Reaktion in verschiedenen Systemen. Der Erfassungsbereich reicht von 10–200 ppm-Lösungen. Die Genauigkeit liegt im Mittel bei ± 0,5% des Sollwertes. Unterhalb 30 ppm sinkt sie auf ca. ±1%. Die Methode wird mit bekannten oxydimetrischen Verfahren verglichen.
Summary A simple procedure for the analysis of -tocopherol is described: -tocopherol in methanol is oxidized with ferric chloride in the presence of a system of catalysts, such as succinic acid, cyclohexane or aromatic nitro-compounds, especially o-nitrobenzoic acid. The content of ferrous salts formed during the oxidation is then assayed by titration with dichlorophenolindophenol-solution in the presence of metaphosphoric acid. 1 ml of the solution corresponds to 40 mcg of -tocopherol. Due to the titration of the intermediate ferrous salts, the method is also suited for the study of the kinetics of oxidation reactions. Examples are given. Solutions containing 10–200 ppm of -tocopherol can be analysed. The accuracy of the method is usually about±0.5%, in. the range below 30 ppm it is slightly higher (±1%).
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112.
Population ratios and polarization of the Na3P J fine structure states following far wing photon excitation of Na-noble gas collision pairs are studied with respect to the underlying interaction potentials and molecular coupling schemes. For this purpose spectral profiles of these quantities, i.e. its dependencies on excitation frequency, have been measured up to ±200 cm?1 detuning from the NaD lines for NaAr and NaHe under nearly single collision conditions. Comparing the measured population ratios with quantummechanical coupled channels calculations the Σ potential well depths differ considerably from results of model potential calculations. Large residualJ=3/2 alignment observed in the far wings disagrees with simple models assuming incoherent excitation and/or full adiabatic reorientation of the radiating dipole along straight trajectories. By comparison with Lewis model calculations, using realistic trajectories and decoupling radius, it is found instead, that realistic trajectories are constitutive for alignment after Σ-excitation (blue wing), whereas coherence between the2Π1/2 and2Π3/2 states determine primarily alignment after Π-excitation (red wing).  相似文献   
113.
The glow discharge may be powered by direct current (dc), radio frequency (rf) and pulsed discharge sources. Each has specific advantages and special features that should be considered by analysts using the various forms of glow discharge spectroscopy. This paper reviews some of the factors that contribute to the selection of a power source for the glow discharge.  相似文献   
114.
Expense and inconvenience have restricted the use of the filtered xenon are lamp (solar simulator) as a UV source for conducting large-scale animal studies. Because sunscreen immunoprotective levels are significantly affected by the UV power spectrum of the source it is imperative that a solar simulating source be used for accurate measurements of sunscreen protection levels that are relevant to human UV exposures from sunlight. However, relatively inexpensive sunlamps, e. g. the UVA-340, that emit a UV power spectrum similar to that of a solar simulator are available. Unlike FS-type UVB sunlamps, which have a significant amount of effective immunosuppressive nonsolar UV energy at wavelengths below 295 nm, the immunosuppression effectiveness spectrum of UVA-340 sunlamps was nearly identical to that of a solar simulator. The purpose of this study was to evaluate this sunlamp for conducting photoimmunological and sunscreen immune protection studies. Groups of C3H mice were exposed to a range of UVA-340 sunlamp doses (0.25 KJ/m2 to 20.0 KJ/m2) to establish a dose-response curve and determine the minimum immune suppression dose (MISD) for induction of local-type suppression of contact hypersensitivity (CH). The MISD, defined as the lowest UV dose given to produce ~50% suppression of the CH response in mice, was determined to be 1.0 kJ/m2 for UVA-340 sunlamps. Immune protection tests on four marketed sunscreen lotions (sun protection factors [SPF] 4, 8, 15 and 30) were then conducted with UVA-340 sunlamps using MISD as the endpoint. The immune protection factors for these sunscreens were equivalent to the level of protection predicated by their labeled SPF. These results are similar to those we have previously obtained using a solar simulator. We conclude from these data that the immunosuppressive effects of UVA-340 sunlamps are similar to those of a solar simulator; however, further studies are needed to determine if UVA-340, or similar, sunlamps are a viable alternative to the solar simulator for conducting large-scale animal experiments that require a relevant UV solar spectrum.  相似文献   
115.
Copolymers of methyl methacrylate and 3-oximino-2-butanone methacrylate (OM) were investigated as deep-UV and e-beam resists. Their increased sensitivity relative to PMMA (up to 50 times) was correlated with the radiation chemical yields of the volatile products and main chain scissions. The degradation of these copolymers, activated by the 3-oximino-2-butanone entity, is discussed in terms of energy absorption mechanisms and the subsequent scission reactions.  相似文献   
116.
117.
Zusammenfassung Eine dünnschichtchromatographische Trennung des Wismuts von einem Überschuß an Metallen der Schwefelwasserstoffgruppe wurde beschrieben. Als Laufmittel dient ein Gemisch von tert.-Butanol, Salzsäure und Wasser. Nach Absaugen der Sorptionsschicht wird das Wismut mit MDCM spektralphotometrisch bestimmt. Standardabweichung und Varianz des Verfahrens werden angegeben.
Summary A thin layer Chromatographic separation of the bismuth from an excess of metal ions of the hydrogen sulfide group is described. A mixture of tert. butanol, hydrochloric acid and water serves as mobile phase. After sucking off the sorption layer, the bismuth is determined spectrophotometrically with MDCM. The standard deviation and the variance of the procedure is given.

Résumé On décrit une séparation par Chromatographie en couche mince du bismuth de métaux en excès du groupe de l'hydrogène sulfuré. On utilise comme éluant un mélange de butanol tert., d'acide chlorhydrique et d'eau. Après aspiration de la couche de sorption, on dose par spectrophotométrie le bismuth par le MDCM. On communique l'écart-type et le coefficient de variation du procédé.
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118.
Zusammenfassung Die Darstellung von Mono-, Di- und Tri-Lithiumcyanurat durch Umsetzung von Cyanursäure mit LiOH bzw. Li2CO3 in hochsiedenden Alkoholen und durch lösungsmittelfreie Festkörperreaktion wird beschrieben. Die Festkörperreaktionen werden mit Hilfe thermoanalytischer Methoden untersucht. Die Reaktion mit LiOH erfolgt in zwei Schritten und ergibt bei 400°C. Trilithium-cyanurat. Unter denselben Bedingungen wird mit Li2CO3 nur Dilithium-cyanurat gebildet. Die Thermolyse von Trilithium-cyanurat bei 550°C liefert in hoher Ausbeute Lithiumcyanat und stellt somit eine einfache Methode zur Darstellung dieser Verbindung in wasserfreier Form dar.
Formation and thermolysis of lithium cyanurates (a simple preparation of anhydrous lithium cyanate)
The formation of mono-, di- and tri-lithium cyanurate by reaction of LiOH or Li2CO3 with cyanuric acid has been investigated as a solid state reaction and by using high boiling alcohols as reaction medium. For investigating the solid state reactions thermoanalytical methods were used. The reaction with LiOH proceeds in two steps yielding trilithium cyanurate at 400°C. Under the same conditions only dilithium cyanurate is formed by reaction with Li2CO3. Lithium cyanate is obtained in high yields by thermolysis of trilithium cyanurate at 550°C. This procedure is therefore a simple method in synthesizing pure anhydrous lithium cyanate.


Mit 3 Abbildungen

Herrn Univ.-Prof. Dr.O. Kratky zum 70. Geburtstag gewidmet.  相似文献   
119.
120.
Trypsin, leucine aminopeptidase, and carboxypeptidase B were separately immobilized on controlled pore glass and reacted with a dipeptide substrate in high concentrations of either acetone or 1-propanol. Hydrolytic activity was demonstrated and evidence for the possible synthesis of peptide polymer is presented. Directed synthesis using amino acids and blocked amino acids as substrates was not successful.  相似文献   
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