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101.
Summary The only method recommended for the direct estimation of ferric iron in presence of HCl is to reduce the ferric iron to ferrous iron and then to titrate against KMnO4 solution by adding Reinhardt-Zimmermann reagent (MnSO4 + H2SO4 + H3PO4). The solubility of the phosphato complexes of ferric chloride and phosphoric acid is much reduced by adding a nonaqueous solvent, ethyl alcohol or acetone. This property has been availed of to find out a method of estimating ferric iron directly against standard solution of phosphoric acid in aqueous-nonaqueous medium using K4Fe(CN)6 or cupferron as external indicators. A slight discrepancy at the end point, however, exists in the direct titration but it can be removed by applying a correction factor determined from the estimated results.  相似文献   
102.
Summary A simple gas-liquid chromatographic method has been developed for determining 3-sulfolene in sulfolane. The method involves thermal decomposition of sulfolene and determination of the 1.3-butadiene evolved, by GLC. Influence of the operating parameters on quantitative decomposition of sulfolene has been studied. The accuracy of the method as studied in the concentration range from 0.05 to 4.0 % (w/v) of 3-sulfolene in sulfolane is found to be within ±3.0%. It is rapid and sensitive down to 10 ppm and has potentialities for on-line applications also.
Bestimmung von 3-Sulfolen in Sulfolan durch Reaktions-Gas-Chromatographie
Zusammenfassung Eine einfache gas-chromatographische Methode wurde entwickelt, die auf der thermischen Zersetzung der Probe und der Bestimmung des dabei aus 3-Sulfolen gebildeten 1,3-Butadiens beruht. Der Einfluß der einzelnen Parameter wurde untersucht. Innerhalb eines Konzentrationsbereichs von 0,05–4,0% 3-Sulfolen ergaben sich Fehler von ±3%. Das Verfahren ermöglicht bis herab zu 10 ppm eine schnelle und empfindliche Bestimmung und eignet sich auch zum on-line Betrieb.
  相似文献   
103.
Summary The effect of methylene blue under different conditions of pH, concentration and frequency of the a. c. ripple used has been investigated on the capacity of the dropping mercury electrode. All the peaks caused by methylene blue at different pH values have been interpreted as due to the reduction of the methylene blue, as indicated by the comprehensive study of the peaks. The halt at about 0.58 Volt at pH 5.8 is due to desorption which develops into a satellite peak if potassium nitrate is used as indifferent electrolyte. It is found that the peak at 1.35 Volt at pH 12.3, first increases with increase in concentration and then diminishes at still higher concentrations. The causes of this have been discussed. The effect of frequency reveals that the reduction reactions involved are rather slow.
Zusammenfassung Der Effekt von Methylenblau unter verschiedenen Verh?ltnissen von Wasserstoff-Ionen-Konzentration, Konzentration und Frequenz des überlagerten Wechselstroms auf die Kapazit?t der Quecksilbertropfelektrode war Gegenstand der Untersuchung. Alle dem Methylenblau zuzuschreibenden Maxima bei verschiedenen pH- Werten lassen sich interpretieren durch eine Reduktion des Methylenblau, wie die eingehende Untersuchung der Maxima zeigt. Der Konstanzbereich bei etwa 0,58 Volt und pH 5,8 ist einer Desorption zuzuschreiben, die ein Begleitmaximum entwickelt, wenn Kaliumnitrat als indifferenter Elektrolyt verwendet wird. Das Maximum bei 1,35 Volt und pH 12,3 w?chst zun?chst bei Steigerung der Konzentration und nimmt dann bei noch h?heren Konzentrationen wieder ab. Die Gründe hierfür werden diskutiert. Der Frequenzeffekt zeigt an, da? die Reduktionsreaktionen ziemlich niedrig sind.
  相似文献   
104.
Summary Thorium and zirconium can be quantitatively precipitated by quinaldinic acid atph 2.7 and 3, respectively. As the precipitates are of nonstoichiometric composition they are to be ignited to oxides. By this reagent thorium can be quantitatively separated from arsenic (As3+), mercury (Hg2+), rare earths, manganese, magnesium and alkaline earths and zirconium from all the aforesaid ions excepting rare earths which contaminate to a slight extent.  相似文献   
105.
106.
Magnesium formate dihydrate has been synthesized by the action of formic acid on anhydrous magnesium oxide. This product analysed as Mg(COOH)2 · 2H2O. Its mode of thermal decomposition has been studied by thermal methods of analysis including simultaneous DTA/mass spectrometry. Nitrogen adsorption surface area of the solid products at various stages of its decomposition have been obtained. X-Ray diffraction and scanning electron micrographs have also been used to interpret the results. The decomposition of magnesium formate took place in three stages, which includes a phase change, at 265°C. The endotherm at 430°C changed to an exotherm in the presence of air; it corresponded to the decomposition of a new anhydrous phase of magnesium formate. The effect of the sample holder and changing atmospheres on the DSC analysis has been investigated. A scheme is presented for the thermal decomposition.  相似文献   
107.
A dielectric study on polyacrylonitrile (PAN), poly-2-hydroxyethyl methacrylate (P-HEMA) and copolymers of acrylonitrile and HEMA in the temperature range 30–150° is reported. The loss peaks occur in the frequency region 0.1–100 kHz at temperatures between 110° and 140 for PAN. In copolymers of acrylonitrile with HEMA, these loss peaks were present although their positions on temperature scale and their peak heights depended on the HEMA content. For P-HEMA no relaxation peak was observed in this range of frequency and temperature. The results for copolymers compared with those for the homopolymers suggest that the loss peaks in PAN are due to molecular motion in amorphous regions.  相似文献   
108.
Clay from the Purmandal area of J&K State was separated into its different size fractions by the method of sedimentation and with Sharple's super centrifuge process. Dilatometric studies were performed on each clay fraction; the results obtained from the dilatation curves are discussed in detail. The results revealed that the finer fraction of clay is bentonitic in nature, whereas the other fractions are felsphatic and micaceous in nature.  相似文献   
109.
This paper describes a photometric assay procedure for the determination of small amounts of salicylamide in the presence of a variety of foreign substances. This method is based on the formation of a blue colored indophenol derivative from the reaction of salicylamide with N,2,6-trichloro-p-benzoquinoneimine.  相似文献   
110.
Equilibrium constants and enthalpies of hydrogen-bond formation of mcresol to various cyclic (crown) and acyclic polyethers have been determined in benzene solvent. Equilibrium constants indicated no evidence for an operative macrocyclic effect; the relationship between the increasing size of the equilibrium constant and the number of ether oxygens was rationalized with a simple statistical thermodynamic model. Enthalpies of interactions ranged between –19 and –23 kJ-mol–1. In agreement with PCILO calculations, enthalpies of interaction were essentially independent of the number of oxygen atoms in the ether; no significant difference in enthalpies of interaction between cyclic and acyclic ethers was found.  相似文献   
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