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991.
János?W?lfling Angéla?Magyar Gyula?SchneiderEmail author 《Monatshefte für Chemie / Chemical Monthly》2003,134(10):1387-1393
Summary. A new synthetic route was developed for the preparation of trans-3-hydroxy-16,17-seco-pregna-5,17(20)-dien-16-al, using Grob fragmentation as the key step. This seco-steroid contains a formyl group and an unsaturated side-chain in a sterically favourable position, and is therefore a promising starting material for the synthesis of novel condensed steroid heterocycles.Received March 22, 2003; accepted April 22, 2003
Published online September 25, 2003 相似文献
992.
Secondary or tertiary amines may be prepared from primary alcohols and primary or secondary amines by treating triphenylphosphine with N-bromosuccinimide (NBS) in the presence of the alcohol at low temperature, followed by addition of the amine and heating for about 1 h. The yield of amine is good to fair, decreasing sharply with sterically congested alcohols and starting amines. 相似文献
993.
E. Colacio-Rodríguez J. D. López-González J. M. Salas-Peregrin 《Journal of Thermal Analysis and Calorimetry》1983,28(1):3-9
Salts [XanH+]2[MCl
4
2-
] (where XanH+=protonated form of xanthine and M=Zn(II), Cd(II) and Hg(II) have been synthesized and studied by IR,1H-NMR, TG and DSC. The metal is not coordinated to the ligand and forms a salt-like structure. The cationic proton is on N(7). Thermal decomposition of these salts occurs in two steps: (i) dehalogenation and (ii) decomposition. Dehalogenation enthalpies have been calculated from DSC curves.
Zusammenfassung (XanH+)2(MCl 4 2- )-Salze (worin XanH+ die protonisierte Form von Xanthin bedeutet und M=Zn(II), Cd(II) oder Hg(II) ist) wurden synthetisiert und mit IR,1H-NMR, TG und DSC untersucht. In diesem Fall liegt keine Koordination des Metalls mit dem Liganden vor, und es bildet sich eine salzartige Struktur aus. Das kationische Proton ist an N(7) lokalisiert. Die thermische Zersetzung dieser Salze erfolgt in zwei Schritten: (i) Dehalogenisierung und (ii) Zersetzung. Dehalogenierungsenthalpien wurden aus DSC-Kurven berechnet.
- -, [XanH+]2[MCl 4 2– ], XanH+ — , M — , . , . . : . - .相似文献
994.
Ram Parkash S. C. Ahluwalia S. C. Sud R. N. Sahni R. C. Paul 《Monatshefte für Chemie / Chemical Monthly》1981,112(6-7):707-711
Heats solution of someLewis acids and bases in acetic anhydride have been determined and the following order of their relative strengths is proposed: SbCl5>SO3>SnCl4>TiCl4>AsCl3 and piperidine>
n-butylamine>potassium acetate>sodium acetate -picoline>quinoline. Heats neutralization of theseLewis acids and bases in acetic anhydride suggest that the major enthalpy change in these neutralization reactions is due to the combination of a proton and the (CH2COOCOCH3)-ion, resulting in the formation of acetic anhydride.
Lösungs- und Neutralisationswärmen von Lewis-Säuren und-Basen in Essigsäureanhydrid
Zusammenfassung Es wurden die Lösungswärmen einigerLewis-Säuren in Essigsäureanhydrid bestimmt und folgende Reihung nach ihrer relativen Stärke vorgeschlagen: SbCl5>SO3>SnCl4>TiCl4>AsCl3 und Piperidin> n-Butylamin>KAc>NaAc-Picolin>Chinolin. Die Neutralisationswärmen dieserLewis-Säuren und-Basen legen nahe, daß der Hauptanteil daran auf die Reaktion eines Protons mit (CH2–COOCOCH3)-zurückzuführen ist.相似文献
995.
The solubilization of benzo[a]pyrene by organic solvents (dioxane, toluene and dichloromethane) and a surfactant (Triton X-100) was investigated. These media were successfully used for the determination of benzo[a]pyrene using fluorescence detection, with excellent limits of detection and large linear analytical ranges. Benzo[a]pyrene was detected in coal washing waters using liquid chromatography with fluorescence detection. The stability of this compound in dioxane was also examined. 相似文献
996.
Burford N Ragogna PJ McDonald R Ferguson MJ 《Chemical communications (Cambridge, England)》2003,(16):2066-2067
Polyphosphorus dications have been synthesised and comprehensively characterised as diphosphine (dppe, dmpe and dpph) linked Ar2P+ Lewis acids (Ar = C6H5); this application of unique homoatomic coordination chemistry provides important building blocks for extended systems. 相似文献
997.
Rosés M 《Journal of chromatography. A》2004,1037(1-2):283-298
The measurement of pH in chromatographic mobile phases has been a constant subject of discussion during many years. The pH of the mobile phase is an important parameter that determines the chromatographic retention of many analytes with acid-base properties. In many instances a proper pH measurement is needed to assure the accuracy of retention-pH relationships or the reproducibility of chromatographic procedures. Three different methods are common in pH measurement of mobile phases: measurement of pH in the aqueous buffer before addition of the organic modifier, measurement of pH in the mobile phase prepared by mixing aqueous buffer and organic modifier after pH calibration with standard solutions prepared in the same mobile phase solvent, and measurement of pH in the mobile phase prepared by mixing aqueous buffer and organic modifier after pH calibration with aqueous standard solutions. This review discusses the different pH measurement and calibration procedures in terms of the theoretical and operational definitions of the different pH scales that can be applied to water-organic solvent mixtures. The advantages and disadvantages of each procedure are also presented through chromatographic examples. Finally, practical recommendations to select the most appropriate pH measurement procedure for particular chromatographic problems are given. 相似文献
998.
Zareen Ahkter Andrew J. Edwards Scott L. Ingham Jack Lewis Ana M. Martin Castro Paul R. Raithby Gregory P. Shields 《Journal of Cluster Science》2000,11(1):217-226
The reaction of the di-gold cation [Au2(dppx)]2+ with the heptanuclear cluster dianion [Os7(CO)20]2– affords the mixed metal cluster [Os7(CO)20{Au2(dppx)}] (x=m (1), e (2), b (3)). On standing, in solution, this complex undergoes decarbonylation to give the cluster [Os7(CO)19{Au2(dppx)}] (x=m (4), e (5), b (6)). The complexes have been characterised spectroscopically, and an X-ray structure determination of the dppm derivative shows that it contains a metal core based on an Os7 edge-bridged bicapped tetrahedron with the two
3-Au atoms capping adjacent triangular Os3 faces of the central tetrahedron. In an analogous reaction, the carbido anion [Os7(H)C(CO)19]– affords the neutral cluster [Os7C(CO)19{Au2(dppm)}] (7) when treated with [Au2(dppm)]2+ in the presence of base. 相似文献
999.
Földvári M. Kovács-Pálffy P. Nagy N. M. Kónya J. 《Journal of Thermal Analysis and Calorimetry》1998,53(2):547-558
Various cation-exchanged montmorillonites (Li+, Na+, Ba2+, Mg2+, Ca2+, Mn2+, Co2+, Cu2+, Ag+, Cd2+, Hg2+, Al3+, Pb2+ and NH4+)
were prepared from calcium montmorillonite and their properties were studied by means of X-ray diffraction and thermal analysis.
The two methods give information on the cation exchange in the interlayer space only. X-ray diffraction studies at room temperature
are mainly suitable for estimation of the exchange of cations of different valencies. At 500°C, when the structure is completely
collapsed, the d value of montmorillonite depends on the non-hydrated ionic radius of the interlayer cation, but the measurement
interval is limited for fine interpretation. The thermoanalytical method is suitable for a better distinction of different
exchangeable cations of higher hydration energy on the basis of the DTG or DDTG curve.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
1000.
Flory-Huggins theory of polymer solutions has been used to express the condition of extrema values in the total sorption, as well as the inversion point in the preferential adsorption parameters for termary polymer systems. Two approaches have been followed, the first considers the binary and ternary interaction parameters independent of polymer concentration and solvent composition. In the second one, this dependence has been introduced. Our attention is focused on the volume fraction of solvent mixture dependence of the above parameters, in order to confirm or not the coincidence between the extrema values and the inversion point. Several cosolvent and cononsolvent ternary polymer systems, have been used to test the validity of the equations obtained. Also, it has been verified, from an experimental point of view, that in cosolvent ternary polymer systems there is coincidence in both compositions while in cononsolvent ternary polymer systems, such coincidence does not appear. 相似文献