全文获取类型
收费全文 | 91773篇 |
免费 | 894篇 |
国内免费 | 425篇 |
专业分类
化学 | 33241篇 |
晶体学 | 847篇 |
力学 | 7092篇 |
数学 | 34065篇 |
物理学 | 17847篇 |
出版年
2023年 | 106篇 |
2021年 | 188篇 |
2020年 | 255篇 |
2019年 | 247篇 |
2018年 | 10533篇 |
2017年 | 10360篇 |
2016年 | 6496篇 |
2015年 | 1259篇 |
2014年 | 676篇 |
2013年 | 997篇 |
2012年 | 4560篇 |
2011年 | 11353篇 |
2010年 | 6163篇 |
2009年 | 6471篇 |
2008年 | 7316篇 |
2007年 | 9406篇 |
2006年 | 934篇 |
2005年 | 1938篇 |
2004年 | 2083篇 |
2003年 | 2448篇 |
2002年 | 1469篇 |
2001年 | 574篇 |
2000年 | 539篇 |
1999年 | 360篇 |
1998年 | 375篇 |
1997年 | 324篇 |
1996年 | 394篇 |
1995年 | 307篇 |
1994年 | 238篇 |
1993年 | 267篇 |
1992年 | 229篇 |
1991年 | 200篇 |
1990年 | 183篇 |
1989年 | 149篇 |
1988年 | 181篇 |
1987年 | 150篇 |
1986年 | 166篇 |
1985年 | 155篇 |
1984年 | 148篇 |
1983年 | 135篇 |
1982年 | 143篇 |
1981年 | 127篇 |
1980年 | 133篇 |
1979年 | 130篇 |
1978年 | 126篇 |
1977年 | 107篇 |
1976年 | 99篇 |
1975年 | 84篇 |
1974年 | 85篇 |
1973年 | 92篇 |
排序方式: 共有10000条查询结果,搜索用时 312 毫秒
991.
J. A. De Schutter F. De Croo G. Van der Weken W. Van den Bossche P. De Moerloose 《Chromatographia》1985,20(3):185-192
Summary A rapid and specific reversed-phase high-performance liquid chromatographic method (RPHPLC) is described for the determination of mebeverine hydrochloride in tablets. Elution was performed on an octyl silane column with a methanol-water mixture (75-25), containing 0.05% hexylamine as silanol-blocking agent, adjusted to pH 5.0 with phosphoric acid. The method gave accurate, precise and reproducible results. The mean recovery of the drug from six synthetic tablet mixtures was 100.0% with a relative standard deviation (RSD) of 0.94%. In order to test the specificity of the method, the interference of the degradation compounds of mebeverine hydrochloride and of the intermediates from the synthesis was investigated. None of them did interfere. By means of mass spectrometry and UV-spectrophotometry, the degradation compounds of mebeverine were identified as veratric acid and as 4-|ethyl-[2-(4-methoxyphenyl)-1-methylethyl]amino| 1-butanol. The stability study proved that mebeverine hydrochloride is very stable in tablets; the tablets still contain more than 95% of the declared drug potency after storage for more than one year at 50°C.Colofac; Duspatal; Duspatalin 相似文献
992.
Mikkelsen Ø Skogvold SM Schrøder KH Gjerde MI Aarhaug TA 《Analytical and bioanalytical chemistry》2003,377(2):322-326
Evaluation of different solid electrode systems for detection of zinc, lead, cobalt, and nickel in process water from metallurgical nickel industry with use of differential pulse stripping voltammetry has been performed. Zinc was detected by differential pulse anodic stripping voltammetry (DPASV) on a dental amalgam electrode as intermetallic Ni–Zn compound after dilution in ammonium buffer solution. The intermetallic compound was observed at –375 mV, and a linear response was found in the range 0.2–1.2 mg L–1 (r2=0.98) for 60 s deposition time. Simultaneous detection of nickel and cobalt in the low g L–1 range was successfully performed by use of adsorptive cathodic stripping voltammetry (AdCSV) of dimethylglyoxime complexes on a silver–bismuth alloy electrode, and a good correlation was found with corresponding AAS results (r2=0.999 for nickel and 0.965 for cobalt). Analyses of lead in the g L–1 range in nickel-plating solution were performed with good sensitivity and stability by DPASV, using a working electrode of silver together with a glassy carbon counter electrode in samples diluted 1:3 with distilled water and acidified with H2SO4 to pH 2. A new commercial automatic at-line system was tested, and the results were found to be in agreement with an older mercury drop system. The stability of the solid electrode systems was found to be from one to several days without any maintenance needed. 相似文献
993.
Oxide ceramic masses react to simple shearing with hardening (peptisation: increase in the shear stress with the shear deformation).
In the present study the correlation between the increase in the shear stress and the porosity, agglomeration processes and
the type of flow are analysed. For this purpose oxide ceramic masses are tested in a shear device especially developed for
pastes and analysed by rheometric experiments, NMR methods and particle size analysis. The results support the hypothesis
that structural changes (hardening, increase in the mean porosity) of the material during the peptisation mainly depend on
the magnitude and not on the kind of the energy input and thus of the type of flow. The fraction of bound (more generally,
the immobilised) water increases with the shear displacement. Also crushing of primary particles could be observed. Both the
crushing of solid particles causing an increased solid surface and the formation of a three-dimensional gel structure are
microscopic effects capable of resulting in the binding or retaining water. On a macroscopic scale these phenomena cause hardening.
Magnetic resonance imaging visualises flow-induced agglomerates, which form owing to the shear flow and increase the porosity
averaged over the whole sample. After the shear experiment rolls of paste can be seen which indicate that the general assumption
of a plane shear flow in the shear device is not warrantable.
Received: 19 July 2001 Accepted: 25 October 2001 相似文献
994.
Improving the catalytic activity of Candida antarctica lipase B by circular permutation 总被引:3,自引:0,他引:3
Lipases (EC 3.1.1.3) play an important role in asymmetric biocatalysis. Tailoring these enzymes to novel, unnatural substrates is one of the primary challenges of protein engineering. We have used circular permutation, the intramolecular relocation of a protein's N- and C-termini, to explore the effects of altered active site accessibility and protein backbone flexibility on the catalytic performance of lipase B from Candida antarctica (CALB). Our combinatorial approach identified 63 unique functional protein permutants of CALB, and kinetic analysis of selected candidates indicated that a majority of enzyme variants either retained or surpassed wild-type CALB activity on a series of standard substrates. Beyond the potential benefits of these tailor-made lipases as new catalysts for unnatural substrates, our study validates circular permutation as a promising general method for lipase engineering. 相似文献
995.
The non-linear dielectric effect (NLDE), that is the increase in the dielectric constant divided by the square of the applied field, is measured for a number of non-polar molecular liquids and for liquid xenon. The values of the NLDE are compared with results in the literature and with values predicted by theory. The agreement with other experiments is quite good, but with theory is very poor, the only exception being Liquid xenon, where agreement is good. A possible explanation is given. The prediction that the NLDE should increase strongly near the critical point due to the divergence of the isothermal compressibility could not be established by experiment. The conclusion is drawn that this failure is due to the reduction by the theory of second-order effects to first-order thermodynamic and molecular properties. 相似文献
996.
Abstract— The photobehavior of the ciliates Climacostomuum virens, Euplotes daidaleos and Paramecium bursaria associated with endosymbiotic green algae ( Chlorella sp.) was compared with that of aposymbiotic ciliates (ciliates free of algae) and with the always aposymbiotic Paramecium arcticum . The aposymbiotic ciliates showed step-up photophobic responses. The responses were more frequent and occurred at lower light intensities when the organisms contained endosymbiotic algae. In contrast, step-down photophobic responses and photoaccumulations, as well as photokinesis, were never observed in aposymbiotic cells. These responses could be found only in ciliates when endosymbionts were present with the exception of C. virens , which showed none of these photoresponses. 相似文献
997.
A high-performance thin-layer chromatographic (HPTLC) method is described for the determination of tributyltin compounds (bis(tri-n-butyltin) oxide, TBTO, and tri-n-butyltin naphthenate, TBTN) and their degradation products (dibutyltin and monobutyltin compounds). The organotin compounds are extracted from wood with ethanol containing 0.5% (v/v) of hydrochloric acid and the separation of the defferent kinds of organotin compounds is achieved by thin-layer chromatography. The sample spots are measured using a scanning densitometer after decomposing the organotin compounds to inorganic tin by ultraviolet irradiation and visualization of the spots with pyrocatechol violet. Applications of the method to detection and quantification of organotin compounds in preservative solutions, in recently impregnated wood, and in wood samples from five-year-old window frames are described. 相似文献
998.
W. Lautsch W. Broser W. Bandel W. Biedermann W. Gehrmann E. Schröder H. Gnichtel I. Zehmisch G. Kurth R. Krüger H. J. Kraege 《Colloid and polymer science》1954,138(3):129-142
Ohne Zusammenfassung
Die Arbeit wurde aus Mitteln des Marshall-Planes (ERP-Mittel) und mit Spenden aus dem „Fonds Chemie“ ausgeführt. Wir sprechen
den zust?ndigen Stellen für die Gew?hrung der Beihilfe unseren verbindlichsten Dank aus. Der Deutschen Forschungsgemeinschaft
danken wir für die überlassung einer Ultrazentrifuge, den Behring-Werken für die uns zur Verfügung gestellten Serumalbumin-
und -globulin-Pr?parate. 相似文献
999.
1000.
Equations between the differential order and the maximum of the fractional-order differential for the specified peak signals are developed based on the variation of the maximum of the specified peak signals at different orders. Also, equations between the differential order and the zero-crossing of the fractional-order differential of the specified peak signals are proposed according to the variation of the zero-crossing of the specified peak signals at different orders. Characteristic paramters of the Gaus- sian peak, Lorentzian peak, and Tsallis peak can be estimated using estimator I and estimator II which are obtained by the equations above. As a result, a new method is presented to resolve the overlapped peaks signal. Firstly, a fractional-order differential of the specified peak signals is obtained with the fractional-order differentiation filter. Then, characteristic paramters of the specified peak signals can be extracted using estimator I and estimator II. Finally, the Tsallis peak is used as a model to assign the overlapping peak signals correctly. Experimental results show that the proposed method is efficient and effective for the simulated overlapping peaks and detected overlapping voltammetric peak signals. 相似文献