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871.
S. Nygren 《Journal of separation science》1979,2(6):319-323
The technique of programming the carrier gas flow rate in gas chromatography, especially in connection with the use of capillary columns shorter than 10 m can significantly accelerate GC analyses. Equations for calculation of the parameters of the exponential flow function and retention data are described. The effects of flow programming in a short capillary column are shown in a few chromatograms. Different programming rates are tested and compared with temperature programming. 相似文献
872.
Summary Packings and stationary phases applied to high resolution separations of proteins, enzymes, and nucleic acids must satisfy
a series of distinct criteria that are different from those usually required by HPLC of low molecular weight non-biologically
active analytes. These requirements have been met through substantial improvements in classical gel media together with novel
developments in silica supports, and have led to a family of products with tailor-made and reproducible properties. Supports
consisting of cross-linked organic gels, and inorganic materials (mostly silicas) are now available with graduated particle
sizes, pore sizes, porosities and surface areas as well as non-porous beads. A whole range of stationary phases, such as reversed
phase, hydrophobic interaction, ion exchanger and affinity packings, were designed for application as chemical sensors for
biopolymer recognition in adsorptive chromatography. The phase systems are operated in the gradient mode, giving high resolution
and high peak capacities. In addition, aqueous liquid-liquid partitioning systems have been developed for the fractionation
of proteins and nucleic acids. Size exclusion media complete the set of HPLC variants enabling a discrimination of proteins
according to their size and shape in an isocratic elution mode. Basically, protein purification and isolation is a multistage
process where-by the HPLC variants are combined in a logistic sequence, utilizing the different selectivities of the phase
systems and thus maximising resolution, speed and throughput. 相似文献
873.
874.
Analysis of alpha-amino acids, proteins, and phenolic compounds was simultaneously performed using three capillaries in capillary electrophoresis with chemiluminescence detection, taking advantage of the micro-space area for reaction/detection at the tip of the capillary. The three capillaries included usual, polymer-containing, and sodium docley sulfate (SDS)-containing migration buffers for separation. The eluted samples from the capillaries, which were inserted into the chemiluminescence detection cell, were mixed with chemiluminescence reagent at the tips of the capillaries to generate visible light. The specific micro-space area for reaction/detection at the tips of the capillaries enabled the simultaneous operation of the three separation modes in the present system. 相似文献
875.
M. BoulovaG. Lucazeau 《Journal of solid state chemistry》2002,167(2):425-434
Nanocrystallites of tungsten oxide samples of 2, 4, 16, 35 and 60 nm of diameter were prepared by cryosol and pyrosol techniques. The pressure- and temperature-induced phase transitions of these samples were monitored by Raman spectrometry from 0.1 MPa to 34 GPa and from 77 to 1200 K. The tetragonal (α)-orthorhombic (β)-monoclinic (γ) transitions in these nanometric samples are strongly downshifted in temperature by comparison with the bulk WO3. For instance, the tetragonal phase which exists above 1171 K for the bulk tungsten oxide can be stabilized at 700 K for the 35 nm sample. In the same way, the monoclinic P21/n-monoclinic P21/c high-pressure-induced transition is slightly shifted from 0.1 GPa to a higher pressure (1.5 GPa). The discussion of these transition-line shifts is based on thermodynamic considerations in which the surface energy of crystallites plays an important role. 相似文献
876.
877.
878.
A procedure is proposed in which the determination of hydroquinone using a flow injection system with electrochemical detection is described. Size and coefficient of variation of the signal are optimised by a desirability function and a central composite design. The robustness of the optimum reached in the optimisation step is evaluated by means a Plackett-Burman design. The optimised FIA system is able to determine hydroquinone with a minimum detectable net concentration of 10 μg l−1 with a false positive probability of 0.05 and a false negative probability less than 0.05. In samples of bleaching cream, the proposed procedure has a recovery of 102.2% with standard deviation of 4.4% and a relative error of 6.2%. 相似文献
879.
A novel flow-injection system is proposed for the rapid measurement of the fish freshness indices K1 and K2: K1=[([HxR+[Hx])×100/([IMP]+[HxR]+[Hx])] and K2=[[Hx]×100/([HxR]+[Hx])], where [IMP], [HxR] and [Hx] are inosine-5′-monophosphate, inosine and hypoxanthine concentrations, respectively. For the estimation of index K1, 5′-nucleotidase immobilized reactor and nucleoside phosphorylase (NP)/xanthine oxidase (XO) coimmobilized reactor were incorporated in series in the flow-injection line made up by a 16-way switching valve with two sample loops. For the estimation of index K2, NP and XO immobilized reactors were also incorporated in the similar flow-line. Two sample portions passed through the flow-line with different residence times so that two peaks were obtained. The first and second peaks obtained in the K1-determining system corresponded to the total of HxR and Hx and the total of Hx, HxR and IMP, respectively. Similarly, the first and second peaks obtained in the K2-determining system corresponded to Hx and the total of Hx and HxR, respectively. Therefore, the indices K1 and K2 can be estimated by where i1 and i2 present the peak current of the first and second peaks, respectively, and f the ratio of the peak currents of the first and second peaks for a Hx standard solution. A sea bream was selected as a model fish and it was stored at 4 °C after death. A good correlation was found between the index K1 and the storage time over a period of 400 h, with a correlation coefficient of 0.992, but no correlation between the index K2 and the storage time. The measurements could be performed at a rate of 22 samples per hour with satisfactory precision (0.6–1.2% R.S.D.), without calibration for each species, accurate weighing of fish meat and any interferences in fish meat. 相似文献
880.
Robert S. Pomeroy Jeffrey D. Kolczynski Jonathan V. Sweedler M. Bonner Denton 《Mikrochimica acta》1989,99(3-6):347-353
A unique simultaneous emission spectrograph is utilized to perform qualitative and quantitative analysis on trace quantities of solid particulates. The atomic emission spectroscopic system consists of a direct current plasma source and an echelle spectrograph with a charge injection device detector, enabling the system to simultaneously measure the wavelength range from 220 nm to 520 nm with 0.02 nm resolution at 300 nm. Monitoring all wavelengths simultaneously allows the qualitative and quantitative determination of most major and minor constituent in a trace quantity of sample with little prior knowledge about the sample. The ability to perform qualitative and quantitative analysis on particulates is demonstrated by evaluating NBS certified coal fly ash, as well as a sample taken from the respirator air filter at an acute care unit in a hospital.Presented in part at the 1989 European Winter Conference on Plasma Spectrochemistry, Reutte, Austria 相似文献