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101.
用峰鉴别技术反相高效液相色谱法测定火锅汤料中微量吗啡 总被引:3,自引:0,他引:3
本文报道了以峰鉴别技术为定性依据的测定火锅汤料中微量吗啡的反相高效液相色谱法。本法采用改良的Stas-otto法分离提取复杂样品中的微量吗啡。由于采用峰鉴别技术,增加了定性参数,大大提高了定性方法的准确性。本法简便、快速。最低检出浓度为0.04mg/L。在数十例样品分析中,与其它仪器分析结果比照,非常符合。 相似文献
102.
《Chemphyschem》2003,4(4):359-365
We studied the thermodynamic stability of a small monomeric protein, staphylococcal nuclease (Snase), as a function of both temperature and pressure, and expressed it as a 3D free‐energy surface on the p,T‐plane using a second‐order Taylor expansion of the Gibbs free‐energy change ΔG upon unfolding. We took advantage of a series of different techniques (small‐angle Xray scattering, Fourier‐transform infrared spectroscopy, differential thermal analysis, pressure perturbation calorimetry and densitometry) in the evaluation of the conformation of the protein and in evaluating the changes in the thermodynamic parameters upon unfolding, such as the heat capacity, enthalpy, entropy, volume, isothermal compressibility and expansivity. The calculated results of the free‐energy landscape of the protein are in good agreement with experimental data of the p,T‐stability diagram of the protein over a temperature range from 200 to 400 K and at pressures from ambient pressure to 4000 bar. The results demonstrate that combined temperature–pressure‐dependent studies can help delineate the free‐energy landscape of proteins and hence help elucidate which features and thermodynamic parameters are essential in determining the stability of the native conformational state of proteins. The approach presented may also be used for studying other systems with so‐called re‐entrant or Tamman loop‐shaped phase diagrams. 相似文献
103.
A five-step model for a quality assurance system is developed for an internal quality control check. It includes the quality
control of the decomposition method and the detection method as steps belonging together. The Wickbold combustion technique
as decomposition method in combination with atomic absorption spectrometry was chosen. The vaporization of the elements mercury,
arsenic, lead, antimony and selenium is based on combustion in an oxyhydrogen flame. To check the efficiency of the analytical
system, the uncertainty of results was calculated on the basis of the "Guide to the Expression of Uncertainty in Measurement".
Received: 13 January 1997 · Accepted: 29 March 1997 相似文献
104.
105.
Delenclos S. Kolinsky C. Longuemart S. Hadj Sahraoui A. Buisine J. M. 《Journal of Thermal Analysis and Calorimetry》2002,70(2):549-558
The photopyroelectric (PPE) method is proposed as a sensitive technique to study a binary mixture of liquid crystals in a
contact preparation. The photothermal signal is generated while scanning the contact preparation. The crystal-smectic A, smectic
A-nematic, and nematic-isotropic interphase boundaries are detected. The displacement of these boundaries due to the variation
of the temperature is monitored. The study of these displacements allows us to draw the complete temperature-concentration
phase diagram of a binary mixtures.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
106.
Villanueva J Villegas V Querol E Avilés FX Serrano L 《Journal of mass spectrometry : JMS》2002,37(9):974-984
In the post-genomic era, several projects focused on the massive experimental resolution of the three-dimensional structures of all the proteins of different organisms have been initiated. Simultaneously, significant progress has been made in the ab initio prediction of protein three-dimensional structure. One of the keys to the success of such a prediction is the use of local information (i.e. secondary structure). Here we describe a new limited proteolysis methodology, based on the use of unspecific exoproteases coupled with matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS), to map quickly secondary structure elements of a protein from both ends, the N- and C-termini. We show that the proteolytic patterns (mass spectra series) obtained can be interpreted in the light of the conformation and local stability of the analyzed proteins, a direct correlation being observed between the predicted and the experimentally derived protein secondary structure. Further, this methodology can be easily applied to check rapidly the folding state of a protein and characterize mutational effects on protein conformation and stability. Moreover, given global stability information, this methodology allows one to locate the protein regions of increased or decreased conformational stability. All of this can be done with a small fraction of the amount of protein required by most of the other methods for conformational analysis. Thus limited exoproteolysis, together with MALDI-TOF MS, can be a useful tool to achieve quickly the elucidation of protein structure and stability. 相似文献
107.
An explicit expression for the analytical first derivative of the Z-averaged perturbation theory taken to second order energy, due to Lee and Jayatilaka, is presented for application to high-spin
systems described by a restricted open-shell Hartree–Fock wavefunction. The use of frozen core orbitals is incorporated into
the derivation.
Received: 23 April 2001 / Accepted: 31 August 2001 / Published online: 9 January 2002 相似文献
108.
E. L. Anderson M. M. Thomason H. T. Mayfield W. Bertsch 《Journal of separation science》1979,2(6):335-342
A versatile two-dimensional gas chromatograph is described, consisting of 2 separate ovens, one intermediate trap, an auxiliary inlet, and the necessary hardware to effect off-line switching according to the principle of Deans. The unit has been designed for use with high resolution glass capillary columns. The performance of individual instrumental components was critically evaluated. Results showed that low dead volume glass to metal connections were required in the manifold and detector lines to minimize extra-column effects. The mass of the intermediate trap must be low to allow rapid heating. Operational parameters are discussed and examples of some applications are shown. 相似文献
109.
Grimme S 《Journal of computational chemistry》2003,24(13):1529-1537
Based on a partitioning of the total correlation energy into contributions from parallel‐ and antiparallel‐spin pairs of electrons, a modified third‐order Møller–Plesset (MP) perturbation theory is developed. The method, termed SCS–MP3 (SCS for spin‐component‐scaled) continues previous work on an improved version of MP2 (S. Grimme, J Chem Phys 2003, 118, 9095). A benchmark set of 32 isogyric reaction energies, 11 atomization energies, and 11 stretched geometries is used to assess to performance of the model in comparison to the standard quantum chemical approaches MP2, MP3, and QCISD(T). It is found, that the new method performs significantly better than usual MP2/MP3 and even outperforms the more costly QCISD method. Opposite to the usual MP series, the SCS third‐order correction uniformly improves the results. Dramatic enhancements are especially observed for the more difficult atomization energies, some of the stretched geometries, and reaction and ionization energies involving transition metal compounds where the method seems to be competitive or even superior to the widely used density functional approaches. Further tests performed for other complex systems (biradicals, C20 isomers, transition states) demonstrate that the SCS–MP3 model yields often results of QCISD(T) accuracy. The uniformity with which the new approach improves for very different correlation problems indicates significant robustness, and suggests it as a valuable quantum chemical method of general use. © 2003 Wiley Periodicals, Inc. J Comput Chem 24: 1529–1537, 2003 相似文献
110.