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31.
J. N. Spencer S. K. Berger C. R. Powell B. D. Henning G. S. Furman W. M. Loffredo E. M. Rydberg R. A. Neubert C. E. Shoop D. N. Blauch 《Journal of solution chemistry》1981,10(7):501-509
Enthalpies of solution and of transfer of amides for the solvents chloroform (CHCl3), methylenechloride (CH2Cl2), carbontetrachloride (CCl4), cyclohexane (C6H12), N,N-dimethylformamide (DMF), N,N-dimethylacetamide (DMA), and ethylacetate (EtOAc) have been used to isolate and quantify the solvation interactions of amides in chlorinated solvents. Specific interactions at the aminde carbonyl and N–H groups have been identified. An analysis of the transfer enthalpies of pyrrole and methylpyrrole from cyclohexane to the chlorinated solvents shows that specific interactions between the pyrroles and these solvents are similar in nature. A means of calculating differences in the transfers of different solutes between the same solvent pair is given.Work done at Lebanon Valley College. 相似文献
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Keri T. Horne Gregory L. Powell Lee M. Daniels 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(5):m302-m303
The title complex [systematic name: pentachloro‐1κ3Cl,2κ2Cl‐tris(diethylphenylphosphino)‐1κP,2κ2P‐dirhenium(II,III)(Re—Re)], 1,3,6‐Re2Cl5(PEt2Ph)3 or [Re2Cl5(C10H15P)3], consists of dirhenium molecules with eclipsed structures similar to those of previously characterized 1,3,6‐Re2Cl5(PR3)3 compounds. The Re—Re bond distance is 2.2262 (3) Å and the metal–metal bond order is 3.5. 相似文献
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James O. Alben Allan A. Croteau Frank G. Fiamingo Craig F. Hemann Virginia A. Molleran Sungjo Park Kimerly A. Powell 《Mikrochimica acta》1988,94(1-6):335-338
Biological applications of infrared spectroscopy have pressed for ever greater instrumental capabilities in terms of spectral sensitivity and quantitative exactness. Improved instrumentation has provided measurement of many vibrational modes in biological samples that previously were lost in noise. With highly optimized sampling conditions, useful measurements have been made with a peak-to-peak noise level less than 5 microabsorbance (5×10–6 absorbance), at 0.5 cm–1 resolution. However, optical and instrumental instabilities often result in sine waves that are not totally removed by the ratio of sample to reference. These often limit effective spectral sensitivity to 50 or 100 microabsorbance, peak-to-peak, and constitute a non-random noise. Non-atmospheric absorptions, especially one at 1959 cm–1 with 0.8 cm–1 band width (FWHM) are reported. The latter is due to a trace impurity in the KBr beam splitter substrate and compensator plate. Improvements in instrumentation and sampling conditions are expected to yield measurements of absorption bands as small as 50 microabsorbance with excellent signal/noise. 相似文献
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Jemal M Huang M Mao Y Whigan D Powell ML 《Rapid communications in mass spectrometry : RCM》2001,15(12):994-999
The feasibility of quantitative bioanalysis by parallel-column liquid chromatography in conjunction with a conventional single-source electrospray mass spectrometer has been investigated using plasma samples containing a drug and its three metabolites. Within a single chromatographic run time, sample injections were made alternately onto each of two analytical columns in parallel at specified intervals, with a mass spectrometer data file opened at every injection. Thus, the mass spectrometer collected data from two sample injections into separate data files within a single chromatographic run time. Therefore, without sacrificing the chromatographic separation or the selected reaction monitoring (SRM) dwell time, the sample throughput was increased by a factor of two. Comparing the method validation results obtained using the two-column system with those obtained using the corresponding conventional single-column approach, the methods on the two systems were found to be equivalent in terms of accuracy and precision. The parallel-column system is simple and can be implemented using existing laboratory equipment with no additional capital outlays. A parallel-column system configured in this manner can be used not only for the within-a-run analysis of two samples containing two different sets of chemical entities, but also for the within-a-run analysis of two samples containing the same set of chemical entities. 相似文献
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The use of anodic stripping voltammetry (ASV) to determine the labile metal fraction in metal/ fulvic acid equilibrium systems is discussed. A method is described for distinguishing between the contributions of processes in the reduction and oxidation steps to the observed anodic (stripping) current. This method, which facilitates separate examination of the two processes, is based on timed addition of fulvic acids during the deposition step, on pH control, and on measurement of sampled-d.c. ASV peak areas (Faradaic charge) for metal/fulvic acid solutions. Results are presented for copper(Il) and lead(Il) complexes with six colloid-free soil-derived fulvic acids. In contrast to differential-pulse ASV, the stripping current measured by sampled-d.c. ASV showed no measurable contribution from ligand adsorption on the mercury drop. For heterogeneous ligand systems, such as fulvic acid, use of stripping peak heights over-estimates the fraction of non-labile metal complex because peak broadening results from the range of complexes formed in the anodic step. 相似文献
38.
Dr. Yan Peng Hagen Kaemmerer Prof. Annie K. Powell 《Chemistry (Weinheim an der Bergstrasse, Germany)》2021,27(61):15044-15066
In this Review we discuss the tuning handles which can be used to steer the magnetic properties of FeIII-4 f “butterfly” compounds. The majority of presented compounds were produced in the context of project A3 “Di- to tetranuclear compounds incorporating highly anisotropic paramagnetic metal ions” within the SFB/TRR88 “3MET”. These contain {FeIII2Ln2} cores encapsulated in ligand shells which are easy to tune in a “test-bed” system. We identify the following advantages and variables in such systems: (i) the complexes are structurally simple usually with one crystallographically independent FeIII and LnIII, respectively. This simplifies theory and anaylsis; (ii) choosing Fe allows 57Fe Mössbauer spectroscopy to be used as an additional technique which can give information about oxidation levels and spin states, local moments at the iron nuclei and spin-relaxation and, more importantly, about the anisotropy not only of the studied isotope, but also of elements interacting with this isotope; (iii) isostructural analogues with all the available (i. e. not Pm) 4 f ions can be synthesised, enabling a systematic survey of the influence of the 4 f ion on the electronic structure; (iv) this cluster type is obtained by reacting [FeIII3O(O2CR)6(L)3](X) (X=anion, L=solvent such as H2O, py) with an ethanolamine-based ligand L′ and lanthanide salts. This allows to study analogues of [FeIII2Ln2(μ3-OH)2(L′)2(O2CR)6] using the appropriate iron trinuclear starting materials. (v) the organic main ligand can be readily functionalised, facilitating a systematic investigation of the effect of organic substituents on the ligands on the magnetic properties of the complexes. We describe and discuss 34 {MIII2Ln2} (M=Fe or in one case Al) butterfly compounds which have been reported up to 2020. The analysis of these gives perspectives for designing new SMM systems with specific electronic and magnetic signatures 相似文献
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The reaction of substituted arylboronic acids with 5-bromo-2-methoxytropone catalyzed by palladium(0) complex furnished 5-arylated tropone derivatives in good yield. 相似文献