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961.
Ernesto Schulz Lang Marcelo Müller Dias Sailer Santos dos Santos Ezequiel M. Vzquez‐Lpez Ulrich Abram 《无机化学与普通化学杂志》2004,630(3):462-465
The compounds [Hg2(μ—SePh)2(SePh)2(PPh3)2] ( I ) and [Hg3Br3(μ—SePh)3] · 2 DMSO ( II ) are formed by reactions of [Hg(SePh)2] with PPh3 in THF( I ) or with HgBr2 in DMSO ( II ) at room temperature. X—ray crystallography reveals that the cluster I consists of a distorted square built by each two Hg and Se atoms. The Hg atoms have almost tetrahedral co‐ordination environments formed by selenium atoms of two (μ‐—SePh) ligands and Se and P atoms of terminal —SePh and PPh3 ligands. The compound II is a six‐membered ring with alternating Hg and Se atoms in the chair conformation. Two DMSO molecules occupy positions below and above the [Hg3Se3] ring with the oxygen atoms directed to the centre of the ring. 相似文献
962.
De Almeida MV De Assis JV Couri MR Anconi CP Guerreiro MC Dos Santos HF De Almeida WB 《Organic letters》2010,12(23):5458-5461
Two synthetic epoxide derivatives, important intermediates in organic synthesis, were obtained from L-quebrachitol, and their conformations were proposed based on spectroscopic analysis. Density functional theory (DFT) calculations of infrared and NMR spectra were shown to be reliable enough for organic chemistry applications. The observed structures were determined with the aid of the DFT spectroscopic data, stressing the relevance and utility of combined experimental/theoretical studies and also the usefulness of the (13)C NMR B3LYP/6-31G(d,p) calculations. 相似文献
963.
In this work a single interface flow system (SIFA) with potentiometric detection was for the first time implemented and applied to the determination of nitrate in waters and plant extracts. The analytical potential of the SIFA system was exploited not only to transport the sample towards detection but also to carry out, in a reproducible and automated way, the tasks associated with sample pre-treatment, namely ionic strength, pH adjustment and interfering species suppression. The advantageous aspects of combining a SIFA system with potentiometry with enhanced simplicity, ease of implementation and automation were further discussed and emphasised.The obtained results showed relative deviations lower than 5%, for both types of samples, with sampling rates of about 40 h−1.In addition, an innovative and straightforward process for constructing plastic membrane ion selective electrodes with a tubular configuration able to be coupled to flow-based analytical systems is also proposed. The developed approach, consisting of assembling the electrode inside a flow tubing connector is very simple to implement, robust, particularly adequate to be combined with flow methodologies and maintains all dynamic and analytical characteristics exhibited by previous assembling processes. 相似文献
964.
M. Paula C. Campello Dr. Sara Lacerda Dr. Isabel C. Santos Dr. Giovannia A. Pereira Dr. Carlos F. G. C. Geraldes Prof. Dr. Jan Kotek Dr. Petr Hermann Dr. Jakub Vaněk Přemysl Lubal Vojtěch Kubíček Dr. Éva Tóth Isabel Santos Dr. 《Chemistry (Weinheim an der Bergstrasse, Germany)》2010,16(28):8446-8465
Complexes of 4,10‐bis(phosphonomethyl)‐1,4,7,10‐tetraazacyclododecane‐1,7‐diacetic acid (trans‐H6do2a2p, H6 L ) with transition metal and lanthanide(III) ions were investigated. The stability constant values of the divalent and trivalent metal‐ion complexes are between the corresponding values of H4dota and H8dotp complexes, as a consequence of the ligand basicity. The solid‐state structures of the ligand and of nine lanthanide(III) complexes were determined by X‐ray diffraction. All the complexes are present as twisted‐square‐antiprismatic isomers and their structures can be divided into two series. The first one involves nona‐coordinated complexes of the large lanthanide(III) ions (Ce, Nd, Sm) with a coordinated water molecule. In the series of Sm, Eu, Tb, Dy, Er, Yb, the complexes are octa‐coordinated only by the ligand donor atoms and their coordination cages are more irregular. The formation kinetics and the acid‐assisted dissociation of several LnIII–H6 L complexes were investigated at different temperatures and compared with analogous data for complexes of other dota‐like ligands. The [Ce( L )(H2O)]3? complex is the most kinetically inert among complexes of the investigated lanthanide(III) ions (Ce, Eu, Gd, Yb). Among mixed phosphonate–acetate dota analogues, kinetic inertness of the cerium(III) complexes is increased with a higher number of phosphonate arms in the ligand, whereas the opposite is true for europium(III) complexes. According to the 1H NMR spectroscopic pseudo‐contact shifts for the Ce–Eu and Tb–Yb series, the solution structures of the complexes reflect the structures of the [Ce(H L )(H2O)]2? and [Yb(H L )]2? anions, respectively, found in the solid state. However, these solution NMR spectroscopic studies showed that there is no unambiguous relation between 31P/1H lanthanide‐induced shift (LIS) values and coordination of water in the complexes; the values rather express a relative position of the central ions between the N4 and O4 planes. 相似文献
965.
Francisco Radler de Aquino Neto Jari Nobrega Cardoso Alberto dos Santos Pereira Maria Conceiao Zupo Fernandes Carlos Alberto Caetano Andre Luiz de Castro Machado 《Journal of separation science》1994,17(4):259-263
HTHRGC was found essential for optimizing representative preparation of high molecular weight samples and enabling fingerprinting of heavy fractions of crude oils and associated paraffinic deposits in production pipelines. Laboratory experiments aimed at simulating the process of paraffin deposition could also be easily evaluated. A comparative investigation of the performance of cold on-column and SPI (PTV type) injectors, in conjunction with high temperature capillary columns, for analysis of high molecular weight fractions, was also conducted during the course of this work. 相似文献
966.
A. F. F. Vasconcelos M. B. Dantas M. G. R. Filho R. Rosenhaim E. H. S. Cavalcanti N. R. Antoniosi Filho F. S. M. Sinfrônio I. M. G. Santos A. G. Souza 《Journal of Thermal Analysis and Calorimetry》2009,97(2):657-660
The influence of drying processes in the biodiesel oxidation was investigated by means of the oxidative induction time obtained
from differential scanning calorimetry data. For this purpose, corn biodiesel was dried by different methods including: chemical
(anhydrous sodium sulfate) and thermal (induction heating, heating under vacuum and with microwave irradiation). The drying
efficiency was evaluated by monitoring IR absorption in the 3,500–3,200 cm−1 range and by the AOCS Bc 2-49 method. In general, the oxidative induction times increased inversely to the heating degree,
except that of microwave irradiation, which was selective to water evaporation and caused low impact over the unsaturation
of biodiesel. The DSC technique was shown to be a powerful tool to evaluate with high level of differentiation the influence
of the drying process on the oxidative stability of biodiesel. 相似文献
967.
968.
Jana Sopkov‐de Oliveira Santos Marc‐Antoine Bazin Jean‐Franois Lohier La?la El Kihel Sylvain Rault 《Acta Crystallographica. Section C, Structural Chemistry》2009,65(7):o311-o313
The stilbene derivative 1,2,3‐trimethoxy‐4‐[(E)‐2‐phenylvinyl]benzene, C17H18O3, (I), and its homocoupling co‐product (E,E)‐1,4‐bis(2,3,4‐trimethoxyphenyl)buta‐1,3‐diene, C22H26O6, (II), both have double bonds in trans conformations in their conjugated linkages. In the structure of stilbene (I), the aromatic rings deviate significantly from coplanarity, in contrast with coproduct (II), the core of which is rigorously planar. The deviation in stilbene (I) seems to be driven by intermolecular electrostatic interactions. Diene (II) sits on a crystallographic inversion centre, which bisects the conjugated linkage. 相似文献
969.
Luciana B. O. dos Santos Carlos M. C. Infante Jorge C. Masini 《Journal of separation science》2009,32(4):494-500
This paper describes the development of a sequential injection chromatography (SIC) procedure for separation and quantification of the herbicides simazine, atrazine, and propazine exploring the low backpressure of a 2.5 cm long monolithic C18 column. The separation of the three compounds was achieved in less than 90 s with resolution >1.5 using a mobile phase composed by ACN/1.25 mmol/L acetate buffer (pH 4.5) at the volumetric ratio of 35:65 and flow rate of 40 μL/s. Detection was made at 223 nm using a flow cell with 40 mm of optical path length. The LOD was 10 μg/L for the three triazines and the quantification limits were of 30 μg/L for simazine and propazine and 40 μg/L for atrazine. The sampling frequency is 27 samples per hour, consuming 1.1 mL of ACN per analysis. The proposed methodology was applied to spiked water samples and no statistically significant differences were observed in comparison to a conventional HPLC–UV method. The major metabolites of atrazine and other herbicides did not interfere in the analysis, being eluted from the column either together with the unretained peak, or at retention times well‐resolved from the studied compounds. 相似文献
970.
A. M. G. F. Azeredo L. M. Q. C. Julião M. S. Santos D. R. Melo J. L. Lipsztein 《Journal of Radioanalytical and Nuclear Chemistry》1994,182(1):127-132
Internal contamination with radioactive materials of mining workers is a common problem in Brazil. This is caused by the presence of uranium, thorium, and their natural decay series associated with the mined ore. The clear examples are the workers at the niobium mine located in the state of Goiás. The niobium is associated with considerable quantities of uranium and thorium, but the mine is not legally subject to radiation protection requirements.Twenty mine workers were evaluated using in vitro bioassay techniques (urine and feces). The fecal samples were analyzed by alpha spectrometry using the method developed in the Bioassay Laboratory of the Instituto de Radioproteção e Dosimetria/CNEN which evaluates thorium and uranium isotopes simultaneously. Minor modifications were introduced to measure a higher level of activity, around 1 Bq of uranium per sample. The urine samples were analyzed by alpha spectrometry for thorium and by fluorimetry for uranium. The results obtained show that a control of the occupationally-exposed workers is necessary. 相似文献