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91.
A one-step solid-phase extraction procedure, based on a new silica gel adsorbent modified with cholesterol groups, has been
investigated for measurement of cotinine in urine. Cotinine is the main metabolite of nicotine in the human body and is analyzed
as a biomarker for assessment of direct or passive exposure to tobacco smoke. New cholesterol-modified adsorbents have been
obtained by chemical modification of silica gel of different porosity with cholesterol ligands. Although recovery by this
extraction procedure were optimum over a relatively broad range of sample pH (3.1–8.0), analytical conditions such as sample
loading, washing and elution conditions, concentration of cotinine to be extracted, and the type of adsorbent used for extraction
were found to affect the efficiency of the procedure and had to be controlled for optimum recovery. When these conditions
were controlled, recovery of cotinine from spiked human urine was reproducible and depended on compound ionization. Quantitative
analysis of cotinine was performed by reversed-phase high-performance liquid chromatography with UV detection.
Presented at: Conference of the Hyphenation of Liquid Chromatography–Nuclear Magnetic Resonance Spectroscopy, Liquid Chromatography–Mass
Spectrometry and Related Topics, Tuebingen, Germany, March 25–29, 2006. 相似文献
92.
93.
Summary A method for the separation of substituted tetraphenylporphyrins by preparative liquid chromatography is reported. The quality of the columns formed by axial compression of various stationary phases is tested. 相似文献
94.
T. Kowalska 《Chromatographia》1991,31(3-4):119-122
Summary Intermolecular interactions between the solute and the moieties constituting the mobile phase significantly contribute to the overall retention pattern of a given solute in a given chromatographic system. In this paper retention of solute is discussed in the case of the B+AB1+AB2 type mobile phase, which, in a quasithermodynamic way, can be divided into seven individual moieties. One evaluates the influence of each moiety on solute retention, and refers these regularities to the polarity of the solutes. 相似文献
95.
Summary Pressure and temperature have significant influence on retention in HPLC. This study investigates the effect of pressure and
temperature on the retention behavior of aromatic hydrocarbons (toluene, ethyl benzene, butyl benzene, pentyl benzene) and
polar, acidic and basic samples (phenol, acetophenone, N,N-dimethyl aniline, benzophenone) on a reversed phase column. The
effect has been studied on non-porous, tetradecyl (C14) coated silica particles. We found that the adsorption-induced decrease of the partial molar volume of the solutes investigated
was between ΔV
m
=5–15 cm3 mol−1. The increment of the decrease of the partial molar volume due to the addition of one CH2 group, for the homologous series of the aromatic hydrocarbons is approximately ΔV
CH2
=2.3 cm3mol−1.
Presented at Balaton Symposium '01 on High-Performance Separation Methods, Siófok, Hungary, September 2–4, 2001. 相似文献
96.
Traditionally, the application of supercritical fluid chromatography has been limited to compounds of relatively low polarity.
Thus, we report here that one secondary amine and two quaternary amine salts were successfully eluted from a Deltabond Cyano-bonded
silica column with the addition of sodium alkylsulfonate to the methanol-modified, carbon dioxide-based mobile phase. A possible
ion-pairing interaction between the positively charged analytes and the anionic part of the sulfonate additive has been proposed.
In another set of experiments, the three amine salts readily eluted from both Ethyl-pyridine-bonded silica and Amino-bonded
silica phases without the need of additive although the peak shapes were less than desirable. The addition of sulfonate salt
to the mobile phase again sharpened the peaks. In the presence of a mixture of methanol and CO2, we suggest that these stationary phases are positively charged. We describe here also for the first time the employment
of a strong silica-based anion exchange (SAX) column for supercritical fluid separation of cationic species. Two elution mechanisms
were proposed for the three amine salts depending upon whether the ionic additive was incorporated into the mobile phase.
Separation as the ion-pair was proposed with an ionic additive in the mobile phase; whereas separation of the intact amine
salt from the positively charged basic stationary phases was suggested to be operational without the ionic additive. 相似文献
97.
The chiral resolving ability of a novel single-isomer cationic β-cyclodextrin (CD), mono-6A-propylammonium-6A-deoxy-β-cyclodextrin chloride (PrAMCD), as a chiral selector in capillary electrophoresis (CE) is reported in this work for the enantioseparation of hydroxy, carboxylic acids and amphoteric analytes. The effect of chiral selector concentration on the resolution was studied. Good resolutions were achieved for hydroxy acids. Optimum resolutions were obtained even at 3.5 mM CD concentration for carboxylic acids. The electrophoretic method showed good linearity and reproducibility in terms of migration times and peak areas, which should make it suitable for routine analysis. In addition, baseline chiral separation of a six-acid mixture was achieved within 20 min. PrAMCD proved to be an effective chiral selector for acidic analytes. 相似文献
98.
《Electroanalysis》2006,18(22):2243-2250
This work is focused on the voltammetric examination of the ion exchange properties of a smectite type clay, before and after its modification by the replacement of its native interlamellar cations (Na+, K+, Ca2+) by hexadecyltrimethylammonium cations (HDTMA+). The raw clay and its organically modified form were first characterized by X‐ray diffraction (XRD) and N2 adsorption–desorption isotherms (BET method) that confirmed the modification via an intercalation process. These materials were subsequently coated onto glassy carbon surfaces, and the resulting modified electrodes were evaluated for the uptake of [Ru(NH3)6]3+ and [Fe(CN)6]3? ions used as redox probes. Some experimental parameters affecting the incorporation of the probes within the film, including the ionic strength, the surfactant loading and the solution pH are thoroughly examined, in order to highlight the mechanism of the process. The possibility of using the surfactant‐intercalated clay modified electrode as an electrochemical sensor for [Fe(CN)6]3? is also evaluated. 相似文献
99.
Arsenidostannates with [SnAs] Nets Isostructural to Grey Arsenic: Synthesis and Crystal Structure of Na[Sn2As2], Na0.3Ca0.7[Sn2As2], Na0.4Sr0.6[Sn2As2], Na0.6Ba0.4[Sn2As2], and K0.3Sr0.7[Sn2As2] The metallic lustrous compounds Na[Sn2As2], Na0.3Ca0.7[Sn2As2], Na0.4Sr0.6[Sn2As2], Na0.6Ba0.4[Sn2As2] and K0.3Sr0.7[Sn2As2] were prepared from melts of mixtures of the elements. The compounds crystallize in the trigonal system (space group R3 m, No. 166, Z = 3) with lattice constants see in “Inhaltsübersicht”. The structures are isotypic to Sr[Sn2As2] containing puckered [SnAs] nets which are stacked with a sequence of six layers. The E(I)/E(II) atoms are located between each second [SnAs] layer in trigonal antiprismatic interstices formed by As atoms. In the resulting [Sn2As2] double layers the ∞2[SnAs] nets are stacked in such a way that additional Sn—Sn contacts arise. 相似文献
100.
1H NMR chemical shifts of solutions of the following cationic surfactants in D2O were determined as a function of their concentrations: cetyltrimethylammonium chloride, CTACl, a 1 : 1 molar mixture of
CTACl and toluene, cetylpyridinium chloride, CPyCl, cetyldimethylphenylam-monium chloride, CDPhACl, cetyldimethylbenzylammonium
chloride, CDBzACl, cetyldimethyl-2-phenylethylammonium chloride, CDPhEtACl, and cetyldimethyl-3-phenylpropylammonium chloride,
CDPhPrACl. Plots of observed chemical shifts versus [surfactant] are sigmoidal, and were fitted to a model based on the mass-action
law. Satisfactory fitting was obtained for the discrete protons of all surfactants. From these fits, we calculated the equilibrium
constant for micelle formation, K, the critical micelle concentration, CMC and the chemical shifts of the monomer, δmon and the micelle δmic. 1H NMR-based CMC values are in excellent agreement with those which we determined by surface tension measurements of surfactant
solutions in H2O, allowing for the difference in structure between D2O and H2O. Values of K increase as a function of increasing the size of the hydrophilic group, but the free energy of transfer per CH2 group of the phenylalkyl moiety from bulk water to the micellar interface is approximately constant, 1.9±0.1 kJ mol-1. Values of (δmic–δmon) for the surfactant groups at the interface, e.g., CH3–(CH2)15–N+(CH3)2 and within the micellar core, e.g., CH3–(CH2)15–N+ were used to probe the (average) conformation of the phenyl group in the interfacial region. The picture that emerges is
that the aromatic ring is perpendicular to the interface in CDPhACl and is more or less parallel to it in CDBzACl, CDPhEtACl,
and CDPhPrACl.
Received: 23 February 1996 Accepted: 29 August 1996 相似文献