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81.
Improved ultrasonic extraction procedure for the determination of polycyclic aromatic hydrocarbons in sediments 总被引:6,自引:0,他引:6
The aim of this work was to optimize an ultrasonic extraction procedure for the determination of polycyclic aromatic hydrocarbons (PAHs) in sediments and to compare it with the reflux procedure using methanolic potassium hydroxide. Sample extracts were purified with a miniaturized silica gel chromatographic column and analyzed by gas chromatography-mass spectrometry (GC-MS). Ultrasonication using n-hexane-acetone (1:1, v/v) solvent mixture on dried homogenized marine sediment gave better precision (smaller relative standard deviation (RSD) values) and comparable quantities of individual PAH's compared to the reflux procedure. Ultrasonication with the n-hexane-acetone (1:1, v/v) mixture, utilizing four 15 min extraction cycles, was found to be sufficient for extracting PAHs from wet sediments. The optimized ultrasonic extraction procedure extracted aliphatic and aromatic hydrocarbons from the National Institute of Standards and Technology SRM 1941a with recoveries greater than 90%. The major advantages of ultrasonication compared to the reflux method are the lower extraction times, simplicity of the apparatus and extraction procedure. The optimized ultrasonication procedure has been used in our laboratory to extract hydrocarbons from naturally wet sediments from rivers, and coastal and marine areas. 相似文献
82.
[Ph3PNSbPh3Cl] ( 1 ) was prepared by oxidative addition of ClNPPh3 to triphenylstibine in dichloromethane solution. The compound is characterized by IR spectroscopy and by an X‐ray structure determination. 1 crystallizes in the monoclinic space group P21/c with four formula units per unit cell. Lattice dimensions at 193 K: a = 925.3(1), b = 1777.2(1), c = 1825.5(1) pm, β = 94.07(1)°, R1 = 0.0228. 1 forms monomeric molecules with tetrahedrally coordinated phosphorus and trigonal‐bipyramidally coordinated antimony atom, the atoms N and Cl being in axial positions. The bond lengths PN and SbN are 155.0(2) and 198.4(2) pm, respectively, the PNSb angle is 138.6(1)°. 1 reacts with iron trichloride to give the known phosphoraneiminato complex [FeCl2(NPPh3)]2. 相似文献
83.
Kurt Girstmair 《Monatshefte für Mathematik》1984,98(3):193-209
The subject of this article are a priori constructions of primitive elements in field extensions. Consider the totality of all separable polynomialsf of degreen over a fieldK with rootsx
1,...,x
n
and prescribed Galois groupG. A vector (b
1,...,b
n
)K
n
is called stably primitive (forG), if, for each suchf,b
1
x
1+...+b
n
x
n
generates the splitting field off. We develop representation theoretical devices to investigate the set of stably primitive vectors geometrically. A fundamental observation is that is either very large or very small (or even empty). These two cases are illustrated by various examples. Moreover, criteria are given to decide which case holds. For a number of groups where is recognized to be small we show. 相似文献
84.
Kurt Sturm 《Zeitschrift für Physik B Condensed Matter》1978,29(1):27-32
The real part of the effective dielectric function is derived analytically in the pseudopotential approximation. For anyk-direction, the theory allows the evaluation of the plasmon dispersion,
p
(k), which is found to be anisotropic in general due to band structure effects. Application of the theory to Al yields an isotropic shift atk=0 of
p
(0)
v
– 0.3 eV and explains the recently observed anisotropic behaviour of the dispersion very well fork < 0.6k
F
. 相似文献
85.
Michael Plate Sigrid Wocadlo Werner Massa Kurt Dehnicke Harald Krautscheid 《无机化学与普通化学杂志》1995,621(3):388-392
Functionalized Alkyne Complexes of Tungsten(VI). Syntheses and Crystal Structures of [WCl4(Et? Se? C?C? Se? Et)(THF)] and [WCl4(Et? Te? C?C? Te? Et)(THF)] The title compounds have been prepared by reactions of [WCl4(SEt2)2] with the alkynes Et? X? C?C? X? Et (X = Se, Te) in CCl4 solution and subsequent addition of tetrahydrofurane. Both complexes were characterized by crystal structure determinations. [WCl4(Et? Se? C?C? Se? Et)(THF)]: Space group P21/n, Z = 4, structure determination with 2942 unique reflections, R = 0.038. Lattice dimensions at 20°C: a = 934.2, b = 1639.5, c = 1189.5 pm, β = 96.497°. [WCl4(Et? Te? C?C? Te? Et)(THF)]: Space group P21/n, Z = 4, structure determination with 4097 unique reflections, R = 0.067, Lattice dimensions at ?70°C: a = 899.2, b = 1691.9, c = 1213.3 pm, β = 96.82°. The complexes have monomeric molecular structures with the oxygen atom of the THF molecules in trans-position to the side-on bound alkyne ligands. 相似文献
86.
Kurt Egger 《Fresenius' Journal of Analytical Chemistry》1961,182(3):161-166
Zusammenfassung 14 Glykoside der Aglykone Kaempferol, Quercetin und Myricetin werden auf ihr Verhalten im Perlon-Dünnschichtchromatogramm geprüft. Es wird gezeigt, daß 3-Monoside, 3-Bioside und 3,7-Glykoside scharf voneinander getrennt werden und an den stark verschiedenen Rf-Werten erkannt werden können. Der Einfluß des Aglykons ist gering; der entscheidende Faktor für den Rf-Wert ist die Glykosidierung.
Herrn Prof. Dr. L. Hörhammer, Herrn Doz. Dr. H. Wagner und Herrn Dr. W. Leeb, München, danke ich sehr für die freundlicherweise erteilte praktische Einführung in die Polyamid-Dünnschichtchromatographie, sowie für die Überlassung einer Probe von Kaempferol-3-rhamnoglucosid. Die Durchführung der hier dargestellten Versuche hielt sich eng an die in den Münchner Laboratorien entwickelten Verfahren.
Die Untersuchungen wurden von der Görres-Gesellschaft zur Pflege der Wissenschaften und von der Deutschen Forschungsgemeinschaft gefördert, wofür an dieser Stelle gedankt sei. Der BASF Ludwigshafen danke ich für die großzügige Überlassung des Polyamids. 相似文献
Summary 14 glycosides of the aglycons quercetin, kaempferol and myricetin were examined for their behaviour in chromatography with polyamide. The results show that the 3-monosides can be easily differentiated from the 3-biosides, as well as from both the 3,7-glycosides, by their sharply different Rf-values. The influence of the aglycon is small; the decisive factor for the Rf-value is the glycosidation.
Herrn Prof. Dr. L. Hörhammer, Herrn Doz. Dr. H. Wagner und Herrn Dr. W. Leeb, München, danke ich sehr für die freundlicherweise erteilte praktische Einführung in die Polyamid-Dünnschichtchromatographie, sowie für die Überlassung einer Probe von Kaempferol-3-rhamnoglucosid. Die Durchführung der hier dargestellten Versuche hielt sich eng an die in den Münchner Laboratorien entwickelten Verfahren.
Die Untersuchungen wurden von der Görres-Gesellschaft zur Pflege der Wissenschaften und von der Deutschen Forschungsgemeinschaft gefördert, wofür an dieser Stelle gedankt sei. Der BASF Ludwigshafen danke ich für die großzügige Überlassung des Polyamids. 相似文献
87.
When α,β-unsaturated γ-dimethoxymethyl cyclohexenones are excited to the S2(π,π*) state, certain unimolecular reactions can be observed to compete with S2 → S1 internal conversion. These reactions do not occur from the S1(n,π*) or the lowest T(π,π* and n,π*) states. They comprise the radical elimination of the formylacetal substituent (cf. 8 , 9 → 32 + 33 ), γ → α formylacetal migration (cf. 6 → 27 , 8 → 30 , 9 → 34 , 12 → 37 ), and a cyclization process involving the transfer of a methoxyl hydrogen to the α carbon and ring closure at the β position (cf. 6 → 28 , 8 → 31 , 12 → 38 , 20 → 40 + 41 ). The quantum yield of the ring closure 20a → 40a + 41a is 0.016 at ≤ 0.05M concentration. It is independent of the excitation wavelength within the π→π* absorption band (238–254 nm), but Φ ( 40a + 41a ) decreases at higher concentrations. According to the experimental data the reactive species of these specifically π→π*-induced transformations is placed energetically higher than the S1(n,π*) state, and it is either identical with the thermally equilibrated S2(n,π*) state, or reached via this latter state. The linear dienone 14 undergoes a similar π→π*-induced cyclization (→ 42 ) whereas the benzohomologue 26 proved unreactive, and the dienone 22 at both n → π and π→π* excitation only gives rise to rearrangements generally characteristic of cross-conjugated cyclohexadienones. 相似文献
88.
Hexanoic acid, heptanoic acid, octanoic acid, nonanoic acid, decanoic acid, and dodecanoic acid are components of the trail pheromone of the ant species Lasius fuliginosus. The acids were extracted from the contents of the rectal ampullae and identified by the mass spectra and gas chromatographic retention times of the corresponding methyl esters. 相似文献
89.
Jørgensen JM Erlacher K Pedersen JS Gothelf KV 《Langmuir : the ACS journal of surfaces and colloids》2005,21(23):10320-10323
The influence of preparation temperature on the size and size distribution of dodecylthiol monolayer protected gold clusters was studied. The monolayer protected clusters (MPCs) were synthesized by two different variations of the Brust-Schiffrin procedure. In all of the experiments, the stoichiometry of the reactants dodecylthiol, HAuCl(4), and sodium borohydride was kept constant, while the temperature was varied in the range of -18 to +90 degrees C. Two series were performed in which an aqueous solution of NaBH(4) was either added over 30 s or all in one portion. The size and size distribution of the MPCs were determined by small-angle X-ray scattering (SAXS) and transmission electron microscopy (TEM). It has been demonstrated that in general the MPC size increases with elevated preparation temperatures. 相似文献
90.
Mono- and Binuclear Dinitrosyl Complexes of Molybdenum and Tungsten. Crystal Structures of (PPh3Me)2[WCl4(NO)2], (PPh3Me)2[MoCl3(NO)2]2, and (PPh3Me)2[WCl3(NO)2]2 The complexes (PPh3Me)2[MCl4(NO)2] (M = Mo, W), and (PPh3Me)2[MCl3(NO)2]2, respectively, are prepared by reactions of the polymeric compounds MCl2(NO)2 with triphenylmethylphosphonium chloride in CH2Cl2, forming green crystals. According to the IR spectra the nitrosyl groups are in cis-position in all cases. The tungsten compounds as well as (PPh3Me)2[MoCl3(NO)2]2 were characterized by structure determinations with X-ray methods. (PPh3Me)2[WCl4(NO)2]: space group C2/c, Z = 4. a = 1874, b = 1046, c = 2263 pm, β = 119.99°. Structure determination with 3492 independent reflexions, R = 0.057. The compound consists of PPh3Me⊕ ions, and anions [WCl4(NO)2]2? with the nitrosyl groups in cis-position (symmetry C2v). (PPh3Me)2[WCl3(NO)2]2: Space group C2/c, Z = 4. Structure determination with 2947 independent reflexions, R = 0.059. (PPH3Me)2[MoCl3(NO)2]2: Space group P1 , Z = 1. a = 989, b = 1134, c = 1186 pm; α = 63.25°, β = 80.69°, γ = 69.94°. Structure determination with 3326 independent reflexions, R = 0.046. The compounds consist of PPh3Me⊕ ions, and centrosymmetric anions [MCl3(NO)2]22?, in which the metal atoms are associated via MCl2M bridges of slightly different lengths. One of the NO groups is in an axial position, the other one in equatorial position (symmetry C2h). 相似文献