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81.
Three simple and sensitive colorimetric methods (A–C) for the determination of melatonin in bulk samples and in pharmaceutical
formulations are described. They are based on the formation of coloured species by reaction of ninhydrin with the drug (method
A, λmax 397 nm) by oxidation of the indol moiety in melatonin with potassium persulphate (method B, λmax 450 nm) or by reduction of osmium (VIII) (method C, λmax 516 nm). Regression analysis of Beer-Lambert plots showed good correlations in concentration ranges between 0.8–14.2, 70.0–140.0
and 2.0–40.0 μg/mL for methods A, B and C, respectively. The molar absorptivity, Sandell sensitivity and detection limit were
calculated. For more accurate analysis, Ringbom optimum concentration ranges were calculated. The validity of the proposed
methods was tested by analysing pharmaceutical formulations containing melatonin. The relative standard deviations were ≤ 0.95%
with recoveries 99.0–101.33%.
Received October 20, 1999. Revision February 10, 1999. 相似文献
82.
This work provides an insight into the effect of incorporating of magnetite nanoparticles on the rheology of fluids. In this respect, polymer-stabilized magnetite nanoparticles were obtained using sodium salt of poly (2-acrylamido-2-methylpropanesulfonate (PAMPS-Na). Monodisperse polymer coated magnetite nanoparticles Fe3O4/poly(styrene-AMPS) copolymer nanoparticles with diameters of 50–300 nm were prepared by radical polymerization in the presence of a ferrofluid coated with PAMPS-Na. The magnetic nanoparticles were easily separated in a magnetic field. The structure of the obtained magnetic nanoparticles was characterized by Fourier transform infrared spectroscopy (FTIR). The morphology and size of the magnetic nanoparticles were determined by transmission electron microscopy (TEM). FTIR and TEM revealed that the Fe3O4 nanoparticles were incorporated into the shells of poly(styrene-AMPS). Aqueous dispersed solutions of a charged hydrophobically modified Fe3O4/poly(styrene-AMPS) copolymer nanoparticles exhibit high viscosities even at low polymer concentrations (0.1 wt %), which is an interesting feature in connection with enhanced oil recovery. Effects of temperature and addition of sodium chloride on the viscosity properties of a semidilute dispersed solution of Fe3O4/poly(styrene-AMPS) copolymer nanoparticles are examined. The results indicated that Fe3O4/poly(styrene-AMPS) copolymer nanoparticles disclose strong interactions between magnetite and coated polymers of both PAMPS-Na and styrene-AMPS copolymers. 相似文献
83.
Firas F. Awwadi Deeb Taher Alaa Maabreh Fadel Z. Alwedian Hamdan Al-Ebaisat Tobias Rüffer Heinrich Lang 《Structural chemistry》2013,24(2):401-408
The analogy of chloride–chloride contacts in compounds containing Fe–Cl1···Cl2–Fe synthons with well-studied organic C–Cl1···Cl2–C interactions has been investigated. The crystal structures of the two tetrahaloferrate(III) salts, [(2-iodopyridinium)2FeX4]X (X = Cl, Br) have been determined. Analysis of these two isomorphous structures and related published structures shows that the arrangement of Fe–Cl1···Cl2–Fe synthons is similar to that of C–Cl1···Cl2–C with the Fe–Cl1···Cl2 and Cl1···Cl2–Fe angles being ~150°. While inter-chlorine distances are less than the sum of van der Waals radii in C–Cl1···Cl2–C units, they are equal to, or longer, than the sum of van der Waals radii in the corresponding Fe–Cl1···Cl2–Fe contacts. This might indicate that the arrangement of Fe–Cl1···Cl2–Fe synthons occurs predominately to reduce repulsive forces rather than as a result of attractive forces. However, it is observed that the halide–halide distance in [(2-iodopyridinium)2FeBr4]Br is shorter than in the isostructural chloride species, which can be explained by the fact that bromine is softer than chlorine. Several intermolecular forces unite the cations and anions within the crystalline lattice of [(2-iodopyridinium)2FeX4]X including N–H···X?, C–I···X–Fe, N(π)···X–Fe, N(π)···I–C, and Fe–X1···X2–Fe contacts. The calculated electron density and electrostatic potential of the [FeX4]? anions and the organic iodopyridinium cations was used to describe the arrangement of these synthons and the hierarchy of the strengths of the respective contacts. 相似文献
84.
A. S. Aly Kh. M. Abu-Zied Alaa El-Din M. Gaafar 《Phosphorus, sulfur, and silicon and the related elements》2013,188(12):3063-3078
In one-pot synthesis 2-arylidene-5,6,7,8-tetrahydrothiazolo[3,2-a] cyclopenteno-thieno[2,3-d] pyrimidine-3,5-diones (3) were prepared via the reaction of a ternary mixture of 2-thioxo-1,3,4,5,6,7-hexahydr cyclopentinothieno [2,3-d]-4-one (2), chloroacetic acid and a proper aldehyde. Compound 2 reacted with 3-chloropent-2, 4-dione in ethanolic potassium hydroxide yielding the S-acetyl acetone derivative 5f . The latter compound reacted with hydrazine hydrate and phenyl hydrazine yielded the 2-pyrazolthio derivative 10a, b. Compound 5f also underwent cyclization on heating with acetic acid—pyridine solution to give 11. The 2-methylthio derivative 5a, when treated with hydrogen peroxide gave the corresponding oxidized product 9. 相似文献
85.
Recent Heterocyclic Compounds from (1,3‐Dioxo‐2,3‐dihydro‐1H‐inden‐2‐ylidene)propanedinitrile
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This review summarizes the literatures dealing with the synthesis of some important nitrogen or nitrogen/sulfur heterocyclic, spiroheterocyclic, and fused heterocyclic compounds. 相似文献
86.
87.
Rajab Abu-El-Halawa Alaa Sarabi Mustafa M. El-Abadelah 《Monatshefte für Chemie / Chemical Monthly》2008,139(10):1251-1255
Interaction between 2,5-dichlorothiophene-3-carbonyl isothiocyanate, accessible via 2,5-dichlorothiophene-3-carbonyl chloride, and model heterocyclic amines produced the respective 2,5-dichloro-N-(substituted aminocarbonothioyl)thiophene-3-carboxamides. Upon heating, the deprotonated form of the latter underwent intramolecular
cyclization to deliver the corresponding 2-(substituted amino)-4H-thieno[3,2-e]-1,3-thiazin-4-ones. The structures of these new bicyclic derivatives and their acyclic precursors are based on microanalytical
and spectral (IR, MS, and NMR) data.
Correspondence: Rajab Abu-El-Halawa, Chemistry Department, Faculty of Science, Al al-Bayt University, Mafraq, Jordan. 相似文献
88.
Aly SM Ho CL Fortin D Wong WY Abd-El-Aziz AS Harvey PD 《Chemistry (Weinheim an der Bergstrasse, Germany)》2008,14(27):8341-8352
The synthesis of polymers of the type (-Cz-C[triple chemical bond]C-PtL(2)-C[triple chemical bond]C-Cz-X-)(n) along with the corresponding model compounds (Ph-PtL'(2)-C[triple chemical bond]C-Cz)(2)-X-, where Cz=3,3'-carbazole, X=nothing, Cz, or F (2,2'-fluorene), L=PBu(3), and L'=PEt(3) are reported. The electronic spectra (absorption, excitation, emission, and ns-transient spectra) and the photophysics of these species in 2-methyltetrahyrofuran (2MeTHF) at 298 and 77 K are presented. Evidence for singlet electron and triplet energy transfer from the Cz chromophore to the F moiety are provided and discussed in detail. The rate for electron transfer is very fast (>4 x 10(11) s(-1)), whereas that for triplet-triplet energy transfer is much slower (approximately 10(3) s(-1)). This work represents a very rare example of studies that address electronic communication in the backbone of a conjugated organometallic polymer. 相似文献
89.
Clément S Aly SM Fortin D Guyard L Knorr M Abd-El-Aziz AS Harvey PD 《Inorganic chemistry》2008,47(23):10816-10824
The homodinuclear d9-d9 ClM(mu-dppm)2MCl2 complexes, 1 (M ) Pt) and 2 (M ) Pd) react with the conjugated and luminescent PCP-NC ligand (3, PCP ) [2.2]paracyclophane) to provide the corresponding d9-d9 terminal[ClPt(mu-dppm)2Pt(CNsPCP)]Cl (4) and d8-d8 A-frame [ClPd(mu-dppm)2(mu-CdNsPCP)PdCl] (5) isocyanide complexes, respectively. These two bimetallic complexes were characterized by IR, 1H, and 31P{1H} NMR and bychemical analysis. IR data (nu(CN) bridging vs terminal) reveal a terminal isocyanide bonding mode for 4 (2147cm(-1)) and an A-frame structure for 5 (1616 cm(-1)). The optical and emission properties of the free isocyanide 3as well as those of the homodinuclear complexes 4 and 5 were studied by UV-visible and luminescence spectroscopy and by photophysical measurements. The unexpected presence of simultaneous intraligand pipi* fluorescence and phosphorescence attributable to the organic PCP-NC ligand, as well as luminescence from the inorganic M2-bonded Pt2(mu-dppm)2 center arising from a lower energy excited LMCT state (ligand-to-metal-charge-transfer) for4 at 77 K, indicates a weak conjugation between the two chromophores and an absence of efficient singlet andtriplet energy transfers. For 5, only the fluorescence and phosphorescence bands of the PCP-NC ligand are observed [since the A-frame XPd(mu-dppm)2(mu-L)PdX (L ) isocyanide, X ) halide) is not luminescent], stressing that the NtC bridge exhibits modest electronic communication properties. 相似文献
90.
Ashraf A. Aly Alaa A Hassan Essmat M. El‐Sheref Mamdouh A. Mohamed Alan B. Brown 《Journal of heterocyclic chemistry》2008,45(2):521-526