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1.
Headspace solvent microextraction (HSME) into a single drop is developed for the determination of six trihalomethanes, CH2Cl2, CHCl3, C4H9Cl, CCl4, C2HCl3, and C2Cl4, in aqueous solution. A drop of benzyl alcohol containing bromoform, as an internal standard, is used for extraction. The analytes are extracted by suspending a 3-microL drop directly from the needle of a microsyringe. The needle passes through the septum of a vessel, and the needle tip appears above the surface of the solution. After the prescribed extraction time, the drop is drawn back into the syringe. The syringe is then removed, and its content is injected directly into a gas chromatography column for analysis. The main parameters affecting the HSME process, such as stirring speed, microdrop volume, sample solution temperature, microsyringe needle temperature, sample volume, solution pH, extracting solvent, and ionic strength of the solution, are studied. Also, the linear range and precision of the method are examined. 相似文献
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The traditional solvent-based matrix-assisted laser desorption ionization (MALDI) preparation method has been used to analyze nonpolar polymers of various molecular weights. High resolution silver cationized oligomers with masses of up to 12 KDa were measured using 9.4 tesla Fourier transform mass spectrometry (FTMS) with an external ionization source. It was observed that when time-of-flight mass spectrometry was used, the spectra of polyethylene polymers showed abundant low mass fragment ions. However, these fragments were absent from the FTMS spectra. 相似文献
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Methyl-5-benzoyl-2-benzimidazole carbamate (mebendazole) is a drug used as an anthelmintic. A high performance liquid chromatography method has been developed in this study to determine mebendazole and its degradation product in the pharmaceutical dosage forms (tablets and suspension). The expected major degradation product of mebendazole in the dosage forms has been prepared, and identified as 2-amino-5-benzoylbenzimidazole. The proposed HPLC assay was found to be selective, accurate (% recoveries were in the range of 99.9-100.9) for both, mebendazole and the degradation product, repeatable and reproducible (replicate measurements for short and long term measurements showed % RSD of =1.4). The methodology could be considered as a stability indicating method for mebendazole in pharmaceutical dosage forms. 相似文献
4.
Mariam Abd El Sater Dr. Mohamed Mellah Dr. Diana Dragoe Emilie Kolodziej Dr. Nada Jaber Dr. Emmanuelle Schulz 《Chemistry (Weinheim an der Bergstrasse, Germany)》2021,27(36):9454-9460
The first immobilization of a pyrene-tagged chromium salen complex through π-π noncovalent interactions on reduced graphene oxide (rGO) is described. A very robust supported catalytic system is obtained to promote asymmetric catalysis in repeated cycles, without loss of activity or enantioselectivity. This specific behavior was demonstrated in two different catalytic reactions (up to ten reuses) promoted by chromium salen complexes, the cyclohexene oxide ring-opening reaction and the hetero-Diels-Alder cycloaddition between various aldehydes and Danishefsky's diene. Furthermore, the chiral chromium salen@rGO has been found to be compatible with a multi-substrate type use, in which the structure of the substrate involved is modified each time the catalyst is reused. 相似文献
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An effective one‐pot, convenient process for the synthesis of 1‐ and 5‐substituted 1H‐tetrazoles from nitriles and amines is described using1,4‐dihydroxyanthraquinone–copper(II) supported on Fe3O4@SiO2 magnetic porous nanospheres as a novel recyclable catalyst. The application of this catalyst allows the synthesis of a variety of tetrazoles in good to excellent yields. The preparation of the magnetic nanocatalyst with core–shell structure is presented by using nano‐Fe3O4 as the core, tetraethoxysilane as the silica source and poly(vinyl alcohol) as the surfactant, and then Fe3O4@SiO2 was coated with 1,4‐dihydroxyanthraquinone–copper(II) nanoparticles. The new catalyst was characterized using Fourier transform infrared spectroscopy, X‐ray diffraction, transmission electron microscopy, field emission scanning electron microscopy, dynamic light scattering, thermogravimetric analysis, vibration sample magnetometry, X‐ray photoelectron spectroscopy, nitrogen adsorption–desorption isotherm analysis and inductively coupled plasma analysis. This new procedure offers several advantages such as short reaction times, excellent yields, operational simplicity, practicability and applicability to various substrates and absence of any tedious workup or purification. In addition, the excellent catalytic performance, thermal stability and separation of the catalyst make it a good heterogeneous system and a useful alternative to other heterogeneous catalysts. Also, the catalyst could be magnetically separated and reused six times without significant loss of catalytic activity. Copyright © 2016 John Wiley & Sons, Ltd. 相似文献
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The vapor pressures and osmotic coefficients of solutions of (R4N)2[MoS4] (R = ethyl, n-propyl and n-butyl) in acetone have been measured by head space-gas chromatography (HS-GC). Experimental data for the osmotic coefficients have been expressed by three thermodynamic models including the ionic interaction model of Pitzer, the electrolyte non-random two liquid (e-NRTL) model and the non-random factor (NRF) model. The ability of the models to fit the osmotic coefficient was compared on the basis of the standard deviation of the fittings. The results show that the considered models provide reliable results, but the Pitzer's model gives better results than the NRTL and the NRF methods, especially in the dilute region. 相似文献
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Nanostructured γ-Al2O3 with high surface area and mesoporous structure was synthesized by sol-gel method and employed as catalyst support for nickel catalysts in methane reforming with carbon dioxide. The prepared samples were characterized by XRD, N2adsorption-desorption,TPR, TPO, TPH, NH3-TPD and SEM techniques. The BET analysis showed a high surface area of 204 m2 g-1and a narrow pore-size distribution centered at a diameter of 5.5 nm for catalyst support. The BET results revealed that addition of lanthanum oxide to aluminum oxide decreased the specific surface area. In addition, TPR results showed that addition of lanthanum oxide increased the reducibility of nickel catalyst. The catalytic evaluation results showed an increase in methane conversion with increasing lanthanum oxide to 3 mol% and further increase in lanthanum content decreased the catalytic activity. TPO analysis revealed that the coke deposition decreased with increasing lanthanum oxide to 3 mol%. SEM and TPH analyses confirmed the formation of whisker type carbon over the spent catalysts. Addition of steam and O2 to dry reforming feed increased the methane conversion and led to carbon free operation in combined processes. 相似文献