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581.
582.
A one-step and in-situ sample preparation method used for quantifying chlorobenzene compounds in water samples has been developed, coupling microwave and headspace single-drop microextraction (MW-HS-SDME). The chlorobenzenes in water samples were extracted directly onto an ionic liquid single-drop in headspace mode under the aid of microwave radiation. For optimization, a Plackett-Burman screening design was initially used, followed by a mixed-level factorial design. The factors considered were: drop volume, aqueous sample volume, stirring speed, ionic strength, extraction time, ionic liquid type, microwave power and length of the Y-shaped glass-tube. The optimum experimental conditions found from this statistical evaluation were: a 5 μL microdrop of 1-hexyl-3-methylimidazolium hexafluorophosphate exposed for 20 min to the headspace of a 30 mL aqueous sample, irradiated by microwaves at 200 W and placed in a 50 mL spherical flask connected to a 25 cm Y-shaped glass-tube. Under the optimised experimental conditions, the response of a high performance liquid chromatographic system was found to be linear over the range studied and with correlation coefficients ranging between 0.9995 and 0.9999. The method showed a good level of repeatability, with relative standard deviations varying between 2.3 and 8.3% (n = 5). Detection limits were found in the low μg L−1 range varying between 0.016 and 0.039 μg L−1. Overall, the performance of the proposed method demonstrated the favourable effect of microwave sample irradiation upon HS-SDME. Finally, recovery studies from different types of environmental water samples revealed that matrix had little effect upon extraction. 相似文献
583.
Javier A. Cabeza Ignacio del Río Robert A. Gossage Lorena Martínez-Méndez Daniel Miguel 《Journal of organometallic chemistry》2007,692(20):4346-4352
The synthesis and characterisation of three novel mononuclear ruthenium(II) complexes containing one of the following chiral auxiliary ligands: 2-amino-(4R)-phenyl-2-oxazoline (amphox), indanyl-2-amino-(4R,5S)-2-oxazoline (aminox) or indanyl-(2′-anilinyl)-(4R,5S)-2-oxazoline (aninox) is described using [Ru2Cl4(η6-p-cym)2] (p-cym = 1-isopropyl-4-methylbenzene) as the Ru starting material. The new complexes have been identified as the neutral derivatives [RuCl2(η6-p-cym)(amphox-κ1Nox)] (1), [RuCl2(η6-p-cym)(aminox-κ1Nox)] (2) and the salt [RuCl(η6-p-cym)(aninox-κ2N,N′)]Cl (3). These materials have been fully characterised (elemental analysis, NMR, IR, conductance, MS, etc.) and, in the case of 2 and 3, structurally elucidated in the solid-state using single crystal X-ray diffraction methods. All three complexes show good catalytic activity (max. conversion >99%, TOF = 424 h−1) but only modest enantio-selectivity (max. ee = 40%) for the transfer hydrogenation reaction of acetophenone with isopropyl alcohol. The complexes were also tested in an asymmetric Diels-Alder reaction involving cyclopentadiene and acrolein (max. conversion >99%, TOF = 42 h−1). In this case, the diastereo-selectivity was good to moderate (max. de = 84%), but the ee values were poor (max. ee = 12%). 相似文献
584.
María Goncalves José Daniel Martínez Mary Lorena Araujo Felipe Brito Giuseppe Lubes Mildred Rodríguez Vito Lubes 《Journal of solution chemistry》2011,40(9):1517-1527
The complex species formed in aqueous solutions (25 °C, I=3.0 mol⋅dm−3 KCl ionic medium) between the V(III) cation and the ligands 6-methylpicolinic acid (MePic, HL), salicylic acid (H2Sal, H2L) and phthalic acid (H2Phtha, H2L) have been studied by potentiometric and spectrophotometric measurements. Application of the least-squares computer program
LETAGROP to the experimental emf(H) data, taking into account the hydrolytic species and hydrolysis constants of V(III), indicates
that under the employed experimental conditions the complexes [VL]2+, [V(OH)L]+, [V(OH)2L], [V(OH)3L]−, [VL2]+, [VL3] and [V2OL4] form in the vanadium(III)–MePic system. Were observed the complexes [VL]+, [VL2]−, [V(OH)L2]2− and [VL3]3− in the vanadium(III)–H2Sal system, and the species [VHL]2+, [VL]+, [V(OH)L], [VHL2], [VL2]−, [V(OH)L2]2−, [V(OH)2L2]3− and [VL3]3− in the vanadium(III)–H2Phtha system. The stability constants of these complexes were determined by potentiometric measurements, and spectrophotometric
measurements were made in order to perform a qualitative characterization of the complexes formed in aqueous solution. 相似文献
585.
A fast, simple, inexpensive, sensitive, efficient and environmental friendly direct ultrasound-assisted dispersive liquid-liquid microextraction (DUSA-DLLME) procedure has been developed to concentrate five nitroaromatic explosives from water samples prior to quantification by gas chromatography-mass spectrometry (GC-MS). An efficient ultrasonic probe has been used to radiate directly the samples producing very fine emulsions from immiscible liquids. A D-optimal design was used for optimizing the factors and to evaluate their influential upon extraction. The optimum experimental conditions were: sample volume, 10 mL; extraction time, 60 s; cycles, 0.6 s(s−1); power of ultrasound energy, 40% (70 W); and, extractant solvent (chlorobenzene) volume, 20 μL. Under the optimized experimental conditions the method presents good level of repeatability with coefficients of variation under 6% (n = 8; spiking level 10 μg L−1). Calculated calibration curves gave high level of linearity with correlation coefficient values between 0.9949 and 0.9992. Limits of detection were ranged between 0.03 and 0.91 μg L−1. Finally, the proposed method was applied to the analysis of two types of water samples, reservoir and effluent wastewater. The samples were previously analysed and confirmed free of target analytes. At 5 μg L−1 spiking level recovery values ranged between 75 and 96% for reservoir water sample showing that the matrix had a negligible effect upon extraction. However, a noticeable matrix effect (around 50% recovery) was observed for effluent wastewater sample. In order to alleviate this matrix effect, the standard addition calibration method was used for quantitative determination. This calibration method supplied recovery values ranged between 71 and 79%. The same conclusions have been obtained from an uncertainty budget evaluation study. 相似文献
586.
M. Abdel-Bary S. Abdel-Samad K. -Th. Brinkmann H. Clement J. Dietrich E. Doroshkevich S. Dshemuchadse K. Ehrhardt A. Erhardt W. Eyrich A. Filippi H. Freiesleben M. Fritsch W. Gast A. Gillitzer J. Gottwald H. J?ger B. Jakob R. J?kel L. Karsch K. Kilian H. Koch M. Krapp J. Kre? E. Kuhlmann A. Lehmann S. Marcello S. Mauro P. Michel K. Móller H. P. Morsch L. Naumann N. Paul C. Pizzolotto Ch. Plettner S. Reimann M. Richter J. Ritman E. Roderburg A. Schamlott P. Sch?nmeier W. Schroeder M. Schulte-Wissermann T. Sefzick M. Steinke G. Y. Sun A. Teufel W. Ullrich G. J. Wagner M. Wagner R. Wenzel A. Wilms P. Wintz P. Wüstner P. Zupranski 《The European Physical Journal A - Hadrons and Nuclei》2010,44(1):7-22
587.
M. Abdel-Bary S. Abdel-Samad K-Th. Brinkmann H. Clement J. Dietrich E. Doroshkevich S. Dshemuchadse K. Ehrhardt A. Erhardt W. Eyrich D. Filges A. Filippi H. Freiesleben M. Fritsch W. Gast J. Georgi A. Gillitzer J. Gottwald D. Hesselbarth H. J?ger B. Jakob R. J?kel L. Karsch K. Kilian H. Koch M. Krapp J. Kre? E. Kuhlmann A. Lehmann S. Marcello S. Marwinski S. Mauro W. Meyer P. Michel K. M?ller H. P. Morsch H. M?rtel L. Naumann N. Paul L. Pinna C. Pizzolotto Ch. Plettner S. Reimann M. Richter J. Ritman E. Roderburg A. Schamlott P. Sch?nmeier W. Schroeder M. Schulte-Wissermann T. Sefzick F. Stinzig M. Steinke G. Y. Sun A. Teufel W. Ullrich G. J. Wagner M. Wagner R. Wenzel A. Wilms P. Wintz S. Wirth P. Wüstner P. Zupranski 《The European Physical Journal A - Hadrons and Nuclei》2010,46(3):435-436
588.
Dr. Lorena Mendive-Tapia Dr. Laia Miret-Casals Dr. Nicole D. Barth Jinling Wang Dr. Anne de Bray Dr. Massimiliano Beltramo Vincent Robert Prof. Dr. Christophe Ampe Prof. Dr. David J. Hodson Prof. Dr. Annemieke Madder Prof. Dr. Marc Vendrell 《Angewandte Chemie (International ed. in English)》2023,62(20):e202302688
The G protein-coupled kisspeptin receptor (GPR54 or KISS1R) is an important mediator in reproduction, metabolism and cancer biology; however, there are limited fluorescent probes or antibodies for direct imaging of these receptors in cells and intact tissues, which can help to interrogate their multiple biological roles. Herein, we describe the rational design and characterization of a new acid-resistant BODIPY-based amino acid (Trp-BODIPY PLUS), and its implementation for solid-phase synthesis of fluorescent bioactive peptides. Trp-BODIPY PLUS retains the binding capabilities of both short linear and cyclic peptides and displays notable turn-on fluorescence emission upon target binding for wash-free imaging. Finally, we employed Trp-BODIPY PLUS to prepare some of the first fluorogenic kisspeptin-based probes and visualized the expression and localization of GPR54 receptors in human cells and in whole mouse pancreatic islets by fluorescence imaging. 相似文献
589.
Zhiming Cheng Dr. Emily J Thompson Dr. Lorena Mendive-Tapia Dr. Jamie I Scott Dr. Sam Benson Dr. Takanori Kitamura Ana Senan-Salinas Dr. Youhani Samarakoon Dr. Edward W Roberts Dr. Maykel A Arias Prof. Dr. Julian Pardo Dr. Eva M Galvez Prof. Dr. Marc Vendrell 《Angewandte Chemie (International ed. in English)》2023,62(8):e202216142
Cytotoxic immune cells, including T lymphocytes (CTLs) and natural killer (NK) cells, are essential components of the host response against tumors. CTLs and NK cells secrete granzyme A (GzmA) upon recognition of cancer cells; however, there are very few tools that can detect physiological levels of active GzmA with high spatiotemporal resolution. Herein, we report the rational design of the near-infrared fluorogenic substrates for human GzmA and mouse GzmA. These activity-based probes display very high catalytic efficiency and selectivity over other granzymes, as shown in tissue lysates from wild-type and GzmA knock-out mice. Furthermore, we demonstrate that the probes can image how adaptive immune cells respond to antigen-driven recognition of cancer cells in real time. 相似文献
590.