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421.
Jelena Golubovi Ana Proti Mira Ze
evi Biljana Otaevi Marija Miki 《Journal of Chemometrics》2014,28(7):567-574
The study of experimental design in conjunction with artificial neural networks for optimization of isocratic ultra performance liquid chromatography method for separation of mycophenolate mofetil and its degradation products has been reported. Experimental design showed to be suitable for selection of experimental scheme, while Kennard‐Stone algorithm was used for selection of training data set. The input variables were column temperature and composition of mobile phase including percentage of acetonitrile, concentration of ammonium acetate in buffer, and its pH value. The retention factor of the most retentive component and selectivity factors were used as the dependent variables (outputs). In this way, artificial neural network has been applied as a predictable tool in solving a method optimization problem using small number of experiments. Network architecture and training parameters were optimized to the lowest root‐mean‐square error values, and the network with 5‐4‐4‐4 topology has been selected as the most predictable one. Predicted data were in good agreement with experimental data, and regression statistics confirmed good ability of trained network to predict compounds retention. The optimal chromatographic conditions included column temperature of 40°C, flow rate of 700 µl min−1, 26% of acetonitrile and 9 mM ammonium acetate in mobile phase, and buffer pH of 5.87. The chromatographic analysis has been achieved within 5.2 min. The validation of the proposed method was also performed considering selectivity, linearity, accuracy, precision, limit of detection, and limit of quantification, and the results indicated that the method fulfilled all required criteria. The method was successfully applied to the analysis of commercial dosage form. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
422.
Ashveen V. NandSudip Ray Marija Gizdavic-NikolaidisJadranka Travas-Sejdic Paul A. Kilmartin 《Polymer Degradation and Stability》2011,96(12):2159-2166
The thermal stability of chemically synthesized polyaniline (PANI) was examined, including granular (G) polyaniline powders formed conventionally in an HCl medium, and nanorod (NR) samples prepared using a falling-pH synthesis. The samples were examined before and after dedoping (dd) using thermogravimetric analysis (TGA), which showed small mass losses in the 200-300 °C temperature range, and greater mass losses due to oxidative degradation at higher temperatures. Furthermore, samples were treated thermally at 100, 125, 150, 175, 200, 250 and 300 °C for 30 min in air. SEM images did not show any pronounced effect on the morphologies of the samples from thermal treatment up to 300 °C. The ratios of the intensities (Q/B) of the predominantly quinonoid (Q) and benzenoid peaks (B) from FTIR spectroscopic analysis revealed that NR-PANI and NR-PANIdd underwent cross-linking upon thermal treatment up to 175 °C and were oxidized after treatment above 175 °C. G-PANI and G-PANIdd also underwent the same chemical changes with oxidation occurring above 200 °C. The free radical scavenging capacity of the samples was evaluated using the 1,1-diphenyl-2-picrylhydrazyl (DPPH) assay, and was found to be independent of the spin concentrations of the samples. All samples exhibited a rapid decline in free radical scavenging capacity when exposed to temperatures above 200 °C, indicating that any polymer processing should be undertaken at temperatures less than this value to achieve high antioxidant activity. 相似文献
423.
Marija Drev Urša Opara Krašovec Mateja Hočevar Marko Berginc Marjeta Kržmanc Maček Marko Topič 《Journal of Sol-Gel Science and Technology》2011,59(2):245-251
The influence that the degree of polyesterification has on a titanium sol (Ti-sol) prepared via the Pechini method that acts
as a matrix in TiO2 pastes used for dye sensitized solar cells is reported. The different content of the polyester in the Ti-sol was realized
by varying the heating time of the Ti-sol. Titanium dioxide pastes were prepared by introducing a commercial TiO2 nanopowder into the Ti-sols. The TiO2 layers were tested as photoanodes in dye-sensitized solar cells (DSSCs). The most appropriate degree of polyesterification
was achieved by heating the Ti-sol for 0.5 and 1 h, while longer heating deteriorates the TiO2 layer morphology. The highest efficiency of the DSSCs based on an ionic liquid electrolyte was 6.3% measured under standard
test conditions (100 mW/cm2, AM 1.5, 25 °C). 相似文献
424.
Marija Alešković Nikola Basarić Kata Mlinarić‐Majerski 《Journal of heterocyclic chemistry》2011,48(6):1329-1335
A facile three‐step synthesis of 2‐(2‐aminophenyl)pyrrole ( 1 ) and 2‐[(2‐aminomethyl)phenyl]pyrrole ( 2 ) is reported by use of Suzuki coupling of N‐Boc‐pyrrol‐2‐yl boronic acid ( 3 ) and o‐substituted aryl halogenides, followed by hydrogenation. The Pd‐catalyzed cross‐coupling reaction is optimized to be applicable to a wide range of substitued aryl halogenides, with electron‐donating and electron‐withdrawing substituents, 5a , 5b , 5c , 5d , 5e , 5f , 5g . Moreover, Pd‐catalyzed coupling of o‐bromoaniline and 3 could be applied for the one‐step preparation of pyrrolo[1,2‐c]quinazolin‐5(6H)‐one ( 8 ). J. Heterocyclic Chem., (2011). 相似文献
425.
A new synthetic approach is presented for the synthesis of naphthoxazoles and fused heterobenzoxazoles. The starting 5-(aryl/furyl/thienyl/pyridyl ethenyl)oxazoles are prepared from the corresponding α,β-unsaturated aldehydes using Van Leusen reagent in very good yields and are transformed into naphthoxazoles and fused heterobenzoxazoles on irradiation under aerobic conditions and in the presence of iodine. 相似文献
426.
We use exact ray trace to calculate the interferometric Dove prism tolerance to manufacturing errors. We model the manufacturing errors by modifying the position of the prism vertices. The normal to the prism faces establishes the direction of the rays. We determine the prism tolerance by analyzing the optical traversed path rays. We evaluate the change in the image quality introduced by the normal deviation. When the manufacturing tolerance is maintained within ±0.35 arc sec, the maximum wave-front deviation is better than λ/10 at 633 nm. We found that a Dove prism with such tolerance introduces an OPD of two orders of magnitude lesser than a commercial Dove prism. The exact ray trace accuracy of the developed program is validated with the commercially available optical-design program OSLO™. The calculated tolerance complements a previous analysis of a Dove prism for its implementation in a rotationally shearing interferometer. 相似文献
427.
Chilla G Kipp T Menke T Heitmann D Nikolic M Frömsdorf A Kornowski A Förster S Weller H 《Physical review letters》2008,100(5):057403
We report on the direct observation of confined acoustic phonons in the photoluminescence spectra of single CdSe-CdS-ZnS nanocrystals, whose ligands were exchanged to poly(ethylene oxide) (PEO) before they were embedded in a PEO matrix. Modeling a nanocrystal as an elastic sphere, the confined acoustic modes can be assigned to purely radial vibrations: the breathing mode and its two first radial harmonics. In addition to acoustic modes, we also observe longitudinal optical modes of the core material and, remarkably, also of both shell materials. 相似文献
428.
Marija Vukomanovi? Miodrag Mitri? Sre?o D. ?kapin Ema ?agar Janez Plavec Nenad Ignjatovi? Dragan Uskokovi? 《Ultrasonics sonochemistry》2010,17(5):902-908
In this work poly(d,l-lactide-co-glycolide) (PLGA) and a poly(d,l-lactide-co-glycolide)/hydroxyapatite (PLGA/HAp) composite processed in an ultrasonic field at higher (25 °C) and lower (8 °C) temperatures were studied with respect to the molecular properties of the obtained materials. The processing of the PLGA and the PLGA/HAp composite in an ultrasonic field resulted in a change of molar mass averages of the polymer/polymeric part of these materials, while an amorphous structure and a 50:50 lactide-to-glycolide co-monomer ratio were preserved without the formation of crystalline oligomers. However, mobility of polymeric chains obtained after ultrasonic processing was lower indicating ordering the structure of polymeric chains as a result of processing. Additionally, it was observed that the mobility of the PLGA macromolecules was lower within the composite in comparison with the mobility of the chains within the PLGA alone in the case when both were obtained after ultrasonic processing. This was a consequence of the structure formation through the interactions between the PLGA and the HAp. Based on these results different degradation rate of PLGA in composite can be expected, which is important in the application of this material for the controlled drug delivery of medicaments. 相似文献
429.
Maja C. Pagnacco Jelena P. Maksimovi Nenad T. Nikoli Danica V. Bajuk Bogdanovi Milan M. Kragovi Marija D. Stojmenovi Stevan N. Blagojevi Jelena V. Senanski 《Molecules (Basel, Switzerland)》2022,27(15)
Indigo carmine is a commonly used industrial blue dye. To determine its concentration in a commercially available food dye composed of a mixture of indigo carmine and D-glucose, this paper characterizes it through (ATR, KBr) FTIR micro-Raman as well as UV/Vis and clock: Briggs–Rauscher (BR) oscillatory reaction methods. The indigo carmine was detected in the bulk food dye only by applying micro-Raman spectroscopy, indicating a low percentage of the indigo carmine present. This research provides an improvement in the deviations from the experimental Raman spectrum as calculated by the B97D/cc-pVTZ level of theory one, resulting in a better geometrical optimization of the indigo carmine molecule compared to data within the literature. The analytical curves used to determine indigo carmine concentrations (and quantities) in an aqueous solution of food dye were applied by means of UV/Vis and BR methods. BR yielded significantly better analytical parameters: 100 times lower LOD and LOQ compared to commonly used UV/Vis. The remarkable sensitivity of the BR reaction towards indigo carmine suggests that not only does indigo carmine react in an oscillatory reaction but also its decomposition products, meaning that the multiple oxidation reactions have an important role in the BR’s indigo carmine mechanism. The novelty of this research is the investigation of indigo carmine using a clock BR reaction, opening new possibilities to determine indigo carmine in other complex samples (pharmaceutical, food, etc.). 相似文献
430.
Tamara Carevi Marina Kosti Biljana Nikoli Dejan Stojkovi Marina Sokovi Marija Ivanov 《Molecules (Basel, Switzerland)》2022,27(20)
Hesperetin is the aglycone of citrus flavonoid hesperidin. Due to the limited information regarding hesperetin antimicrobial potential and emerging need for novel antimicrobials, we have studied its antimicrobial activity (microdilution assay), antibiofilm activity with different assays in two models (mono- and polymicrobial biofilm), and toxicity (MTT and brine shrimp lethality assays). Hesperetin inhibited growth of all Candida isolates (minimal inhibitory concentration, MIC, 0.165 mg/mL), while it’s inhibitory potential towards Staphylococcus aureus was lower (MIC 4 mg/mL). Hesperetin (0.165 mg/mL) reduced ability of Candida to form biofilms and moderately reduced exopolysaccharide levels in biofilm matrix. Effect on the eradication of 24 h old C. albicans biofilms was promising at 1.320 mg/mL. Inhibition of staphylococcal biofilm formation required higher concentrations of hesperetin (<50% inhibition with MIC 4 mg/mL). Establishment of polymicrobial C. albicans-S. aureus biofilm was significantly inhibited with the lowest examined hesperetin concentration (1 mg/mL) in crystal violet and CFU assays. Hesperetin toxicity was examined towards MRC-5 fibroblasts (IC50 0.340 mg/mL) and in brine shrimp lethality assay (LC50 > 1 mg/mL). Hesperetin is efficient in combating growth and biofilm formation of Candida species. However, its antibacterial application should be further examined due to the cytotoxic effects provoked in the antibacterial concentrations. 相似文献