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31.
Samet Solak Mehmet Karakuş 《Phosphorus, sulfur, and silicon and the related elements》2013,188(11):1054-1061
Abstract2,4-Bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulfide (Lawesson’s reagent: LR) was reacted with 1,2:5,6-di-O-cyclohexylidene-α-D-glucofuranose and 1,2:5,6-di-O-isopropylidene-α-D-glucofuranose in toluene and gave rise to crude dithiophosphonic acids. The crude dithiophosphonic acids were treated with excess triethylamine and the triethylammonium salts of dithiophosphonic acids (1) and (2) were isolated by crystallization method. Compounds 1 and 2 were characterized by elemental analysis, IR, and NMR (1H-, 13C- and 31P-) spectroscopies and mass spectrometry. In addition, NMR spectra, the electronic properties (the electronic chemical potential, electronegativity, chemical hardness and the global electrophilicity index) and NBO analysis of compound 2 have been calculated by using the Gaussian 16?W program. The electronic properties were calculated using Highest Occupied Molecular Orbital (HOMO) and Lowest Unoccupied Molecular Orbital (LUMO) energies by density functional method (DFT/B3LYP) at 6-31G(d,p) level. The HOMO and LUMO energies are ?5.9 and ?0.72?eV, respectively. The HOMO–LUMO energy difference is 5.18?eV and this value shows that compound 2 has a high stability and low reactivity. 相似文献
32.
N‐vinylimidazole (VIM), and phenacyl methacrylate (PAMA) copolymerized with different feed ratios using 1,4‐dioxane as a solvent and α,α'‐azobisisobutyronitrile (AIBN) as an initiator at 60°C. Structure and composition of copolymers for a wide range of monomer feed were determined by elemental analysis (content of N for VIM‐units) and by Fourier transform infrared spectroscopy through recorded analytical absorption bands for VIM (670 cm?1 for C‐N of imidazole ring) and PAMA (1730 cm?1 for C?O of ester group) units, respectively. Monomer reactivity ratios for VIM (M1)‐PAMA (M2) pair were determined by the application of conventional linearization methods such as Fineman‐Ross (F‐R) and Kelen‐Tüdös (KT) and a nonlinear error invariable model method using a computer program RREVM. The molecular weights (w and n) and polydispersity indices of the polymers were determined using gel permeation chromatography (GPC). Thermal behaviors of copolymers with various compositions were investigated by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Also, the apparent thermal decomposition activation energies (ΔEd) were calculated by Ozawa method using the SETARAM Labsys TGA thermobalance. The antibacterial and antifungal effects of polymers were also tested on various bacteria, fungi and yeast. 相似文献
33.
A laser induced breakdown spectrometry hyphenated with on-line continuous flow hydride generation sample introduction system, HG-LIBS, has been used for the determination of arsenic, antimony, lead and germanium in aqueous environments. Optimum chemical and instrumental parameters governing chemical hydride generation, laser plasma formation and detection were investigated for each element under argon and nitrogen atmosphere. Arsenic, antimony and germanium have presented strong enhancement in signal strength under argon atmosphere while lead has shown no sensitivity to ambient gas type. Detection limits of 1.1 mg L−1, 1.0 mg L−1, 1.3 mg L−1 and 0.2 mg L−1 were obtained for As, Sb, Pb and Ge, respectively. Up to 77 times enhancement in detection limit of Pb were obtained, compared to the result obtained from the direct analysis of liquids by LIBS. Applicability of the technique to real water samples was tested through spiking experiments and recoveries higher than 80% were obtained. Results demonstrate that, HG-LIBS approach is suitable for quantitative analysis of toxic elements and sufficiently fast for real time continuous monitoring in aqueous environments. 相似文献
34.
Ayşegül Doğan Emirhan Nemutlu M. Aykut Özek Hakan Eroğlu Sedef Kır M. Sinan Beksaç 《Chromatographia》2013,76(21-22):1513-1519
Pregnancy alters pharmacokinetic profile of many drugs, because of altering body volume and metabolism rate. Therefore, dosage rates and concentrations of drugs must be controlled during pregnancy. Here, we identified the pharmacokinetic profile of pre-operatively given cefepime in caesarean section and gynecological operations using a simple, rapid, cost-effective and valid liquid chromatographic method. The chromatographic separation was performed using 40 mM, pH 3.2 phosphate buffer containing 6 % methanol as mobile phase at 0.30 mL min?1 flow rate. Gradient elution with methanol was applied to get shorter analysis time without any interference from plasma endogens. During analyses, temperature of column, autosampler and detector were set as 30, 10 and 40 °C, respectively. The detection wavelength was 260 nm and ceftizoxime was used as internal standard. At the optimum conditions, the cefepime analysis from plasma samples was completed in 7 min. Cefepime was extracted from plasma samples using perchloric acid with a very high recovery rate (99.3 %). The method was fully validated according to the Food and Drug Administration guidelines for bioanalytical method validation, and found to be selective, linear, repeatable, reproducible and robust. After validation studies, the method was applied to five caesarean-sectioned and four non-pregnant sectioned women treated with pre-operative, prophylactic single intravenous dose of cefepime (1 g Maxipime®) in order to determine pharmacokinetic profile of cefepime. Peak serum concentrations of cefepime in caesarean-sectioned women at the arterial port after infusion was 70.11 ± 10.74 μg mL?1. The mean elimination half-life, volume of distribution and calculated area under the concentration–time curve (AUC)0–∞ were 1.10 ± 0.23 h, 14.22 ± 2.29 L and 101.55 ± 10.99 μg h mL?1 for caesarean-sectioned women; and 1.14 ± 0.21 h, 14.76 ± 2.92 L and 104.71 ± 36.34 μg h mL?1 for non-pregnant sectioned women, respectively. The area under curve, elimination half-life, maximum plasma concentration and the mean distribution volume of cefepime were not changed in case of pregnancy. 相似文献
35.
Seven [2.2.1] bridged alkenes were cleaved to the corresponding dialdehyde products by neutral heterogenous oxidation with KMnO4-CuSO4.5H2O. While endo, endo-dimethyl bicyclo[2.2.2]oct-5-ene-2,3-dicarboxylate, [2.2.2] bridged alkene, gave the corresponding α-hydroxy ketone, endo, endo-dimethyl bicyclo[3.2.2]non-8-ene-6,7-dicarboxylate afforded a diketone product. 相似文献
36.
N-Aryl-N,N-diphenacylamine dioximes were prepared by the reaction of corresponding arylamines with α-bromoacetophenone oxime in ethanol-water at room temperature. These compounds reacted with aryl isocyanates in acetonitrile to give imidazooxadiazolones 9. The probable mechanism of the reaction is discussed. 相似文献
37.
Murat Güney Selçuk Eşsiz Arif Daştan Metin Balci Ottorino De Lucchi Ertan Şahin Fabrizio Fabris 《Helvetica chimica acta》2013,96(5):941-950
Stereoisomerically pure endo‐ and exo‐7‐halo‐7‐(trimethylstannyl)benzonorcar‐3‐enes (=endo‐ and exo‐(1‐halo‐1a,2,7,7a‐tetrahydro‐1H‐cyclopropa[b]naphthalen‐1‐yl)trimethylstannane) 4 and 6 were selectively obtained by lithium? tin or magnesium? tin transmetalation in good yields (Scheme 2 and 3). The reaction of these compounds with copper(I) thiophene‐2‐carboxylate (CuTC) produced in both cases the corresponding CS‐symmetric bicyclopropylidene (=cyclopropylidenecyclopropane) syn‐ 1 , a single diastereoisomer (Schemes 5 and 6). The structure of syn‐ 1 was undoubtedly elucidated by X‐ray single crystal diffraction. The coupling mechanism of the carbenoid cyclopropane is discussed (Scheme 7). 相似文献
38.
Serkan Yavuz Hamdi Özkan Gülçin Tok Ali Dişli 《Journal of heterocyclic chemistry》2013,50(6):1437-1440
The substituted pyrolidine derivatives with high stereoselectivity were obtained through cycloaddition reaction in the presence of a Lewis acid namely diethylzinc by solvent‐free grinding method. 相似文献
39.
Gülşah Kalaycı Murat Belivermiş Önder Kılıç Sayhan Topcuoğlu Yavuz Çotuk 《Journal of Radioanalytical and Nuclear Chemistry》2013,295(1):239-244
This study was carried out to better understand the biokinetics of radiocesium in clams living in sediment. The accumulation and depuration kinetics of 134Cs were investigated in the Manila clam (Ruditapes philippinarum) under controlled laboratory conditions. The concentration factor was found to be 3.0 for 134Cs in the whole body; however, the concentration factor in the soft part of the clams (12) was significantly higher than those in the whole body and shell (0.80). The depuration kinetics of the radionuclide were described by a two-component exponential model for the whole body. The biological half-lives in the fast and slow components were found to be 0.63 and 22.1 days, respectively. The depuration kinetics for 134Cs in the soft parts were described by a single-component exponential model with a resultant the biological half-life of 18.0 days. 相似文献
40.
Ayşegül Kahraman Gökay Kaynak Gizem Akkaya Orhan Gürler Sezai Yalçın 《Journal of Radioanalytical and Nuclear Chemistry》2013,295(2):1057-1066
Activity concentrations of gross-β, naturally occurring 226Ra, 232Th, 210Pb, 7Be and anthropogenic 137Cs in epiphytic lichens collected from Uluda? Mountain are presented and discussed with the aim of evaluating potential usability of lichens as a biomonitor. The activity concentrations of gross-β, 137Cs, 40K, 226Ra, 232Th, 210Pb and 7Be in the lichen samples were found to be in the range of 177–707, 4.05–94.26, 86–211, below detection limit (BDL)—19.2, BDL—14.0, 229–872, and 72.1–220.7 Bq kg?1 in dry weight, respectively. 137Cs content in collected epiphytic lichens was in descending order: Parmelia sulcata > Lobaria pulmonaria > Pseudevernia furfuracea > Usnea filipendula. The best biomonitor for 137Cs among the lichen species used in this study was determined as Parmelia sulcata. Pearson’s correlation coefficient was calculated between 137Cs and 40K activity concentrations using a statistical package program (SPSS ver. 17.0) and a negative correlation value (R = ?0,323, p = 0,222) was obtained. The highest 226Ra and 232Th activity concentrations were found in Bo?azova Yaylas? which has a geological structure including granitic rocks. It was found that 137Cs and 7Be activity concentrations in species demonstrated an inverse behaviour. The effect of mean annual precipitation and temperature on 7Be activity concentration was determined using multi regression analysis. Also, correlations between the 137Cs and 7Be, and 40K and 7Be were investigated. 相似文献