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991.
Determination of ascorbic acid and its degradation products by high‐performance liquid chromatography‐triple quadrupole mass spectrometry 下载免费PDF全文
Małgorzata Szultka Magdalena Buszewska‐Forajta Roman Kaliszan Bogusław Buszewski 《Electrophoresis》2014,35(4):585-592
This study describes application of liquid chromatography coupled with triple quadrupole mass spectrometry (LC‐MS) for evaluation of vitamin C stability, the objective being prediction of the degradation products. Detection was performed with an UV detector (UV‐Vis) in sequence with a triple‐quad mass spectrometer in the multiple reaction mode. The negative ion mode of ESI and MS‐MRM transitions of m/z 175→115 (quantifier) and 175→89 (qualifier) for ascorbic acid was used. All the validation parameters were within the range of acceptance proposed by the Food and Drug Administration. The method was fully validated in terms of linearity, LOD, LOQ, accuracy, and interday precision. Validation experiments revealed good linearity with R2 = 0.999 within the established concentration range, and excellent repeatability (9.3%). The LOD of the method was 0.1524 ng/mL whereas the LOQ was 0.4679 ng/mL. LC‐MS methodology proves to be an improved, simple, and fast approach to determining the content of vitamin C and its degradation products with high sensitivity, selectivity, and resolving power within 6 minutes of analysis. 相似文献
992.
Electrochemical derivatization‐capillary electrophoresis‐contactless conductivity detection: A versatile strategy for simultaneous determination of cationic,anionic, and neutral analytes 下载免费PDF全文
Mauro Sérgio Ferreira Santos Fernando Silva Lopes Ivano Gebhardt Rolf Gutz 《Electrophoresis》2014,35(6):864-869
The simultaneous determination of cationic, anionic, and neutral analytes in a real sample was demonstrated by coupling electrochemical (EC) derivatization with counter‐EOF CE‐C4D. An EC flow cell was used to oxidize alcohols from an antiseptic mouthwash sample into carboxylic acids at a platinum electrode in acid medium. The carboxylates formed in the derivatization process and other sample ingredients, such as benzoate, saccharinate, and sodium ions, were separated in counter‐flow mode and detected in one run in Tris‐HCl buffer, pH 8.6. Fewer than 5 min were needed to complete each analysis with the automated flow system comprising solenoid pumps for the management of solutions. Insights into the electrochemistry of benzoic acid, present in the sample matrix, were also gained by EC‐CE‐C4D; more specifically, by applying potentials higher than 1.47 V to the platinum electrode, some formiate and minute amounts of salicylate were detected. 相似文献
993.
This work deals with certain parabanic acid (PA) derivatives because they possess great calculated density (>1.8 g · cm–3) and high content of nitrogen (26 %). Computed ballistic properties of eight different parabanic acid derivatives are presented. The structures were optimized at the B3LYP/6‐31G(d, p) level. The calculated data for PA are found to be compatible with the experimental X‐ray data. The detonation performance analyses were done using empirical Kamlet‐Jacobs equations. Additionally, detonation products were assigned and power index were calculated. All the compounds considered are powerful candidates for high energy materials. 相似文献
994.
The ionic liquid 1‐butyl‐3‐methylimidazolium hydrogensulfate, [bmim]HSO4, turned out to be resistant even to strong oxidizers like SO3. Thus, it should be a suitable solvent for the preparation of polysulfates at low temperatures. As a proof of principle we here present the synthesis and crystal structure of K2(S2O7)(H2SO4), which has been obtained from the reaction of K2SO4 and SO3 in [bmim]HSO4. In the crystal structure of K2(S2O7)(H2SO4) (orthorhombic, Pbca, Z = 8, a = 810.64(2) pm, b = 1047.90(2) pm, c = 2328.86(6) pm, V = 1978.30(8) Å3) two crystallographically unique potassium cations are coordinated by a different number of monodentate and bidentate‐chelating disulfate anions as well as by sulfuric acid molecules. The crystal structure consists of alternating layers of [K2(S2O7)] slabs and H2SO4 molecules. Hydrogen bonds between hydrogen atoms of sulfuric acid molecules and oxygen atoms of the neighboring disulfate anions are observed. 相似文献
995.
Crystals of the bis(tert‐butyl)silylene (DTBS) derivatives of the tartaric acids were synthesized from D ‐, L ‐, rac‐, and meso‐tartaric acid and DTBS bis(trifluoromethanesulfonate): two polymorphs of Si2tBu4(L ‐Tart1,2;3,4H–4) (L ‐ 1a and L ‐ 1b ), the mirror image of the denser modification (D ‐ 1b ) as well as the racemate ( 2 ), and the meso analogue Si2tBu4(meso‐Tart1,3;2,4H–4) ( 3 ). The structures were determined by single‐crystal X‐ray diffraction. The threo‐configured D ‐ and L ‐ (and rac‐) tartrates were coordinated by two tBu2Si units forming five‐membered chelate rings, whereas the erythro‐configured meso‐tartrate formed six‐membered chelate rings. The new compounds were analyzed by NMR techniques, including 29Si NMR spectroscopy, and single‐crystal X‐ray crystallography. 相似文献
996.
α-Hydroxyallylphosphinates were stereoselectively converted to γ-chloro allylphosphinates when treated with Ph3P and CCl4, via substitution of hydroxyl and migration of double bond. The reaction was promoted by phosphonium cation that acted as Lewis acid. 相似文献
997.
Juanjuan Song Xinjian Li Apeng Liang Jingya Li Dapeng Zou Yangjie Wu Yusheng Wu 《Tetrahedron letters》2014
A novel CuI/l-proline catalyzed coupling reaction of 1-Boc-3-iodoazetidine with various arylboronic acids which produced aryloxyazetidine derivatives in moderate to good yields was investigated. 相似文献
998.
Conditions are described for one-pot Brønsted acid and organocatalysed enantioselective α-amination of acetals and associated functionalities. Of the organocatalysts screened, proline tetrazole gave the highest ee, while aqueous monochloroacetic acid proved to be the best Brønsted acid activator regarding minimizing racemization and maximizing product yield. The reaction opens up the way for using masked carbonyl functionalities in organocatalysis. 相似文献
999.
K. Raghavendra Rao Akula Raghunadh Ramamohan Mekala Suresh Babu Meruva T.V. Pratap T. Krishna Dipak Kalita Eppakayala Laxminarayana Bagineni Prasad Manojit Pal 《Tetrahedron letters》2014
A dual reactant/catalyst role of glyoxylic acid in the reaction of isatoic anhydride with various amines afforded a novel, robust and rapid synthesis of 3-(un)substituted quinazolin-4(3H)-ones. This metal catalyst-free reaction proceeds via an unusual and unexpected cleavage of C–C bond. A shorter and common route to two alkaloids, that is, rutaecarpine and evodiamine is also accomplished. 相似文献
1000.
The synthesis of 2,4,6-tris[(4-iodo)phenoxy)]-1,3,5-triazine 6, as a new recyclable nonpolymeric analogue of iodobenzene is achieved using the reaction of 2,4,6-trichloro-1,3,5-triazine with 4-iodophenol in the presence of KOH. The application of 6 as a recyclable ‘iodoarene’ is demonstrated for α-tosyloxylation of enolizable ketones via in situ generation of hypervalent iodine(III) species using PTSA and MCPBA as the terminal oxidant. The recyclability of the reagent 6 was possible owing to the facile recovery and reuse from the reaction mixture due to its near insolubility in methanol. 相似文献