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31.
Summary A method was devised to assay four forms of vitamin C: L-ascorbic acid (AA), dehydroascorbic acid (DHA), ascorbate-2-mono-
and polyphosphate (AMP, APP), as well as ascorbate-2-monosulphate (AMS), in sample series of different fish tissues and feed.
Direct and indirect detection were combined. Sample extractions were carried out with 0.2 mol L−1 sodium acetate buffer (pH 4.8) and extracts were deproteinized after different chemical or enzymatic reactions, with perchloric
acid. The DHA was reduced to AA with dithioerythritol (DTE). Ascorbate oxidase enzyme was used for the detection of background
and an acidic phosphatase enzyme for the hydrolysis of different phosphate esters. Ascorbate-2-sulphate was detected directly
with help of coinjection of the compound. Chromatographic analysis was carried out with a single column isocratic reverse
phase method. The mobile phase was an aqueous buffer of 0.04 M sodium-acetate, 0.05 mM EDTA, 0.5 mM tetrabutylammonium dihydrogen
phosphate (TBA) adjusted to pH 3.76 with 85% H3PO4 and with 24 mL methanol added to 1000 mL. C-18 columns were used with 0.6 mL min−1 flow rate at 23°C. The vitamin C forms were detected by UV absorption at 250 nm. The determination limit was 1.0–5.0 μg g−1 in AA equivalent. The standard deviations were between 1–6% and depended on the concentrations of vitamin C forms and tissues.
Recoveries were between 90–96% in samples.
Presented at: Balaton Symposium on High-Performance Separation Methods, Siófok, Hungary, September 3–5, 1997 相似文献
32.
V. V. Kuznetsov 《Chemistry of Heterocyclic Compounds》2006,42(5):559-569
New examples of the borylation of a series of five-and six-membered saturated 1,3-and 1,3,2-heterocycles with the formation
of cyclic boric esters are described. The probable mechanism of the reaction is discussed.
__________
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 5, pp. 643–654, May, 2006. 相似文献
33.
Roberto Ballini Noelia Araújo Bazn Giovanna Bosica Alessandro Palmieri 《Tetrahedron letters》2008,49(24):3865-3867
A variety of primary and secondary amines give the conjugate reaction with β-nitroacrylates, via an anti-Michael addition, without any catalyst and/or solvent, allowing good yields of β-nitro-α-amino esters. 相似文献
34.
Three-component reaction of alkyl isocyanides and dialkyl acetylenedicarboxylates in the presence of 2,2,2-trifluoro-N-aryl-acetamides in dichloromethane at ambient temperature afforded dialkyl 2-(N-(aryl)-2,2,2-trifluoroacetamido)-3-(alkylimino) methylene-succinate derivatives in excellent yields. 相似文献
35.
A method for determination of intracellular acyl‐coenzyme A esters in Clostridium acetobutylicum (CA) by high performance liquid chromatography (HPLC) was developed and validated. In our experiment, two important intermediates acyl‐coenzyme A esters including acetyl‐CoA, butyryl‐CoA could be baseline separated on a Zobax‐C18 column with mobile phase composed of the acetonitrile and phosphate buffer (pH 5.0). Samples treated with freeze‐thaw and protein precipitated by addition of trichloroacetic acid could be directly injected for determination of acetyl‐CoA, butyryl‐CoA with a recovery higher than 73%. With this method, the metabolite profiling of the acyl‐coenzyme A esters of CA was obtained. The comparison of the metabolite profiling between the model strain ATCC 824 and a mutant strain EA 2018, which produces higher butanol than the former was performed. Some useful information was concluded for understanding the mechanism of CA for selectively producing the solvent. 相似文献
36.
Runjiang Song Yonggui Robin Chi 《Angewandte Chemie (International ed. in English)》2019,58(26):8628-8630
N‐Heterocyclic carbene catalyzed radical reactions are challenging and underdeveloped. In a recent study, Ohmiya, Nagao and co‐workers found that aldehyde carbonyl carbon centers can be coupled with alkyl radicals under NHC catalysis. An elegant aspect of this study is the use of a redox‐active carboxylic ester that behaves as an single‐electron oxidant to convert the Breslow intermediate into a radical adduct and concurrently release an alkyl radical intermediate as a reaction partner. 相似文献
37.
Anne-Sophie RebstockFlorence Mongin François TrécourtGuy Quéguiner 《Tetrahedron》2003,59(27):4973-4977
The ring deprotonation of 2-(2- and 4-pyridyl)benzoic acids using lithium dialkylamides in THF at rt, and the in situ cyclization afforded 4- and 2-azafluorenones, respectively. 1-Azafluorenone was obtained from ethyl 2-(3-pyridyl)benzoate using a similar protocol. 相似文献
38.
Summary A method for the determination of low relative molecular mass carboxylic acids (C1–C4) in water is reported. The acids are converted to p-bromophenacyl esters prior to a glass-capillary gas chromatographic separation. By utilizing electron-caputre detection the detectability is substantially improved compared to flame-ionization detection. A comparison of three different ways to treat the water samples and to produce the derivatives is made. It is shown that the , p-dibromoacetophenone reagent decomposes to a small extent which limits the utility of the reagent. Nevertheless a detection limit for formic acid of approximately 2.5 mgl–1 is obtained. The method is applied to the determination of formic and acetic acids in a paper kraft water sample. 相似文献
39.
40.
Electrochemical oxidation of malonic esters in acetonitrile in the presence of iodides follows two different pathways depending
on the nature of the cation. In the presence of Lil, alkyl 1,1,2,2,3,3-propanetetracarboxylates were obtained in 85–98% yields.
In the presence of Nal, Kl, or Bu4NI, the formation of 1,1,2,2-ethanetetracarboxylates and their subsequent dehydrogenation to ethenetetracarboxylates was the
main reaction pathway.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 3, pp. 620–623, March, 1997. 相似文献