首页 | 本学科首页   官方微博 | 高级检索  
文章检索
  按 检索   检索词:      
出版年份:   被引次数:   他引次数: 提示:输入*表示无穷大
  收费全文   403篇
  免费   22篇
  国内免费   9篇
化学   270篇
晶体学   4篇
力学   18篇
数学   59篇
物理学   83篇
  2023年   1篇
  2022年   8篇
  2021年   16篇
  2020年   14篇
  2019年   28篇
  2018年   31篇
  2017年   24篇
  2016年   29篇
  2015年   12篇
  2014年   25篇
  2013年   54篇
  2012年   37篇
  2011年   26篇
  2010年   12篇
  2009年   22篇
  2008年   19篇
  2007年   22篇
  2006年   13篇
  2005年   8篇
  2004年   5篇
  2003年   3篇
  2002年   1篇
  2001年   5篇
  1997年   2篇
  1994年   1篇
  1989年   2篇
  1985年   2篇
  1981年   1篇
  1980年   2篇
  1978年   4篇
  1977年   2篇
  1975年   1篇
  1974年   2篇
排序方式: 共有434条查询结果,搜索用时 15 毫秒
341.
342.
4-Formylphenyl benzoate was utilized as a versatile precursor for the construction of new series of heterocyclic scaffolds that contain thiazole and thiazolidin-5-one rings. The antibacterial activity of these scaffolds against two types of bacteria was screened and most of them exhibited good activity. Among the synthesized thiazole derivatives, compounds 5, 6, and 8a showed antibacterial activity close to the standard chemotherapeutic (Ampicillin).  相似文献   
343.
Sol–gel coating technology for the preparation of solid-phase microextraction fibers involves a single-step procedure and allows for in situ creation of chemically bonded coatings which are characterized by high thermal and solvent stabilities. A novel titania sol–gel coating was prepared for the first time on a stainless steel fiber and applied for the headspace solid-phase microextraction (HS-SPME) of menthol with gas chromatography and flame ionization detection. Important parameters influencing the efficiency of SPME process, such as extraction time, extraction temperature and ionic strength, were optimized by central composite design. An extraction time of 40 min at 60 °C gave maximum extraction efficiency, when NaCl (10% w/v) was added to the aqueous sample. The analytical characteristics of the proposed method were comparable with other reported fibers. Under optimized conditions, the linearity was between 0.05 and 100 µg mL??1. The relative standard deviations (RSDs) determined at 0.5 µg mL??1 concentration level (n?=?5) were as follows: intra-day RSD 7.26%; inter-day RSD 10.87%; fiber-to-fiber RSD 9.05%. The relative recoveries determined after spiking a mint distillate sample at three concentration levels from 0.067 to 50.0 µg mL??1 varied from 86 to 102%. The proposed method was successfully applied for the analysis of menthol in peppermint samples.  相似文献   
344.
Homopolymerization of methyl acrylate (MA) and methyl methacrylate (MMA) by atom transfer radical polymerization (ATRP) were carried out at 90 °C using methyl-2-bromopropionate (MBP) as initiator, copper halide (CuX, X=Cl, Br) as catalyst, 2,2-bipyridine (bpy) or N,N,N,N,N-pentamethyldiethylenetriamine (PMDETA) as ligand in 1-butanol (less polar and containing OH) and acetonitrile (more polar) solvents. It was found that with CuCl/bpy catalyst ATRP of MA and MMA in 1-butanol proceeded faster than that in acetonitrile. The rate of ATRP of MA and MMA in acetonitrile and 1-butanol was comparable when CuCl/PMDETA used as catalyst system. The number-average molecular weights increased with conversion and polydispersities were low . The ATRP of MA and MMA with vinyl acetate telomer having trichloromethyl end group (PVAc-CCl3) were also used to synthesize new block copolymers. The structures and molecular weight of synthesized PVAc-b-PMA and PVAc-b-PMMA were characterized by 1H NMR, FTIR spectroscopy and gel permeation chromatography (GPC) and shown that the block copolymers were novel.  相似文献   
345.
Summary. Silica sulfuric acid as an inexpensive and recyclable solid acid efficiently catalyzes the Fridedl?nder synthesis of quinolines through a condensation reaction of a 2-aminoaryl ketone with an activated α-CH acid compound under solvent-free conditions in high yields at 100°C.  相似文献   
346.
A new synthesized fluorogenic reagent,8-[(2-pyridine)methylideneamino] quinoline (PMAQ), was utilized for spectrofluorimetric determination of Cu(II) at trace levels. PMAQ, a good fluorogenic reagent, though insoluble in water, but is soluble in ethanol and 20% ethanol-water. The excitation and the fluorescence wavelengths of PMAQ were 310 and 434 nm respectively. When the reagent was complexed with Cu(II), the fluorescence intensity decreased proportionally with the concentration of Cu(II) at pH 4.5 by a static quenching effect. The highest sensitivity to Cu2 determination was shown to be at PMAQ concentration of 1.0×105mol•L-1. In order to enhance the quenching effect, the Cu(II)-PMAQ complex solution was kept at 22 ℃ for 20 min. Though the interferences by Co(II) and Fe(III) were very serious, they were however, completely eliminated by being masked with oxalate and ascorbate ions respectively. The linear dynamic range for Cu(II) determination was between 25—441 µg•L1 with the detection limit of 18 µg•L1 (RSD=3.7%, n=6). The proposed method was successfully applied to the determination of Cu(II) in real samples including human blood serum, commercial tea and wheat flour.  相似文献   
347.
A three-component condensation reaction between an isocyanide, an electron-deficient acetylenic ester and (ethoxycarbonylmethyl)triphenylphosphonium bromide efficiently provides fully substituted N-alkyl-2-triphenylphosphoranylidene glutarimides in a one-pot reaction without any activation or modification.  相似文献   
348.
A novel isocyanide-based four-component reaction between a 2-hydroxybenzaldehyde, Meldrum's acid, an isocyanide, and an aromatic or an aliphatic alcohol efficiently provide 3,4-dihydrocoumarin derivatives in good to excellent yields without using any catalyst or activation. The reaction can be carried out as a simple one-pot protocol at room temperature.  相似文献   
349.
Organotin(IV) complexes of the type [RSnCl3(cis-Ph2PCHCHPPh2)] [R = Me (1), nBu (2), Ph (3)] were prepared by the reaction of RSnCl3 with the rigid bisphosphine ligand, cis-1,2-bis(diphenylphosphino)ethylene in dichloromethane. The complexes have been characterized both in solution and the solid state. Low temperature 31P and 119Sn NMR studies indicate two different phosphorus environments. The crystal structures indicate a weak but chelating mode of coordination of the two phosphorus atoms to tin, leading to a distorted octahedral geometry. In solution the complexes 1-3 undergo a redistribution reaction to form [SnCl4(cis-Ph2PCHCHPPh2)] (4) as one of the products. In order to confirm the redistribution, complex 4 has been prepared separately and characterized both structurally and spectrally.  相似文献   
350.
Let be an open connected subset of the plane, and let be a Banach algebra of analytic functions on . We show that the space of bounded derivations from into is not reflexive. We also obtain similar results when for .

  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号