全文获取类型
收费全文 | 24877篇 |
免费 | 2688篇 |
国内免费 | 3162篇 |
专业分类
化学 | 10529篇 |
晶体学 | 176篇 |
力学 | 666篇 |
综合类 | 236篇 |
数学 | 1704篇 |
物理学 | 4940篇 |
综合类 | 12476篇 |
出版年
2024年 | 51篇 |
2023年 | 253篇 |
2022年 | 463篇 |
2021年 | 538篇 |
2020年 | 564篇 |
2019年 | 638篇 |
2018年 | 508篇 |
2017年 | 580篇 |
2016年 | 740篇 |
2015年 | 964篇 |
2014年 | 1193篇 |
2013年 | 1516篇 |
2012年 | 1756篇 |
2011年 | 1930篇 |
2010年 | 1728篇 |
2009年 | 1831篇 |
2008年 | 2004篇 |
2007年 | 1963篇 |
2006年 | 1795篇 |
2005年 | 1423篇 |
2004年 | 1237篇 |
2003年 | 1042篇 |
2002年 | 1031篇 |
2001年 | 856篇 |
2000年 | 710篇 |
1999年 | 627篇 |
1998年 | 406篇 |
1997年 | 361篇 |
1996年 | 365篇 |
1995年 | 335篇 |
1994年 | 277篇 |
1993年 | 222篇 |
1992年 | 181篇 |
1991年 | 152篇 |
1990年 | 123篇 |
1989年 | 100篇 |
1988年 | 86篇 |
1987年 | 59篇 |
1986年 | 34篇 |
1985年 | 23篇 |
1984年 | 8篇 |
1983年 | 15篇 |
1982年 | 4篇 |
1980年 | 4篇 |
1978年 | 3篇 |
1977年 | 5篇 |
1973年 | 3篇 |
1970年 | 3篇 |
1965年 | 4篇 |
1936年 | 2篇 |
排序方式: 共有10000条查询结果,搜索用时 109 毫秒
991.
Jianing Mi Min Zhang Hongyang Zhang Yuerong Wang Shikun Wu Ping Hu 《Journal of separation science》2013,36(3):593-601
A high‐efficient and environmental‐friendly method for the preparation of ginsenosides from Radix Ginseng using the method of coupling of ultrasound‐assisted extraction with expanded bed adsorption is described. Based on the optimal extraction conditions screened by surface response methodology, ginsenosides were extracted and adsorbed, then eluted by the two‐step elution protocol. The comparison results between the coupling of ultrasound‐assisted extraction with expanded bed adsorption method and conventional method showed that the former was better than the latter in both process efficiency and greenness. The process efficiency and energy efficiency of the coupling of ultrasound‐assisted extraction with expanded bed adsorption method rapidly increased by 1.4‐fold and 18.5‐fold of the conventional method, while the environmental cost and CO2 emission of the conventional method were 12.9‐fold and 17.0‐fold of the new method. Furthermore, the theoretical model for the extraction of targets was derived. The results revealed that the theoretical model suitably described the process of preparing ginsenosides by the coupling of ultrasound‐assisted extraction with expanded bed adsorption system. 相似文献
992.
Ping Wang Hai tao Lv Ai hua Zhang Hui Sun Guang li Yan Ying Han Xiu hong Wu Xi jun Wang 《Journal of separation science》2013,36(21-22):3511-3516
993.
Sample preparation is always the major bottleneck in analytical chemistry for the determination of pesticide residues. Different sample preparation methods have been proposed due to the wide variety of pesticides used and the inherent complexity of the matrices. In this study, different sample preparation methods including SPE, matrix solid‐phase dispersion, the quick, easy, cheap, efficient, rugged, and safe method, and a one‐step completion method were compared and evaluated for extracting pesticides from lotus seeds. Analysis was carried out using GC with electron‐capture detection. The results showed that good recoveries for tested pesticides were obtained by using Florisil in the four methods, and the extraction efficiency of the one‐step completion method was superior to the other three methods. The one‐step completion method was confirmed to have good linearity, reproducibility, stability, and recovery for the detection of 36 pesticides in lotus seed samples. The data collected from this study are expected to prove useful in regulating the concentration of the residues in lotus seeds, as well as in protecting human health from the hazards posed by these residues. 相似文献
994.
Hang‐Ju Zhao Jian‐Ping Ma Qi‐Kui Liu Yu‐Bin Dong 《Acta Crystallographica. Section C, Structural Chemistry》2013,69(7):716-720
A new 1,3,4‐oxadiazole‐containing bispyridyl ligand, namely 5‐(pyridin‐4‐yl)‐3‐[2‐(pyridin‐4‐yl)ethyl]‐1,3,4‐oxadiazole‐2(3H)‐thione (L), has been used to create the novel complexes tetranitratobis{μ‐5‐(pyridin‐4‐yl)‐3‐[2‐(pyridin‐4‐yl)ethyl]‐1,3,4‐oxadiazole‐2(3H)‐thione}zinc(II), [Zn2(NO3)4(C14H12N4OS)2], (I), and catena‐poly[[[dinitratocopper(II)]‐bis{μ‐5‐(pyridin‐4‐yl)‐3‐[2‐(pyridin‐4‐yl)ethyl]‐1,3,4‐oxadiazole‐2(3H)‐thione}] nitrate acetonitrile sesquisolvate dichloromethane sesquisolvate], {[Cu(NO3)(C14H12N4OS)2]NO3·1.5CH3CN·1.5CH2Cl2}n, (II). Compound (I) presents a distorted rectangular centrosymmetric Zn2L2 ring (dimensions 9.56 × 7.06 Å), where each ZnII centre lies in a {ZnN2O4} coordination environment. These binuclear zinc metallocycles are linked into a two‐dimensional network through nonclassical C—H...O hydrogen bonds. The resulting sheets lie parallel to the ac plane. Compound (II), which crystallizes as a nonmerohedral twin, is a coordination polymer with double chains of CuII centres linked by bridging L ligands, propagating parallel to the crystallographic a axis. The CuII centres adopt a distorted square‐pyramidal CuN4O coordination environment with apical O atoms. The chains in (II) are interlinked via two kinds of π–π stacking interactions along [01]. In addition, the structure of (II) contains channels parallel to the crystallographic a direction. The guest components in these channels consist of dichloromethane and acetonitrile solvent molecules and uncoordinated nitrate anions. 相似文献
995.
Xiuquan Jia Jiping Ma Penghua Che Fang Lu Hong Miao Jin Gao Jie Xu 《Journal of Energy Chemistry》2013,22(1):93-97
Direct conversion of fructose-based carbohydrates to 5-ethoxymethylfurfural (EMF) catalyzed by Lewis acid in ethanol was investigated. It was found that BF3·(Et)2O was favorable for 5-hydroxymethylfurfural (HMF) etherification to EMF. BF3·(Et)2O combination with AlCl3·6H2O with the molar ratio of 1 was an effective catalyst system for synthesis of EMF from fructose-based carbohydrates. 55.0%, 45.4% and 23.9% of EMF yields were obtained from fructose, inulin and sucrose under optimized conditions, respectively. 相似文献
996.
Bai‐Zhan Liu Li Yao Sai‐Jing Zheng Wei‐Miao Wang Xiao‐Lan Zhu Jun Yang 《中国化学会会志》2013,60(8):1055-1061
An efficient and sensitive analytical method based on molecularly imprinted solid‐phase extraction (MISPE) and reverse‐phase ultrasound‐assisted dispersive liquid–liquid microextraction (USA‐DLLME) coupled with LC–MS/MS detection was developed and validated for the analysis of urinary 4‐(methylnitrosamino)‐1‐(3‐pyridyl)‐1‐butanol (NNAL), a tobacco‐specific nitrosamine metabolite. The extraction performances of NNAL on three different solid‐phase extraction (SPE) sorbents including the hydrophilic‐lipophilic balanced sorbent HLB, the mixed mode cationic MCX sorbent and the molecularly imprinted polymers (MIP) sorbent were evaluated. Experimental results showed that the analyte was well retained with the highest extraction recovery and the optimum purification effect on MIP. Under the optimized conditions of MIP and USA‐DLLME, an enrichment factor of 23 was obtained. Good linearity relationship was obtained in the range of 5‐1200 pg/mL with a correlation coefficient of 0.9953. The limit of detection (LOD) was 0.35 pg/mL. The recoveries at three spiked levels ranged between 88.5% and 93.7%. Intra‐ and inter‐day relative standard deviations varied from 3.6% to 7.4% and from 5.4% to 9.7%, respectively. The developed method combing the advantages of MISPE and DLLME significantly improves the purification and enrichment of the analyte and can be used as an effective approach for the determination of ultra‐trace NNAL in complex biological matrices. 相似文献
997.
2‐Alkylthio‐3‐alkyl‐5‐phenylmethylidene‐4H‐imidazol‐4‐ones 6 were synthesized by N‐alkylation and S‐alkylation of 2‐thioxo‐5‐phenylmethylidene‐4‐imidazolidinone 5, which was obtained via cyclization of vinyl isothiocyanate 4 with excess ammonium hydroxide (28% NH3 in water). 相似文献
998.
The BiCl3‐catalyzed reaction of pyrroles with electron‐deficient olefins generated the corresponding Michael adducts in high yields. 相似文献
999.
The Knoevenagel condensation of Meldrum's acid with aromatic aldehydes proceeded efficiently in a reusable ionic liquid, ethylammonium nitrate, at room temperature in the absence of any catalyst with high yields. 相似文献
1000.
Terminal alkynes 1 react with Cp2Zr(H)Cl (Cp = η5-C5H5) and CO to give acylzirconocene chloride derivatives 2, which are trapped with arylsulfenyl chlorides to afford (E)-α,β-unsaturated thioesters. 相似文献