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   1796篇
  免费   101篇
  国内免费   20篇
化学   1133篇
晶体学   8篇
力学   58篇
数学   188篇
物理学   530篇
  2024年   5篇
  2023年   22篇
  2022年   43篇
  2021年   98篇
  2020年   56篇
  2019年   70篇
  2018年   73篇
  2017年   56篇
  2016年   126篇
  2015年   102篇
  2014年   118篇
  2013年   128篇
  2012年   150篇
  2011年   126篇
  2010年   57篇
  2009年   57篇
  2008年   97篇
  2007年   95篇
  2006年   65篇
  2005年   64篇
  2004年   58篇
  2003年   46篇
  2002年   28篇
  2001年   15篇
  2000年   6篇
  1999年   7篇
  1998年   2篇
  1997年   10篇
  1996年   2篇
  1995年   8篇
  1994年   7篇
  1993年   7篇
  1992年   7篇
  1991年   8篇
  1990年   14篇
  1989年   12篇
  1988年   10篇
  1987年   9篇
  1986年   8篇
  1985年   7篇
  1984年   4篇
  1983年   4篇
  1982年   2篇
  1981年   6篇
  1980年   3篇
  1978年   2篇
  1976年   3篇
  1975年   3篇
  1965年   2篇
  1931年   1篇
排序方式: 共有1917条查询结果,搜索用时 31 毫秒
21.
In this study, it was aimed to investigate the chemical composition and antioxidant activities of two Euphorbia species. The major component of the fatty acid compositions obtained from the petroleum ether extracts was identified as palmitic acid for Euphorbia gaillardotii and Euphorbia macroclada. The main constituents of the essential oils were identified as arachidic acid for E. gaillardotii and tetratetracontane for E. macroclada. Among the 27 studied compounds, hesperidin, rutin, hyperoside and quinic, malic, gallic and tannic acids were found to be the most abundant compounds in the two Euphorbia species. The methanol extracts of E. gaillardotii and E. macroclada showed strong antioxidant activity in all tested methods. Particularly, IC50 values of E. macroclada methanol extract that was the richest in terms of total phenolic-flavonoid contents were found to be lower than α-tocopherol and butylated hydroxytoluene in β-carotene bleaching, 2,2-diphenyl-1-picrylhydrazyl free and ABTS cation radical scavenging methods.  相似文献   
22.
The industrialisation of lignocellulose conversion is impeded by expensive cellulase enzymes required for saccharification in bioethanol production. Current research undertakes cellulase production from pretreated Saccharum spontaneum through Trichoderma viride HN1 under submerged fermentation conditions. Pretreatment of substrate with 2% NaOH resulted in 88% delignification. Maximum cellulase production (2603 ± 16.39 U/mL/min carboxymethyl cellulase and 1393 ± 25.55 U/mL/min FPase) was achieved at 6% substrate at pH 5.0, with 5% inoculum, incubated at 35°C for 120 h of fermentation period. Addition of surfactant, Tween 80 and metal ion Mn+2, significantly enhanced cellulase yield. This study accounts proficient cellulase yield through process optimisation by exploiting cheaper substrate to escalate their commercial endeavour.  相似文献   
23.
This study is related to the isolation of fungal strain for xylanase production using agro-industrial residues. Forty fungal strains with xylanolytic potential were isolated by using xylan agar plates and quantitatively screened in solid-state fermentation. Of all the tested isolates, the strain showing highest ability to produce xylanase was assigned the code Aspergillus niger LCBT-14. For the enhanced production of the enzyme, five different fermentation media were evaluated. Out of all media, M4 containing wheat bran gave maximum enzyme production. Effect of different variables including incubation time, temperature, pH, carbon and nitrogen sources has been investigated. The optimum enzyme production was obtained after 72 h at 30°C and pH 4. Glucose as a carbon source while ammonium sulphate and yeast extract as nitrogen sources gave maximum xylanase production (946 U/mL/min). This study was successful in producing xylanase by A. niger LCBT-14 economically by utilising cheap indigenous substrate.  相似文献   
24.
In this paper, for the first time, an inorganic–organic hybrid material based on ZnO nanoparticles was anchored to a composite made from polythiophene and hexagonally ordered silica (ZnO/PT/SBA-15) for use in solid-phase fibre microextraction (SPME) of medicinal plants. A homemade SPME apparatus was used for the extraction of volatile components of Ziziphora tenuior L. A simplex method was used for optimisation of five different parameters affecting the efficiency of the extraction. The main constituents extracted by ZnO/PT/SBA-15 and PDMS fibres and hydrodistillation (HD) methods, respectively, included pulegone (51.25%, 53.64% and 56.68%), limonene (6.73%, 6.58% and 8.3%), caryophyllene oxide (5.33%, 4.31% and 4.53%) and 1,8-cineole (4.21%, 3.31% and 3.18%). In comparison with the HD method, the proposed technique could equally monitor almost all the components of the sample, in an easier way, in a shorter time and requiring a much lower amount of the sample.  相似文献   
25.
Polyol‐enhanced dispersive liquid–liquid microextraction has been proposed for the extraction and preconcentration of some organophosphorus pesticides from different samples. In the present study, a high volume of an aqueous phase containing a polyol (sorbitol) is prepared and then a disperser solvent along with an extraction solvent is rapidly injected into it. Sorbitol showed the best results and it was more effective on the extraction recoveries of the analytes than inorganic salts such as sodium chloride, potassium chloride, and sodium sulfate. Under the optimum extraction conditions, the method showed low limits of detection and quantification within the ranges of 12–56 and 44–162 pg/mL, respectively. Enrichment factors and extraction recoveries were in the ranges of 2799–3033 and 84–92%, respectively. The method precision was evaluated at a concentration of 10 ng/mL of each analyte, and relative standard deviations were found to be less than 5.9% for intraday (n = 6) and less than 7.8% for interday (n = 4). Finally, some aqueous samples were successfully analyzed using the proposed method and four analytes (diazinon, dimethoate, chlorpyrifos, and phosalone) were determined, some of them at ng/mL level.  相似文献   
26.
Erythrocentaurin is a relatively simple natural product present among the members of Gentianaceae. A preparative method for the isolation of erythrocentaurin from the ethyl acetate fraction of Enicostemma littorale using medium‐pressure liquid chromatography has been reported. The method consisted of a simple step gradient from 10 to 20% ethyl acetate in n‐hexane. Using a 70 × 460 mm Si60 column, this method is capable of processing 20 g of material in <3 h (purity ≈ 97%). The recovery of erythrocentaurin was 87.77%. Estimation of erythrocentaurin in extracts and fractions based on high‐pressure thin‐layer chromatography was carried out on silica gel 60 F254 plates with toluene/ethyl acetate/formic acid (80:18:2 v/v/v) as the mobile phase. The densitometric analysis was performed at 230 nm. A well‐separated compact band of erythrocentaurin appeared at Rf 0.54 ± 0.04. The analytical method showed good linearity in the concentration range of 200–1500 ng/band with a correlation coefficient of 0.99417. The limits of detection and quantification were found to be ≈60 and ≈180 ng/band, respectively. Erythrocentaurin exhibited a concentration‐dependent α‐amylase inhibition (IC50 1.67 ± 0.28 mg/mL). The outcome of the study should be considered for pharmacokinetic and biotransformation studies involving E. littorale.  相似文献   
27.
Amination of 1,1‐dimethylhydrazine with NH2Cl or hydroxylamine‐O‐sulfonic acid yields 2,2‐dimethyltriazanium (DMTZ) chloride ( 3 ) and sulphate ( 4 ), respectively. The DMTZ cation was paired with the nitrogen‐rich anions 5‐aminotetrazolate ( 5 ), 5‐nitrotetrazolate ( 6 ), 5,5′‐azobistetrazolate ( 7 ), and azide ( 8 ), yielding a new family of energetic salts. The synthesis was carried out by metathesis reactions of salts 3 or 4 and a suitable silver or barium salt. To minimize the risks involved when using heavy metal salts, we used electrodialysis for the synthesis of azide 8 , which avoids the use of highly sensitive species. The DMTZ derivatives were characterized by IR and multinuclear NMR spectroscopy, elemental analysis, and X‐ray diffraction. Thermal stabilities were measured using DSC analysis and their sensitivities towards classical stimuli were determined using standard tests. Lastly, the relationship between hydrogen bonding in the solid state and sensitivity is discussed.  相似文献   
28.
In this paper, Sturmian comparison theory is developed for the pair of second‐order differential equations; first of which is the nonlinear differential equations of the form (1) and the second is the half‐linear differential equations (2) where Φα (s ) = |s |α  ? 1s and α 1 > ? > α m  > β  > α m  + 1 > ? > α n  > 0. Under the assumption that the solution of  2 has two consecutive zeros, we obtain Sturm–Picone type and Leighton type comparison theorems for  1 by employing the new nonlinear version of Picone formula that we derive. Wirtinger type inequalities and several oscillation criteria are also attained for  1 . Examples are given to illustrate the relevance of the results. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   
29.
In this study, for the first time, an organic solvent-free air-assisted liquid–liquid microextraction method has been reported for the extraction and preconcentration of phthalic acids (o-phthalic acid, m-phthalic acid, and p-phthalic acid) from edible oil samples. The method is based on the repeated aspirating/injection of an alkaline aqueous solution and the oil sample mixture in a conical bottom centrifuge tube to form a cloudy solution. After phase separation by centrifuging, the sedimented phase is directly analyzed by high-performance liquid chromatography–diode array detection. Under the optimum extraction conditions, the method showed low limits of detection and quantification between 0.11–0.29 and 0.28–0.91 ng mL?1, respectively. Extraction recoveries and enrichment factors were from 81 to 97% and 406 to 489, respectively. The relative standard deviations for the analysis of 5 ng mL?1 of each analyte were less than 5.9% for intraday (n = 6) and interday (n = 5) precisions. Finally, different oil samples were successfully analyzed using the proposed method and m-phthalic acid, and p-phthalic acid were determined in some of them at ng mL?1 level.  相似文献   
30.
This study presents an easy and cost-effective flow-based cloud point extraction (CPE) method for determining partial amounts of two organophosphorus pesticides (phosalone and ethion) in seawater by HPLC–UV–Vis. In continues CPE methodology, the effect of the different column packing type such as carbon nanotube, polyacrylonitrile nanofiber and fiberglass on pesticide extraction was investigated. The Triton X-100 was utilized as nonionic surfactant, and moreover, effect of different parameters such as pH, temperature, extraction time, surfactant concentration, type and volume of the eluent solution on the extraction efficiency was optimized. Under optimum conditions, the figures of merit of the method for phosalone and ethion were obtained as: the enrichment factor (172 and 166), line range (0.8–300 and 0.5–300 µg L?1, R 2 = 0.9973 and 0.9982), relative standard deviation in concentration of 200 µg L?1 (%RSD = %5.4 and %7.99, N = 5) and limit of detection (LOD = 0.24 and 0.14 µg L?1). The suggested method was successfully used for determination of phosalone and ethion in Chabahar Bay seawaters with satisfactory results.  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