全文获取类型
收费全文 | 25130篇 |
免费 | 458篇 |
国内免费 | 104篇 |
专业分类
化学 | 14009篇 |
晶体学 | 163篇 |
力学 | 763篇 |
综合类 | 9篇 |
数学 | 3471篇 |
物理学 | 7277篇 |
出版年
2023年 | 115篇 |
2022年 | 318篇 |
2021年 | 397篇 |
2020年 | 360篇 |
2019年 | 319篇 |
2018年 | 409篇 |
2017年 | 364篇 |
2016年 | 625篇 |
2015年 | 525篇 |
2014年 | 610篇 |
2013年 | 976篇 |
2012年 | 1257篇 |
2011年 | 1440篇 |
2010年 | 804篇 |
2009年 | 762篇 |
2008年 | 1211篇 |
2007年 | 1185篇 |
2006年 | 1066篇 |
2005年 | 1502篇 |
2004年 | 1535篇 |
2003年 | 1082篇 |
2002年 | 723篇 |
2001年 | 609篇 |
2000年 | 558篇 |
1999年 | 354篇 |
1998年 | 291篇 |
1997年 | 292篇 |
1996年 | 358篇 |
1995年 | 316篇 |
1994年 | 307篇 |
1993年 | 328篇 |
1992年 | 324篇 |
1991年 | 264篇 |
1990年 | 217篇 |
1989年 | 205篇 |
1988年 | 179篇 |
1987年 | 175篇 |
1986年 | 174篇 |
1985年 | 224篇 |
1984年 | 212篇 |
1983年 | 184篇 |
1982年 | 187篇 |
1981年 | 184篇 |
1980年 | 168篇 |
1979年 | 150篇 |
1978年 | 176篇 |
1977年 | 138篇 |
1976年 | 134篇 |
1974年 | 132篇 |
1973年 | 122篇 |
排序方式: 共有10000条查询结果,搜索用时 15 毫秒
981.
It has been developed an automatic stop-flow procedure for sequential photometric determination of anionic and cationic surfactants in a same sample of water. The flow system was based on multicommutation process that was designed employing two solenoid micro-pumps and six solenoid pinch valves, which under microcomputer control carry out fluid propelling and reagent solutions handling. A homemade photometer using a photodiode as detector and two light emitting diodes (LEDs) with emission at 470 nm (blue) and 650 nm (red) as radiation sources, which was tailored to allow the determination of anionic and cationic surfactants in waters. The procedure for anionic surfactant determination was based on the substitution reaction of methyl orange (MO) by the anionic surfactant sodium dodecylbenzene sulfonate (DBS) to form an ion-pair with the cetyl pyridine chloride (CPC). Features such as a linear response ranging from 0.35 to 10.5 mg L−1 DBS (R = 0.999), a detection limit of 0.06 mg L−1 DBS and a relative standard deviation of 0.6% (n = 11) were achieved. For cationic surfactant determination, the procedure was based on the ternary complex formation between cationic surfactant, Fe(III) and chromazurol S (CAS) using CPC as reference standard solution. A linear response range between 0.34 and 10.2 mg L−1 CPC (R = 0.999), a detection limit of 0.05 mg L−1 CPC and a relative standard deviation of 0.5% (n = 11) were obtained. In both cases, the sampling throughput was 60 determinations per hour. Reagents consumption of 7.8 μg MO, 8.2 μg CPC, 37.2 μg CAS and 21.6 μg Fe(III) per determination were achieved. Analyzing river water samples and applying t-test between the results found and those obtained using reference procedures for both surfactant types provide no significant differences at 95% confidence level. 相似文献
982.
I. M. J. J. van de Ven-Lucassen M. F. Kemmere P. J. A. M. Kerkhof 《Journal of solution chemistry》1997,26(12):1145-1167
The Taylor dispersion technique is used to measure the ternary mutual diffusion coefficients of aqueous nonelectrolyte solutions at 25°C. The dispersion of the injected solutes is recorded by a differential refractometer and an ultraviolet-visible detector. The diffusion coefficients are calculated directly by fitting the theoretical dispersion equations to about six experimental curves simultaneously. If the ternary diffusion effects in the measured dispersion profiles are not confused by the inaccuracy of the experimental method or an unfavorable relative detector sensitivity, the diffusion coefficients are precise. For the system methanol + acetone + water, it is shown that the Taylor dispersion method is unsuitable for the determination of all the diffusion coefficients if the methanol mole fraction is less than 0.45 or the acetone mole fraction if more than 0.001. 相似文献
983.
采用体积排斥色谱法/ 示差折光指数/ 直角激光光散射/ 示差粘度三检测联用技术表征了氘化聚苯乙烯、聚苯乙烯和氘化聚苯乙烯- 聚异戊二烯。结果表明,在θ条件下,虽然氘化聚苯乙烯的化学依赖性常数υT,DPS比聚苯乙烯的化学依赖性常数υT,PS大,但25 ℃时在四氢呋喃中,氘化聚苯乙烯的分子尺寸仍小于聚苯乙烯的分子尺寸。由于嵌段共聚物的淋洗体积随组成变化,所以用传统的SEC/RI得不到准确的分子量。经比较膜渗透、小角激光光散射和基质辅助激光脱吸与离子化时间飞行质谱等的实验结果,证明体积排斥色谱法/ 示差折光指数/ 直角激光光散射/ 示差粘度三检测技术能准确地得到氘化二嵌段共聚物的分子量以及其它重要信息。 相似文献
984.
João Miller de Melo Henrique Pablo Cañizares Cristina Saez Elisama Vieira dos Santos Manuel Andrés Rodrigo 《Current Opinion in Electrochemistry》2021
Treatment of polluted soil is one of the priorities in the search of a more sustainable planet. Electrochemically assisted soil remediation has been considered a good option for removing organic contaminants contained in soil, including the removal of volatile organic compounds, associated with gaseous streams produced during the treatment. Also, recently, electrochemical gas treatment technologies have been appointed as promising for the treatment of volatile organic compounds. In this work, we review the current opinion about the most recent studies in both areas. The first section focuses on the production of gaseous compounds during soil remediation by conventional and electrochemical systems. The second section describes the recent progress in the integration of adsorption and absorption with electrochemical processes. Finally, we discuss the holistic application of assisted electrochemical technologies in soil remediation, considering also emerging processes recently published in the literature. 相似文献
985.
Mariana R. Lopes Carlos J. A. de Souza Marina Q. R. B. Rodrigues Daniela A. Costa Ancély F. dos Santos Leandro L. de Oliveira Humberto J. O. Ramos Valéria M. Guimarães Wendel B. Silveira Flávia M. L. Passos Luciano G. Fietto 《Applied biochemistry and biotechnology》2014,172(5):2412-2424
An extracellular β-glucanase secreted by Kluyveromyces marxianus was identified for the first time. The optimal conditions for the production of this enzyme were evaluated by response surface methodology. The optimal conditions to produce β-glucanase were a glucose concentration of 4 % (w/v), a pH of 5.5, and an incubation temperature of 35 °C. Response surface methodology was also used to determine the pH and temperature required for the optimal enzymatic activity. The highest enzyme activity was obtained at a pH of 5.5 and a temperature of 55 °C. Furthermore, the enzyme was partially purified and sequenced, and its specificity for different substrates was evaluated. The results suggest that the enzyme is an endo-β-1,3(4)-glucanase. After optimizing the conditions for β-glucanase production, the culture supernatant was found to be effective in digesting the cell wall of the yeast Saccharomyces cerevisiae, showing the great potential of β-glucanase in the biotechnological production of soluble β-glucan. 相似文献
986.
Thays de Souza Lima Fábio Ruiz Simões 《International journal of environmental analytical chemistry》2017,97(8):768-782
This study is aimed to develop an electroanalytical methodology using a boron-doped diamond electrode to determine simultaneously and selectively carbendazim (CBZ) and carbaryl (CAR). In previous studies using cyclic voltammetry oxidation, peaks were observed at 1.03 V (CBZ) and 1.44 V (CAR), with characteristics of an irreversible process controlled by diffusion of species, with a supporting electrolyte of BR buffer (0.1 mol L?1) and pH adjusted to 6.0. The differences between the potentials for both pesticides, about 400 mV, indicate the possibility of selective determination of CBZ and CAR. The square-wave voltammetric parameters were optimised. The best separation conditions were pH 6.0, square-wave frequency of 100 s?1, pulse amplitude of 50 mV and scan increment of 2.0 mV. These parameters were used to obtain the calibration curves of CBZ and CAR. An analytical curve was constructed in the range concentration of CBZ of 1.3 mg L?1 to 15.3 mg L?1 and CAR of 1.0 mg L?1 to 11.4 mg L?1, respectively. The limits of detection (LOD) and limits of quantification (LOQ) for CBZ were 0.40 mg L?1 and 1.30 mg L?1, respectively. For CAR, the LOD and LOQ were 0.30 mg L?1 and 1.00 mg L?1, respectively. Sensitivity values were 0.78 and 2.60 µA/mg L?1 for CBZ and CAR, respectively. The electroanalytical method was applied in Mikania glomerata infusions. The recovery values were 106.2% and 116.5% for CBZ and CAR, respectively. The results show that the developed method is suitable for application in medicinal plant samples. 相似文献
987.
988.
Solid-phase micro extraction (SPME) and headspace derivatization of clenbuterol followed by GC–FID and GC–SIMMS quantification 总被引:1,自引:0,他引:1
Solid-phase micro extraction (SPME) and on-fiber derivatization followed by Gas Chromatography coupled with Flame Ionization Detection (GC-FID) or Selected Ion Monitoring Mass Spectrometry (GC-SIMMS) allows for simple yet sensitive quantification for the hexamethyldisilazane derivative of the beta-agonist clenbuterol. Using an 85- micro m polyacrylate fiber, the analysis method is optimized with respect to extraction time, derivatization time and temperature, and solution pH. In addition, the use of a rapid temperature ramping injection port allows for optimization of fiber desorption conditions. Under optimal conditions, the limits of detection for the hexamethyldisilazane derivative of clenbuterol are 1.1 ppb by FID and 0.20 ppb by SIMMS. 相似文献
989.
990.
Ines Baer Beatriz de la Calle Philip Taylor 《Analytical and bioanalytical chemistry》2010,396(1):443-456
This review gives an overview of current knowledge about 3-monochloropropane-1,2-diol (3-MCPD) formation and detection. Although
3-MCPD is often mentioned with regard to soy sauce and acid-hydrolysed vegetable protein (HVP), and much research has been
done in that area, the emphasis here is placed on other foods. This contaminant can be found in a great variety of foodstuffs
and is difficult to avoid in our daily nutrition. Despite its low concentration in most foods, its carcinogenic properties
are of general concern. Its formation is a multivariate problem influenced by factors such as heat, moisture and sugar/lipid
content, depending on the type of food and respective processing employed. Understanding the formation of this contaminant
in food is fundamental to not only preventing or reducing it, but also developing efficient analytical methods of detecting
it. Considering the differences between 3-MCPD-containing foods, and the need to test for the contaminant at different levels
of food processing, one would expect a variety of analytical approaches. In this review, an attempt is made to provide an
up-to-date list of available analytical methods and to highlight the differences among these techniques. Finally, the emergence
of 3-MCPD esters and analytical techniques for them are also discussed here, although they are not the main focus of this
review. 相似文献