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   3624篇
  免费   208篇
  国内免费   135篇
化学   773篇
晶体学   86篇
力学   407篇
综合类   22篇
数学   86篇
物理学   354篇
综合类   2239篇
  2024年   17篇
  2023年   41篇
  2022年   58篇
  2021年   58篇
  2020年   72篇
  2019年   56篇
  2018年   63篇
  2017年   85篇
  2016年   91篇
  2015年   99篇
  2014年   172篇
  2013年   180篇
  2012年   213篇
  2011年   200篇
  2010年   147篇
  2009年   178篇
  2008年   181篇
  2007年   180篇
  2006年   193篇
  2005年   188篇
  2004年   165篇
  2003年   148篇
  2002年   124篇
  2001年   122篇
  2000年   101篇
  1999年   93篇
  1998年   87篇
  1997年   106篇
  1996年   86篇
  1995年   81篇
  1994年   74篇
  1993年   43篇
  1992年   48篇
  1991年   52篇
  1990年   46篇
  1989年   40篇
  1988年   38篇
  1987年   19篇
  1986年   10篇
  1985年   1篇
  1984年   2篇
  1982年   2篇
  1981年   2篇
  1979年   2篇
  1957年   2篇
  1955年   1篇
排序方式: 共有3967条查询结果,搜索用时 15 毫秒
991.
Xi Cheng 《Talanta》2007,71(3):1083-1087
In this paper, a polyamide-modified carbon paste electrode in capillary zone electrophoresis with amperometric detection (CZE-AD) was firstly applied to the determination of four carbamate pesticides: fenobucarb, isoprocarb, metolcarb and carbaryl. The four carbamates were hydrolyzed in alkalescent aqueous solutions, resulting in the formation of 2-sec-butylphenol, 2-isopropylphenol, m-cresol and α-naphthol, which could be determined by amperometry after capillary electrophoretic separation. Under the selected optimum conditions, the four analytes could be perfectly separated within 23 min. The linear ranges of 2-sec-butylphenol, 2-isopropylphenol and m-cresol were from 1.0 × 10−7 to 2.0 × 10−5 mol L−1 and that of α-naphthol was from 2.0 × 10−7 to 2.0 × 10−5 mol L−1 and their detection limits were 3.0 × 10−8, 3.0 × 10−8, 3.0 × 10−8 and 6.0 × 10−8 mol L−1, respectively (S/N = 3). Fenobucarb, isoprocarb, metolcarb and carbaryl can be indirectly determined by this CZE-AD method with recovery of 105, 104, 110 and 98% and R.S.D. of 4, 3, 4 and 3%, respectively. Above results demonstrated that this method was of high sensitivity, good repeatability and could be used in the rapid determination of the pesticide residues.  相似文献   
992.
Summary This paper discusses the use of capillary zone electrophoresis (CZE) with indirect UV detection for the separation and detection of ions. By use of a 70 cm×75 μm i.d. capillary at −15 kV and an electrophoretic buffer containing sodium chromate, 1-butanol, and cetyltrimethylammonium bromide as electroosmotic-flow modifier (pH 8) nine inorganic and organic anions were separated in less than 10 min. By use of the same type of capillary at 20 kV and an electrophoretic buffer containing imidazole and 18-crown-6 (pH 5) eight cations were separated in less than 5 min. The different variables that affect the separation were studied and optimized; the compounds were detected at low mg L−1 levels after hydrodynamic injection under pressure. The method was tested with osmotically treated waters, and the results compared with those obtained by ion chromatography for anion analysis and by atomic absorption spectroscopy for cation analysis.  相似文献   
993.
S. Fu  F. Li  S. G. Chu  X. B. Xu 《Chromatographia》2002,56(1-2):69-72
Summary Acapillary zone electrophoretic method has been optimized to improve selectivity and resolution in the analysis of chlorophenols in waste water. Use of a buffer system containing organic solvent dramatically improved the separation of chlorophenols. It was shown that selectivity was strongly affected by electrolyte pH and the presence of organic modifiers. The results show that the determination of all seventeen chlorinated derivatives of phenol in water can be achieved by use of a single organic modifier. For example, with acetone as organic modifier all 17 chlorophenols could be separated and determined within 20 min. The standard deviation of migration times and peak areas of the chlorophenols were in the ranges 0.48–0.67% and 3.9–5.1% respectively. Detection linear ranges covered two orders of magnitude of concentration with correlation coefficients of 0.998–1.000, except for 4-chlorophenol. Quantitative aspects of capillary zone electrophoresis are also discussed. It was concluded that capillary zone electrophoresis is a potential method for determination of chlorophenol pollutants in waste water.  相似文献   
994.
Summary Several migration modes suitable for capillary zone electrophoretic (CZE) separation of metal ions in the form of 8-hydroxyquinoline-5-sulphonic acid complexes are described and compared. Superior analysis time, resolution, efficiency and detectability were achieved using reversed movement of anionic metal complexes (in the anode-to-cathode direction) under the action of the electroosmotic flow. This method allows the CZE analysis of multicomponent mixtures of transition metal ions as well as aluminium within about six minutes.  相似文献   
995.
Capillary zone electrophoresis (CZE) with on-line UV-detection was used for the determination of arsenite, arsenate, monomethylarsonic acid, dimethylarsinic acid, arsenobetaine and arsenocholine. The method is simple and rapid (<10 min) and allows the determination of six different arsenic species without sample pretreatment. Several instrumental parameters were studied to obtain the best performance (pH of buffer, injection mode, injection time, applied voltage). To determine the arsenic compounds, the instrument was used with a negative potential applied to the injection side of the capillary so that the anions can migrate towards the anode because of their own mobility and charge. The capillary wall was coated with an electro-osmotic flow modifier which reversed the electro-osmotic flow and thus increased also the overall migration of the anions towards the anode. The influence of high concentrations of matrix components such as NaCl, KNO3 and NaNO3, as well as the presence of acids such as HNO3 and HCl was studied. CZE was used for the determination of the oxidation state of arsenic in percolate waters and in the leachate of solidified arsenic containing waste. The lowest detectable concentration was about 100 g/l. A comparison with the results obtained with hydride generation coupled to ICP-MS was made.  相似文献   
996.
The effects of pH on separation parameters such as migration mobility, resolution, sensitivity, column efficiency and peak shape were emphatically studied. Better separation of magnolol and honokiol using capillary zone electrophoresis was achieved by optimizing pH in the range 5.0–11.7. The influences of applied voltage and temperature were also investigated. We adopted a better sample extraction procedure by which higher contents of honokiol and magnolol with sample compositions unchanged were obtained. The analysis was performed with direct UV detection using a 10 mM borate-10 mM phosphate buffer at pH of 11.6. The method was successfully applied to the simultaneous determination of magnolol and honokiol inMagnolia officinalis bark within 9 min.  相似文献   
997.
通过分析IGBT的短路特性,提出了驱动与保护电路、缓冲电路的设计方法,最后介绍了一种实用的死区补偿方法,提高了整机的可靠性,有效减少了因开关时滞、死区造成的逆变器输出电压畸变。  相似文献   
998.
公路平曲线超高运用研究   总被引:1,自引:0,他引:1  
从理论上对平曲线超高进行了分析;对不同半径的超高取值进行安全性评价,提出超高事故多发段的处理对策及常用组合曲线的超高过渡处理办法。  相似文献   
999.
对柴达木盆地冷湖地区可地浸砂岩型铀矿的铀矿化特征及成矿条件进行了分析,通过研究发现在冷湖地区有较好的铀矿化,认为铀矿化主要受层间氧化带控制,并指出了该地区的铀矿化带.  相似文献   
1000.
车轮钢形变断裂过程的原位研究及氢影响   总被引:1,自引:0,他引:1  
在扫描电镜下对CL60车轮钢单边缺口薄试样(厚度≤0.5mm)进行了原位拉伸实验,并研究了氢的影响.在金相显微镜下观察了带预裂纹的厚度为30mm的楔形张开加载试样开裂过程.结果表明,对薄试样拉伸变形时,不论是否有氢,先共析铁素体优先发生塑性变形,微裂纹沿先共析铁素体与珠光体团的边界形核、扩展;在有氢的情况下,微裂纹更容易通过夹杂物的剥落或夹杂物与基体界面的分离而萌生;薄试样拉伸主要是韧窝断口;对厚试样,裂纹主要通过珠光体中渗碳体片层开裂而扩展,断口也因此主要呈解理特征.  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