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   6001篇
  免费   783篇
  国内免费   646篇
化学   3942篇
晶体学   36篇
力学   237篇
综合类   60篇
数学   69篇
物理学   3086篇
  2024年   5篇
  2023年   84篇
  2022年   192篇
  2021年   236篇
  2020年   277篇
  2019年   200篇
  2018年   176篇
  2017年   313篇
  2016年   345篇
  2015年   314篇
  2014年   404篇
  2013年   435篇
  2012年   483篇
  2011年   382篇
  2010年   291篇
  2009年   363篇
  2008年   365篇
  2007年   377篇
  2006年   307篇
  2005年   261篇
  2004年   267篇
  2003年   210篇
  2002年   197篇
  2001年   135篇
  2000年   127篇
  1999年   125篇
  1998年   112篇
  1997年   98篇
  1996年   63篇
  1995年   57篇
  1994年   41篇
  1993年   40篇
  1992年   32篇
  1991年   24篇
  1990年   26篇
  1989年   15篇
  1988年   12篇
  1987年   9篇
  1986年   7篇
  1985年   6篇
  1984年   3篇
  1983年   1篇
  1982年   2篇
  1981年   3篇
  1980年   2篇
  1979年   1篇
  1978年   2篇
  1977年   2篇
  1973年   1篇
排序方式: 共有7430条查询结果,搜索用时 27 毫秒
81.
制备了脱乙酰基魔芋葡甘聚糖(d-KGM)的溶胶-凝胶,用红外光谱表征了其脱乙酰基前后的结构转化.探讨了d-KGM溶胶-凝胶的制备条件对其成膜性能及酶固定化的影响.在此基础上将d-KGM用于电极表面葡萄糖氧化酶的固定,制备了相应的葡萄糖传感器,并对传感器的工作条件进行了优化.所制备的传感器灵敏度为240 nA/mmol/L,线性范围为0.1~8 mmol/L,表观米氏常数KM为19.6 mmol/L,稳定性好,寿命长.实验结果表明d-KGM是一种可用于生物传感器中酶固定化的优良材料.  相似文献   
82.
化学发光消耗型锰传感器   总被引:6,自引:0,他引:6  
化学和生物发光是由化学反应产生的一种光辐射,不需要任何光源。又由于它们具有高灵敏度、宽线性范围和相对比较便宜的仪器等优点,因而在化学和生物传感器领域引起了广泛的兴趣。已用于H_2O_2、乳酸和胆固醇等多种生物活性物质的测定,但未见有金属离子传感器的报道。本文发展了一种新型的全固态模式的消耗型锰离子化学发光传感器。该传感器将除待测物外的所有化学发光反应试剂全部固定在阴离子交换树脂Amberlyst A-27上,于化学发光反应之前,将一定量化学发光试剂从固定化试剂柱上洗脱,与样品中的锰离子产生化学发光。已成功地应用于水样中痕量锰离子的测定。每个固定化试剂柱可连续使用100次以上。 1 实验部分 1.1 仪器和试剂 化学发光传感器由流动系统和检测系统两部分组成。其中流动系统主要由蠕动泵、六通阀、固定化试剂柱和流通池组成。检测系统由光电信增管、负高压、放大器和记录仪组成(图1)。  相似文献   
83.
动力学—压电石英晶体传感器测定水中微量汞的研究   总被引:4,自引:0,他引:4  
基于涂银压电石英晶体对CN^-离子的灵敏响应,应用汞对六氰合铁酸钾与邻二氮杂菲反应的动力学催化作用,建立了动力学-PQC传感器单面触液测定微量汞的新方法。研究了PQC传感器对汞的响应机理,响应曲线,实验条件及共存离子干扰情况。  相似文献   
84.
研究了固相微萃取(SPME)和二氧化锡气体传感器的联用技术对果蔬中有机磷农药残留乐果、氧乐果、甲胺磷、乙酰甲胺磷、马拉硫磷、敌百虫等的快速检测。结果表明,在85℃下,解吸8min,二氧化锡气体传感器在2min内完成对有机磷农药残留的快速检测。零解吸时间测量的甲胺磷的动态响应曲线表明。SPME/二氧化锡气体传感器联用技术对分析SPME的解吸平衡非常有利。  相似文献   
85.
A novel tumor-detection system consisting of complementmediated cytolytic reaction and an image processing system was developed for the simple and rapid determination of tumor cells. The present system consists of a CCD image sensor, image memory board, personal computer, and microscope. When monoclonal antibody 3C4, which is specific to the guinea pig hepatoma L-10, was added to cell suspension, only L-10 cytolysis occurred. Cytolysis caused a decrease in brightness of the cells observed by phase-contrast microscopy. The phase contrast image of the cells before cytolysis was converted to a digitalized signal and stored in computer memory. After cytolysis, a brightness threshold above that of lysed cells was subtracted from the digitalized signal and compared to the signal stored before reaction. L-10 cells in mixed cell suspension were determined specifically by the system. Measurement time was only 2 sec and overall time, including reaction time, was approximately 30 min. Since this method does not require a cell washing process, automation of the whole system is possible.  相似文献   
86.
Sangeun Cho  Chan Kang 《Electroanalysis》2007,19(22):2315-2320
A nonenzymatic glucose sensor with good selectivity for the ascorbic acid oxidation is presented. After the gold polycrystalline electrode was subjected to amalgamation treatment, two advantageous effects were observed. One is the enhancement of the surface roughness and the other is an increase in the catalytic current in the glucose oxidation. Besides the known first effect, the latter provided another advantageous effect in a fabrication of nonenzymatic glucose sensor. Using a gold electrode subjected to amalgamation treatment for 60 s, two calibration curves for glucose oxidation at two different potentials of ?0.1 V and 0.25 V were obtained and compared. At the potential of ?0.1 V, at which no ascorbic acid was oxidized and no interference effect was observed, a current sensitivity of 16 μA cm?2 mM?1 from zero to 10 mM glucose concentration range was obtained. At the other potential of 0.25 V, at which ascorbic acid was easily oxidized, a satisfactory calibration curve with negligible ascorbic acid interference was also obtained together with a more enhanced current sensitivity of 32 μA cm?2 mM?1.  相似文献   
87.
Yantasee W  Timchalk C  Weitz KK  Moore DA  Lin Y 《Talanta》2005,67(3):617-624
There is a need to develop reliable portable analytical systems for on-site and real-time biomonitoring of lead (Pb) from both occupational and environmental exposures. Saliva is an appealing matrix since it is easily obtainable, and therefore a potential substitute for blood due to existing reasonably good correlation between Pb levels in blood and saliva. The microanalytical system is based on flow-injection/stripping voltammetry with a wall-jet (flow-onto) microelectrochemical cell. Samples that contain as little as 1% saliva can cause electrode fouling, resulting in significantly reduced responsiveness and irreproducible quantitations. In addition, incomplete Pb release from salivary protein can also yield a lower Pb response than expected. This paper evaluates the extent of in vitro Pb-protein binding and the optimal pretreatment for releasing Pb from the saliva samples. Even in 50% by volume of rat saliva, the electrode fouling was not observed, due to the appropriate sample pretreatment and the constant flow of the sample and acidic carrier that prevented passivation by the protein. The system offered a linear response over a low Pb range of 1-10 ppb, low detection limit of 1 ppb, excellent reproducibility, and reliability. It also yielded the same Pb concentrations in unknown samples as did the ICP-MS. These encouraging results suggest that the microanalytical system represents an important analytical advancement for real-time non-invasive biomonitoring of Pb.  相似文献   
88.
紫外分光光度法测定甲砜霉素片的含量   总被引:4,自引:0,他引:4  
根据甲砜霉素的紫外吸收特征,建立了以乙腈-水为溶媒、(225±1)nm为最大吸收波长的紫外分光光度法。方法的线性范围为0.5~25.0μg/mL,平均回收率为99.92%,RSD为0.30%。用对照品比较法测定5批甲砜霉素片的含量,并与中国药典方法的测定结果进行比对,结果表明,两种方法的测定结果基本一致。  相似文献   
89.
This article describes the preparation and performance of an optical sensor for continuous measurement of chloride at extracellular (serum) levels (20–200mM). The sensor is based on dynamic quenching of the fluorescence of lucigenin which was photo-immobilized on a hydrogel. Quenching occurs via a collisional mechanism, and the decrease in fluorescence intensity on exposure to 100mM chloride typically is –60%. It allows the determination of chloride in the 1 to 200mM concentration range, with a precision of ±3mM at 120mM. Bromide, iodide and salicylate act as interferents, while the effect of pH and oxygen is negligibly small. The sensor displays strong fluorescence intensity, excellent reproducibility, long-term stability, response times in the order of 2–5min, and is used in a commercial serum and blood chloride analyzer.Received January 21, 2003; accepted April 6, 2003 Published online July 28, 2003  相似文献   
90.
紫外分光光度法测定蔬菜鲜样中的硝酸盐   总被引:9,自引:0,他引:9  
建立了紫外分光光度法测定蔬菜鲜样中硝酸盐含量的方法,经t检验证明,该方法的测定结果与酚二磺酸法无显著性差异,RSD小于4.5%,方法操作简便,适用于蔬菜中硝酸盐含量的测定。  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