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   1326篇
  免费   124篇
  国内免费   155篇
化学   1054篇
晶体学   25篇
力学   62篇
综合类   40篇
数学   24篇
物理学   400篇
  2025年   4篇
  2024年   28篇
  2023年   29篇
  2022年   66篇
  2021年   65篇
  2020年   68篇
  2019年   53篇
  2018年   50篇
  2017年   51篇
  2016年   55篇
  2015年   45篇
  2014年   69篇
  2013年   78篇
  2012年   98篇
  2011年   63篇
  2010年   62篇
  2009年   63篇
  2008年   63篇
  2007年   80篇
  2006年   66篇
  2005年   70篇
  2004年   53篇
  2003年   53篇
  2002年   39篇
  2001年   44篇
  2000年   36篇
  1999年   23篇
  1998年   18篇
  1997年   10篇
  1996年   15篇
  1995年   12篇
  1994年   8篇
  1993年   16篇
  1992年   9篇
  1991年   8篇
  1990年   8篇
  1989年   12篇
  1988年   5篇
  1987年   1篇
  1985年   1篇
  1984年   3篇
  1983年   1篇
  1982年   1篇
  1981年   2篇
  1959年   1篇
排序方式: 共有1605条查询结果,搜索用时 15 毫秒
21.
建立了快速测定Pb(Ⅱ)的瑞利散射(RLS)新方法。在Tris-HCl缓冲介质中,溴化十六烷基三甲基铵(CTMAB)增敏溴甲酚绿(BCG),使瑞利散射显著增强,最大瑞利散射峰位于345nm,CTMAB-BCG进一步与Pb(Ⅱ)结合后生成的三元复合物的瑞利散射增强程度(|ΔIRLS|)与0.006~0.41mg/L范围Pb(Ⅱ)的质量浓度呈线性关系,定量限为0.053mg/kg。方法用于萝卜红色素中Pb(Ⅱ)的测定,回收率为98.5%~102%,相对标准偏差为1.8%~2.5%。  相似文献   
22.
    
2D covalent organic frameworks (COFs) are receiving ongoing attention in semiconductor photocatalysis. Herein, we present a photocatalytic selective chemical transformation by combining sp2 carbon‐conjugated porphyrin‐based covalent organic framework (Por‐sp2c‐COF) photocatalysis with TEMPO catalysis illuminated by 623 nm red light‐emitting diodes (LEDs). Highly selective conversion of amines into imines was swiftly afforded in minutes. Specifically, the π‐conjugation of porphyrin linker leads to extensive absorption of red light; the sp2 ?C=C? double bonds linkage ensures the stability of Por‐sp2c‐COF under high concentrations of amine. Most importantly, we found that crystalline framework of Por‐sp2c‐COF is pivotal for cooperative photocatalysis with (2,2,6,6‐tetramethylpiperidin‐1‐yl)oxyl (TEMPO). This work foreshadows that the outstanding hallmarks of COFs, particularly crystallinity, could be exploited to address energy and environmental challenges by cooperative photocatalysis.  相似文献   
23.
Artificial red cells with crosslinked hemoglobin membranes   总被引:1,自引:0,他引:1  
Artificial cells containing concentrated hemoglobin (Hb) solution were prepared by interfacial polymerization of Hb with glutaraldehyde (GA) in liquid membrane capsules (LMC). A solution containing 30% of Hb was emulsified in mineral oil as red cell-size microdroplets, and this emulsion was dispersed in an aqueous phase containing glutaraldehyde to form LMC. The LMC were semipermeable templates that held the microdroplets of Hb in suspension while GA diffused through the oil to the microdroplet surfaces. The GA crosslinked Hb at the surface of each microdroplet to form an artificial red-cell membrane encapsulating Hb solution. A water-soluble surfactant was used to eject the cells from the LMC and suspend them in saline. Several surfactants were evaluated. Cell size was controlled by agitation speed during preparation of the original emulsion. Cells of 2.52 = ±1.69 μm were prepared. The encapsulated Hb retained capacity to bind and release O2. The cells had aP 50 of 8.9 torr (1200 Pa) and a capacity of 0.55 cc O2/g of total Hb, indicating that the crosslinked portion of the Hb did not contribute to O2 transport.  相似文献   
24.
A simple, rapid and inexpensive solidified floating organic drop microextraction (SFODME) and flow injection flame atomic absorption spectrometric determination (FI-FAAS) method for copper were developed. 3-amino-7-dimethylamino-2-methylphenazine (Neutral red, NR) was used as the complexing agent. Several factors affecting the microextraction efficiency, such as, pH, NR and sodium dodecylbenzenesulfonate (SDBS) concentration, extraction time, stirring rate, and temperature were investigated and optimized. Under optimized experimental conditions an enrichment factor of 541 was obtained for 100 mL of sample solution. The calibration graph was linear in the range of 0.5–20.0 ng mL− 1 and the limit of detection (3 s) was 0.18 ng mL− 1, the limit of quantification (10 s) was 0.58 ng mL− 1. The relative standard deviation (RSD) for 10 replicate measurements of 10 ng mL− 1 copper was 2.7%. The developed method was successfully applied to the extraction and determination of copper in different certified reference materials (Estuarine water, Slew 3 and fortified water, TM 23.2) and real water samples and satisfactory results were obtained.  相似文献   
25.
加替沙星-茜素红体系的紫外特性及加替沙星的测定   总被引:1,自引:0,他引:1  
加替沙星与茜素红反应可形成配合物,使茜素红的紫外吸光度增强,且加替沙星浓度在0.20~110.00mg.L-1范围内与吸光度呈良好的线性关系,以此为基础,建立了测定加替沙星的新方法.将此方法用于片剂、粉针剂和尿液中加替沙星含量的测定,结果与文献报道的荧光法一致.  相似文献   
26.
新型双钼酸盐红色荧光粉的制备及发光性能研究   总被引:1,自引:0,他引:1  
采用高温固相法合成了一种新型的白光LED用双钼酸盐红色荧光粉,利用XRD,F-4500等对其进行了研究。结果表明:该系列荧光粉可以被近紫外光(396 nm)和蓝光(466 nm)有效激发,发射峰值位于615 nm(Eu3+离子的5D0→7F2跃迁)的红光;而且在钾铕双钼酸盐荧光粉KEu(MoO4)2中引入适量的钨酸能加强其发光强度,而不改变样品的发射光谱的形状和发射峰的位置。此外,在确定WO24-/MoO42最佳比值的前提下,文章还详细探讨了碱金属离子相互置换对样品发光性能影响的机制。  相似文献   
27.
《Analytical letters》2012,45(5):955-969
ABSTRACT

Simple, sensitive and selective methods for the determination of trimethoprim (TMP) in pure form and in pharmaceutical formulations are described. The methods are based on the reaction of TMP as a π-electron donor with bromothymol blue (BTB), bromocresol green (BCG) and alizarin red S (ARS) as electron acceptors. The coloured products are quantified spectrophotometrically at their corresponding λmax.

Beer's law is obeyed in case of BTB in the range 2.9-23.2 μg/ml (CHCl3), 2.9-20.0 μg/ml (CH2Cl2) and 5.0-29.0 μg/ml (ClC6H5), in the case of BCG 2.9-27.5 μg/ml (H2O/alc.), 2.9-18.3 μg/ml (CHCl3) and 2.9-20.3 μg/ml (CH2Cl2) and for ARS in the range 3.0-12.0 μg/ml in H2O/alc medium.

The specific absorptivities, molar absorptivities, Sandell sensitivities, standard deviations and percent recoveries are evaluated. Application of the suggested methods to dosage forms is presented and compared with the pharmacopoeial method. The interference from additives and sulfa compounds, especially sulfamethoxazole, has been overcome by extraction into chloroform or methylene chloride.  相似文献   
28.
采用聚丙烯酰胺凝胶法合成了BaTiO3纳米颗粒,利用X射线衍射、傅里叶变换红外光谱、透射电镜和紫外-可见漫反射光谱对样品进行了表征.结果表明,以柠檬酸酸为络合剂、pH=2且在700℃焙烧时可制备出单相BaTiO3纳米颗粒,其形状较为规整,近似呈球形,平均粒径约为55 nm,光学带隙值为3.25 eV.以偶氮染料甲基红为目标降解物,研究了BaTiO3纳米颗粒的光催化性能.结果表明,在紫外光照射下该纳米颗粒表现出较高的催化活性,光催化机理主要为光生空穴的直接氧化.  相似文献   
29.
光谱法和电化学法研究中性红与小牛胸腺DNA的相互作用   总被引:2,自引:0,他引:2  
利用紫外 可见和圆二色光谱(CD)法和伏安方法,研究了小分子染料中性红(NR)与小牛胸腺DNA(CTDNA)的相互作用。实验表明在NR低浓度下,NR能嵌入至核酸双螺旋的碱基内部在G C处与核酸结合,而在较高浓度情况下,嵌入的NR分子与后来的在核酸双螺旋外部的NR分子相互作用发生聚集,从而堆积在DNA双螺旋的表面,同时使核酸的构象由B型转变为Z型。用光谱滴定的方法获得NR与CTDNA作用内部结合常数,分别为:Ka1=2 4×104mol·L-1·cm-1和Ka2=2 1×10-2mol·L-1·cm-1。  相似文献   
30.
提出了共振瑞利散射光谱法测定人体血浆,尿样中加替沙星含量的方法。在p H5.5~6.5的HAc-Na Ac缓冲溶液中,加替沙星(Gatifloxacin,GTFX)与Tb(Ⅲ)反应形成的二元螯合物共振瑞利散射(Resonance Rayleigh Scattering,RRS)强度极弱,但当其进一步与酸性染料茜素红反应形成三元离子缔合物时,RRS显著增强,其最大散射波长分别位于373 nm和605nm处。在373 nm处,方法的线性范围和检出限分别为0~5.26μg·m L-1和7.5 ng·m L-1。本法简便、快速,并具有良好的选择性,用于片剂,人尿液和血浆中加替沙星含量的测定,其回收率在96.1~104.5%。  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