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   4010篇
  免费   48篇
  国内免费   93篇
化学   2054篇
晶体学   13篇
力学   1097篇
综合类   3篇
数学   348篇
物理学   636篇
  2024年   5篇
  2023年   55篇
  2022年   36篇
  2021年   46篇
  2020年   87篇
  2019年   47篇
  2018年   47篇
  2017年   55篇
  2016年   71篇
  2015年   118篇
  2014年   154篇
  2013年   180篇
  2012年   210篇
  2011年   232篇
  2010年   164篇
  2009年   241篇
  2008年   209篇
  2007年   257篇
  2006年   227篇
  2005年   200篇
  2004年   248篇
  2003年   176篇
  2002年   116篇
  2001年   81篇
  2000年   88篇
  1999年   78篇
  1998年   88篇
  1997年   61篇
  1996年   64篇
  1995年   64篇
  1994年   46篇
  1993年   58篇
  1992年   36篇
  1991年   67篇
  1990年   33篇
  1989年   24篇
  1988年   23篇
  1987年   28篇
  1986年   25篇
  1985年   29篇
  1984年   23篇
  1983年   13篇
  1982年   19篇
  1981年   10篇
  1979年   4篇
  1978年   3篇
  1977年   1篇
  1976年   1篇
  1974年   1篇
  1970年   1篇
排序方式: 共有4151条查询结果,搜索用时 15 毫秒
51.
流动注射在线阴离子树脂预富集火焰原子吸收测定痕量铜   总被引:10,自引:0,他引:10  
刘劲松  陈恒武 《分析化学》1998,26(11):1369-1371
研究了以阴离子交换树脂作吸附剂的流动注射在线微柱预富集火焰原子吸收测定铜的新方法。在最佳条件下富集150s,富集23倍,检出限0.2μg/L,RSD为1.6%,分析速度20次/h。天然水样中可能存在的离子不干扰铜的测定。所建立的方法已用于水样中痕量铜的测定。  相似文献   
52.
钯的高选择性流动注射分析方法的研究   总被引:2,自引:0,他引:2  
Pd(Ⅱ)与DBC-偶氮氯膦在硫酸介质中经加热发生络合显色反应,将此显色反应与流动注射分析技术结合,研究了影响该流动注射显色体系的各种因素,建立了钯的流动注射分析方法.用该方法可不经分离直接测定二次阳极泥和氯化渣中的钯.  相似文献   
53.
A simple and accurate method has been developed for the determination of total mercury in environmental and biological samples. The method utilises an off-line microwave digestion stage followed by analysis using a flow injection system with detection by cold vapour atomic absorption spectrometry.

The method has been validated using two certified reference materials (DORM-1 dogfish and MESS-2 estuarine sediment) and the results agreed well with the certified values. A detection limit of 0.2 ng g−1 Hg was obtained and no significant interference was observed. The method was finally applied to the determination of mercury in river sediments and canned tuna fish, and gave results in the range 0.1–3.0 mg kg−1.  相似文献   

54.
Du J  Li Y  Lu J 《Talanta》2001,55(6):183-1058
It was found that the weak chemiluminescence produced from the reaction of polyhydroxy phenols with luminol in alkaline solution could be strongly enhanced by ferricyanide and ferrocyanide. Based on this found, a new flow injection chemiluminescence method is proposed for the determination of four polyhydroxy phenols: pyrogallol, phlorglucinol, quinol and resorcinol. The detection limits of the method are 0.03 μg ml−1 pyrogallol, 0.03 μg ml−1 phlorglucinol, 0.04 μg ml−1 quinol, and 0.02 μg ml−1 resorcinol. The possible mechanism of CL reactions is also discussed briefly.  相似文献   
55.
A parallel-plate flow chamber consisting of two transparent electro-conductive glass plates was constructed. The two glass plates were set parallel to each other and connected to a potentiostat apparatus to regulate the strength of the electric field between the plates. A microbial cell suspension was flowed through the chamber. This system enabled the application of an electrostatic force to suspend charged particles, e.g. microbial cells, existing between the two plates. The time course of the cell attachment of Pseudomonas syringae pv. atropurpurea NIAES 1309 suspended in 10 mM phosphate buffer solution (pH 7.0) to the glass plate was investigated at various electric field strengths ranging from −4.2 to +4.1 V cm−1. The attachment rate and the maximum number of attached cells increased linearly with the increase in the strength of the positive electric field. In contrast, the rate and the number of cells decreased linearly with the decrease in the strength of the negative electric field. These linear relations gave a specific value for the strength of the electric field (−5.9 ± 0.7 V cm−1) where the electrostatic repulsion and the microbial attachment force were thought to be equal, resulting in no cell attachment. From this value, the electrostatic repulsion, i.e. the microbial attachment force, was calculated to be 5.0 × 10−11 N cell−1 for cells of average size.  相似文献   
56.
Chaozhang Huang 《Talanta》2007,73(2):274-281
Mesoporous titanium dioxide as a novel solid-phase extraction material for flow injection micro-column preconcentration on-line coupled with ICP-OES determination of trace metals (Co, Cd, Cr, Cu, Mn, Ni, V, Ce, Dy, Eu, La and Yb) in environmental samples was described. Possessing a high adsorption capacity towards the metal ions, mesoporous titanium dioxide has found to be of great potential as an adsorbent for the preconcentration of trace metal ions in samples with complicated matrix. The experimental parameters including pH, sample flow rate, volume, elution and interfering ions on the recovery of the target analytes were investigated, and the optimal experimental conditions were established. Under the optimized operating conditions, a preconcentration time of 90 s and elution time of 18 s with enrichment factor of 10 and sampling frequency of 20 h−1 were obtained. The detection limits of this method for the target elements were between 0.03 and 0.36 μg L−1, and the relative standard deviations (R.S.D.s) were found to be less than 6.0% (n =7, c =5 ng mL−1). The proposed method was validated using a certified reference material, and has been successfully applied for the determination of the afore mentioned trace metals in natural water samples and coal fly ash with satisfactory results.  相似文献   
57.
A glucose biosensor with enzyme immobilised by sol–gel technology was constructed and evaluated. The glucose biosensor reported is based on encapsulated GOX within a sol–gel glass, prepared with 3-aminopropyltriethoxy silane, 2-(3,4-epoxycyclohexyl)-ethyltrimetoxy silane and HCl. A flow system incorporating the amperometric biosensor constructed was developed for the determination of glucose in the 1×10−4–5×10−3 mol l−1 range with a precision of 1.5%. The results obtained for the analysis of electrolytic solution for iv administration and human serum samples showed good agreement between the proposed method and the reference procedure, with relative error <5%.  相似文献   
58.
流动注射在线共沉淀预富集火焰原子吸收法测定痕量铜   总被引:3,自引:0,他引:3  
研究了以Ni^2+-DDTC为共沉淀载体,流动注射在线共沉淀预富集-火焰原子吸收光谱法测定痕量铜的体系,在0.3mol.L^-1的硝酸介质中,铜离子在编织反应器中与Ni^2+-DDTC(产生共沉淀,并被收集在编织器内壁上,用甲基异丁基酮(MIBK)在线洗脱沉积物并引入火争原子化器中测定。当富集时间为40s时,40μg.L^-1的铜10次测定的相对标准偏差为3.0%,灵敏度提高60倍,检出限(3σ)  相似文献   
59.
评述了近几年来电化学检测在流动注射分析中的应用,展望了流动注射电化学分析法的发展动向。  相似文献   
60.
流动注射在线萃取-火焰原子吸收法测定食用盐中的锌   总被引:1,自引:0,他引:1  
基于锌与 1 (2 吡啶偶氮 ) 2 萘酚 (简称PAN)形成的配合物可被氯仿萃取 ,从高盐基体样品中分离富集锌 ,利用自行设计的分相器 ,实验确定了最佳的流动注射在线萃取 火焰原子吸收光度法测定锌的流路系统和化学反应条件。在选定的工作条件下 ,其RSD和检出限分别为 4 3 % (c=0 6 μg/mL ,n =1 1 )和0 0 3 μg/mL ,测定速度为 2 5样 /h。用于实际样品的测定 ,加标回收率为 97%~1 0 6 %。  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