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   7774篇
  免费   369篇
  国内免费   258篇
化学   3423篇
晶体学   14篇
力学   228篇
综合类   40篇
数学   135篇
物理学   865篇
综合类   3696篇
  2024年   10篇
  2023年   38篇
  2022年   80篇
  2021年   112篇
  2020年   105篇
  2019年   103篇
  2018年   119篇
  2017年   160篇
  2016年   140篇
  2015年   213篇
  2014年   297篇
  2013年   349篇
  2012年   540篇
  2011年   457篇
  2010年   322篇
  2009年   400篇
  2008年   406篇
  2007年   530篇
  2006年   478篇
  2005年   418篇
  2004年   426篇
  2003年   385篇
  2002年   320篇
  2001年   253篇
  2000年   220篇
  1999年   184篇
  1998年   158篇
  1997年   157篇
  1996年   137篇
  1995年   152篇
  1994年   94篇
  1993年   113篇
  1992年   101篇
  1991年   76篇
  1990年   88篇
  1989年   64篇
  1988年   48篇
  1987年   27篇
  1986年   22篇
  1985年   24篇
  1984年   14篇
  1983年   10篇
  1982年   12篇
  1981年   16篇
  1980年   8篇
  1979年   7篇
  1978年   7篇
  1970年   1篇
排序方式: 共有8401条查询结果,搜索用时 46 毫秒
81.
De Marco R  Phan C 《Talanta》2003,60(6):1215-1221
The direct flow injection potentiometric (FIP) analysis of phosphate in hydroponic nutrient solution has been carried out using a cobalt-wire ion-selective electrode (ISE). Synthetic hydroponic nutrient solution, commercial hydroponic nutrient solution and working hydroponic farm nutrient solution were analysed for phosphate using the FIP technique. It is shown that FIP results compare favourably to standard methods of analysis such as spectrophotometry and indirect photometric ion-pair chromatography. Reproducible FIP response curves with a slope of −(47.57±0.03) mV per decade and intercept of −(169.7±0.1) mV were obtained for four separate calibrations in the concentration range 5.0×10−4–1.0×10−2 M H2PO4. Anion corrections for interferences by Cl, NO3 and SO42− were applied to all samples using the selectivity coefficients determined independently using a fixed interference method. Nevertheless, it was found that anion corrections were not necessary, as the deviations fell within the bounds of experimental error for the cobalt-wire ISE technique (i.e.±2–5% R.S.D.). The proposed FIP method enables the direct determination of phosphate in hydroponic nutrient solutions.  相似文献   
82.
Sakai T  Piao S  Teshima N  Kuroishi T  Grudpan K 《Talanta》2004,63(4):893-898
Flow injection spectrofluorimetry with in-line Winklers procedure was developed for the dissolved oxygen (DO) determination. 2-Thionaphthol reacted with iodine produced by Winkler’s method to form fluorescence inactive disulfide compound. To automate the process completely, a 5-channel flow system with a newly designed 16-way valve was assembled. The system consisted of a dispersion coil (DC), a precipitate formation coil (PFC), a precipitate dissolving coil (PDC), and extraction coil (EC). A calibration can be constructed by using a standard iodine solution for dissolved oxygen. The calibration graph was linear over the range 1.2×10−4∼6.0×10−4 mol l−1 iodine (1.96∼9.80 mg O l−1)). The relative standard deviation (n=6) was below 0.3% for the 4×10−4 mol l−1 iodine (6.27 mg O l−1) determination. The sample throughput was 12/h.  相似文献   
83.
《Electroanalysis》2004,16(8):633-639
A potentiometric sensor constructed from a mixture of 25% (m/m) spinel‐type manganese oxide (lambda‐MnO2), 50% (m/m) graphite powder and 25% (m/m) mineral oil is used for the determination of lithium ions in a flow injection analysis system. Experimental parameters, such as pH of the carrier solution, flow rate, injection sample volume, and selectivity for Li+ against other alkali and alkaline‐earth ions and the response time of this sensor were investigated. The sensor response to lithium ions was linear in the concentration range 8.6×10?5–1.0×10?2 mol L?1 with a slope 78.9±0.3 mV dec?1 over a wide pH range 7–10 (Tris buffer), without interference of other alkali and alkaline‐earth metals. For a flow rate of 5.0 mL min?1 and a injection sample volume of 408.6 μL, the relative standard deviation for repeated injections of a 5.0×10?4 mol L?1 lithium ions was 0.3%.  相似文献   
84.
崔洪波  孙君燕 《分析化学》1992,20(7):790-793
本文对微型管状离子选择电极在流动条件下的电化学特征进行了研究,并设计了新的集成微管路离子选择以电极功能块。用此微型装置测定了土壤、血清、水和药物中的K~+、Na~+、pH、Cl~-、F~-、阿托品、东茛菪碱,并和各种标准方法作了比较,获得满意分析结果。  相似文献   
85.
反向流动注射化学发光法测定痕量铁   总被引:10,自引:1,他引:10  
周延秀  孙杰 《分析化学》1997,25(3):334-337
基于邻菲别名林对高碘酸钾-碱性鲁米诺-铁体系发光强度的增敏作用建立了水体中总铁的反向流动性化学发光检测方法。该法线性范围在1×10^-4-10mg/L,检测限为3×10^-6mg/L,对于5×10^-3mg/L Fe测定9次的相对标准偏差为0.9%。此方法已用在水处理中总铁的监测。  相似文献   
86.
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   
87.
During one year continuous use of on-column injection, the typical advantages described in our first report have fully been confirmed. In addition the analysis of large sample volumes has proved promising. Only minor modifications have been applied to the on-column injector device. Broad evidence has been gathered showing that full separation efficiency of the capillary columns after on-column injection is attained only when cold trapping or the solvent effect, as band shortening mechanisms, are working- While, under the conditions of on-column injection, cold trapping is less efficient than with other injection techniques, the opposite holds true for the solvent effect. Compared with splitless injection, the danger of excessive solvent condensation on the column is increased. A working rule is presented for establishing the optimal chromatographic conditions for handling large sample volumes while ensuring full separation efficiency yet avoiding harm to the column.  相似文献   
88.
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   
89.
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   
90.
A heated injection system for a microprocessor-controlled GC has been developed for the (GC)2 analysis of the volatile phase of whole smoke of a cigarette. Effects of injection port temperature and the presence of a Cambridge filter pad are demonstrated. Chromatograms are shown for smoke samples with and without a Cambridge Filter with the sample valve oven at 25°, 165° and 205°C. The use of a flame ionization and a nitrogen-phosphorous detector is illustrated.  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