全文获取类型
收费全文 | 96933篇 |
免费 | 6377篇 |
国内免费 | 7175篇 |
专业分类
化学 | 66724篇 |
晶体学 | 875篇 |
力学 | 5286篇 |
综合类 | 759篇 |
数学 | 11405篇 |
物理学 | 25436篇 |
出版年
2024年 | 127篇 |
2023年 | 906篇 |
2022年 | 1803篇 |
2021年 | 1970篇 |
2020年 | 2403篇 |
2019年 | 2361篇 |
2018年 | 2272篇 |
2017年 | 2891篇 |
2016年 | 3420篇 |
2015年 | 2819篇 |
2014年 | 3410篇 |
2013年 | 6742篇 |
2012年 | 5007篇 |
2011年 | 4896篇 |
2010年 | 4113篇 |
2009年 | 5697篇 |
2008年 | 5387篇 |
2007年 | 6144篇 |
2006年 | 5219篇 |
2005年 | 4455篇 |
2004年 | 3828篇 |
2003年 | 3793篇 |
2002年 | 3921篇 |
2001年 | 2960篇 |
2000年 | 2894篇 |
1999年 | 2570篇 |
1998年 | 2402篇 |
1997年 | 1704篇 |
1996年 | 1663篇 |
1995年 | 1545篇 |
1994年 | 1461篇 |
1993年 | 1136篇 |
1992年 | 1099篇 |
1991年 | 939篇 |
1990年 | 784篇 |
1989年 | 664篇 |
1988年 | 684篇 |
1987年 | 634篇 |
1986年 | 538篇 |
1985年 | 503篇 |
1984年 | 519篇 |
1983年 | 296篇 |
1982年 | 435篇 |
1981年 | 359篇 |
1980年 | 263篇 |
1979年 | 271篇 |
1978年 | 153篇 |
1977年 | 123篇 |
1976年 | 81篇 |
1973年 | 66篇 |
排序方式: 共有10000条查询结果,搜索用时 31 毫秒
981.
环境样品中痕量邻苯二甲酸酯的分离与测定 总被引:11,自引:0,他引:11
本文研究了以小粒径(10-40μ)硅胶柱色谱分离富集、反相高效相色谱分析测定大气颗粒物、土主植物样品中痕量邻苯二甲酸酯的方法,方法操作简单,回收率高,空白值低,利用该方法分析了部分环境样品中邻苯二甲酯酯含量。 相似文献
982.
河口水体中痕量稀土元素的共沉淀预富集-电感耦合等离子体质谱法测定研究 总被引:3,自引:0,他引:3
建立了氢氧化铟共沉淀预富集 -电感耦合等离子体质谱法测定河口水体中痕量稀土元素的方法。实验结果表明 ,在80mg·L -1的In3 +和pH9.5的实验条件下 ,在1.0L水样中添加5.0~200.0ng的混合稀土标准溶液 ,均能定量回收 ,回收率在82.2 %~106.9 %之间。方法的分析流程空白为0.04(Tb)~10.17(La)ng·L -1,检出限在0.17(Yb)~1.46(La)ng·L-1之间 ,精密度 (RSD ,n=3)小于11.7 % ,可满足河口淡水和海水样品中的痕量稀土元素定量分析的要求 相似文献
983.
本工作建立了室温下用凝胶色谱法(GPC)测定聚2,6-二甲基苯醚(PPO)树脂分子量、分子量分布的方法。淋洗剂不采用文献申报道的毒性较大者,也不在较高柱温下进行,而采用甲苯(或氯仿)在室温下测定。对样品在甲苯中溶解温度、浓度和稳定性等都进行了系统研究,找到了最优化条件。GPC数据结合改性PPO(MPPO)产品性能测定结果,经仔细分析找到了影响MPPO产品质量的一个重要因素是PPO树脂中低分子量部分含量。它与产品冲击强度有明显的依赖关系。提出了一个从CPC谱图确定低分子量部分含量的方法。 相似文献
984.
温度及pH敏感的树枝状高分子衍生物合成及药物控制释放研究 总被引:3,自引:0,他引:3
对合成的系列聚酰胺-胺型(PAMAM)树枝状高分子进行端基的羟基化和氯乙酰化两步修饰,使PAMAM最外层接上烷基氯.以修饰产物为引发剂,通过原子转移自由基引发甲基丙烯酸N,N-二甲氨基乙酯(DMAEMA)聚合得到树枝状PAMAM高分子衍生物,并对其结构用FTIR、1H-NMR和粒径分析进行了表征.紫外可见分光光度仪测定证实此高分子具有温度及pH敏感性.通过对小分子药物控制释放研究表明,此树枝状高分子衍生物通过环境pH值可有效地控制小分子药物的释放. 相似文献
985.
Comprehensive two-dimensional liquid chromatographic separation by means of a combination of ion-exchange chromatography (IEC)
and reversed-phase liquid chromatography (RPLC) has been realized and applied to the analysis of components of a traditional
Chinese medicine Flos Lonicera. In the first dimension the components of a Flos Lonicera extract is separated on strong anion-exchange (SAX) column according to the charge-exchange properties of the components.
In the second dimension the components are further fractionated by reversed-phase liquid chromatography (on ODS) on the basis
of their hydrophobicity. The RPLC effluent is desalted and split and the components are identified on-line by use of both
diode-array detection and mass spectrometry with atmospheric pressure chemical ionization (APCI–MS). In this way, the extract
of Flos Lonicera can be rapidly separated, desalted, and analyzed, with determination of molecular weight. More than 58 components of an extract
of Flos Lonicera were well resolved and six were tentatively identified from their UV and mass spectra. 相似文献
986.
离子色谱法同时测定水中六种阳离子 总被引:3,自引:0,他引:3
研究了用抑制电导离子色谱法一次进样同时测定水中Li^ ,Na^ , NH4^ ,Mg^2 ,Ca^2 的色谱法条件,相对标准偏差小于0.5%,加标回收率在97.5%-104.0%。在水质分析中运用t检验法,比较了用钙、镁离子浓度计算和传统方法测定的总硬度之间是否存在显著性差异。 相似文献
987.
M. Piñeiro-Iglesias M. Miñones-Vázquez E. Vázquez-Blanco S. Muniategui-Lorenzo P. López-Mahía D. Prada-Rodríguez 《Chromatographia》2002,56(7-8):483-488
Summary The aim of this work is to establish the best conditions for concentration and purification steps in the trace analysis of
aliphatic and polycyclic aromatic hydrocarbons (PAH) from atmospheric particulate matter by gas chromatography-flame ionisation
detection (GC-FID) and high performance liquid chromatography with ultraviolet and fluorescence detection (HPLC-UV-FL). The
best results for the more volatile compound were obtained with a combination of rotary evaporation and a stream of nitrogen
(near to 100% for aliphatic hydrocarbons and from 70 to 105% for PAH). Two types of solid phase extraction (SPE)cartridges
(Supelclean
tm
LC-Silica SPE tubes and Sep-Pak? Plus silica cartridges) and glass column were examined for the purification and fractionation step. Blank chromatograms of
both types of cartridges analysed by GC-FID made this study difficult, because a PSS (programmed split-splitless) injector
was employed thereby increasing the sensitivity. This problem was not observed in the HPLC-UV-FL blank chromatograms of these
cartridges. Glass columns filled with silica and alumina were chosen because no interference was found in the GC-FID blank
chromatograms and the best recoveries in the fractionation of both aliphatic hydrocarbons and PAH were achieved. This is especially
important when aliphatic hydrocarbons concentrations are lower than 1 μg mL−1. Finally, the selected conditions were applied to the analysis of hydrocarbons in real atmospheric particulate samples. 相似文献
988.
989.
LC-MS/MS method for the confirmatory determination of aromatic amines and its application in textile analysis 总被引:1,自引:0,他引:1
Sutthivaiyakit P Achatz S Lintelmann J Aungpradit T Chanwirat R Chumanee S Kettrup A 《Analytical and bioanalytical chemistry》2005,381(1):268-276
A confirmation method for the determination of 18 aromatic amines originating from azo dyes after reductive cleavage was developed. The method is based on the use of high-performance liquid chromatography/tandem mass spectrometry with atmospheric-pressure chemical ionization. For the identification of the analytes one precursor ion and two daughter ions (multi-reaction monitoring, MRM) were selected and the LC-MS/MS parameters optimized to obtain high sensitivity and selectivity. The linear ranges varied from 0.1–1 to 30–50 g mL–1 with correlation coefficients of 0.99 or better. The applicability of the method to determine o-tolidine (3,3-dimethylbenzidine) and 3,3-dimethoxybenzidine in textiles following reductive cleavage of acid red 114, trypan blue, and Chicago sky blue 6B was demonstrated. 相似文献
990.
The carbobenzyloxy (cbz) protecting group is evaluated for it's potential to enhance the resolution of chiral amine enantiomers using high-performance liquid chromatography (HPLC) and supercritical fluid chromatography (SFC). A series of cbz derivatives of commercially available racemates was prepared and analyzed by enantioselective chromatography using a variety of mobile phases and polysaccharide and Pirkle-type chiral stationary phases (CSPs). The cbz-derivatized product consistently demonstrated enhanced chiral resolution under HPLC and SFC conditions. Improved selectivity and resolution combined with an automated preparative HPLC or SFC system can lead to the rapid generation of highly purified enantiomers of desirable starting materials, intermediates or final products. 相似文献