全文获取类型
收费全文 | 2501篇 |
免费 | 49篇 |
国内免费 | 63篇 |
专业分类
化学 | 2510篇 |
晶体学 | 1篇 |
力学 | 2篇 |
综合类 | 16篇 |
数学 | 2篇 |
物理学 | 82篇 |
出版年
2024年 | 1篇 |
2023年 | 14篇 |
2022年 | 18篇 |
2021年 | 28篇 |
2020年 | 39篇 |
2019年 | 26篇 |
2018年 | 30篇 |
2017年 | 28篇 |
2016年 | 50篇 |
2015年 | 63篇 |
2014年 | 53篇 |
2013年 | 118篇 |
2012年 | 140篇 |
2011年 | 140篇 |
2010年 | 138篇 |
2009年 | 121篇 |
2008年 | 93篇 |
2007年 | 118篇 |
2006年 | 132篇 |
2005年 | 98篇 |
2004年 | 103篇 |
2003年 | 50篇 |
2002年 | 39篇 |
2001年 | 39篇 |
2000年 | 47篇 |
1999年 | 44篇 |
1998年 | 39篇 |
1997年 | 35篇 |
1996年 | 46篇 |
1995年 | 43篇 |
1994年 | 62篇 |
1993年 | 45篇 |
1992年 | 71篇 |
1991年 | 39篇 |
1990年 | 43篇 |
1989年 | 34篇 |
1988年 | 68篇 |
1987年 | 32篇 |
1986年 | 43篇 |
1985年 | 89篇 |
1984年 | 43篇 |
1983年 | 18篇 |
1982年 | 28篇 |
1981年 | 15篇 |
1980年 | 21篇 |
1979年 | 25篇 |
1978年 | 3篇 |
1977年 | 1篇 |
排序方式: 共有2613条查询结果,搜索用时 687 毫秒
61.
62.
Alfred Deege Heribert Husmann Eduard Hübinger Frank Kobor Gerhard Schomburg 《Journal of separation science》1993,16(10):587-593
Complex mixtures of partially alkylated cyclodextrins can be analyzed by both HPLC and high temperature capillary GC. Because of the limited efficiency of LC, suitable analytical and preparative separations can be achieved only with systems of carefully optimized selectivity. Using LC it has been possible to isolate and purify single cyclodextrin species from very complex mixtures of components which contain unreacted hydroxyl groups in addition to the alkoxy groups. Analysis of the reaction mixtures and of fractions taken from LC separations can be performed with advantage by high resolution capillary GC at high temperatures between 300 and 400 °C. The thermal stability of partially alkylated cyclodextrins in high temperature GC is considerably increased by trimethylsilylation of the free hydroxyl groups. Fast atom bombardment mass spectrometry and proton NMR were used to identify species isolated from the preparative LC separations. 相似文献
63.
选用HP-NINOWax毛细管色谱柱及氢火焰离子化检测器(FID),采用程序升温,建立了4种脂肪烷基二甲基叔胺的分析方法。结果表明,4种脂肪烷基二甲基叔胺质量浓度在0.005~1.0 g/L范围内,其峰面积与质量浓度有良好的线性关系,相关系数(R2)在0.9996以上。检出限(LODs,信噪比为3)在0.001~0.002 g/L之间,定量限(LOQs,信噪比为10)在0.003~0.005 g/L之间,回收率在90%~130%之间,相对标准偏差为1.3%~6.9%(n=6)。方法的线性范围宽、回收率高、选择性好,可用于叔胺的产品质量分析及生产过程控制分析。利用该方法对阳离子表面活性剂合成反应中十六烷基二甲基叔胺进行监测,结果很好地符合双分子亲核取代反应。该方法比滴定分析法更快速、精确,与液相色谱法相比,不需要进行柱前衍生或者使用色谱-质谱联用仪器。 相似文献
64.
65.
Surface modification of soft-glass capillaries for gas chromatography by treatment with water vapour
“Leaching” or “etching” by strong mineral acids seems to be a necessary pretreatment step for the most commonly used deactivation procedures of glass capillaries by reaction with either polyethylene glycol or silylation reagents. The acidic sites which are formed on the surface during this acid treatment cannot be completely removed by the subsequent deactivation process. This drawback can be overcome by performing the leaching with water vapour, resulting in an accumulation of cations at the surface and a decrease in the number of silanol groups. Capillaries of this type show excellent properties for the chromatography of strongly basic compounds. After the wash-out of the alkaline surface layer, the acidity of the support is suited for the chromatography of strongly basic as well as strongly acidic compounds. Due to a lack of reactive acidic sites, special deactivation procedures have to be applied to capillaries produced in this way. 相似文献
66.
The possibility to perform gas chromatographic analysis using both a mass detector and a selective nitrogen-phosphorous detector will enable highly sensitive analytical results and an optimal identification reliability. In this work we describe an easily workable technical solution, which has been accomplished in our laboratory and the application of the above system to analytical procedures for the detection and determination of nitrogenous herbicides in drinking water and phosphorylated pesticides in agricultural products is discussed. 相似文献
67.
用硅胶-氧化铝柱色谱预分离和色谱-质谱分析研究了两种褐煤超临界流体抽提物中脂肪烃馏分组成结构特征。结果表明,除主要成份正构烷烃(C_(13)~C_(33))外,尚有少量的类异戊二烯烃(姥鲛烷、植烷等)和萜烷。其中萜烷以五环三萜为主(C_(27)、C_(29)~C_(32)藿烷类化合物),并有一定量的C_(27)、C_(29)和C_(30)藿烯,倍半萜和三环二萜烷含量很少。未检出甾烷。此外,还检出一完整系列的烯烃。试验结果表明,超临界流体抽提条件对褐煤抽出物各组分、含量及其分布有一定的影响。 相似文献
68.
Summary Diaromatics are geochemically significant constituents of crude oils. Their determination is usually achieved by elaborate prefractionation methods, such as medium pressure liquid chromatography and HPLC, prior to capillary gas chromatography. The present contribution describes the quantitative analysis of methylnaphthalenes, ethylnaphthalenes, and dimethylnaphthalenes in selected crude oils by two-dimensional capillary GC. Since the method does not comprise any work-up procedure the determination of geochemical parameters (alkylnaphthalene concentration ratios) is performed on the original, untreated crude oil samples. Accordingly, the analytical results reflect the original composition. The influence by evaporational losses in the laboratory is minimized. 相似文献
69.
Selective detection and identification of Se containing compounds--review and recent developments 总被引:5,自引:0,他引:5
The complexity of selenium (Se) chemistry in the environment and in living organisms presents broad analytical challenges. The selective qualitative and quantitative determination of particular species of this element is vital in order to understand selenium's metabolism and significance in biology, toxicology, clinical chemistry and nutrition. This calls for state-of-the-art analytical techniques such as hyphenated methods that are reviewed with particular emphasis on interfaced separation with element-selective detection and identification of the detected selenium compounds. Atomic spectral element specific detection for monitoring chromatographic eluent enabled quantitative determination of selenium species in selenized yeast and qualitative measurement for breath samples. Gas chromatography with atomic emission detection (AED) of ethylated species and fluoroacid ion pair HPLC applied to the analysis of currently produced or archived selenized yeast and Brassica juncea have revealed the presence of a previously unrecognised Se-S amino acid, S-(methylseleno)cysteine. 相似文献
70.
气相色谱法测定废水中的烷基汞 总被引:4,自引:1,他引:4
以巯基棉(SCF)为吸附剂,用柱上富集技术,浓缩富集水中的烷基汞(氯代甲基汞,氯代乙基汞)。用少量的2mol/LHCl洗脱,用甲苯作萃取剂从洗脱液中萃取烷基汞。对于简单水体,该有机相可直接用于气相色谱测定;对于复杂水体,采用反萃取的方法测定,即可进一步浓缩,又可减少背景峰。用玻璃填充柱-电子捕获检测器响应的气相色谱法测定,最低检测限为8.6×10 ̄(-12)g,可检测到废水中0.34ng/L的单一烷基汞(2.5L水样)。对样品的保存条件也作了探索。 相似文献