全文获取类型
收费全文 | 9775篇 |
免费 | 644篇 |
国内免费 | 694篇 |
专业分类
化学 | 9538篇 |
晶体学 | 11篇 |
力学 | 64篇 |
综合类 | 113篇 |
数学 | 94篇 |
物理学 | 1293篇 |
出版年
2024年 | 9篇 |
2023年 | 128篇 |
2022年 | 452篇 |
2021年 | 333篇 |
2020年 | 282篇 |
2019年 | 304篇 |
2018年 | 302篇 |
2017年 | 437篇 |
2016年 | 531篇 |
2015年 | 477篇 |
2014年 | 445篇 |
2013年 | 636篇 |
2012年 | 766篇 |
2011年 | 649篇 |
2010年 | 529篇 |
2009年 | 620篇 |
2008年 | 483篇 |
2007年 | 623篇 |
2006年 | 453篇 |
2005年 | 455篇 |
2004年 | 425篇 |
2003年 | 248篇 |
2002年 | 197篇 |
2001年 | 174篇 |
2000年 | 132篇 |
1999年 | 130篇 |
1998年 | 105篇 |
1997年 | 100篇 |
1996年 | 109篇 |
1995年 | 91篇 |
1994年 | 73篇 |
1993年 | 65篇 |
1992年 | 68篇 |
1991年 | 56篇 |
1990年 | 66篇 |
1989年 | 36篇 |
1988年 | 25篇 |
1987年 | 30篇 |
1986年 | 15篇 |
1985年 | 6篇 |
1984年 | 13篇 |
1983年 | 7篇 |
1982年 | 9篇 |
1981年 | 2篇 |
1980年 | 5篇 |
1979年 | 4篇 |
1976年 | 3篇 |
1975年 | 1篇 |
1966年 | 1篇 |
1959年 | 2篇 |
排序方式: 共有10000条查询结果,搜索用时 0 毫秒
91.
Robert J. Houben Hans-Gerd M. Janssen Piet A. Leclercq Jacques A. Rijks Carel A. Cramers 《Journal of separation science》1990,13(10):669-673
A simple and versatile system is described for the on-line coupling of SFE to capillary GC. The interfacing consists of a programmed temperature vaporizer (PTV) injector. With this injector it is possible to combine solute trapping, elimination of a high flow of extraction fluid, and quantitative transfer of solutes to the seperation column. The problems caused by impurities in the extraction fluid in on-line SFE-GC are discussed. Simple methods are described for the purification of commercially available carbon dioxide. The trapping efficiency of the PTV injector is studied. Applications of the SFE-PTV-GC system are given for the analysis of polymer anti-degradants, polar compounds, and samples with environmental relevance. 相似文献
92.
A novel extraction method, namely dynamic ultrasound-assisted extraction, is investigated. This technique is efficient with respect to both time and solvent consumption because it utilizes ultrasonic energy in dynamic mode during extraction. Polyphenols (chlorogenic acid, esculetin, rutin, scopoletin, and quercitrin) are extracted from a tobacco (Nicotina tobaccum L.) sample for 10 min with 6 mL of solvent. Fresh solvent is continuously pumped through the sample, with which the analytes can be rapidly extracted, and the possibility of degradation efficiently avoided. Methanol involving 0.5% w/v ascorbic acid was used as extraction solvent; optimal flow rate and extraction time were investigated. The extract was cleaned up by C18 disposable cartridge. The spiked and nonspiked tobacco samples were used for the evaluation of the proposed method. Recoveries obtained were varied from 96 to 108% and RSDs from 2.0 to 4.6%. This extraction technique was revealed to recover larger amounts of polyphenols from tobacco, compared to the static ultrasound-assisted extraction method. 相似文献
93.
人尿中异黄酮的高效液相色谱分析 总被引:3,自引:1,他引:3
建立了测定人尿中异黄酮组分(大豆苷原、黄豆黄素、雌马酚、染料木黄酮)含量的反相高效液相色谱法。在尿样中加入黄酮作为内标,异黄酮经酶解后在pH=7.0中性条件下用乙酸乙酯(1∶1)提取,然后用0.02%TFA-M eOH-ACN三元梯度洗脱的方法分离异黄酮。在该条件下,大豆苷原、黄豆黄素、雌马酚、染料木黄酮的检出限分别为12.9 nmol/L、13.9 nmol/L、71.6 nmol/L和11.8 nmol/L;回收率均在89%以上。本方法具有测试步骤简单、准确度高、重现性好等优点,适合大批量样品测定。 相似文献
94.
Jerzy Strzelbicki Witold A. Charewicz Yung Liu Richard A. Bartsch 《Journal of inclusion phenomena and macrocyclic chemistry》1989,7(3):349-361
Separation efficiencies and selectivities in solvent extraction of Co(II) and Ni(H) ammine cations from aqueous solutions into chloroform and toluene and in transport through bulk toluene membranes by proton-ionizable crown ethers have been determined. Six proton-ionizable crown ethers with differing lipophilicities, polyether cavity sizes and ionizable groups (carboxylic and sulfonic acid functions) were examined. Higher selectivity and efficiency for Co(II) ammine cation extraction was observed for the more lipophilic, proton-ionizable crown ethers. Highly lipophilic crown carboxylic acids provided effective and selective transport of Co(II) ammine cations through bulk toluene membranes.Presented in part at the 6th International Symposium on High Purity Materials in Science and Technology: Preparation, Characterization and Application of Well-Defined Materials, Dresden, GDR, May 1985, Poster D91, Poster Abstracts, pp. 144, 145.All extraction and transport experiments were conducted at this location. 相似文献
95.
本文提出用CHCl_3选择性萃取稀土-二安替匹啉甲烷-I~三元络合物的方法,从铁、镍合金中分离微量稀土元素,借偶氮胂Ⅲ光度测定。本文较为详细地研究了稀土三元络合物的定量萃取条件及Cu(Ⅱ).W(Ⅵ)对萃取的影响等。在确定的最佳分离及测定条件下,大多数金属离子不干扰测定。方法的测定下限为0.001%RE,相对标准偏差小于8.0%。 相似文献
96.
97.
A capillary zone electrophoresis (CZE) method with ultraviolet-visible detection has been established and validated for the determination of five phenothiazines: thiazinamium methylsulfate, promazine hydrochloride, chlorpromazine hydrochloride, thioridazine hydrochloride, and promethazine hydrochloride in human urine. Optimum separation was obtained on a 64.5 cm x 75 microm bubble cell capillary using a buffer containing 150 mM tris(hydroxymethyl)aminomethane and 25% acetonitrile at pH 8.2, with temperature and voltage of 25 degrees C and 20 kV, respectively. Naphazoline hydrochloride was used as an internal standard. Field-amplified sample injection (FASI) has been applied to improve the sensitivity of the detection. Considering the influence of parameters affecting the on-line preconcentration (nature of preinjection plug, sample solvent composition, injection times, and injection voltage) and due to the significant interactions among them, in this paper we propose for the first time the application of a multivariate approach to carry out the study. The optimized conditions were as follows: preinjection plug of water for 7 s at 50 mbar, electrokinetic injection for 40 s at 6.2 kV, and 32 microm of H3PO4 in the sample solvent. Also, a solid-phase extraction (SPE) procedure is developed to obtain low detection limits and an adequate selectivity for urine samples. The combination of SPE and FASI-CZE-UV allows adequate linearities and recoveries, low detection limits (from 2 to 5 ng/mL), and satisfactory precisions (3.0-7.2% for an intermediate RSD %). 相似文献
98.
O. I. Artyushin E. V. Sharova I. L. Odinets S. V. Lenevich V. P. Morgalyuk I. G. Tananaev G. V. Pribylova G. V. Myasoedova T. A. Mastryukova B. F. Myasoedov 《Russian Chemical Bulletin》2004,53(11):2499-2507
An efficient method for the synthesis of secondary alkylamides of phosphorylacetic acids (APA) was proposed. The method involves amidation of ethyl phosphorylacetates with primary aliphatic amines. The scope of reaction was determined. Reactions with ethylenediamine and 1,4-diaminobutane yield the corresponding bisamides; in the case of 1,3-diaminopropane, N-(3-aminopropyl)diphenylphosphorylacetamide or N,N-propylenebis(diphenylphosphorylacetamide) was obtained, depending on the reaction conditions. The extraction of americium(III) complexes and the sorption of uranium(VI) by sorbents with physically sorbed APA from nitric acid solutions were studied. There is no correlation between the partition coefficient of americium(III) and the structure of APA; in the sorption of uranium(VI), the degree of extraction depends on the complexone structure.__________Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 2394–2402, November, 2004. 相似文献
99.
100.
阴阳离子型表面活性剂双水相萃取色氨酸衍生物和牛血清白蛋白 总被引:7,自引:0,他引:7
溴化十二烷基三乙胺(C12NE)和十二烷基硫酸钠(SDS)在一定条件下混合可以形成具有清晰界面的两个水相,称为阴阳离子型表面活性剂双水相。作者研究了利用该双水相萃取3种色氨酸衍生物和牛血清白蛋白的可能性.文中采用工作曲线校正扣除表面活性剂背景的影响,萃取结果准确可信。 相似文献