全文获取类型
收费全文 | 10391篇 |
免费 | 503篇 |
国内免费 | 128篇 |
专业分类
化学 | 7372篇 |
晶体学 | 92篇 |
力学 | 510篇 |
综合类 | 3篇 |
数学 | 1274篇 |
物理学 | 1771篇 |
出版年
2024年 | 24篇 |
2023年 | 93篇 |
2022年 | 473篇 |
2021年 | 433篇 |
2020年 | 359篇 |
2019年 | 444篇 |
2018年 | 450篇 |
2017年 | 370篇 |
2016年 | 606篇 |
2015年 | 420篇 |
2014年 | 572篇 |
2013年 | 1068篇 |
2012年 | 816篇 |
2011年 | 774篇 |
2010年 | 558篇 |
2009年 | 451篇 |
2008年 | 496篇 |
2007年 | 439篇 |
2006年 | 311篇 |
2005年 | 318篇 |
2004年 | 193篇 |
2003年 | 192篇 |
2002年 | 160篇 |
2001年 | 83篇 |
2000年 | 55篇 |
1999年 | 64篇 |
1998年 | 41篇 |
1997年 | 52篇 |
1996年 | 48篇 |
1995年 | 35篇 |
1994年 | 39篇 |
1993年 | 20篇 |
1992年 | 37篇 |
1991年 | 33篇 |
1990年 | 30篇 |
1989年 | 36篇 |
1988年 | 33篇 |
1987年 | 34篇 |
1986年 | 30篇 |
1985年 | 37篇 |
1984年 | 35篇 |
1983年 | 21篇 |
1982年 | 28篇 |
1981年 | 19篇 |
1980年 | 23篇 |
1979年 | 20篇 |
1978年 | 18篇 |
1977年 | 13篇 |
1976年 | 15篇 |
1974年 | 16篇 |
排序方式: 共有10000条查询结果,搜索用时 15 毫秒
101.
Flow injection chemiluminescence determination of hydrazine by oxidation with chlorinated isocyanurates 总被引:1,自引:0,他引:1
A rapid and sensitive flow injection chemiluminescence (CL) method is described for the determination of hydrazine based on the CL generated during its reaction with either sodium dichloroisocyanurate (SDCC) or trichloroisocyanuric acid (TCCA) in alkaline medium. The emission intensity is greatly enhanced if dichlorofluorescein (DCF) as sensitizer is present in the reaction medium. The presence of citrate prevents the precipitation of some cations in the reaction medium and also causes an enhancement in emission intensity. The effect of analytical and flow injection variables on these CL systems and determination of hydrazine are discussed. The optimum parameters for the determination of hydrazine were studied and were found to be the following: SDCC and TCCA both 1x10(-3) M; NaOH, 2x10(-1) M; DCF, 5x10(-6) M; citrate, 1x10(-3) M and flow rate, 3.8 ml min(-1). The optimized method yielded 3sigma detection limits of 2x10(-7) and 3x10(-7) M for hydrazine with SDCC and TCCA oxidants, respectively. The method is simple, fast, sensitive, and precise and was applied to the determination of hydrazine in water samples. 相似文献
102.
Ali Z. Abu-Zuhri 《Microchemical Journal》1984,29(3):345-349
A spectrophotometric study of the Th(IV) complex of a new reagent 2-(5-Bromo-2- pyridylazo)-5-diethylaminophenol (5-Br-PADAP) is presented. A reddish brown complex is formed at pH 4.86, and shows maximal absorbance at 580 nm with molar absorptivity of 1.66 × 105 mol−1 cm−1 liter. Beer's law is obeyed over the range 0.0 to 15 μg of thorium. Rare earths ions like La3+, Ce3+, and Y3+ do not interfere because they form complexes with 5-Br-PADAP at higher pH's (>9.94) (1). A new method for determining trace amounts of thorium is proposed, which possesses the advantages of high sensitivity and selectivity. 相似文献
103.
The oxidation of some xylenols with iodine in aqueous ethanolic solutions in the presence of silver ions as a catalyst was investigated and used for microdetermination of these reductants. The study of these redox reactions and the microdetermination of these phenols were performed by volumetric and spectrophotometric methods. These methods were compared. The spectrophotometric method was more accurate at very low concentrations (60–488 μg). The volumetric methods used silver ions as catalyst. The potentiometric method is more accurate than the visual method. Possible schemes for the course of these redox reactions were suggested. One electron processes for oxidation of xylenols have been indicated. 相似文献
104.
105.
Syed Laik Ali 《Analytical and bioanalytical chemistry》1973,262(4):278-282
The different aspects of Vitamin D3 determination and the data reported in the literature are discussed. The spectrophotometric determination of Vitamin D3 in cod-liver oil is carried out after the alkaline saponification, extraction of unsaponified parts, precipitation of accompanying sterols and the column- and thin-layer chromatographic purification and separation of vitamin D3 on 40 cm plates from other vitamins. The dyestuff α-naphtholbenzein is suited well as standard substance for the better location and identification of vitamin D3 zone on the thin-layer plate. The results obtained from the chemical method were checked through the simultaneous biological determination. 相似文献
106.
A novel 3D polymeric heteropolynuclear sodium(I) lead(II) complex containing different ligands, [NaPb(ClO4)(en)(NO2)2] was synthesized and characterized by elemental analysis and IR, and 1H‐, 13C‐, and 207Pb‐NMR spectroscopy. The single‐crystal X‐ray data of [NaPb(ClO4)(en)(NO2)2]n established that the complex is a three‐dimensional polymer, [(en)Pb(μ3‐ONO)2Na(μ3‐ONO)2Na(μ‐O2ClO2)Na]n. The Pb and Na atoms have four‐ and eight‐coordinate geometry, respectively. The lone pair of electrons at the PbII atom is ‘stereochemically active’. 相似文献
107.
Enhancing the enzymatic hydrolysis of cellulosic materials using simultaneous ball milling 总被引:1,自引:0,他引:1
Mais Ursula Esteghlalian Ali R. Saddler John N. Mansfield Shawn D. 《Applied biochemistry and biotechnology》2002,98(1-9):815-832
One of the limiting factors restricting the effective and efficient bioconversion of softwood-derived lignocellulosic residues
is the recalcitrance of the substrate following pretreatment. Consequently, the ensuing enzymatic process requires relatively
high enzyme loadings to produce monomeric carbohydrates that are readily fermentable by ethanologenic microorganisms. In an
attempt to circumvent the need for larger enzyme loadings, a simultaneous physical and enzymatic hydrolysis treatment was
evaluated. A ball-mill reactor was used as the digestion vessel, and the extent and rate of hydrolysis were monitored. Concurrently,
enzyme adsorption profiles and the rate of conversion during the course of hydrolysis were monitored. α-Cellulose, employed
as a model substrate, and SO2-impregnated steam-exploded Douglas-fir wood chips were assessed as the cellulosic substrates. The softwood-derived substrate
was further posttreated with water and hot alkaline hydrogen peroxide to remove >90% of the original lignin. Experiments at
different reaction conditions were evaluated, including substrate concentration, enzyme loading, reaction volumes, and number
of ball beads employed during mechanical milling. It was apparent that the best conditions for the enzymatic hydrolysis of
α-cellulose were attained using a higher number of beads, while the presence of air-liquid interface did not seem to affect
the rate of saccharification. Similarly, when employing the lignocellulosic substrate, up to 100% hydrolysis could be achieved
with a minimum enzyme loading (10 filter paper units/g of cellulose), at lower substrate concentrations and with a greater
number of reaction beads during milling. It was apparent that the combined strategy of simultaneous ball milling and enzymatic
hydrolysis could improve the rate of saccharification and/or reduce the enzyme loading required to attain total hydrolysis
of the carbohydrate moieties. 相似文献
108.
Ramin Ghorbani‐Vaghei Mohammad Ali Zolfigol Nasrin Moshfeghifar Nadiya Koukabi Gholamabbas Chehardoli 《中国化学会会志》2007,54(3):791-794
An efficient method for the oxidative coupling of thiols to their corresponding disulfides by new reagents poly(N‐bromobenzene‐1,3‐disulfonylamide) PBBS , N,N,N′,N′‐tetrabromobenzene‐1,3‐disulfonylamide TBBDA and DABCO‐bromine complex is described. The reaction was applicable to a variety of thiols with high chemoselectivity. 相似文献
109.
Mohammad Ali Zolfigol Khodabakhsh Niknam Mojtaba Bagherzadeh Arash Ghorbani‐Choghamarani Nadiya Koukabi Maryam Hajjami Eskandar Kolvari 《中国化学会会志》2007,54(5):1115-1118
Tribromoisocyanuric acid (TBCA) and Oxone®‐MX systems were used as effective oxidizing agents for the oxidation of thiols to their corresponding disulfides under mild conditions at room temperature with good to excellent yields. 相似文献
110.
Solid Phase Extraction and Flame Atomic Absorption Spectrometric Determination of Trace Amounts of Zinc and Cobalt Ions in Water Samples 总被引:1,自引:0,他引:1
A simple and rapid method for the preconcentration of Co2+ and Zn2+ as their 2-guanidino-benzimidazole chelates is proposed using an octadecyl silica cartridge. The retained analytes were recovered with a mixture of 5mL of 0.01M HNO3 and 5mL of methanol. The metal ions in the effluent were determined by flame atomic absorption spectrometry. The effect of different parameters, such as sample matrix, amount of ligand, type of eluent for elution of ions from cartridge, flow rates of sample solution and eluent, breakthrough volume, and limit of detection, were evaluated. The effects of various cationic and anionic interferences on the percent recovery of Co2+ and Zn2+ were also studied. Quantitative extraction efficiencies were obtained by elution of the cartridge with a minimal amount of solvent. Hence, with a typical preconcentration factor of 50, the limits of detections of the proposed method are 0.26 and 1.62ngmL–1 for Zn2+ and Co2+, respectively. The method was applied to the determination of zinc and cobalt ions in different water samples. 相似文献