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61.
Migaku Kawaguchi Norihiro Sakui Noriya Okanouchi Koichi Saito 《Analytica chimica acta》2005,533(1):57-65
A new method, stir bar sorptive extraction (SBSE) with in situ derivatization and thermal desorption (TD)-gas chromatography-mass spectrometry (GC-MS), which is used for the determination of trace amounts of chlorophenols, such as 2,4-dichlorophenol (2,4-DCP), 2,4,6-trichlorophenol (2,4,6-TrCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP) and pentachlorophenol (PCP), in tap water, river water and human urine samples, is described. The derivatization conditions with acetic acid anhydride and the SBSE conditions such as extraction time are investigated. Then, the stir bar is subjected to TD followed by GC-MS. The detection limits of the chlorophenols in tap water, river water and human urine samples are 1-2, 1-2, and 10-20 pg ml−1 (ppt), respectively. The calibration curves for the chlorophenols are linear and have correlation coefficients higher than 0.99. The average recoveries of the chlorophenols in all the samples are higher than 95% (R.S.D. < 10%) with correction using added surrogate standards, 2,4-dichlorophenol-d5, 2,4,6-trichlorophenol-13C6, 2,3,4,6-tetrachlorophenol-13C6 and pentachlorophenol-13C6. This simple, accurate, sensitive and selective analytical method may be applicable to the determination of trace amounts of chlorophenols in liquid samples. 相似文献
62.
Kodera M Shimakoshi H Nishimura M Okawa H Iijima S Kano K 《Inorganic chemistry》1996,35(17):4967-4973
A mononucleating tripyridine ligand, 2-(bis(2-pyridyl)methyl)-6-methylpyridine (L(1)), and a dinucleating hexapyridine ligand, 1,2-bis[2-(bis(2-pyridyl)methyl)-6-pyridyl]ethane (L(2)), have been prepared. The reaction of a carbanion of 2,6-lutidine with 2-bromopyridine affords L(1) which is converted to L(2) quantitatively by treating with tert-butyllithium and 1,2-dibromoethane. (&mgr;-Oxo)bis(&mgr;-acetato)diiron(III) complexes [Fe(2)(O)(OAc)(2)(L(1))(2)](ClO(4))(2) (1) and [Fe(2)(O)(OAc)(2)L(2)](ClO(4))(2) (2) have been synthesized and characterized by means of infrared, UV/vis, mass, and M?ssbauer spectroscopies and by measuring magnetic susceptibility and cyclic voltammograms. All the spectral data are consistent with the (&mgr;-oxo)bis(&mgr;-acetato)diiron(III) core structure in both 1 and 2. A relatively strong molecular ion peak at m/z 865 corresponding to [{Fe(2)O(OAc)(2)L(2)}(ClO(4))](+) in a FAB mass spectrum of 2 suggests the stabilization of the (&mgr;-oxo)bis(&mgr;-acetato)diiron(III) core structure by L(2) in a solution state. The compound 2.DMF.2-PrOH.H(2)O, chemical formula C(44)Cl(2)Fe(2)H(51)N(7)O(16), crystallizes in the monoclinic space group C2/c with a = 22.034(6) ?, b = 12.595(5) ?, c = 20.651(7) ?, beta = 121.49(2) degrees, and Z = 4. The cation has 2-fold symmetry with the bridging oxygen atom on the 2-fold axis: Fe-(&mgr;-O) = 1.782(5) ?, Fe-O-Fe = 123.6(6) degrees, and Fe.Fe = 3.142(3) ?. The diiron(III) core structure of 2 seems to be stabilized by encapsulation of the ligand. Compound 2 is the first example of a discrete (&mgr;-oxo)bis(&mgr;-acetato)diiron(III) complex with a dinucleating ligand. 相似文献
63.
A simple and highly sensitive method called thermal desorption (TD)-gas chromatography-mass spectrometry (GC-MS), which is used for the determination of trace amounts of 4-nonylphenol (NP) and 4-tert.-octylphenol (OP) in water samples, is described. NP and OP in samples are extracted from water samples and concentrated by the stir bar sorptive extraction (SBSE) technique. A stir bar coated with polydimethylsiloxane (PDMS) is added to a 2.0 ml water sample and stirring is carried out for 60 min at room temperature (25 °C) in a headspace vial. Then the extract is high sensitively analyzed by TD-GC-MS without any derivatization step. The optimum SBSE conditions are realized at an extraction time of 60 min. The detection limits are 0.02 ng ml−1 for NP and 0.002 ng ml−1 for OP. The method shows good linearity over the concentration range of 0.1-10 ng ml−1 for NP and 0.01-10 ng ml−1 for OP, and the correlation coefficients are higher than 0.999. The average recoveries of NP and OP are higher than 97% (R.S.D.: 3.6-6.2%) with correction using the added surrogate standards, 4-(1-methyl) octylphenol-d5 and deuterium 4-tert.-octylphenol. This simple, accurate, sensitive and selective analytical method may be used in the determination of trace amounts of NP and OP in tap and river water samples. 相似文献
64.
Yoshiyuki Mizuhata Nobuhiro Takeda Norihiro Tokitoh 《Phosphorus, sulfur, and silicon and the related elements》2013,188(4-5):947-948
The reductive debromination of an very crowded bis(bromodiaryl- silyl)butadiyne 2 was performed with potassium graphite to give the corresponding 2-allenyl-1-benzosilole 3 was isolated as a main product. 相似文献
65.
66.
Dr. Tatsuya Yanagisawa Prof. Dr. Yoshiyuki Mizuhata Prof. Dr. Norihiro Tokitoh 《Chemistry (Weinheim an der Bergstrasse, Germany)》2021,27(44):11273-11278
The reversible addition of olefins to a phosphanylalumane, P−Al single-bond species, was investigated. The P−Al bond added to ethylene and relatively small terminal alkenes (propylene and hex-1-ene) at room temperature to give the corresponding alkene adducts. Heating the terminal alkene adducts released the corresponding alkenes and regenerated the P−Al bond, but no release of ethylene was observed even under vacuum conditions. The reactivity of ethylene adduct as a new saturated C2 vicinal P/Al-based FLP was also investigated. The ethylene adduct was found to undergo complexation with nitriles to give the corresponding nitrile adducts to the Al center, which retained the ethylene tether as in the case of the corresponding P/B-based FLP. However, the reactivity of ethylene toward CO2 and benzaldehyde differed from that of the P/B system giving the corresponding adducts. 相似文献
67.
The new tripeptide reported here is composed of (R)-2-(3-aminophenoxy)propionic acid and is a bowl-shaped receptor that simultaneously binds both cations and anions of acetylcholine chloride and benzyltrimethylammonium compounds. An intriguing conformational change of the host was observed in the complexation of the ionic pair, where anion-induced flipping of the amide group on the macrocycle occurred. 相似文献
68.
69.
Nobuhiro Takeda Norihiro Tokitoh Renji Okazaki 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1):633-636
The first rotational isomers of stable selenoaldehydes are synthesized by deselenation of cyclic polyselenides having an efficient steric protection group, 2, 4, 6-tris[bis(trimetylsilyl)methyl]phenyl (Tbt). Reactions of these selenoaldehydes with W(CO)5.THF gives the corresponding η1-selenoaldehyde tungsten complexes, the structures of which are established by X-ray crystallography. 相似文献
70.
Yoshiaki Miyamoto Norihiro Wada Dr. Takahiro Soeta Dr. Shuhei Fujinami Prof. Dr. Katsuhiko Inomata Prof. Dr. Yutaka Ukaji 《化学:亚洲杂志》2013,8(4):824-831
The stereoselective direct transformation of N‐(propargylic)hydroxylamines into cis‐2‐acylaziridines was achieved by the combined use of AgBF4 and CuCl. Copper salts were found to promote the transformation of the intermediary 4‐isoxazolines into 2‐acylaziridines and both 3‐aryl‐ and 3‐alkyl‐substituted 2‐acylaziridines could be prepared by using this method. Furthermore, subsequent 1,3‐dipolar cycloaddition of azomethine ylides that were generated in situ from the intermediary 2‐acylaziridines with maleimides was achieved in a stereoselective one‐pot procedure to afford the corresponding 2‐acylpyrrolidines, which consisted of an octahydropyrrolo[3,4‐c]pyrrole skeleton. 相似文献