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81.
A method is described for fast dual-column separation of pesticides by use of dual low thermal mass gas chromatography–mass spectrometry (dual LTM-GC–MS) with different temperature programming. The method can provide two total ion chromatograms with different separation on DB-5 and DB-17 in a single run, which allows improved identification capability, even with short analysis time (<17 min). Also simultaneous detection with MS and elemental selective detector, e.g. pulsed flame photometric detection (PFPD) was evaluated for fast dual-column separation of 82 pesticide mixtures including 27 phosphorus pesticides. Dual LTM-GC–MS/PFPD was applied to analysis of pesticides in a brewed green tea sample with dual stir bar sorptive extraction method (dual SBSE). 相似文献
82.
Birgit Heying Ute Ch. Rodewald Rainer P?ttgen Kenichi Katoh Yuzuru Niide Akira Ochiai 《Monatshefte für Chemie / Chemical Monthly》2005,38(4):655-661
The equiatomic ytterbium–transition metal–germanides YbCuGe and YbIrGe were synthesized in single crystalline form from CuGe and IrGe master alloys and ytterbium via the Bridgman technique and they were characterized through their X-ray powder patterns. The structures were refined from X-ray single crystal diffractometer data: NdPtSb type, P63mc, a=421.36(8), c=703.9(1) pm, wR2=0.0234, 210 F2 values, 11 variable parameters, BASF=0.35(9) for YbCuGe and TiNiSi type, Pnma, a=671.09(6), b=421.55(5), c=757.16(7) pm, wR2=0.0782, 519 F2 values, 20 variable parameters for YbIrGe. The copper (iridium) and germanium atoms build up [CuGe] and [IrGe] networks. In YbCuGe the two-dimensional [CuGe] network consists of puckered layers of Cu3Ge3 hexagons (247pm Cu–Ge) that are charge balanced and separated by the ytterbium atoms. In contrast, the ordered Ir3Ge3 hexagons show a strong orthorhombic distortion and the [IrGe] network is three-dimensional with a distorted tetrahedral germanium coordination around iridium with almost equal Ir–Ge distances (252–259pm). The ytterbium atoms fill cages within this network. The cell volumes of YbCuGe and YbIrGe are indicative for purely trivalent ytterbium. 相似文献
83.
84.
Bungo Ochiai Tomomi Nagasawa Yasuhiro Asano Daisuke Nagai Atsushi Sudo Takeshi Endo 《Journal of polymer science. Part A, Polymer chemistry》2007,45(13):2820-2826
Thermal behaviors were monitored by infrared thermographic analysis in the copolymerization of a spiroorthoester and a bifunctional oxetane with thermally latent initiators [benzyl tetrahydrothiophenium hexafluoroantimonate (BTHT) and benzyl 4‐hydroxyphenyl methyl sulfonium hexafluoroantimonate (BPMS)]. The copolymerization with BPMS increased the temperature during the copolymerization more than that with BTHT, whereas the exothermicities were lowered with the increase in the initial feed ratio of the spiroorthocarbonate monomer. The high exothermicity in the copolymerization with BPMS is ascribable to the faster propagation of the oxetane monomer with a high heat of polymerization, and this is supported by model reactions and computational calculation. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 2820–2826, 2007 相似文献
85.
Tomomi Nagasawa Bungo Ochiai Takeshi Endo 《Journal of polymer science. Part A, Polymer chemistry》2007,45(8):1388-1393
Infrared (IR) thermography was employed to monitor temperature changes during the copolymerization of a spiroorthoester monomer with an oxetane monomer initiated with a benzyl sulfonium salt. The temperature changes in the polymerizations decreased with the increase of the initial feed ratios of the spiroorthocarbonate monomer. For instance, the temperature in the copolymerization of the equimolar mixture of both of the monomers increased only ~1 °C, whereas that in the homopolymerization of the oxetane monomer increased more than 20 °C. This result indicates that the copolymerization employing spiroorthocarbonate monomers effectively suppress temperature increase, which are responsible to shrinkage during cooling. The suppression of polymerization shrinkage by spiroorthocarbonate was also confirmed by density measurement of the polymers using a gas pycnometer. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 1388–1393, 2007. 相似文献
86.
Ozao R. Ochiai M. Yoshida H. Ichimura Y. Inada T. 《Journal of Thermal Analysis and Calorimetry》2001,64(3):923-932
Gamma-alumina membrane was prepared from anodic (amorphous) alumina (AA) obtained in a sulphuric acid electrolyte. The transformation
scheme, i.e., the crystallization to form metastable alumina polymorphs and the final transition to α-Al2O3 with heating was studied by TG-DTA and X-ray diffraction (XRD) using fixed time (FT) method. When heating at a constant rate,
the crystallization occurred at 900°C or higher and the final formation of α-Al2O3 occurred at 1250°C or higher, which temperatures were higher than the case of using anodic (amorphous) alumina prepared from
oxalic acid electrolyte. Relative content of S of the products was obtained by transmission electron microscope (TEM)-energy
dispersive spectroscopy (EDS). The proposed thermal change of anodic alumina membrane prepared from sulphuric acid is as follows:
1. At temperatures lower than ca 910°C: Formation of a quasi-crystalline phase or a polycrystalline phase (γ-, δ- and θ-Al2O3);
2. 910–960°C: Progressive crystallization by the migration of S toward the surface within the amorphous or the quasi-crystalline
phase, forming S-rich region near the surface;
3. 960°C: Change of membrane morphology and the quasi-crystalline phase due to the rapid discharge of gaseous SO2;
4. 960–1240°C: Crystallization of γ-Al2O3 accompanying δ-Al2O3; and
5. 1240°C: Transition from γ-Al2O3 (+tr. δ-Al2O3) into the stable α-Al2O3.
The amorphization which occurs by the exothermic and the subsequent endothermic reaction suggests the incorporation of SO3 groups in the quasi-crystalline structure.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
87.
Ozao R. Yoshida H. Ichimura Y. Inada T. Ochiai M. 《Journal of Thermal Analysis and Calorimetry》2001,64(3):915-922
The thermal change of anodic alumina (AA), particularly the exothermic peak followed by the endothermic peak at ca 950°C was
studied in detail by mainly using simultaneous TG-DTA/FTIR. The gradual loss of mass up to ca 910°C is attributed to dehydration.
When heated at a constant rate by using TG-DTA, an exothermic peak with subsequent endothermic peak is observed at ca 950°C,
but the exothermic peak becomes less distinct with decreasing heating rate. It has been found that gaseous SO2 accompanying a small amount of CO2 is mainly discharged at this stage. The reaction in this stage can be considered roughly in two schemes. The first scheme
can be said collectively as crystallization, in which the migration of S or C trapped inside the crystal lattice of the polycrystalline
phase (γ-, δ-, and θ-Al2O3, which presumably accompanies a large amount of amorphous or disordered phase) occurs. In the second scheme, the initial
polycrystalline (+amorphous) phase crystallizes into a quasi-crystallineγ-Al2O3-like metastable phase after amorphization. Conclusively,after the distinct exo- and endothermic reactions, the amorphous
phase crystallizes intoγ-Al2O3, presumably accompanying small amount of δ-Al2O3. It is also found that, when maintained isothermally, the metastable phases undergo transformation into the stable α-Al2O3 at 912°C.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
88.
Kobayashi S Ohmae M Ochiai H Fujikawa S 《Chemistry (Weinheim an der Bergstrasse, Germany)》2006,12(23):5962-5971
Hyaluronidase (HAase) catalyzes multiple enzymatic polymerizations with controlling regio- and stereoselectivity perfectly. This behavior, that is, the single enzyme being effective for multireactions and retaining the enzyme catalytic specificity, is not usual, and hence, HAase is a supercatalyst. Various sugar oxazoline monomers prepared based on the concept "transition-state analogue substrate" were successfully polymerized and copolymerized with HAase catalysis, yielding natural and unnatural glycosaminoglycans. 相似文献
89.
Ochiai M Suefuji T Miyamoto K Shiro M 《Chemical communications (Cambridge, England)》2003,(12):1438-1439
The single crystal X-ray structure of the supramolecular complex formed between diphenyl-lambda3-iodane (Ph2IBF4) or 1-alkynyl(phenyl)-lambda3-iodane [Bu(t)CCI(Ph)BF4] and 1,10-phenanthroline indicates a hitherto unknown distorted trigonal bipyramidal geometry around iodine(III), in which 1,10-phenanthroline acts as a bidentate ligand and occupies equatorial sites. 相似文献
90.
Yoshinao Tamaru Hirofumi Ochiai Tatsuya Nakamura Kazunori Tsubaki Zen-ichi Yoshida 《Tetrahedron letters》1985,26(45):5559-5562
2-Carboethoxyethylzinc iodide and 3-carboethoxypropylzinc iodide are generated by the reaction of the corresponding iodoesters with Zn-Cu couple and utilized for the palladium catalyzed coupling reaction with acid chloride to quantitatively provide gamma- and delta- keto esters, respectively. 相似文献