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981.
The quantitative analysis of Cr in super alloys with the presence of a wide variety of elements, Al, B, C, Co, Cu, Hf, Fe, Mn, Mo, Ni, Nb, P, Si, S, Ti, Ta, W, Zr; and trace amounts (a few ppm) of Pb, Se, Bi, Tl and Te has been studied. Persulfate oxidation and diphenylcarbazide photometric method were studied with the purpose of developing a relatively fast and reliable measurement for Cr by wet chemical analysis. The results indicate that the latter is supperior to the former in practical view. In the photometric method, solid sample (0.1g alloys) when treated with HClO4 and H2SO4 took ca. 72 hrs. for complete dissolution. When treated with HCl followed by HNO3, 0.1 g alloys were completely dissolved within 1&1/2; hours. The best experimental conditions for diphenylcarbazide photometric determination of Cr was thus established. Photometric determination of Cr complexes was made at 540 nm. 相似文献
982.
The major reactions of aryl substituted N-t-butylbenzamides upon electron-impact involve direct cleavage of a methyl radical, the loss of a butene molecule with the transfer of one hydrogen, or the loss of a butenyl radical with the transfer of two hydrogens. The last of these processes parallels the mass spectral behavior of aliphatic amides. Substituent effects indicate that electron-withdrawing groups on the aromatic ring enhance the two hydrogen transfer process, while electron-donating groups enhance the single hydrogen transfer process. Ion abundances, ionization potentials and appearance potentials are discussed with respect to correlation with σ+ values. 相似文献
983.
This study investigated and compared some techniques for the preparative isolation of terpene trilactones, including ginkgolides (GA and GB, etc.) and bilobalide (BB), from Ginkgo biloba leaves. The crude Ginkgo biloba L. extracts (GBE) were prepared using an extractor with solvent refluxing operated under an optimal extraction condition. The extraction yield was 20-23% and the purity of terpene trilactones was about 1.0-1.4 wt%. Before the isolation operations, the extracts were dissolved in de-ionized water. The isolation procedures included the method of liquid-liquid extraction and the method of column chromatography. For the method of liquid-liquid extraction using ethyl acetate as the organic solvent operated under the optimal extraction conditions, the purity, concentration ratio, and yield of terpene trilactones were 13.5-18.0%, 15-16, and >99%. For the method of column chromatography, XAD-7HP, XAD-4, and C-18 adsorbents with different polarities were used as the packing materials. Only for the XAD-7HP column, a part of more polar impurities was efficiently separated with the majority of terpene trilactones by a proper step-gradient elution, which resulted in an efficient isolation: the purity, concentration ratio, and yield of terpene trilactones were approximately 20, approximately 15, and approximately 80%. In comparison, the XAD-7HP column achieved the highest purity, but at the expense of the yield of terpene trilactones; on the contrary, the liquid-liquid extraction method, achieving the highest yield but with a slightly lower purity, was proved to be superior to the method of column chromatography in the current isolation stage. 相似文献
984.
1,4-Dioxane impurity in nonionic surfactants and cosmetics were analyzed using solid-phase microextraction (SPME) coupled with gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS). Experimental results show that there is no significant difference using SPME-GC and SPME-GC-MS for analysis of 1,4-dioxane in three types of nonionic surfactants at the 95% confidence level. The relative standard deviation (R.S.D.) values of each analytical method were smaller than 3%. The amount of 1,4-dioxane was found to vary from 11.6 +/- 0.3 ppm to 73.5 +/- 0.5 ppm in 30% of nonionic surfactants from manufacturers in Taiwan. These methods were linear over the studied range of 3-150 ppm with correlation coefficients higher than 0.995. The recoveries of 1,4-dioxane for these nonionic surfactants following SPME were all higher than 96 +/- 1% (n = 3). The detection limits of 1,4-dioxane for these nonionic surfactants following SPME were from 0.06 ppm to 0.51 ppm. The experimentally determined level of 1,4-dioxane in cosmetics from manufacturers in Taiwan varied from 4.2 +/- 0.1 ppm to 41.1 +/- 0.6 ppm in 22% of daily used cosmetics following SPME coupled with GC and GC-MS. Conventional solvent extraction takes around 1 h for extraction and reconcentration but SPME takes only around 10 min. SPME provides better analyses of 1,4-dioxane in nonionic surfactants and cosmetics than conventional solvent extraction and head space pretreatments in term of simplicity, speed, precision, detection limit, and solvent consumption. 相似文献
985.
Diantipyrylmethane and tiron spectrophotometric determinations of Ti in the super alloys, Inconel 718 and Inconel 600, have been studied thoroughly. Both reagents formed stable yellow complexes with Ti(IV) in acidic medium. The possible interference from Ni, Fe and Cr was examined. Interference from Fe(III) was eliminated by the reduction of Fe(III) to Fe(II). Cr was removed as chromyl chloride which led to a dramatic improvement in the analytical results for Ti by the tiron photometric method. However, the removal of Cr was not necessary when the diantipyrylmethane method was employed. Consequently, lengthy manipulation of super alloys was required for the tiron determination. These two spectrophotometric methods are compared in terms of simplicity, reproducibility and accuracy. 相似文献
986.
J. C. Salamone C. C. Tsai Q. Anwaruddin A. P. Olson M. Arnold T. Nagabhushanam S. Sawan A. C. Watterson 《Journal of polymer science. Part A, Polymer chemistry》1984,22(9):2005-2016
In this article are described the solution properties of ampholytic ionomers obtained by the radical copolymerization of styrene with the ion-pair comonomer 3-methacrylamidopropyltrimethylammonium, 2-acrylamido-2-methylpropanesulfonate. The solution properties were studied in mixed solvents, with a good solvent for the polystyrene backbone and another for the ionic moieties, and in the individual good solvent of benzyl alcohol. The data obtained strongly support extensive intermolecular ionic interactions in solution. 相似文献
987.
[C(4)H(3)N(CH(2)NMe(2))-2]AlMe(2) (1) is prepared in 88% yield by the reaction of substituted pyrrole [C(4)H(4)N(CH(2)NMe(2))-2] with 1 equiv of AlMe(3) in methylene chloride. Reaction of compound 1 with 1 equiv of phenyl isocyanate in toluene generates a seven-membered cycloaluminum compound [C(4)H(3)N[CH(2)NPh(CONMe(2))]-2] AlMe(2) (2). The phenyl isocyanate was inserted into the aluminum and dimethylamino nitrogen bond and induced an unusual rearrangement which results in C-N bond breaking and formation. A control experiment shows that the reaction of substituted pyrrole [C(4)H(4)N(CH(2)NMe(2))-2] with 1 equiv of phenyl isocyanate in diethyl ether yields a pyrrolyl attached urea derivative [C(4)H(3)N(CH(2)NMe(2))-2-[C(=O)NHPh]-1] (3). The demethanation reaction of AlMe(3) with 1 equiv of 3 in methylene chloride at 0 degrees C afforded O-bounded and N-bounded aluminum dimethyl compounds [C(4)H(3)N(CH(2)NMe(2))-2-[C(=O)NPh]-1]AlMe(2) (4a) and [C(4)H(3)N(CH(2)NMe(2))-2-[CO(=NPh)]-1]AlMe(2) (4b) in a total 78% yield after recrystallization. Both 4a and 4b are observed in (1)H NMR spectra; however, the relative ratio of 4a and 4b depends on the solvent used. Two equivalents of AlMe(3) was reacted with 3 in methylene chloride to yield a dinuclear aluminum compound AlMe(3)[C(4)H(3)N(CH(2)NMe(2))-2-[C(=O)NPh]-1] AlMe(2) (5). Reaction of 5 with another equivalent of ligand 3 results in the re-formation of compounds 4a and 4b. 相似文献
988.
Introductionlnthcstud}ofmcthaneoxidativccoupIing(0CM),aseriesofcatalystshavebeendevelopedandox}'genspeciesoncatal}'stst"ereinvestigatedextensively.Alotofpapershavebeenpublishedonthisarea.Anongkindsof0CMcatalystsmetalhalidespromotedmctaloxides.cspcciall}'Li /Mg0catal}'stl1~3l.havcbecnmostoftenstudied.Themostpromisingindustrialoncshavebeenthoughttoberarcearthoxidesbasedcatalysts.H.L.Wanelajl#Ihavesuccessfull\'madeuseofmetalfluoridesin0CM,andfoundthebcttcrpron1otingcffectofmctalfluoridcstomc… 相似文献
989.
It A proposed that the M-cluster cage (Kim-Rees model) in active N2-ase can exert shape-selective molecular-sieve effects in molecular recognition of exogenous substrates, by providing inside multinuclear active-sites the cavity for N2, C2H2, cyclopropene, and N2O reduction, with [Mo-3Fe]-site available only for N2 reduction: on the other handn-RC— CH,n-RC— N,n-RN-C , C—N– and N3
–, are bound outside the cavity at the [2Fe]-site left by the labilizable ligand Y. A terminal carboxylate of the Mo-bound (R)-homocitrate is just in position to protect a H2-evolution site on the P-cluster pair from CO inhibition, and also to take part in mediating a P-cluster-to-Mo-site H+-relay system (involving two hydrogen-bonded H2O) specifically required for N. reduction. The nonreducibility of CO at the [Mo-3Fe]-site is also explained. Experimental support for molecular-sieve effects of M-cluster cage has been obtained from the observed decrease in ethene-cis-d: selectivity by competitive inhibition of HC—CH reduction in D2O by N—N.Dedicated to Jiaxi Lu on the occasion of his 80th birthday. 相似文献
990.
Harold Rosenberg Tsu-Tzu Tsai Ngoc Kim Ngo 《Journal of polymer science. Part A, Polymer chemistry》1982,20(1):1-13
A method for the first synthesis of high molecular weight carbonate-containing siloxanylene polymers was successfully developed. The procedure covered the preparation and polymerization of pure carbonate-containing bis-silanols which included bis(4-hydroxydimethylsilylphenyl)-carbonate, bis[4-(1-hydroxy-1,1,3,3-tetramethyldisiloxanyl)-phenyl] carbonate, and their meta analogs. Because conventional siloxane polymerization methods, such as the heterocondensation of bis-silanols with diaminosilanes or homocondensation reactions catalyzed by alkali reagents, decomposed carbonate linkages, a new polymerization technique that involved the use of phosgene was used. The procedure was both facile and effective in the polymerization of other arylene bis-silanols. 相似文献