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61.
Arsenic speciation is of increasing interest to the food industry, as concerns about high total arsenic concentrations in
food can often be alleviated to a great extent if the ratio of toxic, less toxic and non-toxic arsenic compounds in the sample
is known.
The lipid matrix of fish oil is a challenge in the determination of arsenic species, as current methods for this type of analysis
require the analyte to be water-soluble. In this study, two sample preparation techniques were applied. One the one hand water-soluble
species were extracted with methanol/water, on the other, acid digestion was applied to release lipid-soluble arsenic compounds
into the aqueous phase. Ion chromatography – inductively coupled plasma mass spectrometry (IC-ICP-MS) was used for separation
and sensitive element-specific detection of arsenic compounds. Additional experiments, including alkaline hydrolysis, were
carried out to find out more about the type of lipids arsenic is bound to in fish oil.
Up to eight different arsenic species were detected and quantified in fish oil with dimethylarsinate being the major compound
both in the aqueous extract and in the acid digest. No inorganic arsenic was detected in the aqueous extract, and the maximum
concentration of arsenate determined in the acid digest was 0.05 μg g−1.
The total arsenic concentration determined by ICP-MS ranged from <0.1 to 5 μg g−1. With regard to the mass balance, approximately 1% of the total arsenic content was extractable with methanol/water, whereas
the sum of arsenic species quantified after acid digestion yielded 85–100% of the total arsenic content. It was confirmed
that the large fraction of arsenic in fish oil not extractable on an aqueous basis consists of organoarsenic compounds.
This new approach in sample preparation makes the complete characterization of the arsenic content in the sample possible
with regard to the respective species, providing necessary information required for risk assessment. 相似文献
62.
Regina Y. Moriya Adilson R. Gonçalves Marta C. T. Duarte 《Applied biochemistry and biotechnology》2005,121(1-3):171-181
Organosolv (ethanol/water and acetosolv) pulps were treated with Bacillus pumilus xylanase for 4, 8, and 12 h and compared with commercial Cartazyme HS xylanase-treated pulps. Treatment of ethanol/water pulps with B. pumilus xylanase increased viscosity by 40% in 8 h of treatment compared with pulps treated without enzyme. However, acetosolv pulps treated with B. pumilus xylanase lost viscosity. Ethanol/water pulps treated with Cartazyme had a viscosity of 18.5 cP in 4 h of treatment. In the acetosolv pulps treated with commercial enzyme, the loss of viscosity was 20% compared with pulps treated without enzyme. Ethanol/water pulps treated with B. pumilus and Cartazyme had similar effects: a 44% reduction in kappa number for pulps treated with enzyme followed by alkaline extraction compared with pulps treated with alkaline extraction. In acetosolv pulps treated with B. pumilus, the kappa number was from 12 to 18, compared with pulps treated without enzyme, which had a 40% reduction in 4 and 12 h and a 60% reduction in 8 h. Cartazyme-treated acetosolv pulps had a kappa number of 14 in 4 and 8 h of treatment. For 12 h of treatment, the kappa number was 8. Fourier transform infrared spectra of the pulps showed that enzyme-treated pulps had changes in the 1000 cm?1 absorption owing to a C-O bond present in esters. Using principal component analysis, it is possible to differentiate the unbleached pulps and enzyme-treated pulps. 相似文献
63.
Preconcentration Systems Using Polyurethane Foam/Me-BDBD for Determination of Copper in Food Samples
Valfredo Azevedo Lemos Daniel Rodrigues Vieira Cleber Galvão Novaes Marcelo Eça Rocha Moacy Selis Santos Regina Terumi Yamaki 《Mikrochimica acta》2006,153(3-4):193-201
A new reagent, 6-[2′-(6′-methyl-benzothiazolylazo)]-1,2-dihydroxy-3,5-benzenedisulfonic acid (Me-BDBD), was synthesised and
used in on-line and off-line systems for copper preconcentration by solid-phase extraction. Spectrophotometry and Flame Atomic
Absorption Spectrometry (FAAS) were the detection techniques. Polyurethane foam loaded with Me-BDBD packed in a minicolumn
was used as sorbent in both systems. The spectral characteristics of Me-BDBD were investigated. The optimum pH values for
maximum sorption of the metal are between 7.0 and 8.5. Copper was desorbed with 0.05 and 0.50 mol L−1 hydrochloric acid solutions, for on-line and off-line systems, respectively. The effects of several foreign substances on
the adsorption of copper are reported. The enrichment factors obtained were 7 (on-line) and 26 (off-line) for the systems.
The proposed procedures allowed the determination of copper with detection limits of 3.4 and 1.4 μg L−1 (0.85 and 0.35 μg per gram of sample) for on-line and off-line systems, respectively. The precision of the procedures was
also calculated: 3.2 (on-line) and 1.9% (off-line). The validation of the procedures was carried out by analysis of certified
reference material. The copper contents in corn and rice flour and black tea samples were determined by applying the proposed
procedures. 相似文献
64.
Sandra Jiménez-Alonso Ana Estévez-Braun Ángel G. Ravelo Rafael Zárate Matías López 《Tetrahedron》2007,63(14):3066-3074
Several bis-pyrano-l,4-benzoquinones have been synthesized by a double domino Knoevenagel hetero Diels-Alder reaction. The synthetic approach is highly efficient allowing the construction of complex polycyclic scaffolds with six new σ-bonds. These reactions performed more efficiently and more rapidly using microwave irradiation. The resulting bis-pyrano-1,4-benzoquinones are the first examples of a double domino Knoevenagel hetero Diels-Alder reaction. Our approach represents a novel contribution to the chemistry of 2,5-dihydroxy-l,4-benzoquinones and the first general method for the synthesis of bis-pyranobenzoquinones. 相似文献
65.
Copper exchanged on beta zeolites are extremely active and selective for the catalytic oxidation of ammonia to nitrogen and water and this activity correlates to the ease of reduction of the copper species. 相似文献
66.
P. Sandra 《Journal of separation science》1989,12(2):82-86
Chromatographic resolution is a well defined concept, which is expressed in terms of column efficiency N, separation factor α, and retention factor k. The influence of the three factors on resolution is discussed and illustrated by examples taken from capillary gas chromatography. 相似文献
67.
Cataldo L Dutan C Misra SK Loss S Grützmacher H Geoffroy M 《Chemistry (Weinheim an der Bergstrasse, Germany)》2005,11(11):3463-3468
The EPR spectrum of the novel radical Mes*(CH3)P--PMes* (Mes*=2,4,6-(tBu)3C6H2) was measured in the temperature range 100-300 K, and was found to be drastically temperature dependent as a result of the large anisotropy of the 31P hyperfine tensors. Below 180 K, a spectrum of the liquid solution is accurately simulated by calculating the spectral modifications due to slow tumbling of the radical. To achieve this simulation, an algorithm was developed by extending the well-known nitroxide slow-motion simulation technique for the coupling of one electron spin to two nuclear spins. An additional dynamic process responsible for the observed line broadening was found to occur between 180 K and room temperature; this broadening is consistent with an exchange between two conformations. The differences between the isotropic 31P couplings associated with the two conformers are shown to be probably due to an internal rotation about the P--P bond. 相似文献
68.
Krystyna Bogdanowicz-Szwed Regina Gil 《Monatshefte für Chemie / Chemical Monthly》2004,35(12):1415-1425
A convenient method is described for the synthesis of functionalized spiro[cycloalkanono-2,3-thiophenes] by treatment of cyclic 3-oxoacid thioanilides with -nitrostyrenes. Reaction of the obtained products with acetic anhydride yielded the corresponding oxime acetates. 相似文献
69.
Cini R Tamasi G Defazio S Corsini M Zanello P Messori L Marcon G Piccioli F Orioli P 《Inorganic chemistry》2003,42(24):8038-8052
The reaction of trans-[RuCl(2)(PPh(3))(3)] (Ph = C(6)H(5)) with 2-thio-1,3-pyrimidine (HTPYM) and 6-thiopurines (TPs) produced mainly crystalline solids that consist of cis,cis,trans-[Ru(PPh(3))(2)(N,S-TPYM)(2)] (1) and cis,cis,trans-[Ru(PPh(3))(2)(N(7),S-TPs)(2)]X(2) (X = Cl(-), CF(3)SO(3)(-)). In the case of TPs, other coordination isomers have never been isolated and reported. Instead, the mother liquor obtained after filtration of 1 produced red single crystals of trans,cis,cis-[Ru(PPh(3))(2)(N,S-TPYM)(2)].2H(3)O(+).2Cl(-) (2.2H(3)O(+).2Cl(-)). Selected ruthenium(II)-thiobase complexes were studied for their structural, reactivity, spectroscopic, redox, and cytotoxic properties. Single crystals of 1 contain thiopyrimidinato anions chelated to the metal center via N and S. The Ru[bond]N bonds are significantly elongated for 1 [2.122(2) and 2.167(2) A] with respect to 2 [2.063(3) A] because of the trans influence from PPh(3). The coordination pseudo-octahedron for 2 is significantly elongated at the apical sites (PPh(3) ligands). Solutions of cis,cis,trans isomers in air are stable for weeks, whereas those of 2 turn green within 24 h, in agreement with the respective redox potentials. cis,cis,trans- and trans,cis,cis-[Ru(PH(3))(2)(N,S-TPYM)(2)], as optimized through the DFT methods at the Becke3LYP level are in good agreement with experimental geometrical parameters (1 and 2), with cis,cis,trans being more stable than trans,cis,cis by 3.88 kcal. The trend is confirmed by molecular modeling based on semiempirical (ZINDO/1) and molecular mechanics (MM) methods. Cytotoxic activity measurements for cis,cis,trans-[Ru(PPh(3))(N-THZ)(N(7),S -H(2)TP)(2)]Cl(2) (4) (THZ = thiazole, H(2)TP = 6-thiopurine) and cis,cis,trans-[Ru(PPh(3))(2)(N(7),S-HTPR)2]Cl(2) (5) (HTPR = 6-thiopurine riboside) against ovarian cancer cells A2780/S gave IC(50) values of 17 +/- 1 and 29 +/- 9 microM, respectively. Furthermore, the spectral analysis of HTPYM, TPs, and their Ru(II) complexes in solution shows that intense absorptions occur in the UVA/vis region of light, whereas standard nucleobases absorb in the UVB region. 相似文献
70.
A computerized peak deconvolution software and mass spectra were successfully applied for the deconvolution of overlapped peak cluster in the chromatogram obtained separating the complex mixture of pesticides by retention time locking gas chromatography-mass spectroscopy. The method based on the unique fragment ions in the spectra can be used for deconvolution of peak clusters if mass spectra of overlapped peaks differ. This method allows determining actual retention times of overlapped peaks. Peak areas found by this method however, cannot be used naturally for the quantitative purposes as the abundance of fragment ions used for this deconvolution procedure can dramatically differ. Computer assisted deconvolution of peaks in the peak clusters gives more realistic peak area ratios as at this method it is supposed equal response for all peaks overlapped in a cluster. 相似文献