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81.
Nara O 《Analytica chimica acta》2011,(1):91-102
I describe an interchangeable twin vessel (J, N) automatic glass recrystallizer that eliminates the time-consuming recovery and recycling of crystals for repeated recrystallization. The sample goes in the dissolution vessel J containing a magnetic stir-bar K; J is clamped to the upper joint H of recrystallizer body D. Empty crystallization vessel N is clamped to the lower joint M. Pure solvent is delivered to the dissolution vessel and the crystallization vessel via the head of the condenser A. Crystallization vessel is heated (P). The dissolution reservoir is stirred and heated by the solvent vapor (F). Continuous outflow of filtrate E out of J keeps N at a stable boiling temperature. This results in efficient dissolution, evaporation and separation of pure crystals Q. Pure solvent in the dissolution reservoir is recovered by suction. Empty dissolution and crystallization vessels are detached. Stirrer magnet is transferred to the crystallization vessel and the role of the vessels are then reversed. Evacuating mother liquor out of the upper twin vessel, the apparatus unit is ready for the next automatic recrystallization by refilling twin vessels with pure solvent. We show successive automatic recrystallization of acetaminophen from diethyl ether obtaining acetaminophen of higher melting temperatures than USP and JP reference standards by 8× automatic recrystallization, 96% yield at each stage. Also, I demonstrate a novel approach to the determination of absolute purity by combining the successive automatic recrystallization with differential scanning calorimetry (DSC) measurement requiring no reference standards. This involves the measurement of the criterial melting temperature T0 corresponding to the 100% pure material and quantitative ΔT in DSC based on the van’t Hoff law of melting point depression. The purity of six commercial acetaminophen samples and reference standards and an eight times recrystallized product evaluated were 98.8 mol%, 97.9 mol%, 99.1 mol%, 98.3 mol%, 98.4 mol%, 98.5 mol% and 99.3 mol% respectively. 相似文献
82.
83.
A novel chiral selector, clindamycin succinate, was synthesized and first used as a chiral selector in capillary electrophoresis (CE). The chiral resolution ability of this kind of clindamycin derivation was studied by CE using some racemic drugs as model analytes. From the experimental results, it was found that both resolution and selectivity of the selector were dependent on the following parameters: concentration of chiral selectors, pH of the running buffer, temperature of the capillary column, applied voltage and organic modifier used. The results show that the chiral selector possesses high resolution toward some racemic drugs, including ofloxacin, chlorphenamine, tryptophan, propranolol, sotalol and metoprolol. Excellent chiral resolution of these tested drugs was achieved under the optimal conditions of 50 mM clindamycin succinate, 10% MeOH v/v, 50 mM Tris buffer, pH 4.0, at 22 kV and 20 °C within 25 min. 相似文献
84.
Authenticity assessment of flavoured strawberry foods was performed using headspace-solid phase microextraction (HS-SPME) coupled to gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS). An authenticity range was achieved, investigating on the carbon isotope ratio of numerous selected aroma active volatile components (methyl butanoate, ethyl butanoate, hex-(2E)-enal, methyl hexanoate, buthyl butanoate, ethyl hexanoate, hexyl acetate, linalool, hexyl butanoate, octyl isovalerate, γ-decalactone and octyl hexanoate) of organic Italian fresh strawberries. To the author's knowledge, this is the first time that all these components were investigated simultaneously by GC-C-IRMS on the same sample. The results were compared, when applicable, with those obtained by analyzing the HS-SPME extracts of commercial flavoured food matrices. In addition, one Kenyan pineapple and one fresh Italian peach were analyzed to determine the δ(13)C(VPDB) of the volatile components common to strawberry. The δ(13)C(VPDB) values are allowed to differentiate between different biogenetic pathways (C(3) and CAM plants) and more interestingly between plants of the same CO(2) fixation group (C(3) plants). Additional analyses were performed on all the samples by means of Enantioselective Gas Chromatography (Es-GC), measuring the enantiomeric distribution of linalool and γ-decalactone. It was found that GC-C-IRMS and Es-GC measurements were in agreement to detect the presence of non-natural strawberry aromas in the food matrices studied. 相似文献
85.
Ortín A Torres-Lapasió JR García-Álvarez-Coque MC 《Journal of chromatography. A》2011,1218(16):2240-2251
Samples with a large number of compounds or similarities in their structure and polarity may yield insufficient chromatographic resolution. In such cases, however, finding conditions where the largest number of compounds appears sufficiently resolved can be still worthwhile. A strategy is here reported that optimises the resolution level of chromatograms in cases where conventional global criteria, such as the worst resolved peak pair or the product of elementary resolutions, are not able to detect any separation, even when most peaks are baseline resolved. The strategy applies a function based on the number of "well resolved" peaks, which are those that exceed a given threshold of peak purity. It is, therefore, oriented to quantify the success in the separation, and not the failure, as the conventional criteria do. The conditions that resolve the same amount of peaks are discriminated by either quantifying the partial resolution of those peaks that exceed the established threshold, or by improving the separation of peaks below it. The proposed approach is illustrated by the reversed-phase liquid chromatographic separation of a mixture of 30 ionisable and neutral compounds, using the acetonitrile content and pH as factors. 相似文献
86.
Abstract The IR spectra of the linkage isomers [Pd(bipy)(SCN)2] and [Pd(bipy)(NCS)2] have been determined in the C≡N stretching region (2200–2000 cm?1) and below 500 cm?1. The band shifts resulting from deuteration of the 2,2′-bipyridine (bipy) ring and 15NCS-labelling are shown to provide a ready means for distinguishing between the internal ligand modes, the μPd-N(bipy) and μPd-SCN/μPd-NCS vibrations. The assignment technique has been further extended to the complexes [Pt(bipy)(SCN)2] and [Pd(phen)(SCN)2] (phen = 1,10-phenanthroline). Finally, a comparison between the IR spectra of [Pd(bipy)(NCO)2], [Pd(bipy)(NCS)2] and [Pd(bipy)(SCN)2] reveals that the frequencies μM-NCO, μM-NCS and μM-SCN decrease in the sequence NCO > NCS > SCN. 相似文献
87.
Studies of the perturbing effect of the trifluoromethylanthryl carbinol used as chiral solvating agent (CSA) upon the 1H NMR spectra of chiral α-O-substituted β-hydroxylamides demonstrated the ability of this fluoroalcohol to afford diastereomeric solvates with these solutes. Thus, for all the tested amides, there is at least one possibility to proceed to their enantiomeric discrimination by 1H NMR using CSA. The method was developed to determine (later and indirectly) a possible chiral recognition during in vitro enzymatic hydrolysis in locust biological tissues of N-acylaziridines conceived as proinsecticides of carboxylic acids, in view to eventually optimize their efficiency. 相似文献
88.
Patricia Sakon Williams Frederick J. Troendle Kunisi S. Venkatasubban Robert Rothchild 《光谱学快报》2013,46(7):1229-1251
The 200 MHz 1H NMR spectra of the analgesic, famprofazone, 1, have been studied in CDCl3 solution at ambient temperatures with the achiral lanthanide shift reagent (LSR) tris (6, 6, 7, 7, 8, 8, 8-heptaf luoro-2, 2-dimethyl-3, 5-octanedionato) europium (III), Eu(FOD)3, 2, for spectral simplification, and with the chiral LSR, tris [3-(heptafluoropropylhydroxymethylene) - (+) camphorato] europium (III), Eu (HFC)3, 3. Lanthanide induced shift (LIS) magnitudes suggested predominant LSR binding at the carbonyl oxygen. Substantial enantiomeric shift differences were observed for several nuclei of 1 with added 3 which could permit direct determinations of enantiomeric excess. 相似文献
89.
The 1H and 13C NMR spectra of methaqualone, 1, have been extensively studied using one and two-dimensional techniques. These 300 MHz 1H and 75 MHz 13C studies have allowed rigorous assignments to be made for the methyl groups and the quinazolinone nucleus. The 60 MHz 1H spectra for 1 in CDCl3 have been examined with 相似文献
90.