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101.
102.
《Analytical letters》2012,45(16):2553-2565
Online matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) is reported with in situ matrix/analyte aerosol mixing. The analyte and matrix were dissolved in separate solvents and pneumatically atomized into particles. Continuous flows of analyte particles and matrix droplets in nitrogen were mixed in a tee. The resulting particles were sampled using a nozzle, focused into a beam with an aerodynamic lens system, and vertically deposited continuously on a movable target. The matrix/analyte mixture was desorbed/ionized using a 266 nanometers pulsed laser at an incident angle of 45°. The nascent ions were analyzed using reflectron TOF MS. The performance of online MALDI-TOF MS was evaluated by the analysis of palmityl palmitate with the lithium salt of 2, 4-dihydroxybenzoic acid as the matrix. Strong and stable MALDI signals of palmityl palmitate were obtained. The matrix solvent mixture and the analyte concentration were optimized and the results demonstrate the development of an alternative for online MALDI analysis. 相似文献
103.
104.
R. Geißler M. Saraji-Bozorgzad T. Streibel E. Kaisersberger T. Denner R. Zimmermann 《Journal of Thermal Analysis and Calorimetry》2009,96(3):813-820
A variety of crude oil samples have been investigated by the combined methods of thermal analysis and mass spectrometry by
means of a newly developed prototype of a thermogravimetry—single photon ionisation time-of-flight mass spectrometer coupling
(TG-SPI-TOFMS). Single photon ionisation (SPI) was conducted utilising a novel electron beam pumped argon excimer lamp (EBEL)
as photon source, and a TOFMS with orthogonal acceleration has been applied for the detection of the mass to charge signals.
The advantage of the soft SPI technique over EI for the analysis of such complex samples could be clearly demonstrated, as
the aliphatic hydrocarbons present in crude oil may be detected via their respective molecular ion signals, not showing the
intense fragmentation typical for EI spectra of this substance class. The application of SPI revealed furthermore two distinct
decomposition regions, dominated by evaporation and pyrolysis processes, respectively. Moreover, different crude oils could
be distinguished by TA/SPI mass spectra due to their unique molecular signatures. 相似文献
105.
A methodology for the chromatographic separation and analysis of three of the most popular artificial sweeteners (aspartame, saccharin, and sucralose) in water and beverage samples was developed using liquid chromatography/time-of-flight mass spectrometry (LC/TOF-MS). The sweeteners were extracted from water samples using solid-phase extraction (SPE) cartridges. Furthermore, several beverages were analyzed by a rapid and simple method without SPE, and the presence of the sweeteners was confirmed by accurate mass measurements below 2-ppm error. The unambiguous confirmation of the compounds was based on accurate mass measurements of the protonated molecules [M+H]+, their sodium adducts and their main fragment ions. Quantitation was carried out using matrix-matched standard calibration and linearity of response over 2 orders of magnitude was demonstrated (r > 0.99). A detailed fragmentation study for sucralose was carried out by time-of-flight and a characteristic spectrum fingerprint pattern was obtained for the presence of this compound in water samples. Finally, the analysis of several wastewater, surface water and groundwater samples from the US showed that sucralose can be found in the aquatic environment at concentrations up to 2.4 μg/L, thus providing a good indication of wastewater input from beverage sources. 相似文献
106.
Blagoj S. Mitrevski Prapin Wilairat Philip J. Marriott 《Journal of chromatography. A》2010,1217(1):127-135
The application of comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC × GC-TOFMS) for the analysis of six anabolic agents (AAs) in doping control is investigated in this work. A non-polar–polar column configuration with 0.2 μm film thickness (df) second dimension (2D) column was employed, offering much better spread of the components on 2D when compared to the alternative 0.1 μm df2D column. The proposed method was tested on the “key” AA that the World Anti-Doping Agency (WADA) had listed at the low ng mL−1 levels (clenbuterol, 19-norandrosterone, epimethendiol, 17α-methyl-5α-androstane-3α,17β-diol, 17α-methyl-5β-androstane-3α,17β-diol and 3′-OH-stanozolol). The compounds were spiked in a blank urine extract obtained by solid-phase extraction, hydrolysis and liquid–liquid extraction; prior to analysis they were converted to the corresponding trimethylsilyl (TMS) derivatives. The limit of detection (LOD) was below or equal to the minimum required performance limit (MRPL) of 2 ng mL−1 defined by WADA, and the correlation coefficient was in the range from 0.995 to 0.999. The method allows choosing an ion from the full mass spectra which shows the least interference from the matrix and/or the best sensitivity; this can only be done if full scan mass spectral data are available. The advantage of GC × GC over classical one-dimensional GC (1D GC), in terms of separation efficiency and sensitivity, is demonstrated on a positive urine control sample at a concentration of 5 ng mL−1. The obtained similarity to the in-house created TOFMS spectra library at this level of concentration was in the range from 822 to 932 (on the scale from 0 to 999). Since full mass spectral information are recorded, the method allows the retro-search of non-target compounds or new “designer steroids”, which cannot be detected with established GC–MS methods that use selected ion monitoring (SIM) mode. 相似文献
107.
108.
Direct analysis in real time-mass spectrometry (DART-MS) was employed as a novel fast method to identify traditional Chinese herbal medicine (TCHM). In order to obtain high quality mass spectra, the ionization temperature was optimized for every kind of sample. With minimal or no sample pretreatment, major TCHM components, including alkaloids, flavonoids and some ginsenosides, were directly detected within several seconds, while thirteen ginsenosides need derivatization to get good mass spectra. Pseudoginsenoside F11, compound K, protopanaxatriol (PPT) and protopanaxadiol (PPD), for the first time were detected without derivatization. Among five of eight tested Chinese herbal medicines, Rhizoma Corydalis, Bulbus Fritillariae Thunbergii, Arecae Semen, Ramulus Uncariae Cum Uncis and Scutellariae Radix, were first time identified by DART-MS. In addition, the ionization mechanisms of major herbal components, alkaloids, flavonoids and ginsenosides, were discussed in detail. Our results demonstrated that DART-MS could provide a rapid, reliable and environmental friendly method for the rapid identification of TCHM, and may be applicable to other plants. 相似文献
109.
A simple technique of preparing a continuous laminar liquid flow in vacuum (liquid beam) was developed and combined with multiphoton ionization and a time-of-flight mass spectrometer. This technique was applied to the study on resonance photoionization of an aniline (AN)-propanol (PrOH) solution (0.1 – 0.3 M). Binary cluster ions of aniline and propanol, AN+(PrOH)n (n ≤ 1), and protonated propanol cluster ions, H+(PrOH)n (n ≤ 1), were observed as product ions in the gas phase. The relative intensities of AN+PrOH and those of H+(PrOH)2 were measured as functions of the excitation laser power and the concentration of aniline in the propanol solution. The dependences of the ion intensities on the laser power and the AN concentration are explained in terms of a Coulomb ejection model, where the ions are ejected from the surface by Coulomb repulsion exerted from neighboring ions. It is also concluded that H+(PrOH)n is produced by a proton transfer reaction from an aniline ion to solvent molecules in the solution. 相似文献
110.
van der Westhuizen R Ajam M De Coning P Beens J de Villiers A Sandra P 《Journal of chromatography. A》2011,1218(28):4478-4486
Fully synthetic jet fuel (FSJF) produced via Fischer-Tropsch (FT) technology was recently approved by the international aviation fuel authorities. To receive approval, comparison of FSJF and crude-derived fuel and blends on their qualitative and quantitative hydrocarbon composition was of utmost importance. This was performed by comprehensive two-dimensional gas chromatography (GC×GC) in the reversed phase mode. The hydrocarbon composition of synthetic and crude-derived jet fuels is very similar and all compounds detected in the synthetic product are also present in crude-derived fuels. Quantitatively, the synthetic fuel consists of a higher degree of aliphatic branching with less than half the aromatic content of the crude-derived fuel. GC×GC analyses also indicated the presence of trace levels of hetero-atomic impurities in the crude-derived product that were absent in the synthetic product. While clay-treatment removed some of the impurities and improved the fuel stability, the crude-derived product still contained traces of cyclic and aromatic S-containing compounds afterwards. Lower level of aromatics and the absence of sulphur are some of the factors that contribute to the better fuel stability and environmental properties of the synthetic fuel. GC×GC was further applied for the analysis of products during Jet Fuel Thermal Oxidation Testing (JFTOT), which measures deposit formation of a fuel under simulated engine conditions. JFTOT showed the synthetic fuel to be much more stable than the crude-derived fuel. 相似文献