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Stable isotope methods are potentially quite useful for validating natural or enhanced mineral degradation of contaminants. For this reason, a continuous flow gas chromatograph (GC), isotope ratio mass spectrometer (IRMS) has been coupled with a quadrupole mass selective detector (MSD) to allow simultaneous mass spectral and stable carbon isotope ratio data to be obtained from a single chromatographic analysis. This allows the target contaminant and any extra-cellular degradation intermediates to be both qualified and quantified. Previously acceptable limits of precision (0.3 parts per mil) are undesirable given the small fractionation observed during aerobic degradation. To further understand the fate of organic contaminants and to gain information about the metabolic degradative pathway employed by a microorganism, routine isotopic analyses on a range of analytes have been performed. Quantities of sample producing mass-44 ion beam signal (I(44)) of 2 x 10(-10) to 1 x 10(-8) A were analysed. When the IRMS was tuned for high sensitivity, ion source nonlinearities were overcome by peak height correction from an algorithm that was produced using known isotopic standards of varying concentrations. This led to sample accuracy of <0.01 per thousand and sample precision of 0.1 per thousand. Copyright 1999 John Wiley & Sons, Ltd. 相似文献
23.
KM Clauwaert Van Bocxlaer JF HJ Major JA Claereboudt WE Lambert Van den Eeckhout EM Van Peteghem CH De Leenheer AP 《Rapid communications in mass spectrometry : RCM》1999,13(14):1540-1545
This paper describes the investigation of the potential of a quadrupole orthogonal acceleration time-of-flight mass spectrometer (Q-TOF) equipped with an atmospheric pressure ionisation interface for quantitative measurements of small molecules separated by reversed phase liquid chromatography. To this end, the detection limits and linear dynamic range in particular were studied in an LC/MS/MS experiment using 3,4-methylenedioxymethamphetamine standards and 3,4-methylenedioxyethylamphetamine for internal standardisation. In a second phase, the experiment was repeated with real biological extracts (whole blood, serum, and vitreous humour). A calibration for 3,4-methylenedioxymethamphetamine and its metabolite 3,4-methylenedioxyamphetamine was prepared in each of these matrices again using 3,4-methylenedioxyethylamphetamine as internal standard. The resulting quantitative data were compared with those obtained by liquid chromatography with fluorescence detection for the same extracts. The Q-TOF results revealed excellent sensitivity and a linear dynamic range of nearly four decades (2-10 000 pg on-column, r(2) = 0.9998, 1/x weighting). Furthermore, all the calibration curves prepared in biological material were superimposable, LC/MS/MS and LC-fluorescence, and the quantitative results for actual samples compared very favourably. It was concluded that the Q-TOF achieves a linear dynamic range for quantitative LC/MS/MS work exceeding that of fluorescence detection and at much better absolute sensitivity. Copyright 1999 John Wiley & Sons, Ltd. 相似文献
24.
S. Bashir R. W. McCabe C. Boxall M. S. Leaver D. Mobbs 《Journal of nanoparticle research》2009,11(3):701-706
Forced hydrolysis of Fe(III) ions in acidic media was performed under controlled synthetic conditions to produce α- and β-FeOOH
iron oxides. The forced hydrolysis synthesis was carried out, separately, in an aqueous medium and the lamellar lyotropic
liquid crystalline phase of a commercial non-ionic surfactant/water system. The FT-IR analyses confirmed formation of α- and
β-FeOOH iron oxides in the aqueous and the surfactant media with slight formation of ferrihydrite and haematite. TEM micrographs
have shown that particles formed in the lamellar lyotropic phase are smaller than those produced in the aqueous medium with
their smallest size dimension being constrained in the nanometre scale with a size ranging between 5 and 100 nm. Particles
produced in the nanoscale size appeared to have different optical properties compared to their counterparts produced in the
microscale size. 相似文献
25.
Lifetimes of high spin states up to {
}=22+ in the yrast positive parity bands have been measured to investigate the shape evolution with increasing spin in 72, 74Se. The Q
t values derived from these measurements indicate that prolate shape stabilizes for 72Se, while a triaxial shape develops for 74Se at higher spins. Comparison of the observed trend in Q
t with spin for 72, 74Se with that of the corresponding kryptones isotones emphasizes the stability provided by N=38 prolate shell gap even at high rotational frequency. 相似文献
26.
Andrew J. Parker Colin Boxall Malcolm J. Joyce 《Journal of Radioanalytical and Nuclear Chemistry》2013,298(2):797-802
The potential of 40K as a radioactive tracer analogue of 137Cs in ion exchange experiments is reported. Solutions of varying concentrations of potassium chloride (KCl) have been monitored radiometrically in a sodium iodide well-counter to determine the activity-concentration relationship. Ion exchange reactions using an exemplar ion exchange resin, KCl and non-radioactive caesium chloride (CsCl) solutions have been studied radiometrically. The adsorbed amounts of potassium and caesium are observed, inferred from displaced K+ ions, to be consistent with the total exchange capacity of the resin. Adsorption isotherm models have been applied to the experimental data, with the Freundlich isotherm observed to fit the data with the highest degree of consistency. The reported results indicate that decontamination techniques involving hazardous isotopes of anthropogenic origin such as 137Cs can be developed, evaluated and optimised by substituting a chemically and physically similar non-hazardous radioactive isotope, in this case 40K. This represents a means by which innovative decontamination techniques and regimes might be identified without the need to use 137Cs and thus avoids additional generation of radioactive wastes. 相似文献
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Hydroxamic acids (XHAs) are organic compounds with affinities for cations such as Fe3+, Np4+ and Pu4+ and have been identified as useful reagents in nuclear fuel reprocessing. Acid catalyzed hydrolysis of free XHAs is well
known and may impact negatively on reprocessing applications. The hydrolysis of metal-bound XHAs within metal ion-XHA complexes
is less understood. With the aid of speciation diagrams, we have modelled UV-visible spectrophotometric kinetic studies of
the acid-catalyzed hydrolysis of acetohydroxamic acid (AHA) bound to the model ion Fe(III). These studies have yielded the
following information for the hydrolysis of AHA in the Fe(AHA)2+ complex at 293 K: (i) the order with respect to [H+] during the rate determining step, m=0.97, is the same as for the free ligand, indicating a similarity of mechanisms; and (ii) the kinetic rate parameter, k
1=1.02×10−4 dm3⋅mol−1⋅s−1, is greater than that for the free ligand, k
0=1.84×10−5 dm3⋅mol−1⋅s−1 for pH>−0.5, a result that is consistent with a Hammett analysis of the system. 相似文献
30.
Hydroxamic acids are salt free, organic compounds with affinities for cations such as Fe3+, Np4+ and Pu4+, and have been identified as suitable reagents for the control of Pu and Np in advanced nuclear fuel reprocessing. The results
of a UV-visible, near-IR spectrophotometric study of the 1:1 and 2:1 complexes formed between formo- and aceto-hydroxamic
acids (FHA, AHA) and Np(IV) ions are interpreted using speciation diagrams for the identification of the species present at
different pH and ligand to metal ratios. A kinetic model that describes the instability of the complex due to hydrolysis of
the hydroxamate moiety, previously developed for the Fe(III)-AHA complexes (Andrieux et al. in J. Solution Chem. 36:1201–1217,
[2007]), is tested here against experimental Np(IV)-FHA data. Consequently, the complexation constant for formation of the 1:1
Np(IV)-FHA complex in nitric acid is estimated at K
1=2715 and indications are that complexation protects the ligand against hydrolysis at 0.1>pH>−0.1. 相似文献