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41.
《Surface and interface analysis : SIA》2005,37(7):589-607
The accuracy of quantitative XPS analysis can be improved using predetermined transmission functions. Two different calibration methods are used for estimating the transmission function T(E) of a photoelectron spectrometer, applying a survey spectra approach (SSA) and a quantified peak‐area approach (QPA) to minimize the quantification error. For the SSA method, Au, Ag and Cu spectra measured with the Metrology Spectrometer II have been used. The new QPA method was built up from Au 4f, Au 4d, Au 4p3/2, Ag 3d, Ag 3p3/2, Cu 3p, Cu 2p3/2, Ge 3p and Ge 2p3/2 standard peak areas, applying adequate ionization cross‐sections and mean free path lengths for different pass energies (10 and 50 eV), lens modes (large area, large area XL, small area 150) and x‐ray sources (Al/Mg Twin and Al Mono). In the energy range 200–1500 eV a transmission function T(E) = a0 + b1E (where a0, b1 and b2 are variable parameters) was found to give an appropriate approximation for eight tested spectrometer settings, implementing the largest changes in the case of pass energy variations. Determination and application of the transmission functions were integrated in the XPS analysis software (UNIFIT 2004) and tested by means of an Ni90Cr10 alloy. The results demonstrate the practicability of the SSA and QPA methods, giving decreased errors of <8% in comparison with errors up to 38% obtained using Wagner's sensitivity factors. Copyright © 2005 John Wiley & Sons, Ltd. 相似文献
42.
Summary A new porous polyaromatic ester packing was synthetized for high performance liquid chromatography. The relationship between retention and chain length of the members of homologous series of alkylbenzenes, N-alkylanilines, alkylarylethers, alkylbenzoates and alkylarylketones on this new stationary phase using different eluents was investigated. Using the alkylarylketone scale the retention indices of the homologues and test compounds were calculated. The results were compared with those obtained for poly (styrene-divinylbenzene) polymers. For both types of packing the first members of each homologous series gave non-linear behaviour. The methylene group index increments are different for the studied homologous series; thus there is no simple additivity of the retention indices. The efficiency of the porous polymeric columns is a function of the capacity factor of the solute and the organic component of the eluent. 相似文献
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High nuclearity paramagnetic, spin-coupled transition metal clusters and grids are fascinating chemists and physicists partly because of their structural beauty, and the challenge of creating them, but also because of their novel physical properties. Magnetic interactions between the spin centers are a primary focus. This review will examine a selection of Mn(II) polynuclear grids and clusters, with nuclearities in the range Mn4 to Mn9. Theoretical treatments of the magnetic properties are discussed, and approaches to solving the exchange problem for ‘large’ spin systems related to computational difficulties. A freely available software package (MAGMUN4.1) is presented as a means of dealing simply with spin-coupled clusters in general, and symmetry reduction methods are discussed briefly as a means of dealing with ‘large’ spin systems. 相似文献
47.
G. Glöckner 《Chromatographia》1987,23(7):517-524
Summary Prerequisite of quantitative evaluation in chromatography is equivalence of sample composition and detector signal. This includes
complete retention and proper elution of all sample constituents. In polymer HPLC, complete retention requires a poor starting
eluent, a sufficiently active column, and a low ratio of injection volume to column volume. On small pore columns, insufficient
retention caused the polymer to elute either in the interstitial volume (sample exclusion), together with the sample solvent,
or immediately after the solvent plug.Stat-copoly(styrene/ethyl methacrylate) samples are more difficultly retained thanstat-copoly(styrene/acrylonitrile) specimes. With the former copolymer it could be shown that incomplete retention did not cause
sample demixing. In order to gain complete retention, non-exclusion HPLC of polymers should be performed with columns whose
solvent volume is at least 50 times as large as the injection volume. This consequence is of practical importance in chromatographic
cross-fractionation where rather large volumes of SEC eluate are injected into the apparatus for gradient HPLC. 相似文献
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Per Hyltoft Petersen 《Accreditation and quality assurance》2002,7(11):488-493
The validity of any model depends on its ability to imagine the situation or problem to which it is applied. Further, the
assumptions made in relation to the model are determining for the actual outcome. Within the field of clinical biochemistry
a lot of models for analytical quality specifications, based on a variety of concepts and ’clinical settings’, have been proposed.
A hierarchical structure for application of these approaches and models has been agreed on at several occasions in 1999. In
this hierarchy, the highest rank is given to evaluation of analytical quality specifications based on ’clinical settings’/’clinical
outcome’ models, followed by specifications based on biological variation and on ’clinicians opinions’. This contribution,
deals with the problems of combining random and systematic errors and the implications of application of different models
to a variety of clinical settings.
Received: 1 June, 2002 Accepted: 17 July 2002
Presented at the European Conference on Quality in the Spotlight in Medical Laboratories, 7–9 October 2001, Antwerp, Belgium 相似文献
50.
Several on-column sample preconcentration modes--large-volume sample stacking using the EOF pump (LVSEP), LVSEP with anion-selective exhaustive injection (LVSEP-ASEI) and field-amplified sample injection with sample matrix removal using the electroosmotic flow (EOF) pump (FAEP)--were used to analyze some nonsteroidal anti-inflammatory drugs (NSAIDs) by capillary electrophoresis, and then compared. Methanol was the background electrolyte solvent to suppress the EOF. The effect of the type and length of the solvent plug, and the sample injection time were investigated in FAEP to determine the conditions that provided the best response. LVSEP, LVSEP-ASEI, and FAEP improved the sensitivity of the peak area by 100-, 1200-, and 1800-fold, respectively. The methodology developed, in combination with solid-phase extraction (SPE), was applied to the analysis of water samples. 相似文献