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941.
Miniaturizing all dimensions of apparatus, such as electronics and computers, is the current trend followed by scientists
in various fields. The idea of Lab-on-a-Chip has significantly expanded and found its broad applications in analytical chemistry.
Microplasmas can act as a sample excitation source and are the miniaturized versions of full-sized plasmas. These can be created
in various forms, such as direct current, microwave induced, capacitively coupled and inductively coupled plasmas. Scaling
down the size would reduce the amount of gases, liquids and consumables required, as well as the sample analysis time, which
in turn would decrease the operating costs. Therefore, several research groups are involved in the development of microplasmas
for utilisation in analytical instruments. 相似文献
942.
943.
944.
A capillary zone electrophoresis (CZE) method with ultraviolet-visible detection has been established and validated for the determination of five phenothiazines: thiazinamium methylsulfate, promazine hydrochloride, chlorpromazine hydrochloride, thioridazine hydrochloride, and promethazine hydrochloride in human urine. Optimum separation was obtained on a 64.5 cm x 75 microm bubble cell capillary using a buffer containing 150 mM tris(hydroxymethyl)aminomethane and 25% acetonitrile at pH 8.2, with temperature and voltage of 25 degrees C and 20 kV, respectively. Naphazoline hydrochloride was used as an internal standard. Field-amplified sample injection (FASI) has been applied to improve the sensitivity of the detection. Considering the influence of parameters affecting the on-line preconcentration (nature of preinjection plug, sample solvent composition, injection times, and injection voltage) and due to the significant interactions among them, in this paper we propose for the first time the application of a multivariate approach to carry out the study. The optimized conditions were as follows: preinjection plug of water for 7 s at 50 mbar, electrokinetic injection for 40 s at 6.2 kV, and 32 microm of H3PO4 in the sample solvent. Also, a solid-phase extraction (SPE) procedure is developed to obtain low detection limits and an adequate selectivity for urine samples. The combination of SPE and FASI-CZE-UV allows adequate linearities and recoveries, low detection limits (from 2 to 5 ng/mL), and satisfactory precisions (3.0-7.2% for an intermediate RSD %). 相似文献
945.
Danielle Giron S. Monnier M. Mutz P. Piechon T. Buser F. Stowasser K. Schulze M. Bellus 《Journal of Thermal Analysis and Calorimetry》2007,89(3):729-743
Adequate very sensitive quantification methods are needed for the development and are also now required for the monitoring
of undesirable solid form(s) as routine tests. The pre-requisite for quantitation are selectivity, sensitivity and most important
the purity of standards and their proper storage, what is a challenge for metastable forms.
Several analytical techniques are available such as X-ray diffraction, spectroscopy, thermal analysis and microcalorimetry.
The different steps of the validation of the analytical methods and problems to be solved are discussed. Examples illustrate
the different techniques and compare their possible advantages and limits. The relative standard deviation of measurements
should allow for checking the homogenization procedure of mixtures for calibration. The validation should be carried out following
ICH guidelines for validation of analytical methods. Comparison of different techniques in adequate concentration range add
confidence in the analytical results. 相似文献
946.
Andrzej Czerwiński Iwona Kiersztyn Michał Grdeń 《Journal of Solid State Electrochemistry》2003,7(6):321-326
The effect of temperature on hydrogen and deuterium electrosorption into a palladium LVE (limited-volume electrode) has been
investigated. A decrease in hydrogen capacity (H/Pd ratio) with increasing temperature has been observed. Temperature strongly
influences the plots of measured H(D)/Pd values vs. potential scan rate. In addition, hydrogen absorption was found to be
dependent on the composition of the surrounding electrolyte solution. These results have confirmed the hypothesis that two
different mechanisms of hydrogen desorption from the palladium electrode take place, namely electrochemical oxidation and
non-electrochemical recombination. Further, the ratio between the rate constants for these two processes has been found to
change with temperature.
Electronic Publication 相似文献
947.
Summary The thermal behavior of KH2PO4, NaH2PO4 and Na2HPO4 under non-isothermal conditions using TG method with different heating rates was studied. The values of the reaction rate were processed by means of Friedmans differential-isoconversional method. A dependence of the activation energy vs. conversion was observed. Therefore a procedure based on the compensation effect (suggested by Budrugeac and Segal) was applied. A less speculative data processing protocol was offered by the non-parametric kinetics method suggested by Serra, Nomen and Sempere. Three steps were observed by non-isothermal heating: a dehydration, a dimerization and a polycondensation. The differences in the intimate reaction mechanism are determined by the initial number of water molecules. 相似文献
948.
Employing hot tungsten filament to thermal dissociate molecular hydrogen,we generated gas phase atomic hydrogen under ultra-high vacuum(UHV)conditions and investigated its interaction with Pt(111) surface.Thermal desorption spectroscopy(TDS)results demonstrate that adsorption of molecular hy- drogen on Pt(111)forms surface Had species whereas adsorption of atomic hydrogen forms not only surface Had species but also bulk Had species.Bulk Had species is more thermal-unstable than surface Had species on Pt(111),suggesting that bulk Had species is more energetic.This kind of weakly- adsorbed bulk Had species might be the active hydrogen species in the Pt-catalyzed hydrogenation reactions. 相似文献
949.
Ahmad Shaabani Abbas Rahmati Soheila Naderi 《Monatshefte für Chemie / Chemical Monthly》2007,138(6):553-557
Summary. Reaction of triphenylphosphine and an electron deficient acetylenic ester in the presence of strong N–H acid such as alkyl
and aryl sulfamides or acetamide produces phosphorous ylides at room temperature in CH2Cl2. The aryl sulfamide phosphoranes undergo a smooth transformation reaction in boiling toluene and produce iminophosphoranes. 相似文献
950.
Crown ethers were reacted with HN-proton-donor molecules to obtain crystalline molecular host-guest complexes. It was found that complexes with crown ethers of different structure are formed, depending on the linear dimensions and mode of steric shielding of active centers of the proton-donor molecules.Translated from Zhurnal Obshchei Khimii, Vol. 74, No. 12, 2004, pp. 2030–2033.Original Russian Text Copyright © 2004 by Wang, Ganin.This revised version was published online in April 2005 with a corrected cover date. 相似文献