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991.
A new reactor and a novel in-situ sampling technique were developed for the study of the synthesis of CeO2 powders produced from dissolved cerium nitrate salts. The conical reactor minimized particle recirculation and provided a
highly symmetrical and undisturbed plasma flow suitable for the analysis of the phenomena affecting the formation of CeO2 powders. Both a calorimetric study of the reactor and a thermodynamic analysis of CeO2 formation were conducted. The sampling probe is described and near-isokinetic sampling was achieved. The sampled particles
were collected using a miniature wet collection system, i.e. a mist atomizer and a custom-made spray chamber. A numerical
simulation of the velocity and temperature fields of the plasma gas in the reactor was done using Fluent. A comprehensive
droplet-to-particle formation mechanism presented elsewhere is revisited and expanded based on calorimetry, thermodynamics
of CeO2 formation, numerical simulations and collected particles. No traces of other oxidation states other than CeO2 were found. 相似文献
992.
Anna Daghetti Carlo Gatti Sergio Trasatti 《Journal of Electroanalytical Chemistry》1985,196(1):179-197
Three isotherms are considered: Frumkin's Bennes' and Mohilner's. The relationship between the interaction parameters in the first two and the adsorbate activity coefficient in the last is discussed. The significance of various standard states for the definition of ΔG° ads is analysed. The operational derivation of ΔG°ads in the three cases and the relationship between the resulting three quantities are illustrated. The isotherms have been used to describe the adsorption of 1,4-dioxane on a polarized Hg electrode. The analysis has been carried out both at constant potential and constant charge. The picture emerging in each of the three cases is discussed in the light of the results obtained in the other two. It is concluded that the three approaches give the same qualitative information about the interfacial behaviour of dioxane, especially as far as the effect of the electric field and the particle-particle lateral interaction are concerned. The usefulness of the Frumkin isotherm for analysing promptly experimental adsorption data is thus maintained. Limitations of the present approach are discussed. 相似文献
993.
R. A. Alieva S. Z. Gamidov F. M. Chyragov A. A Azizov 《Journal of Analytical Chemistry》2005,60(12):1114-1117
A method is developed for cadmium and zinc preconcentration on a minicolumn packed with a new chelating polymer sorbent. The effects of the test solution pH and volume, the sample matrix composition, the eluent volume, and the sample and eluent flow rates are studied. Zinc and cadmium in the eluate are determined by flame atomic absorption spectrometry. Under optimal conditions, the determined ion recovery is more than 95%. The detection limits (3σ, n = 20) are found to be 15.0 (Cd) and 17.2 (Zn) ng/mL. The developed method is employed for cadmium and zinc determination in samples of seawater and water obtained after oil pumping. 相似文献
994.
An amperometric detector with a small thin mercury film electrode is described. The device demonstrates advantageous operational
characteristics such as small dispersion (D<2) and “memory effect” (me<0.6%), extensive maximum sample frequency (msf −200
samples/h), and high sensitivity. It has been proven useful in flow-injection analysis at a constant potential under hydrodynamic
conditions. 相似文献
995.
In the course of investigations on equestrian supplemental products for the presence of doping substances, two products were found to contain forbidden substances. As reported earlier a plant extract (Mexican cactus extract) named “Energy 5” contained the anabolic androgenic steroids (AAS) stanozolol, 17β-hydroxy-17α-methyl-5α-androstane-3β-ol (3β,5α-THMT) as well as mestanolone not declared on the label. In the present study, a product called “Super Kalm Paste” was tested. Analysis by gas chromatography - mass spectrometry (GC-MS) revealed that the preparation contained the class I anti-arrhythmics quinine (trade names KinidinTM, Durules) and cinchonine. The samples were prepared according to a sample preparation procedure established for anabolic steroids in nutritional supplements for humans. The sample treatment comprised the extraction and purification of the analytes as well as the chemical conversion with N-methyl-N-trimethylsilyl-trifluoracetamide (MSTFA) to yield the trimethylsilyl (TMS)-derivatives. To verify whether the administration of such products could lead to positive doping tests, a pilot excretion study on “Energy 5” was conducted with two geldings, and urine samples were collected. Gas chromatography - high resolution mass spectrometry (GC-HRMS) after solid phase extraction and mixed derivatisation has demonstrated the presence of the stanozolol metabolite 16β-hydroxy-stanozolol in urine samples after “Energy 5” application. 相似文献
996.
An efficient and environmentally friendly method preparing 2H-azirines in good yield has been achieved by microwave irradiation of vinyl azides in solvent free conditions. 相似文献
997.
Krzysztof Stolarczyk Renata Bilewicz Anna Skwierawska Jan F. Biernat 《Journal of inclusion phenomena and macrocyclic chemistry》2004,49(1-2):173-179
Properties of monolayers of azocrown compound self-assembled on gold substrates were studied using voltammetry and scanning tunneling microscopy. The surface concentrations of this compound in monolayers were determined from the area of the voltammetric reduction peaks. The area per one molecule estimated from voltammetry experiments is 0.65 nm2. This value was comparable with the limiting molecular area of the compound in the Langmuir–Blodgett film at the air–water interface. We also observed the presence of gold clusters and other gold structures by STM when a gold electrode modified with azocrown compound was dipped into the tetrachloroaurate solution. Even better spectra of clusters were obtained following one voltammetric scan in the range 0.5 to ?0.6 V. After more cycles or if we condition the electrode at 0.4 V the clusters aggregate into wires. 相似文献
998.
Anna Kowalska Zygmunt Kowalski Andrzej Kotarba Andrzej Barański 《Mikrochimica acta》1990,100(5-6):349-353
The analytical procedure of determination of Fe(II) in the presence of Fe(III) in milligram samples is proposed. A solid sample is dissolved in hydrochloric acid in argon atmosphere. Subsequently, the pH-value of the solution is fixed and Fe(III) complexed by phosphoric buffer. At the next step Fe(II) is oxidized by -molybdosilicic acid. Finally, the intensity of colouring caused by the reduced form of the acid is measured at the wavelength 770 nm. The proper treatment of the sample during oxidation, and immediately before, is decisive for the accuracy of the analysis. The method was verified by means of the analysis of synthetic magnetite. The theoretical content of Fe(II) was 24.12%, the determined one was 24.02 ± 0.10%. The method was applied to the determination of the homogeneity of an iron catalyst for ammonia synthesis. 相似文献
999.
Dusanka Ž. Obadović Anikó Vajda Maya Garić A. Bubnov Vera Hamplová M. Kašpar Katalin Fodor-Csorba 《Journal of Thermal Analysis and Calorimetry》2005,80(2):519-523
Summary Thermal properties of a homologous series of ferroelectric liquid crystals S-(-)-[4-(2-n-alkoxy-propionyloxy)]biphenyl-4'-[n-alkoxy-(3,5-dimethyl)]benzoate have been investigated by polarizing optical microscopy and differential scanning calorimetry.
The mesophases were identified and confirmed by X-ray too. Three binary mixtures were prepared from the individual homologues.
In one of the mixtures (Mix1), the ferroelectric SmC* phase has broadened and became enantiotropic. This mesophase remained
monotropic in the other two mixtures (Mix2, Mix3). The chiral nematic N* phase did not appear in Mix1, but remained monotropic
for the other two mixtures. Two molecular parameters, the layer spacing and the average intermolecular distance have been
calculated from the X-ray results for the homologues and their mixtures. An intercalated tail-to-tail packing of molecules
was found both in the single compounds and their mixtures resulting in the layer spacing about half of the molecular length
of the single compounds. 相似文献
1000.