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971.
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
972.
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
973.
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
974.
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
975.
Gámiz-Gracia L Cuadros-Rodrı́guez L Almansa-López E Soto-Chinchilla JJ Garcı́a-Campaña AM 《Talanta》2003,60(2-3):523-534
A new formal strategy in the multidimensional optimisation of the experimental variables affecting the chemiluminescence (CL) detection in flow injection analysis (FIA) is proposed here. The strategy implies several steps, being the most significant: selection of the variables to be studied and their experimental domain; use of a screening design to detect significant variables and interactions into the experimental region; study of the main effect of variables and second-order interactions; and finally application of a Draper-Lin small composite design (orthogonal) to obtain the optimum values of the significant variables. The methodology is applied to the determination of methylamine by FIA based on the use of the peroxyoxalate CL (PO-CL) reaction. Considering the high number of experiments required due to the different chemical and instrumental variables to be taken account and their adequate compatibility to obtain maximum sensitivity, the methodology offers a rigorous study of the main effects and interactions, achieving a reduction of experimental work. 相似文献
976.
Branco LC Serbanovic A da Ponte MN Afonso CA 《Chemical communications (Cambridge, England)》2005,(1):107-109
The combination of ionic liquids (ILs) as solvents in the asymmetric Sharpless dihydroxylation (AD) with the use of scCO(2) in the separation process allows a very simple, efficient, clean and robust system for the reuse of the AD catalytic system, which also does not need the use of organic solvents either for the reaction or for the separation of products and allows the isolation of the diol, in high yield and enantiomeric excess and basically without contamination with osmium. 相似文献
977.
Let Ω be an open subset of , N ? 3, containing 0. We consider the solutions of ?Δu(x) + g(u(x)) = f(x) in Ω-{0}, where g is nondecreasing and f is bounded and we study the possible singularities at 0: when u(x) = o(|x|1 ? N) we prove that u is isotropic near 0 and show that either it is a C1 function in Ω (removable singularity) or |x|N ? 2u(x) → c, c ≠ 0 (weak singularity) or |x|N ? 2 |u(x) |→ + ∞ (strong singularity). We also characterize the g's for which solutions with a weak singularity exist and improve a previous removability result of H. Brézis and L. Véron (Arch. Rational Mech. Anal.23 (1979), 153–166). 相似文献
978.
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
979.
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