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91.
Summary The method developed for simultaneous determination of hydrogen (by means of an equivalent amount of iodine) and of nitrogen by a volumetric method, is based on a flash combustion technique in a stream of CO2 (100 ml/min) with controlled addition of O2 (20%). Hydrogen is determined by conversion of water into hydrogen chloride on anhydrous magnesium chloride heated at 600–650° C, and reaction of the hydrogen chloride with Ag2OI2 at 220° C to yield iodine, which is collected on silver and weighed. The precision of the determination of hydrogen is excellent, the standard deviation being 0.008–0.017% abs., about a tenth of that obtained by the classical methods. The error in the determination of hydrogen was ±0.006% abs.
Gleichzeitige Bestimmung von Wasserstoff als dessen Jodäquivalent und von Stickstoff auf volumetrischem Wege
Zusammenfassung Die entwickelte Methode zur gleichzeitigen Bestimmung von Wasserstoff in Form seines Jodäquivalents und von Stickstoff auf gasvolumetrischem Wege beruht auf der Entflammungsmineralisation im CO2-Strom (100 cm3/min) mit kontrolliertem Zusatz von O2 (20%). Der Gasstrom wird zusätzlich über P2O5 getrocknet. Die dem Wasserstoff äquivalente Jodmenge wird an metallischem Silber gebunden und gravimetrisch bestimmt, wobei Wasser bei 600–650° C mit Magnesiumchlorid in Chlorwasserstoff übergeführt wird, der nachfolgend bei 220° C mit Ag2Oj2 zu Jod umgesetzt wird. Für Verbindungen, die neben C, H, N und O auch Br, Cl, P und S enthalten, werden Wasserstoffresultate mit hoher Präzision erzielt:s H beträgt 0,008 bis 0,017% absolut und ist etwa 10mal kleiner als bei den üblichen, klassischen Methoden. Die Genauigkeit der Wasserstoffbestimmung entspricht einem mittleren Fehler=±0,006% absolut. Die Resultate für den Wasserstoff und Stickstoff verlangen eine Blindwertkorrektur.相似文献
92.
The study of the phenomena related to the motion of particles flowing in the proximity of the wall is pursued for purely cognitive reason as well as for some important practical purposes in various fields of technology, biology and medicine.When small spherical rigid particles move in the direction parallel to the surface their velocity is smaller than that of the fluid and depends on the ratio of the distance from the wall to the particle radius. The velocity of a particle falling down in a vertical cylinder is maximal in an eccentric position. A sphere in contact with the wall remains stationary. Translational velocity of spherical rigid particles the dimension of which are comparable to that of the tube is only slightly dependent of their lateral position. The differences in the flow parameters of deformable particles in comparison with rigid ones depend on the particle and fluid viscosity coefficient. When the particles move perpendicularly toward the wall, their velocity decreases as the particle approaches the surface. The change of particle velocity is inversely proportional to the gap.There are several theories explaining the influence of the channel diameter on the suspension viscosity (sigma phenomenon); a modern approach is based on the analysis of rheological properties of suspensions. The explanations of the Fahraeus effect (i.e. the fact that the concentration of particles flowing in a tube linking two containers are smaller than that in the containers) are based on non-uniform particle distribution in a transverse cross section and on the differences of velocities of particles and medium. The deviation of the velocity profile of a suspension of rigid particles flowing through a tube from the parabolic shape (blunting) does not depend on the flow velocity; as concerns deformable particles, however, this effect is the smaller the greater is the flow velocity.When the Reynolds number for particles is greater than 10-3, there appears a component of particle velocity perpendicular to the streamline direction.This phenomenon is the cause of the lateral migration of particles. Neutrally buoyant rigid particles migrate to a certain concentrical region situated between the tube axis and the wall (tubular pinch region). Deformable neutrally buoyant particles migrate towards the tube axis, and deformable non-neutrally buoyant particles may move either toward the tube axis or toward the wall.In the research on the influence of the flow delimiting surface on the motion of particles in suspension a considerable progress has recently been made.However, the phenomena in this field are extremely complex. At present, two main types of approach may be distinguished. On a microscopic level direct interactions between particles and surfaces are analyzed. A macroscopic approach consists in treating particle suspension as fluid, and overall influence of the surface on its properties are studied. A comprehensive theory linking these two levels has not yet emerged. 相似文献
93.
We consider the motion of compressible viscous fluids around a rotating rigid obstacle when the velocity at infinity is non zero and parallel to the axis of rotation. We prove the existence of weak solution. 相似文献
94.
We prove a separable reduction theorem for σ-porosity of Suslin sets. In particular, if A is a Suslin subset in a Banach space X, then each separable subspace of X can be enlarged to a separable subspace V such that A is σ-porous in X if and only if A∩V is σ-porous in V. Such a result is proved for several types of σ-porosity. The proof is done using the method of elementary submodels, hence the results can be combined with other separable reduction theorems. As an application we extend a theorem of L. Zají?ek on differentiability of Lipschitz functions on separable Asplund spaces to the nonseparable setting. 相似文献
95.
Iwona Kwiecień Grażyna Adamus Marek Kowalczuk 《Rapid communications in mass spectrometry : RCM》2012,26(23):2673-2682
96.
Piotr Kulpinski Marek Namyslak Tomasz Grzyb Stefan Lis 《Cellulose (London, England)》2012,19(4):1271-1278
UV- active cellulose fibers were obtained by dry-wet method spinning an 8?% by weight α-cellulose solution in N-methylomorpholine-N-oxide (NMMO) modified by europium-doped gadolinium oxyfluoride Gd4O3F6:Eu3+ containing 5?mol (%) of the dopant. Photoluminescent nanoparticles were introduced in the in powder form into a polymer matrix during the process of cellulose dissolution in NMMO. The dependencies of emission intensity on excitation energy and the concentration of Gd4O3F6:Eu3+ nanoparticles in the final cellulosic products were examined by photoluminescence spectroscopy (excitation and emission). The fiber structure was studied by X-ray powder diffraction analysis. The size and dispersity of the nanoparticles in the polymer matrix were evaluated using scanning electron microscopy and X-ray microanalysis. The influence of different concentration particles (in the range from 0.5 to 5?% by weight) on the mechanical properties of the fibers, such as tenacity and elongation at break, were determined. 相似文献
97.
The influence of solvents and catalysts on the formation of soluble and insoluble polymer during cationic polymerization of 2,5-dimethyl-l,5-hexadiene was studied. In nonpolar medium (n-heptane or without solvent) the amount of the insoluble part is dependent on the catalyst used and increases as follows: BF3 ? AlBr3 < TiCl4. Especially soluble polymers are obtained in a solution of methylene chloride or in a mixture of methylene chloride-nitrobenzene. The temperature range studied, -30° to -78°, did not show any important influence on the polymer composition. It was found that the bulky anion of the initiator and the polarity of the medium considerably influenced cyclization during intra-intermolecular propagation of the polymer chain. 相似文献
98.
The polymerization of isobutylene with VCl4 in n-heptane or in the bulk does not proceed in the dark at temperatures lower than -20°C, yet it may be induced by the addition of styrene, α-methylstyrene, p-divinylbenzene, 1,3-butadiene, isoprene, and 2,3-dimethyl-1,3-butadiene. In these cases the polymerizations proceed with variously long induction periods depending on the type of comonomer used. The shortest induction period was observed after the addition of p-divinylbenzene and 2, 3-dimethyl-1, 3-butadiene. In a nonpolar medium the copolymerization of isobutylene with isoprene or butadiene in the dark gives rise to copolymers insoluble in heptane, benzene, and CCl4, while co-polymers formed with the effect of light are soluble. Unlike polymerizations carried out in a nonpolar solution, the polymerization of isobutylene with VCl4 in methyl chloride proceeds spontaneously in the absence of protonic coinitiators. Also, soluble copolymers of isobutylene with isoprene or butadiene arise in the copolymerization in methylchloride solution irrespective of the procedure used when the copolymerization is carried out (in the dark or with the effect of light). Polymerizations and copolymerizations carried out both in nonpolar and in polar solutions are inhibited by the presence of oxygen. 相似文献
99.
Heteroaromatic N-oxides bearing various functionalities are readily and selectively converted under mild conditions into the corresponding bases using TiCl4/SnCl2. 相似文献
100.
Fuzzy identification of cutting acoustic emission with extended subtractive cluster analysis 总被引:1,自引:0,他引:1
This paper presents fuzzy acoustic emission identification in high precision hard turning process based on extended subtractive
cluster analysis combined with the least-square estimation method. The fuzzy identification method provides a simple way to
arrive at a definite conclusion based upon the information obtained with the difficulty in understanding the exact physics
of the machining process. The experimental results prove that the proposed method is efficient and feasible. 相似文献