983 resultados para Determination method


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A new method for the titrimetric determination of perchlorate has been developed, based on its reduction to chloride by iron(II) in a strong sulphuric acid medium at high temperature. The effect of variables, such as the sulphuric acid concentration, the temperature and the period of heating, on the extent of reduction has been studied and the optimal conditions for analytical determination of perehlorate derived.

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A colorimetric assay for the quantitative determination of catecholic compounds was developed. The method was based on the observation that a red color was formed when nitrite was added to a solution containing pyrocatechol and sodium tungstate. Aromatic amines interfere with the reaction but this could be overcome by the addition of formaldehyde. When interfering substances are present along with pyrocatechol, it can be readily separated by paper chromatography and estimated after elution from the filter paper.

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One mole of diethyl dixanthogen reacts with 26 moles of chloramine-T, and this reaction can be used for the determination of the dixanthogen. Higher alkyl dixanthogens react in a more complicated fashion, but may still be estimated using an empirical correction.

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In five-membered aromatic heterocyclic ring systems, a relation between the ratio of the distance between the two α to the two β protons and the covalent radii of the heteroatom is given. It is found that a similar relation is valid for the van der Waals radii also.

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Parkin (1978) suggested the velocity method based on the observation that the theoretical rate of consolidation and time factor plot on a log-log scale yields an initial slope of 1:2 up to 50% consolidation. A new method is proposed that is an improvement over Parkin's velocity method because it minimizes the problems encountered in using that method. The results obtained agree with the other methods in use.

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The behaviour of saturated soils undergoing consolidation is very complex, It may not follow Terzaghi's theory over the entire consolidation process, Different soils may behave in such a way as to fit into Terzaghi's theory over some specific stages of the consolidation process (percentage of consolidation), This may be one of the reasons for the difficulties faced by the existing curve-fitting procedures in obtaining the coefficient of consolidation, c(v). It has been shown that the slope of the initial linear portion of the theoretical log U-log T curve is constant over a wider range of degree of consolidation, U, when compared with the other methods in use, This initial well-defined straight line in the log U-log T plot intersects the U = 100% line at T = pi/4, which corresponds to U = 88.3%, The proposed log delta-log t method is based on this observation, which gives the value of c(v) through simple graphical construction, In the proposed method, which is more versatile, identification of the characteristic straight lines is very clear; the intersection of these lines is more precise and the method does not depend upon the initial compression for the determination of c(v).

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A sensitive and selective liquid chromatographic-tandem mass spectrometric (LC-MS-MS) method was developed to determine olanzapine (OLZ) in human urine. After solid-phase extraction with SPE cartridge, the urine sample was analysed on a C-18 column (Symmetry 3.5 mu m, 50 x 4.6 mm i.d) interfaced with a triple quadrupole tandem mass spectrometer. Positive electrospray ionization was employed as the ionization source. The mobile phase consisted of ammonium acetate (pH 7.8)-acetonitrile (10:90, v/v). The method was linear over a concentration range of 1-100 ngml(-1). The lower limit of quantitation was 1 ngml(-1). The intra-day and inter-day relative standard deviation across three validation runs over the entire concentration range was < 11.5 %. The accuracy determined at three concentrations (8.0, 50.0 and 85.0 ngml(-1) OLZ) was within +/- 1.21 % in terms of relative errors.

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A novel method is proposed for fracture toughness determination of graded microstructurally complex (Pt,Ni)Al bond coats using edge-notched doubly clamped beams subjected to bending. Micron-scale beams are machined using the focused ion beam and loaded in bending under a nanoindenter. Failure loads gathered from the pop-ins in the load-displacement curves combined with XFEM analysis are used to calculate K-c at individual zones, free from substrate effects. The testing technique and sources of errors in measurement are described and possible micromechanisms of fracture in such heterogeneous coatings discussed.

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Hydrogen peroxide (H2O2) level in biological samples is used as an important index in various studies. Quantification of H2O2 level in tissue fractions in presence of H2O2 metabolizing enzymes may always provide an incorrect result. A modification is proposed for the spectrofluorimetric determination of H2O2 in homovanillic acid (HVA) oxidation method. The modification was included to precipitate biological samples with cold trichloroacetic acid (TCA, 5% w/v) followed by its neutralization with K2HPO4 before the fluorimetric estimation of H2O2 is performed. TCA was used to precipitate the protein portions contained in the tissue fractions. After employing the above modification, it was observed that H2O2 content in tissue samples was >= 2 fold higher than the content observed in unmodified method. Minimum 2 h incubation of samples in reaction mixture was required for completion of the reaction. The stability of the HVA dimer as reaction product was found to be > 12 h. The method was validated by using known concentrations of H2O2 and catalase enzyme that quenches H2O2 as substrate. This method can be used efficiently to determine more accurate tissue H2O2 level without using internal standard and multiple samples can be processed at a time with additional low cost reagents such as TCA and K2HPO4.

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A two-dimensional model has been developed based on the experimental results of stainless steel remelting with the laminar plasma technology to investigate the transient thermo-physical characteristics of the melt pool liquids. The influence of the temperature field, temperature gradient, solidification rate and cooling rate on the processing conditions has been investigated numerically. Not only have the appropriate processing conditions been determined according to the calculations, but also they have been predicted with a criterion established based on the concept of equivalent temperature area density (ETAD) that is actually a function of the processing parameters and material properties. The comparison between the resulting conditions shows that the ETAD method can better predict the optimum condition.

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The use of growth layers in teeth as an indicator of age in odnotocetes and pinnipeds was suggested by Laws (1954) and since then the method has been used extensively in both marine and non-marine mammals. Dentinal growth layers are groups (growth layer groups) of repetitive alternating bands which in cross-section are similar to growth rings in trees. The most commonly used methods for counting growth layer groups (GLGs) are by undecalcified longitudinal thin sections (150 um) or decalcified and stained thin sections (10-30 um). In longitudinal sections viewed with light microscopy, GLGs appear as opaque and translucent cones nestled one inside another, with the oldest dentine Iying adjacent to the enamel, and the newest layer borderinq the pulp cavity.

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The content of free formaldehyde (FA) in minced fish muscle was measured by the following procedure: A mixture of minced fish muscle and water was deproteinized by means of the Carrez reagent. The FA content of the filtrate was determined reflectometrically using the Reflectoquant test strips and the RQflex. The results agreed well with the colorimetrically (Nash test) measured FA content. Der Gehalt an freiem Formaldehyd (FA)in Fischerzeugnissen wurde mit folgender Methode bestimmt: Zerkleinertes Fischfleisch wurde mit Wasser homogenisiert und mit Carrez-Reagenz enteiweißt. Der Formaldehydgehalt des Filtrates wurde reflektometrisch unter Verwendung von Reflectoquant-Teststätbchen und des RQflex ermittelt. Die Ergebnisse stimmten gut mit kolorimetrisch (Nash Test) gemessenen FA-Gehalten überein.