Analyzing alloys

Examples Pure metal powders may be compressed into solid discs or cylinders which can be used as electrodes. Likewise, the analyzing alloys can also be used. 

The lattice parameter of a binary solid solution of B in A depends only on the percentage of B in the alloy, as long as the solution is unsaturated. This fact can be made the basis for chemical analysis by parameter measurement. All that is needed is a parameter vs. composition curve, such as curve be of Fig. 12-8(b), which can be established by measuring the lattice parameter of a series of previously analyzed alloys. This method has been used in diffusion studies to measure the change in concentration of a solution with distance from the original interface. Its accuracy depends entirely on the slope of the parameter-composition curve. In alpha brasses, which can contain from 0 to about 40 percent zinc in copper, an accuracy of +1 percent zinc can be achieved without difficulty. 

Inorganic analytes that are neutral in aqueous solutions may still be analyzed if they can be converted to an acid or base. For example, N03 can be quantitatively analyzed by reducing it to NH3 in a strongly alkaline solution using Devarda s alloy, a mixture of 50% w/w Cu, 45% w/w Al, and 5% w/w Zn. 

An alloy of chromel containing Ni, Fe, and Cr was analyzed by a complexation titration using EDTA as the titrant. A 0.7176-g sample of the alloy was dissolved in ITNOa and diluted to 250 mb in a volumetric flask. A 50.00-mb aliquot of the sample, treated with pyrophosphate to mask the Fe and Cr, required 26.14 mb of 0.05831 M EDTA to reach the murexide end point. A second 50.00-mb aliquot was treated with hexamethylenetetramine to mask the Cr. Titrating with 0.05831 M EDTA required 35.43 mb to reach the murexide end point. Einally, a third 50.00-mb aliquot was treated with 50.00 mb of 0.05831 M EDTA, and back titrated to the murexide end point with 6.21 mb of 0.06316 M Cu +. Report the weight percents of Ni, fe, and Cr in the alloy. 

Chemical analysis of the metal can serve various purposes. For the determination of the metal-alloy composition, a variety of techniques has been used. In the past, wet-chemical analysis was often employed, but the significant size of the sample needed was a primary drawback. Nondestmctive, energy-dispersive x-ray fluorescence spectrometry is often used when no high precision is needed. However, this technique only allows a surface analysis, and significant surface phenomena such as preferential enrichments and depletions, which often occur in objects having a burial history, can cause serious errors. For more precise quantitative analyses samples have to be removed from below the surface to be analyzed by means of atomic absorption (82), spectrographic techniques (78,83), etc. 

A simple ealibration eurve based on distilled water is suitable for tungsten determination (linearity range is 1-50 mg/dm of W), no interferenee from Fe, Co, Cr, Ni was found. The aeeuraey of the method is eonfirmedby analysis of eertified referenee materials of high alloy steels and niekel based alloys (in range of 0.3 to 15 % W). The analyzed values are agreeing well with the eertified values. 

VERBA-XRF eoneeption effieieney shows itself in numeral methods analyzing ferrous alloys and powder-like materials like raw materials for eement industry, slag, eleetrolysis preeipitations in non-ferrous metallurgy. 

For water, organic and water-organic metal salts mixtures the dependence of integral and spectral intensities of coherent and non-coherent scattered radiation on the atomic number (Z), density, oscillator layer thickness, chemical composition, and the conditions of the registering of analytical signals (voltage and tube current, tube anode material, crystal-analyzer) was investigated. The dependence obtained was compared to that for the solid probes (metals, alloys, pressed powder probes). 

Of course, the most reliable and accurate method of quantitative analysis is to calibrate each element with standards prepared in matrices similar to the unknown being analyzed. For a survey technique that is used to examine such a wide variety of materials, however, standards are not available in many cases. When the technique is used mainly in one application (typing steels, specifying the purity of alloys for a selected group of elements, or identifying impurities in silicon boules and... 

Corrosion products formed as thin layers on metal surfaces in either aqueous or gaseous environments, and the nature and stability of passive and protective films on metals and alloys, have also been major areas of XPS application. XPS has been used in two ways, one in which materials corroded or passivated in the natural environment are analyzed, and another in which well-characterized, usually pure metal surfaces are studied after exposure to controlled conditions. 

Phase transitions in two-dimensional (adsorbed) layers have been reviewed. For the multicomponent Widom-Rowlinson model the minimum number of components was found that is necessary to stabilize the non-trivial crystal phase. The effect of elastic interaction on the structures of an alloy during the process of spinodal decomposition is analyzed and results in configurations similar to those found in experiments. Fluids and molecules adsorbed on substrate surfaces often have phase transitions at low temperatures where quantum effects have to be considered. Examples are layers of H2, D2, N2, and CO molecules on graphite substrates. We review the PIMC approach, to such phenomena, clarify certain experimentally observed anomahes in H2 and D2 layers and give predictions for the order of the N2 herringbone transition. Dynamical quantum phenomena in fluids are also analyzed via PIMC. Comparisons with the results of approximate analytical theories demonstrate the importance of the PIMC approach to phase transitions, where quantum effects play a role. 

In a previous work we showed that we could reproduce qualitativlely the LMTO-CPA results for the Fe-Co system within a simple spin polarized canonical band model. The structural properties of the Fe-Co alloy can thus be explained from the filling of the d-band. In that work we presented the results in canonical units and we could of course not do any quantitative comparisons. To proceed that work we have here done calculations based on the virtual crystal approximation (VGA). In this approximation each atom in the alloy has the same surrounding neighbours, it is thus not possible to distinguish between random and ordered alloys, but one may analyze the energy difference between different crystal structures. 

Similar alloys have been investigated theoretically more and more in the last years LiSi [9], CsPb [10], MgBi [11]. Such previous investigations on the conductivity of alloys were based on simulation data for only one composition. We analyze, for the first time, by means of computer simulation, the strong variation of the conductivity with concentration - ranging from metallic to semimetallic behaviour. 

Ia/Icu (/a = intensity of Ka for copper in the alloy Icu — corresponding intensity for pure copper) for alloys containing the following weight-fractions of copper 0.01 (0.0099) 0.04 (0.0373) 0.53 (0.504) 0.88 (0.867). This excellent agreement can be further improved by applying suitable corrections. There probably is no better way of analyzing metallic samples for which a point-to-point exploration on a minute scale is required. 

PUCI3, and MgCl2 to form a 50/50 mole % NaCl-CaCl salt phase and a molten Am-Pu-Mg-Ca alloy which is immiscible in the above salt(lO). After cooling, the metal phase is cleaved away from the salt phase and the salt phase is analyzed. Little, if any, Am or Pu remains in the salt phase and the salt residues can be discarded to waste. Metal recovery begins by evaporating magnesium and calcium from the residual metal button at about 800°C in vacuum. The americium can then be distilled away from the plutonium in a vacuum still operated at 1200°C, using yttria ceramic vessels to contain the molten metal fraction. The bottoms fraction contains the plutonium which is recycled back into the main plutonium stream. 

All but three of these samples were analyzed chemically and spectroscopically by the Smith-Emery Company of Los Angeles. The chemical analyses (Table 1) agreed with the synthetic compositions to within +0-3%. Duplicate 2 g. samples of each of sixteen of the alloys were analyzed and found to have the same composition, showing the alloys to be homogeneous. 

Salomon and Shirley [296] have performed Mossbauer-source experiments on Fe( Os) alloys with less than 0.1 at% osmium against a metallic Ir absorber. Their spectra were well-resolved magnetic eight-line patterns, which the authors could satisfactorily analyze using the Hamiltonian... 

With due regard to the lateral variations in composition which can arise as a consequence of source geometry and positioning (discussed in Section II), it is vise to analyze the alloy film at a number of representative points. For example, if a catalytic reaction was carried out over an alloy film deposited inside a spherical vessel maintained at a constant temperature over its entire area, then the mean alloy composition (and the uniformity of composition) is required. A convenient procedure is to cut glass reaction vessels carefully into pieces at the end of the experiment and to determine the composition by X-ray fluorescence analysis of a number of representative pieces. Compositions of Pd-Ag alloy films (40) determined at 12 representative parts of a spherical vessel from the intensities of the AgK 12 and PdKau fluorescent X-ray emissions are shown in Table V mean compositions are listed in the first column. (The Pd and Ag sources were separate short concentric spirals.) In other applications of evaporated alloy films to adsorption and catalytic studies, as good or better uniformity of composition was achieved. Analyses of five sections of a cylindrical... 

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