Analysis alloys

Point Of analysis Alloy Zone of welded joint Object of investigation Content of elements, wt.% ... 

Ura] Metallography, thermal analysis Alloys up to 68 mass% Fe hquidus surface of A1 comer... 

Nearly all experimental eoexistenee eurves, whether from liquid-gas equilibrium, liquid mixtures, order-disorder in alloys, or in ferromagnetie materials, are far from parabolie, and more nearly eubie, even far below the eritieal temperature. This was known for fluid systems, at least to some experimentalists, more than one hundred years ago. Versehaflfelt (1900), from a eareflil analysis of data (pressure-volume and densities) on isopentane, eoneluded that the best fit was with p = 0.34 and 8 = 4.26, far from the elassieal values. Van Laar apparently rejeeted this eonelusion, believing that, at least very elose to the eritieal temperature, the eoexistenee eurve must beeome parabolie. Even earlier, van der Waals, who had derived a elassieal theory of eapillarity with a surfaee-tension exponent of 3/2, found (1893)... 

The determination of silicon is commonly encountered in metallurgical and mining laboratories responsible for the analysis of ores, slags, and alloys. The volatilization gravimetric method, which is appropriate for samples containing high concentrations of silicon, was described earlier in Method 8.2. 

The amount of iron and manganese in an alloy can be determined by precipitating the metals with 8-hydroxyquinoline, C9H7NO. After weighing the mixed precipitate, the precipitate is dissolved and the amount of 8-hydroxyquinoline determined by another method. In a typical analysis, a 127.3-mg sample of an alloy containing iron, manganese, and other metals was dissolved in acid and... 

Method 8.2 describes a procedure for determining Si in ores and alloys. In this analysis a weight loss of 0.21 g corresponds to 0.1 g of Si. Show that this relationship is correct. 

The ability to control selectivity by carefully selecting the working electrode s potential, makes controlled-potential coulometry particularly useful for the analysis of alloys. For example, the composition of an alloy containing Ag, Bi, Cd, and Sb... 

Miscellaneous Samples Besides environmental and clinical samples, differential pulse polarography and stripping voltammetry have been used for the analysis of trace metals in other samples, including food, steels and other alloys, gasoline, gunpowder residues, and pharmaceuticals. Voltammetry is also an important tool for... 

The concentration of Ni in a new alloy is determined by a neutron activation analysis using the method of external standards. A 0.500-g sample of the alloy and a 1.000-g sample of a standard alloy known to contain 5.93% w/w Ni are irradiated with neutrons in a nuclear reactor. When irradiation is complete, the sample and standard are allowed to cool, and the gamma-ray activities are measured. Given that the activity is 1020 cpm for the sample and 3540 cpm for the standard, determine the %w/w Ni in the alloy. 

Polymer additives Polymer alloys Polymer analysis... 

Analytical Procedures. Standard methods for analysis of food-grade adipic acid are described ia the Food Chemicals Codex (see Refs, ia Table 8). Classical methods are used for assay (titration), trace metals (As, heavy metals as Pb), and total ash. Water is determined by Kad-Fisher titration of a methanol solution of the acid. Determination of color ia methanol solution (APHA, Hazen equivalent, max. 10), as well as iron and other metals, are also described elsewhere (175). Other analyses frequendy are required for resia-grade acid. For example, hydrolyzable nitrogen (NH, amides, nitriles, etc) is determined by distillation of ammonia from an alkaline solution. Reducible nitrogen (nitrates and nitroorganics) may then be determined by adding DeVarda s alloy and continuing the distillation. Hydrocarbon oil contaminants may be determined by ir analysis of halocarbon extracts of alkaline solutions of the acid. 

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. 

National Institute of Standards and Technology (NIST). The NIST is the source of many of the standards used in chemical and physical analyses in the United States and throughout the world. The standards prepared and distributed by the NIST are used to caUbrate measurement systems and to provide a central basis for uniformity and accuracy of measurement. At present, over 1200 Standard Reference Materials (SRMs) are available and are described by the NIST (15). Included are many steels, nonferrous alloys, high purity metals, primary standards for use in volumetric analysis, microchemical standards, clinical laboratory standards, biological material certified for trace elements, environmental standards, trace element standards, ion-activity standards (for pH and ion-selective electrodes), freezing and melting point standards, colorimetry standards, optical standards, radioactivity standards, particle-size standards, and density standards. Certificates are issued with the standard reference materials showing values for the parameters that have been determined. 

Bursting tests have been carried out on neatly a hundred thick-walled cylinders made of carbon, low alloy, and stainless steels, together with some nonferrous materials. The diameter ratio of the cylinders varied from 1.75 to 5.86, and some tests were carried out at 660°C. An analysis of the results (19) showed that 90% of the cylinders burst within 15% of the value given by equation 17. 

Two approaches have been taken to produce metal-matrix composites (qv) incorporation of fibers into a matrix by mechanical means and in situ preparation of a two-phase fibrous or lamellar material by controlled solidification or heat treatment. The principles of strengthening for alloys prepared by the former technique are well estabUshed (24), primarily because yielding and even fracture of these materials occurs while the reinforcing phase is elastically deformed. Under these conditions both strength and modulus increase linearly with volume fraction of reinforcement. However, the deformation of in situ, ie, eutectic, eutectoid, peritectic, or peritectoid, composites usually involves some plastic deformation of the reinforcing phase, and this presents many complexities in analysis and prediction of properties. 

Analysis. Indium can be detected to 0.01 ppm by spectroscopic analysis, using its characteristic lines in the indigo blue region, at wavelengths 4511.36, 4101.76, 3256.09, and 3093.36 nm. Procedures for the quantitative deterrnination of indium in ores, compounds, alloys, and for the analysis of impurities in indium metal are covered thoroughly in the Hterature (6). 

Referee Methods. The American Society for Testing Materials (ASTM) has collected a series of standard referee methods for the analysis of magnesium and its alloys (78). These methods are accurate over a larger range of concentration than the production methods, but are time consuming ia thek apphcation. The methods are based on potentiometric titration, photometric methods, or gravimetric methods. The photometric methods are most common and are relatively straightforward. 

Standard Test Methods For Chemical Analysis of Magnesium and Magnesium Alloys, ASTM E-35 to 88, American Society for Testing and Materials, Philadelphia, Pa., 1992. 

Qualitative Analysis. Nitric acid may be detected by the classical brown-ring test, the copper-turnings test, the reduction of nitrate to ammonia by active metal or alloy, or the nitrogen precipitation test. Nitrous acid or nitrites interfere with most of these tests, but such interference may be eliminated by acidifying with sulfuric acid, adding ammonium sulfate crystals, and evaporating to alow volume. 

The predorninant method for the analysis of alurninum-base alloys is spark source emission spectroscopy. SoHd metal samples are sparked direcdy, simultaneously eroding the metal surface, vaporizing the metal, and exciting the atomic vapor to emit light ia proportion to the amount of material present. Standard spark emission analytical techniques are described in ASTM ElOl, E607, E1251 and E716 (36). A wide variety of weU-characterized soHd reference materials are available from major aluminum producers for instmment caUbration. 

Chemical analysis methods maybe used for assay of silver alloys containing no interfering base metals. Nitric acid dissolution of the silver and precipitation as AgCl, or the Gay-Lussac-VoUiard titration methods are used iaterchangeably for the higher concentrations of silver. These procedures have been described (4). 

The variety of AES techniques requires careful evaluation for selecting the proper approach to an analytical problem. Table 4 only suggests the various characteristics. More detailed treatment of detection limits must include consideration of spectral interferences (191). AES is the primary technique for metals analysis in ferrous and other alloys geological, environmental, and biological samples water analysis and process streams (192). 

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