Tantalum determination

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The molybdenum, tungsten and tantalum concentration influence on LCD nickel-ferrous HRS resistance, used for gas turbine installations parts is investigated. The tests were carried out on modeling compositions. Samples were molded on the basis of an alloy of the ZMI-3C. The concentration of tantalum varied from 0 up to 5% with a step of 0,5%. The contents of elements were determined by a spectral method. 

In order to carry out depth profiling with AES, the sputtering rate must be determined. The sputtering rate is usually measured by determining the time required to sputter through a layer of known thickness. Anodized tantalum foils are convenient for this purpose since the oxide thickness can easily be controlled and since the interface between the metal and the oxide is relatively sharp [43]. 

Two kinds of tantalum-containing initial solutions were chosen according to their ionic complex structure. The first one contained mostly TaF6 ions (Ta F = 1 18) while the second was characterized predominantly by TaF72 ions (Ta F = 1 6.5). The ionic composition of the solutions was determined by Raman spectroscopy. 

The structure of LiTa02F2, as reported by Vlasse et al. [218], is similar to a ReC>3 type structure and consists of triple layers of octahedrons linked together through their vertexes. The layers are perpendicular to the c axis, and each layer is shifted, relative to the layer below, by half a cell in the direction (110). Lithium atoms are situated in the centers of the tetragonal pyramids (coordination number = 5). The other lithium atoms are statistically distributed along with tantalum atoms (coordination number = 6) at a ratio of 1 3. The sequence of the metal atoms in alternating layers is (Ta-Li) - Ta - (Ta-Li). Positions of oxygen and fluorine atoms were not determined. The main interatomic distances are (in A) Ta-(0, F) - 1.845-2.114 Li-(0, F) - 2.087-2.048 (O, F)-(0,F) - 2.717-2.844. 

The tantalum strip solution was used for the preparation, by precipitation and thermal treatment, of tantalum oxide. The product was determined to be of high purity grade. Table 62 presents typical analysis results. 

Optimal parameters for the extraction, washing and stripping of niobium were determined to be number of stages for all three processes - 4, volumetric ratios Vorg Vaqu are 1 1, 20 1 and 8 1, respectively. Additional fine purification of the extractant was recommended by stripping of tantalum and niobium remainders using a 0.5% wt. ammonia solution. This additional stripping leads to final concentrations of both tantalum and niobium in the extractant that are < 0.001 g/1. Table 62 shows the purity of niobium oxide prepared by the described method. 

Another application of the electrolysis of tantalum and niobium in fluoride melts is in the preparation of intermetalic compounds as a result of the interaction between the electrochemically precipitating metal and the cathode material. Based on an investigation of the electrochemical reduction of K2TaF7 or K2NbF7 in a LiF - NaF melt on nickel cathodes, Taxil and Qiao [565] determined the appropriate conditions for the formation of TaNi3 or NbNi3 in the form of stable phases in the bulk of the obtained layer. 

Amongst other devices used to produce the required atoms in the vapour state are the Delves cup which enables the determination of lead in blood samples the sample is placed in a small nickel cup which is inserted directly into an acetylene-air flame. The tantalum boat is a similar device to the Delves cup in this case the sample is placed into a small tantalum dish which is then inserted into an acetylene-air flame. The use of these devices, especially for small sample volumes, has now been largely superseded by the graphite furnace. 

McIntyre, N. S., Cook M. G., and Boase, D. G. "Flameless Atomic Absorption Determination of Cobalt, Nickel, and Copper - A Comparison of Tantalum and Molybdenum Evaporation Surfaces". Anal. Chem. (1974), 46, 1983-1987. 

TLC atomic emission spectrometric (AES) method was developed to determine tantalum in molybdenum alloys containing > 0.5% tantalum. The procedure involves the separation of tantalum from molybdenum alloy on a silica gel layer (0.3 mm thick) using 10.0-MHCl -f acetone (1 1) as developer and the subsequent determination of tantalum by AES [43]. 

Nuclear resonance absorption for the 136 keV transition has been established by Steiner et al. [174]. The authors used a metal source and an absorber of metallic tantalum to determine the mean lifetime of the 136 keV level from the experimental line width ( 52.5 mm s for zero effective absorber thickness) and found a value of 55 ps. This has been the only report so far on the use of the 136 keV excited state of Ta for Mossbauer experiments. 

Halliday et al. [396] have described a simple rapid graphite furnace method for the determination of lead in amounts down to 1 xg/l in polluted seawater. The filtered seawater is diluted with an equal volume of deionised water, ammonium nitrate added as a matrix modifier, and aliquots of the solution injected into a tantalum-coated graphite tube in an HGA-2200 furnace atomiser. The method eliminates the interference normally attributable to the ions commonly present in seawater. The results obtained on samples from the Firth of Forth (Scotland, UK) were in good agreement with values determined by anodic stripping voltammetry. 

Thallium has been determined in 10 ml of ashed serum or in urine by extracting with sodium diethyldithiocarbamate into MIBK n°). More recently, Savory and co-workers 1131 described a wet digestion procedure for 50 ml of urine or 5 ml of serum in which the thallium is separated by extracting the bromide into ether, evaporating the ether and then taking up in dilute acid for aspiration. As little as 0.1 ppm is determined in urine. Curry et al.114) determined less than 1 ng of thallium in 200 /d of urine by using the tantalum sample boat technique. The sample in the boat is dried by holding the boat 1 cm from the flame and then it is inserted into the flame where it is vaporized. A similar procedure is used for >3 ng of thallium in 50-100/al of blood, except that the blood is preashed with 3 drops of nitric acid. Since the tantalum boat method is susceptible to interelement interferences, the method of standard additions is used for calibration. 

A chloric acid digestion was used by Backer 2 391 for the preparation of tissue samples. The digest is simply diluted to determine iron, zinc, and copper. The tantalum sampling boat technique was used by Emmermann and Luecke 2531 to measure lead, zinc, and silver in prepared soil solutions. White 1S81 treated ashed plants with hydroxylamine in IN hydrochloric acid to reduce and dissolve oxides of manganese, prior to its determination by atomic absorption spectroscopy. 

Niobium minerals, especially columbite, are also associated with other valuable minerals, such as tantalum, zircon and rare earth minerals. Pyrochlore and a mixture of pyrochlore and columbite have different origins, and therefore, beneficiation of pyrochlore and columbite are different from that of the mixed tantalum niobium ores. In actual plant practice, the treatment process is significantly different from that used for mixed niobium tantalum ores. This is due to the fact that the beneficiation process is largely determined by the nature of gangue minerals present in the ore. In most cases, the beneficiation process applicable for pyrochlore ore cannot be successfully applied for beneficiation of tantalum/ niobium ores. 

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