Niobium determination

PAM,. spectropliotoniciric dctcrniination of vanadium photometric dctenniiiation of niobium in the presence of trietlianolamine spectrophotomelric determination of bismuth in the presence of 1,3-diphenylguanidinc spectrophotometric determination of yttrium in the presence of Ttephiramine formation constants of mmplexes with Hoflll) measured... 

Spectroscopic methods for the deterrnination of impurities in niobium include the older arc and spark emission procedures (53) along with newer inductively coupled plasma source optical emission methods (54). Some work has been done using inductively coupled mass spectroscopy to determine impurities in niobium (55,56). X-ray fluorescence analysis, a widely used method for niobium analysis, is used for routine work by niobium concentrates producers (57,58). Paying careful attention to matrix effects, precision and accuracy of x-ray fluorescence analyses are at least equal to those of the gravimetric and ion-exchange methods. 

Oxide superconductors have been known since the 1960s. Compounds such as niobium oxide [12034-57-0] NbO, TiO, SrTi02, and AWO, where A is an alkah or alkaline earth cation, were found to be superconducting at 6 K or below. The highest T observed in oxides before 1986 was 13 Kin the perovskite compound BaPb Bi O, x = 0.27. Then in 1986 possible superconductivity at 35 K in the La—Ba—Cu—O compound was discovered (21). The compound composition was later determined to be La 85 A the Y—Ba—Cu—O system was pubUshed in 1987 and reported a transition... 

Loop Tests Loop test installations vary widely in size and complexity, but they may be divided into two major categories (c) thermal-convection loops and (b) forced-convection loops. In both types, the liquid medium flows through a continuous loop or harp mounted vertically, one leg being heated whilst the other is cooled to maintain a constant temperature across the system. In the former type, flow is induced by thermal convection, and the flow rate is dependent on the relative heights of the heated and cooled sections, on the temperature gradient and on the physical properties of the liquid. The principle of the thermal convective loop is illustrated in Fig. 19.26. This method was used by De Van and Sessions to study mass transfer of niobium-based alloys in flowing lithium, and by De Van and Jansen to determine the transport rates of nitrogen and carbon between vanadium alloys and stainless steels in liquid sodium. 

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. 

Niobium oxide obtained by plasma chemical decomposition is an ultra-fine powder with a specific surface area, as determined by the BET method, of about 20-30 m2/g. The estimated average particle size does not exceed 0.1 pm. 

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. 

Kolosov, Matychenko and Novichkov reported [566] on the investigation of the electrolysis of pure niobium from K2NbF7 dissolved in a LiF - NaF - KF eutectic melt (called a FLINAK melt). Conditions for obtaining highly uniform niobium coatings thicker than 5 pm were determined. 

Synthetic standards will serve when suitable analyzed standards are unavailable. For example, graduated amounts of Nb205 (niobium to be determined) can be added to each of a series of mixtures of Si02 and Fe203 that cover the expected range of sample absorbances. 

Figure 8-9 shows how the calibration for niobium varies with the background counting rate at a single Nb2Os concentration. Similar curves have been proved useful in a large number of uranium determinations on shipping pulp and ores. 

The discussion will be restricted to cases for which a complete structure-determination exists. Again, as with the niobium compounds, but even more pronouncedly, the occurrence of metal-metal bonds (340) (see Table XIV) is most significant. 

In contrast to chloride compounds, niobium oxides have a VEC of 14 electrons, due to an overall anti-bonding character of the a2u state, caused by a stronger Nb-O anti-bonding contribution. In some cases, the VEC cannot be determined unambiguously due to the uncertainty in the electron distribution between the clusters and additional niobium atoms present in the majority of the structures. The 14-electron compounds exhibit semiconducting properties and weak temperature-independent paramagnetism. Unlike niobium chlorides, the oxides do not exhibit a correlation between the electronic configuration and intra-cluster bond distances. 

Chong et al. [742] have described a multielement analysis of multicomponent metallic electrode deposits, based on scanning electron microscopy with energy dispersive X-ray fluorescence detection, followed by dissolution and ICP-MS detection. Application of the method is described for determination of trace elements in seawater, including the above elements. These elements are simultaneously electrodeposited onto a niobium-wire working electrode at -1.40 V relative to an Ag/AgCl reference electrode, and subjected to energy dispersive X-ray fluorescence spectroscopy analysis. Internal standardisation... 

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. 

Precipitation inhibitors, dispersants contrasted, 3 686 Precipitation leachate procedure, synthetic, 25 868-869 Precipitation reactions, for niobium and tantalum determination, 27 142-143 Precipitation reagents, protein, 22 133 Precipitation with compressed antisolvent (PCA) process, 24 17, 18 Precipitator dust, in phosphorus manufacture, 19 12 Precipitators, electrostatic, 23 180 Precision agriculture, 23 328 26 269-270 Precision measurement techniques, noble gases in, 27 370 Precision scales, 26 245 Preconcentration, of uranium ores, 25 401 Pre-crosslinked polychloroprene grades, 19 852... 

The use of both 8(CH3) values and iftM- H) magnitudes does, however, allow determination of the coordination mode in many instances (e.g., 462). Problems due to ligand dissociation are frequently evident in H-NMR studies of sulfoxide complexes. Thus the dimethyl sulfoxide adduct of niobium oxychloride (409) undergoes solvolysis in acetoni-... 

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