Determination of niobium in zirconium-niobium alloys

A rapid control determination of niobium in 50% zirconium/50% niobium master-alloy is described; it is a direct spectrophotometric procedure, based on the reaction of niobium ions with hydrogen peroxide in concentrated sulphuric acid. The procedure is suitable for the examination of zirconium alloys containing niobium in the range 0.1 to about 60%. At least 1% of chromium, cobalt, copper, manganese, nickel or tantalum, does not interfere. Interference due to optical absorption by the peroxy-complexes of titanium, tungsten, molybdenum and vanadium is not significant in the determination of niobium above about 1%, provided that these metals are not in excess of about 0.5%, 0.25%, 0.1% and 0.02%, respectively. To compensate for optical absorption due to iron(III), a solution of the sample, not treated with peroxide, is used.     

Analysis of alloys of titanium,niobium and tantalum by ion exchange

A procedure for the analysis of alloys of titanium, niobium and tantalum is described. After dissolution the metals are separated by ion exchange in hydrochloric-hydrofluoric acid media. Finally the metals are determined spectrophotometrically,     

Colorimetric determination of niobium in titanium alloys

There is need for a method for the determination of niobium in titanium alloys, since niobium-titanium alloys are becoming increasingly important. The determination of niobium in this type of alloy is an extremely difficult matter. Many approaches were tried before the problem was solved. In the method proposed in this paper the sample is dissolved in a mixture of hydrofluoric and nitric acids, the solution evaporated to a small volume, and boric acid added. Two tannic acid separations are then made to separate the niobium from the bulk of the titanium. The niobium, is determined colorimetrically by the thiocyanate method using a water-acetone medium. A study was made of the possible interference of elements that might be present in titanium alloys. It was found that the presence of tantalum causes two opposing tendencies. Tantalum can cause high results for niobium because it forms a complex with thiocyanate which is visually colorless but shows some absorption. Tantalum can cause low results for niobium by hindering the development of the niobium color. The resultant effect of the tantalum depends upon the amount of tantalum present, the amount of niobium present and the ratio of tantalum to niobium. The presence of more than one per cent. tungsten can lead to high results for niobium. Other elements that might be present in titanium alloys do not interfere with the method. The procedure is designed for titanium alloys containing 0.05 to 10 per cent. niobium. The method is reasonably rapid. Six determinations can be finished in two days. The method should be applicable to many other materials besides titanium alloys.     

Determination of niobium and tantalum in binary alloys and zirconium alloys

Recent developments in the metallurgy of niobium, tantalum and zirconium have necessitated provision of analytical procedures for determining niobium and tantalum in the presence of each other and in the presence of zirconium. For this purpose, absorptioinetric procedures based on the formation of yellow coloured complexes, between pyrogallol and niobium or tantalum, have been critically examined. Direct absorptiometric procedures are described, which are suitable for determining niobium or tantalum in the range 2 to 7%; when either of these metals exceeds 7%, differential absorptiometric procedures are recommended. Corrections must lie made for absorption due to the presence of other metals which form complexes with pyrogallol. In tlie determination of niobium or tantalum up to 5%, the precision of the method is about ±0.05%. About 12 determinations can be made in a day, by one analyst.     

X-ray fluorescence determination of niobium in iron-niobium alloys

Summary An X-ray fluorescence method is described for the determination of niobium in iron-niobium alloy in the concentration range from 0.1–2% of niobium. The sample is dissolved in a mixture of nitric and hydrofluoric acid and is converted to a stable oxide. This oxide is uniformly ground with boric acid and a weighed quantity of it is pressed into a circular pellet. The pellet is exposed to an X-ray beam from a tungsten target. The resulting fluorescent X-ray beam is dispersed using an LiF crystal and the intensity of the NbK -line is measured by a scintillation counter. A set of synthetic standards covering the above range is prepared using highpurity chemicals and a working curve for the estimation of niobium is established. The accuracy of the method is checked by analysing synthetic samples. The standard deviation of the method ranged from 0.5% at 5% Nb to 3.5% at 0.1% of Nb concentration.

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Röntgenfluorescenzspektroskopische Niobbestimmung in Eisen-Niob-Legierungen

Zusammenfassung Die Methode erlaubt eine Niobbestimmung im Konzentrationsbereich von 0,1–2% Niob. Die Probe wird in Salpetersäure/Flußsäure gelöst und in ein stabiles Oxid überführt, das mit Borsäure vermahlen und zu einer Tabelette gepreßt wird. Zur Röntgenfluorescenzmessung (W-Röhre, LiF-Kristall) wird die NbK -Linie herangezogen (Szintillationszähler). Mit Hilfe hochreiner Reagentien wurden synthetische Standards für den genannten Konzentrationsbereich hergestellt. Die Genauigkeit wurde mit Hilfe synthetischer Proben überprüft (Standardabweichung 0,5 % bei 5% Nb, 3,5% bei 0,1% Nb).

     

Determination of niobium in rocks, ores and alloys by atomic-absorption spectrophotometry

Niobium, in concentrations as low as 0.02% Nb(2)O(5), is determined in a variety of materials without separation or enrichment. Chemical and ionization interferences are controlled, and sensitivity is increased, by maintaining the iron, aluminium, hydrofluoric acid and potassium content within certain broad concentration limits. There is close agreement with the results of analyses by emission spectrographic, electron microprobe and X-ray fluorescence methods.     

The determination of zirconium in its binary alloys with niobium and tantalum

A procedure is presented for the determination of zirconium in the presence of niobium or tantalum. The bulk of the niobium or tantalum is first removed by extracting with hexone from a 10M hyclrofluoric acid, 6M sulphuric acid solution of the sample. The zirconium is then. separated from any unextractcd earth, acid element by precipitation with ammonium hydroxide followed by the addition of hydrogen peroxide. Under these conditions, both the niobium and tantalum form soluble peroxy complexes whereas the zirconium is completely precipitated from solution. After the separation of the precipitate by filtration, it is re-dissolved in hydrochloric acid and the zirconium concentration is finally determined by titration with ethylenediaminetetraacetic acid.     

Simultaneous determination of trace niobium, tantalum and tungsten in ferrous and non-ferrous alloys

A method is presented for the determination of niobium, tantalum and tungsten in steel and non-ferrous alloys, based on hydrolysis with sulphurous acid followed by X-ray fluorescence measurements. The limit of determination is about 0.002% and the standard deviation is 0.002 at the 0.05% level. Results below 0.01% by this method are only semiquantitative.     

Comparison of an instrumental and modified Kjeldahl technique for determination of nitrogen in niobium and tantalum alloys

Results obtained for the determination of nitrogen in two tantalum alloys and six niobium alloys by modified Kjeldahl and Leco TC-30 nitrogen—oxygen determinator are compared. In the 5–25 ppm range, for tantalum alloys, the relative standard deviation was 3–9% by the Kjeldahl procedure and 9–11% by the instrumental technique. In the range 30–80 ppm, for niobium alloys, the relative standard deviation was 2–8% by the Kjeldahl procedure and 5–7% by the instrumental technique.     

Analysis of uranium-zinc alloys

Zinc can be determined in zinc-uranium alloys by titration with Versene (ethylcnediaminetetra-acetic acid), using Murexide as the indicator. Carbonate is added before the titration to mask the uranium.     

Determination of niobium and tantalum in some ores and special alloys by inductively coupled plasma atomic emission spectrometry

A fast analytical method for the determination of niobium and tantalum in ores and special alloys by inductively coupled plasma atomic emission spectrometry has been developed. Optimum conditions for the determination of both metals in the plasma were worked out and possible interferences were studied before attempting the determination in the real samples. Ores are dissolved in a mixture of HCl, HF and H₃PO₄ acids while for the special alloy a HCl+H₂O₂ mixture is used. The resulting solutions are diluted to the mark with tartaric acid before their final direct nebulization into the plasma. Other elements present did not interfere in the determination of Nb or Ta at concentration levels similar to those found in the analyzed samples. The results obtained determining niobium and tantalum in pyrochlore and special alloys by the proposed procedure are in good agreement with the certified values.     

Peroxide compounds of niobium

Summary 1. A study of the reaction of sodium and potassium metaniobates with hydrogen peroxide at 0° showed that for low H₂O₂ concentrations (3–6%) peroxide compounds of niobium are formed Na(K)NbO₄· nH₂O (n=1.5–3.5). With high H₂O₂ concentrations (10–54%) the compounds formed are not those described in the literature but more soluble peroxide compounds of the perhydrate type Na(K)NbO₄-nH₂O₂· mH₂O (n=1.3–1.5; m =1.5-3), rather unstable at 0°.At –10° the perhydrates of permetaniobates form in a more stable form and with a higher content of active oxygen (11–12.3%); they were separated and studied in the solid state.     

Analysis of vanadium-titanium ores and alloys

A new spectrophotometric method for determining titanium in vanadium-titanium ore with 2,2'-biquinoxalyl was developed. The analytical procedure to dissolve samples and separate titanium from vanadium and tin was elaborated as well. Furthermore, vanadium and iron were determined in the ore investigated.     

Compton scattering study on the electronic properties of niobium carbide and niobium nitride

The electronic structure, experimental Compton profile and the chemical bonding mechanism of niobium carbide and niobium nitride are studied on the basis of the band structure calculations, using a self-consistent, all-electron, linear combination of Gaussian orbitals (LCGO) calculation based on density functional theory. Isotropic Compton profiles of niobium carbide have been measured, using a conventional technique based on 59.54 keV gamma-radiation with a solid state detector. The agreement between the experimental and the theoretical momentum density is very good. It is shown that the anisotropies at low momentum are heavily influenced by the particular shape of the Fermi surface. The charge distributions resulting from valence bands in different regions of the unit cell are discussed. The limitations of the rigid band structure model are illustrated and general trends in the chemical bonding are discussed.     

Crystallization of niobium germanosilicate glasses

Niobium germanosilicate glasses are potential candidates for the fabrication of transparent glass ceramics with interesting non-linear optical properties. A series of glasses in the (Ge,Si)O₂-Nb₂O₅-K₂O system were prepared by melting and casting and their characteristic temperatures were determined by differential thermal analysis. Progressive replacement of GeO₂ by SiO₂ improved the thermal stability of the glasses. Depending on the composition and the crystallization heat-treatment, different nanocrystalline phases—KNbSi₂O₇, K₃Nb₃Si₂O₁₃ and K_3.8Nb₅Ge₃O_20.4 could be obtained. The identification and characterization of these phases were performed by X-ray diffraction and Raman spectroscopy.The 40 GeO₂-10 SiO₂-25 Nb₂O₅-25 K₂O (mol%) composition presented the higher ability for volume crystallization and its nucleation temperature was determined by the Marotta's method. An activation energy for crystal growth of ∼529 kJ/mol and a nucleation rate of 9.7×10¹⁸ m⁻³ s⁻¹ was obtained, for this composition. Transparent glass ceramics with a crystalline volume fraction of ∼57% were obtained after a 2 h heat-treatment at the nucleation temperature, with crystallite sizes of ∼20 nm as determined by transmission electron microscopy.     

Analytical applications of niobium arsenate

Summary A reproducible and chemically stable inorganic ion-exchanger, niobium arsenate has been prepared by mixing acidic solutions of niobium sulphate and sodium aresenate in the ratio 1∶4 under different conditions. Its exchange behaviour after heat treatment has been studied. The analytical utility of this material is illustrated by its ability to separate quantitatively Ni(II) from V(V) and Fe(III). Mn(II) from V(V) and Fe(III).