SU853419A1 - Mixture for spectral detection of impurities in tantalum and niobium - Google Patents

Description

The invention relates to the field of spectral analysis, in particular to the quantitative determination of impurity elements in tantalum or niobium of high purity. To determine most of the impurities (51, Mn, Md, Fe, Nb, Cr, Al, Sn, V, Mo, Zr, N1, Co, -Cs, Ti, Cu, Ag), a mixture of oxidized to pentoxide is known. tantalum sample (60-85%), carbon powder (weight. 15-40%) and sodium chloride (weight. 6-10%) CIT which is used to determine most of the impurities (S1, Mn, MD, Fe, Mb, Cr, Al, Sn, .V, Mo, Zn, Co, Ca, Ti, Cu, Ag). This mixture has a low sensitivity with respect to the determination of molybdenum in tantalum up to 1.10 and does not allow the determination of such impurities as tungsten, sodium, affecting the properties of, for example, tantalum powders. Closest to the invention is a mixture for the spectral determination of impurities in tantalum or niobium, containing a sample oxidized to the si of the metal being analyzed and a fermentation mixture based on chloride 2. Chloride silver is used as a chloride in the ratio of 3: 1 weight), and the buffer mixture contains 1 0.1-0.6 wt.% phosphorus in the form of ammonium phosphate. This mixture allows molybdenum and tungsten to be determined in the range of 1.10. - 1.10%. The difference in the blackness of the analytical lines and the background with a content of 0.001% of these impurities is W = 0.40; Mo 0, 50; Co - 0.90. The disadvantage of this mixture is the high cost and limited analysis. The aim of the invention is to increase the reproducibility, reduce the cost and empower the analysis. The goal is achieved by the fact that in a known mixture for the spectral determination of impurities in tantalum or niobium, containing a sample oxidized to pentoxide of an exchisable metichish and a buffer mixture based on chloride, the buffer mixture contains potassium sulphate, and as lead chloride is lead chloride; the ratio of the components in the mixture, wt.%:

tantalum pioxide (niobi) 75-84

lead chloride 9.8–18.8 potassium sulfate 4.2–6.3 Tantalum pentoxide, lead chloride, potassium sulfate with the following ratio of components were used to prepare the mixture.

Table 1

Table continuation

The resulting mixtures allowed us to obtain the following values of the difference between the blackening of the analytical lines and the background with a content of tungsten, molybdenum, copper, cobalt, calcium, and sodium in an amount of 0.001% kg1 each.

table 2

Claims (1)

Mixture No. 4, having a slightly higher value of L5 for wolfgsha, significantly increases the background of the spectrum. The range of detectable contents is: tungsten, molybdenum, cobalt, sodium 0.0001 - 0.1%; copper 0, 0001 - 0.01%; Calcium 0.000 - 0.03 The reliability of the results was checked on artificial samples of tanta la and niobium and compared with the determination of impurities by known methods. Artificial samples were prepared on the basis of purely defined samples for months of tantalum pentoxide and niobium pentoxide by carefully rubbing them with the calculated amount of oxides of purified elements. From a comparison of data on the analysis of high-frequency tantalum obtained by known methods and the proposed mixture, it follows that the magnitude of the resulting discrepancy is less than the maximum permissible error, which indicates the reliability of the results of the proposed mixture. Thus, the use of the proposed mixture consisting of oxidized The second up to tantalum pentoxide or niobium sample in the amount of 75-84%, lead chloride, 9.8-18.8% potassium sulfide 4.2 - 6.3% allows you to simultaneously determine tungsten, molybdenum, copper, cobalt, calcium , n Trier in a broad range from 0.1 to 1.10%. According to a known method, the determination of the indicated elements in such an interval of values is carried out on three mixtures. At the same time, the use of lead chloride and potassium sulphide allows one to remove the mixture and analysis by eliminating costly silver chloride, to increase the reproducibility of the results by better rubbing the mixture and eliminating the decomposition of silver chloride. Claims of the invention A mixture for spectral determination of impurities in tantalum or niobium, containing a sample oxidized to the pentoxide of the analyzed metal, a buffer mixture of y-based chloride, characterized in that, in order to increase the reproducibility and jgacmH of anashiz capabilities, buffer; the mixture contains potassium sulfate, and chlorine is used as the chloride; whisty lead, with the next amount — Sources of Information, the ratio of the components taken into account in the examination mixture, weight%: 1. USSR author's certificate tantalum pentoxide 524083, cl. G 01 J 3/40, 1973. Niobium 75-842. USSR author's certificate lead chloride 9.8-18.8, 515950, cl. G 01 J 3/40, 1973. potassium sulfate 4.2-6.3 (prototype).