SU1270690A1 - Mixture for spectrum determining impurities in tantalum - Google Patents

Abstract

The invention relates to a mixture for the spectral determination of impurities in tantalum, can be used in various fields of industry and allows for improved analysis accuracy. A sample oxidized to tantalum oxide (mass fraction 80.8%) is mixed in a mass ratio of 5: 1 with a buffer mixture consisting of lead chloride (mass fraction 9.6–9.8%), potassium sulfate (mass fraction 6 , 5%) and monosodium phosphate (mass fraction 2.0-4.0%). The sample tablet is placed in the crater of the bilge glass electrode and burned in a 12 A direct current arc. Spectra are recorded either with a quantomer or onto a photographic film using a diffraction spectrograph. 2 tab.

Description

This invention relates to analytical chemistry, and specifically to methods; spectral determination of impurities in tantalum and its compounds, and can be used for analytical control in various areas of the national economy,

The purpose of the invention is to increase the accuracy of the analysis.

Example. The mixture was tested on samples of tantalum oxide obtained by 1 and 2 methods. The assessment of the accuracy of the determination was carried out by the method introduced-found.

The results of the analysis are presented in table. one.

Table 1

For analysis, a sample oxidized to tantalum oxide (mass fraction 80.8%) is mixed in a mass ratio of 5: 1 with a buffer mixture consisting of lead chloride (mass fraction 9.7%), potassium sulfate (mass fraction 6.5% ) and monosubstituted ammonium phosphate (mass fraction 3%). Using a measuring device, a tablet prepared in this way with a 0.25 cm sample is placed in the crater of the gumming electrode and burned in a 12 A DC arc (exposure time 20 s). Spectra are recorded either by

 a quantometer (for example, DFS-36), or onto a photographic plate using a diffraction spectrograph (for example, DFS-13).

Standard deviation Sj. coincides with the standard deviation of the methodology TU 95.203-82 and is 0.17 for wolfrate, molybdenum, copper, calcium, cobalt and 0.20 for sodium.

The mechanism of action of monophosphate phosphate in the proposed solution is reduced to the leveling of the pace.

31270690-4

The temperature rise of the different probing effect is explained by the presence of an electrode in the crater in history that the structure of the ammonium ion reagents leads to a convergence of the flow conditions. In this case, a positive 5-lytic signal is shown in Table 2.

Claims (1)

The minimum amount of monosubstituted ammonium phosphate in the analyzed mixture corresponds to a value of 2%, at which the coincidence of analytical signals is observed, and the upper limit is 4%, where an increase in the amount of reagent leads to a decrease in the detection sensitivity. Invention Formula A mixture for the spectral determination of impurities in tantalum, containing table 2 a sample is oxidized to tantalum oxide, and a buffer mixture of lead chloride and potassium sulfate, characterized in that, in order to improve the ACCURACY of the analysis, monosodium ammonium phosphate is introduced into it in the following ratio of components,% by mass Lead chloride 9, 6-9.8 Potassium sulfate 6.5-6.6 Ammonium phosphate 2.0-4.0 Tantalum oxide Else.