SU1059475A1 - Method of probe preparation for determination of impurity elements in zirconium by spectral technique - Google Patents

Abstract

A METHOD FOR PREPARING SAMPLES FOR DETERMINING IMPURITY ELEMENTS IN CIRCONY BY SPECTRAL METHOD, including mixing an oxidized sample with a halogen-impregnating additive, characterized in that, in order to increase the sensitivity and accuracy of the analysis, as a halogen-containing additive, you can use the same applications, the same application patterns, the same applications, the use of the application, the halogen content and the halogen-containing additive, in order to increase the sensitivity and accuracy of the analysis. May %: Bismuth fluoride 7-9 Sodium chloride 7-9. The oxidized sample Else

Description

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The invention relates to an analytical chemist, namely to methods of spectral analysis, and can be used to determine impurity elements in zirconium and its compounds.

A known method for determining impurities in zirconium by the method of fractional evaporation with a carrier in a direct current arc. The method is based on the determination of impurities in fractional evaporation with a carrier in a direct current arc. Fractional evaporation of impurities is carried out from a pre-oxidized sample, to which 10% barium carbonate (carrier) and 0.05% cobalt oxide (internal standard) are added. The method is designed to determine A1, Ni, Ti, Cu, Na, Mo, Gr, Mg, Sn, PB With sensitivity, a Li, Be, Mn with 1-3 1.

The disadvantage of this method is the low sensitivity of the determination of impurities A1, Ca, Sn, Cr.

The closest to the proposed technical essence and the achieved effect is the method of sample preparation for the spectral analysis of impurities in zirconium. According to this method, a halogen-containing additive of silver chloride in a ratio of 4: 1 by mass of ZrOjAgCls is introduced into zirconium oxide. The sensitivity of the determination of A1, PB, B, Fe, gd, Caj Si, Mg, Mn, Mo ,, Ti, Cr finds-SY at the level n-lO-- n-10-% 2J. ,

The disadvantage of this method is low sensitivity with respect to A1, PB, B, Fe, Si, Mo, Ni, Sn, Ti and Cr, as well as the use of silver chloride as a halogen-containing additive, which undergoes light decomposition under the action of light. its chlorinating ability changes in an uncontrolled manner, which leads to an increase in random and systematic errors. The relative standard deviation of a single determination (Br) is 0.20-0.3.

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

The goal is achieved by the fact that according to the method involving mixing the oxidized sample with a halogen-containing additive, a mixture of bismuth fluoride and sodium chloride is used as the halogen-containing additive at the following ratio of components, wt.%:

Bismuth fluoride 7-9

Sodium chloride 7-9

The oxidized sample Else

The sum of the method is that with the introduction of the additive fluoride.

bismuth and sodium chloride to pro

the stability of the conditions increases. fractional evaporation of impurities and excitation of atomic spectra of certain impurity elements, decreases the spectral background and increases

intensity of the spectral lines of impurity elements.

Using single bismuth fluoride or sodium chloride, as well as their

0 mixture at the ratios of components below and above mentioned, the sensitivity of the determination of such elements in impurities decreases by a factor of almost 3 to 10 — such as A: L, Cd, Ti, Ca, etc.

5 Example. Analysis of zirconium alloy containing 1% niobium.

The oxidized alloy sample is mixed with a halogen-containing additive in the ratio of 5: 1.

For 1 g of the oxidized alloy, 20 mg of the mixture is taken, which contains 100 mg of BiFj and 100 mg of NaCl. Then, 20 mg of the prepared sample is placed and compacted into carbon glasses such as a glass with the dimensions: outer

 diameter and height of the cup b and 4 mm di-, ammeter and depth of the channel 3.5 and 3.0 mm and diameter and height of the neck 3.5 and 3.5 mm respectively Further, the spectra of the reference and alloy samples are excited in an alternating current arc at a current of 20 A and recorded on a DFS-13 spectrograph. Exposure is 30s. Comparison samples, used for plotting calibration graphs, are prepared on the basis of zirconium oxide with the addition of an alloying component in an amount equal to its average content in the alloy being alloyed. The additives of the doping components are introduced in the form of the corresponding oxides.

Spectral lines 5 (in nM) are used as analytical lines: AI 394.4, Be 234.8, B 249.7, Fe 259.8, Cd 228.8, Ca 430.2, Si 251.6, Mg 280 , 2, Mn 257.6, Cu 324.7, Mo 317.0, Ni 300.2, NB 309.4, Sn 317.5 PB 280.2, Ti 336.1 Cr 425.4 W 283.1,

The results of the analysis of the alloy. The content of impurities wt.% Ge.,

. VtC "F V AV f

Cr 2.4.10- ,, Ni: i, 510V A1 3.10L

W.cl.iO- The relative standard deviation of the ex-LINE definition (Sr) is 0.15 0, 20.

0 The results of determination of the impurity content, which are elemental in zirconium and zirconium alloys, are presented in the table.

The content of halogen-containing additives in a mixture of bismuth fluoride and sodium chloride is 8.0 wt.% Each.

The content of the remaining impurities turned out to be less than the lower limit of the range of detectable SmAc contents. dale % Y, for Sn 3-1 (G, for Be, Mg 1-10-, for ca, for Ca,

Mo, PB, Ti 1-104 dl in s-10J, and

for W 1-10. Relative average

the standard deviation of a single determination (Sr) is 0.15 0, 20.

I.

: Thus, the proposed method allows an increase in the sensitivity and accuracy of determining

.A1, PB, B, Fe, Si, Mo, Hi, Sn, Ti, Cr In zirconium and its compounds.

Claims (1)

METHOD FOR PREPARING A SAMPLE FOR DETERMINING IMPURITY ELEMENTS I IN ZIRCONIA BY A SPECTRAL METHOD, comprising mixing an oxidized sample with a halogen-containing additive, characterized in that,. in order to increase the sensitivity and accuracy of the analysis, a mixture of bismuth fluoride and sodium chloride is used as a halogen-containing additive in the following components, May. %: Bismuth fluoride Sodium chloride. Oxidized Sample Ratio 7-9 7-9 Rest