GOST 26473.13-85

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  ГОСТ 26473.13-85

GOST 26473.13−85 Alloys and alloys based on vanadium. Method of spectral analysis (with Change No. 1)

GOST 26473.13−85

Group B59

STATE STANDARD OF THE USSR

ALLOYS AND MASTER ALLOYS BASED ON VANADIUM

Method of spectral analysis

Vanadium base alloys and alloying elements. Method of spectral analysis

AXTU 1709

Valid from 01.07.86
to 01.07.91*
_______________________________
* Expiration removed
by the decree of Gosstandart of the USSR from 14.05.91 N 680
(IUS N 8, 1991). — Note the manufacturer’s database.

DEVELOPED by the Ministry of nonferrous metallurgy of the USSR

PERFORMERS

Yu. A. Karpov, E. G. Nembrini, V. G., Miscreants, V. V. Nedler, V. M. Mikhailov, L. G. Agapova, G. N. Andrianov, A. V. Antonov, V. D. Dozen, M. A. Desyatkova, T. I. Kirillova, L. I. Kirsanov, I. E. Korepin, V. A. Orlova, N. Rasnitsyn, N. Suvorova, N. L. Tomasev, M. W. Schmidt, L. N. Filimonov

INTRODUCED by the Ministry of nonferrous metallurgy of the USSR

Member Of The Board Of A. P. Snurnikov

APPROVED AND put INTO EFFECT by Decision of the USSR State Committee on standards of 25 March 1985 N 752

The Change N 1, approved and put into effect by the Decree of the USSR State Committee on management of quality and standards from 14.05.91 N 678 from 01.01.92

Change No. 1 made by the manufacturer of the database in the text IUS N 2, 1990


This standard applies to alloys and alloys based on vanadium, and sets the spectral method (inductively coupled plasma as the excitation source spectrum) of the definition of components given in table.1.

Table 1

The method is based on the intensity of analytical lines of the designated element from its concentration in the solution sprayed in an argon inductively bound plasma.

(Changed edition, Rev. N 1).

1. GENERAL REQUIREMENTS

1.1. General requirements for methods of analysis GOST 26473.0−85.

2. APPARATUS, REAGENTS AND SOLUTIONS

Spectral-analytical complex, consisting of a high frequency generator (27, 12 MHz) plasma torch spray system, polychromator and monochromator with inverse linear dispersion is not worse than 0.5 nm/mm with photoelectric registration of radiation intensity, controlling computer.

Argon according to GOST 10157−79.

Analytical scale.

Libra technical.

Tile electric.

Glasses chemical glass with a capacity of 100 cm.

Volumetric flasks with a capacity of 50, 100, 500 cm.

Pipettes with a capacity of 5, 10, 20 and 25 cmwith no divisions.

Pipettes with a capacity of 5, 10 cmwith divisions.

Measuring beakers with a capacity of 25 and 50 cm.

Cup platinum with a capacity of 30 cm.

Cup of glass-carbon with a capacity of 30 cm.

Sulfuric acid GOST 4204−77, diluted 1:1.

Nitric acid GOST 4461−77 diluted 1:1.

Hydrochloric acid by the GOST 3118−77, diluted 1:1.

Hydrofluoric acid according to GOST 10484−78.

Hydrogen peroxide according to GOST 10929−76.

Aluminium metal according to GOST 11069−74*, grade A-99.
______________
* On the territory of the Russian Federation GOST 11069−2001. — Note the manufacturer’s database.

Vanadium metal, with a mass fraction of vanadium is not less than 99.9%, in the form of small chips.

Tungsten metal in the form of powder or fine chips containing not less than 99.9% tungsten.

The iron is recovered in powder form, containing not less than 99,9% of iron.

Manganese metal according to GOST 6008−82*, mark Mr-00.
______________
* On the territory of the Russian Federation GOST 6008−90. — Note the manufacturer’s database.

Molybdenum metal powder or fine shavings, containing at least 99.9% molybdenum.

Niobium metal in the form of powder or fine chips containing not less than 99.9% niobium.

The titanium metal in the form of a small chip containing not less than 99.9% titanium.

Chrome metal according to GOST 5905−79*.
______________
* On the territory of the Russian Federation GOST 5905−2004. — Note the manufacturer’s database.

The zirconium metal in the form of chips containing not less than 99.9% zirconium.

(Changed edition, Rev. N 1).

2.1. Preparation of standard solutions

A standard solution of aluminium (spare) containing 1 mg/cmof aluminium

0.1 g of aluminum metal is placed in a beaker with a capacity of 100 cm, poured 5cmof hydrochloric acid diluted 1:1, cover with a watch glass and dissolve with a moderate heat. Upon dissolution of the sample flow 10 cmof sulphuric acid diluted 1:1, heating was continued to release sulfuric acid vapors, cooled, poured 50 cmof water, heated to dissolve the salts, and transfer the resulting solution into a measuring flask with a capacity of 100 cmand adjusted to the mark with water.

Solution of aluminum (work) containing 0.1 mg/cmof aluminium. In a volumetric flask with a capacity of 100 cmpipetted 10cmbackup solution, adjusted to the mark with water.

A standard solution of vanadium containing 1 mg/cmvanadium

0.1 g of vanadium metal placed in a beaker with a capacity of 100 cmand dissolved by heating at 350−400 °C in a mixture of 5 cmof nitric acid, diluted 1:1, and 10 cmof sulphuric acid diluted 1:1. Upon dissolution of the sample heating was continued until the vapors escaping sulfuric acid, cooled, poured 50 cmof water, heated to dissolve the salts, transfer the resulting solution into a measuring flask with a capacity of 100 cmand adjusted to the mark with water.

Standard solution tungsten (spare) containing 1 mg/cmtungsten

0.1 g of metal tungsten is placed in a glass-carbon Cup, pour 2 cmhydrofluoric acid, drop by drop nitric acid and gently heated until complete dissolution of the sample. Pour 10 cmof sulphuric acid diluted 1:1, heating was continued to highlight the vapours of sulphuric anhydride, cooled, washed the walls of the Cup with water, pour 2 cmof hydrogen peroxide, transfer the solution into volumetric flask with a capacity of 100 cm, cooled, adjusted to the mark with water.

A solution of tungsten (work) containing 0.1 mg/cmtungsten. In a volumetric flask with a capacity of 100 cmpipetted 10cmbackup solution, adjusted to the mark with water.

Standard solution of iron (spare) containing 1 mg/cmiron

0.1 g of iron metal is placed in a beaker with a capacity of 100 cmand dissolved by heating at 200 °C in a mixture of 5 cmof nitric acid, diluted 1:1, and 5 cmof water. Upon dissolution of the sample flow 10 cmof sulphuric acid diluted 1:1, and heating was continued to release sulfuric acid vapors, cooled, poured 50 cmof water, heated to dissolve the salts, and transfer the resulting solution into a measuring flask with a capacity of 100 cm, adjusted to the mark with water.

A solution of iron (working) containing 0.01 mg/cmof iron. In a volumetric flask with a capacity of 500 cmpipetted 5 cmbackup solution, adjusted to the mark with water.

A standard solution of manganese (spare) containing 1 mg/cmof manganese

0.1 g of manganese metal is placed in a beaker with a capacity of 100 cmand dissolved under moderate heating in 5 cmof nitric acid, diluted 1:1. Upon dissolution of the sample flow 10 cmof sulphuric acid diluted 1:1, and heating was continued to release sulfuric acid vapors, cooled, poured 50 cmof water, heated to dissolve the salts, and transfer the resulting solution into a measuring flask with a capacity of 100 cmand adjusted to the mark with water.

A solution of manganese (working) containing 0.01 mg/cmof manganese. In a volumetric flask with a capacity of 500 cmpipetted 5 cmbackup solution, adjusted to the mark with water.

A standard solution of molybdenum (spare) containing 1 mg/cmof molybdenum

0.1 g of metallic molybdenum were placed in a glass with a capacity of 100 cmand dissolved by heating at 350−400 °C in 5 cmof nitric acid, diluted 1:1. After dissolution, the sample flow 10 cmof sulphuric acid diluted 1:1, and heating was continued to release sulfuric acid vapors, cooled, poured 50 cmof water, heated to dissolve the salts, transfer the resulting solution into a measuring flask with a capacity of 100 cmand adjusted to the mark with water.

Solution of molybdenum (working) containing 0.1 mg/cmof molybdenum. In a volumetric flask with a capacity of 100 cmpipetted 10cmbackup solution, adjusted to the mark with water.

A standard solution of niobium (spare) containing 1 mg/cmof niobium

0.1 g of niobium metal is placed in a glass-carbon Cup, pour 5 cmof concentrated nitric acid, a few drops of hydrofluoric acid and dissolve with a moderate heat, adding in the course of dissolution several times by drops of hydrofluoric acid. Upon dissolution of the sample flow 10 cmof sulphuric acid diluted 1:1, heating was continued to release sulfuric acid vapors, cooled, poured 10 cmof water, 2 cmof hydrogen peroxide, the resulting solution was transferred into a measuring flask with a capacity of 100 cmand adjusted to the mark with water.

The solution of niobium (working) containing 0.1 mg/cmniobium. In a volumetric flask with a capacity of 100 cmpipetted 10cmbackup solution, adjusted to the mark with water.

A standard solution of titanium (spare) containing 1 mg/cmtitanium

0.1 g of titanium metal is placed in a beaker with a capacity of 100 cmand dissolved by heating in 10 cmof sulphuric acid diluted 1:1. Upon dissolution of the sample poured 5 cmof nitric acid, diluted 1:1, and heating was continued to release sulfuric acid vapors, cooled, poured 50 cmof water, heated to dissolve the salts, transfer the resulting solution into a measuring flask with a capacity of 100 cmand adjusted to the mark with water.

A solution of titanium (working) containing 0.1 mg/cmof titanium. In a volumetric flask with a capacity of 100 cmpipetted 10cmbackup solution, adjusted to the mark with water.

Standard solution of chromium (spare) containing 1 mg/cmchrome

0.1 g of chromium metal is placed in a beaker with a capacity of 100 cmand dissolved by heating in 10 cmof sulphuric acid diluted 1:1. Upon dissolution of the sample poured 5 cmof nitric acid, diluted 1:1, heating was continued to release sulfuric acid vapors, cooled, poured 50 cmof water, heated to dissolve the salts, transfer the resulting solution into a measuring flask with a capacity of 100 cmand adjusted to the mark with water.

A solution of chromium (work) containing 0.01 mg/cmchrome. In a volumetric flask with a capacity of 500 cmpipetted 5 cmbackup solution, adjusted to the mark with water.

Standard solution zirconium (spare) containing 1 mg/cmof Zirconia

0.1 g of metallic zirconium is placed in a glass-carbon Cup, pour 5 cmof concentrated nitric acid, a few drops of hydrofluoric acid and dissolve with a moderate heat, adding in the course of dissolution several times by drops of hydrofluoric acid. Upon dissolution of the sample flow 10 cmof sulphuric acid diluted 1:1, heating was continued to release sulfuric acid vapors, cooled, poured 10 cmof water, 2 cmof hydrogen peroxide, the resulting solution was transferred into a measuring flask with a capacity of 100 cmand adjusted to the mark with water.

A solution of zirconium (working) containing 0.1 mg/cmzirconium. In a volumetric flask with a capacity of 100 cmpipetted 10cmbackup solution, adjusted to the mark with water.

(Changed edition, Rev. N 1).

3. ANALYSIS

3.1. Preparation of working solutions comparison (PC)

(Changed edition, Rev. N 1).

3.1.1. Preparation of working solutions comparison for the analysis of alloys or alloys based on vanadium with a mass fraction of aluminium (from 1 to 50%); vanadium (from 20 to 90%); iron (from 0.1 to 10%); manganese (0.1 to 10%); molybdenum (from 5 to 30%); titanium (from 5 to 25%); temple (from 0.1 to 50%).

Series 1, the solution N 1 (PC 1−1). In a volumetric flask with a capacity of 100 cmsuccessively introduced 1 cmstandard working solution of aluminum 2 cmstandard solution vanadium 10 cmstandard working solution of iron and 10 cmof standard working solution of manganese, 5 cmstandard working solution of molybdenum, 5 cmstandard working solution of titanium, 10 cmof standard working solution of chrome is brought to the mark with water.

The composition of the solution of the PC 1−1 shown in table.2.

Series 1, solution N 2 (PC 1−2). In a volumetric flask with a capacity of 100 cmsuccessively introduced 5 cmstandard alternate solution of aluminum 10 cmof a standard solution of vanadium, 1 cmstandard fallback solution of iron, 1 cmstandard fallback solution of manganese, 3 cmstandard fallback solution of molybdenum, 2.5 cmstandard backup solution titanium, 5 cmstandard alternate solution chromium, adjusted to the mark with water. The composition of the solution PC 1−2 are given in table.2.

Table 2

Series 1, solution of N 3 (PC 1−3). In a volumetric flask with a capacity of 100 cmsuccessively introduced:

1 cmstandard working solution of aluminium,

10 cmstandard working solution of iron,

10 cmstandard working solution of manganese,

10 cmstandard working solution of chromium,

bring to mark with water. The composition of the solution PC 1−3 are given in table.2.

Series 1, the solution N 4 (PC 1−4). In a volumetric flask with a capacity of 100 cmsuccessively introduced 1 cmstandard fallback solution of aluminum, 1 cmstandard fallback solution of iron, 1 cmstandard fallback solution of manganese, 1 cmstandard backup solution chromium, adjusted to the mark with water. The composition of the solution PC 1−4 are given in table.2.

3.1.2. Preparation of working solutions of comparison for the analysis of alloys of the vanadium and tungsten with a mass fraction of aluminum (0.1 to 1%); vanadium (from 70 to 90%); tungsten (1 to 10%); iron (0.1 to 1%); manganese (0.1 to 1%); chromium (from 0.1 to 1%).

Series 2, solution 1 (PC 2−1). In a volumetric flask with a capacity of 100 cmsuccessively introduced 5 cmstandard solution of vanadium, 1 cmstandard working solution of tungsten was adjusted to the mark with water. The composition of the solution PC 2−1 are given in table.3.

Table 3

Series 2, solution N 2 (PC 2−2). In a volumetric flask with a capacity of 100 cmsuccessively introduced 10 cmstandard solution vanadium 10 cmstandard working solution of tungsten was adjusted to the mark with water. The composition of the solution PC 2−2 is shown in table.3.

3.1.3. Preparation of working solutions comparison for the analysis of master alloys based on vanadium with a mass fraction of aluminum (from 10 to 30%); vanadium (from 50 to 90%); iron (0.1 to 1%); manganese (0.1 to 1%); niobium (from 1 to 30%); zirconium (1 to 20%); chromium (from 0.1 to 1%).

Series 3, a solution of N 1 (PC 3−1). In a volumetric flask with a capacity of 100 cmsuccessively introduced 1 cmstandard fallback solution of aluminium 5 cmof a standard solution of vanadium, 1 cmstandard working solution of niobium, 1 cmstandard working solution of zirconium was adjusted to the mark with water.

The composition of the solution PC 3−1 are shown in table.4.

Table 4

Series 3, a solution of N 2 (PC 3−2). In a volumetric flask with a capacity of 100 cmsuccessively introduced 3 cmstandard fallback solution of aluminum 10 cmof a standard solution of vanadium, 3 cmstandard fallback solution of niobium 2 cmstandard fallback solution of zirconium was adjusted to the mark with water. The composition of the solution PC 3−2 are given in table.4.

3.1.1−3.1.3. (Changed edition, Rev. N 1).

3.2. Preparation of samples for analysis

3.2.1. Analysis of master alloys or alloys based on vanadium with a mass fraction of aluminium (from 1 to 50%); iron (from 0.1 to 10%), manganese (0.1 to 10%), molybdenum (from 5 to 30%), titanium (from 5 to 25%), chromium (from 0.1 to 50%).

A portion of the sample weighing 0.1 g was placed in a beaker with a capacity of 100 cmand dissolved by heating in a mixture of 10 cmof sulphuric acid diluted 1:1 with 5 cm.of nitric acid diluted 1:1. Upon dissolution of the sample heating was continued until the vapors escaping sulfuric acid, cooled, poured 50 cmof water, heated to dissolve the salts, transfer the resulting solution into a measuring flask with a capacity of 100 cmand adjusted to the mark with water.

(Changed edition, Rev. N 1).

3.2.2. (Deleted, Rev. N 1).

3.2.3. Analysis of alloys of the vanadium and tungsten and analysis of master alloys or alloys based on vanadium with a mass fraction of aluminium (10 to 30%), iron (0.1 to 1%), manganese (0.1 to 1%), niobium (from 1 to 30%), zirconium (1−20%), chromium (0.1 to 1%).

A portion of the sample weighing 0.1 g was placed in a platinum or glassy carbon Cup, pour 5 cmof concentrated nitric acid, a few drops of hydrofluoric acid and dissolve with a moderate heat, adding in the course of dissolution several times by drops of hydrofluoric acid. Upon dissolution of the sample flow 10 cmof sulphuric acid diluted 1:1, heating was continued to release sulfuric acid vapors, cooled, poured 10 cmof water, 2 cmof hydrogen peroxide, heated to dissolve the salts, transfer the solution into a volumetric flask with a capacity of 100 cmand adjusted to the mark with water.

(Changed edition, Rev. N 1).

3.2.4. The solutions obtained by PP.3.2.1 or 3.2.2 is used to determine the impurities of aluminum, iron, manganese and chromium at a content of from 0.1 to 1%; for definition of components with a mass fraction more than 1% of the resulting solution is diluted: take 5cmof the solution in a volumetric flask with a capacity of 50 cmand was adjusted to the mark with water.

Simultaneously with the analysis of a series of samples through all stages of the analysis spend control experience. The solution in the reference experiment is used as a background solution.

(Added, Rev. N 1).

3.3. To perform the assay

(Changed edition, Rev. N 1).

3.3.1. Spectral-analytical complex ready to work according to «Working instruction manual for spectral-analytical complex» (RI). All of the following actions is performed in accordance with RI.

3.3.2. Include plasma and set its parameters:

the power fed to the plasma — 1,0−1,2 kW;

the consumption of plasma — forming argon of 0.2−0.8 DM/min;

the flow-rate of argon — 12−20 DM/min;

the spray flow rate of argon of 0.2−0.6 DM/min;

the feed rate of solution into the plasma and 1.8−3.0 cm/min.

3.3.3. Perform a profiling operation on polychromator and the monochromator.

3.3.4. The mode of operation of the spectrometer:

the integration time is 10 s;

method of measurement of the analytical signal:

polychromator — integration is at its peak;

monochromator — integrating the intensity in the maximum of the peak after a preliminary search it when scanning in the vicinity of the analytical line.

Wavelength of analytical spectral lines are given in table.5. Allowed to use other methods of measurements in accordance with the RI.

Table 5

The use of other wavelengths free of spectral interference caused by the composition of the analyzed alloys (alloy).

3.3.5. Switches the voltage on the PMT corresponding to the analytical lines of the determined elements in poly — and monochromator set to the position providing the excess value of the analytical signal above the background for the PC 1−1, 1−3 PC, PC PC 2−1 or 3−1 at least 20 PC 1−2, PC 1−4, PC PC 2−2 or 3−2 — not less than 50 relative units and the value of relative standard deviation () of three parallel measurements is not more than 3%.

3.3.6. Sequentially injected into the plasma corresponding solutions comparison, selected based on the composition of the analyzed alloys (alloys). With the help of a special program using the least squares method to get the numerical coefficients of the polynomial approximating the calibration characteristics for each of the identified elements.

The calibration characteristics is obtained in the coordinates (1), where 1 is the intensity of the analytical lines of the element minus the intensity of the emission spectrum for the solution in the reference experiment at the wavelength of the analytical line of the element; is the concentration of the element in solution comparison, µg/cm.

3.3.7. Solutions of samples analysed successively introduced into the plasma and measure the intensity of the analytical lines of the determined elements and background. In accordance with the program for each solution is performed in 3 dimensions and calculates the average value, which is the result of one parallel definition. After the introduction and measure 4−5 of the sample solution, repeat measurement solutions comparison. The values obtained must not differ by more than 1% of the original (p.3.3.6). Otherwise sprayed into the plasma again, the corresponding solutions comparison and get with the program numerical coefficients taking into account the drift of the calibration parameters for each analyzed element, then continue the analysis.

3.3.8. With the help of a special program on a display screen or printout get: symbols of the determined elements, the values of analytical signals and the corresponding concentrations of the determined elements in the samples.

3.3.1−3.3.8. (Added, Rev. N 1).

4. PROCESSING OF THE RESULTS

4.1. Mass fraction of impurity is defined () in percent is calculated by the formula

,

where is the mass concentration determined by the impurity in the sample solution, µg/cm;

 — the volume of the sample solution, cm;

 — the weight of the portion of the sample,

4.2. Mass fraction of the designated component (a) in percent is calculated by the formula

,

where is the mass concentration of the analyte in the test solution, µg/cm;

 — the volume of the sample solution, cm;

 — the weight of the portion of the sample,

4.3. The values of permissible differences given in table.6.

Table 6

Section 4. (Changed edition, Rev. N 1).