GOST 9519.2-77

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  ГОСТ 9519.2-77

GOST 9519.2−77 Babbit calcium. Method of spectral analysis on synthetic standard samples (with Amendments No. 1, 2)

GOST 9519.2−77

Group B59

INTERSTATE STANDARD

CALCIUM BABBITS

Method of spectral analysis on synthetic standard samples

Lead-calcium bearing alloys. Method of spectral analysis on synthetic standart specimens

AXTU 1709

Date of introduction 1978−01−01

INFORMATION DATA

1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy

DEVELOPERS

B. C. Chumachenko, L. I. Punin, V. I. Petrov, A. I. Pogonina, S. D. Demchenko, R. P. Petrova

2. APPROVED AND promulgated by the DECREE of the State Committee of standards of Ministerial Council of the USSR from 15.04.77 N 946

3. INTRODUCED FOR THE FIRST TIME

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

5. Limitation of actions taken by Protocol No. 3−93 Interstate Council for standardization, Metrology and certification (ICS 5−6-93)

6. EDITION (July 2000) with Amendments No. 1, 2, approved in October 1982, June 1987 (ICS 1−83, 10−87)


This standard applies to calcium babbits and sets the method of spectral analysis on synthetic standard samples of the enterprise.

The method is based on measuring the relative intensities of spectral lines of the sample in the excitation spectra of the discharge arc AC.

Method sets the determination of impurities and main components of calcium babbits in the range of mass fraction of, %:

calcium is from 0.2 to 1.5;

sodium from 0.2 to 1.2;

tin, from 0.5 to 3.0;

of magnesium, from 0.01 to 0.20;

of bismuth is from 0.05 to 0.25;

of antimony from 0.05 to 0.5;

aluminum from 0.01 to 0.5;

of copper, from 0.01 to 0.5.

(Changed edition, Rev. N 1, 2).

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis and security requirements — according to GOST 9519.0.

(Changed edition, Rev. N 1).

1.2−1.5. (Deleted, Rev. N 1).

Sec. 2. (Deleted, Rev. N 1).

3. APPARATUS, REAGENTS AND MATERIALS

The quartz spectrograph medium dispersion being a lighting system (SP-30, SP-28, etc.).

Arc generator, AC, DG-2 and light source.

Microphotometer MF-2.

Three-step attenuator.

Coals spectral-clear stamps-2 in the form of bars with diameter 6 mm.

Installation (set of cutters) for sharpening carbon electrodes with a crater of size 4x4 mm, or a truncated cone with ground diameter of 2 mm, or hemisphere.

Photographic plates of type I according to GOST 10691.0.

Analytical scale type ADV-200.

Watch-glasses.

Mortar with pestle, agate or Jasper.

Drying Cabinet.

Muffle furnace with thermostat, providing a temperature of 750−800 °C.

Boxy glass.

The desiccator.

Files.

Tongs crucible.

The N developer 1 and fixer.

Hydrolysis of the ethyl alcohol of the highest purification.

Calcium carbonate according to GOST 4530.

The anhydrous sodium carbonate according to GOST 83.

Magnesium carbonate according to GOST 6419.

Tin dioxide (oxide), h.d. a.

Antimony oxide, h.d. a.

Lead oxide by ND.

Aluminium oxide, C. D. and.

Copper oxide according to GOST 16539.

Bismuth oxide according to GOST 10216.

Magnesium oxide according to GOST 4526.

Note. Permitted to use other equipment, materials and reagents, subject to obtaining the accuracy of the analysis is not lower than this standard.


(Changed edition, Rev. N 1).

4. PREPARATION OF SYNTHETIC STANDARD SAMPLES OF THE ENTERPRISE

4.1. For each grade of alloy is preparing a series of synthetic standard samples of the enterprise, which are a mixture of metal oxides. Head first, prepare the samples and then by diluting the appropriate series of synthetic standard samples of the enterprise.

Head samples are a mixture of the oxides with a maximum content of all impurities.

The calculation of the mass of sample for each item produced by the formula

,

where  — mass fraction of the input element, %;

 — the weight of the head sample, g;

 — molecular weight chemical compounds that contain the input element;

 — the atomic weight of the input element;

 — the number of atoms of the input element comprising molecules of chemical compounds.

To account for amendments to the content of the basic substance, the mass of the sample corrected by multiplying the results obtained on the coefficient , where the content of the basic substance used in a chemical reagent.

Base (lead oxide) is introduced into a mixture of calculation , where the whole mass of the synthetic standard sample of the enterprise;  — the sum of all the injected impurities.

4.2. To prepare standard samples of head companies are taking the sample in accordance with table.1 or calculate the weight by the formula (p.4.1) pre-dried anhydrous reagents.

Table 1

Elements content in the head samples (per 10 g)

Extension table 1

The reagents are placed in an agate or a Jasper mortar, moistened with a small amount of alcohol and dissolved to dry. This operation is repeated 6−7 times for 6−7 h until a homogeneous mass.

Ready prototype and electrodes with the standard samples of the enterprise stored in a desiccator.

4.3. A series of synthetic standard samples of the enterprise weighing 2 or 3 grams is prepared from a primary sample serial dilution, that is, each subsequent synthetic factory standard sample is prepared by dilution of the previous two times.

When diluted every new mixture triturated, adding alcohol 4−5 times within 3 hours.

Note. The work requires great care. To avoid loss of trace impurities is not to prevent «wypalania» mix on the edges of the mortar.

4.1−4.3. (Changed edition, Rev. N 1, 2).

4.4. Preparation of the material of a standard sample of the enterprise and its certification is carried out in accordance with GOST 9519.1.

(Added, Rev. N 2).

5. PREPARATION FOR ASSAY

5.1. Synthetic standard samples of the enterprise, dried in an oven at 100−120 °C for 30 min, tightly Packed into the crater of a carbon electrode and used within 1 h.

(Changed edition, Rev. N 1).

5.2. The test sample with a file cleaned of surface dirt, then clean with a file removed about 1 g of the shavings for analysis. Part of the shavings tightly Packed into the crater of the carbon electrode.

The finished electrodes are put in a porcelain crucible and placed for 2−3 min in a muffle furnace heated to 750−800 °C.

They are heated to a brick-red color.

6. ANALYSIS

6.1. A carbon electrode prepared in accordance with the PP.5.1 and 5.2, strengthen the lower electrode holder tripod spectrograph.

As the second set of electrode carbon rod, sharpened to a hemisphere or a truncated cone with the base 2 mm. Distance between electrodes 1.5 mm set pattern.

6.2. As a source of spectra excitation using arc generator, AC, DG-2. Mode arc current 5 A. the slit Width of the spectrograph set to 0.012 mm, the height of the intermediate diaphragm is 5 mm.

6.3. On the slit of a spectrograph establish a three-tier reliever to ensure the normal densities of the blackening of analytical lines with single shooting for all concentrations.

6.4. Synthetic spectra of standard samples of the enterprise and the investigated samples are photographed three times, randomizer order take consecutive photographs of the spectra of synthetic standard samples of the enterprise and samples.

(Changed edition, Rev. N 1).

6.5. A photographic plate of the type I placed in the cassette so as to cover the investigated range of the spectrum.

6.6. Annealing of the samples produced within 5 s. exposure Time 35−45 with selected depending on the sensitivity of photographic plates.

6.7. Processing of photographic plates produced according to GOST 10691.0.

6.8. The wavelengths of the analytical lines and lines of comparison are given in table.1A.

Table 1A

Note. When a sample of zinc superimposed line zinc 330,2 nm line of sodium 330,2 nm. The lack of zinc in the samples control in the more sensitive line zinc 334,5 nm. The appearance of the line zinc sodium determine the chemical or atomic absorption method.

6.9. The optical density of the analytical line () and lines () is measured by microphotometer.

6.10. On the measured values the calculated difference of the optical densities of the analytical lines and comparison lines , averaging these values along three parallel spectrograms, getting . Calibration curve constructed in the coordinates for each of the photographic plates on which the photographed spectra of the analyzed samples and synthetic standard samples of the enterprise.

6.11. Position monitoring of the calibration curve carried out according to standard samples periodically.

The offset of the calibration curve is considered valid when the condition

,

where the result of the analysis, %;

 — mass fraction, given in the certificate of standard sample, %;

 — the allowable difference shown in table.3, %;

the value of the certified characteristics, %.

6.8−6.11. (Added, Rev. N 2).

7. PROCESSING OF THE RESULTS

7.1−7.3. (Deleted, Rev. N 2).

7.4. For the results analysis be the arithmetic mean of results of three parallel measurements. The allowable divergence between the most differing data at a confidence level of 0.95 does not exceed the values given in table.3.

Table 3*

________________
* Table 2. (Deleted, Rev. N 2).

The numerical values of the results of the analysis should end with the figure of the same kind, and corresponding standard indicators of the chemical composition specified in the standards for grades.

(Changed edition, Rev. N 2).

7.5. The reproducibility of the analysis of the same samples (), made at different times in different laboratories according to this method, must satisfy the condition

,

where  — the allowable difference specified in table.3, %.

7.6. In case of contact analysis results in the critical region of the tolerance field on the element content in the alloy of a given brand (normalized border vintage composition according to GOST 1209), the sample is analyzed by chemical methods 1219.1 according to GOST-GOST 1219.8.

7.5, 7.6. (Added, Rev. N 2).