GOST 9717.2-82

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  ГОСТ 9717.2-82

GOST 9717.2−82 Copper. Method of spectral analysis on a metal standard samples with photographic registration of spectrum (with Amendments No. 1, 2)

GOST 9717.2−82

Group B59

STATE STANDARD OF THE USSR

COPPER

Method of spectral analysis on a metal standard samples with photographic registration of spectrum

Copper. Method of spectral analysis of metal standart specimens with photographic registration of spectrum

AXTU 1709

Date of introduction 1983−07−01

INFORMATION DATA

1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR

DEVELOPERS

A. M. Rytikov, A. A. Nemodruk, M. V. Taubkin, M. P., Burmistrov, I. A. Vorobyev

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from 24.03.82 N 1199

3. REPLACE GOST 9717.2−75

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

5. The expiration time limit is removed by the Resolution of Gosstandart from 03.11.92 N 1481

6. The re-release (may 1997) with Amendments No. 1, 2 approved in December 1987 and November 1992 (ICS 2−88, 2−93)


This standard sets the method of spectral analysis on a metal standard samples (SS) with photographic registration of spectrum copper according to GOST 859*.
_______________
* On the territory of the Russian Federation the document is not valid. Valid GOST 859−2001. — Note the manufacturer’s database.

The method is based on the excitation spectrum of the metal samples arc discharge AC followed his photographic registration.

The method allows to determine the content of impurities in of copper in the range of mass fraction:

The method is characterized by the relative standard deviation of single measurement is given in table.1.

Table 1

(Changed edition, Rev. N 2).

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis according to GOST and GOST 25086 9717.1*.
________________
* On the territory of the Russian Federation the document is not valid. Standards 31382−2009. — Note the manufacturer’s database.

2. APPARATUS, MATERIALS AND SOLUTIONS

Spectrograph with high resolution for photographing the ultraviolet region of the spectrum (ISP-30, STE-1 and other types).

A constant current source to power the arc, providing a voltage of 200−400 V and currents up to 10 A.

AC source (generator powerplant-1 with a tripod of the type of PCS-16, DG-2 with stand type PCS-16, DG-2 with stand type, PCS-9, IVS-21, IVS-28).

Microphotometer MF2 or FFI-460.

Spectromancer PS-18 or other type.

Fixture for grinding copper electrodes, machine model CP-35.

Spectrographic plates.

Metol (para-metilaminofenazon) according to GOST 25664.

Hydroquinone (paradoxians) according to GOST 19627.

Sanitarily anhydrous sodium GOST 195.

Sodium carbonate according to GOST 83.

Potassium bromide according to GOST 4160.

Sodium thiosulfate crystal according to GOST 244.

Acetic acid according to GOST 61.

Nitric acid according to GOST 4461 diluted 1:10.

The technical rectified ethyl alcohol according to GOST 18300. Consumption of alcohol per one definition in ' 10

Standard samples for composition of copper for spectral analysis.

Developer for photographic plates of the spectral types 1, 2, «Micro» and ES prepared by mixing equal volumes of solutions 1 and 2 before use.

Solution 1: 2.5 g of metol 12 g of hydroquinone and 100 g semitecolo sodium dissolved in 500−700 cmof water and add water to 1 DM.

Solution 2: 100 g of sodium carbonate and 7 g of potassium bromide dissolved in 500−700 cmof water and add water to 1 DM; it allowed the application and other high contrast developers.

Fixing solution: 300 g sodium thiosulfate, 25 g of sodium semitecolo and 8 cmof acetic acid are dissolved in 1 DMdistilled water; allowed the use of other fixing solutions.

Allowed to use other equipment, equipment and materials, provided that the metrological characteristics of the analysis, no worse than provided by this standard.

Distilled water according to GOST 6709.

(Changed edition, Rev. N 1, 2).

3. PREPARATION FOR ASSAY

3.1. Of the sample and standard samples prepared in the form of rods with a diameter of 7−8 mm, length 30 to 60 mm of two cores from each test sample. The ends of the rods sharpened to a hemisphere or a truncated cone with a diameter of 1.5−1.7 mm, etched for cleaning the surface of impurities in nitric acid, diluted 1:10, washed with water, alcohol and dried.

The mass of the rods, the spectra being photographed on the same photographic plate, shall not differ by more than 1 g.

It is possible to manufacture rods of the indicated size of chips, powder, etc., by fusing at a temperature (1225±25) °C in a graphite crucible required diameter. The alloy is kept in the molten state of not more than 1 minutes, then the crucibles are placed in cold water and quickly cooled.

(Changed edition, Rev. N 2).

4. ANALYSIS

4.1 Sample or clamped in the upper and lower clamps of the tripod.

Between the ends of the electrodes, separated by 1.5−2.5 mm, light arc either AC or DC power 6−9 A. the content of silver is used in arc AC current of 4 A.

The interelectrode gap is set at a template, or micrometer screw. The arc length and the source position on the optical axis are controlled by the projection lens and screen mounted out of phase from the source to the slit. It is also allowed to use any other lighting system that provides uniform intensity of the line in the focal plane of the instrument.

The spectra photographed with a spectrograph with quartz optics medium variance type of ISP-30 or by using a diffraction spectrograph of STE-1, etc. depending on the type of spectrograph, the slit width varies from 0.007 to 0.015 mm.

To ensure the normal optical density of the analytical lines and the background is allowed to use photographic plates of different sensitivity, but the minimum of the measured optical density of the background should be at least 0.25.

Exposure time and distance from the light source to the slit of the spectrograph is adjusted depending on the sensitivity of the used photographic plates, ensuring the normal density of the background of the continuous spectrum. An increase in the density of the background due to the veils, lighting, etc. is not allowed.

Pre-firing is 10−15 s. the exposure Time is at least 20 C.

For each sample, or photograph of not less than two spectrograms.

(Changed edition, Rev. N 2).

4.2. Processing of photoplates

Show photographic plates in developer, fix in fixing solution, washed in running water and dried.

5. PROCESSING OF THE RESULTS

5.1. The optical densities of the analytical lines and lines of comparison spectrograms measured with microphotometry.

The wavelengths of the analytical lines and lines of comparison, as well as ranges of mass fractions of elements for the type of spectrograph ISP-30 are given in table.2, for a diffraction spectrograph of STE-1 — in table.3.

Table 2

Note. Background 1 — the minimum value of the optical density of the background measured near the analytical line from the shorter wavelength.

Background 0 background 259,715 nm. A maximum distance of 0.09 mm from the line of antimony 259,806 nm to shorter wavelengths.

Background 2 — the optical density of weak molecular lines 235,08 nm, which is in the calculations taken as the density of the background.

Background 3 — minimum value of optical density of the background measured near the analytical line from the longer wavelengths.

Background 4 — the maximum value of the optical density of the background, measured at a distance of 0.13 mm from the lead line 283,307 nm in the direction of long waves.

Background 5 — the minimum value of the optical density of the background, measured between lines of copper 288,29 and 288,53 nm.

Table 3

Note. Background 1 — the minimum value of the optical density of the background measured near the analytical line from the shorter wavelength.

Background 2 — background 259,715 nm.

Background 3 — minimum value of optical density of the background measured near the analytical line from the long waves.

Background 4 — optimal density of weak molecular lines 235,08 nm, which is in the calculations taken as the density of the background.


Allowed the use of other analytical lines and comparisons provided that they provide the metrological characteristics and lower limits of detectable concentrations of elements that meet the requirements of this standard.

Calibration graphs constructed in the coordinates:

or ,

where is the relative intensity of the line of the element and the line of comparison (background);

 — the difference between the optical densities of the lines of the designated element and the comparison lines (copper);

 — mass fraction of the element.

The basic method for graphing is a method of «three standards»; it allowed the use of other methods of graphing method, for example, the solid calibration curve, standard method of control, etc.

Mass fraction of the designated contents of elements find the calibration schedule for the value found in the table of application , calculated over three (two) spectrograms.

5.2. The analysis result should be the arithmetic mean of two parallel definitions, if the difference between them at a confidence probability of 0.95 does not exceed the value calculated by the formula

,

where is the arithmetic mean of two parallel definitions %;

 — relative standard deviation.

If exceeded , repeat analysis of new batches of the same sample. In the case of repeated discrepancies analyze a new sample.

5.1, 5.2. (Changed edition, Rev. N 2).

5.3. The reproducibility of the results of primary and repeated tests are considered satisfactory if the discrepancy between the results of the two tests does not exceed the value calculated by the formula

.

5.4. Control of accuracy of analysis results according to the GOST 25086 standard samples for composition of copper not less than once per quarter.

5.3, 5.4. (Added, Rev. N 2).