GOST 9716.1-79

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  ГОСТ 9716.1-79

GOST 9716.1−79 Alloy copper and zinc. Method of spectral analysis on a metal standard samples with photographic registration of spectrum (with Change No. 1)

GOST 9716.1−79

Group B59

INTERSTATE STANDARD

ALLOYS COPPER-ZINC

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

Copper-zinc alloys. Method of spectral analysis of metal standard spesimens
with photographic registration of spectrum

AXTU 1709

Date of introduction 1981−01−01

INFORMATION DATA

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

DEVELOPERS

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

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from 26.12.79 N 5045

3. REPLACE GOST 9716.1−75

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

5. Limitation of actions taken by Protocol No. 5−94 of the Interstate Council for standardization, Metrology and certification (ICS 11−12−94)

6. The re-release (Oct 1998) with amendment No. 1, approved in July 1990 (IUS 11−90)


This standard sets the method of spectral analysis on a metal standard samples (SS) with photographic registration of spectrum and applies to brass stamps LS59−1, L63, LO70−1, l96, L68, L60, L70, L80, L85, L90, LO60−1, LO62−1, LO90−1, 58−2 LS, LS 63−3, 74−3 BOS, BOS 64−2, LS 60−1, LA 77−2, Lamsh 77−2-0,05, MESS 60−1-1, LAN 59−3-2, LMCA 57−3-1, LM 58−2, Lancz 75−2-2,5−0,5−0,5 according to GOST 15527*.
______________
* On the territory of the Russian Federation GOST 15527−2004. — Note the manufacturer’s database.

The method is based on the excitation spectrum of the arc discharge AC followed by registration of it on the plate with a spectrograph. Mass fraction of detectable elements find for the calibration graphics using the measured values of the difference of optical densities of the analytical lines and «internal standards» in the spectrograms of the alloy.

The method allows to determine in brass iron, lead, Nickel, aluminum, tin, silicon, arsenic, bismuth, antimony, and phosphorus in the range of mass fraction, indicated in the table.1.

Table 1

The precision and reproducibility of analysis are characterized by the values of the permissible differences given in table.2, for the confidence probability =0,95.

Table 2

Notes:

1. When verifying compliance with established standards of permissible differences of the two results of parallel measurements for be the arithmetic mean of the first and second results of parallel measurements of the impurities in the same sample.

2. When verifying compliance with established standards of permissible differences of the two results of the analysis for taking the average of the two results of the analysis of the same sample obtained at different times.


The interval defined by the mass fraction of elements can be extended both in smaller and in a big way through the use of the SOP and depending on the applied instruments and methods of analysis.

(Changed edition, Rev. N 1).

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis according to GOST 25086.

(Changed edition, Rev. N 1).

2. APPARATUS, MATERIALS AND SOLUTIONS

Spectrograph for photographing the ultraviolet region of the spectrum with medium-resolution type ICP-30.

Source current — the alternating current arc (generator powerplant-1 with a tripod of the type of PCS-16, DG-2 with stand type PCS-9 and IVS-21).

Microphotometer type MF2 or FFI-460.

Spectromancer PS-18 or other type.

Electrodes of copper grade M1 or coal grade C3 in the form of bars with diameter 6−7 mm, sharpened to a hemisphere or truncated cone.

A device for grinding coal or copper electrodes, machine model CP-35.

Lathe for sharpening and analyze samples on the plane of the type of TV 16.

Photographic plates of the spectral types 1, 2, «Micro», ES, UPS sensitivity from 0.5 to 60 units.

Metol (para-metilaminofenazon).

Hydroquinone (paradoxians) according to GOST 19627.

Sodium sulphate anhydrous according to GOST 195.

The anhydrous sodium carbonate according to GOST 83.

Potassium bromide according to GOST 4160.

Chernovetskiy crystalline sodium (thiosulfate) according to GOST 244.

Acetic acid according to GOST 61.

Distilled water according to GOST 6709.

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; prepared as follows: 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; is prepared as follows: 100 g of sodium carbonate and 7 g of potassium bromide dissolved in 500−700 cmof water and add water to 1 DM.

You can also use other contrasting working developers.

Developer for photographic plates of the spectral type UFS; prepared as follows: 2.2 g of metol, 8.8 grams of hydroquinone, 96 g semitecolo sodium, 48 g of sodium carbonate and 5 g of potassium bromide dissolved in 500−700 cmof water and add water to 1 DM.

Fixing solution; prepared as follows: 300 g of sodium thiosulfate, 25 g of sodium semitecolo and 8 cmof acetic acid are dissolved in 1 DMdistilled water.

You can also use other fixing solutions.

The use of other measuring instruments with the metrological characteristics of equipment and technical characteristics are not worse, and reagents for quality not lower than the above. Measuring instruments must be certified in accordance with GOST 8.326*.
______________
* On the territory of the Russian Federation there are PR 50.2.009−94. — Note the manufacturer’s database.

(Changed edition, Rev. N 1).

3. PREPARATION FOR ASSAY

3.1. Sample preparation and analysis must be the same type for each series of measurements. Mass of the sample and should not vary by more than 2 times.

Sample preparation is carried out with a sweep of one of its faces on a plane with a file or cutting tool (the machine) without coolant and lubricant.

When photographing each of a spectrum of the stripped surface should be a flat pad with a diameter of not less than 10 mm without holes, scratches, cracks, and slag inclusions. Before photographing spectra for removing contamination of the analyzed samples and wipe WITH ethanol.

(Changed edition, Rev. N 1).

4. ANALYSIS

4.1. The sample (or CO) is clamped in the lower clamp of the tripod and fed by coal or copper electrode so that the distance from ubeskrivelig plot to the edge of the sample was not less than the sparking spots (2−5 mm).

Between the ends of the electrodes, separated by 1.5−2.5 mm, light arc AC power 3−8 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.

The spectra photographed with a quartz spectrograph medium dispersion type of ISP-30. The slit of the spectrograph — 0,015 mm. With the aim of reducing the exposure time and obtaining high resolution of the spectrograph used astigmatic coverage of the gap with complete filling of the collimator lens. It may be recommended to use a spherical single-lens condenser with a focal length of 75 mm, located at a distance of 300 mm from the slit, and 72 mm from the light source.

It is also allowed to use any other lighting system that provides uniform intensity of the line in the focal plane of the instrument.

To ensure the normal optical density of the analytical lines and the background is allowed to use photographic plates of different sensitivity, however, 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.

The exposure time should be not less than 15 s. the time of the preliminary firing is 15 C.

For each sample (or samples) pictures of two spectrograms.

4.2. Processing of photographic plates.

A manifestation of photographic plates depending on the type carried out in the respective developer (see section 2) at a temperature of 18−20 °C.

After washing photographic plates in running water they are fixed in fixing solution, washed in running water and dried.

4.1, 4.2. (Changed edition, Rev. N 1).

5. PROCESSING OF THE RESULTS

5.1. The optical densities of the analytical lines and «internal standards» in the spectrograms are measured with the aid of microphotometer.

The analytical lines chosen depending on the grade alloy.

The wavelengths of the analytical lines and «internal standards» (background) are shown in table.3.

Table 3

Note. «Background 1» means the minimum value of the optical density of the background measured near the analytical line from the longer wavelengths.

«Background 2» means the minimum value of the optical density of the background measured near the analytical line from the shorter wavelength;

«Background 3» means the optical density of weak molecular lines 235,08 nm, which is in the calculations assumed to be the density of the background;

«Background 4» means the minimum value of the optical density of the background, measured between lines of copper 288,29 and 288,53 nm;

«Background 5» means 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.


Allowed the use of other analytical, internal standards, sources of spectra excitation subject to obtaining the metrological characteristics are not worse than specified in this standard.

The primary method recommended to perform the analysis, is the method of «three standards». Allowed the use of other methods of graphing, for example, the method of solid calibration curve, method of control and standard.

In the spectrogram, using microphotometry measure the blackening of analytical lines of the determined elements and background . Calculate a value .

Find the arithmetic mean of the results obtained on the two spectrograms of each standard sample (), count in the application table and build a calibration curve in the coordinates where  — mass fraction of impurities in the standard samples, %. For the calibration chart find the content of impurities for each of the two spectrograms obtained for one sample.

The final result of the analysis be the arithmetic mean of results of two parallel measurements obtained on the same photographic plate.

If the difference between parallel determinations exceeds the permissible differences given in table.2, the photographing of the spectra is repeated on the second photographic plate. In this case, the final result of the analysis be the arithmetic mean of four parallel measurements.

Control of accuracy of analysis results is carried out according to GOST 25086 using state, industry standard samples or standard samples of the enterprise.

(Changed edition, Rev. N 1).