GOST 13348-74

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  ГОСТ 13348-74

GOST 13348−74 lead-antimony Alloys. Method of spectral analysis (with Amendments No. 1, 2, 3)

GOST 13348−74

Group B59

INTERSTATE STANDARD

LEAD-ANTIMONY ALLOYS

Method of spectral analysis

Antimonous antimonides. Method of spectral analysis

ISS 77.120.60
AXTU 1709

Date of introduction 1975−01−01

INFORMATION DATA

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

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from 24.05.74 N 1299

Change No. 3 adopted by the Interstate Council for standardization, Metrology and certification (Protocol No. 8, dated 12.10.95)

The adoption of the changes voted:

3. REPLACE GOST 13348−67

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

5. Limitation of actions taken by Protocol No. 4−93 of the Interstate Council for standardization, Metrology and certification (ICS 4−94)

6. EDITION (July 2003) with Changes 1, 2, 3, approved in August 1983, June 1989, February 2001 (IUS 12−83, 10−89, 5−2001)


This standard applies to lead-antimony alloys and establishes a spectral method for the determination of copper, antimony, bismuth, silver, arsenic, tin, tellurium and zinc.

Method of spectral analysis based on spark excitation spectrum with photographic or photoelectric registration of the emission of spectral lines.

(Changed edition, Rev. N 1, 3).

1. GENERAL REQUIREMENTS

1.1. A sample selected according to GOST 1292 and to deliver on spectral analysis in the form of cast rods of circular cross section with a diameter of 7−10 mm and a length of 50−100 mm or in the form of cylinders with a diameter of 20−40 mm and a height of 10−50 mm.

Standard samples and incoming samples must be adequate in structure, shape and size, the analyzed surface should be treated in the same way.

(Changed edition, Rev. N 3).

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

(Changed edition, Rev. N 2).

1.3. Method of spectral analysis allows to identify the main components and impurities in mass fractions, %:

of antimony, 0.1 to 8;

of copper, from 0.001 to 0.3;

bismuth — from 0.01 to 0.08;

silver from 0.001 to 0.03;

of arsenic from 0.002 to 0.4;

tin — from 0.002 to 0.5;

tellurium — from 0,004 to 0.06;

zinc — from 0,0009 to 0.1.

(Changed edition, Rev. N 1, 2, 3).

1A. SAFETY REQUIREMENTS

1.1. When performing tests, it is necessary to comply with the safety requirements according to GOST 1293.0* and normative-technical documentation approved in the established order.
______________
* On the territory of the Russian Federation GOST 1293.0−2006. — Note the manufacturer’s database.

(Added, Rev. N 1).

1.1 a.1. All devices used for the spectral analysis of lead-antimony alloys, must be equipped with devices for grounding according to GOST 12.2.007.0 and GOST 12.1.030 and grounded in accordance with the requirements of the Rules for electrical installations approved by Glavgosenergonadzora.

1.1.2. To prevent entering the working area of harmful substances emitted in the sources of spectra excitation and bad acting on the body in quantities exceeding the maximum allowable concentration to protect against electromagnetic radiation and prevent sunburn by ultraviolet rays, each a source of excitation spectra should be placed inside of the device, equipped with an integrated exhaust air inlet according to GOST 12.4.021 and protective screen.

1.1.3. The machine is used for grinding carbon electrodes must have a built-in exhaust air inlet to prevent the ingress of carbon dust in the air, in quantities exceeding maximum permissible concentration.

1.1.4. Preparation of samples for analysis (dissolution, evaporation, and the taking of test portions, grinding, gasket carbon electrodes) must be in the pits, equipped with built-in exhaust air terminals.

1.1.5. Permissible noise levels on workplaces should correspond to GOST 12.1.003.

Monitoring of noise level at the workplace of laboratory facilities should be carried out according to GOST 12.1.050.

1.1.6. Laboratory facilities of spectral analysis shall conform to the requirements of the rules for arrangement and maintenance of laboratories and points of spectral analysis, approved in the established order.

1.1 a.1−1.1 a.6. (Added, Rev. N 2).

2. APPARATUS, MATERIALS AND REAGENTS

Set of equipment for emission spectral analysis with photographic (types spectrograph ISP-30 and DFS-8) or photovoltaic (quantometer type MFS-8) registration of the spectrum, providing the necessary sensitivity, allowing for a single exposure to range from 210 to 350 nm.

Generator spark types, IG-3, IVS-23 and others, allowing to obtain capacity from 0.01 to 0.02 µf, the inductance of 0.15 or 0.55 mH (one or two train per half cycle), current from 1.4 to 3 A.

Microphotometer of any type, intended for measuring the density of blackening of spectral lines.

Standard samples to construct calibration curve, produced and certified according to GOST 8.315.

Crucible furnace with temperature up to 500 °C.

Crucibles of graphite or graphite-refractory.

Mold for casting rods.

Files for sharpening rods.

Carbon electrodes, carbon brand p-3, sharpened to a truncated cone with ground diameter of 3.5 and 2 mm.

Photographic plates spectrographic types SFC-02, the SFC-03, NT-2SV at THAT 6−43−1475 or other types, allowing to obtain the desired sensitivity of the determined elements.

Metalhydrogen developer of the following composition:

Note. Allowed to use developer and fixer of a different composition. The time of development of photographic plates of all types — of (7±1) min at a temperature of 18−20 °C.

When taking batches for the preparation of developer and fixer are used analytical and technical scales with a weighing error of no more than 0.0002 g and 0.01 g, respectively.

The use of other devices, materials and reagents, subject to obtaining the metrological characteristics are not inferior to the specified in this standard.

Instruments must be certified in accordance with the requirements of GOST 8.326*.
_______________
* On the territory of the Russian Federation there are PR 50.2.009−94.

(Changed edition, Rev. N 1, 2, 3).

3. ANALYSIS

3.1. Determination of antimony and tin in excess of 0.3 percent copper, bismuth and silver within the limits specified in claim 1.3.

As the source excitation spectrum using spark discharge obtained by generator type IG-3. The generator is enabled by a complex scheme and works in «soft» mode: capacity of 0.01 microfarads, an inductance of 0.15 or 0.55 mH (one or two train per half-cycle), the current intensity of 1.4−1.6 And an auxiliary spark gap of 2.8 mm analytical gap of 2.5 mm Spectra on photographed plates spectrographic types SFC-02, the SFC-03, NT-2SV.

On the slit of a spectrograph establish a three-tier reliever. The slot width 0,020 mm. intermediate chart round or 5 mm. exposure Time 20−40 sec depending on the sensitivity of photographic plates. The lower electrode serves as the analyzed sample in the form of a rod, sharpened on the plane. The upper electrode is a carbon rod sharpened to a truncated cone.

Photometric the following pairs of lines:

Sb of 323.2 or 326,7 or 302,9 nm — Pb 322,0 or 311,8 nm

324,7 nm si — Pb 322,0 or 311,8 nm

306,7 nm Bi — Pb 322,0 or 311,8 nm

328,0 nm Ag — Pb 322,0 or 311,8 nm

Sn 284,0 or 303,4 nm — Pb 322,0 or 311,8 nm.

(Changed edition, Rev. N 1, 3).

3.2. Determination of arsenic, tellurium, antimony (0.1 and 0.3%), tin (less than 0.3%) and zinc.

As a source of excitation spectra using the spark generator of the type IG-3. The generator is enabled by a complex scheme and working in «hard» mode: capacitance is 0.02 µf, the inductance of 0.15 mH, the current strength of 2.8 to 3 And specifies the interval of 2.8 mm analytical gap 2.5 mm gap width 0,020 mm. intermediate diaphragm — round. The exposure time of 60 without pre-sparking. The lower electrode serves as the analyzed sample in the form of a rod, sharpened on the plane. The upper electrode is a carbon rod sharpened to a truncated cone.

Photometric the following pairs of lines:

As 234,9 nm — Pb 233,2 or 223,7 nm

Those 238,5 nm — Pb 233,2 or 223,7 nm, Pb 238,8 nm or background at a distance of 6 divisions of the micrometer screw from the side of long wavelengths

The amount of 231.1 nm Sb — Pb 233,2 or 223,7 nm

326,7 nm or Sb — Pb 322,0 or 311,8 nm

235,4 nm Sn — Pb 233,2 or 223,7 nm

334,5 nm Zn — Pb 322,0 nm.

When performing analysis on the device with photoelectric registration of spectrum (MFS-8 and others) to select the optimal conditions of excitation and registration of the spectra to achieve the necessary sensitivity and accuracy of analysis results. As counter electrode is used, offered by the manufacturer of the device, or carbon rod, sharpened to a truncated cone with ground diameter of 1.0 mm. Analytical lines and lines of comparison used are the same as those specified in the PP.3.1 and 3.2, or pick up experimentally other, giving the necessary sensitivity and free from overlap of interfering lines.

(Changed edition, Rev. N 1, 2, 3).

4. PROCESSING OF THE RESULTS

4.1. Spectra of unknown samples and standard samples are photographed on the same plate by six and three times respectively. The blackening of analytical lines () and compare () are measured on microphotometer. The calibration graphs are built in coordinates , where is the average of the three values ,  — known mass fraction of impurities determined in the standard samples in percent. According to the obtained values from the graphs determine the mass fraction of impurities in the analyzed samples. The final result of the analysis taking the arithmetic mean of the results of two parallel measurements obtained on a single photographic plate, each of the three spectrograms. Discrepancies between the results of parallel measurements at a confidence probability of 0.95 does not exceed the allowable absolute differences calculated by the formula

or ,

where is the relative standard deviation results of parallel measurements;

 — the arithmetic mean of parallel definitions;

 — the critical importance of scale sampling normal population, equal to 2.77 at 0.95 and 2.

The discrepancy between the two results of the analysis of the same samples at a confidence level of 0.95 does not exceed the allowable absolute differences calculated by the formula

,

where is the arithmetic mean of the two results of the analysis.

When working on devices with photoelectric registration of spectrum of the calibration graphs built in the coordinates where the certified value of the mass fraction of the element in the standard samples;  — the readings of the output of the measuring device, is proportional to the logarithm of the intensity of the lines of the designated element and element comparison.

For quantometers whose testimony the output of the device proportional to the relative line intensities, calibration graphs are built in coordinates .

The result of the analysis taking the arithmetic mean of two parallel definitions, each definition of the three dimensions.

(Changed edition, Rev. N 1, 2, 3).

4.2. Control of the correctness of the results of the analysis carried out using standard samples or by comparing the analysis results with data obtained by independent method at 1293.1 GOST — GOST 1293.5, 1293.10 GOST — GOST 1293.12.

When checking with standard samples the results of the analysis are considered correct, if the reproduced content of the determined component in different from the certified specifications in the certificate WITH no more than 0.71.

When checking independent method, the analysis results are considered valid if the difference between the results of spectral determination and control method satisfies the following inequality (in two parallel determinations):

,

where and  — mass fraction of component defined control and spectral methods, respectively, %;

and  — the permissible discrepancy between the results of parallel measurements for control and spectral methods, respectively, %.

(Added, Rev. N 2).