GOST 1429.13-77

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  ГОСТ 1429.13-77

GOST 1429.13−77 Solders tin-lead. Spectral method of determination of impurities of antimony, copper, bismuth, arsenic, iron, Nickel, zinc, aluminium using the synthetic calibration samples (with Amendments No. 1, 2)

GOST 1429.13−77*

Group B59

STATE STANDARD OF THE USSR

SOLDERS TIN-LEAD

Spectral method of determination of impurities
antimony, copper, bismuth, arsenic, iron, Nickel, zinc, aluminum
with the use of synthetic calibration samples

Tin-lead solders.
Spectral method for the determination of addition of antimony, copper,
bismuth, arsenic, iron, nickel, zinc, aluminium using the synthetic graduated samples*

AXTU 1709**
_________________
* The name of the standard. Changed the wording, Rev. N 2.
** Added, Rev. N 2.

Date of introduction 1978−01−01

The decision of the State standards Committee of the USSR Council of Ministers dated 11 April 1977, N 886 the period of validity set with 01.01.78

PROVEN in 1982 by the Resolution of Gosstandart from 21.01.83. 328 N validity extended until 01.01.88**
_____________
** Expiration removed Protocol MGS (IUS N 2, 1993). — Note the manufacturer’s database.

* REPRINT March 1983 with the Change in N 1, approved in January 1983; Post. N 326 from 21.01.83 (ICS 5−1983).

The Change N 2 approved and put into effect with 01.02.88 by the resolution of Gosstandart of the USSR from 30.06.87 N 3016

Change No. 2 made by the manufacturer of the database in the text IUS N 11, 1987


This standard establishes a spectral method for the determination of mass fractions of impurities in tin-lead solders: of antimony from 0.1 to 2; copper from 0.001 to 0.1; bismuth from 0.001 to 0.2; arsenic from 0.005 to 0.05; iron from 0.001 to 0.02; Nickel, from 0.001 to 0.08; zinc from 0.001 to 0.002 and aluminum of 0.001 to 0.002%.

The method is based on transforming a test sample of the metal in the oxide. The oxidized sample is mixed with carbon powder and placed in the crater, the lower carbon electrode. For the excitation spectrum using the arc AC (for determination of zinc — arc DC). Spectrum arc photographing the spectrograph. Then measure the blackening of analytical lines and «internal standard». Concentrations of the determined elements are found in the calibration schedule.

(Changed edition, Rev. N 1, 2).

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis according to GOST 1429.0−77.

2. APPARATUS, MATERIALS, REAGENTS

The quartz spectrograph of any type with photographic or photoelectric registration of spectrum, allowing to work in the ultraviolet region.

Arc generator of alternating current.

A constant current source.

A muffle furnace with thermostatic control.

Drying Cabinet.

Cup quartz varicellae.

Conical flasks or beakers.

Crucibles porcelain with GOST 9147−80.

Mortar agate or from glass.

Libra torsion or analytical.

Microphotometer.

Bath or electric hot plate.

Photographic plates spectrographic types SP-I, SP-II.

Graphite electrodes grades C-2, C-3 with the crater’s depth and diameter 3 mm.

Developer and fixer according to GOST 2817−50. Allowed the use of the photographic material of another composition.

Ethyl alcohol according to GOST 5962−67*.
_________________
* On the territory of the Russian Federation GOST R 51652−2000. — Note the manufacturer’s database.

Nitric acid GOST 4461−77, H. h surpassed.

Lead oxide, h. d. a. according to GOST 9199−77.

Tin oxide, h. d. a. according to GOST 22516−77.

Antimony 3-oxide, h.d. a.

Copper oxide, h. d. a. under GOST 16539−79.

Aluminium oxide, C. D. and.

Zinc oxide, h. d. a. according to GOST 10262−73.

Bismuth oxide, h. d. a. according to GOST 10216−75.

Iron oxide, h. d. a. according to GOST 4173−77.

Arsenic oxide, h.d. a.

Nickel oxide, h. d. a. according to GOST 4331−78.

(Changed edition, Rev. N 1, 2).

3. PREPARATION FOR ASSAY

3.1. The preparation of calibration samples

For the spectral analysis of tin-lead solders requires 7 sets of calibration samples:

I kit — based on corresponding solder POS 60 for the analysis of solders 61 POS; POS 61M; Piss 61−0,5;

II kit is based on the corresponding solder POS 40 for the analysis of solders 40 PIC; Piss 40−0,5; Piss 40−2;

III kit — based on corresponding solder POS 10 for the analysis of solders POS 10; 10−2 Piss; Piss 8−3;

IV set based on corresponding solder POS 50 for the analysis of solders AS 50−18; Piss 50−0,5;

V kit — based on corresponding solder POS 30 for the analysis of solders Piss 35−0,5; 35−2 Piss; Piss 30−0,5; 30−2 Piss; Piss 25−0,5; Piss 25−2;

VI set based on corresponding solder POS 18 for the analysis of solders 18−2 Piss; Piss 15−2; Poss 18−0,5;

VII kit — based on corresponding solder POS 5 for the analysis of solders 5−1 Piss; Piss 4−6.

Basis for the preparation of calibration samples is a mixture of appropriate amounts of the oxides of lead and tin.

In the main sample, containing 1% impurity of copper, aluminum, zinc, bismuth, iron, arsenic, Nickel, and 5% admixture of antimony, calculated on the metal, the latter is administered in the form of oxides or salts. The sample was stirred with ethanol in an agate mortar, then dried, calcined and thoroughly mixed.

Workers of the calibration samples is prepared by successive dilution of each previous sample of the corresponding basis. Prepare a series of samples with a mass fraction of from 0.2 to 0.001% of copper, bismuth, arsenic, iron, Nickel, zinc, aluminium; from 2 to 0.1% lead.

(Changed edition, Rev. N 2).

4. ANALYSIS

4.1. The analysis of solders, except for the determination of zinc

Weighed samples of the solder mass of 0.5−1 g was placed in a conical flask or a glass, pour 15−20 cmof nitric acid, diluted 1:1. The sample is dissolved with moderate heating. The solution was evaporated to dryness, and then calcined, the resulting nitrate salt in a muffle furnace for 20 minutes at a temperature of 450−500 °C. Obtained by dissolving and calcining the precipitate of metal oxides are thoroughly mixed with carbon powder in a ratio of 1:1, fill in craters of the carbon electrodes, having a size of 3x3 mm, buried with alcohol and dried in a drying Cabinet. When spectrographically electrodes are placed so that the bottom electrode was the electrode with the sample, the upper electrode is coal, sharpened to a truncated cone with the diameter of the pad is 1.5−2 mm. Spectra excited in the arc AC 10−12 A. the exposure Time, an intermediate aperture, the width of the gap and the analytical gap choose the best for obtaining intensity spectra at normal pochernenija. Spectra recorded on two albums — the shortwave part of the type SP-II, far — type SP-I. the Spectra of the samples for calibration and each sample is photographed on the same photographic plate.

The time of the plate: 3 min for type SP-I and 4 min for type SP-II at the temperature of the developer 19±1 °C.

4.2. The analysis of solders in the determination of zinc

Calibration samples and control samples (no coal powder) Packed in craters of the carbon electrodes, having a size of 3x3 mm, buried with alcohol and dried in a drying Cabinet. When spectrographically electrodes are placed so that the lower electrode — anode was the electrode with the sample, the upper electrode is coal, sharpened to a truncated cone with the diameter of the pad is 1.5−2 mm. Spectra excited in the arc DC 7 A. the exposure Time, an intermediate aperture, the width of the gap and the analytical gap choose the best for obtaining intensity spectra at normal pochernenija. Spectra of the samples for calibration and each sample is photographed on the same photographic plate. The analytical gap of 2 mm. the time of the plate 3 min at developer temperature of 19±1 °C.

Spectra recorded on the disc type SP-I.

4.1, 4.2. (Changed edition, Rev. N 2).

5. PROCESSING OF THE RESULTS

5.1. Analytical lines and «internal standard» are given in table.1.

Table 1

The results of electrophoretic spectra of the calibration samples to build calibration graphs in the coordinate .

The contents of the designated impurities and zinc find on the charts.

(Changed edition, Rev. N 1).

5.2. Allowable absolute differences the results of the analysis at a confidence level of 0.95, should not exceed the values given in table.2.

Table 2

(Changed edition, Rev. N 1, 2).