By visiting this site, you accept the use of cookies. More about our cookie policy.

GOST 1429.13-77

GOST R ISO 15353-2014 GOST P 55080-2012 GOST R ISO 16962-2012 GOST R ISO 10153-2011 GOST R ISO 10280-2010 GOST R ISO 4940-2010 GOST R ISO 4943-2010 GOST R ISO 14284-2009 GOST R ISO 9686-2009 GOST R ISO 13899-2-2009 GOST 18895-97 GOST 12361-2002 GOST 12359-99 GOST 12358-2002 GOST 12351-2003 GOST 12345-2001 GOST 12344-88 GOST 12350-78 GOST 12354-81 GOST 12346-78 GOST 12353-78 GOST 12348-78 GOST 12363-79 GOST 12360-82 GOST 17051-82 GOST 12349-83 GOST 12357-84 GOST 12365-84 GOST 12364-84 STATE STANDARD P 51576-2000 GOST 29117-91 GOST 12347-77 GOST 12355-78 GOST 12362-79 GOST 12352-81 GOST P 50424-92 STATE STANDARD P 51056-97 GOST P 51927-2002 GOST P 51928-2002 GOST 12356-81 GOST R ISO 13898-1-2006 GOST R ISO 13898-3-2007 GOST R ISO 13898-4-2007 GOST R ISO 13898-2-2006 STATE STANDARD P 52521-2006 GOST P 52519-2006 GOST R 52520-2006 GOST P 52518-2006 GOST 1429.14-2004 GOST 24903-81 GOST 22662-77 GOST 6012-2011 GOST 25283-93 GOST 18318-94 GOST 29006-91 GOST 16412.4-91 GOST 16412.7-91 GOST 25280-90 GOST 2171-90 GOST 23401-90 GOST 30642-99 GOST 25698-98 GOST 30550-98 GOST 18898-89 GOST 26849-86 GOST 26876-86 GOST 26239.5-84 GOST 26239.7-84 GOST 26239.3-84 GOST 25599.4-83 GOST 12226-80 GOST 23402-78 GOST 1429.9-77 GOST 1429.3-77 GOST 1429.5-77 GOST 19014.3-73 GOST 19014.1-73 GOST 17235-71 GOST 16412.5-91 GOST 29012-91 GOST 26528-98 GOST 18897-98 GOST 26529-85 GOST 26614-85 GOST 26239.2-84 GOST 26239.0-84 GOST 26239.8-84 GOST 25947-83 GOST 25599.3-83 GOST 22864-83 GOST 25599.1-83 GOST 25849-83 GOST 25281-82 GOST 22397-77 GOST 1429.11-77 GOST 1429.1-77 GOST 1429.13-77 GOST 1429.7-77 GOST 1429.0-77 GOST 20018-74 GOST 18317-94 STATE STANDARD P 52950-2008 GOST P 52951-2008 GOST 32597-2013 GOST P 56307-2014 GOST 33731-2016 GOST 3845-2017 STATE STANDARD P ISO 17640-2016 GOST 33368-2015 GOST 10692-2015 GOST P 55934-2013 GOST P 55435-2013 STATE STANDARD P 54907-2012 GOST 3845-75 GOST 11706-78 GOST 12501-67 GOST 8695-75 GOST 17410-78 GOST 19040-81 GOST 27450-87 GOST 28800-90 GOST 3728-78 GOST 30432-96 GOST 8694-75 GOST R ISO 10543-99 GOST R ISO 10124-99 GOST R ISO 10332-99 GOST 10692-80 GOST R ISO 17637-2014 GOST P 56143-2014 GOST R ISO 16918-1-2013 GOST R ISO 14250-2013 GOST P 55724-2013 GOST R ISO 22826-2012 GOST P 55143-2012 GOST P 55142-2012 GOST R ISO 17642-2-2012 GOST R ISO 17641-2-2012 GOST P 54566-2011 GOST 26877-2008 GOST R ISO 17641-1-2011 GOST R ISO 9016-2011 GOST R ISO 17642-1-2011 STATE STANDARD P 54790-2011 GOST P 54569-2011 GOST P 54570-2011 STATE STANDARD P 54153-2010 GOST R ISO 5178-2010 GOST R ISO 15792-2-2010 GOST R ISO 15792-3-2010 GOST P 53845-2010 GOST R ISO 4967-2009 GOST 6032-89 GOST 6032-2003 GOST 7566-94 GOST 27809-95 GOST 22974.9-96 GOST 22974.8-96 GOST 22974.7-96 GOST 22974.6-96 GOST 22974.5-96 GOST 22974.4-96 GOST 22974.3-96 GOST 22974.2-96 GOST 22974.1-96 GOST 22974.13-96 GOST 22974.12-96 GOST 22974.11-96 GOST 22974.10-96 GOST 22974.0-96 GOST 21639.9-93 GOST 21639.8-93 GOST 21639.7-93 GOST 21639.6-93 GOST 21639.5-93 GOST 21639.4-93 GOST 21639.3-93 GOST 21639.2-93 GOST 21639.0-93 GOST 12502-67 GOST 11878-66 GOST 1763-68 GOST 13585-68 GOST 16971-71 GOST 21639.10-76 GOST 2604.1-77 GOST 11930.7-79 GOST 23870-79 GOST 11930.12-79 GOST 24167-80 GOST 25536-82 GOST 22536.2-87 GOST 22536.11-87 GOST 22536.6-88 GOST 22536.10-88 GOST 17745-90 GOST 26877-91 GOST 8233-56 GOST 1778-70 GOST 10243-75 GOST 20487-75 GOST 12503-75 GOST 21548-76 GOST 21639.11-76 GOST 2604.8-77 GOST 23055-78 GOST 23046-78 GOST 11930.11-79 GOST 11930.1-79 GOST 11930.10-79 GOST 24715-81 GOST 5639-82 GOST 25225-82 GOST 2604.11-85 GOST 2604.4-87 GOST 22536.5-87 GOST 22536.7-88 GOST 6130-71 GOST 23240-78 GOST 3242-79 GOST 11930.3-79 GOST 11930.5-79 GOST 11930.9-79 GOST 11930.2-79 GOST 11930.0-79 GOST 23904-79 GOST 11930.6-79 GOST 7565-81 GOST 7122-81 GOST 2604.3-83 GOST 2604.5-84 GOST 26389-84 GOST 2604.7-84 GOST 28830-90 GOST 21639.1-90 GOST 5640-68 GOST 5657-69 GOST 20485-75 GOST 21549-76 GOST 21547-76 GOST 2604.6-77 GOST 22838-77 GOST 2604.10-77 GOST 11930.4-79 GOST 11930.8-79 GOST 2604.9-83 GOST 26388-84 GOST 14782-86 GOST 2604.2-86 GOST 21639.12-87 GOST 22536.8-87 GOST 22536.0-87 GOST 22536.3-88 GOST 22536.12-88 GOST 22536.9-88 GOST 22536.14-88 GOST 22536.4-88 GOST 22974.14-90 GOST 23338-91 GOST 2604.13-82 GOST 2604.14-82 GOST 22536.1-88 GOST 28277-89 GOST 16773-2003 GOST 7512-82 GOST 6996-66 GOST 12635-67 GOST 12637-67 GOST 12636-67 GOST 24648-90

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 cmГОСТ 1429.13-77 Припои оловянно-свинцовые. Спектральный метод определения примесей сурьмы, меди, висмута, мышьяка, железа, никеля, цинка, алюминия с использованием синтетических градуировочных образцов (с Изменениями N 1, 2)of 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 designated element Analytical lines, nm The line «internal standard» Sn, nm
Arsenic 234,9
Background
Antimony 287,7
278,5
Bismuth 306,7
322,3 or 311,8
Copper 327,3
322,3 or 311,8
Iron 302,0
322,3 or 311,8
Aluminium 308,2
322,3 or 311,8
Nickel 305,0
322,3 or 311,8
Zinc 330,2
322,0 or
  345,5
background



The results of electrophoretic spectra of the calibration samples to build calibration graphs in the coordinate ГОСТ 1429.13-77 Припои оловянно-свинцовые. Спектральный метод определения примесей сурьмы, меди, висмута, мышьяка, железа, никеля, цинка, алюминия с использованием синтетических градуировочных образцов (с Изменениями N 1, 2).

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 ГОСТ 1429.13-77 Припои оловянно-свинцовые. Спектральный метод определения примесей сурьмы, меди, висмута, мышьяка, железа, никеля, цинка, алюминия с использованием синтетических градуировочных образцов (с Изменениями N 1, 2)of 0.95, should not exceed the values given in table.2.

Table 2

     
The designated element The content of element, % The acceptable absolute differences, %
Antimony 0,1−0,3
0,03
  0,3−0,5
0,1
  0,5−1,0
0,2
  1,0−2,0 0,4
Copper 0,001−0,003
About 0.0006
  0,003−0,005
0,002
  0,005−0,01
0,003
  0,01−0,03
0,006
  0,03−0,05
0,01
  0,05−0,1
0,02
Bismuth 0,001−0,003
About 0.0006
  0,003−0,005
0,002
  0,005−0,01
0,003
  0,01−0,03
0,006
  0,03−0,05
0,01
  0,05−0,1
0,02
  0,1−0,2
0,03
Iron 0,001−0,003
About 0.0006
  0,003−0,005
0,002
  0,005−0,01
0,003
  0,01−0,02
0,006
Nickel 0,001−0,003
About 0.0006
  0,003−0,005
0,002
  0,005−0,01
0,003
  0,01−0,03
0,006
  0,03−0,05
0,01
  0,05−0,08
0,02
Aluminium 0,001−0,002
About 0.0006
Arsenic 0,005−0,01
0,003
  0,01−0,03
0,006
  0,03−0,05
0,01
Zinc 0,001−0,002
About 0.0006



(Changed edition, Rev. N 1, 2).