GOST 1429.1-77

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  ГОСТ 1429.1-77

GOST 1429.1−77 Solders tin-lead. Methods for determination of antimony (with Amendments No. 1, 2)

GOST 1429.1−77*

Group B59

STATE STANDARD OF THE USSR

SOLDERS TIN-LEAD

Methods for determination of antimony

Tin-lead solders.
Methods for the determination of antimony*

AXTU 1709**
_________________
* The name of the standard. Changed the wording, Rev. N 2.
** Code standard. Introduced later, 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 N 327 the term of validity extended until 01.01.88**
_____________
** Expiration removed Protocol MGS (IUS N 2, 1993). — Note the manufacturer’s database.

REPLACE GOST 1429.1−69

* REPRINT March 1983 with the Change in N 1, approved in January 1983; Post. N 324 from 21.01.83 (ICS 5−1983).

The Change N 2 approved and put into effect by the Decree of the USSR State Committee for standards from 30.06.87 N 3015 with 01.02.88

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

This standard specifies methods for determining the mass fraction of antimony in tin-lead solder alloys: extraction-photometric (with mass fraction of antimony from 0.002 to 0.5%) and three-dimensional bromatometric (when the mass fraction of antimony from 0.5 to 6%).

(Changed edition, Rev. N 2).

1. GENERAL REQUIREMENTS

1.1. General requirements for methods of analysis GOST 1429.0−77.

2. EXTRACTION-PHOTOMETRIC METHOD for the DETERMINATION of ANTIMONY (in mass fraction of antimony from 0.002 to 0.5%)

______________
* The name of the section. Changed the wording, Rev. N 2.

2.1. The essence of the method.

The method is based on extraction with toluene of hexachlorobuta brilliant green and measuring the optical density of the extract.

2.2. Apparatus, reagents and solutions

Photoelectrocolorimeter or spectrophotometer.

Sulfuric acid according to GOST 4204−77.

Hydrochloric acid by the GOST 3118−77, diluted 3:1.

Tin dichloride according to GOST 36−78, a solution with a mass fraction of 10%, prepared in concentrated hydrochloric acid.

Sodium atomistically according to GOST 4197−74, a solution with a mass fraction of 10%.

Urea according to GOST 6691−77, saturated solution; prepared as follows: 100 g of urea dissolved in 100 cmof hot water.

Brilliant green aqueous solution with a mass fraction of 0.1%.

Toluene according to GOST 5789−78.

Sodium sulphate anhydrous according to GOST 4166−76.

Antimony stamps su-00 GOST 1089−82.

Standard solutions of antimony.

Solution a (basic); prepared as follows: 0.1 g of metallic antimony is dissolved by heating in 5 cmof concentrated sulfuric acid, cooled and diluted with 20 cmof hydrochloric acid, diluted 3:1. The solution is again cooled, transferred into a measuring flask with volume capacity of 1000 cm, adjusted to the mark with hydrochloric acid, diluted 3:1 and thoroughly mixed. 1 cmof the solution contains 0.0001 g of antimony.

Solution B is prepared as follows: 10 cmof the solution And transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with hydrochloric acid, diluted 3:1, and stirred. 1 cmof solution B contains 0,00001 g of antimony. Solution B is prepared on the day of application.

(Changed edition, Rev. N 2).

2.3. Analysis.

2.3.1. Attachment of the solder mass 0.5 g (when the mass fraction of antimony from 0.002 to 0.1%) or 0.2 g (for a mass fraction of antimony from 0.1 to 0.5%) were placed in a glass with a capacity of 100 cm, pour 5 cmof concentrated sulfuric acid and dissolved by heating.

Upon dissolution of the main mass of sample should be avoided high temperature, and then increase the heat for removal of sulfur from the walls of the glass. After sulfur removal can enjoy a glass watch glass and heated until complete decomposition of sample.

A glass of cool, add 50 cmof hydrochloric acid, diluted 3:1, slightly heated to dissolve the salts, cooled and transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with hydrochloric acid, diluted 3:1, and stirred.

Take 10 cmof the solution (at a mass fraction of antimony from 0.002 to 0.1%) or 5 cm(with a mass fraction of more than 0.1 to 0.5%) and placed in a beaker with a capacity of 100 cm. Then add in a drop of a solution of dichloride of tin, mix and leave for 1 min, injected 1 cmof solution azotistykh sodium, mixed well and left for 5 min, the solution poured an equal volume of water, 1 cmof a saturated urea solution, mixed for 15 s and transferred to a separatory funnel with a capacity of 150 or 200 cm. The contents of the funnel was diluted with water (washing her glass several times) to a volume of 100 cm, were selected if aliquota part 10 cm, or 50 cm, were selected if aliquota part 5 sm.

To the solution in separating funnel pour 1 cmof solution of brilliant green, 30 cmof toluene and extracted for 1 min. After separation of phases the lower aqueous layer discarded. Filter paper drain tube separating funnel from droplets of moisture and poured the toluene layer in a dry volumetric flask with a capacity of 50 cm, which contribute 0.3 g of anhydrous sodium sulfate. Bring to mark with toluene, close the bottle glass glass stopper and stirred. After 10 minutes measure the optical density on a photoelectrocolorimeter with a red light filter (wavelength 656 nm) in a cuvette with a layer thickness of 1 cm.

A solution of comparison used toluene.

At the same time through the analysis of spend control experience.

Mass fraction of antimony found by the calibration schedule, taking into account the correction for the reagents.

2.3.2. Construction of calibration curve

In glasses with a capacity of 100 cmeach placed 0; 0,5; 1,0; 2,0; 4,0; 6,0 cmstandard solution B and dilute to 10 cmof hydrochloric acid, diluted 3:1. Further analysis is carried out as specified in clause 2.3.1.

The found values of optical density of solutions and their corresponding weight fractions of antimony building a calibration curve, taking into account the correction for the reagents.

2.3.1, 2.3.2. (Changed edition, Rev. N 2).

2.4. Processing of the results

2.4.1. Mass fraction of antimony () in percent is calculated by the formula

,

where is the mass of antimony, was found in the calibration schedule g;

100 — volume of the test solution, cm;

 — volume aliquote part of the solution, cm;

 — the weight of the portion,

(Changed edition, Rev. N 2).

2.4.2. Allowable absolute differences the results of the analysis at a confidence level of 0.95, should not exceed the values given in table.1.

Table 1

(Changed edition, Rev. N 1, 2)

3. BROMATOMETRIC VOLUMETRIC METHOD FOR THE DETERMINATION OF THE MASS FRACTION OF ANTIMONY (0,5−6%)

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* The name of the section. Changed the wording, Rev. N 2.

3.1. The essence of the method.

The method is based on dissolving the sample in sulfuric acid with subsequent titration of the amount of antimony and arsenic with potassium bromate in cernogolovka the solution using methyl orange as indicator.

3.2. Reagents and solutions

Sulfuric acid according to GOST 4204−77.

Hydrochloric acid by the GOST 3118−77.

Note. On titration 20 cmof hydrochloric acid should not be consumed more than 0.1 cmpolnovatogo potassium.


Methyl orange (4'-dimethylaminoazobenzene-4-sulfonic acid sodium salt), 0,1% solution.

Antimony stamps su-00 GOST 1089−82.

Potassium branovitsky according to GOST 4457−74, solution concentration (1/6КВгО)=0,025 mol/l; prepared as follows: 0,6854 polnovatogo g of potassium is dissolved in water, transferred to a measuring flask with volume capacity of 1000 cm, adjusted to the mark with water and mix.

(Changed edition, Rev. N 2).

3.3. Analysis

3.3.1. A portion of the solder mass 0.5 g is placed in a conical flask with a capacity of 250 cm, flow 20 cmof concentrated sulfuric acid, heated, avoiding high temperature. After dissolution of the main mass of sample flask content is heated at high temperature for removal of sulfur from the walls of the flask. Then close down the watch glass and heated until complete decomposition of sample and whitening of the sludge. The flask is cooled, carefully while stirring the solution pour 50 cmof water on the wall of the flask, 10 cmof concentrated acid. The contents of the flask were stirred and boiled for 10 min. In a flask, add 50 cmof cold water, 2 drops of methyl orange and titrated the solution of antimony potassium polnovatogo with careful stirring until the disappearance of the pink coloration of the solution.

At the same time through the analysis of spend control experience and amend the titration results.

3.3.2. The installation of the mass concentration of the solution polnovatogo potassium.

Four to five flasks with a capacity of 250 cmis placed 0.05 g powdered metallic antimony, poured 20 cmof concentrated sulfuric acid and dissolved by heating. Then the flask was cooled, poured carefully with stirring, 50 cmwater, 10 cmof concentrated hydrochloric acid, stirred and boiled for 10 min. In a flask, add 50 cmof cold water, two drops methyl orange and titrate with a solution of potassium polnovatogo with careful stirring until the disappearance of the pink color.

The mass concentration of a solution of potassium polnovatogo expressed in g/cmof antimony, calculated by the formula

,

where  — the weight of the portion of metallic antimony, g;

the volume of the solution polnovatogo potassium consumed in the titration of antimony, cm;

the volume of the solution polnovatogo potassium consumed for titration of the control experience, cm.

3.3.1, 3.3.2. (Changed edition, Rev. N 2).

3.4. Processing of the results

3.4.1. Mass fraction of antimony () in percent is calculated by the formula*

,

where  — volume of the solution polnovatogo potassium consumed in the titration of sample solution, cm;

the volume of the solution polnovatogo potassium consumed for titration of the solution in the reference experiment, cm;

 — mass concentration polnovatogo potassium, expressed in g/cmof antimony;

 — the mass of sample, g;

 — mass fraction of arsenic in the sample under study, determined from a separate sample, %;

1,625 is the ratio of the mass fraction of arsenic for antimony.
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When determining antimony in very small mass fractions of arsenic (thousandths of a percent) of pranevich

b.

3.4.2. 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

3.4.1, 3.4.2. (Changed edition, Rev. N 2).