GOST 22974.1-96

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  ГОСТ 22974.1-96

GOST 22974.1−96 fused welding Fluxes. Methods of flux decomposition

GOST 22974.1−96

Group B09

INTERSTATE STANDARD

FUSED WELDING FLUXES

Methods of flux decomposition

Melted welding fluxes. Methods of flux decomposition

ISS 77.040
AXTU 0809

Date of implementation 2000−01−01

Preface

1 DEVELOPED by the Interstate technical Committee for standardization MTK 72; the Institute of electric them. E. O. Paton of NAS of Ukraine

SUBMITTED to the State Committee of Ukraine for standardization, Metrology and certification

2 ADOPTED by the Interstate Council for standardization, Metrology and certification (Protocol No. 9 dated April 12, 1996)

The adoption voted:

3 Resolution of the State Committee of the Russian Federation for standardization and Metrology, dated April 21, 1999 N 134 inter-state standard GOST 22974.1−96 introduced directly as state standard of the Russian Federation from January 1, 2000

4 REPLACE GOST 22974.1−85

1 Scope

This standard specifies the methods of decomposition fluxes: the smelting and acid (for determination of mass fraction of manganese oxide (II), aluminum oxide, calcium oxide, magnesium oxide, iron (III) oxide, of phosphorus, of zirconium oxide and titanium oxide (IV).

2 Normative references

The present standard features references to the following standards:

GOST 3118−77 hydrochloric Acid. Specifications

GOST 4199−76 Sodium tetraborate 10-aqueous. Specifications

GOST 4204−77 sulfuric Acid. Specifications

GOST 4332−76 Potassium carbonate — sodium carbonate. Specifications

GOST 4461−77 nitric Acid. Specifications

GOST 7172−76 Potassium preservatory. Specifications

GOST 9656−75 boric Acid. Specifications

GOST 10484−78 hydrofluoric Acid. Specifications

GOST 11293−89 Gelatin food. Specifications

GOST 22974.0−96 fused welding Fluxes. General requirements for methods of analysis

3 General requirements

General requirements for methods of analysis GOST 22974.0.

4 the Method of decomposition fluxes by melting

4.1 the essence of the method

The method is based on the fusion of the flux linkage with a mixture of potassium carbonate — sodium carbonate and sodium tetraborate or boric acid, dissolving the melt in hydrochloric acid and separation of the formed silicic acid with gelatin.

4.2 Reagents and solutions

Sulfuric acid according to GOST 4204, diluted 1:1.

Hydrochloric acid according to GOST 3118, diluted 1:1 and 5:95.

Hydrofluoric acid according to GOST 10484.

Boric acid according to GOST 9656.

Potassium carbonate — sodium carbonate according to GOST 4332.

Potassium preservatory according to GOST 7172.

Sodium tetraborate 10-water according to GOST 4199 dehydrated: sodium tetraborate was placed in a platinum Cup in a muffle furnace slowly heated to 400−450 °C. Then the porous mass after cooling is ground and placed in a jar with a glass stopper.

Gelatin food according to GOST 11293, solution mass concentration of 0.01 g/cm.

The beach: mix five parts by weight of potassium carbonate — sodium carbonate and one part by weight of sodium tetraborate or boric acid.

4.3 Decomposition of the flux melting

4.3.1 the Linkage of flux with a mass of 0.5 g is fused with 6 g of flux in a platinum crucible with lid at a temperature of 950−1050 °C for 30 min. the Melt was poured on a polished plate of stainless steel. Crucible, cover and melt is placed in a beaker with a capacity of 300−400 cmand decompose in 50 cmof hydrochloric acid (1:1), covered with a glass glass. Out from a glass crucible and cover them thoroughly rinsed with water.

The resulting solution was evaporated before the salt extraction, is poured 10 cmof the gelatin solution and diluted to a volume of 50 cm.

The solution is stirred for 3−5 min with a glass rod and leave in a warm place at a temperature of 50−70 °C for 10−15 min.

The precipitate of silicic acid is filtered off, the filter «white ribbon», washed several times with hot hydrochloric acid (5:95) and several times with hot water (stock solution).

The sediment filter is placed in a platinum crucible, dried and calcined for 15−20 minutes at a temperature of 950−1050 °C. To the cooled crucible, add 5−10 drops of sulfuric acid (1:1), 5−8 cmhydrofluoric acid and evaporated to dryness. The dry residue is calcined at a temperature of 950−1050 °C for 3−5 min. the Residue in the crucible is fused with 2 g of potassium peacemaking at a temperature of 700−750 °C for 3−5 min. M dissolved in 5−10 cmof hydrochloric acid (1:1) and added to the main solution. The solution was transferred to a volumetric flask with a capacity of 250 cmof water and bring to mark. The solution is used for determining manganese oxide (II), iron (III) oxide, aluminum oxide, calcium oxide, magnesium oxide, zirconium oxide, titanium oxide (IV), and phosphorus.

5 the Method of acid decomposition fluxes

5.1 the essence of the method

The method is based on decomposition of fluxes in mixtures of perchloric or sulfuric, nitric and hydrofluoric acid in the removal of silicon in the form of crematoria.

5.2 Reagents and solutions

Nitric acid according to GOST 4461.

Sulfuric acid according to GOST 4204, diluted 1:1.

Hydrochloric acid according to GOST 3118, diluted 1:1.

Hydrofluoric acid according to GOST 10484.

Chloric acid, diluted 1:1.

Boric acid according to GOST 9656.

Acid chloride, saturated boric acid: 57% perchloric acid (1:1) or undiluted 36% is heated to 50−60 °C and saturated with boric acid.

Potassium preservatory according to GOST 7172.

5.3 Decomposition of the flux of perchloric acid

5.3.1 Weighed flux weighing 0.5 g is placed in a platinum Cup, moisten with water, add 30 cmof perchloric acid (1:1), 5 cmnitrogen and 10 cmhydrofluoric acids and evaporated to copious fumes of perchloric acid.

Wash with water the walls of the Cup, pour 10−20 cmof perchloric acid saturated with boric acid, and evaporated to dryness. The dry residue is calcined for 2−3 minutes at a temperature of 750−800 °C.

Calcined residue is fused with 4−5 g peacemaking potassium at a temperature of 750−800 °C for 3−5 min. M leached at 50 cmhydrochloric acid (1:1) under heating. The contents of the Cup is transferred to a volumetric flask with a capacity of 250 cmof water and bring to mark.

The solution is used for determining manganese oxide (II), iron (III) oxide, aluminum oxide, calcium oxide, magnesium oxide, zirconium oxide, titanium oxide (IV), and phosphorus.

5.4 Decomposition of the flux of sulfuric acid

5.4.1 the Linkage of flux with a mass of 0.5 g was placed in a platinum Cup, moisten with water, add 20 cmhydrofluoric acid, 10 cmof sulphuric acid (1:1). The contents of the Cup is heated to a decomposition of the sample, pour 5 cmof nitric acid and evaporated until the termination of allocation of steams of sulfuric acid. Residual sulfuric acid was removed, holding the Cup in a muffle at a temperature of 950−1050 °C for 2−3 min. a Cup of cooled, poured 50−60 cmof hydrochloric acid (1:1) and heated to dissolve the salts. If the bottom of the Cup will stay intact particles flux, their filtered off and fused with potassium pyroterrorism on 4.3.1. The solution was transferred to a volumetric flask with a capacity of 250 cmof water and bring to mark.

The solution is used for determining manganese oxide (II), iron (III) oxide, aluminum oxide, calcium oxide, magnesium oxide, phosphorus.