GOST 22974.9-96

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  ГОСТ 22974.9-96

GOST 22974.9−96 fused welding Fluxes. Methods for determination of titanium oxide (IV)

GOST 22974.9−96

Group B09

INTERSTATE STANDARD

FUSED WELDING FLUXES

Methods for determination of titanium oxide (IV)

Melted welding fluxes. Methods of titanium oxide (IV) determination

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 22974.9−96 introduced directly as state standard of the Russian Federation from January 1, 2000

4 REPLACE GOST 22974.9−85

1 Scope

This standard establishes photometric methods for determination of titanium oxide (IV) with diantipyrylmethane and with chromotrope acid at a content of from 0.5 to 10% and hydrogen peroxide at a content of from 7 to 40%.

2 Normative references

The present standard features references to the following standards:

GOST 199−78 Sodium acetate 3-water. Specifications

GOST 3118−77 hydrochloric Acid. Specifications

GOST 4204−77 sulfuric Acid. Specifications

GOST 4208−72 Salt oxide and ammonium double sulfate (salt Mora). Specifications

GOST 4461−77 nitric Acid. Specifications

GOST 6552−80 orthophosphoric Acid. Specifications

GOST 7172−76 Potassium preservatory. Specifications

GOST 10929−76 Hydrogen peroxide. Specifications

GOST 19807−91 Titanium and titanium alloy wrought. Brand

GOST 22180−76 oxalic Acid. Specifications

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

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

3 General requirements

General requirements for methods of analysis GOST 22974.0.

4 Photometric method for the determination of titanium oxide (IV) with diantipyrylmethane

4.1 the essence of the method

The method is based on the interaction in acidic medium with a tetravalent titanium diantipyrylmethane with the formation of the complex compound, painted in Golden yellow color. Optical density of the solution measured on a spectrophotometer at a wavelength of 480 nm or photoelectrocolorimeter with a green filter.

4.2 Equipment, reagents and solutions

Spectrophotometer or photoelectrocolorimeter.

Nitric acid according to GOST 4461.

Sulfuric acid according to GOST 4204, solutions of the mass concentrations of 0.05 g/cmand 0.1 g/cmand diluted 1:4.

Hydrochloric acid according to GOST 3118, density of 1.19 g/cmand diluted 1:1.

Potassium preservatory according to GOST 7172.

Sodium acetate 3-water according to GOST 199, solution mass concentration of 0.05 g/cm.

Titanium dioxide.

Titanium metal according to GOST 19807.

Ascorbic acid, a solution of mass concentration of 0.05 g/cm.

Paper of the Congo.

Diantipyrylmethane, solution mass concentration of 0.01 g/cm: 10 g diantipyrylmethane and 5 g of ascorbic acid was placed in a volumetric flask with a capacity of 1000 cm, pour in 150 cmof water and carefully 15 cmsulphuric acid of density 1.84 g/cm, heated to dissolve the sample, cool and add water to the mark. The solution is filtered on a filter «white ribbon».

Standard solutions of titanium oxide.

Solution a: 1 g svejeprigotovlennogo of titanium dioxide at a temperature of 1000 °C melted in a platinum Cup with 10 g of potassium peacemaking to enlightenment of the melt at a temperature of 800−900 °C. the Cooled melt is dissolved in 50 cmof sulfuric acid mass concentration of 0.1 g/cm, transferred to a measuring flask with volume capacity of 1000 cm, made up to the mark with sulfuric acid mass concentration of 0.05 g/cmand stirred. 0,5995 g of titanium sponge was dissolved with heating in 50 cmof sulphuric acid (1:4) in a flask with a capacity of 250 cm, covered with watch glass. Upon dissolution of the sample titanium solution is oxidized to bleaching with nitric acid and evaporated to release thick vapors of sulfuric acid. The solution was cooled, poured 50 cmof the sulphuric acid solution of the mass concentration of 0.05 g/cm, transferred to a measuring flask with volume capacity of 1000 cmand the same acid was adjusted to the mark.

Solution a has a mass concentration of titanium oxide (IV) 0,001 g/cm.

Solution B: 10 cmsolution And transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with sulfuric acid mass concentration of 0.05 g/cmand stirred.

Solution B has a mass concentration of titanium oxide

(IV) 0.0001 g/cm.

4.3 analysis

4.3.1 After the decomposition of the flux by melting according to GOST 22974.1 25 cmbasic solution is placed in a beaker with a capacity of 300−400 cm, add 5 cmof concentrated nitric acid, carefully pour 10 cmof concentrated sulfuric acid and is evaporated to dense fumes of sulfuric acid. The glass solution was cooled, washed with water wall of glass and the evaporation is repeated again, then the solution in the glass is again cooled, poured 100 cmof water and heated until complete dissolution of sulfate salts. The contents of the beaker transferred to a volumetric flask with a capacity of 250 cm, made up to the mark with water and mix.

Select aliquot part of the solution of 5−20 cm(depending on the content of titanium oxide in the flux) in a volumetric flask with a capacity of 100 cm, neutralized with sodium acetate solution until the pink color of Congo paper, and then added dropwise a solution of hydrochloric acid (1:1) until the color of Congo paper blue. Add 5 cmof ascorbic acid solution and leave on for 10−15 minutes until full recovery of iron. Then add 10 cmof hydrochloric acid density of 1.19 g/cmfor destruction of the coloured compounds formed by titanium with ascorbic acid, add 25 cmof the solution diantipyrylmethane, adjusted to the mark with water and mix. After 30−50 min, measure the optical density on the spectrophotometer to a wavelength of 480 nm or photoelectrocolorimeter with a green optical filter in a ditch with thickness of the absorbing layer is 50 mm. as a solution comparison using the solution in the reference experiment, carried out through all stages of the analysis. The weight of the titanium oxide (IV) find the calibration gr

the Afik.

4.3.2 After the decomposition of the flux by dissolving in acids according to GOST 22974.1 25 cmbasic solution is transferred to a volumetric flask with a capacity of 250 cm, made up to the mark with water and mix.

Select aliquot part of the solution 5−20 cm, and further analysis is carried out for 4.3.1.

4.4 Construction of calibration curve

In six volumetric flasks with a capacity of 100 cmconsistently make 0,5; 1,0; 2,0; 3,0; 4,0 and 5,0 cmstandard solution B, which corresponds to 0,00005; 0,0001; 0,0002; 0,0003; of 0.0004 and 0.0005 g of titanium oxide (IV). In the seventh flask standard solution of titanium oxide (IV) is not added. Add 5 cmof ascorbic acid and further analysis is carried out for 4.3.1.

Solution comparison is the solution, in which there is a standard solution of titanium oxide (IV).

4.5 Processing of results

4.5.1 the Mass percent of titanium oxide (IV) , %, is calculated by the formula

, (1)

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

 — the weight of the portion of the flux corresponding to aliquote part of the solution,

4.5.2 Standards of accuracy and standards for monitoring the accuracy of determining the mass fraction of titanium oxide (IV) is given in table 1.


Table 1

Percentage

5 Photometric method for the determination of titanium oxide (IV) with chromotrope acid

5.1 the essence of the method

The method is based on the formation of complex compounds of titanium with chromotrope acid, colored depending on the concentration of titanium from yellow to red-brown color. The optical density measured on the spectrophotometer at a wavelength of 453 nm or photoelectrocolorimeter with a green filter.

5.2 Equipment, reagents and solutions

Spectrophotometer or photoelectrocolorimeter.

Sulfuric acid according to GOST 4204, solutions of the mass concentrations of 0.05 g/cm, 0.1 g/cmand diluted 1:4.

Salt of iron (II) and ammonium double sulfate (salt Mora) according to GOST 4208, solution mass concentration of 0.04 g/cm(40 g of salt Mora is dissolved in 900 cm. of water. After complete dissolution of salt Mora add 100 cmof concentrated sulfuric acid).

Potassium preservatory according to GOST 7172.

Oxalic acid according to GOST 22180, solution mass concentration of 0.05 g/cm.

Chromotrope acid disodium salt: 3 g dissolved in 100 cmof water.

Titanium metal according to GOST 19807.

Standard solutions of titanium oxide (IV) are prepared according to 4.2

.

5.3 analysis

After the decomposition flux according to GOST 22974.1 25 cmof the solution was placed in a beaker with a capacity of 300−400 cm, add 5 cmof concentrated nitric acid, carefully pour 10 cmof concentrated sulfuric acid and is evaporated to dense fumes of sulfuric acid. The glass solution was cooled, washed well with water the walls of the beaker and evaporated, then the contents of the glass again cooled, poured 100 cmof water and heated until complete dissolution of sulfate salts. The contents of the beaker transferred to a volumetric flask with a capacity of 250 cm, made up to the mark with water and mix well.

Select aliquot part of the solution is 10−50 cm(depending on the content of the titanium oxide (IV) in the flux) in a volumetric flask with a capacity of 100 cm, add 10 cmof salt solution Mora, 20 cmof a solution of oxalic acid, 4 cmchromotrope acid (after addition of each reagent is well mixed), adjusted to the mark with water and measure the optical density on the spectrophotometer to a wavelength of 453 nm or photoelectrocolorimeter with a green optical filter in a ditch with thickness of the absorbing layer 30 mm. as a solution comparison solution is used in the reference experiment, carried out through all stages of the analysis. The weight of the titanium oxide (IV) find the calibration for gra

fico.

5.4 Construction of calibration curve

In a volumetric flask with a capacity of 100 cmconsistently contribute 1; 2; 3; 4; 5 and 6 cmstandard solution B, which corresponds to 0,0001; 0,0002; 0,0003; 0,0004; 0.0005 and 0.0006 g of titanium oxide (IV). In the seventh flask is added a standard solution of titanium oxide (IV). Add accordingly 9; 8; 7; 6; 5; 4 cmsulfuric acid mass concentration of 0.05 g/cm, and 10 cmof salt Mora and further analysis is carried out according to 5.3.

5.5 processing of the results

5.5.1 Mass fraction of titanium oxide (IV) , %, is calculated by the formula

, (2)

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

 — the weight of the portion of the flux corresponding to aliquote part of the solution,

5.5.2 Standards of accuracy and standards of accuracy of determining the mass fraction of titanium oxide (IV) is given in table 1.

6 Photometric method for the determination of titanium oxide (IV) with hydrogen peroxide

6.1 the essence of the method

The method is based on the ability of the titanium ions to form hydrogen peroxide in an acidic medium complex compound colored in yellow color. The interfering effect of ferric iron is removed by addition of a solution of phosphoric acid. Optical density of the solution measured on a spectrophotometer at a wavelength of 390 nm or photoelectrocolorimeter with a blue filter.

6.2 Apparatus, reagents and solutions

Spectrophotometer or photoelectrocolorimeter.

Nitric acid according to GOST 4461.

Orthophosphoric acid according to GOST 6552.

Sulfuric acid according to GOST 4204, diluted 1:4, and the mass concentration of 0.05 g/cm.

Hydrogen peroxide according to GOST 10929.

Titanium metal according to GOST 19807.

Titanium dioxide.

A standard solution of titanium oxide (IV) are prepared according to 4.2.

6.3 analysis

6.3.1 After the decomposition of the flux by melting according to GOST 22974.1 2−5 cmcore solution is placed in a beaker with a capacity of 200−250 cm, add 2−3 cmof concentrated nitric acid, carefully pour 10 cmof concentrated sulfuric acid and is evaporated to dense fumes of sulfuric acid. The glass solution was cooled, washed with water the walls of the beaker and evaporating again, and then solution into the beaker cool, add 20 cmof water to dissolve the sulfate salts and the solution transferred to a volumetric flask with a capacity of 100 cm. Pour 10 cmof sulphuric acid (1:4), 30 cmwater 2 cmof phosphoric acid, 5 cmof hydrogen peroxide, made up to the mark with water and mix. Optical density of the solution measured on a spectrophotometer at a wavelength of 390 nm or photoelectrocolorimeter with a blue filter in a cell with thickness of the absorbing layer 30 mm.

As a solution comparison solution is used in the reference experiment, conducted through the entire course of the analysis.

The weight of the titanium oxide (IV) find the calibration graph

the IR.

6.3.2 After acid decomposition flux according to GOST 22974.1 2−5 cmbasic solution is transferred to a volumetric flask with a capacity of 100 cm, flow 10 cmof sulphuric acid (1:4), 50 cmof water, 2 cmof phosphoric acid, 5 cmof hydrogen peroxide and further analysis is carried out according to 6.3.1.

6.4 Construction of calibration curve

In six volumetric flasks with a capacity of 100 cmmaking 0,5; 1,0; 1,5; 2,0; 2,5; 3,0 cmstandard solution A, which corresponds to 0,0005; 0,001; 0,0015; 0,0020; and 0,0030 0,0025 g of titanium oxide (IV). In the seventh flask make 3 cmof sulfuric acid mass concentration of 0.05 g/cm. Then pour 10 cmof sulphuric acid (1:4), 10 cmwater and 2 cmof phosphoric acid, 5 cmof hydrogen peroxide, made up to the mark with water and mix. Optical density of the solution measured on a spectrophotometer a wavelength of 390 nm or photoelectrocolorimeter thickness of the absorbing layer 30 mm. In a solution of comparison, using a solution in which not introduced a standard solution of titanium oxide (IV

).

6.5 processing of the results

6.5.1 Mass fraction of titanium oxide (IV) , %, is calculated by the formula

, (3)

where is the mass of titanium oxide (IV) was found in the calibration schedule g;

 — the weight of the portion of the flux corresponding to aliquote part of the solution,

6.5.2 the Norms of accuracy and norms of the accuracy of determining the mass fraction of titanium oxide (IV) is given in table 1.