GOST R 51928-2002

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  ГОСТ Р 51928-2002

GOST R 51928−2002 Alloys and powders heat-resistant Nickel-based. Methods of boron determination

GOST R 51928−2002

Group B39

STATE STANDARD OF THE RUSSIAN FEDERATION

ALLOYS AND POWDERS HEAT-RESISTANT NICKEL-BASED

Methods of boron determination

Nickel-based fire-resistant alloys.
Methods for determination of boron

OKS 77.080
AXTU 0709

Date of introduction 2003−03−01

Preface

1 DEVELOPED AND SUBMITTED by the Technical Committee for standardization TC 145 «monitoring Methods of steel products"

2 ADOPTED AND put INTO EFFECT by the Resolution of Gosstandart of Russia from August 14, 2002 N 305-St

3 INTRODUCED FOR THE FIRST TIME

1 Scope

This standard establishes photometric methods for determination of boron: 4,4'-deoxyguanylate or 4,4'-dimethoxydimethylsilane in mass fraction of boron from 0.0005% to 0.03%; Al-resorcinol and tioninom in mass fraction of boron from 0.001% to 0.05%; curcumin in mass fraction of boron from 0.001% to 0.05% in superalloys and powder on a Nickel basis.

2 Normative references

The present standard features references to the following standards:

GOST 83−79 Sodium carbonate. Specifications

GOST 200−76 Sodium posterolaterally 1-water. Specifications

GOST 3117−78 Ammonium acetate. Specifications

GOST 3118−77 hydrochloric Acid. Specifications

GOST 3760−79 Ammonia water. Specifications

GOST 4204−77 sulfuric Acid. Specifications

GOST 4328−77 Sodium hydroxide. Specifications

GOST 4461−77 nitric Acid. Specifications

GOST 4463−76 Sodium fluoride. Specifications

GOST 6552−80 orthophosphoric Acid. Specifications

GOST 6563−75 technical articles made of noble metals and alloys. Specifications

GOST 9656−75 boric Acid. Specifications

GOST 10652−73 Salt is the disodium Ethylenediamine-N, N, N', N'-tetraoxane acid 2-water (Trilon B). Specifications

GOST 11125−84 nitric Acid of high purity. Specifications

GOST 14261−77 hydrochloric Acid of high purity. Specifications

GOST 14262−78 sulphuric Acid of high purity. Specifications

GOST 18270−72 acetic Acid of high purity. Specifications

GOST 20490−75 Potassium permanganate. Specifications

GOST 24147−80 aqueous Ammonia of high purity. Specifications

GOST 28473−90 Iron, steel, ferroalloys, chromium and manganese metal. General requirements for methods of analysis

GOST R 51652−2000 rectified ethyl Alcohol from food raw material. Specifications

3 General requirements

General requirements for methods of analysis GOST 28473.

4 Photometric method for the determination of boron with 4,4'-deoxyguanylate or 4,4'-dimethoxydimethylsilane in mass fractions of from 0.0005% to 0.03%

4.1 the essence of the method

The method is based on formation of colored complex compounds of boron with 4,4'-widespread-dibenzoylmethane or 4,4'-dimethoxydimethylsilane in the environment of glacial acetic and sulphuric acids in the presence of the organic phase.

Boron is pre-separated from the main components of the alloy by extraction of the chloroform solution of 2-isopropyl-5-methyl-1,3-hexanediol or 2,2,4-trimethyl-1,3-pentadione.

4.2 Equipment, reagents and solutions

Spectrophotometer or photoelectrocolorimeter with all accessories for measurements in the visible region of the spectrum.

a pH meter.

The platinum crucible according to GOST 6563.

The hydrochloric acid according to GOST 3118 or GOST 14261.

Nitric acid according to GOST 4461 or GOST 11125.

Sulfuric acid according to GOST 4204 or GOST 14262.

Sulphuric acid, diluted 1:1.

Orthophosphoric acid according to GOST 6552.

Acetic acid according to GOST 18270.

Inspection of acetic acid on the content of the aldehyde: to 20 cmof acetic acid are added 1 cmof solution of potassium permanganate.

In the absence of aldehyde the color of potassium permanganate should not disappear within 15 minutes, a brown coloration of manganese dioxide should also not appear.

Potassium permanganate according to GOST 20490, a solution of 1 g/DM.

Chloroform medical.

2-isopropyl-5-methyl-1,3-hexandiol (IPMG), the solution was diluted (1:19) in chloroform.

2,2,4-trimethyl-1,3-pentandiol (TMPD), a solution of 40 g/lin chloroform.

Ethyl alcohol according to GOST R 51652.

Sodium carbonate according to GOST 83.

4,4'-deoxyguanylate, a solution of 3.75 g/DMacetic acid: 0.375 g of 4,4'-dioxidine-solmetra dissolved in 100 cmof acetic acid at low heat, cool. When stored in a dark place, the solution is usable for one month.

Boric acid according to GOST 9656.

The standard solutions of boron.

Solution a: 5,7154 g of boric acid are dissolved in 300 cmof water in a volumetric flask with a capacity of 1 DM, made up to the mark with water and mix.

1 cmstandard solution contains 0.001 g of boron.

Solution B: 10 cmsolution And transferred to a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix.

1 cmstandard solution B contains 0.0001 g of boron.

Solution: 10 cmof a solution transferred to a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix. Prepare immediately before use.

1 cmstandard solution contains 0,00001 g

Bora.

4.3 analysis

4.3.1 the Procedure of sample dissolution

The weight of the portion of the alloy is 0.25−1 g in accordance with table 1 was placed in a quartz glass with a capacity of 100 cm, 30 cm, pour themixture of hydrochloric and nitric acids in the ratio 3:1 or 8:1, 2 cmof phosphoric acid, a glass cover made of PTFE and the sample is dissolved with moderate heating.


Table 1

After dissolution, the sample flow 10 cmof sulphuric acid (1:1).

The solution was evaporated prior to the allocation of steams of sulfuric acid, rinse the lid of PTFE, and the side of the Cup with water and again evaporated to fumes of sulfuric acid.

Salt dissolved in 5 cmof hydrochloric acid when heated, pour the 30−40 cmof water and heated until complete dissolution of salts. The insoluble residue is filtered through a dense filter in a quartz glass with a capacity of 200 cm, a glass rubbed with a small piece of filter wand with a rubber tip. A glass filter and washed several times with hot water. The filter is placed in a platinum crucible, incinerated, burned, and calcined at 600−700 °C. the Residue in the crucible is fused with 1 g of sodium carbonate at 950−1000 °C for 15−20 min. the Melt is dissolved in hot water, adding 1−2 cmof hydrochloric acid with mild heating, attached to the filtrate and evaporate the solution to 10−15 cm. Add a few drops of nitric acid and evaporated to release vapors of sulfuric acid.

4.3.2 Procedure to separate boron from the main alloy components

Salt is dissolved in 30 cmof water with the addition of 5 cmof hydrochloric acid under heating, cooled.

The solution is poured into a measuring flask with a capacity of 50−100 cm(table 1), made up to the mark with water and mix. The solution is filtered over a dry dense quartz filter in a dry flask, discarding first portion of filtrate.

Aliquot part of the solution (table 1) was placed in a separating funnel with a capacity of 50−100 cm, poured 10 cmof the solution IPMG or TMPD. Separatory funnel shaken for 1 min and after separation of the layers the organic layer, filter through dry cotton wool, poured into a dry volumetric flask with a capacity of 25 cm. The extraction is repeated. The organic layer is decanted into the same volumetric flask. The extract in the flask topped up to the mark solution IPMG or TMPD and stirred.

4.3.3 Spectrophotometric assay procedure

Aliquot part extract 1 cmis placed in a dry volumetric flask with a capacity of 25 cm, add 1 cmof a solution of 4,4'-dioxymethylene or 4,4'-dimethoxybenzophenone, mix, add 0.5 cmof sulphuric acid, mix and leave for 2−2,5 hours Then diluted with 25 cm ofethyl alcohol, mix. Measure the optical density of colored solution with spectrophotometer at a wavelength of 440 nm or photoelectrocolorimeter with a filter having a region of transmittance in the wavelength interval from 420 to 460 nm. The thickness of the light absorbing layer of the cell is chosen so to obtain the optimal value of optical density.

As a comparison, using a solution of water or ethanol.

A lot of find boron in the calibration schedule subject to amendments the reference experiment.

4.3.4 Construction of calibration curve

In quartz beakers with a capacity of 100 cmis placed a measured volume of a standard solution of boron B, are shown in table 2.


Table 2

All the glasses are poured acid as the dissolution of the sample, and then act in accordance with 4.3.1−4.3.3.

From the values of absorbance of analyzed solutions is subtracted the value of optical density in the reference experiment. On the found values of optical density and corresponding mass of the boron build the calibration graph.

5 Photometric method for the determination of boron with h-resorcinol and tioninom in mass fractions of from 0.001% to 0.05%

5.1 the essence of the method

The method is based on formation of colored complex compounds of boron with h-resorcinol and tioninom at pH 5.0 to 5.2.

Boron is pre-separated from the main components of the alloy by extraction of the chloroform solution of 2-isopropyl-5-methyl-1,3-hexanediol or 2,2,4-trimethyl-1,3-pentadione with subsequent reextraction with sodium hydroxide solution.

5.2 the Instrument, reagents and solutions

Acid hydrochloric, diluted 1:1.

Hydrochloric acid, solution of molar concentration 0.5 mol/DM.

Acetic acid, a solution of molar concentration 0.5 mol/DM.

Ammonia water according to GOST 3760 or GOST 24147.

Ammonia water, solution of molar concentration 0.5 mol/DM.

Buffer solution. Mix equal volumes of acetic acid and ammonia solution and set the pH 5.0 to 5.2 on pH-meter reagents by the addition of acetic acid or ammonia.

Sodium hydroxide according to GOST 4328.

Sodium hydroxide solution of molar concentration of 1.0 mol/DM.

Sodium hydroxide, a solution of 20 g/DM.

Al-resorcinol, disodium salt, solution molar concentration of 0.001 mol/DM.

0,0494 g, Al-resorcinol dissolved in 100 cmof water.

Tionin 2-water dye for microscopy, alcoholic solution of molar concentration of 0.001 mol/DM.

0,029 g thionine dissolved in 100 cmof ethanol.

Salt is the disodium Ethylenediamine-N, N, N', N'-tetraoxane acid 2-water (Trilon B) according to GOST 10652, a solution of molar concentration 0.05 mol/DM.

Of 1.86 g Trilon B dissolved in 100 cmof water.

The rest of the reagents, equipment and solutions — for 4.2.

5.3 analysis

5.3.1 Preparation of test solution

The weight of the portion of the alloy is 0.2−0.5 g in accordance with table 3 was placed in a quartz glass with a capacity of 100 cm, 30 cm, pour themixture of hydrochloric and nitric acids in the ratio 3:1 or 8:1, 2 cmof phosphoric acid, a glass cover made of PTFE and the sample is dissolved with moderate heating. After dissolution, the sample flow 8 cmof sulphuric acid (1:1).


Table 3

Then do as specified in 4.3.1.

5.3.2 Procedure to separate boron from the main alloy components

Salt is dissolved in 30 cmof water with the addition of 5 cmof hydrochloric acid under heating, cooled.

The solution is poured into a measuring flask with a capacity of 50−100 cm(table 3), made up to the mark with water and mix. The solution is filtered over a dry dense quartz filter in a dry flask, discarding first portion of filtrate.

Aliquot part of the solution is 20 cmis placed in a separating funnel with a capacity of 50 cm, 5−10 cm pour thesolution IPMG or TMPD. Separating funnel is shaken for 1−2 min. and after separation of the layers the organic layer drained into another separatory funnel with a capacity of 50 cm. The extract is washed for 30 with 10 cmof water, acidulated with hydrochloric or sulphuric acid (1 drop acid per 10 cmof water). The washed organic layer is drained into a third separatory funnel with a capacity of 50 cm, flow 10 cmof sodium hydroxide and conduct the Stripping of boron by shaking for 1−2 min. the Organic layer discarded.

The aqueous alkaline layer is drained into a glass with a capacity of 5

0 cm.

5.3.3 Spectrophotometric assay procedure

To subject the solution poured water up to 20 cm, 0.5 cmof the solution Trilon B, mix and set pH of 5.0 to 5.2 solutions of hydrochloric acid or sodium hydroxide for pH meter. Then add exactly 5 cmAl-resorcinol and 1 cmof thionine, the contents of the beaker transferred to a volumetric flask with a capacity of 50 cm, rinse walls of beaker with buffer solution, made up to the mark the same buffer solution and stirred.

After 18 hours, measure the optical density of colored solution with spectrophotometer at a wavelength of 510 nm or photoelectrocolorimeter in the range of wavelengths of 490−530 nm. The thickness of the light absorbing layer is chosen so to obtain the optimal value of optical density.

As a solution comparison solution is used in the reference experiment. A lot of find boron in the calibration schedule subject to amendments the reference experiment.

5.3.4 Construction of calibration curve

In quartz beakers with a capacity of 100 cmis placed a measured volume of a standard solution of boron shown in table 4.


Table 4

All the glasses are poured acid as the dissolution of the sample, and then act in accordance with 5.3.1 to 5.3.3.

On the found values of optical density and corresponding mass of the boron build the calibration graph.

6 Photometric method for the determination of boron with curcumin in mass fractions of from 0.001% to 0.05%

6.1 the essence of the method

The method is based on formation of colored complex compounds of boron with curcumin in the environment of glacial acetic and sulphuric acids in the presence of acetate buffer solution.

6.2 Apparatus, reagents and solutions

Sodium posterolaterally according to GOST 200.

A mixture of acetic and sulphuric acids (1:1): 100 cmacetic acid carefully, while cooling water is added to 100 cmof concentrated sulfuric acid. Prepare immediately before use.

Ammonium acetate according to GOST 3117.

Buffer solution: 225 g of ammonium acetate are dissolved in 400 cmof water by heating, cool, add 300 cmof acetic acid, transfer the solution into a volumetric flask with a capacity of 1 DM, made up to the mark with water, mix.

Sodium fluoride according to GOST 4463, a solution of 40 g/DM. Stored in a vessel made of polyethylene.

Curcumin, a solution of 1.25 g/DMacetic acid: 0.125 g of curcumin is dissolved in 60 cmof acetic acid at low heat, cooled, transferred to a volumetric flask with a capacity of 100 cm, made up to the mark with acetic acid and stirred. Prepare immediately before use.

The rest of the reagents, equipment and solutions — for 4.2.

6.3 analysis

6.3.1 Preparation of test solution

The weight of the alloy 0.1−0.5 g in accordance with table 5 was placed in a quartz glass with a capacity of 100 cm, 30 cm, pour themixture of hydrochloric and nitric acids in the ratio 3:1 or 8:1, 5 cmof phosphoric acid, a glass cover made of PTFE and the sample is dissolved with moderate heating.


Table 5

After dissolution, the sample flow 10 cmof sulphuric acid (1:1).

Then do as specified in 4.3.1.

6.3.2 Spectrophotometric assay procedure

Salt is dissolved in 30 cmof water with the addition of 5 cmof hydrochloric acid when heated, add 3 g phosphonoacetate sodium, heated to boiling and gently boil under lid for 15 minutes, cool. The solution was transferred to a volumetric flask with a capacity of 50 cm, made up to the mark with water and mix. The solution is filtered over a dry dense quartz filter in a dry flask, discarding first portion of filtrate.

6.3.2.1 Preparation of test solution

Aliquot part of the solution 1 cmis placed in a dry plastic container with a capacity of 100 cmadd 6 cmof a mixture of acetic and sulphuric acids (1:1), 6 cmof a solution of curcumin, stirring after adding each reagent, and left for 2.5 h Then poured 1 cmof orthophosphoric acid, mix and leave for 30 min.

Pour the 30 cmbuffer solution, mix thoroughly and after 15 min measure the optical density of colored solution with spectrophotometer at a wavelength of 543 nm and the photoelectrocolorimeter at a wavelength range of from 520 to 560 nm. The thickness of the light absorbing layer is chosen so to obtain the optimal value of optical density.

As a solution comparison, using aliquot part of the solution in which boron is previously transferred in the fluoride complex.

6.3.2.2 preparation of the solution comparison

Aliquot part of the solution 1 cmis placed in a dry plastic container with a capacity of 100 cm, 0.2 cm is addeda solution of sodium fluoride, stir thoroughly and leave for 1 hour

Add 6 cmof a mixture of acetic and sulphuric acids (1:1), 6 cmof a solution of curcumin. Then do as specified in 6.3.2.1.

A lot of find boron in the calibration schedule subject to amendments the reference experiment.

6.3.3 Construction of calibration curve

In quartz glasses put a measured amount of a standard solution In Bora 0,00; 0,50; 1,00; 2,00; 3,00; 4,00; 5,00 cm.

All the glasses are poured acid as the dissolution of the sample and then receives, as specified in 6.3.1 and 6.3.2.

On the found values of optical density and corresponding mass of the boron build the calibration graph.

7 Processing of results

7.1 Mass percent of boron , %, is calculated by the formula

, (1)

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

 — the weight of the portion of alloy,

7.2 error Norms and standards for monitoring the accuracy of results of measuring the mass fraction of boron is given in table 6.


Table 6

Percentage