GOST 24018.4-80
GOST 24018.4−80 heat-resistant Alloys on a Nickel basis. Methods for determination of bismuth (with Amendments No. 1, 2)
GOST 24018.4−80
Group B39
INTERSTATE STANDARD
ALLOYS HIGH-TEMPERATURE NICKEL-BASED
Methods for determination of bismuth
Nickel-based fire-resistant alloys.
Methods for the determination of bismuth
ISS 77.120.40
AXTU 0809
Date of introduction 1981−07−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of metallurgy of the USSR
2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from
3. INTRODUCED FOR THE FIRST TIME
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced |
The number of the paragraph, subparagraph |
| GOST 849−97 |
2, 5 |
| GOST 859−2001 |
2, 5 |
| GOST 1277−75 |
2 |
| GOST 3118−77 |
2, 5 |
| GOST 3760−79 |
2, 5 |
| GOST 4204−77 |
2 |
| GOST 4232−74 |
2 |
| GOST 4329−77 |
2 |
| GOST 4461−77 |
2, 5 |
| GOST 5817−77 |
2, 5 |
| GOST 6344−73 |
2 |
| GOST 9722−97 |
2, 5 |
| GOST 10157−79 |
5 |
| GOST 10928−90 |
2, 5 |
| GOST 11125−84 |
2, 5.2 |
| GOST 14261−77 |
2, 5.2 |
| GOST 14262−78 |
2 |
| GOST 20478−75 |
2 |
| GOST 24018.0−90 |
1.1 |
| GOST 24147−80 |
2 |
5. Limitation of actions taken by Protocol No. 7−95 Interstate Council for standardization, Metrology and certification (ICS 11−95)
6. EDITION (August 2004) with Changes No. 1, 2 approved in December 1985, December 1990 (IUS 4−86, 3−91)
This standard sets the photometric method for the determination of bismuth (in mass fractions of from 0.0005% to 0,010%) and flameless atomic absorption method for the determination of bismuth (at a mass fraction of from 0.0002% to 0.01%).
(Changed edition, Rev. N 2).
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis according to GOST 24018.0.
A. Photometric method for the determination of bismuth
The essence of the method
The method is based on the education in the medium of sulfuric acid of 1 mol/DMyellow colored complex compound of bismuth with potassium iodide composition K (BiI
). Bismuth is pre-separated from the main components of the alloy by precipitation as a sulfide by thioacetamide in ammoniacal solution (pH 7.5) in the presence of tartaric acid as complexing agents.
(Added, Rev. N 2).
2. APPARATUS, REAGENTS AND SOLUTIONS
Spectrophotometer or photoelectrocolorimeter.
a pH meter.
Thermometer.
Hydrochloric acid according to GOST 3118, GOST 14261 and diluted 1:1 and 1:100.
Nitric acid according to GOST 4461, GOST 11125 and diluted 1:1.
A mixture of hydrochloric and nitric acids: the 150 cmof hydrochloric acid add 50 cm
of nitric acid, stirred; and diluted 1:1, prepared immediately before use.
Sulfuric acid according to GOST 4204, GOST 14262.
Ammonia water according to GOST 3760, GOST 24147 and diluted 1:200.
Tartaric acid according to GOST 5817, a solution with a mass concentration of 50 g/cm, (g/DM
).
Ammonium neccersarily according to GOST 20478, a solution with a mass concentration of 25 g/cm, (g/DM
).
Silver nitrate according to GOST 1277, a solution with a mass concentration of 0.1 g/cm(g/DM
).
The thioacetamide aqueous solution with a mass concentration of 2 g/cm(g/DM
).
Aljumokalievyh alum GOST 4329, a solution with a mass concentration of 1 g/cm(g/DM
).
Potassium iodide according to GOST 4232, a solution with a mass concentration of 10 g/cm, (g/DM
).
Thiourea according to GOST 6344, solution with a mass concentration of 2 g/cm(g/DM
).
Universal indicator paper pH 1−10.
Nickel brand H0 according to GOST 849.
Nickel powder according to GOST 9722.
Copper grade М00бк according to the GOST 859.
The copper nitrate solution with a mass concentration of 1 g/cm(g/DM
):
1 g of copper metal is dissolved by heating in 15−20 cmof nitric acid (1:1). The solution was cooled, transferred to a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix.
Bismuth brands Ви0; Vi00; Ви000; Ви0000 according to GOST 10928.
Standard solutions of bismuth.
Solution a: 0.1 g of bismuth dissolved in 30 cmof nitric acid (1:1) under heating, cooled, poured 10 cm
of sulphuric acid, evaporated to start the selection of vapors of sulfuric acid and cooled. The solution was transferred to a volumetric flask with a capacity of 1 DM
, cooled, made up to the mark with water and mix.
1 cmstandard solution contains 0.0001 g of bismuth.
Solution B: 10 cmsolution And placed in a volumetric flask with a capacity of 100 cm
, pour 2 cm
of sulfuric acid, cooled, made up to the mark with water and mix.
1 cmstandard solution B has the 0.00001 g of bismuth.
(Changed edition, Rev. N 1, 2).
3. ANALYSIS
3.1. The weight of the alloy: 1 g when the mass fraction of bismuth from 0.0005% to 0.005%; 0.5 g when the mass fraction of bismuth of more than 0.005% to 0,010% were placed in a glass (or flask) with a capacity of 250−300 cm, 30 cm, pour the
mixture of hydrochloric and nitric acid, cover with watch glass and dissolved under heating. The solution was evaporated to a volume of approximately 10 cm
. Add 30 cm
of water, 15−20 cm
of tartaric acid solution, 1 cm
of a solution of copper nitrate and heated for 5 min. Solution was cooled, poured 20−25 cm
of ammonia solution and again heat for 5−8 min, Set pH 7.5 with hydrochloric acid (1:1) using pH meter. Dilute the solution with water to approximately 150 cm
, heated to 85 °C — 90 °C, pour 10 cm
of a solution of thioacetamide and incubated for 10 min at the same temperature. Newly poured 10 cm
of a solution of thioacetamide, and leave the solution to precipitate for 2 h at 40 °C — 50 °C and cooled. The precipitate is filtered off sulphides in two medium density filter (white ribbon), washed 7−8 times with cold water. The filtrate is discarded. The filter cake is dissolved 40−50 cm
(chunks 10 cm
) of a hot mixture of hydrochloric and nitric acids (1:1) and washed the filter 2−3 times with hot water collecting the filtrate and washings in a beaker, in which was conducted the deposition.
To the obtained solution add 2 cmof sulphuric acid, the solution evaporated to start the selection of vapors of sulfuric acid and cooled. Wash the side of the Cup with water and re-evaporated prior to the allocation of sulphuric acid fumes. Salt is dissolved in 50 cm
of water, add 5 cm
of a solution of silver nitrate, 10 cm
naternicola solution of ammonia, heated for 3−5 min, poured 10 cm
of the solution aljumokalievyh alum and a solution of ammonia to a faint smell. The contents of the beaker heated for 3−5 min, the precipitate was filtered off on a medium density filter (white ribbon) and washed 3−4 times with hot ammonia solution (1:200). The filtrate is discarded. The residue is dissolved in 30 cm
hot mixture of hydrochloric and nitric acids (1:1), collecting the solution in a glass, which conducted the deposition. Then pour 2 cm
of sulphuric acid, evaporated the solution to start the selection of vapors of sulfuric acid and cooled. Wash the side of the Cup with water, again evaporated solution prior to the selection of vapors of sulfuric acid and cooled. Salt dissolved in 10−15 cm
of water, the solution transferred to a volumetric flask with a capacity of 50 cm
, is diluted with water up to 30−35 cm
, flow 10 cm
of a solution of potassium iodide and mix. The solution is kept for 2−3 min, add 2.5 cm
of a solution of thiourea portions in 2−3 hours for the recovery of free iodine, made up to the mark with water and mix.
Optical density of the solution measured on a spectrophotometer at 
The contents of bismuth find the calibration schedule subject to amendments the reference experiment.
3.2. Construction of calibration curve
Five cups (or flasks) with a capacity of 250−300 cmis placed 0.5 g of metallic Nickel or Nickel powder. Four cups (or flasks) poured successively 0,5; 1,0; 3,0; 5,0 cm
standard solution B of bismuth. The fifth glass (or flask) used for carrying out control of the experience. All glasses add 30 cm
of a mixture of hydrochloric and nitric acids. Then do as stated in claim 3.1, from the values of absorbance of analyzed solutions is subtracted the value of optical density in the reference experiment.
The found values of optical density of solutions and their corresponding masses of bismuth build the calibration graph.
3.1, 3.2. (Changed edition, Rev. N 1, 2).
4. PROCESSING OF THE RESULTS
4.1. Mass fraction of bismuth () in percent is calculated by the formula
where — weight of bismuth, was found in the calibration schedule g;
— the weight of the portion of alloy,
4.2. The absolute differences of the results of the parallel definitions should not exceed (at p = 0.95) of permissible values, specified in table.2.
(Changed edition, Rev. N 2).
B. Flameless atomic absorption method for the determination of bismuth
The essence of the method
The method is based on measuring absorption of radiation by free atoms of bismuth at a wavelength of 223,1 or 306,8 nm, formed with the introduction of the analyzed solution in the electrothermal atomizer. Bismuth is pre-separated from the main components of the alloy by precipitation as a sulfide by thioacetamide in ammoniacal solution (pH 7.5) in the presence of tartaric acid as a complexing agent and copper sulfide as a collector.
5. APPARATUS, REAGENTS AND SOLUTIONS
Atomic absorption spectrophotometer with electrothermal atomizer.
Lamp for determination of bismuth.
Argon of high purity according to GOST 10157 or a mixture of argon with 5% hydrogen.
a pH meter.
Thermometer.
Hydrochloric acid according to GOST 3118, GOST 14261 and diluted 1:1.
Nitric acid according to GOST 4461, GOST 11125 and diluted 1:1.
A mixture of hydrochloric and nitric acids: the 150 cmof hydrochloric acid add 50 cm
of nitric acid, and mix; dilute 1:1. The mixture of acids prepared immediately before use.
Tartaric acid according to GOST 5817, a solution of 500 g/DM.
Ammonia water according to GOST 3760.
The thioacetamide solution of 20 g/DM.
Copper grade М00бк according to the GOST 859.
Copper nitrate, solution 0,01 g/cm1 g of copper metal is dissolved by heating in 15−20 cm
of nitric acid (1:1).
The solution was cooled, transferred to a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix.
Nickel brand H0 according to GOST 849.
Nickel powder according to GOST 9722.
Bismuth brands Ви0, Vi00, Ви000, Ви0000 according to GOST 10928.
Standard solutions of bismuth:
Solution a: 0.1 g of bismuth dissolved in 30 cmof nitric acid by heating, the solution was transferred to a volumetric flask with a capacity of 1 DM
, made up to the mark with water and mix. 1 cm
standard solution contains 0.0001 g of bismuth.
Solution B: 10 cmsolution And placed in a volumetric flask with a capacity of 100 cm
, add 10 cm
of nitric acid, made up to the mark with water and mix.
1 cmstandard solution B has the 0.00001 g of bismuth.
Solution: 10 cmof solution B is placed in a volumetric flask with a capacity of 100 cm
, add 10 cm
of nitric acid, made up to the mark with water and mix. The solution is prepared immediately before use.
1 cmstandard solution contains 0,000001 g of bismuth.
6. ANALYSIS
6.1. A portion of the alloy by weight (table.1) is placed in a beaker or flask with a capacity of 250−300 cm, 20−30 cm, pour the
mixture of hydrochloric and nitric acid, cover with watch glass and dissolve the sample when heated.
Table 1
| Mass fraction of bi, % |
The mass of charge, g |
| From of 0.0002 to 0.002 incl. |
0,5 |
| SV. Of 0.002 «to 0.005 « |
0,2 |
| «0,005» 0,01 « |
0,1 |
The solution was evaporated to a volume of approximately 10 cm. Add 30 cm
of water, 15−20 cm
of tartaric acid solution, 1 cm
of a solution of copper nitrate and heated for 10 min.
The solution is cooled, add 20−25 cmof ammonia and heated again for 5−8 min, Set pH 7.5 with hydrochloric acid (1:1) using pH meter. The solution is diluted with water to a volume of approximately 150 cm
, heated to 85 °C — 90 °C, pour 10 cm
of a solution of thioacetamide, incubated 10 min at the same temperature. Newly poured 10 cm
of a solution of thioacetamide, and leave the solution to precipitate for 2 h at 40 °C — 50 °C and cooled.
The precipitate is filtered off sulphides in two medium density filter (white ribbon), washed 7−8 times with cold water. The filtrate is discarded. The filter cake was dissolved in 40−50 cm(chunks 10 cm
) of a hot mixture of hydrochloric and nitric acids, diluted (1:1) and washed the filter 2−3 times with hot water collecting the filtrate and washings into the beaker (or flask), which produced the deposition. The solution was evaporated to dryness, the salt dissolved in 5 cm
of nitric acid and again evaporated to dryness. Salt is dissolved in 10 cm
of nitric acid (1:1) when heated, covering the glass or flask glass, cool. The solution was transferred to a volumetric flask with a capacity of 50 cm
, made up to the mark with water, mix.
Take a micropipette aliquot part of the solution, equal to 20 micysmf, injected into the electrothermal atomizer and record the amount of radiation absorption by using a registered device. For measurements taken at least three alikvotnih parts of the solution.
A lot of bismuth find the calibration schedule, as amended kontrolnog
on experience.
6.2. Preparation of the device for measuring
Activation of the device, setting the spectrophotometer at the resonant radiation, the adjustment of the control unit, block, atomization is carried out according to the instructions supplied with the device.
The conditions for the determination of bismuth:
analytical line () — 223,1 nm
— 306,8 nm;
— the spectral slit width of 0.2 nm;
— drying time at 100 °C — 10 s;
— the decomposition at 560 °C — 15 s;
— a time of atomization in the 1930 °S — 10.
Determination of bismuth is carried out in the full flow of inert gas with disabling it on stage atomization.
6.3. Construction of calibration curve
Seven of cups (or flasks) with a capacity of 250−300 cmis placed hinge is metallic Nickel or Nickel powder in accordance with the table.1.
Six of cups (or flasks) poured consistently 1, 2, 4, 6, 8, 10 cmstandard solution Into the bismuth. The seventh beaker (or flask) used for carrying out control of the experience.
All the glasses are poured at 20−30 cmof a mixture of hydrochloric and nitric acid, cover with watch glass and dissolve the sample when heated. The solutions were evaporated to a volume of approximately 10 cm
, add 30 cm
of water, 20 cm
of a solution of tartaric acid and heated for 10 min Then do as indicated in the claims.5.3.1 and
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 bismuth build the calibration graph.
7. PROCESSING OF THE RESULTS
7.1. Mass fraction of bismuth () in percent is calculated by the formula
where — weight of bismuth, was found in the calibration schedule g;
— the weight of the portion of alloy,
7.2. The absolute differences of the results of the parallel definitions should not exceed (at p = 0.95) of permissible values, specified in table.2.
Table 2
| Mass fraction of bi, % |
The absolute allowable difference, % |
| From to from 0.0002 to 0.0005 incl. |
0,0002 |
| SV. Of 0.0005 «to 0.001 « |
0,0005 |
| «Of 0.001» to 0.002 « |
0,001 |
| «Of 0.002» to 0.005 « |
0,002 |
| «0,005» 0,01 « |
0,003 |
Section B. (Introduced later, Rev. N 2).
