GOST 22536.9-88
GOST 22536.9−88 carbon Steel and unalloyed cast iron. Methods for determination of Nickel
GOST 22536.9−88
Group B09
STATE STANDARD OF THE USSR
CARBON STEEL AND UNALLOYED CAST IRON
Methods for determination of Nickel
Carbon steel and unalloyed cast iron.
Methods for determination of nickel
AXTU 0809
Valid from 01.01.90
to 01.07.95*
______________________________
* Expiration removed
Protocol N 4−93 inter-state Council
for standardization, Metrology and certification.
(IUS N 4, 1994). — Note the CODE.
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of ferrous metallurgy of the USSR
PERFORMERS
D. K. Nesterov, PhD. tech. Sciences; S. I. Rudyuk, PhD. tech. Sciences; S. V. Spirina, PhD. chem. Sciences (head of subject); V. F. Kovalenko, PhD. tech. science; N. N. Gritsenko, PhD. chem. Sciences; L. I. birch; O. M. Kirzhner
2. APPROVED AND put INTO EFFECT by decision of the USSR State Committee for standards from
3. REPLACE GOST 22536.9−77
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced |
The number of the paragraph, subparagraph |
| GOST 849−70 |
2.1.2, 4.2 |
| GOST 3118−77 |
2.1.2, 3.2, 4.2 |
| GOST 3652−69 |
2.1.2, 3.2 |
| GOST 3760−79 |
2.1.2, 3.2 |
| GOST 4160−74 |
2.1.2 |
| GOST 4204−77 |
2.1.2 |
| GOST 4328−77 |
2.2.2 |
| GOST 4457−74 |
2.1.2 |
| GOST 4461−77 |
2.1.2, 3.2, 4.2 |
| GOST 5457−75 |
4.2 |
| GOST 5817−77 |
3.2 |
| GOST 5828−77 |
2.1.2, 2.2.2, 3.2 |
| GOST 5845−79 |
2.2.2 |
| GOST 11125−84 |
2.1.2, 3.2, 4.2 |
| GOST 13610−79 |
2.1.2, 4.2 |
| GOST 14261−77 |
3.2, 4.2 |
| GOST 18300−87 |
2.1.2, 3.2 |
| GOST 19522−74 |
3.2 |
| GOST 20478−75 |
2.2.2 |
| GOST 22536.0−87 |
1.1 |
| GOST 24364−80 |
2.2.2 |
| GOST 25336−82 |
3.2 |
This standard specifies the photometric (mass fraction in Nickel from 0.01 to 0.50%), gravimetric (when the mass fraction of Nickel from 0.1 to 0.5%) and atomic absorption (at a mass fraction of Nickel from 0.02 to 0.50%) methods for determination of Nickel.
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis GOST 22536.0−87.
1.2. The error of the result of the analysis (under confidence probability = 0,95) does not exceed the limit
shown in the table, when the conditions are met:
the discrepancy between the results of two (three) parallel dimensions should not exceed (with a confidence probability = 0,95) of the values
(
) given in the table;
played in the standard sample, the value of the mass fraction of Nickel must not vary from certified more than acceptable (at a confidence level =0,85) the value
given in the table.
If any of the above conditions, a second measurement of the mass fraction of Nickel. If in repeated measurements the precision requirement of the results are not met, the results of the analysis recognize the incorrect measurements cease to identify and eliminate the causes of violation of the normal course of analysis.
The divergence of the two middle results of an analysis performed under different conditions (for example, when the control intralaboratory reproducibility) shall not exceed (with a confidence probability = 0,95) of the values
given in the table.
| The allowable divergence, % | |||||||||
| Mass fraction of Nickel, % |
|
| |||||||
From |
0,01 |
to |
0,02 |
incl. |
0,003 |
0,004 |
0,003 |
0,004 |
0,002 |
| SV. | 0,02 | « | 0,05 | « | 0,005 |
0,006 | 0,005 | 0,006 | 0,003 |
| « | 0,05 | « | 0,10 | « | 0,008 |
0,010 | 0,008 | 0,010 | 0,005 |
| « | 0,10 | « | 0,2 | « | 0,013 |
0,016 | 0,013 | 0,016 | 0,008 |
| « | 0,2 | « | 0,5 | « | 0,020 | 0,026 | 0,021 | 0,026 | 0,013 |
2. THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF NICKEL
2.1. The determination of Nickel (0,01−0,5%) in steel and cast iron with a mass fraction of manganese up to 2%.
2.1.1. The method is based on the formation of red color complex compounds of Nickel with dimethylglyoxime in ammoniacal medium in the presence of potassium bromide and Bromeliaceae and measuring the optical density of the colored solution at a wavelength of 530 nm.
2.1.2. Equipment and reagents
Spectrophotometer or photoelectrocolorimeter.
Sulfuric acid GOST 4204−77 and diluted 1:4 and 1:1.
Nitric acid GOST 4461−77 or GOST 11125−84 and diluted 3:2.
Hydrochloric acid by the GOST 3118−77 and diluted 1:4.
Citric acid according to GOST 3652−69, a solution with a mass concentration of 100 g/DM.
Potassium bromide according to GOST 4160−74.
Potassium branovitsky according to GOST 4457−74.
A solution of potassium bromide and bromoperoxidase: 39 g of potassium bromide and 10 g of potassium polnovatogo dissolved in water in a volumetric flask with a capacity of 1 DM, made up to the mark with water and mix.
Ammonia water according to GOST 3760−79 and diluted 3:2.
Rectified ethyl alcohol according to GOST 18300−72.
Dimethylglyoxime according to GOST 5828−77, a solution with a mass concentration of 10 g/DMof 10 g dimethylglyoxime was dissolved in ethanol in a volumetric flask with a capacity of 1 DM
, made up to the mark with ethanol and mix; before use, the solution was filtered.
Radio engineering carbonyl iron according to GOST 13610−79.
The primary Nickel GOST 849−70.
Standard solutions of Nickel.
Solution a: 1,000 g of metallic Nickel is dissolved with moderate heating in 35 cmof nitric acid (3:2), poured 30 cm
of sulphuric acid (1:4), evaporated prior to the selection of vapors of sulfuric acid and cooled. Salt is dissolved in 100−150 cm
of water, the solution transferred to a volumetric flask with a capacity of 1 DM
, cooled, made up to the mark with water and mix.
1 cmof the solution contains 0.001 g of Nickel.
Solution B: 50 cmsolution And placed in a volumetric flask with a capacity of 500 cm
, made up to the mark with water and mix.
1 cmof a solution contains 0.0001 g of Nickel.
Solution: 50 cmof a solution is placed in a volumetric flask with a capacity of 100 DM
, made up to the mark with water and mix.
1 cmof the solution contains 0,00005
g of Nickel.
2.1.3. Analysis
Weighed samples of 0.5 g were placed in a glass with a capacity of 200−250 cm, dissolved in 30 cm
of sulphuric acid (1:4) with moderate heat and oxidize with nitric acid, adding it dropwise until the termination of foaming solution. After cooling, if dissolved in 100−120 cm
of water, the solution transferred to a volumetric flask with a capacity of 250 cm
, cooled, made up to the mark with water and mix.
The solution is filtered through a dry filter into a flask with a capacity of 250 cm, discarding the first two portions of the filtrate. Aliquote two parts of a solution of 25 cm
is placed in a volumetric flask with a capacity of 100 cm
and with constant stirring successively poured into each volumetric flask 20 cm
of the citric acid solution, 5 cm
of hydrochloric acid (1:4), 10 cm
of a solution of potassium bromide and Bromeliaceae and 2−3 min of 25 cm
of ammonia solution (3:2). The solutions were mixed and immediately cooled to 20 °C.
In one of the flasks poured 1 cmof solution dimethylglyoxime in the other and 1 cm
of ethanol. The solutions were topped up to the mark with water and mix thoroughly. Within 25 minutes measure the optical density of colored solution with spectrophotometer at a wavelength of 530 nm or photoelectrocolorimeter with a filter having maximum transmission in the wavelength range of 530−550 nm.
As a solution comparison, using aliquot part of the analysis of a solution containing all reagents except dimethylglyoxime.
The analysis results calculated by a calibration chart or by comparison with a standard sample similar in composition to the sample and carried through all the stages and
analysis.
2.1.4. Construction of calibration curve
2.1.4.1. When the mass fraction of Nickel of 0.01−0.05%.
Seven of cups with a capacity of 250 cmis placed 0.5 g of carbonyl iron. Six of them added standard solution In the amount 0,5; 1,0; 2,0; 3,0; 5,0; 6,0 cm
, which corresponds to 0,000025; 0,000050; 0,000100; 0,000150; 0,000250 and 0,000300 g of Nickel. The seventh glass is used for solution preparation comparison. Conduct further analysis as given in claim
2.1.4.2. When the mass fraction of Nickel 0,05−0,50%.
Seven of cups with a capacity of 250 cmis placed 0.5 g of carbonyl iron. Six of them add standard solution B in an amount of 2; 5; 10; 15; 20; 30 cm
, which corresponds to 0,0002; 0,0005; 0,0010; 0,0015; 0,0020; 0,0030 g of Nickel. The seventh glass is used for solution preparation comparison. Conduct further analysis as given in claim
On the found values of optical density and corresponding weight values of Nickel to build a calibration curve. Allowed construction of calibration curve in the coordinates: the optical density is the mass fraction of Nickel.
2.2. The determination of Nickel (0,05−0,50%) in steel and cast iron with a mass fraction of manganese up to 1%.
2.2.1. The method is based on formation of colored in brown-red complex compound of Nickel with dimethylglyoxime in an alkaline medium in the presence of ammonium naternicola and measuring the optical density of the colored solution at a wavelength of 440 nm. The interfering influence of iron eliminated by converting it into a wine-acid complex.
2.2.2. Equipment and reagents
Potassium-sodium vinocity according to GOST 5845−79, a solution with a mass concentration of 200 g/DM.
Sodium hydroxide according to GOST 4328−77, a solution with a mass concentration of 200 g/DMor potassium hydroxide according to GOST 24364−80 the solution with a mass concentration of 250 g/DM
.
Ammonium neccersarily according to GOST 20478−75, a solution with a mass concentration of 30 g/DM, freshly prepared.
Dimethylglyoxime according to GOST 5828−77, a solution with a mass concentration of 10 g/DMsolution of sodium hydroxide or potassium hydroxide with a mass concentration of 50 g/DM
.
2.2.3. Analysis
Weighed samples of 0.5 g (with a mass fraction of Nickel 0,05−0,20%) and 0.2 g (for a mass fraction of Nickel 0,2−0,5%) were placed in a glass with a capacity of 200 cmand is dissolved as provided in claim
After dissolution, the sample solution is boiled to remove oxides of nitrogen, cooled and transferred to volumetric flask with a capacity of 100 cm, made up to the mark with water and mix. In the analysis of cast irons or in the case of precipitation of silicic acid part of the solution filtered through a dry filter into a dry flask, discarding first portion of filtrate.
Aliquote two parts of a solution at 10 cmis placed in a volumetric flask with a capacity of 100 cm
, sequentially poured into each flask 20 cm
water, 10 cm
of a solution of potassium-sodium Vinokurova 10 cm
of sodium hydroxide (or potassium hydroxide) 10 cm
solution naternicola ammonium, stirring thoroughly after adding each reagent. In one of the flasks poured 10 cm
of the solution dimethylglyoxime. After 3−5 min the contents of the flask brought to the mark with water, mix and measure the optical density of the solution on the spectrophotometer at a wavelength of 440 nm or photoelectrocolorimeter with a filter having maximum transmission in the wavelength range of 430−450 nm. As a solution comparison, using aliquot part of the analysis of a solution containing all the reagents except dimethylglyoxime.
The analysis results calculated by a calibration chart or by comparison with a standard sample similar in composition to the sample and carried through all stages of the analysis
for.
2.2.4. Construction of calibration curve
Six glasses with a capacity of 250 cmis placed 0.5 or 0.2 g carbonyl iron depending on the sample samples. Five of them add standard solution B in an amount of 2; 3; 5; 8; 12 cm
, which corresponds to 0,0002; 0,0003; 0,0005; 0,0008; 0,0012 g of Nickel. The sixth glass is used for solution preparation comparison. Conduct further analysis as given in claim
On the found values of optical density and corresponding weight values of Nickel to build a calibration curve. Allowed construction of calibration curve in the coordinates:
optical density — the mass fraction of Nickel.
2.3. The separation of the manganese in the dioxide in the determination of Nickel (0,05−0,50%) in steel and cast iron with a mass fraction of manganese above 1%.
A portion of the sample weight of 0.5 or 0.2 g were placed in a glass with a capacity of 250 cm, is dissolved in 30 cm
of sulphuric acid (1:4), with moderate heat. After dissolution of the sample poured nitric acid until the termination of foaming solution and in excess of 2−3 cm
. The solution was boiled, wash away the side of the Cup with water, pour 10 cm
of sulphuric acid and evaporated to fumes of sulfuric acid. Of salt dissolved in 100 cm
of water when heated. To the solution are added 1 g of potassium Bromeliaceae, heated to boiling and boiled for 5 min.
The solution was cooled, transferred to a volumetric flask with a capacity of 250 cm, made up to the mark with water and mix. The solution is filtered through dense dry filter into a dry flask, discarding first portion of filtrate.
Aliquot part of 25 cmis placed in a beaker with a capacity of 250 cm
, 5−10 cm poured
hydrochloric acid and evaporated to fumes of sulfuric acid, the treatment with hydrochloric acid is carried out two more times. The solution is evaporated until the appearance of sulphuric acid fumes, pour 1 cm
of hydrochloric acid, 10 cm
of water and dissolved salts when heated. The solution was cooled and transferred to volumetric flask with a capacity of 100 cm
. Further analysis is carried out according to claim
2.2.3.
2.4. Processing of the results
2.4.1. Mass fraction of Nickel () in percent is calculated by the formula
where is the mass of Nickel in the sample was found in the calibration schedule g;
— the weight of the portion of the sample,
2.4.2. Norms of accuracy and norms control the accuracy of determining the mass fraction of Nickel in the table.
2.4.3. The method used in the dispute in the assessment of quality carbon steel and unalloyed cast iron.
3. GRAVIMETRIC METHOD FOR THE DETERMINATION OF NICKEL
3.1. The essence of the method
The method is based on deposition of Nickel dimethylglyoxime in the ammonia environment in the presence of tartaric acid for the binding of iron and weighing the resulting precipitate of oxide of Nickel or a Nickel dimethylglyoximate.
3.2. Equipment and reagents
Electric type SNOL providing adjustment of the temperature with an accuracy of ± 10 °C.
The Cabinet laboratory type dryer SNOL providing adjustment of the temperature with an accuracy of ± 10 °C.
Desiccator, according to GOST 25336−82.
Hydrochloric acid by the GOST 3118−77 or GOST 14261−77 diluted 1:20 and 1:1.
Nitric acid GOST 4461−77 or GOST 11125−84.
Ammonia water according to GOST 3760−79 diluted 1:1 and 1:100.
Tartaric acid according to GOST 5817−77, a solution with a mass concentration of 500 g/DM.
Citric acid monohydrate and anhydrous according to GOST 3652−69, a solution with a mass concentration of 250 g/DM.
Ammonium radamisty according to GOST 19522−74, a solution with a mass concentration of 50 g/DM.
Rectified ethyl alcohol GOST 18300−87.
Dimethylglyoxime according to GOST 5828−77: 1 g of reagent was dissolved in 100 cmof ethanol.
3.3. Analysis
The weight of steel or cast iron weighing 2 g were placed in a glass with a capacity of 400−500 cmand dissolved in 40−50 cm
of hydrochloric acid (1:1), with moderate heat.
After dissolution of the sample poured dropwise nitric acid until the termination of foaming solution and 2−3 drops excess.
The solution was evaporated to dryness. To the dry residue add 10 cmof hydrochloric acid (1:1), evaporated to dryness and cooled.
After cooling to the dry residue add 10 cmof hydrochloric acid (1:1), heated to dissolve the salts, add 100 cm
of hot water and filtered (if a precipitate has formed of silicic acid and graphite) using the filter «white ribbon». Filter the precipitate was washed several times with hot hydrochloric acid (1:20) to remove ions of iron (control is carried out by reaction with ammonium radamisty). Filter the precipitate discarded.
The filtrate was adjusted to volume of 300−350 cm, 40 cm poured
the solution of tartaric acid, or 20 cm
of a solution of citric acid, carefully neutralized with ammonia solution until the appearance of a weak smell and poured 10 cm
of the solution dimethylglyoxime with constant stirring.
Solution to precipitate dimethylglyoximate of Nickel is heated to 60−70 °C, allow to stand in a warm place for 2−3 hours, then filtered through the filter «white ribbon».
The glass is washed over the filter 2−3 times with cold ammonia solution (1:100) and washed the filter residue 1−2 times with the same solution. The filter cake is dissolved in 30 cmof hot hydrochloric acid (1:1) and washed 5−6 times with hot water collecting the filtrate and washings in a beaker, in which was conducted the deposition. This was followed by re-deposition of Nickel, as shown above.
The washed pellet of dimethylglyoximato Nickel with the filter wrapped in another slightly damp filter was placed in a porcelain crucible, previously ignited to constant mass at 800 °C and weighed, the filter with sediment was dried in a crucible, carefully incinerated, preventing ignition, and then calcined in an electric furnace at 650−700 °C to constant weight. Cool the crucible and residue in a desiccator and weighed. Simultaneously with the execution of the analysis carried out control experience for contamination of reagents.
The determination of Nickel is allowed to finish weighing the dried sediment of dimethylglyoximato Nickel (at a mass fraction of Nickel in the steel is less than 0.2%). In this case, the precipitate was filtered off on a glass filter crucible No. 3, pre-dried and brought to constant weight. The walls of the beaker and the precipitate is washed with ammonia solution (1:100) and 5−6 times with warm water. The crucible with the precipitate is placed in a drying Cabinet and dried at a temperature of 110−120 °C to constant weight. The crucible with residue was cooled in a desiccator and weighed. Simultaneously with the execution of the analysis carried out control experience of pollution, reacti
the second world war.
3.4. Processing of the results
3.4.1. Mass fraction of Nickel () in percent is calculated by the formula
where is the mass of the crucible with the precipitate of oxide of Nickel or a Nickel dimethylglyoximate, g;
— weight of crucible without sediment, g;
— the mass of the crucible with the sediment in the reference experiment, g;
— weight of crucible without sediment, g;
the coefficient of 0,2032 in terms of dimethylglyoximate of Nickel on Nickel and 0,7858 in terms of Nickel oxide to Nickel;
— the weight of the portion of the sample,
3.4.2. Norms of accuracy and norms control the accuracy of determining the mass fraction of Nickel in the table.
4. ATOMIC ABSORPTION METHOD FOR THE DETERMINATION OF NICKEL
4.1. The essence of the method
The method is based on measuring the degree of absorption of resonance radiation by free atoms of Nickel formed as a result of spraying the test solution in a flame air-acetylene.
4.2. Equipment and reagents
Atomic absorption spectrophotometer.
Lamp with hollow cathode for the determination of Nickel.
Acetylene, dissolved and gaseous GOST 5457−75.
The compressor supplying compressed air, or compressed air.
Hydrochloric acid by the GOST 3118−77 or GOST 14261−77 and diluted 1:1.
Nitric acid GOST 4461−77 or GOST 11125−84.
Radio engineering carbonyl iron according to GOST 13610−79, a solution with a mass concentration of 50 g/l: 50 grams of carbonyl iron is dissolved in 400 cm
of hydrochloric acid (1:1), added dropwise nitric acid until the end of foaming, is evaporated to wet salts, add 40−50 cm
of hydrochloric acid and again evaporated to wet salts. This operation is repeated. Of salt dissolved in 100 cm
of hydrochloric acid (1:1), cooled, transferred to a volumetric flask with a capacity of 1 DM
, adjusted to the mark with water, mix and filter the solution through a filter of medium density.
The primary Nickel GOST 849−70.
Standard solutions of Nickel.
Solution a: 0,5000 g of metallic Nickel dissolved in 10 cmsalt and 10 cm
of nitric acid. 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 cmof the solution contains 0.0005 g of Nickel.
Solution B (prepared immediately before use): 20 cmstandard solution And placed in a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix.
1 cmof a solution contains 0.0001 g n
the ikel.
4.3. Preparation of the device
The preparation instrument to the analysis carried out in accordance with the attached instructions.
Set the spectrophotometer at a resonance line 232 nm. After switching on the gas flow and ignition of the burner spray water into the flame and set the zero readings.
4.4. Analysis
4.4.1. The weight of steel or cast iron with a mass of 1 g (in mass fraction of Nickel from 0.02 to 0.1%) or 0.5 g (at a mass fraction of Nickel from 0.1 to 0.2%) or 0.2 g (for a mass fraction of Nickel from 0.2 to 0.5%) were placed in a glass with a capacity of 100 cmand dissolved by heating in 15 cm
of hydrochloric acid and 5 cm
of nitric acid. The solution was evaporated to dryness, cooled, poured 5cm
of hydrochloric acid 20−30 cm
of water and heated to dissolve the salts. The cooled solution was transferred to volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix. The solution is filtered through dry filter «white ribbon», discarding the first two portions of the filtrate. To prepare the solution in the reference experiment in a volumetric flask with a capacity of 100 cm
poured a solution of carbonyl iron and carried through all stages of the analysis.
Is sprayed into the flame of the solution in the reference experiment, and then analyze the solutions in order of increasing mass fraction of Nickel to obtain stable readings for each solution. Prior to introduction into the flame each of the analyzed solution is sprayed water to wash the system and check the zero point.
From the mean values of absorbance of each test solution subtract the mean value of optical density in the reference experiment.
The weight of the Nickel find at the calibration schedule
.
4.4.2. Construction of calibration curve
In seven volumetric flasks with a capacity of 100 cmplaced at 20, 10 or 4 cm
of solution carbonyl iron depending on sample tests, in six successively poured 1,5; 3,0; 5,0; 7,0; 10,0; 12,5 cm
standard solution B, which corresponds to 0,00015; 0,00030; 0,00050; 0,00070; 0,00100; 0,00125 g of Nickel. The seventh flask is used for the reference experiment. The contents of the flask brought to the mark with water, mixed and further analysis is carried out according to claim
On the found values of optical density and corresponding weight values of Nickel to build a calibration curve.
4.5. Processing of the results
4.5.1. Mass fraction of Nickel () in percent is calculated by the formula
where is the mass of Nickel in the sample was found in the calibration schedule g;
— the weight of the portion of the sample,
Norms of accuracy and norms control the accuracy of determining the mass fraction of Nickel in the table.
