GOST 22536.11-87
GOST 22536.11−87 carbon Steel and unalloyed cast iron. Methods for the determination of titanium (with Change No. 1)
GOST 22536.11−87
Group B09
STATE STANDARD OF THE USSR
CARBON STEEL AND UNALLOYED CAST IRON
Methods for determination of titanium
Carbon steel and unalloyed cast iron.
Methods for determination of titanium
AXTU 0809
Valid from 01.01.88
to 01.01.98*
_______________________________
* Expiration removed
Protocol N 7−95 Interstate Council
for standardization, Metrology and certification
(IUS N 11, 1995). — 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. science; N.N. Gritsenko, PhD. chem. Sciences (head of subject); V. F. Kovalenko, PhD. tech. Sciences; S. V. Spirina, PhD. chem. Sciences (head of subject); O. M. Kirzhner
2. APPROVED AND put INTO EFFECT by decision of the USSR State Committee for standards from 20.02.87 N 301
3. REPLACE GOST 22536.11−77
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| |
|
| The designation of the reference document referenced |
The number of the paragraph, subparagraph, enumeration, applications
|
GOST 22536.0−87
|
1.1 |
GOST 4204−77
|
2.2 |
GOST 14262−78
|
2.2 |
GOST 4461−77
|
2.2 |
GOST 11125−84
|
2.2 |
GOST 3118−77
|
2.2, 3.2 |
GOST 14261−77
|
2.2, 3.2 |
GOST 13610−79
|
2.2 |
GOST 7172−76
|
2.2 |
GOST 3760−79
|
2.2 |
GOST 19807−74
|
2.2 |
GOST 20015−74
|
3.2 |
GOST 4780−78
|
3.2 |
5. REPRINTING. December, 1987
The Change No. 1 approved by resolution of Gosstandart of the USSR from 28.03.90 No. 659, introduced in step with 01.10.90 and published in IMS No. 6, 1990
Change the text IUS N 6, 1990
This standard specifies the photometric (with a mass fraction of titanium from 0.01 to 0.10%) and extraction-photometric (when the mass fraction of titanium from 0.005 to 0.10%) methods for determination of titanium in carbon steel and unalloyed cast iron.
(Changed edition, Rev. N 1).
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis GOST 22536.0−87.
2. PHOTOMETRIC METHOD
2.1. The essence of the method
The method is based on formation of yellow colored coordination compounds of titanium with diantipyrylmethane in hydrochloric acid medium and measuring the light absorption of the resulting complex at a wavelength of 395 nm. The influence of iron (III) and vanadium (V) eliminate the addition of ascorbic acid.
(Changed edition, Rev. N 1).
2.2. Equipment and reagents
Photoelectrocolorimeter or spectrophotometer.
Sulfuric acid GOST 4204−77 or GOST 14262−78 and diluted 1:4, 1:2 and 1:20.
Nitric acid GOST 4461−77 or GOST 11125−84.
Hydrofluoric acid according to GOST 10484−84.
Hydrochloric acid by the GOST 3118−77 or GOST 14261−77 diluted 1:1, 1:6 and 1:9.
Ascorbic acid according to normative-technical documentation, solution with a mass concentration of 100 g/DM
, freshly prepared.
Carbonyl iron according to GOST 13610−79.
Diantipyrylmethane according to normative-technical documentation, solution with a mass concentration of 50 g/DM, freshly prepared: 50 g diantipyrylmethane dissolved in 300 cmof hydrochloric acid, diluted 1:6, is filtered through the filter «white ribbon» in a volumetric flask with a capacity of 1 DM, made up to the mark with the same acid and mix.
Universal indicator paper.
Potassium preservatory according to GOST 7172−76.
Ammonia water according to GOST 3760−79.
Titanium metal according to GOST 19807−74*.
_______________
* Standards 19807−91. — Note the CODE.
Titanium dioxide according to normative-technical documentation.
Titanium sulphate, standard solutions.
Solution a: 0,1668 g svejeprigotovlennogo at 1000 °C the titanium dioxide is placed in a platinum crucible and fused with 2−3 g of potassium peacemaking at 750−800 °C.
After cooling, the melt is dissolved in 300 cmof sulphuric acid, diluted 1:20, transferred to a volumetric flask with a capacity of 1 DM, made up to the mark diluted 1:20 with sulfuric acid and mix. 1 cmof the solution contains 0.0001 g of titanium.
The mass concentration of a standard solution set as follows: 50 cmstandard solution And placed in a beaker with a capacity of 200−250 cm, dilute with water to 100 cm, poured with stirring a solution of ammonia to pH 8−9 by universal indicator and then in excess of 3−5 cm. The solution with the precipitated sludge is heated to boiling, the precipitate is filtered off on the filter «white ribbon» and washed 3−4 times with warm water, containing in 1 DM10 cmof ammonia. The filter with precipitate was placed in a preheated to constant mass and weighed platinum crucible, incinerated and calcined at 1000−1100 °C to constant weight. After cooling in the desiccator the crucible and precipitate are weighed.
Simultaneously conduct control experience for contamination of reagents.
Mass concentration of sulfate of titanium 
, expressed in grams of titanium per 1 cmof a solution, calculated by the formula
,
where 
is the mass of the crucible with the precipitate of titanium dioxide, g;
— weight of crucible without precipitate titanium dioxide, g;
— the mass of the crucible with the sediment in a control experiment, g;
— weight of crucible without the sediment in a control experiment, g;
0,5996 — the ratio of titanium dioxide to titanium;
— the volume of sulfate solution of titanium, taken for installation of the titer, cm.
Preparation of a standard solution And may be of metallic titanium. For this 0.1 g of titanium metal is placed in a beaker with a capacity of 200−250 cm, 50 cm pouredsulphuric acid, diluted 1:2, and dissolved under heating. After dissolution in a beaker was added dropwise nitric acid to the bleaching solution and evaporated until the appearance of dense sulphuric acid fumes. The solution was cooled, carefully wash off the side of the Cup with water and again evaporated to the appearance of sulphuric acid fumes. After cooling, the solution is transferred to a volumetric flask with a capacity of 1 DM, made up to the mark with sulfuric acid diluted 1:20, and stirred.
Solution B: (prepared immediately before use): 10 cmsolution And placed in a volumetric flask with a capacity of 100 cm, made up to the mark with sulfuric acid diluted 1:20, and stirred.
1 cmof solution B contains 0,00001 g of titanium.
(Changed edition, Rev. N 1
).
2.3. Analysis
2.3.1. The weight of steel or cast iron weighing 0.5 g were placed in a glass with a capacity of 250 cmand dissolved in 25 cmof sulphuric acid, diluted 1:4 with a moderate heat, covered with a glass watch glass. After complete dissolution of the sample carefully poured drop by drop nitric acid until the termination of foaming and the excess of 1 cm. The solution was boiled to remove oxides of nitrogen, and then evaporated until the appearance of sulphuric acid fumes. The contents of the Cup cool, wash the walls of the beaker and watch glass with water, poured 30 cmof 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. In the analysis of cast irons or in the case of precipitation of silicic acid solution after dissolution of the salts was filtered through a filter «white ribbon» with a small number of filtrowanie mass and washed the precipitate and the filter 5−6 times with hot water. The filtrate and the washings collected in a volumetric flask with a capacity of 100 cm.
The filter with precipitate was placed in a platinum crucible, dried, incinerated and calcined at 800−900 °C. the Precipitate is moistened with 2−3 drops of sulphuric acid, diluted 1:4, poured 5−6 cmhydrofluoric acid and cautiously evaporated to sulphuric acid fumes. The residue in the crucibles was calcined for 5−10 minutes at 800−900 °C and fused with 1 g of potassium peacemaking. The melt is cooled, dissolved by heating in 20−30 cmof hydrochloric acid, diluted 1:9. The resulting solution was attached to the filtrate in a volumetric flask with a capacity of 100 cm. The solution in the flask was adjusted to the mark with water and mix. Part of the solution filtered through a dry filter into a dry flask, discarding first portion of filtrate.
In two volumetric flasks with a capacity of 100 cmis placed aliquote part of the solution to 25 cmwhen the mass fraction of titanium from 0.01 to 0.05% and at 10 cmwhen the mass fraction of titanium of 0.05−0.1%. Add 15 cmof a solution of ascorbic acid, stirred and incubated for 5−7 min. Then add 15 cmof hydrochloric acid diluted 1:1, and one flask of 10 cmsolution diantipyrylmethane. Then add 10 cmof hydrochloric acid diluted 1:1, and one flask of 10 cmsolution diantipyrylmethane. The solutions in flasks topped up to the mark with water and mix. After 40 min, measure the optical density of analyzed solution on a photoelectrocolorimeter with a filter having maximum transmission in the range of 390−405 nm or on a spectrophotometer at a wavelength of 395 nm. As a solution the comparison is used a solution prepared without adding diantipyrylmethane. The thickness of the absorbing layer of the cell is chosen so to obtain the optimal value of optical density.
Simultaneously with the execution of the analysis carried out control experience for contamination of reagents.
From the values of absorbance of each test solution subtract the value of optical density in the reference experiment. The mass of titanium is find a calibration chart or by comparison with a standard sample.
(Amended,
Izm. N 1).
2.3.2. Construction of calibration curve
Six glasses with a capacity of 250 cmis placed 0.5 g carbonyl iron or steel, similar in composition to the analyzed and do not contain titanium. In the determination of titanium in the range of 0.05−0.1% in five of them add a standard solution And in the amount of 2,5; 3,0; 4,0; 4,5; 5,0 cm, which corresponds to 0,00025; 0,0003; 0,0004; is 0 00 045; 0.0005 g of titanium. In the determination of titanium in the range of 0.01−0.05% in five glasses add standard solution B in an amount of 2,5; 5,0; 10,0; 20,0; 25,0 cm, which corresponds to 0,000025; 0,000050; 0,000100; 0,000200; 0,000250 g of titanium. The sixth glass is used for the reference experiment. Next, carry out analysis as specified in claim 2.3.1. On the found values of optical density and corresponding weight values of titanium to build the calibration graph. Allowed construction of calibration curve in the coordinates: the optical density is the mass fraction of titanium.
(Changed the wording. Izm. N 1).
2.4. Processing of the results
2.4.1. Mass fraction of titanium 
in percent is calculated by the formula
,
where is the mass of titanium in the sample was found in the calibration schedule g;
— the weight of the portion,
2.4.2. Norms of accuracy and norms control the accuracy of determining the mass fraction of titanium in the table.
| |
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The allowable divergence,%
|
| Mass fraction of titanium,% |
The error analysis results
 ,% |
two secondary results of the analysis performed under various conditions
 |
two parallel definitions  |
three parallel definitions  |
the results of the analysis of a standard sample certified values  |
| From |
0,005 |
to |
0,01 |
incl. |
0,0024 |
0,0030 |
0,0025 |
0,0030 |
0.0016 inch
|
| SV. |
0,01 |
« |
0,02 |
« |
0,004 |
0,004 |
0,004 |
0,004 |
0,002
|
| « |
0,02 |
« |
0,05 |
« |
0,006 |
0,007 |
0,006 |
0,007 |
0,004
|
| « |
0,05 |
« |
0,1 |
« |
0,010 |
0,013 |
0,011 |
0,013 |
0,007
|
(Changed the wording. Izm. N 1).
3. EXTRACTION-PHOTOMETRIC METHOD
3.1. The essence of the method
The method is based on formation of yellow colored coordination compounds of titanium with diantipyrylmethane and chloride tin, extracting it with chloroform, and measuring the light absorption of the extract at a wavelength of 395 nm.
3.2. Equipment and reagents
Equipment and reagents according to claim 2.2 with the addition of:
hydrochloric acid by the GOST 3118−77 or GOST 14261−77 and diluted 1:9;
chloroform according to GOST 20015−74;
tin metal granules according to normative-technical documentation;
tin dichloride 2-water on the other-09−5393−88, a freshly prepared solution of 200 g of chloride of tin dissolved in 145 cmhot hydrochloric acid. The solution is cooled, add a few granules tin and top up with water to 1 DM.
Carbonyl iron according to GOST 13610−79, a solution with a mass concentration of 20 g/DM: 2.0 g of iron carbonyl was placed in a beaker with a capacity of 250 cmand dissolved in 25 cmof sulphuric acid, diluted 1:4 with a moderate heat. After complete dissolution of the sample carefully poured drop by drop nitric acid until the termination of foaming and the excess of 1 cm. The solution was boiled to remove oxides of nitrogen, and then evaporated until the appearance of sulphuric acid fumes. The contents of the Cup cool, wash the side of the Cup 50 cmhydrochloric acid, diluted 1:9 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 hydrochloric acid diluted 1:9, and stirred.
(Changed edition, Rev. N 1
).
3.3. Analysis
3.3.1. The weight of steel or cast iron with a mass of 1 g (in mass fraction of titanium from 0.005 to 0.01%) and 0.5 g (when the mass fraction of titanium from 0.01 to 0.1%) were placed in a glass with a capacity of 250 cmand dissolved in 25 cmof sulphuric acid, diluted 1:4 with a moderate heat, covered with a glass watch glass. After complete dissolution of the sample carefully poured drop by drop nitric acid until the termination of foaming and the excess of 1 cm. The solution was boiled to remove oxides of nitrogen, and then evaporated until the appearance of sulphuric acid fumes. The contents of the Cup cool, wash the walls of the beaker and watch glass with water, poured 30 cmof hydrochloric acid diluted 1:9 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 hydrochloric acid diluted 1:9, and stirred. In the analysis of the iron solution is filtered through a filter «white ribbon» in a volumetric flask with a capacity of 100 cmand washed 5−6 times with hydrochloric acid diluted 1:9.
The filter with precipitate was placed in a platinum crucible, dried, incinerated and calcined at 800−900 °C. the Precipitate is moistened with 2−3 drops of sulphuric acid, diluted 1:4, poured 5−6 cmhydrofluoric acid and cautiously evaporated to sulphuric acid fumes. The residue in the crucibles was calcined for 5−10 minutes at 800−900 °C and fused with 1 g of potassium peacemaking. The melt is cooled, dissolved by heating in 20−30 cmof hydrochloric acid diluted 1:9, the resulting solution was attached to the filtrate in a volumetric flask with a capacity of 100 cm. The solution in the flask was adjusted to the mark with hydrochloric acid diluted 1:9, and stirred.
Aliquot part of the solution is equal to 20 cm(when the mass fraction of titanium from 0.005 to 0.05%) and 10 cm(when the mass fraction of titanium from 0.05 to 0.1%), were placed in a glass with a capacity of 100 cm, flow 15 cmof ascorbic acid solution and mix. After 5 minutes pour 15 cmof hydrochloric acid diluted 1:9, 10 cmdiantipyrylmethane and again stirred solution. After 40 min the solution was transferred to a separatory funnel with a capacity of 200 cm, washing the walls of the beaker with hydrochloric acid diluted 1:9, pour 5 cmof a solution of chloride of tin, mix and pour 20 cmof chloroform.
Separatory funnel shaken for 1 min and after separation of the layers the organic layer decanted into a volumetric flask with a capacity of 50 cm. The extraction is repeated twice, adding 5 cmof chloroform and collecting the organic layers to the same flask. The extract in the flask topped up to the mark with chloroform, stirred and filtered through a dry filter into a dry flask, which is stoppered. Measure the optical density of the colored extract on a photoelectrocolorimeter with a filter having maximum transmission in the range of 390−405 nm or on a spectrophotometer at a wavelength of 395 nm. As a solution the comparison used the chloroform.
The thickness of the absorbing layer of the cell is chosen so to obtain the optimal value of optical density.
Simultaneously with the execution of the analysis carried out control experience for contamination of reagents.
From the values of absorbance of each test solution subtract the value of optical density in the reference experiment.
The mass of titanium is find a calibration chart or by comparison with a standard sample.
(Modified redakts
ia, Rev. N 1).
3.3.2. Construction of calibration curve
Six glasses are placed at 10 cm(when the mass fraction of titanium 0,005−0,01%) or 5 cm(for the mass concentration of titanium of 0.01−0.05%) or 2.5 cm(for the mass concentration of titanium of 0.05−0.1%) solution of carbonyl iron, five of them consecutively poured 1; 2; 3; 4; 5 cmstandard solution B titanium, which corresponds to the 0.00001; 0,00002; 0,00003; 0,00004; 0,00005 g of titanium. The sixth glass is used for the reference experiment.
Liquid in the glasses poured at 15 cmof ascorbic acid solution and mix. After 5 minutes pour 15 cmof hydrochloric acid diluted 1:9, 10 cmdiantipyrylmethane solution and mixed again. The solution was prepared for extraction as described in section 3.3.1. When measuring light absorption in a solution of comparison, using the extract of the sixth glass, not containing titanium. On the found values of optical density and corresponding weight values of titanium to build the calibration graph. Allowed construction of calibration curve in the coordinates: the optical density is the mass fraction of titanium.
(Changed edition, Rev. N 1)
.
3.4. Processing of the results
3.4.1. Mass fraction of titanium (
) in percent is calculated by the formula
,
where is the mass of titanium in the sample was found in the calibration schedule g;
— the weight of the portion of the sample corresponding to aliquote part of the solution,
(Changed edition, Rev. N 1).
3.4.2. Norms of accuracy and norms control the accuracy of determining the mass fraction of titanium in the table.
(Changed edition, Rev. N 1).
