GOST 15027.9-77
GOST 15027.9−77 Bronze without tin. Methods for determination of antimony (with Amendments No. 1, 2)
GOST 15027.9−77
Group B59
INTERSTATE STANDARD
BRONZE WITHOUT TIN
Methods for determination of antimony
Non-tin bronze.
Methods for the determination of antimony
AXTU 1709
Date of introduction 1979−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
2. APPROVED AND promulgated by the Decree of the State Committee of standards of Ministerial Council of the USSR from
3. REPLACE GOST 15027.9−69
4. The standard fully complies ST SEV 1542−79
5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced |
Section number, paragraph, sub-paragraph |
| GOST 435−77 |
2.2 |
| GOST 493−79 |
Chapeau |
| GOST 614−97 |
Chapeau |
| GOST 1089−82 |
2.2, 3.2, 5.2, 6.2 |
| GOST 3118−77 |
2.2, 3.2, 5.2, 6.2 |
| GOST 3760−79 |
2.2, 3.2 |
| GOST 4166−76 |
2.2, 3.2 |
| GOST 4197−74 |
2.2, 3.2 |
| GOST 4204−77 |
2.2, 3.2, 5.2, 6.2 |
| GOST 4461−77 |
2.2, 3.2, 5.2, 6.2 |
| GOST 5456−79 |
2.2 |
| GOST 5789−78 |
2.2, 3.2 |
| GOST 6691−77 |
5.2 |
| GOST 10484−78 |
2.2 |
| GOST 10929−76 |
2.2, 3.2, 5.2 |
| GOST 18175−78 |
5.2 |
| GOST 20490−75 |
Chapeau |
| GOST 25086−87 |
2.2, 5.2 |
| THAT 6−09−4011−75 |
5.2 |
| THAT 6−09−5384−88 |
2.2, 3.2 |
6. Limitation of actions taken by Protocol No. 3−93 Interstate Council for standardization, Metrology and certification (ICS 5−6-93)
7. EDITION with Amendments No. 1, 2 approved in February 1983, March 1988 (IUS 6−83, 6−88)
This standard specifies the extraction-photometric method for the determination of antimony with crystal violet (when the mass fraction of antimony from 0.001% to 0.6%), extraction-photometric method for the determination of antimony with brilliant green (when the mass fraction of antimony from 0.1% to 0.65%) and atomic absorption method for the determination of antimony (in mass fraction of antimony from 0.001% to 0.05% and from 0.05% to 0.6%) in tin bronze according to GOST 18175, GOST and GOST 614 493.
(Changed edition, Rev. N 1).
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis GOST 25086 with the addition of sec. 1 GOST 15027.1.
(Changed edition, Rev. N 1).
2. EXTRACTION-PHOTOMETRIC METHOD FOR THE DETERMINATION OF ANTIMONY WITH CRYSTAL VIOLET
2.1. The essence of the method
The method is based on extraction of pentavalent antimony toluene in the form of hexachlorobuta crystal violet and measuring the optical density of the extract after the separation of antimony by its coprecipitation with manganese dioxide and dissolve the precipitate in hydrochloric acid.
2.2. Apparatus, reagents and solutions
Photoelectrocolorimeter or spectrophotometer.
Hydrofluoric acid according to GOST 10484.
Nitric acid according to GOST 4461 and diluted 1:1 and 1:100.
Hydrochloric acid according to GOST 3118 and diluted 7:3, 3:1 and 1:1.
Sulfuric acid according to GOST 4204, diluted 1:1 and 1:5 solution of 0.25 mol/DM.
Ammonia water according to GOST 3760 and diluted 1:1.
Potassium permanganate according to GOST 20490, a solution of 10 g/DM.
Manganese sulfate according to GOST 435, a solution of 50 g/DM.
Tin dichloride TU 6−09−5384, solution 100 g/lin hydrochloric acid, diluted 1:1.
Sodium atomistically according to GOST 4197, solution 100 g/DM.
Urea according to GOST 6691, saturated solution; prepared as follows: 100 g of urea dissolved in 100 cmof hot water.
Crystal violet solution 2 g/DM.
Toluene according to GOST 5789.
Sodium sulphate anhydrous according to GOST 4166.
Cerium (IV) sulfate solution 0.4 g/lin 0.25 mol/DM
sulfuric acid.
Hydroxylamine hydrochloric acid according to GOST 5456, a solution of 1 g/DM.
Antimony GOST 1089 brand Su00.
Solutions of antimony.
Solution A, prepared as follows: 0.1 g of antimony is dissolved by heating in 50 cmof concentrated sulfuric acid. The solution was transferred to a volumetric flask with a capacity of 1 DM
, 175 cm poured
sulphuric acid, diluted 1:1, cooled, made up to the mark with water and mix.
1 cmof the solution contains 0.0001 g of antimony.
Solution B is prepared as follows: 10 cmof solution A is placed in a volumetric flask with a capacity of 100 cm
, 70 cm pour
concentrated hydrochloric acid, diluted to the mark with water and mix.
1 cmof solution B contains 0,00001 g of antimony.
(Amended
, Edit. N 1).
2.3. Analysis
2.3.1. A portion of the bronze mass, given in table.1, dissolved by heating in 5−10 cmof nitric acid, diluted 1:1 in glass with a capacity of 250 cm
, covered with watch glass. The solution was cooled, the watch glass rinsed with water. The solution is diluted with water to a volume of 50 cm
. In the analysis of silicon bronze alloy a portion of 0.5 g is placed in a platinum Cup, add 10 cm
of nitric acid, diluted 1:1, 2 cm
hydrofluoric acid and heated until dissolved. After cooling the walls of the Cup is washed with a small amount of water, add 3 cm
of concentrated sulfuric acid and evaporated to start the selection of a white smoke of sulfuric acid. The Cup is cooled, wash the walls with a little water and repeat the evaporation to start the selection of a white smoke of sulfuric acid. After cooling, dissolve salt in 5 cm
of nitric acid, diluted 1:1, transfer the solution into a glass with a capacity of 250 cm
, and diluted with water to a volume of 50 cm
, then (for conventional and silicon-bronze), the resulting solution is neutralized with ammonia until the appearance of the precipitate copper hydroxide, which persisted during stirring, and add a pipette of 0.5 cm
of nitric acid, diluted 1:1, then add 1 cm
of solution of potassium permanganate, cover the beaker watch glass and the solution is heated nearly to boiling. Then add 1 cm
of a solution of manganese sulphate and boil for 2 minutes the Solution is allowed to stand for 1 h, after which the precipitate was filtered off on a tight filter, washing out the beaker and the residue 4−5 times with hot nitric acid, diluted 1:100 prior to the disappearance of the colour of copper nitrate.
The filter with the sediment was transferred to a beaker, which was carried out the precipitation, add 10−15 cmof concentrated sulfuric acid, 20−25 cm
of concentrated nitric acid and evaporate the solution to start the selection, the dense white smoke of sulfuric acid. If the solution is colored, add another 5−10 cm
of concentrated nitric acid and repeat the evaporation. The glass is cooled, the side of the Cup washed with water and evaporated the solution until damp salts. After cooling, to the residue is added 7 cm
of hydrochloric acid diluted 7:3, and heated at a temperature of 80−95 °C until complete dissolution of salts. The solution was transferred to a separatory funnel with a capacity of 100−150 cm
, washed the Cup 3 cm
of hydrochloric acid diluted 7:3 and it bring the solution volume up to 10 cm
. When the mass fraction of antimony in excess of 0.01% solution transferred to an appropriate volumetric flask (see table 1) and dilute to the mark with hydrochloric acid diluted 7:3.
Table 1
| Mass fraction of SB, % | The mass of charge, g | The volume aliquote part of the solution, cm |
The volume of solution, cm |
| From 0.001 to 0.005 |
1 | All |
- |
| SV. 0,005 «0,01 |
0,5 | All | - |
| «To 0.01» to 0.05 |
1 | 10 | 100 |
| «0,05» 0,1 |
1 | 5 | 100 |
| «0,1» 0,2 |
0,5 | 10 | 250 |
| «0,2» 0,4 |
0,5 | 5 | 250 |
| «0,4» 0,6 |
0,2 | 5 | 250 |
In this case, select the specified in table.1 aliquot part of the solution in the separatory funnel with a capacity of 150 cmand add hydrochloric acid diluted 7:3, to a volume of 10 cm
. Add to separatory funnel, drop 1−2 drops of solution of tin dichloride to a bleaching solution, mix and leave for 1 min Then add 1 cm
of a solution of sodium attestatio, funnel closed with a stopper and shake for 2 minutes Open the funnel. After 2 min add 1 cm
of a solution of urea and stirred for 30 s. Then add the 68 cm
of water, 10 drops of crystal violet solution, mix, add 25 cm
of toluene and extracted for 1 min.
In another embodiment, added to 10 cmof hydrochloric acid solution in a separating funnel 0.5 cm
of a solution of cerium (IV), stirring after 1 min. add 1 cm
of a solution of hydroxylamine hydrochloride, stirred and after a minute add 60 cm
of water. The solution was stirred, was added 50 cm
toluene, 10 drops of crystal violet and extracted for 1 min.
After phase separation, the lower aqueous layer is discarded and the organic layer is poured into a dry beaker with a capacity of 50 cmcontaining 0.2 g of anhydrous sodium sulfate.
Measure the optical density of the extract on photocolorimeter with a red filter (=590−610 nm) in a cuvette with a length of 2 cm or a spectrophotometer with a cuvette length of 1 cm at a wavelength of 610 nm. Solution comparison is toluene.
Note. In that case, if the analysis will not be completed during the day, it can be interrupted after the deposition of antimony with manganese dioxide or after evaporation of a solution of sulfuric acid.
The content of antimony found by calibration g
Rafik.
2.3.2. Construction of calibration curve
In a separating funnel with a capacity of 150 cmadministered 0; 0,5; 1,0; 2,0; 3,0; 4,0 and 5.0 cm
of a solution and add hydrochloric acid diluted 7:3, up to 10 cm
. Add 1−2 drops of solution of tin dichloride, mix and leave for 1 min, further analysis are as indicated in claim
The found values of optical density of solutions and their corresponding concentrations of antimony in building the calibration curve.
2.3.1−2.3.2. (Changed edition, Rev. N 1).
2.4. Processing of the results
2.4.1. Mass fraction of antimony () in percent is calculated by the formula
where is the mass of antimony, was found in the calibration schedule g;
— the weight of the portion corresponding to aliquote part of the solution,
2.4.2. The absolute discrepancies in the results of parallel measurements (the rate of convergence) must not exceed the permissible values given in table.1A.
Table 1A
| Mass fraction of SB, % |
|
|
| From 0.001 to 0.005 incl. |
0,0005 | 0,001 |
| SV. 0,005 «0,01 |
0,001 | 0,002 |
| «0,01» 0,025 |
0,002 | 0,005 |
| «Of 0.025» to 0.05 |
0,004 | 0,01 |
| «0,05» 0,10 |
0,010 | 0,02 |
| «To 0.10» to 0.20 |
0,020 | 0,05 |
| «0,20» 0,65 |
0,040 | 0,10 |
(Changed edition, Rev. N 2).
2.4.3. The absolute discrepancies of the analysis results obtained in two different laboratories or two of the results of analysis obtained in the same laboratory but under different conditions (a measure of reproducibility) shall not exceed the values given in table.1A.
2.4.4. Control of accuracy of analysis results
Control of accuracy of analysis results is carried out according to State standard samples without tin bronzes, certified in the prescribed manner, a comparison of the results obtained photometric and atomic absorption methods or by the method of additives in accordance with GOST 25086.
2.4.3,
3. EXTRACTION-PHOTOMETRIC METHOD FOR THE DETERMINATION OF ANTIMONY WITH BRILLIANT GREEN
3.1. The essence of the method
The method is based on extraction with toluene painted in the blue-green color hexachlorobuta brilliant green and measurement of the optical density of the extract.
The method allows to determine the antimony in the background all components of bronze without their prior separation.
3.2. Apparatus, reagents and solutions
Photoelectrocolorimeter or spectrophotometer.
Nitric acid according to GOST 4461, diluted 1:1.
Hydrochloric acid according to GOST 3118, diluted 3:1 and 1:1.
Sulfuric acid according to GOST 4204, and diluted 1:5.
Tin dichloride on the other 6−09−5384, a freshly prepared solution of 100 g/lin hydrochloric acid, diluted 1:1.
Sodium atomistically according to GOST 4197, solution 100 g/DM.
Urea according to GOST 6691 saturated solution; prepared as follows: 100 g of urea dissolved in 100 cmof hot water.
Diamond green, a solution of 2 g/DM.
Toluene according to GOST 5789.
Antimony GOST 1089 brand Su00.
Standard solutions of antimony.
Solution A, prepared as follows: 0.05 g of antimony is dissolved by heating in 25 cmconcentrated sulphuric acid. The solution was cooled, transferred to a volumetric flask with a capacity of 500 cm
, made up to the mark with sulfuric acid diluted 1:5, and stirred.
1 cmof the solution contains 0.0001 g of antimony.
Solution B is prepared as follows: 10 cmof the solution And transferred to a volumetric flask with a capacity of 100 cm
, made up to the mark with hydrochloric acid, diluted 3:1, and stirred.
1 cmof solution B contains 0,00001 g of antimony.
Solution B is prepared on the day of application.
Sodium sulphate anhydrous according to GOST 4
166.
3.3. Analysis
3.3.1. The sample of bronze with a mass of 0.1 g dissolved in 10 cmof nitric acid, diluted 1:1 in glass with a capacity of 250 cm
, covered with watch glass during heating. After dissolution of the sample clock glass and sides of beaker rinse with water, add 3 cm
of concentrated sulfuric acid and evaporate until a white smoke of sulfuric acid. Cool the solution, wash the side of the Cup with a little water and repeat the evaporation. To the residue poured 20 cm
of hydrochloric acid, diluted 3:1, dissolved salts and transferred to a volumetric flask with a capacity of 100 cm
, and then topped to the mark with hydrochloric acid, diluted 3:1, and stirred.
In a separating funnel with a capacity of 150 cmtaken 5 cm
of the analyzed solution, add two drops of solution of chloride of tin, mix and leave for 1 min and Then injected 1 cm
of solution azotistykh sodium, mixed well and left for 5 min. then add 1 cm
of a solution of urea, mix 30 s and diluted with water to 50 cm
. Then injected 1 cm
of solution of brilliant green, 30 cm
of toluene and extracted by shaking for 1 min.
After separation of phases the lower aqueous layer is discarded and the organic layer is poured into a dry beaker with a capacity of 50 cmcontaining 0.2 g of anhydrous sodium sulfate. After 10 minutes measure the optical density on the spectrophotometer at a wavelength of 640 nm or photoelectrocolorimeter with a red lens filter when
=590−610 nm in a cuvette length of 1 cm with a Solution of comparison is toluene. The content of antimony found by the calibration
graphics.
3.3.2. Construction of calibration curve
In a separating funnel with a capacity of 150 cmadministered 0; 0,5; 1,0; 1,5; 2,0; 2,5; 3,0 and 3.5 cm
of a solution and add hydrochloric acid, diluted 3:1, up to 5 cm
. Add two drops of solution of tin dichloride, and then mix and leave for 1 min then inject 1 cm
of a solution of sodium attestatio and further analysis are as indicated in claim
The found values of optical density of solutions and their corresponding grades of antimony building a calibration curve.
4. PROCESSING OF THE RESULTS
4.1. Mass fraction of antimony () in percent is calculated by the formula
where is the mass of antimony, was found in the calibration schedule g;
— the weight of the portion corresponding to aliquote part of the solution,
4.2. The absolute discrepancies in the results of parallel measurements (the rate of convergence) must not exceed the permissible values given in table.1A.
(Changed edition, Rev. N 2).
4.3. The absolute discrepancies of the analysis results obtained in two different laboratories or two of the results of analysis obtained in the same laboratory but under different conditions (a measure of reproducibility) shall not exceed the values given in table.1A.
4.4. Control of accuracy of analysis results
Control of accuracy of analysis results is carried out according to claim
4.3, 4.4. (Added, Rev. N 2).
5. ATOMIC ABSORPTION METHOD for the DETERMINATION of ANTIMONY (IN MASS FRACTION of ANTIMONY from 0.001% to 0.05%)
5.1. The essence of the method
The method is based on measuring the absorption of light by atoms of antimony, formed by the introduction of the analyzed solution in the flame acetylene-air after prior extraction of antimony by its coprecipitation with manganese dioxide.
5.2. Apparatus, reagents and solutions
Atomic absorption spectrometer with a radiation source for antimony.
Nitric acid according to GOST 4461 diluted 1:1 and 1.5 mol/DMsolution.
Sulfuric acid according to GOST 4204, diluted 1:1, 1:4, and the solution of 2.5 mol/DM.
Hydrochloric acid according to GOST 3118, solution 1 mol/DM.
Hydrofluoric acid according to GOST 10484.
Ammonia water according to GOST 3760.
Manganese nitrate on the EAST 6−09−4011, a solution of 20 g/DM.
Potassium permanganate according to GOST 20490, a solution of 10 g/DM.
Hydrogen peroxide according to GOST 10929.
Antimony GOST 1089 with a mass fraction of antimony is not less than 99.9%.
Standard solutions of antimony.
Solution A, prepared as follows: 0.25 g of antimony is dissolved by heating in 10 cmof sulphuric acid, the solution was cooled, transferred to a volumetric flask with a capacity of 500 cm
and topped to the mark with a solution of 2.5 mol/DM
sulfuric acid.
1 cmof the solution contains 0.0005 g of antimony.
Solution B is prepared as follows: 10 cmof solution A is placed in a volumetric flask with a capacity of 100 cm
and then filled to the mark with a solution of 2.5 mol/DM
sulfuric acid.
1 cmof solution B contains 0,00005 g
antimony.
5.3. Analysis
5.3.1. For bronzes with a mass fraction of silicon to 0.05%
The weight of bronze weighing 2 g were placed in a glass with a capacity of 250 cmand dissolved by heating in 20 cm
of nitric acid, diluted 1:1. Nitrogen oxides are removed by boiling and the solution diluted with water to a volume of 50 cm
. Add 5 cm
of a solution of nitrate of manganese, the solution is neutralized with ammonia until the appearance of the precipitate copper hydroxide, add 18 cm
of nitric acid, diluted 1:1, and water to a volume of 90 cm
. The solution is heated to boiling, add 10 cm
of a solution of potassium permanganate, and boil for 2 min. after 30 min the precipitate was filtered off on a tight filter and washed the beaker and the precipitate 4−5 times a hot solution of 1.5 mol/DM
nitric acid. The deployed filter is washed with water in a glass, which conducted the deposition, the filter is washed with 10 cm
of hot sulfuric acid solution, diluted 1:4 with a few drops of hydrogen peroxide solution and then with water.
The washed filter is discarded and the solution was evaporated to wet salts. After cooling, add 8 cmof solution of 1 mol/DM
hydrochloric acid, the mass fraction of antimony and 0.02% solution transferred to a volumetric flask or a test tube calibration up to 10 cm
, while the mass fraction of antimony in excess of 0.02% solution transferred to a volumetric flask with a capacity of 25 cm
and then filled to the mark with a solution of 1 mol/DM
of hydrochloric acid.
Measure the atomic absorption of antimony in the flame acetylene-air at a wavelength of 217,6 or the amount of 231.1 nm in parallel with the calibration of the races
torami.
5.3.2. For bronzes, with a mass fraction of silicon in excess of 0.05%
The weight of bronze weighing 2 g was placed in a platinum Cup and dissolved by heating in 20 cmof nitric acid, diluted 1:1, and 2 cm
hydrofluoric acid. After dissolution, add 10 cm
sulphuric acid diluted 1:1, and the solution was evaporated until a white smoke of sulfuric acid. The residue is cooled, rinse the walls of the Cup with water and evaporated again until a white smoke of sulfuric acid. The residue is cooled, the walls of the Cup should be rinsed with 20 cm
of water, heat the solution transferred to a beaker with a capacity of 250 cm
, top up with water to a volume of 50 cm
, add 5 cm
of a solution of manganese nitrate and further analysis is carried out as specified in clause 5.3.1
.
5.3.3. Construction of calibration curve
In seven of eight glasses with a capacity of 250 cmis placed 0,4; 1,0; 2,0; 4,0; 6,0; 8,0 and 10.0 cm
standard solution B. In all the cups add water to a volume of 50 cm
, add 5 cm
of a solution of manganese nitrate and further analysis is carried out as specified in clause
5.4. Processing of the results
5.4.1. Mass fraction of antimony () in percent is calculated by the formula
where is the concentration of antimony was found in the calibration schedule, g/cm
;
— the volume of the final sample solution, cm
;
— the weight of the portion,
5.4.2. The absolute discrepancies in the results of parallel measurements (the rate of convergence) must not exceed the permissible values given in table.1A.
(Changed edition, Rev. N 2).
5.4.3. The absolute discrepancies of the analysis results obtained in two different laboratories or two of the results of analysis obtained in the same laboratory but under different conditions (a measure of reproducibility) shall not exceed the values given in table.1A.
5.4.4. Control of accuracy of analysis results
Control of accuracy of analysis results is carried out according to claim
5.4.3,
6. ATOMIC ABSORPTION METHOD for the DETERMINATION of ANTIMONY (IN MASS FRACTION of ANTIMONY from 0.05% to 0.6%)
6.1. The essence of the method
The method is based on measuring the absorption of light by atoms of antimony, formed by the introduction of the analyzed solution in the flame acetylene-air.
6.2. Apparatus, reagents and solutions
Atomic absorption spectrometer with a radiation source for antimony.
Nitric acid according to GOST 4461.
Hydrochloric acid according to GOST 3118 and solutions 2 and 1 mol/DM.
A mixture of acids, is prepared as follows: the amount of nitric acid mixed with three volumes of hydrochloric acid.
Sulfuric acid according to GOST 4204.
Antimony GOST 1089 with a mass fraction of antimony is not less than 99.9%.
Standard solution of antimony; prepared in the following way: 0.25 g of antimony is dissolved by heating in 10 cmof sulphuric acid, the solution was cooled, diluted with a solution of 2 mol/DM
of hydrochloric acid, transferred to a volumetric flask with a capacity of 500 cm
and topped to the mark with a solution of 2 mol/DM
of hydrochloric acid.
1 cmof the solution contains 0.0005 g of antimony.
6.3. Analysis
6.3.1. The sample of bronze with a weight of 1 g was placed in a beaker with a capacity of 250 cmand dissolved by heating in 10 cm
of a mixture of acids. The solution was cooled, transferred to a volumetric flask with a capacity of 100 cm
and then filled to the mark with a solution of 1 mol/DM
of hydrochloric acid.
Measure the atomic absorption of antimony in the flame acetylene-air at a wavelength of 217,6 or the amount of 231.1 nm parallel to the calibration solutions.
6.3.2. Construction of calibration curve
In nine out of ten volumetric flasks with a capacity of 100 cmplaced 0,4; 1,0; 2,0; 4,0; 6,0; 8,0; 10,0; 12,0 and 14.0 cm
standard solution of antimony and topped to the mark with 2 mol/DM
hydrochloric acid solution.
Measure the atomic absorption of antimony as described in Chapter
6.4. Processing of the results
6.4.1. Mass fraction of antimony () in percent is calculated by the formula
where is the concentration of antimony was found in the calibration schedule, g/cm
;
— the volume of the final sample solution, cm
;
— the weight of the portion,
6.4.2. The absolute discrepancies in the results of parallel measurements (the rate of convergence) must not exceed the permissible values given in table.1A.
(Changed edition, Rev. N 2).
6.4.3. The absolute discrepancies of the analysis results obtained in two different laboratories or two of the results of analysis obtained in the same laboratory but under different conditions (a measure of reproducibility) shall not exceed the values given in table.1A.
6.4.4. Control of accuracy of analysis results
Control of accuracy of analysis results is carried out according to claim
6.4.3,
