GOST 1953.13-79
GOST 1953.13−79 Bronze tin. Method for the determination of manganese (with Amendments No. 1, 2)
GOST 1953.13−79
Group B59
INTERSTATE STANDARD
BRONZE TIN
Methods for determination of manganese
Tin bronze.
Methods for the determination of manganese
AXTU 1709
Date of introduction 1981−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from
3. REPLACE GOST 1953.13−76
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
The designation of the reference document referenced |
Section number, paragraph, sub-paragraph |
GOST 8.315−97 |
4.4; 5.4.4 |
GOST 1953.1−79 |
1.1 |
GOST 3118−77 |
5.2 |
GOST 4197−74 |
2 |
GOST 4204−77 |
2 |
GOST 4461−77 |
2; 5.2 |
GOST 6008−90 |
5.2 |
GOST 6552−80 |
2 |
GOST 20490−75 |
2 |
GOST 25086−87 |
1.1; 4.4; 5.4.4 |
5. Limitation of actions taken by Protocol No. 5−94 of the Interstate Council for standardization, Metrology and certification (ICS 11−12−94)
6. EDITION with Amendments No. 1, 2 approved in February 1983, August 1990 (IUS 6−83, 11−90)
This standard sets the photometric and atomic absorption methods for the determination of manganese (0.05% to 0.3%) in tin bronze.
(Changed edition, Rev. N 2).
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis GOST 25086 with the Supplement according to claim 1.1 GOST 1953.1.
(Changed edition, Rev. N 1, 2).
2A. PHOTOMETRIC METHOD
2A.1. The essence of the method
The method is based on measuring the formed color of the permanganate ion after oxidation of manganese (II) to manganese (VII) ignobilis potassium.
Sec. 2A. (Added, Rev. N 2).
2. APPARATUS, REAGENTS AND SOLUTIONS
Photoelectrocolorimeter or spectrophotometer.
Nitric acid according to GOST 4461, diluted 1:1.
Orthophosphoric acid according to GOST 6552.
Sulfuric acid according to GOST 4204.
The mixture of acids to dissolve; prepared as follows: 200 cmnitric acid, diluted 1:1 were mixed with 10 cmof phosphoric acid and 50 cmof sulfuric acid.
Potassium cognately.
Potassium permanganate according to GOST 20490, 0.1 N. solution.
Sodium atomistically according to GOST 4197, a solution of 50 g/DM.
A standard solution of manganese; prepared as follows: 9.1 cmobtained with 0.1 N. solution of potassium permanganate is placed in a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix. The solution was stored in a flask made of dark glass.
1 cmof the solution contains 0.0001 g of manganese.
3. ANALYSIS
3.1. The sample of bronze with a weight of 1 g when the mass fraction of manganese from 0.05% to 0.1% and 0.2 g when the mass fraction of manganese from 0.1% to 0.3% is placed in a beaker with a capacity of 100 cm, 35 cm add amixture of acids, cover with a watch glass and dissolved under heating. After dissolution, the sample is rinsed glass and walls of beaker with water and boil for 1−2 min to remove the oxides of nitrogen. The solution was cooled, diluted with water to 50 cm, was added 0.3 g jednolitego potassium is heated nearly to boiling and allowed to stand in a water bath at 80−90 °C for about 20 min. After cooling, the solution is transferred to a volumetric flask with a capacity of 100 cm, made up to the mark with water, mix and measure optical density of solution in cuvette with thickness of absorbing layer 1 cm at a photoelectrocolorimeter with a green filter or on spectrophotometer at 528 nm. A solution of comparison, using the same sample solution, in which manganese acid reduced to divalent manganese by the addition dropwise of a solution of sodium attestatio.
3.2. Construction of calibration curve
In flasks with a capacity of 100 cmconsistently placed 0; 2,0; 4,0; 6,0; 8,0; 10,0 and 12.0 cmstandard solution of manganese, made up to the mark with water and measure the optical density of the solution, as stated in claim 3.1, using a solution not containing manganese as a solution of comparison.
4. PROCESSING OF THE RESULTS
4.1. Mass fraction () in percent is calculated by the formula
,
where — the amount of manganese was found in the calibration schedule g;
— the weight of the portion,
4.2. Discrepancies in the results of parallel definitions should not exceed the values of permissible differences (the rate of convergence for 3), specified in the table.
Mass fraction of sulfur, % |
, % |
, % |
From 0.05 to 0.10 incl. |
0,006 |
0,008 |
SV. Of 0.10 «to 0.20 « |
0,01 |
0,01 |
«To 0.20» to 0.30 « |
0,02 |
0,03 |
(Changed edition, Rev. N 2).
4.3. Discrepancies in the results analysis, 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 the table.
4.4. Control of accuracy of analysis results is carried out according to State standard samples of tin bronzes, re-approved by GOST 8.315, or by additives or by comparison of the results obtained by atomic absorption method, in accordance with GOST 25086.
4.5. The photometric method is used in case of disagreement in assessing the quality of tin bronzes.
4.3−4.5. (Added, Rev. N 2).
5. ATOMIC ABSORPTION METHOD FOR THE DETERMINATION OF MANGANESE
5.1.The essence of the method
The method is based on measuring the absorption of light by atoms of manganese formed during the introduction of the analyzed solution in the flame acetylene-air.
5.2. Apparatus, reagents and solutions
Atomic absorption spectrometer with a radiation source for manganese.
Nitric acid according to GOST 4461 and diluted 1:1.
Hydrochloric acid according to GOST 3118.
A mixture of acid: mix one volume of nitric acid with three volumes of hydrochloric acid.
Manganese GOST 6008.
The solution of manganese: 0.1 g of manganese dissolved by heating in 10 cmof nitric acid (1:1). The solution was transferred to a volumetric flask with a capacity of 1 DMand topped to the mark with water.
1 cmof the solution contains 0.0001 g of manganese.
5.3. Analysis
5.3.1. The weight of bronze weighing 0.1 g was dissolved with heating in 10 cmof a mixture of acids. The solution was transferred to a volumetric flask with a capacity of 100 cmand top up with water to the mark.
Measure the atomic absorption of manganese in the flame acetylene-air at a wavelength of 279.5 nm parallel to the calibration solutions.
5.3.2. Construction of calibration curve
In four of the five volumetric flasks with a capacity of 100 cmis placed 0,5; 1,0; 2,0 and 3,0 cmstandard solution of manganese. All flasks is poured 10 cmof the mixture of acids and then filled to the mark with water.
Measure the atomic absorption of manganese, as specified in clause
5.4. Processing of the results
5.4.1. Mass fraction of manganese () in percent is calculated by the formula
,
where is the concentration of manganese was found in the calibration schedule, g/cm;
— the volume of the sample solution, cm;
— the weight of the portion of the sample,
5.4.2. Discrepancies in the results of parallel definitions should not exceed the values of permissible differences (the rate of convergence for 3), specified in the table.
5.4.3. Discrepancies in the results analysis, 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 the table.
5.4.4. Control of accuracy of analysis results is carried out according to State standard samples of tin bronzes, re-approved by GOST 8.315, or by additives or by comparison of the results obtained by the photometric method according to GOST 25086.
Sec. 5. (Added, Rev. N 2).