GOST 1953.4-79
GOST 1953.4−79 Bronze tin. Methods for determination of phosphorus (with Amendments No. 1, 2)
GOST 1953.4−79
Group B59
INTERSTATE STANDARD
BRONZE TIN
Methods for determination of phosphorus
Tin bronze.
Methods for the determination of phosphorus
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. The standard fully complies ST SEV 1531−79
4. REPLACE GOST 1953.4−74
5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
The designation of the reference document referenced |
The number of the paragraph, subparagraph |
GOST 8.315−97 |
2.4.4, 3.4.4 |
GOST 613−79 |
Chapeau |
GOST 614−97 |
Chapeau |
GOST 1953.1−79 |
1.1 |
GOST 1953.9−79 |
2.2 |
GOST 2062−77 |
3.2 |
GOST 3118−77 |
2.2, 3.2 |
GOST 3760−79 |
3.2 |
GOST 3765−78 |
2.2, 3.2 |
GOST 4144−79 |
3.2 |
GOST 4198−75 |
2.2 |
GOST 4217−77 |
3.2 |
GOST 4328−77 |
3.2 |
GOST 4461−77 |
3.2 |
GOST 5017−74 |
Chapeau |
GOST 9336−75 |
2.2 |
GOST 9656−75 |
2.2 |
GOST 10929−76 |
2.2 |
GOST 18300−87 |
3.2 |
GOST 20490−75 |
3.2 |
GOST 22180−76 |
3.2 |
GOST 22867−77 |
3.2 |
GOST 25086−87 |
1.1, 2.4.4, 3.4.4 |
6. Limitation of actions taken by Protocol No. 5−94 of the Interstate Council for standardization, Metrology and certification (ICS 11−12−94)
7. EDITION with Amendments No. 1, 2 approved in February 1983, August 1990 (IUS 6−83,11−90)
This standard sets the photometric method for the determination of phosphorus (from 0.005% to 1.2%) and titrimetric method (0.3% to 1.2%) in tin bronze according to GOST 5017, GOST GOST 613 and 614.
The standard fully complies ST SEV 1531−79.
(Changed edition, Rev. N 1, 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).
2. The PHOTOMETRIC METHOD for the DETERMINATION of PHOSPHORUS (from 0.01% to 0.5%)
2.1. The essence of the method
The method is based on formation of yellow phosphomolybdenum complex and the measurement of its optical density.
2.2. Apparatus, reagents and solutions
Photoelectrocolorimeter or spectrophotometer.
Hydrochloric acid according to GOST 3118.
Nitric acid according to GOST 4461 and diluted 2:3, 1:1 and 1:5.
Boric acid according to GOST 9656, a solution of 40 g/DM.
Ammonia water according to GOST 3760.
Potassium permanganate according to GOST 20490, a solution of 10 g/DM.
The mixture of acids to dissolve is prepared as follows: 320 cmof concentrated nitric acid and 120 cmof hydrochloric acid diluted with water to 1000 cm.
Ammonium undeviatingly meta GOST 9336; is prepared as follows: 2.5 g of ammonium anadalucia dissolved in 500−700 cmof hot water in a volumetric flask with a capacity of 1 DM, the solution is cooled to room temperature, add 20 cmof nitric acid, made up to the mark with water, mixed and filtered.
Ammonium molybdate according to GOST 3765, recrystallized from alcoholic solution, a freshly prepared solution of 100 g/DM(recrystallization of ammonium molybdate according to GOST 1953.9. Determination of silicon).
Hydrogen peroxide (perhydrol) according to GOST 10929, 3% solution.
Potassium phosphate according to GOST odnosemjannyj 4198.
The standard solutions of phosphorus is prepared as follows: 0,4395 g of single phosphate or potassium 0,4586 g twosemester sodium phosphate (previously dried at 105 °C to constant weight) was placed in a volumetric flask with a capacity of 250 cm(solution A), 500 cm(solution B) and 1000 cm(In solution), dissolved in water, made up to the mark with water and mix.
Solution A contains 0.0004 g of phosphorus.
Solution B contains 0.0002 g of phosphorus.
The solution contains 0.0001 g fo
store.
2.3. Analysis
2.2−2.3. (Changed edition, Rev. N 1).
2.3.1. The sample of bronze with a weight of 1 g when the mass fraction of phosphorus from 0.005% to 0.1% is placed in a beaker with a capacity of 250−300 cm, add 20 cmof the mixture of acids for dissolving, the beaker cover watch glass, and dissolve first in cold and then when heated to complete dissolution of the sample. The solution is poured 1 cmof hydrogen peroxide, heated to boiling and boiled for 3 min to remove the oxides of nitrogen (do not allow the violent and prolonged boiling of the solution).
Walls of glass and the glass is then rinsed with water, poured 10 cmof the solution vadeevaloo ammonium 10 cmof ammonium molybdate solution, mix well, cool and transfer the solution into volumetric flask with a capacity of 50 cm, made up to the mark with water and mix.
Optical density of the solution is measured on a photoelectrocolorimeter with a blue filter in a cell with thickness of the absorbing layer 3 cm or a spectrophotometer cuvette absorbing layer 1 cm at a wavelength of 440 nm.
A solution of comparison, using the solution of the same sample, but without adding vadeevaloo ammonium molybdate and ammonium.
2.3.2. Construction of calibration curve
In a volumetric flask with a capacity of 50 cmplaced 0; 0,5; 1,0; 2,0; 4,0; 6,0; 8,0; 10,0; 12,0 and 14.0 cmstandard solution Into the phosphorus and 15 cmof the mixture of acids, 1 cmof hydrogen peroxide. Further analysis is carried out as specified in clause
Optical density of the solution is measured relative to the solution not containing phosphorus.
2.3.1,
2.3.3. The weight of bronze weighing 0.5 g when the mass fraction of phosphorus in excess of 0.1% was placed in a beaker with a capacity of 100 cm, add 20 cmof the mixture of acids to dissolve and moderately heated to complete dissolution. Add 1 cmof hydrogen peroxide solution and gently boil for 3−5 minutes, avoiding loud and prolonged boiling. Then add 10 cmof a solution of ammonium anadalucia, cooled, transferred to a volumetric flask with a capacity of 100 cm, add 10 cmof molybdate ammonium solution, made up to the mark with water and mix. After 5 min measure the optical density of the solution on a photoelectrocolorimeter with a blue filter or on a spectrophotometer at a wavelength of 470 nm in a cuvette with a thickness of absorbing layer 1 cm with a Solution of comparison is the sample solution, which is not a solution of molybdate of ammonium.
2.3.4. Construction of calibration curve
Ten cups with a capacity of 100 cmis placed 0.5 g of copper and eight of them add 1,0; 2,0; 3,0; 5,0 and 10 cmstandard solution B; 8,0; 10,0 and 15,0 cmstandard solution A.
All glasses add 20 cmof a mixture of acids and then do as described in claim
According to the obtained results build a calibration curve.
2.3.3,
2.4. Processing of the results
2.4.1. Mass fraction of phosphorus () in percent is calculated by the formula
,
where is the mass of phosphorus was found in the calibration schedule g;
the weight of bronze,
2.4.2. 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 phosphorus, % |
, % |
, % |
From 0.005 to 0.01 incl. |
0,001 |
0,001 |
SV. 0,01 «0,02 « |
0,002 |
0,003 |
«0,02» 0,05 « |
0,003 |
0,004 |
«0,05» 0,10 « |
0,005 |
0,007 |
«0,1» 0,2 « |
0,01 |
0,01 |
«0,2» 0,5 « |
0,02 |
0,03 |
«0,5» 0,8 « |
0,03 |
0,04 |
«0,8» 1,2 « |
0,05 |
0,07 |
(Changed edition, Rev. N 2).
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.
2.4.4. 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 comparing the results obtained with titrimetric method, in accordance with GOST 25086.
2.4.3,
3. TITRIMETRIC METHOD for the DETERMINATION of PHOSPHORUS (from 0.3% to 1.2%)
3.1.The essence of the method
The method is based on the precipitation of phosphorus in the form of phosphoromolybdate ammonium, dissolving the precipitate in alkali titrated solution and the titration of the excess of its acid solution.
3.2. Reagents and solutions
Nitric acid according to GOST 4461 and diluted 1:1.
Hydrochloric acid according to GOST 3118 and diluted 1:1 and 0.1 mol/DM.
Bromatologia acid according to GOST 2062.
Oxalic acid according to GOST 22180.
The mixture of acids to dissolve, freshly prepared; prepared as follows: mix one volume of nitric acid and three volumes of hydrochloric acid.
Oxalic acid 0.05 mol/DMsolution; prepared as follows: 6,3034 g of oxalic acid, previously dried at 105 °C, placed in a volumetric flask with a capacity of 1 DM, is dissolved in 100 cmof water, made up to the mark with water and mix.
Ammonia water according to GOST 3760.
Potassium permanganate according to GOST 20490, a solution of 40 g/DM.
Potassium atomistically according to GOST 4144, a solution of 50 g/DM.
Potassium nitrate according to GOST 4217, solution 20 g/DM.
Ammonium nitrate according to GOST 22867.
Ammonium molybdate according to GOST 3765.
Solution molibdate reagent; prepared as follows: 80 g ammonium molybdate are dissolved cold in 640 cmof water to which was added 160 cmof ammonia, and the solution poured in a thin stream with constant stirring into a mixture consisting of 720 cmof water and 480 cmof concentrated nitric acid, and mix. After 3−5 days, the solution was filtered.
The technical rectified ethyl alcohol according to GOST 18300.
Phenolphthalein by ND, a solution of 10 g/lin ethanol.
Sodium hydroxide according to GOST 4328, 0.1 mol/DMsolution; prepared as follows: 4 g of sodium hydroxide were placed in a glass with a capacity of 300 cm, dissolved in boiled water, cooled, transferred to a volumetric flask with a capacity of 1 DM, made up to the mark with water and mix.
Coefficient setting molarity of sodium hydroxide solution 25 cmof 0.1 mol/DMsolution of sodium hydroxide was placed in a flask with a capacity of 250 cm. Add 2−3 drops of phenolphthalein, and stirring continuously, titrate with 0.05 mol/DMsolution of oxalic acid until discoloration of the solution.
The ratio of the molarity of sodium hydroxide is calculated by the formula
,
where — the volume of 0.05 mol/DMsolution of oxalic acid consumed for titration, sm.
3.3. Analysis
A sample of alloy weighing 1 g is placed in a conical flask with a capacity of 250 cm, add 20 cmof a mixture of acid, cover with watch glass and dissolved under heating. The glass is rinsed with concentrated hydrochloric acid, the solution is evaporated to a volume of 2−3 cm, add 10 cmbromatological acid and evaporated to dryness. Into the flask add 10 cmof concentrated hydrochloric acid and again evaporated to dryness. Evaporation with concentrated hydrochloric acid repeated 3−4 times for complete removal of tin. To the dry residue add 10 cmof hydrochloric acid diluted 1:1 add 80−100 cmof water and heated to 60−70 °C to dissolve the salts. Add potassium permanganate solution until the precipitation of manganese dioxide, poured dropwise a solution of potassium attestatio to the disappearance of the precipitate of manganese dioxide. Then add 10 g of ammonium nitrate and 30 cmsolution molibdate reagent, mix well for 3−5 min to loss yellow phosphoromolybdate and allowed to stand overnight.
The precipitate was filtered off on a tight filter with filtrowanie ground. The glass and the filter cake washed with potassium nitrate solution until the disappearance of acid reaction (sample on the indicator paper) or proceed as follows: into a test tube put 1−2 cmof filtrate 2−3 drops of solution of phenolphthalein and a drop of sodium hydroxide solution. Pink color indicates the fullness of the washing of the precipitate.
The washed precipitate is transferred to a flask in which to carry out the precipitation, dissolved in 0.1 mol/DMsolution of sodium hydroxide, crushed the filter stirring, add 3−5 drops of solution of phenolphthalein and octarepeat excess of sodium hydroxide 0,1 n solution of hydrochloric acid to bleaching of dissolving
RA.
3.2, 3.3. (Changed edition, Rev. N 2).
3.4. Processing of the results
3.4.1. Mass fraction of phosphorus () in percent is calculated by the formula
,
where — the volume of 0.1 mol/DMsolution of sodium hydroxide, cm;
— the volume of 0.1 mol/DMhydrochloric acid solution spent in the titration of excess sodium hydroxide, cm;
— coefficient of normality of the sodium hydroxide solution;
— the titer of 0.1 mol/DMsolution of sodium hydroxide, equal 0,000135 g/cmphosphorus;
— hanging alloy,
(Changed edition, Rev.
N 1).
3.4.2. Discrepancies in the results of parallel definitions should not exceed the permissible differences (the rate of convergence for 3), specified in the table.
(Changed edition, Rev. N 2).
3.4.3. 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.
3.4.4. Control of accuracy of analysis results is carried out according to State standard samples of tin bronzes, re-approved by GOST 8.315, or a comparison of the results obtained by the photometric method according to GOST 25086.
3.4.3,