GOST 19251.5-79
GOST 19251.5−79 Zinc. Methods for determination of tin (with Amendments No. 1, 2, 3)
GOST 19251.5−79
Group B59
STATE STANDARD OF THE USSR
ZINC
Methods for determination of tin
Zinc. Methods of tin determination
AXTU 1709
Date of introduction 1980−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
DEVELOPERS
V. I. Lysenko, L. I. Maksay, R. D. Cohen, V. A. Kolesnikov, N. Romanenko, R. A. Pestova
2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from
3. Change No. 3 adopted by the Interstate Council for standardization, Metrology and certification (Protocol No. 7 dated 26.04.96)
The adoption voted:
The name of the state |
The name of the national authority for standardization |
The Republic Of Azerbaijan |
Azgosstandart |
The Republic Of Armenia |
Armastajad |
The Republic Of Belarus |
Gosstandart Of Belarus |
The Republic Of Kazakhstan |
Gosstandart Of The Republic Of Kazakhstan |
The Republic Of Kyrgyzstan |
Kyrgyzstandart |
The Republic Of Moldova |
Moldovastandart |
Russian Federation |
Gosstandart Of Russia |
The Republic Of Tajikistan |
Tajikistandart |
The Republic Of Turkmenistan |
The main state inspection of Turkmenistan |
The Republic Of Uzbekistan |
Standards |
Ukraine |
Gosstandart Of Ukraine |
4. INSTEAD 19251.5 GOST-73
5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
The designation of the reference document referenced |
Item number |
GOST 860−75 |
2.2, 3.1 |
GOST 2603−79 |
2.2 |
GOST 3118−77 |
2.2, 3.1 |
GOST 3652−69 |
2.2 |
GOST 3760−79 | 2.2, 3.1 |
GOST 3773−72 |
3.1 |
GOST 4147−74 | 3.1 |
GOST 4204−77 |
2.2, 3.1 |
GOST 4233−77 |
3.1 |
GOST 4461−77 |
2.2, 3.1 |
GOST 5429−74 |
3.1 |
GOST 10929−76 |
2.2 |
GOST 11293−89 |
2.2 |
GOST 18300−87 |
2.2 |
GOST 19251.0−79 |
1.1 |
GOST 20490−75 |
2.2 |
GOST 22159−76 |
3.1 |
6. Limitation of actions taken on the Protocol 4−93 Interstate Council for standardization, Metrology and certification (ICS 4−94)
7. REPRINT (January 1998) with Amendments No. 1, 2, 3, approved in October 1984, April 1989, June 1996 (ICS 1−85, 7−89, 9−96)
This standard specifies the photometric and polarographic methods for determination of tin with its mass fraction of 0.0005 to 0.06%.
(Changed edition, Rev. N 3).
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis and security requirements — according to GOST 19251.0.
(Changed edition, Rev. N 1).
2. PHOTOMETRIC METHOD
2.1. The essence of the method
The method is based on dissolving the sample in nitric acid, deposition of tin in the form of metalbands acid on the manganese dioxide in a solution of nitric acid 1 mol/DMand subsequent measurement of light absorption of colored complex of tin phenylfluorone at a wavelength of 510 nm.
The sensitivity of the method is 5 µg of tin in the amount of 25 cm.
(Changed edition, Rev. N 3).
2.2. Apparatus, reagents and solutions
Spectrophotometer or photoelectrocolorimeter of any kind for measurements in the visible region of the spectrum.
Nitric acid according to GOST 4461, diluted 1:1, and a solution of 1 mol/DM.
Hydrochloric acid according to GOST 3118, and diluted 1:1.
Sulfuric acid according to GOST 4204, diluted 1:4, and the solution of 2.5 mol/DM.
Ascorbic acid, a solution of 20 g/DM, freshly prepared.
Citric acid according to GOST 3652, solution 100 g/l, freshly prepared.
Ammonia water according to GOST 3760.
Hydrogen peroxide according to GOST 10929.
Potassium permanganate according to GOST 20490, a solution of 6 g/DM.
Manganese nitrate, a solution of 10 g/DM.
Gelatin food according to GOST 11293, a solution of 10 g/DM.
Acetone according to GOST 2603.
Ethyl alcohol according to GOST 18300.
Phenylfluorone (2, 3, 7, trixi, 9-phenyl, 6-fluoro), a solution of 1 g/DM; a portion of the reagent a mass of 0.1 g was dissolved with heating in a flask with a capacity of 100 cm, 50 cmof ethanol with the addition of 0.5 cmof hydrochloric acid. The solution was cooled, transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with ethanol and mix. The solution is stored in container made of dark glass.
Tin stamps O1 according to GOST 860.
Standard solutions of tin.
Solution a: a portion of finely powdered tin mass 0,1000 g is placed in a conical flask with a capacity of 100 cmand dissolved by heating in 10 cmof sulphuric acid, the solution was cooled, transferred to a volumetric flask with a capacity of 1 DM, adjusted to the mark with sulphuric acid 2,5 mol/land stirred.
1 cmof solution A contains 0.1 mg of tin.
Solution B: in a volumetric flask with a capacity of 100 cmwith a pipette measure out 10 cmof solution A, was adjusted to the mark with sulphuric acid 2,5 mol/land stirred.
1 cmof a solution contains 0.01 mg of tin.
(Amended
, Edit. N 2, 3).
2.3. Analysis
2.3.1. Suspension zinc weight 1,0000 g (with mass fraction of tin from 0.0005 to 0.005%), 0,5000 g (with mass fraction of tin from 0.005 to 0.01%) or 0,1000 g (with mass fraction of tin from 0.01 to 0.06%) dissolved in 10 cmof nitric acid, diluted 1:1, heated to remove oxides of nitrogen, dilute with water to 100 cmand pour 3 cmof a solution of nitrate of manganese. The solution is neutralized with ammonia to release the brown hydroxide of manganese, and add 20 cmof nitric acid, diluted 1:1. The solution is heated to boiling, poured 10 cmof the potassium permanganate solution, add water to 150 cm, boil for 5 minutes and leave it for 50−60 minutes in a warm place.
The precipitate was filtered off on a medium density filter, washed and the flask in which to carry out the deposition, 5−6 times a hot solution of nitric acid 1 mol/DM. Residue from a deployed filter, washed with a small amount of water in the flask, which carried out the deposition, the filter is treated with 10 cmof hot sulfuric acid, diluted 1:4 with addition of 6−7 drops of hydrogen peroxide, the filter is then washed two times with hot water. The resulting solution is poured into a glass with a capacity of 100 cm, evaporated to sulphuric acid fumes, cooled, rinse the walls of the glass 3−4 cmof water and evaporated to dryness. To the cooled residue poured 2.5 cmof sulfuric acid solution 2.5 mol/DM, 2 cmof a solution of ascorbic acid; heated to dissolve, cooled, poured into a volumetric flask with a capacity of 25 cm, sequentially with stirring, add 2 cmof the citric acid solution, 1 cmof solution of gelatin, 3 cmof acetone, 1 cmof solution phenylfluorone, made up to the mark with water, mix, leave for 1 hour for development of colour. Optical density of the solution is measured in the relevant cuvette at a wavelength of 510 nm. Solution comparison is the solution of the reference experiment.
The content of tin is set by the calibration schedule.
(Redrafted From
m. N 2, 3).
2.3.2. To build a calibration curve in seven of the eight cups capacity 100 cmmeasure 0,5; 1,0; 2,0; 3,0; 4,0; 5,0 and 6.0 cmstandard solution B, which corresponds to 5; 10; 20; 30; 40; 50 and 60 µg of tin, evaporated to dryness and cooled. In each glass, add 2.5 cmof sulfuric acid solution 2.5 mol/DM, 2 cmof ascorbic acid and behave as specified in claim
According to the obtained values of optical density of solutions and the corresponding content of tin to build a calibration curve.
2.4. Processing of the results
2.4.1. Mass fraction of tin , %, is calculated by the formula
,
where — weight of tin in the solution was found in the calibration schedule, mcg;
— the weight of the portion.
(Changed edition, Rev. N 3).
2.4.2. The absolute values of the differences between the results of two parallel measurements (rate of convergence) and the results of the two tests (index of reproducibility) with a confidence level should not exceed the values permitted discrepancies listed in the table.
Mass fraction of tin, % |
The permissible difference for parallel definitions % |
The permissible discrepancy between the results of the analysis % |
To from 0,0005 0,0010 incl. |
0,0002 |
0,0003 |
SV. 0,0010 «0,0030 « |
0,0004 |
About 0.0006 |
«0,0030» 0,0060 « |
About 0.0006 |
0,0008 |
«0,0060» 0,0100 « |
0,0010 |
0,0015 |
«0,0100» 0,0300 « |
0,0015 |
0,0022 |
«0,0300» 0,060 « |
0,003 |
0,004 |
(Changed edition, Rev. N 2).
3. POLAROGRAPHIC METHOD
The method is based on dissolving the sample in nitric acid, separation of lead in the form of double salts with a sulfate of strontium and polarography of tin in sodium chloride background at a potential of minus 0.5 V relative to the saturated calomel electrode.
The sensitivity of the method for determination of tin on the oscilloscope polarography 0.05 mg/DM, variable-current — 0.002 mg/DM.
3.1. Apparatus, reagents and solutions
Polarography oscillographic or polarograph AC.
Nitric acid according to GOST 4461, diluted 1:1.
Hydrochloric acid according to GOST 3118.
Sulfuric acid according to GOST 4204, and diluted 1:1, 1:5 and 1:20.
Ammonia water according to GOST 3760.
Hydrazine dihydrochloride according to GOST 22159.
Iron chloride according to GOST 4147, a solution of 20 g/DM.
Sodium chloride according to GOST 4233, does not contain lead.
Ammonium chloride according to GOST 3773.
Washing the ammonium-ammonia liquid containing in 1 DM10 g of ammonium chloride and 20 cmof ammonia.
Strontium nitrate according to GOST 5429, a solution of 100 g/DM.
Background electrolyte: in a polyethylene vessel with a capacity of 2 DMare placed 200 g of sodium chloride, 40 g of hydrazine dihydrochloride, 50 cmhydrochloric acid, the volume was adjusted to 2 DMwater and stirred.
Tin stamps O1 according to GOST 860.
A standard solution of tin: a portion of finely ostertagi tin mass 0,1000 g is placed in a conical flask with a capacity of 250 cm, flow 10 cmof sulphuric acid, heated until complete dissolution of the sample, cooled, transferred to a volumetric flask with a capacity of 1 DM, adjusted to the mark with sulfuric acid diluted 1:5, and stirred.
1 cmof the solution contains 0.1 mg of tin.
Calibration solutions of tin: in five out of six volumetric flasks with a capacity of 200 cmmeasure respectively 0,5; 1,0; 2,0; 4,0 and 6,0 cmstandard solution of tin, add to the labels of background electrolyte and stirred. The solutions contain, respectively, 0,25; 0,5; 1,0; 2,0 and 3,0 mg/DMtin.
Acid askor
binova.
3.2. Analysis
The weight of zinc weight of 2,5000 g (mass fraction of tin and 0.005%) and 1.0000 g (higher mass fraction of 0.005%) was placed in a conical flask with a capacity of 250 cm, 40 cm pournitric acid, diluted 1:1, cover with a watch glass, heated to dissolve the sample and removal of nitrogen oxides, rinse the glass with water.
The solution was cooled, poured 15 cmof a solution of nitrate of strontium, dilute with water to 100 cm, is added in small portions with stirring 10 cmof sulphuric acid diluted 1:1 and leave in the fridge with running cold water for 30 minutes the Precipitate was filtered off on a tight double filter of «blue ribbon», collecting the filtrate in a conical flask with a capacity of 250 cm. The residue in the flask and on the filter is washed six times with cold sulphuric acid, diluted 1:20.
To the filtrate poured 2cmof a solution of ferric chloride, is stirred and heated to 60−70 °C, poured ammonia to separation into the precipitate of hydroxides of iron and tin, give an excess of ammonia 10 cm, leave in warm oven for 20−25 min, after which the precipitate was filtered through a filter of medium density. The flask and precipitate was washed three times with hot wash liquid, and then twice with hot water.
The deployed filter wash 25−30 cmhot background electrolyte in a conical flask with a capacity of 50−100 cm, cover with a watch glass, heated to boiling and boiled for 3−5 minutes, leave in warm place plate to the bleaching solution (if within 20 min the solution is not discolored, then add a few crystals of ascorbic acid), cooled, transferred to a volumetric flask with a capacity of 50 cm, made up to the mark and the background electrolyte and stirred.
Part of the solution is poured into the polarographic cell and conduct polarography tin with a corresponding current range and the half-wave potential of minus 0.5 V relative to the saturated calomel electrode. Simultaneously carried polarographically solution in the reference experiment.
The values of the wave height of the analyzed solution is subtracted the value of the wave height in the reference experiment and calculate the contents of
fishing.
3.1, 3.2. (Changed edition, Rev. N 2, 3).
3.3. Processing of the results
3.3.1. Mass fraction of tin , %, is calculated by the formula
,
where the wave height of tin in the sample solution, mm;
— volume of the volumetric flask, cm;
— the concentration of tin in calibration solution, mg/DM;
wave height of tin in the calibration solution, mm;
— the weight of the portion of the sample,
3.3.2. The absolute values of the results of two parallel measurements (rate of convergence) and the results of the two tests (index of reproducibility) with a confidence level should not exceed the values permitted discrepancies listed in the table.
(Changed edition, Rev. N 2).