GOST 15027.10-77
GOST 15027.10−77 Bronze without tin. Methods for determination of tin (with Amendments No. 1, 2)
GOST 15027.10−77
Group B59
INTERSTATE STANDARD
BRONZE WITHOUT TIN
Methods for determination of tin
Non-tin bronze.
Methods for the determination of tin
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 15027.10−69
4. The standard fully complies ST SEV 1528−79.
Standard corresponds to ISO 4751−84 in part of bronze without tin
5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced |
Section number, paragraph, sub-paragraph |
| GOST 61−75 |
3.2 |
| GOST 199−78 |
3.2 |
| GOST 493−79 |
Chapeau |
| GOST 614−97 |
Chapeau |
| GOST 859−2001 |
2.2 |
| GOST 860−75 |
2.2, 3.2, 5.2, 6.2, 7.2 |
| GOST 1277−75 |
3.2 |
| GOST 2768−84 |
5.2 |
| GOST 3117−78 |
4.2 |
| GOST 3118−77 |
2.2, 3.2, 7.2 |
| GOST 3652−69 |
5.2 |
| GOST 3760−79 |
2.2, 3.2, 4.2, 5.2, 6.2 |
| GOST 4139−75 |
3.2 |
| GOST 4166−76 |
2.2 |
| GOST 4204−77 |
3.2, 4.2, 5.2, 6.2 |
| GOST 4233−77 |
2.2, 3.2 |
| GOST 4328−77 |
3.2 |
| GOST 4461−77 |
3.2, 4.2, 5.2, 6.2, 7.2 |
| GOST 4658−73 |
4.2 |
| GOST 6006−78 |
2.2 |
| GOST 6344−73 |
2.2 |
| GOST 9293−74 |
4.2 |
| GOST 10484−78 |
5.2, 6.2 |
| GOST 10652−73 |
4.2 |
| GOST 10929−76 |
2.2, 3.2, 5.2, 6.2 |
| GOST 11293−89 |
3.2, 5.2 |
| GOST 18175−78 |
Chapeau |
| GOST 18300−87 |
3.2, 5.2 |
| GOST 20490−75 |
5.2, 6.2 |
| GOST 25086−87 |
1.1, 2.4.4, 4.4.2 b |
| THAT 6−09−4011−75 |
5.2, 6.2 |
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 tin using quercetin, a photometric method for the determination of tin with application phenylfluorone (with mass fraction of tin from 0.01% to 0.5%), a polarographic method for the determination of tin (with mass fraction of tin from 0.001% to 0.5%) and atomic absorption method for the determination of tin (with mass fraction of tin from 0.01% to 0.25% and from 0.25% to 0.5%) in tin bronze according to GOST 18175, GOST and GOST 614 493.
(Changed the wording. Izm. N 1, 2).
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).
2. THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF TIN USING QUERCETIN
2.1. The essence of the method
The method is based on formation of colored complex compounds of tin with quercetin extracted n-butyl alcohol hydrochloric acid solution. The interfering influence of iron can be eliminated by addition of thiourea.
2.2. Apparatus, reagents and solutions
Photoelectrocolorimeter or spectrophotometer.
Hydrochloric acid according to GOST 3118 and diluted 1:4 and 1:10.
Hydrogen peroxide according to GOST 10929, 30% solution.
Ammonia water according to GOST 3760 and diluted 1:1.
Thiourea according to GOST 6344, solution 100 g/DM.
Sodium chloride according to GOST 4233.
Sodium sulphate anhydrous according to GOST 4166.
Normal butyl alcohol according to GOST 6006.
Quercetin, a solution of 0.4 g/lin n-butyl alcohol.
Copper according to GOST 859 brand MO.
A standard solution of copper, prepared as follows: 2.5 g of copper is dissolved in 30 cmof concentrated hydrochloric acid, adding dropwise hydrogen peroxide. The excess hydrogen peroxide is decomposed by boiling, the solution was transferred to a volumetric flask with a capacity of 250 cm
, made up to the mark with water and mix.
1 cmof the solution contains 0.01 g of copper.
Tin GOST 860 brand 01.
Standard solutions of tin.
Solution A, prepared as follows: 0.1 g of tin are placed in a conical flask with a capacity of 100 cm, are added 1 g of sodium chloride, 20 cm
of concentrated hydrochloric acid, 1 cm
of hydrogen peroxide (gradually, drop by drop) and heated at 60−70 °C. By the end of the dissolution, the temperature was raised to 80 °C. the Solution was cooled, transferred to a volumetric flask with a capacity of 1 DM
, adding hydrochloric acid, diluted 1:10, up to the mark and mix.
1 cmof the solution contains 0.0001 g of tin.
Solution B is prepared as follows: 25 cmsolution And transferred to a volumetric flask with a capacity of 250 cm
, made up to the mark with hydrochloric acid diluted 1:10, and stirred.
1 cmof solution B contains 0,00001 g tin. Solution B is prepared on the day Prim
Anania.
2.3. Analysis
2.3.1. A portion of the sample weighing 1 g is placed in a beaker with a capacity of 250 cm, add 5 sodium chloride, 20 cm
of concentrated hydrochloric acid and heated. In the heating process is administered 7−10 cm
of hydrogen peroxide in small portions to dissolve the sample. After complete dissolution, the solution was evaporated to a volume of 3−4 cm
, transferred into a volumetric flask with a capacity of 250 cm
, was adjusted to the mark with water and mix. Aliquot part of the solution of volume 25 cm
(with mass fraction of tin from 0.01% to 0.1%) or 5 cm
(with mass fraction of tin from 0.1% to 0.5%) was placed in a separating funnel with a capacity of 150 cm
.
When determining the tin content of siliceous or svintsoviy the bronze, in the presence of sediment, aliquot part taken from a pre-filtered solution.
The solution in separating funnel neutralized with ammonia dropwise until a slightly alkaline reaction on Congo paper and then pour 5 cmof hydrochloric acid, diluted 1:4, 20 cm
solution of thiourea, dilute with water to 50 cm
, injected 25 cm
of a solution of quercetin in n-butyl alcohol and vigorously shaken for 5 min. After separation of phases the lower aqueous layer discarded, avoiding the remainder of the aqueous phase, and the organic layer is poured into a dry beaker with a capacity of 50 cm
containing 0.2 g of anhydrous sodium sulfate, and after 5 minutes measure the optical density in a cuvette of 10 mm length on a photoelectrocolorimeter with a blue or purple filter (
=420−450 nm), or on the spectrophotometer at a wavelength of 440 nm. Solution comparison is the solution of quercetin in n-butyl
alcohol.
2.3.2. Construction of calibration curve
In a separating funnel with a capacity of 150 cmtaken at 10 cm
of a standard solution of copper (for bronze with a mass fraction of tin from 0.01% to 0.1%, with aliquotes part 25 cm
) or 2 cm
of a standard solution of copper (for bronze with a mass fraction of tin from 0.1% to 0.5%, with aliquotes part 5 cm
, consistently administered 0, 1, 3, 5, 7 and 10 cm
standard solution B tin.) The solutions were neutralized with ammonia to slightly alkaline environment at the paper of the Congo, poured 5cm
of hydrochloric acid, diluted 1:4, and further analysis is carried out as specified in clause
The found values of optical density calibration curve build
.
2.4. Processing of the results
2.4.1. Mass fraction of tin () in percent is calculated by the formula
where — weight of tin, was found in the calibration schedule g;
— the weight of the portion corresponding to aliquote part,
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.1.
Table 1
| Mass fraction of tin, % |
|
|
| From 0.01 to 0.03 |
0,003 | 0,007 |
| SV. 0,03 «0,06 |
0,006 | 0,01 |
| «0,06» 0,12 |
0,012 | 0,03 |
| «And 0.12» to 0.25 |
0,02 | 0,05 |
| «0,25» 0,50 |
0,03 | 0,07 |
2.4.3. The absolute discrepancies of the analysis results obtained in two laboratories, or two analysis results obtained in the same laboratory but under different conditions (a measure of reproducibility) shall not exceed the values given in table.1.
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, by comparing the results of analysis of the obtained photometric and atomic absorption methods or by a method of additives in accordance with GOST 25086.
2.4−2.4.4. (Added, Rev. N 2).
3. THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF TIN WITH APPLICATION PHENYLFLUORONE AFTER SEPARATION OF THE ANION EXCHANGER
3.1. The essence of the method
The method is based on measuring the optical density of the colored complex compounds of tin (IV) with phenylfluorone after prior separation of tin from accompanying elements on the anion exchanger.
3.2. Apparatus, reagents and solutions
Photoelectrocolorimeter or spectrophotometer.
The column of ion exchange, which is a burette with a capacity of 20−25 cmwith an inner diameter of 10−15 cm
; the upper part of the burette ends in a drip funnel. In the lower end of the burette lay a pad of glass wool with a height of 5 mm, which was pre-boiled with hydrochloric acid.
Nitric acid according to GOST 4461.
Hydrochloric acid according to GOST 3118 and diluted 1:9, 1:20, solutions 5 and 0.1 mol/DM.
Hydrogen peroxide according to GOST 10929.
Sodium chloride according to GOST 4233, saturated solution.
Sulfuric acid according to GOST 4204, diluted 1:4 and 1:9.
Ammonia water according to GOST 3760, diluted 1:1.
Phenolphthalein (indicator) solution in alcohol 1 g/DM.
Sodium acetate according to GOST 199.
Acetic acid according to GOST 61.
A buffer solution with a pH of 4.3; prepared as follows: 100 g of sodium acetate dissolved in 300 cmof water, transferred to a volumetric flask with a capacity of 1 DM
, poured 168 cm
acetic acid and add water to the mark.
Rectified ethyl alcohol according to GOST 18300.
Potassium rodanistye according to GOST 4139, a solution of 10 g/DM.
Phenylfluorone, alcohol solution 0.25 g/l; prepared as follows: 0.025 g phenylfluorene dissolved in 30 cm
of ethanol with the addition of 8−10 drops of concentrated sulfuric acid with stirring. After dissolution, the sample solution was transferred to volumetric flask with a capacity of 100 cm
and then filled to the mark with ethanol.
Gelatin food according to GOST 11293, solution 5 g/l; prepared as follows: 0.5 g of gelatin soaked in 20 cm
of cold water and after 20 minutes, add 80 cm
of water, heated to 70 °C, stirring the solution until complete dissolution of the sample. You should use freshly prepared solution.
Sodium hydroxide according to GOST 4328, solution 50 and 100 g/DM.
Silver nitrate according to GOST 1277, a solution of 10 g/DM.
Tin GOST 860 brand 01.
Standard solutions of tin.
Solution A, prepared as follows: 0.1 g of tin dissolved by heating in 10 cmof concentrated sulfuric acid, adding five drops of nitric acid, evaporated until a white smoke of sulfuric acid, cooled, transferred to a volumetric flask with a capacity of 1 DM
and topped to the mark with sulfuric acid diluted 1:4.
1 cmof the solution contains 0.0001 g of tin.
Solution B is prepared on the day of application as follows: 25 cmsolution And placed in a volumetric flask with a capacity of 250 cm
and dilute to the mark with sulfuric acid diluted 1:9.
1 cmof solution B contains 0,00001 g tin.
The Anion Exchange Resin And
N-1 and EDE-10P.
3.3. Preparation for assay
3.3.1 Preparation of the anion exchanger
50 g of ion exchange resins fraction 0.25−0.5 mm is soaked in a saturated solution of sodium chloride for 24 h for swelling. Then the sodium chloride solution is washed by decantation and washed anion exchange resin with hydrochloric acid diluted 1:20, to colorless wash solution negative reaction for iron romanistik potassium. The resin was sequentially washed with a solution of sodium hydroxide 50 g/DM, and then with a solution of 100 g/DM
the complete removal of chloride ions (reaction with silver nitrate), the resin was washed with water until a weakly alkaline reaction wash liquid. Thereafter, the anion exchanger is filled with water, stir and transfer into the column. The layer of resin in the column should be smooth, without air bubbles.
For translation of the anion exchanger in chloroform before passing the test solution through the anion exchanger is passed a solution of 5 mol/DMhydrochloric acid at a speed of 3 cm
/min in quantities of 100−150 cm
.
3.4. Analysis
3.4.1.The weight of bronze weighing 0.5 g (with mass fraction of tin from 0.01 to 0.1%) or 0.1 g (with mass fraction of tin of 0.1−0.5%) were placed in a glass with a capacity of 150 cm, add 5 g of sodium chloride and dissolved in 15 cm
of a solution of 5 mol/DM
of hydrochloric acid, periodically adding hydrogen peroxide to completely dissolve the sample. The solution is boiled for 1−2 min until complete destruction of excess hydrogen peroxide. Then heating was stopped, the solution was cooled, poured 25 cm
solution of 5 mol/DM
hydrochloric acid, wash the side of the Cup with water (5−7 cm
), add two drops of nitric acid, the mixture was heated and boiled for 2−3 min to remove the oxides of nitrogen. Then heating was stopped, the solution was cooled and passed through a column filled with anion exchange resin in chloroform, at a speed of 3 cm
/min For the elution sorbirovannoe copper glass column and washed with 200 cm
of a solution of 5 mol/DM
hydrochloric acid at a speed of 3 cm
/min.
Desorption tin spend 250 cmof solution 0.1 mol/DM
hydrochloric acid at the same rate in a volumetric flask with a capacity of 250 cm
and the same acid diluted to the mark. Aliquot part of the solution, equal to 10 cm
, were placed in a glass, pour 3 cm
of concentrated sulfuric acid and evaporate until a white smoke of sulfuric acid.
Salt dissolved in 5 cmof water, the solution was transferred to volumetric flask with a capacity of 50 cm
(for rinsing the glass used no more than 10 cm
of water), neutralized with ammonia, diluted 1:1 in the presence of phenolphthalein are then added dropwise sulfuric acid diluted 1:9 before the disappearance of color of the indicator and 10 cm
in excess. The solution was stirred, poured 2cm
of a solution of gelatin, 5 cm
solution phenylfluorone 10 cm
buffer solution and leave for 5 mins then add water to the mark (solution pH should be 1.1 to 1.2). At each addition of the reagent the solution was stirred and after 30 min, measure the optical density of the solution on the spectrophotometer or photoelectrocolorimeter with a yellow-green optical filter at a wavelength of 508 nm in a cuvette length of 1 cm with a Solution of comparison is the solution of Koh
— controlling experience.
3.4.2. Construction of calibration curve
In a volumetric flask with a capacity of 50 cm, is placed successively 0, 1, 2, 3, 4 and 5 cm
standard solution B tin and top up to volume of 10 cm
sulfuric acid, diluted 1:9. Neutralized with ammonia in the presence of phenolphthalein are then added dropwise sulfuric acid diluted 1:9 before the disappearance of color of the indicator and 10 cm
in the excess and continue further analysis, as described in Chapter
The found values of optical densities build the calibration graph.
3.5. Processing of the results
3.5.1. Mass fraction of tin () in percent is calculated by the formula
where — weight of tin, was found in the calibration schedule g;
— the weight of the portion corresponding to aliquote part,
3.5.2. The absolute discrepancies in the results of parallel measurements (the rate of convergence) must not exceed the permissible values given in table.1.
(Changed edition, Rev. N 2).
3.5.3. The absolute discrepancies of the analysis results obtained in two laboratories, or two analysis results obtained in the same laboratory but under different conditions (a measure of reproducibility) shall not exceed the values given in table.1.
3.5.4. Control of accuracy of analysis results
Control of accuracy of analysis results of tin is carried out according to claim
3.5.3,
4. POLAROGRAPHIC METHOD FOR THE DETERMINATION OF TIN
4.1. The essence of the method
The method is based on the separation of tin by the coprecipitation from a hydroxide of beryllium in ammonium-chloride buffer solution containing Trilon B, with subsequent polarographic determination of tin in hydrochloric acid background. The half-wave potential (peak) recovery of tin of about minus 0.5 V (saturated calomel element).
4.2. Apparatus, reagents and solutions
Polarograph type AC-PPT-1.
Polarography oscillographic-type-5122 or other suitable polarograph AC complete with all accessories.
The polarographic cell, made of glass, with a capacity of 40 cm, with a remote electrode (saturated calomel electrode) and mercury-drip cathode.
Nitrogen gas according to GOST 9293.
Mercury GOST 4658 stamps r0, dehydrated.
Hydrochloric acid according to GOST 3117, concentrated, dilute 1:1 and 1:3.
Nitric acid according to GOST 4461, diluted 1:1.
Beryllium nitrate, an aqueous solution 100 g/DM.
Ammonia water according to GOST 3760 and 2% solution.
Sulfuric acid according to GOST 4204.
Salt is the disodium Ethylenediamine-N, N, N', N'-tetraoxane acid, 2-water (Trilon B) according to GOST 10652, solution 0,1 mol/DM.
Tin GOST 860 brand 00.
Standard solutions of tin.
Solution A, prepared as follows: a portion of tin of 0.1 g was placed in a conical flask with a capacity of 250 cmand dissolved in 10−15 cm
of sulfuric acid. After the dissolution of tin and the solution was cooled poured 100 cm
of water and 50 cm
of concentrated hydrochloric acid, transfer the solution into a volumetric flask with a capacity of 1 DM
, made up to the mark with water and mix.
1 cmof solution A contains 0.1 mg of tin.
Solution B is prepared as follows: pipetted 10 cmof solution A in a volumetric flask with a capacity of 100 cm
, made up to the mark with hydrochloric acid diluted 1:3 and stirred.
1 cmof a solution contains 0.01 mg of tin.
Solution B is prepared before the application
eniem.
4.3. Analysis
A portion of the alloy (tab.2) is placed in a beaker with a capacity of 250 cm, cover with a watch glass and dissolved in 20 cm
of nitric acid, diluted 1:1, and 5 cm
of concentrated hydrochloric acid with mild heating. After dissolution of the alloy solution was cooled, add 5 cm
of a solution of nitrate of beryllium, washed the glass and the side of the Cup with water, heated to 70−80 °C and to the solution was added 20 cm
of a solution of Trilon B. the Solution is again heated to 80 °C, diluted to a total volume of 150 cm
and add ammonia until the formation of a soluble deep blue ammonia complex of copper and 5 cm
of ammonia in excess. The solution is kept in a hot bath for 30−40 min, then hot filtered through a dense filter of «blue ribbon» and washed precipitate on the filter 5−7 times 2% hot solution of ammonia.
Table 2
| Mass fraction of tin, % |
The mass of charge, g | Polarographically the volume of solution, cm |
| From 0.001 to 0.003 |
1 | 40 |
| SV. Of 0.003 «to 0.01 |
1 | 20 |
| «0,01» 0,025 |
1 | 10 |
| «0,025» 0,5 |
0,5 | 5 |
| «Of 0.5» to 0.1 |
0,5 | 2 |
| «0,1» 0,5 |
0,1 | 10 |
The funnel with the precipitate was placed on glass, which conducted the deposition, the precipitate was dissolved in 20 cmof hot hydrochloric acid, diluted 1:3, adding a few drops of hydrogen peroxide in the presence of manganese bronze.
The filter is washed with 20 cmof hot water, diluted the solution to 150 cm
of water, add 15 cm
Trilon B and repeat the precipitation.
After three perioadele the filter cake is dissolved in 25 cmof hydrochloric acid diluted 1:3, transferred to a volumetric flask with a capacity of 50 cm
, adjusted solution to the mark with the same hydrochloric acid solution and stirred.
At the same time spend control experience.
Aliquot part of the obtained solution (see table.2) is transferred into a polarographic cell, previously washed with hydrochloric acid diluted 1:3. The solution in the cell is degassed flowing nitrogen for 5−7 minutes, then stop stirring and remove the cathodic polarization curve in the voltage range from minus 0.25 to minus 0.7 V. the Peak recovery of tin recorded at minus 0.5 V. the Sensitivity of the recording instrument are selected so that the height of the peak of tin was at least 15 mm.
The tin content find by the method of standard additions. Aliquot part of the solution A or B, depending on the tin content, is introduced into polarographically solution, pass nitrogen for 3 min and lead further analysis as well as in the determination of tin in the analyzed solution. The value of the standard additives are selected so that the height of the peak of tin after the introduction of the additive increased 1.5−2 times. The volume of standard addition should not exceed 0.5 cm
.
4.4. Processing of the results
4.4.1. Mass fraction of tin () in percent is calculated by the formula
where is the height of the peak of tin in polarography solution in the reference experiment, mm.
— the height of the peak of tin in polarography the test solution, mm;
— the height of the peak of tin in polarography solution after the introduction of standard additives, mm;
— the volume of standard addition, cm
;
— concentration of standard solution, g/cm
;
— the weight of alloy taken for polarography,
G.
4.4.2. The absolute discrepancies in the results of parallel measurements (the rate of convergence) must not exceed the permissible values given in table.3.
Table 3
| Mass fraction of tin, % |
|
|
| From 0.001 to 0.003 |
0,0002 | 0,0005 |
| SV. 0,003 «to 0,006 |
0,0005 | 0,001 |
| «0,006» 0,010 |
0,001 | 0,002 |
| «0,01» 0,025 |
0,002 | 0,005 |
| «Of 0.025» to 0.05 |
0,005 | 0,01 |
| «0,05» 0,1 |
0,01 | 0,02 |
| «0,1» 0,5 |
0,02 | 0,05 |
(Changed edition, Rev. N 2).
4.4.2. 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.3.
4.4.2 b. 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, or by a method of additives in accordance with GOST 25086.
4.4.2 a, 4.4.2 b. (Added, Rev. N 2).
4.4.3. The differences in the assessment of the quality of bronze used polarographic method.
5. THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF TIN WITH PHENYLFLUORONE AFTER SEPARATION BY COPRECIPITATION WITH MANGANESE DIOXIDE
5.1. The essence of the method
The method is based on measuring the optical density of the colored complex compounds of tin with vinyltoluene in the presence of ascorbic and citric acids, masking iron and antimony, respectively, after prior separation of the tin by the coprecipitation with manganese dioxide.
5.2. Apparatus, reagents and solutions
Photoelectrocolorimeter or spectrophotometer.
Nitric acid according to GOST 4461, diluted 1:1 and solution 2 mol/DM.
Sulfuric acid according to GOST 4204, and diluted 1:1 and 1:4 and a solution of 2 mol/DM.
Hydrofluoric acid according to GOST 10484.
Ascorbic acid according to normative-technical documentation, solution 20 g/l, freshly prepared.
Citric acid according to GOST 3652, a solution of 200 g/DM, freshly prepared.
Ammonia water according to GOST 3760.
Manganese nitrate on the other 6−09−4011, a solution of 50 g/DM.
Potassium permanganate according to GOST 20490, a solution of 10 g/DM.
Hydrogen peroxide according to GOST 10929.
Acetone GOST 2768.
Rectified ethyl alcohol according to GOST 18300.
Gelatin food according to GOST 11293, a solution of 10 g/DM, freshly prepared.
Phenylfluorone, alcoholic solution of 0.5 g/l; prepared as follows: 0.05 g phenylfluorene dissolved by heating in 50 cm
of ethyl alcohol, adding 1 cm
of sulfuric acid diluted 1:1. The solution was cooled, transferred to a volumetric flask with a capacity of 100 cm
, made up to the mark with ethyl alcohol and store in a dark place.
Tin GOST 860 with a mass fraction of tin is not less than 99.9%.
Standard solutions of tin.
Solution A, prepared as follows: 0.1 g of tin are dissolved in 10 cmof concentrated sulfuric acid, the solution was cooled, transferred to a measuring flask with volume capacity of 1000 cm
, made up to the mark with a solution of 2 mol/DM
sulfuric acid and stirred.
1 cmof the solution contains 0.0001 g of tin.
Solution B is prepared as follows: 25 cmsolution And placed in a volumetric flask with a capacity of 250 cm
, made up to the mark with a solution of 2 mol/DM
sulfuric acid and stirred.
1 cmof solution B contains 0,00
001 g of tin.
5.3. Analysis
5.3.1. For bronzes with a mass fraction of silicon to 0.05%
A portion of the alloy depending on the mass fraction of tin (see table.4) is placed in a beaker with a capacity of 250 cm, and dissolved in 10 cm
of nitric acid, diluted 1:1, when heated. 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 (at a mass proportion of manganese in the alloy, a 2% solution of nitrate of manganese is not added), the solution is neutralized with ammonia until the appearance of the precipitate copper hydroxide, add 24 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 8−10 times a hot solution of 1 mol/DM
nitric acid until the disappearance of the blue color formed of copper nitrate. 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.
Table 4
| Mass fraction of tin, % | The mass of charge, g | The volume of sample solution, cm |
The volume aliquote part of the solution, cm |
The volume of 2 mol/DM |
| From 0.01 to 0.06 |
1 | 100 | 10 | 0,5 |
| SV. 0,06 «0,12 |
1 | 100 | 5 | 1,5 |
| «And 0.12» to 0.25 | 0,5 | 250 | 10 | 0,5 |
| «0,25» 0,50 | 0,5 | 250 | 5 | 1,5 |
The washed filter is discarded and the filtrate is evaporated to release white smoke of sulfuric acid. To the cooled residue is added, at a mass fraction of tin from 0.01% to 0.12% — 20 cm, while the mass fraction of tin in excess of 0.12% in 50 cm
solution of 2 mol/DM
sulfuric acid and the solution transferred to an appropriate volumetric flask (see table 4), made up to the mark with water and mix.
Aliquot part of the solution (see table.4) is placed in a volumetric flask with a capacity of 25 cm, add specified in table.4 the volume of solution 2 mol/DM
sulphuric acid and alternately, mixing after addition of each reagent, add 2cm
of a solution of ascorbic acid 5 cm
of the citric acid solution, 1 cm
of solution of gelatin, 3 cm
of acetone, 2 cm
of mortar phenylfluorone, made up to the mark with water and mix. After 30 min measure optical density of solution on a photoelectrocolorimeter with a yellow green filter or on spectrophotometer at a wavelength of 510 nm in a cuvette length of 1 cm with a Solution of comparison is the solution of the reference experiment.
(Changed edition, Rev. N
2).
5.3.2. For bronzes with a mass fraction of silicon in excess of 0.05%
A portion of the alloy (see table.4) is placed in a platinum Cup and dissolved in 10 cmof nitric acid, diluted 1:1, and 2−3 cm
hydrofluoric acid when heated.
After dissolution, add 10 cmsulphuric 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 50 cmplaced 1,0; 2,0; 3,0; 4,0; 5,0; 6,0 and 7.0 cm
standard solution B tin, the solutions were evaporated to dryness and cooled. All glasses add 2.5 cm
solution of 2 mol/DM
sulphuric acid, heat the solution, add 2 cm
of ascorbic acid solution, cooled and further analysis is carried out as specified in clause
Solution comparison is the solution not containing the tin.
According to the obtained results build a calibration curve.
5.4. Processing of the results
5.4.1. Mass fraction of tin () in percent is calculated by the formula
where — weight of tin, was found in the calibration schedule g;
— the weight of the portion corresponding to aliquote part of the solution,
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.1.
(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.1.
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 TIN (WITH MASS FRACTION of TIN from 0.01% to 0.25%)
6.1. The essence of the method
The method is based on measuring the absorption of light by atoms of tin, formed during the introduction of the analyzed solution in the flame acetylene-air or acetylene-nitrous oxide, after a preliminary separation of the tin by the coprecipitation with manganese dioxide.
6.2. Apparatus, reagents and solutions
Atomic absorption spectrometer with a radiation source for tin.
Nitric acid according to GOST 4461, diluted 1:1 and a solution of 1.5 mol/DM.
Sulfuric acid according to GOST 4204, diluted 1:1, 1:4, and the solution of 2.5 mol/DM.
Hydrofluoric acid according to GOST 10484.
Ammonia water according to GOST 3760.
Manganese nitrate on the other 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.
Tin GOST 860 with a mass fraction of tin is not less than 99.9%.
A standard solution of tin; prepared as follows: 0.25 g of tin dissolved by heating in 20 cmof concentrated sulfuric 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 mol/DM
sulfuric acid and stirred.
1 cmof the solution contains 0.0005 g tins
.
6.3. Analysis
6.3.1. For bronzes with a mass fraction of silicon to 0.05%
A portion of the alloy depending on the mass fraction of tin (see table.5) is placed in a beaker with a capacity of 250 cmand dissolved by heating in nitric acid, diluted 1:1, the volume of which is taken in accordance with the specified in table.5.
Table 5
| Mass fraction of tin, % | The mass of charge, g | The volume of solution of nitric acid, diluted 1:1, see |
| From 0.01 to 0.10 |
2 | 20 |
| SV. Of 0.10 «to 0.25 |
1 | 10 |
Nitrogen oxides are removed by boiling and the solution diluted with water to a volume of 50 cm. Pour 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 cm
of solution of 1 mol/DM
of hydrochloric acid, transferred to a volumetric flask or a test tube calibration up to 10 cm
and then filled to the mark with a solution of 1 mol/DM
of hydrochloric acid.
Measure the atomic absorption of tin in the flame of acetylene-air or acetylene-nitrous oxide at a wavelength of 286,3 nm 224,6 or in parallel with calibration solvents
Rami.
6.3.2. For bronzes with a mass fraction of silicon in excess of 0.05%
A portion of the alloy (see table.5) is placed in a platinum Cup and dissolved by heating in nitric acid, diluted 1:1, the volume of which is taken in accordance with the specified in table.5, and 2 cmhydrofluoric 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
6.3.3. Construction of calibration curve
In seven of eight glasses with a capacity of 250 cmis placed 0,4; 1,0; 2,0; 3,0; 4,0; 5,0 and 6.0 cm
of a standard solution of tin. 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
According to the obtained results build a calibration curve.
6.4. Processing of the results
6.4.1. Mass fraction of tin () in percent is calculated by the formula
where is the concentration of tin 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.1.
(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.1.
6.4.4. Control of accuracy of analysis results
Control of accuracy of analysis results by State standard samples is carried out according to claim
6.4.3,
7. ATOMIC ABSORPTION METHOD for the DETERMINATION of TIN (WITH MASS FRACTION of TIN from 0.25% to 0.5%)
7.1. The essence of the method
The method is based on measuring the absorption of light by atoms of tin, formed during the introduction of the analyzed solution in the flame acetylene-air or acetylene-nitrous oxide.
7.2. Apparatus, reagents and solutions
Atomic absorption spectrometer with a radiation source for tin.
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.
Tin GOST 860 with a mass fraction of tin is not less than 99.9%.
Standard solutions of tin.
Solution A, prepared as follows: 0.5 g of tin are dissolved in a water bath 10 cmof the 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 2 mol/DM
of hydrochloric acid.
1 cmof the solution contains 0.005 g of tin.
Solution B is prepared as follows: 10 cmof the solution And transferred to a volumetric flask with a capacity of 100 cm
and then filled to the mark with a solution of 2 mol/DM
of hydrochloric acid.
1 cmof a solution contains 0.0005 g olo
VA.
7.3. Analysis
7.3.1. 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, rinse walls of beaker with a solution of 1 mol/DM
of hydrochloric acid and topped up to the mark with the same acid.
Measure the atomic absorption of tin in the flame of acetylene-air or acetylene-nitrous oxide at a wavelength of 286,3 nm 224,6 or parallel to the calibration solutions.
7.3.2. Construction of calibration curve
Ten of the eleven volumetric flasks with a capacity of 100 cmis placed 4,0; 10,0 cm
standard solution B, and 2,0; 3,0; 4,0; 6,0; 8,0; 10,0; 12,0 and 14.0 cm
standard solution And tin. All the flasks made up to the mark solution of 2 mol/DM
of hydrochloric acid.
Measure the atomic absorption of tin as specified in clause
7.4. Processing of the results
7.4.1. Mass fraction of tin () in percent is calculated by the formula
where is the concentration of tin was found in the calibration schedule, g/cm
;
— the volume of the sample solution, cm
;
— the weight of the portion,
7.4.2. The absolute discrepancies in the results of parallel measurements (the rate of convergence) must not exceed the permissible values given in table.1.
(Changed edition, Rev. N 2).
7.4.3. The absolute discrepancies of the analysis results obtained in two different laboratories or two of the results of the analysis conducted in the same laboratory but under different (a measure of reproducibility) shall not exceed the values given in table.1.
7.4.4. Control of accuracy of analysis results
Control of accuracy of analysis results of tin is carried out according to claim
7.4.3,
