GOST 9853.13-96
GOST 9853.13−96 Titan spongy. Method for determination of tin
GOST 9853.13−96
Group B59
INTERSTATE STANDARD
TITANIUM SPONGE
Method for determination of tin
Sponge titanium. Method for determination of tin
ISS 77.120*
AXTU 1709
_________________________________
* In the index «National standards», 2008
OKS 77.120, 77.120.50 — note the manufacturer’s database.
Date of introduction 2000−07−01
Preface
1 DEVELOPED by the Interstate technical Committee for standardization MTK 105, Ukrainian research and design Institute of titanium
SUBMITTED to the State Committee of Ukraine for standardization, Metrology and certification
2 ADOPTED by the Interstate Council for standardization, Metrology and certification (Protocol No. 9 dated April 12, 1996)
The adoption voted:
| The name of the state | The name of the national authority for standardization |
| The Republic Of Azerbaijan |
Azgosstandart |
| The Republic Of Belarus |
Gosstandart Of Belarus |
| The Republic Of Kazakhstan |
Gosstandart Of The Republic Of Kazakhstan |
| Russian Federation |
Gosstandart Of Russia |
| Turkmenistan |
The main state inspection of Turkmenistan |
| Ukraine |
Gosstandart Of Ukraine |
3 Resolution of the State Committee of the Russian Federation for standardization and Metrology dated 19 October 1999 No. 353-St inter-state standard GOST 9853.13−96 introduced directly as state standard of the Russian Federation from July 1, 2000.
4 INTRODUCED FOR THE FIRST TIME
1 Scope
This standard sets the photometric method for the determination of tin (with mass fraction of tin from 0.005% to 0.02%) in the spongy titanium according to GOST 17746.
The method is based on the formation in sulfuric acid medium at pH 3 colloidal solution of complex compounds of tin (IV) with phenylfluorone yellow-orange color, and then measure the optical density of the solution.
2 Normative references
The present standard features references to the following standards:
GOST 8.315−97 State system for ensuring the uniformity of measurements. The standard samples. The main provisions, the order of development, certification, approval, registration and application
GOST 61−75 acetic Acid. Specifications
GOST 199−78 Sodium acetate 3-water. Specifications
GOST 2603−79 Acetone. Specifications
GOST 3760−79 Ammonia water. Specifications
GOST 4165−78 Copper II sulphate 5-water. Specifications
GOST 4204−77 sulfuric Acid. Specifications
GOST 4461−77 nitric Acid. Specifications
GOST 5817−77 tartaric Acid. Specifications
GOST 7298−79 Hydroxylamine sulfate. Specifications
GOST 10779−97 polyvinyl alcohols. Specifications
GOST 10929−76 Hydrogen peroxide. Specifications
GOST 11293−89 Gelatin. Specifications
GOST 14261−77 hydrochloric Acid of high purity. Specifications
GOST 17746−96 spongy Titanium. Specifications
GOST 18300−87 ethyl rectified technical. Specifications
GOST 23780−96 spongy Titanium. Methods of sampling and sample preparation
GOST 25086−87 non-ferrous metals and their alloys. General requirements for methods of analysis
3 General requirements
3.1 General requirements for the method of analysis according to GOST 25086.
3.2 Selection and preparation of samples is carried out according to GOST 23780.
3.3 Mass fraction of tin is determined by two batches.
4 measuring instruments and auxiliary devices
The spectrophotometer or photoelectric colorimeter KFK-2.
Hydrochloric acid according to GOST 14261, diluted 1:1.
Sulfuric acid according to GOST 4204, 1.84 g/cm
, and diluted 1:1, 1:3, 1:4, 1:9.
Nitric acid according to GOST 4461.
Acid chloride according to the current normative document, solution mass concentration of 300 g/DM.
Tartaric acid according to GOST 5817, solution mass concentration of 200 g/DM.
Acetone according to GOST 2603.
Ammonia water according to GOST 3760, solution mass concentration of 250 g/DM.
Copper sulfate (copper sulphate) according to GOST 4165, solution mass concentration 10 g/DM.
Of hydroxylamine sulfate (hydroxylamine sulphate) according to GOST 7298, solution mass concentration of 20 g/DM.
Tionale according to the normative document, solution mass concentration of 20 g/lin acetone.
The washing liquid: a solution containing in 1000 cmwater 10 cm
solution thionalide mass concentration of 20 g/DM
.
Ethanol (ethyl alcohol) rectified technical GOST 18300.
Phenylfluorone (2, 6, 7, trioxo-9-(dimethyl-AMINOPHENYL)-fluoro-6) according to the current normative document, solution mass concentration of 0.3 g/DM: 0.03 g phenylfluorene dissolved in ethanol, added with 1 cm
of sulfuric acid solution (1:1) and topped up with ethanol to a volume of 100 cm
. The solution should have a pink color.
Hydrogen peroxide according to GOST 10929, solution mass concentration of 30 g/DM.
The polyvinyl alcohol according to GOST 10779, solution mass concentration 10 g/DMor food gelatin according to GOST 11293, solution mass concentration of 5 g/DM
, freshly prepared.
Sodium acetate (sodium acetate) 3-water according to GOST 199.
Acetic acid according to GOST 61, solution mass concentration of 700 g/DM.
Buffer solution with a pH of 3: 20 g of sodium acetate are dissolved in 70 cmof water, filtered in a volumetric flask with a capacity of 200 cm
, 48 cm, add
acetic acid, made up to the mark with water and mix.
State standard samples according to GOST 8.315.
4-NITROPHENOL according to the current normative document, solution mass concentration of 1 g/DM.
Standard solutions of tin.
Solution a: 0.1 g of tin are dissolved in 10 cmof sulphuric acid and evaporated until the appearance of sulphuric acid fumes. The residue was cooled to room temperature, dissolved in 50 cm
of sulfuric acid solution (1:9), transferred to a measuring flask with volume capacity of 1000 cm
, top up with sulphuric acid solution (1:9) to the mark and mix; best to use within 3 months.
1 cmof the solution contains 0.0001 g of tin.
Solution B: 2 cmof solution A is placed in a volumetric flask with a capacity of 100 cm
, top up with sulphuric acid solution (1:9) to the mark and mix; prepare before use.
1 cmof solution B contains 0,000002 g tin.
5 procedures for measuring
5.1 Sample weight of 2 g is placed in a conical flask with a capacity of 200 cm, add 100 cm
of hydrochloric acid (1:1), beaker cover watch glass or glass funnel and heated until complete dissolution of the sample, maintaining constant volume with the same solution of hydrochloric acid.
The solution was cooled to room temperature, transferred into a beaker with a capacity of 300 cm, put the glass with the solution on the stove and heated to boiling. The solution was added dropwise nitric acid until the disappearance of the purple color, go 30 cm
of sulfuric acid solution (1:1) and evaporated to the appearance of sulphuric acid fumes.
The solution was cooled to room temperature, wash the side of the Cup with water, place the beaker with the solution on the stove, is evaporated until the appearance of fumes of sulfuric acid and heating was continued for 5 min.
The solution was cooled, poured 60−70 cmof water, 20 cm
of a solution of tartaric acid, heated to boiling and cooled to room temperature.
The solution is neutralized with ammonia solution on the paper of the Congo to the lilac colouring of paper, pour 1 cmof a solution of sulphate of copper, 5 cm
of a solution of hydroxylamine sulphate, 25 cm
of sulfuric acid solution (1:3) and add water to about 200 cm
.
The solution is heated to about 333 K and poured 8 cmsolution thionalide (for deposition of tin) with vigorous stirring. For a better coagulation of the precipitate and a complete selection of tin in the solution was periodically stirred and leave for 10−12 hours.
The solution was then filtered through filter «blue ribbon», washed the precipitate on the filter 5−6 times the flushing fluid, the filter with the sediment was placed in a beaker, which led the deposition of tin, poured 20 cmof nitric acid, 5 cm
of hydrochloric acid, 4 cm
of sulfuric acid is
1.84 g/cm
. Cover the beaker porcelain Cup and the solution is evaporated until the appearance of sulphuric acid fumes.
The solution was cooled to room temperature, wash the side of the Cup with water, again evaporated until the appearance of fumes of sulfuric acid and heating was continued for 5 min.
The solution was cooled to room temperature, poured 60−70 cmwater, 5 cm
of a solution of tartaric acid and heated to boiling.
The solution was cooled to room temperature, neutralized with ammonia solution on the paper of the Congo to the lilac colouring of paper, pour 3 cmof a solution of hydroxylamine sulphate, 25 cm
of sulfuric acid solution (1:3) and add water to about 200 cm
.
The solution is heated to about 333 K, poured 8 cmsolution tionality for the secondary deposition of tin and then do as described above, starting with step deposition of tin to the operation of the dual evaporation of sulfuric acid.
The solution was then cooled, poured 40 cmof water, heated to dissolve the salts, cooled to room temperature, transferred to a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix.
Aliquot part of the solution 2 cmis placed in a volumetric flask with a capacity of 50 cm
, add 1−2 drops of a solution of 4-NITROPHENOL and neutralized with ammonia solution until yellow-green color. Then poured dropwise a solution of sulfuric acid (1:9) to the bleaching solution, add 1.4 cm
of sulfuric acid solution (1:1), 5 cm
of hydrogen peroxide solution, 10 cm
buffer solution, 5 cm
solution of polyvinyl alcohol or of 2.5 cm
gelatin solution and 1 cm
of solution phenylfluorone. The solution was topped to the mark with water and mix. After 30−40 min measure the optical density of the solutions at a wavelength of 490−510 nm.
Solution comparison is R
actor control experience.
5.2 For constructing a calibration curve in five out of six volumetric flasks with a capacity of 50 cmis placed 1,0; 2,0; 3,0; 4,0; 5,0 cm
standard solution B, which corresponds to the 0,000002; 0,000004; 0,000006; 0,000008; 0,000010 g tin. The sixth flask, a solution which is a solution of the reference experiment, pour 1 cm
of sulfuric acid solution (1:9). To all flasks add water to a volume of 20 cm
, 1−2 drops of a solution of 4-NITROPHENOL and neutralized with ammonia solution until yellow-green color.
Then do as specified in 5.1.
According to the obtained values of optical density and corresponding mass of tin to build a calibration curve.
6 Processing of measurement results
Mass fraction of tin ,%, is calculated by the formula
where — weight of tin in the sample solution found by the calibration schedule g;
— total volume of sample solution, cm
;
— the mass of sample, g;
— volume aliquote parts of a solution of the sample, cm
.
7 the Permissible error of measurement
7.1 the discrepancy between the measurement results and analysis results (at a confidence probability of 0.95) shall not exceed the permissible values given in table 1.
Table 1
Percentage
| Mass fraction of tin | The permissible discrepancy between the results of the parallel measurements |
The permissible discrepancy between the results of the analysis | The margin of error of measurement |
| From 0.005 to 0.020 incl. | 0,002 |
0,003 | 0,002 |
7.2 accuracy Control of the results of the analysis carried out according to standard sample in accordance with GOST 25086.
Allowed to monitor the accuracy of analysis results by the method of additives in accordance with GOST 25086.
Additives is a standard solution A.
8 qualifications
To perform analysis allowed the analyst qualification not less than 4th level.
