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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, ГОСТ 9853.13-96 Титан губчатый. Метод определения олова1.84 g/cmГОСТ 9853.13-96 Титан губчатый. Метод определения олова, 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/DMГОСТ 9853.13-96 Титан губчатый. Метод определения олова.

Tartaric acid according to GOST 5817, solution mass concentration of 200 g/DMГОСТ 9853.13-96 Титан губчатый. Метод определения олова.

Acetone according to GOST 2603.

Ammonia water according to GOST 3760, solution mass concentration of 250 g/DMГОСТ 9853.13-96 Титан губчатый. Метод определения олова.

Copper sulfate (copper sulphate) according to GOST 4165, solution mass concentration 10 g/DMГОСТ 9853.13-96 Титан губчатый. Метод определения олова.

Of hydroxylamine sulfate (hydroxylamine sulphate) according to GOST 7298, solution mass concentration of 20 g/DMГОСТ 9853.13-96 Титан губчатый. Метод определения олова.

Tionale according to the normative document, solution mass concentration of 20 g/lГОСТ 9853.13-96 Титан губчатый. Метод определения оловаin acetone.

The washing liquid: a solution containing in 1000 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаwater 10 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаsolution thionalide mass concentration of 20 g/DMГОСТ 9853.13-96 Титан губчатый. Метод определения олова.

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/DMГОСТ 9853.13-96 Титан губчатый. Метод определения олова: 0.03 g phenylfluorene dissolved in ethanol, added with 1 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof sulfuric acid solution (1:1) and topped up with ethanol to a volume of 100 cmГОСТ 9853.13-96 Титан губчатый. Метод определения олова. The solution should have a pink color.

Hydrogen peroxide according to GOST 10929, solution mass concentration of 30 g/DMГОСТ 9853.13-96 Титан губчатый. Метод определения олова.

The polyvinyl alcohol according to GOST 10779, solution mass concentration 10 g/DMГОСТ 9853.13-96 Титан губчатый. Метод определения оловаor food gelatin according to GOST 11293, solution mass concentration of 5 g/DMГОСТ 9853.13-96 Титан губчатый. Метод определения олова, freshly prepared.

Sodium acetate (sodium acetate) 3-water according to GOST 199.

Acetic acid according to GOST 61, solution mass concentration of 700 g/DMГОСТ 9853.13-96 Титан губчатый. Метод определения олова.

Buffer solution with a pH of 3: 20 g of sodium acetate are dissolved in 70 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof water, filtered in a volumetric flask with a capacity of 200 cmГОСТ 9853.13-96 Титан губчатый. Метод определения олова, 48 cm, addГОСТ 9853.13-96 Титан губчатый. Метод определения оловаacetic 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/DMГОСТ 9853.13-96 Титан губчатый. Метод определения олова.

Standard solutions of tin.

Solution a: 0.1 g of tin are dissolved in 10 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof sulphuric acid and evaporated until the appearance of sulphuric acid fumes. The residue was cooled to room temperature, dissolved in 50 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof sulfuric acid solution (1:9), transferred to a measuring flask with volume capacity of 1000 cmГОСТ 9853.13-96 Титан губчатый. Метод определения олова, top up with sulphuric acid solution (1:9) to the mark and mix; best to use within 3 months.

1 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof the solution contains 0.0001 g of tin.

Solution B: 2 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof solution A is placed in a volumetric flask with a capacity of 100 cmГОСТ 9853.13-96 Титан губчатый. Метод определения олова, top up with sulphuric acid solution (1:9) to the mark and mix; prepare before use.

1 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof 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 cmГОСТ 9853.13-96 Титан губчатый. Метод определения олова, add 100 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof 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 cmГОСТ 9853.13-96 Титан губчатый. Метод определения олова, 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 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof 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 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof water, 20 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof 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 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof a solution of sulphate of copper, 5 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof a solution of hydroxylamine sulphate, 25 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof sulfuric acid solution (1:3) and add water to about 200 cmГОСТ 9853.13-96 Титан губчатый. Метод определения олова.

The solution is heated to about 333 K and poured 8 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаsolution 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 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof nitric acid, 5 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof hydrochloric acid, 4 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof sulfuric acid is ГОСТ 9853.13-96 Титан губчатый. Метод определения олова1.84 g/cmГОСТ 9853.13-96 Титан губчатый. Метод определения олова. 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 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаwater, 5 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof 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 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof a solution of hydroxylamine sulphate, 25 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof sulfuric acid solution (1:3) and add water to about 200 cmГОСТ 9853.13-96 Титан губчатый. Метод определения олова.

The solution is heated to about 333 K, poured 8 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаsolution 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 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof water, heated to dissolve the salts, cooled to room temperature, transferred to a volumetric flask with a capacity of 100 cmГОСТ 9853.13-96 Титан губчатый. Метод определения олова, made up to the mark with water and mix.

Aliquot part of the solution 2 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаis placed in a volumetric flask with a capacity of 50 cmГОСТ 9853.13-96 Титан губчатый. Метод определения олова, 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 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof sulfuric acid solution (1:1), 5 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof hydrogen peroxide solution, 10 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаbuffer solution, 5 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаsolution of polyvinyl alcohol or of 2.5 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаgelatin solution and 1 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof 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 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаis placed 1,0; 2,0; 3,0; 4,0; 5,0 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаstandard 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 cmГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof sulfuric acid solution (1:9). To all flasks add water to a volume of 20 cmГОСТ 9853.13-96 Титан губчатый. Метод определения олова, 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 ГОСТ 9853.13-96 Титан губчатый. Метод определения олова,%, is calculated by the formula

ГОСТ 9853.13-96 Титан губчатый. Метод определения олова, (1)


where ГОСТ 9853.13-96 Титан губчатый. Метод определения олова — weight of tin in the sample solution found by the calibration schedule g;

ГОСТ 9853.13-96 Титан губчатый. Метод определения олова — total volume of sample solution, cmГОСТ 9853.13-96 Титан губчатый. Метод определения олова;

ГОСТ 9853.13-96 Титан губчатый. Метод определения олова — the mass of sample, g;

ГОСТ 9853.13-96 Титан губчатый. Метод определения олова — volume aliquote parts of a solution of the sample, cmГОСТ 9853.13-96 Титан губчатый. Метод определения олова.

7 the Permissible error of measurement

7.1 the discrepancy between the measurement results and analysis results (at a confidence probability ГОСТ 9853.13-96 Титан губчатый. Метод определения оловаof 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 ГОСТ 9853.13-96 Титан губчатый. Метод определения олова

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.