GOST 9853.12-96

• gost-985312-96.pdf (216.79 KiB)
  ГОСТ 9853.12-96

GOST 9853.12−96 Titan spongy. Method for the determination of zirconium

GOST 9853.12−96

Group B59

INTERSTATE STANDARD

TITANIUM SPONGE

Method for the determination of zirconium

Sponge titanium. Method for determination of zirconium

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:

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 9853.12−96 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 zirconium sponge titanium (at a mass fraction of zirconium from 0.001% to 1.0%) according to GOST 17746.

The method is based on the formation of a yellow-red complex compound of zirconium selenology orange in sulfuric acid medium and subsequent measurement of 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 3760−79 Ammonia water. Specifications

GOST 3773−72 Ammonium chloride. Specifications

GOST 4204−77 sulfuric Acid. Specifications

GOST 4461−77 nitric Acid. Specifications

GOST 10652−73 Salt is the disodium Ethylenediamine-N, N, N', N'-tetraoxane acid 2-water (Trilon B)

GOST 17746−96 spongy Titanium. 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 zirconium is determined by two batches.

3.4 the construction of calibration curve, each calibration point is based on the average of the results of the two measurements.

4 measuring instruments and auxiliary devices

Spectrophotometer type SF-46 or photoelectric concentration colorimeter KFK-2, or similar device.

Sulfuric acid according to GOST 4204, concentrated, dilute 1:4 solution of molar concentration 0.5 mol/DM.

Nitric acid according to GOST 4461.

Trilon B according to GOST 10652, a solution of molar concentration 0.05 mol/DM.

Ascorbic acid according to the State Pharmacopoeia X, solution mass concentration of 50 g/DM, freshly prepared.

Selenology orange, according to existing normative document, solution mass concentration of 1 g/DM.

Ammonium chloride (ammonium chloride) according to GOST 3773.

Ammonia water according to GOST 3760, solution mass concentration of 250 g/DM.

Standard samples according to GOST 8.315.

Hypochlorite Zirconia (zirconium oxychloride) 8-water according to the current normative document.

Filter obezdolennyh «red tape» according to the current normative document.

Standard solutions of zirconium.

Solution a: 3,533 g hypochlorite Zirconia is dissolved in 40 cmof concentrated sulfuric acid, the solution transferred into a measuring flask with volume capacity of 1000 cm, made up to the mark with water and mix.

1 cmof the solution contains 0.001 g of zirconium.

Solution B: aliquote part 1 cmof solution A is placed in a volumetric flask with a capacity of 100 cm, made up to the mark solution of 0.5 mol/DMsulfuric acid.

1 cmof solution B has the 0.00001 g of zirconium.

5 procedures for measuring

5.1 When determining the mass fraction of zirconium from 0.001% to 0.1%

A sample weighing 0.2−1.0 g were placed in a glass with a capacity of 100 cmor a conical flask, poured 40 cmof sulfuric acid solution (1:4) and lead dissolving when heated. After complete dissolution of the sample in the sample solution was added dropwise nitric acid until the disappearance of violet colour, add 2−3 drops of excess solution is evaporated until the appearance of sulphuric acid fumes and cooled.

The solution is evaporated to a syrup diluted with hot water to a volume of 50 cm, add 1−1. 5 g of ammonium chloride and stirring, the precipitated amount of Sesqui-oxides with a solution of aqueous ammonia until a clear stable smell. After deposition, the solution was cooled to a warm state and filtered through the filter «red ribbon». The precipitate is washed with hot water with a few drops of ammonia.

Filter the precipitate is transferred with water into a glass with a capacity of 250 cm, injected 4 cmof concentrated sulphuric acid and evaporated until the appearance of the lungs of sulfuric acid vapor.

The precipitate dissolves with the appearance of sulphuric acid fumes. The obtained transparent solution was cooled, 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, according to table 1 is placed into two volumetric flasks with a capacity of 50 cm, a solution of sulfuric acid in accordance with table 1, 2 cmof a solution of ascorbic acid. Aliquotes to one portion add 0.5 cmof the solution Trilon B. In both flasks with solutions are added in 1 cmkylinalove orange, made up to the mark with water and mix.


Table 1

After 15 min measure the optical density of the solution at a wavelength of 540 nm and the thickness of the absorbing layer is 50 mm. Solution comparison the solution serves as the reference experiment with the introduction of Trilon B.

5.2 in determining the mass fraction of zirconium than 0.1%

A sample weighing 0.1−0.2 g of titanium was placed in a conical flask with a capacity of 100 cm, flow 18 cmof sulfuric acid solution (1:4) and conduct the dissolution under heating, maintaining the initial volume by adding water. The resulting solution is added dropwise nitric acid until the disappearance of the purple color and the solution is evaporated until the appearance of sulphuric acid fumes. Evaporated solution is diluted with a small amount of water, transferred into a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix.

Aliquot part of the solution, according to table 1 is placed into two volumetric flasks with a capacity of 50 cm, a solution of sulfuric acid in accordance with table 1, 2 cmof a solution of ascorbic acid. Aliquotes to one portion add 0.5 cmof the solution Trilon B. In both flasks with solutions are added in 1 cmkylinalove orange, made up to the mark with water and mix. Then do as above.

The mass of zirconium in the sample is calculated according to the calibration schedule

.

5.3 Construction of calibration curve

In eight of the nine volumetric flasks with a capacity of 50 cmplaced 0,25; 0,5; 1,0; 2,0; 3,0; 4,0; 5,0 and 8.0 cmof a standard solution B, which corresponds to 0,0000025; 0,000005; 0,00001; 0,00002; 0,00003; 0,00004; 0,00005; 0,00008 g of zirconium. A ninth solution of the flask is a solution of the reference experiment.

The solutions in all flasks was diluted to 20 cmwith a sulfuric acid solution with a concentration of 0.5 mol/DM, add 2 cmof ascorbic acid, 1 cmof solution kylinalove orange, made up to the mark with water and mix.

After 15 min measure absorbance at a wavelength of 540 nm.

According to the obtained values of optical density and corresponding mass of zirconium to build a calibration curve.

6 Processing of measurement results

Mass fraction of zirconium ,%, is calculated by the formula

, (1)

where is the mass of zirconium 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 2.


Table 2

Percentage

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 additions.

Additives is a standard solution A.

8 qualifications

To perform analysis allowed the analyst qualification not less than 4th level.