GOST 9853.11-96

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  ГОСТ 9853.11-96

GOST 9853.11−96 Titan spongy. Method for determination of copper

GOST 9853.11−96

Group B59

INTERSTATE STANDARD

TITANIUM SPONGE

Method for determination of copper

Sponge titanium. Method for determination of copper

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 9853.11−96 introduced directly as state standard of the Russian Federation from July 1, 2000.

4 INTRODUCED FOR THE FIRST TIME

1 Scope

This standard specifies the extraction-photometric method for the determination of copper (at a mass fraction of copper from 0.0005% to 0.2%) in the spongy titanium according to GOST 17746.

The method is based on the formation of complex compounds of copper with sodium diethyldithiocarbamate in ammoniacal medium, with subsequent extraction of the complex with chloroform and measuring the optical density of the extract.

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 859−78* Copper. Brand
________________
* On the territory of the Russian Federation GOST 859−2001, here and hereafter. — Note the manufacturer’s database.

GOST 3760−79 Ammonia water. Specifications

GOST 4204−77 sulfuric Acid. Specifications

GOST 4461−77 nitric Acid. Specifications

GOST 4517−87 Reagents. Methods for the preparation of accessory reagents and solutions used in the analysis

GOST 8864−71 Sodium N, N-diethyldithiocarbamate 3-water. Specifications

GOST 9656−75 boric Acid. Specifications

GOST 10484−78 hydrofluoric 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 18300−87 ethyl rectified technical. Specifications

GOST 20015−88 Chloroform. 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 copper 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

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

pH meter pH-121.

Sulfuric acid according to GOST 4204.

Hydrofluoric acid according to GOST 10484.

Boric acid according to GOST 9656.

Nitric acid according to GOST 4461, diluted 1:1.

Trilon B according to GOST 10652.

Bidistilled water, prepared according to GOST 4517.

Ammonia water according to GOST 3760, solution mass concentration of 100 g/DM.

Chloroform according to GOST 20015.

Copper grade MO according to the GOST 859.

Ammonium citrate (ammonium citrate) according to the current normative document, solution mass concentration of 300 g/DM.

Diethyldithiocarbamate sodium 3-water according to GOST 8864, solution mass concentration of 1 g/DM(usable 2−3 days).

Ethanol (ethyl alcohol) according to GOST 18300.

Standard samples according to GOST 8.315.

Standard solutions of copper.

Solution a: 0.1 g of copper (99.95% purity) was dissolved in a solution of nitric acid. The solution was boiled to remove oxides of nitrogen, cooled to room temperature, transferred into a measuring flask with volume capacity of 1000 cm, made up to the mark with water and mix; the solution is usable for 3 months.

1 cmof the solution contains 0.0001 g of copper.

Solution B: 20 cmsolution And placed in a volumetric flask with a capacity of 200 cm, made up to the mark with water and mix; prepare before use.

1 cmof solution B has the 0.00001 g of copper.

5 procedures for measuring

5.1 a sample mass of 0.1−1.0 g was placed in a quartz glass with a capacity of 100 cm, flow 25 cmof sulfuric acid solution (1:1), add dropwise 1−2 cmhydrofluoric acid and dissolved by heating. After complete dissolution of the sample is added dropwise nitric acid until the disappearance of the violet color of the solution and 2−3 drops of its excess, the solution boiled to remove oxides of nitrogen.

The solution was cooled, transferred to a polyethylene beaker with a capacity of 200 cm, add 20 cmof ammonium citrate solution, 10 cmof the solution Trilon B, then add small portions of ammonia water to pH 8.5.

The solution was cooled to room temperature and transferred to a separatory funnel with a capacity of 250 cm. Pour 10 cmof a solution of sodium diethyldithiocarbamate, 10 cmof chloroform and shaken for 2 min. the Organic layer is separated in a volumetric flask with a capacity of 25 cm, repeat the extraction, adding each time 5 cmof chloroform. The combined extracts in the flask was adjusted to the mark with chloroform, mix and measure the optical density of the solution at a wavelength of 440 nm and the thickness of the absorbing layer of 10 mm Solution comparison is the solution of the reference experiment.

Mass of copper in the sample is calculated according to the calibration gra

fico.

5.2 For constructing the calibration curve in six of the seven plastic cups with a capacity of 200 cmis placed 0,5; 1,0; 3,0; 5,0; 10,0; 20,0 cmstandard solution B, which corresponds to 0,000005; 0,000010; 0,000030; 0,000050; 0,000100; 0,000200 g of copper. The solution of the seventh glass is a solution in the reference experiment. All the glasses are poured 25 cmof sulphuric acid diluted 1:1, and further receives, as described in 5.1.

According to the obtained values of optical density and corresponding mass of copper to build the calibration graph.

6 Processing of measurement results

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

, (1)

where is the mass of copper in the sample solution found by the calibration schedule g;

 — the weight of the portion,

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

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 qualifications at least 4-th category