GOST 19863.11-91

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  ГОСТ 19863.11-91

GOST 19863.11−91 Alloy of titanium. Method for the determination of palladium

GOST 19863.11−91

Group B59

STATE STANDARD СОЮ3А SSR

ALLOYS OF TITANIUM

Method for the determination of palladium

Titanium alloys.
Method for the determination of palladium

AXTU 1709

Date of introduction 1992−07−01

INFORMATION DATA

1. DEVELOPED AND INTRODUCED by the Ministry of aviation industry of the USSR

DEVELOPERS

V. G. Davydov, doctor of engineering. Sciences; V. A. Moshkin, PhD. tech. Sciences; G. I. Friedman, PhD. tech. Sciences; L. A. Tenyakova

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee on management of quality and standards from 5.05.91 N 625

3. REPLACE GOST 19863.11−80

4. The frequency of inspection — 5 years

5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

This standard sets the photometric method for the determination of palladium (with a mass fraction of from 0.05 to 1.0%).

1. GENERAL REQUIREMENTS

1.1. General requirements for methods of analysis GOST 25086 with the Supplement.

1.1.1. For the results analysis be the arithmetic mean of results of two parallel measurements.

2. THE ESSENCE OF THE METHOD

The method is based on dissolving the sample in hydrochloric and bridgestation acids in the presence of tartaric acid, the formation at pH 1 complex compounds of palladium with nitroso-R-salt, colored red-orange color, and measuring the optical density of the solution at a wavelength of 510 nm. The color of the complex is stable for one day.

The definition does not interfere with niobium, molybdenum, vanadium, aluminum; prevent zirconium and chromium at their ratio to palladium greater than 1:1.

3. APPARATUS, REAGENTS AND SOLUTIONS

Spectrophotometer or photoelectrocolorimeter.

Thermometer liquid-in-glass or mercury up to 100 °C with a scale division of 1°.

Hydrochloric acid according to GOST 3118 density of 1.19 g/cmand a solution of 1:1.

Nitric acid according to GOST 4461 density of 1,35−1,40 g/cm.

Acids mixture: one part nitric acid and three parts hydrochloric acid.

Tartaric acid according to GOST 5817, a solution of 500 g/DM.

Hydrofluoric acid according to GOST 10484.

Boric acid according to GOST 9656.

Acid bridgestation: 280 cmhydrofluoric acid at a temperature of (10±2) °C add portions 130 g of boric acid and stirred. The reagent is prepared and stored in a plastic container.

Nitroso-R-salt, a solution of 1 g/DM.

Palladium according to GOST 13462 brand PD of 99.9.

Palladium standard solution: 0.1 g of palladium were placed in a glass with a capacity of 100 cm, poured 10 cmof the mixture of acids, moderate heat until dissolved, evaporated to dry salts, poured 5cmof hydrochloric acid and again evaporated to dryness. The operation is repeated.

The dry residue is dissolved in 5 cmof hydrochloric acid, poured 10 cmof water, heated to boiling and boiled for 1 min. the Solution was cooled to room temperature, 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 0.0001 g of palladium.

4. ANALYSIS

4.1. A portion of the sample weight in accordance with table.1 is placed in a conical flask with a capacity of 100 cm, flow 10 cmof hydrochloric acid, 2cmbridgestation acid, 10 cmof a solution of tartaric acid, mixed and moderately heated to complete dissolution.

Table 1

To the solution add 5−10 drops of nitric acid until the termination of allocation of gas bubbles and the disappearance of a purple color, then the solution was cooled to room temperature, add 20 cmof a solution of tartaric acid, transferred to a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix.

4.2. Aliquot part of the solution was 10 cm,transferred to a conical flask with a capacity of 100 cm, top up with water to 80 cm, poured 10 cmof the solution, nitroso-R-salt and heated to boiling.

The solution was cooled to room temperature, transferred to a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix.

4.3. Optical density of the solution is measured at a wavelength of 510 nm in a cuvette with a layer thickness fotometricheskogo 30 mm. Solution comparison the solution serves as the reference experiment, which is prepared according to claim 4.1 all used in the analysis reagents.

Mass fraction of palladium is determined according to the calibration schedule.

4.4. Construction of calibration curve

In eight of the nine conical flasks with a capacity of 100 cmmeasured from microburette 0,2; 0,4; 0,6; 0,8; 1,0; 1,2; 1,4; 1,6 cmstandard solution palladium, pour in 1 cmof a hydrochloric acid solution at 80 cmof water and then continue on PP.4.2 and 4.3.

Solution comparison is the solution in which palladium is not entered.

According to the obtained values of optical density of the solutions and their corresponding masses of palladium to build the calibration graph.

5. PROCESSING OF THE RESULTS

5.1. Mass fraction of palladium () in percent is calculated by the formula

,

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

 — weight of sample in aliquote part of the solution,

5.2. Discrepancies in the results must not exceed the values given in table.2.

Table 2