GOST 9853.17-96

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  ГОСТ 9853.17-96

GOST 9853.17−96 Titan spongy. Method for the determination of palladium

GOST 9853.17−96

Group B59

INTERSTATE STANDARD

TITANIUM SPONGE

Method for the determination of palladium

Sponge titanium.
Method for determination of palladium

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 9853.17−96 introduced directly as state standard of the Russian Federation from July 1, 2000.

4 INTRODUCED FOR THE FIRST TIME

1 Scope

This standard establishes the atomic absorption method for the determination of palladium (with mass fraction of palladium from 0.005% to 0.015%) in the spongy titanium according to GOST 17746.

The method is based on measuring atomic absorption of palladium in electrothermal atomization mode at a wavelength 247,6 nm.

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 10157−79 Argon gaseous and liquid. Specifications

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

GOST 11125−84 nitric Acid of high purity. Specifications

GOST 13462−79 Palladium and palladium alloys. Brand

GOST 14261−77 hydrochloric Acid of high purity. Specifications

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 methods of analysis GOST 25086.

3.2 Selection and preparation of samples is carried out according to GOST 23780.

3.3 Mass fraction of palladium is determined in 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

Atomic absorption spectrophotometer equipped with a graphite atomizer.

The spectral lamp with a hollow cathode for palladium.

Argon gas according to GOST 10157.

Nitric acid according to GOST 11125.

Hydrochloric acid according to GOST 14261, of 1.19 g/cmand diluted 1:1.

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

Palladium brand PD 99,9 GOST 13462.

Standard samples according to GOST 8.315.

Standard solutions of palladium.

Solution a: 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 to 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.

Solution B: 5 cmsolution And placed in a volumetric flask with a capacity of 50 cm, add 20 cmof a hydrochloric acid solution (1:1), made up to the mark and mix. The solution is prepared before use.

1 cmof solution B contains 0,00001 g of palladium.

Ethylenediamine-N, N, N', N'-tetraoxane acid disodium salt (Trilon B) according to GOST 10652, solution mass concentration 10 g/DM.

5 procedures for measuring

5.1 the sample sample weighing 0.5 g was placed in a beaker with a capacity of 100 cm, flow 20 cmof hydrochloric acid and lead dissolving when heated, covered with a glass watch glass and maintaining the volume of solution in the glass about 20 cmby the addition of hydrochloric acid.

After complete dissolution of the sample is added dropwise nitric acid to the bleaching solution and boil for 1−2 min. the Solution was cooled to room temperature, transferred to a volumetric flask with a capacity of 100 cm, 70 cm, addhydrochloric acid solution (1:1), 5 cmof the solution Trilon B, made up to the mark with water and mix.

To prepare the solution in the reference experiment in a beaker with a capacity of 100 cmis placed 20 cmof hydrochloric acid, heated to boiling, add 2−3 drops of nitric acid and boil for 1−2 min. the Solution was cooled, transferred to a volumetric flask with a capacity of 100 cm, 70 cm, addhydrochloric acid solution (1:1), 5 cmof the solution Trilon B, made up to the mark with water and mix.

Carry out construction of calibration curve or the graduation of the device when operating in the automatic re

the bench.

5.2 for the mass concentration of palladium from 0.005% to 0.015% in six sample beakers with a capacity of 100 cmis placed 0.5 g of sponge titanium with a palladium content of less than 0.005% and conduct dissolution as specified in 5.1.

The solutions were transferred into volumetric flask with a capacity of 100 cm, in five out of six volumetric flasks poured 2,5; 4,0; 5,0; 6,0; 7,5 cmstandard solution B, which corresponds to 0,25; 0,40; 0,50; 0,60; 0,75 ág/cmpalladium.

The sixth solution of the flask is a solution of titanium.

Poured in all six flasks at 5 cmof the solution Trilon B and a solution of hydrochloric acid (1:1) to the mark and mix.

5.2.1 Injected into the graphite cuvette with microdontia with a capacity of 0.02 cmconsistently the solution in the reference experiment, a solution of titanium and solutions containing a standard solution of palladium, in order of increasing concentration of palladium. Measurement of atomic absorption of palladium is carried out in a mode with electrothermal atomization with the parameters given in table 1.


Table 1

At the stage of atomization, the argon flow is stopped.

From the values of atomic absorption solutions containing additives of palladium standard solution, subtract the value of atomic absorption of a solution of titanium. According to the obtained values of the difference between of atomic absorption and corresponding mass concentrations of palladium (µg/cm) build a calibration curve in accordance with GOST 25086, which define the mass concentration of palladium in the solution in the reference experiment and in the solution of titanium.

5.3 When the apparatus is in an automatic mode is his graduation. To do this in four glasses with a capacity of 100 cmplaced the sponge titanium sample weight of 0.5 g with a palladium content of less than 0.005% and conduct dissolution as specified in 5.1.

The solutions were transferred to volumetric flasks with a capacity of 100 cm. In three of the four volumetric flasks with solutions of titanium pour 2,5; 5,0; 7,5 cmstandard solution B, which corresponds to 0,25; 0,50; 0,75 ág/cmpalladium.

The solution to the fourth flask is a solution of titanium.

Pour in all four flasks at 5 cmof the solution Trilon B, aqueous hydrochloric acid (1:1) to the mark and mix.

The solution in the reference experiment prepared as described in 5.1.

5.3.1 In a graphite cuvette with microdontia with a capacity of 0.02 cm, introduce a solution of titanium, then in ascending order of the concentration of palladium in solutions containing additives of a standard solution of palladium and carry out the calibration of an instrument.

Measurement of atomic absorption of palladium is carried out in the regime 5.2.1.

5.4 Further introduced into a graphite cuvette and the solutions in the reference experiment and analyze samples and conduct measurement of atomic absorption in palladium mode 5.2.1.

After every 4−5 measurements of atomic absorption is carried out the purification of the graphite cuvette: the cuvette microdontia administered in the dose of water is 0.02 cmand carry out atomization mode 5.2.1.

6 Processing of measurement results

Mass fraction of palladium in % is calculated by the formula

, (1)

where is the mass concentration of palladium in the sample solution, µg/cm;

 — mass concentration of palladium in the solution in the reference experiment, µ g/cm;

 — the volume of the sample solution, cm;

 — 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 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.

Control the accuracy of the results of the analysis carried out by the method of additives in accordance with GOST 25086.

Additives is a standard solution B.

8 qualifications

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