GOST 9853.22-96

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  ГОСТ 9853.22-96

GOST 9853.22−96 Titan spongy. Methods for determination of Nickel

GOST 9853.22−96

Group B59

INTERSTATE STANDARD

TITANIUM SPONGE

Methods for determination of Nickel

Sponge titanium. Methods for determination of nickel

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 9853.22−96 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 (mass fraction in Nickel from 0.005% to 0.15%) and atomic absorption (mass fraction in Nickel from 0.001% to 0.01%) methods for determination of Nickel in sponge titanium according to GOST 17746.

Extraction-photometric method based on formation of complex compounds of Nickel with dimethylglyoxime in the ammonia environment, its extraction with chloroform and subsequent measurement of optical density of the extract at a wavelength of 360 nm.

Atomic absorption method is based on measuring atomic absorption of Nickel at a wavelength of 232,0 nm in the electrothermal atomization mode.

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 849−97* Nickel primary. Specifications
________________
* On the territory of the Russian Federation GOST 849−2008, 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 5828−77 Dimethylglyoxime. Specifications

GOST 10157−79 Argon gaseous and liquid. Specifications

GOST 11125−84 nitric Acid of high purity. Specifications

GOST 14261−77 hydrochloric Acid of high purity. Specifications

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 methods of analysis GOST 25086.

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

3.3 Mass fraction of Nickel 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 Extraction-photometric method

4.1 measuring instruments and auxiliary devices

The spectrophotometer or photoelectric colorimeter concentration of type KLF-2, or similar device.

Sulfuric acid according to GOST 4204, diluted 1:1.

Hydrochloric acid according to GOST 14261, diluted 1:1.

Nitric acid according to GOST 4461, of 1.40 g/cm, diluted 1:1.

Ammonium tartrate (ammonium vinocity) according to the current normative document, solution mass concentration of 200 g/DM.

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

Ethanol (ethyl alcohol) rectified technical GOST 18300.

Dimethylglyoxime according to GOST 5828, an alcoholic solution of the mass concentration of 10 g/DM.

Chloroform according to GOST 20015.

Indicator paper litmus according to the current normative document.

The brand N22 Nickel GOST 849.

Standard samples according to GOST 8.315.

Standard solutions of Nickel.

Solution a: 0.2 g of Nickel dissolved in 15 cmof a hydrochloric acid solution and 5 cmof nitric acid (1:1) when heated, is evaporated to dryness, then add 10 cmof hydrochloric acid and again evaporated to dryness. Evaporation again when you add a solution of hydrochloric acid. Then add 100 cmof the hydrochloric acid solution, 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 0.0002 g of Nickel.

Solution B: 5 cmsolution And placed in a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix; prepare before use.

1 cmof solution B contains 0,00001 g

Nickel.

4.2 procedures for measuring

4.2.1 Sample the sample weight of 1.0 g (with a mass fraction of Nickel from 0.005% to 0.05%) and a weight of 0,5 g (with a mass fraction of Nickel in excess of 0.05% to 0.15%) is placed in a conical flask with a capacity of 250 cm, flow 40 cmof sulfuric acid solution and dissolved by heating. After complete dissolution, add dropwise nitric acid to the bleaching solution and is evaporated until the appearance of fumes of sulphuric anhydride. The solution was then 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 5−10 cmis placed in a beaker with a capacity of 300 cm, add 10 cmof a solution of tartrate of ammonium, diluted with water to 80 cm, neutralized with ammonia solution on litmus paper to obtain a slightly alkaline reaction. The solution was cooled, transferred to a separatory funnel, add 3 cmof a solution dimethylglyoxime injected 6 cmof chloroform (poured from a burette) and shaken for 2 min.

The solution is kept for delamination for 1−2 minutes, then the chloroform extract was separated in a dry vial with a glass stopper. Re-extraction was carried out for 1 min, adding 5 cmof chloroform. Extracts combine, filtered through a dry paper filter and measure the optical density at a wavelength of 360 nm in the thickness of the absorbing layer is 20 mm.

Solution comparison is the chloroform extract control experience.

The mass of Nickel in the sample is calculated according to the calibration graph

the IR.

4.2.2 For constructing the calibration curve of seven glasses with a capacity of 300 cmis placed 80 cmwater, 10 cmof a solution of tartrate of ammonia, 2−3 drops of ammonia solution. In six of the seven glasses are placed 0,5; 1,0; 2,0; 3,0; 4,0; 5,0 cmstandard solution B, which corresponds to 0,000005; 0,00001; 0,00002; 0,00003; 0,00004; 0,00005 g of Nickel.

The solution of the seventh glass is a solution in the reference experiment. Solution from glasses alternately transferred to a separatory funnel and then do as specified in 4.2.1.

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

4.3 the Processing of the measurement results

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

, (1)

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

 — weight of sample in aliquote part of the solution,

4.4 Permissible error of measurement

4.4.1 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

4.4.2 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 A.

5 Atomic absorption method

5.1 measuring instruments and auxiliary devices

Spectrophotometer atomic absorption equipped with graphite atomizer with the radiation source, the spectral lines of Nickel.

Argon according to GOST 10157.

Hydrochloric acid according to GOST 14261, diluted 1:1.

Nitric acid according to GOST 11125, of 1.40 g/cmand diluted 1:1.

Titanium sponge grade TG-100 GOST 17746.

The brand N22 Nickel GOST 849.

Standard samples according to GOST 8.315.

Standard solutions of Nickel.

Solution a: 0.1 g of Nickel dissolved in 15 cmof a hydrochloric acid solution and 5 cmof nitric acid (1:1) when heated, is evaporated to dryness. Then add 10 cmof hydrochloric acid and again evaporated to dryness. Evaporation again when you add a solution of hydrochloric acid. Then add 100 cmof the hydrochloric acid solution, 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 Nickel.

Solution B: 5 cmsolution And placed in a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix.

1 cmof solution B contains 0,000005 g no

Kehl.

5.2 procedures for measuring

5.2.1 Sample the sample weighing 1.0 g was placed in a conical flask with a capacity of 100 cm, 70 cm pour thehydrochloric acid solution (1:1), beaker cover watch glass or funnel glass and lead dissolving when heated on the stove, maintaining the solution volume in the flask of about 40 cmby the addition of the same solution of hydrochloric acid.

After complete dissolution of the sample is added dropwise nitric acid until the disappearance of the violet color of the solution and boil for 1−2 min. the Solution was cooled to room temperature, transferred to a volumetric flask with a capacity of 100 cmand mixed.

To prepare the solution in the reference experiment in the conical flask with a capacity of 100 cmis placed 70 cmof a hydrochloric acid solution (1:1), heated to boiling, add 3−4 drops of nitric acid and boil for 1−2 min. the solution was Then cooled to room temperature, transferred to a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix. Measurement of atomic absorption of Nickel is carried out, as shown in table 2.


Table 2

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

Before measuring the atomic absorption of the sample solutions and the reference experiment is carried out construction of calibration curve or the graduation of the instrument, if it works in automatic mode.

5.2.2 Construction of calibration curve

5.2.2.1 When the mass fraction of Nickel from 0.001% to 0.003% in six conical flasks with a capacity of 100 cmplaced at 1.0 g titanium sponge with a mass fraction of Nickel less than 0.001% and conduct dissolution as specified in 5.2.1.

The solutions were transferred to volumetric flasks with a capacity of 100 cm, in five out of six volumetric flasks add 2,0; 3,0; 4,0; 5,0; 6,0 cmstandard solution B, which corresponds to the mass concentration of the added Nickel 0,10; 0,15; 0,20; 0,25; 0,30 µg/cm.

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

5.2.2.2 When the mass fraction of Nickel in excess of 0.003% to 0.01% in six conical flasks with a capacity of 100 cmplaced at 1.0 g titanium sponge with a mass fraction of Nickel less than 0.001% and conduct dissolution as specified in 5.2.1.

The solutions were transferred to volumetric flasks with a capacity of 100 cm, in five out of six volumetric flasks add 6,0; 10,0; 12,0; 16,0; 20,0 cmstandard solution B, which corresponds to the mass concentration of the added Nickel 0,30; 0,50; 0,60; 0,80; 1.0 g/cm.

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

5.2.2.3 Solutions in all flasks is poured to the mark with water and mix. Microdonation with a capacity of 0.02 cmis introduced into a graphite cuvette sequentially a solution of the reference experiment, the sample solution and the solutions containing the standard solutions of Nickel, in increasing order of Nickel concentration.

From the values of atomic absorption solutions containing additives of a standard solution of Nickel, 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 Nickel (µg/cm) build a calibration curve. The mass concentration of Nickel in solution in the reference experiment and the sample is calculated according to the calibration schedule.

5.2.2.4 In the case when the instrument is in automatic mode and held his graduation, the sample of titanium sponge with a mass of 1,0 g with a mass fraction of Nickel less than 0.001% is placed in eight conical flasks with a capacity of 100 cm, poured in 70 cmof a hydrochloric acid solution and then produce a dissolution as specified in 5.2.1.

The solutions were transferred to volumetric flasks with a capacity of 100 cm.

When the mass fraction of Nickel from 0.001% to 0.003% in three of the four volumetric flasks with solutions of titanium sponge add 2,0; 4,0; 6,0 cmstandard solution B, which corresponds to the mass concentration of the added Nickel 0,10; 0,20; 0,30 µg/cm.

When the mass fraction of Nickel in excess of 0.003% to 0.01% in three of the four volumetric flasks with solutions of titanium sponge add 6,0; 12,0; 20.0 cmstandard solution B, which corresponds to the mass concentration of the added Nickel 0,30; 0,60; 1.0 g/cm.

The solutions in all flasks is poured to the mark with water and mix.

The solution in the reference experiment prepared as described in 5.2.1.

Microdonation with a capacity of 0.02 cmis introduced into a graphite cuvette and a solution of titanium sponge, and then in ascending order of the concentration of Nickel in solutions containing additives of a standard solution of Nickel, and carried out the calibration of an instrument. Measurement of atomic absorption of Nickel is carried out in the regime 5.2.1.

Then injected into the graphite cuvette, the solutions in the reference experiment and the sample and hold measurement of atomic absorption of Nickel in the regime 5.2.1.

After every 4−5 measurements of atomic absorption is carried out the purification of the graphite cuvette: microdonation introduce water into it and spend the atomization process in the mode in 5.2.

1.

5.3 Processing of results of measurements

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

. (2)

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

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

 — the volume of the sample solution, cm;

 — the weight of the portion

.

5.4 the Permissible error of measurement

5.4.1 Discrepancy between the measurement results and analysis results (at a confidence probability of 0.95) shall not exceed the permissible values given in table 3.


Table 3

Percentage

5.4.2 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 B.

6 qualifications

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