GOST 13047.2-2014

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  ГОСТ 13047.2-81

GOST 13047.2−2014 Nickel. Cobalt. Methods for determination of Nickel in Nickel

GOST 13047.2−2014

INTERSTATE STANDARD

NICKEL. COBALT

Methods for determination of Nickel in Nickel

Nickel. Cobalt. Methods for determination of nickel in nickel

ISS 77.120.40

Date of introduction 2016−01−01

Preface

Goals, basic principles and procedure of works on interstate standardization have been established in GOST 1.0−92 «interstate standardization system. Basic provisions» and GOST 1.2−2009 «interstate standardization system. Interstate standards, rules and recommendations on interstate standardization. Rules of development, adoption, application, renewal and cancellation"

Data on standard

1 DEVELOPED by Interstate technical committees for standardization MTK 501 Nickel and MTC 502 «Cobalt"

2 as AMENDED by the Federal Agency for technical regulation and Metrology (Rosstandart)

3 ACCEPTED by the Interstate Council for standardization, Metrology and certification (Protocol of October 20, 2014 N 71-N)

The adoption voted:

4 by Order of the Federal Agency for technical regulation and Metrology of June 24, 2015 N 816-St inter-state standard GOST 13047.2−2014 introduced as the national standard of the Russian Federation from 1 January 2016.

5 REPLACE GOST 13047.2−2002


Information about the changes to this standard is published in the annual reference index «National standards», and the text changes and amendments — in monthly information index «National standards». In case of revision (replacement) or cancellation of this standard a notification will be published in the monthly information index «National standards». Relevant information, notification and lyrics are also posted in the information system of General use — on the official website of the Federal Agency for technical regulation and Metrology on the Internet

1 Scope

This standard specifies electrogravimetry (with Nickel mass fraction to 98.8%) and calculated (at a mass fraction of Nickel over the 98.8%) methods for determination of Nickel in Nickel GOST 849.

2 Normative references

This standard uses the regulatory references to the following standards:

GOST 849−2008 Nickel primary. Specifications

GOST 3118−77 Reagents. Hydrochloric acid. Specifications

GOST 3760−79 Reagents. The aqueous ammonia. Specifications

GOST 3769−78 Reagents. The ammonium sulfate. Specifications

GOST 4204−77 Reagents. Sulphuric acid. Specifications

GOST 4328−77 Reagents. Sodium hydroxide. Specifications

GOST 4461−77 Reagents. Nitric acid. Specifications

GOST 5457−75 Acetylene, dissolved and gaseous. Specifications

GOST 5828−77 Reagents. Dimethylglyoxime. Specifications

GOST 5845−79 Reagents. Potassium-sodium vinocity 4-water. Specifications

GOST 6012−2011 Nickel. Methods of chemical-atomic-emission spectral analysis

GOST 6563−75 technical articles made of noble metals and alloys. Specifications

GOST 9722−97 Nickel Powder. Specifications

GOST 11125−84 nitric Acid of high purity. Specifications

GOST 13047.1−2014 Nickel. Cobalt. General requirements for methods of analysis

GOST 13047.4−2014 Nickel. Cobalt. Methods for determination of cobalt in Nickel

GOST 13047.6−2014 Nickel. Cobalt. Methods for determination of carbon

GOST 13047.7−2014 Nickel. Cobalt. Methods of determining sulphur

GOST 13047.8−2014 Nickel. Cobalt. Method for determination of silicon

GOST 13047.9−2014 Nickel. Cobalt. Method of determination of phosphorus

GOST 13047.10−2014 Nickel. Cobalt. Methods for determination of copper

GOST 13047.11−2014 Nickel. Cobalt. Method of determining zinc

GOST 13047.12−2014 Nickel. Cobalt. Methods for determination of antimony

GOST 13047.13−2014 Nickel. Cobalt. Methods for determination of lead

GOST 13047.14−2014 Nickel. Cobalt. Methods for determination of bismuth

GOST 13047.15−2014 Nickel. Cobalt. Method for determination of tin

GOST 13047.16−2014 Nickel. Cobalt. Methods for determination of cadmium

GOST 13047.17−2014 Nickel. Cobalt. Methods of iron determination

GOST 13047.18−2014 Nickel. Cobalt. Methods for determination of arsenic

GOST 13047.19−2014 Nickel. Cobalt. Method for the determination of aluminium

GOST 13047.20−2014 Nickel. Cobalt. Method for determination of magnesium

GOST 13047.21−2014 Nickel. Cobalt. Methods for determination of manganese

GOST 18300−87 ethyl rectified technical. Specifications

GOST 20478−75 Reagents. Ammonium neccersarily. Specifications

GOST 24147−80 aqueous Ammonia of high purity. Specifications

Note — When using this standard appropriate to test the effect of reference standards in the information system of General use — on the official website of the Federal Agency for technical regulation and Metrology on the Internet or in the annual information index «National standards» published as on January 1 of the current year, and the editions of the monthly information index «National standards» for the current year. If the reference standard is replaced (changed), when using this standard should be guided by replacing (amended) standard. If the reference standard is cancelled without replacement, then the situation in which the given link applies to the extent that does not affect this link.

3 General requirements and safety requirements

General requirements for methods of analysis used by the quality of distilled water and glass labware and safety at work — according to GOST 13047.1.

4 Electrogravimetry method

4.1 Method of analysis

The method is based on weighing of Nickel, cobalt, copper and zinc emitted by electrolysis on a platinum cathode from the ammonium medium and the determination of the mass of Nickel remaining in the solution after carrying out electrolysis, spectrophotometric or atomic absorption method. The mass fraction of cobalt, copper and zinc is determined according to GOST 13047.4, 13047.10 GOST, GOST 13047.11 or GOST 6012 are taken into account when processing the results of the analysis.

A spectrophotometric method based on measurement of light absorption at a wavelength of 440 nm of a solution of complex compounds of Nickel with dimethylglyoxime in an alkaline medium in the presence of an oxidant — ammonium naternicola.

Atomic absorption method based on measurement of absorption at a wavelength of 232,0 nm resonance radiation by atoms of Nickel, the resulting fiery atomization when spraying the sample solution in flame acetylene-air.

4.2 measuring instruments, auxiliary devices, materials, reagents and solutions

Installation for electrolysis with ammeter, voltmeter and rheostat, providing carrying out the electrolysis while stirring the solution at a current of from 3 to 4 A and a voltage of 2 to 3 V.

Atomic absorption spectrometer for measurements in the flame acetylene-air.

Lamp with hollow cathode for the excitation of spectral lines of Nickel.

Spectrophotometer or photoelectrocolorimeter, which provides measurements in the wavelength range of 420 to 460 nm.

The electrodes are platinum mesh according to GOST 6563.

Acetylene gas according to GOST 5457.

Nitric acid according to GOST 4461, if necessary, purified by distillation, or according to GOST 11125, diluted 1:1 and 1:9.

Sulfuric acid according to GOST 4204, diluted 1:1 and 1:4.

Hydrochloric acid according to GOST 3118, diluted 1:1.

Ammonia water according to GOST 3760, if necessary, cleaned, or according to GOST 24147, diluted 1:9.

Ammonium sulfate according to GOST 3769.

Ammonium neccersarily according to GOST 20478, solution mass concentration of 0.03 g/cm.

Sodium hydroxide according to GOST 4328, solution mass concentration of 0.05 g/cm.

Potassium-sodium vinocity 4-water according to GOST 5845, solution mass concentration of 0.2 g/cm.

Dimethylglyoxime according to GOST 5828, solution mass concentration of 0.01 g/cmin sodium hydroxide solution.

The technical rectified ethyl alcohol according to GOST 18300.

Universal indicator paper [1]*.

Filters obestochennye [2]* other filters or medium density.
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* See Bibliography. — Note the manufacturer’s database.


The primary Nickel GOST 849 with a mass fraction of Nickel is not more of 99.93%.

Nickel powder according to GOST 9722.

The Nickel solutions of known concentration.

The solution And the mass of Nickel concentration 0.001 g/cmis prepared as follows: a portion of primary Nickel or Nickel powder in a weight 1,0000 g placed in a beaker with a capacity of 250 cm, flow 20 to 25 cmof nitric acid, diluted 1:1, dissolved by heating, boil for 2−3 min. When using Nickel powder in the solution is filtered over pre-rinsed two or three times with nitric acid, diluted 1:9, a filter (red or white ribbon). The filter is washed five or six times with hot water and discarded. The solution is poured 20 cmof sulphuric acid diluted 1:1, evaporated to release vapors of sulfuric acid and cooled. Poured from 80 to 100 cmof distilled water, dissolve salt when heated and cooled. The solution is transferred into a measuring flask with volume capacity of 1000 cmand adjusted to the mark with distilled water.

Solution B mass concentration of Nickel 0.0001 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cmtransfer 10 cmof solution A, pour 5 cmof sulphuric acid, diluted 1:4, adjusted to the mark with distilled water.

Solution of the mass concentration of Nickel 0,00001 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cmtransfer 10 cmof the solution B, adjusted to the mark with distilled water.

4.3 Preparation for analysis

4.3.1 To construct the calibration curve in the mass determination of Nickel by spectrophotometric in volumetric flasks with a capacity of 100 cmtransfer 1, 2, 4, 6, 8 and 10 cmof solution, pour 10 cmVinokurova potassium-sodium and then carry out the analysis in accordance with 4.4.4.

The mass of Nickel in the calibration solutions is 0,00001; 0,00002; 0,00004; of 0.00006; and 0,00010 0,00008 g.

The light absorption values of the calibration solutions and corresponding masses of Nickel to build a calibration curve taking into account the light absorption values of the calibration solution, is prepared without introducing a solution containing Nickel.

4.3.2 For the construction of calibration curve in the determination of the mass of a Nickel atomic absorption method in a volumetric flask with a capacity of 250 cmcarry 1, 2, 4, 6, 8 and 10 cmof a solution, pour 10 cmof sulphuric acid, diluted 1:4, adjusted to the mark with distilled water and measure the absorbance in accordance with 4.4.5.

The mass of Nickel in the calibration solutions is 0,0001; 0,0002; 0,0004; about 0.0006; and 0,0008 0,0010 g.

4.4 analysis

4.4.1 Sample the sample weight of 1,000 g was placed in a beaker or flask with a capacity of 250 cm, flow 15 to 20 cmof nitric acid, diluted 1:1, dissolved by heating, boil for 2−3 min, cooled, poured 15 cmsulphuric acid diluted 1:1, the solution is evaporated to release vapors of sulfuric acid and cooled.

Pour 50 to 60 cmof distilled water, add 3 to 4 g of ammonium sulfate, dissolved salts when heated and cooled. Poured, with stirring, ammonia until the smell and another 80 cm.

Solution and the precipitate is kept in a warm place for 25−30 min., filtered through a filter (red or white ribbon), collecting the filtrate in a beaker with a capacity of 250 cm, the filter and the precipitate washed two or three times with ammonia diluted 1:9, the filtrate is used in accordance with 4.4.2.

The filter cake is dissolved in a volume of 10 to 15 cmhot hydrochloric acid, diluted 1:1, the filter is washed three or four times with hot water, collecting the filtrate in a beaker, in which was conducted the deposition. The solution is poured 10 cmof sulphuric acid diluted 1:1, evaporated to release vapors of sulfuric acid, cooled, poured 20 to 30 cmof distilled water and dissolved salts when heated. The solution was transferred to a volumetric flask with a capacity of 250 cmand used in accordance with 4.4.3.

4.4.2 the filtrate was poured into distilled water to a volume of 200 cmand the electrolysis is carried out for 1.0 to 1.5 h while stirring the solution using a pre-weighed platinum electrodes at a current of from 3 to 4 A and a voltage of 2 to 3 V. After the bleaching solution the side of the Cup and protruding parts of the electrodes are washed with distilled water, poured from 15 to 20 cmof distilled water and the electrolysis is carried out for 10−15 min.

The electrodes taken out from the solution, washed with distilled water, turn off the current. The electrodes are washed with ethanol, dried at a temperature of from 95 °C to 105 °C for 15−20 minutes, cool and weigh.

4.4.3 After the electrolysis, the solution is evaporated to a volume of 40 to 50 cmand poured sulphuric acid, diluted 1:1, to pH 1−2 by universal indicator paper. The solution attached to the solution in a volumetric flask with a capacity of 250 cm, adjusted to the mark with distilled water and determine the mass of Nickel by spectrophotometry in accordance with 4.4.4 or atomic absorption method in accordance with 4.4.5.

4.4.4 When using the spectrophotometric method in a volumetric flask with a capacity of 100 cmstand aliquot part of the solution for 4.4.3, poured 10 cmVinokurova potassium-sodium, 10 cmof sodium hydroxide solution, 5 cmsolution naternicola ammonium, 10 cmsolution dimethylglyoxime in sodium hydroxide solution, adjusted to the mark with distilled water.

After 5−7 min. measure the light absorption of the solution on the spectrophotometer at a wavelength of 440 nm or photoelectrocolorimeter at a wavelength range of 420 to 460 nm. A solution of comparison, using the calibration solution, in which before surging solutions for the formation of complex compounds is added two or three drops of sulphuric acid, diluted 1:1, and you have not entered a solution containing Nickel.

The value of the light absorption of the sample solution find the mass of Nickel for calibration graphics, built in 4.3.1, taking into account the dilution factor of the solution.

4.4.5 When using the atomic absorption method, the absorption of sample solution in 4.4.3 and calibration solutions for 4.3.2 at a wavelength of 232,0 nm, slit width 0.2 nm measured at least two times, sequentially spraying them in the flame acetylene-air, wash the system with distilled water, check the zero point and the stability of the calibration curve.

According to the obtained values of absorbance of the calibration solutions and corresponding masses of Nickel to build a calibration curve.

The value of absorbance of sample solution find the mass of Nickel in the calibration schedule.

In one analysis performed two or three parallel definitions.

4.5 Processing the analysis results

Mass fraction of Nickel X % is calculated by the formula:

, (1)

where Mis the mass of the cathode after electrolysis, g;

M — mass of the cathode before electrolysis, g;

M — mass of the anode before the electrolysis, g;

M — mass of anode after electrolysis, g;

Mis the mass of Nickel in sample solution, g;

M — weight of sample, g;

X — mass fraction of cobalt in the sample, %;

X — mass fraction of copper in the sample, %;

X — mass fraction of zinc in sample, %.

4.6 accuracy Control analysis

Control of accuracy of analysis results is carried out according to GOST 13047.1.

The expanded uncertainty of the results of the analysis of U is 0.3%.

Regulations control precision — the repeatability limits r the results of two or three parallel definitions are, respectively, 0.2% and 0.3%; the limit of reproducibility R for the two analysis results is 0.4% at a confidence probability P=0,95.

5 Calculation method

Mass fraction of Nickel (if Nickel mass fraction of more than 98.8 per cent) define the calculation method. To do this, find the sum of the mass fraction of impurities, normalized to GOST 849, GOST certain 13047.4, 13047.6 GOST — GOST 13047.21 or GOST 6012, taken, without rounding, and subtracted from 100%.

The result is rounded up to the number of significant digits specified in the tables of chemical composition according to GOST 849.

Bibliography

[1] THE 6−09−1181−89* universal indicator Paper to determine the pH of 7−14 and 1−10
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* The one referred to here and hereinafter, not shown. For additional information, please refer to the link. — Note the manufacturer’s database.


[2] THE 6−09−1678−95* Filters obestochennye (white, red, blue tape)
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* Valid on the territory of the Russian Federation.