GOST 13047.5-2014

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  ГОСТ 13047.5-2014

GOST 13047.5−2014 Nickel. Cobalt. Methods for determination of Nickel in cobalt

GOST 13047.5−2014

INTERSTATE STANDARD

NICKEL. COBALT

Methods for determination of Nickel in cobalt

Nickel. Cobalt. Methods for determination of nickel in cobalt

ISS 77.120.40

Date of introduction 2016−01−01

Preface

Goals, basic principles and main 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 13047.5−2014 introduced as the national standard of the Russian Federation from 1 January 2016.

5 REPLACE GOST 13047.5−2002


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 the spectrophotometric and atomic absorption methods for the determination of Nickel (at a mass fraction of Nickel from 0,0010% to 0.60%) in cobalt GOST 123 and cobalt powder to GOST 9721. As an arbitration method is atomic absorption method.

2 Normative references

This standard uses the regulatory references to the following standards:

GOST 83−79 Reagents. Sodium carbonate. Specifications

GOST 123−2008 Cobalt. Specifications

GOST 849−2008 Nickel primary. Specifications

GOST 3118−77 Reagents. Hydrochloric acid. Specifications

GOST 3760−79 Reagents. The aqueous ammonia. Specifications

GOST 3773−72 Reagents. The ammonium chloride. 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 9721−79 cobalt Powder. Specifications

GOST 9722−97 Nickel Powder. Specifications

GOST 10929−76 Reagents. Hydrogen peroxide. Specifications

GOST 11125−84 nitric Acid of high purity. Specifications

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

GOST 14261−77 hydrochloric Acid of high purity. Specifications

GOST 18300−87 ethyl rectified technical. Specifications

GOST 20015−88 Chloroform. Specifications

GOST 20478−75 Reagents. Ammonium neccersarily. Specifications

GOST 22280−76 Reagents. Sodium citrate 5,5-water. 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 laboratory glassware and safety at work — according to GOST 13047.1.

4 a spectrophotometric method

4.1 Method of analysis

The method is based on measuring light absorption at a wavelength of 440 nm of a solution of complex compounds of Nickel with dimethylglyoxime after its preliminary extraction with chloroform.

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

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

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

Hydrochloric acid according to GOST 3118, if necessary, purified by distillation, or according to GOST 14261, diluted 1:24.

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

Hydrogen peroxide according to GOST 10929.

Ammonia water according to GOST 3760, if necessary, purified by distillation, or according to GOST 24147, diluted 1:1 and 1:19.

Ammonium chloride according to GOST 3773.

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

Sodium hydroxide according to GOST 4328, solution mass concentration of 0.04 g/cm.

Sodium citrate according to GOST treasuremania 22280, solution mass concentration of 0.03 g/cm.

Sodium carbonate according to GOST 83, 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 ethanol and the solution of the mass concentration of 0.01 g/cmin the sodium hydroxide solution the mass concentration of 0.04 g/cm.

The technical rectified ethyl alcohol according to GOST 18300.

Chloroform according to GOST 20015 or Pharmacopoeia [1].

Universal indicator paper at [2]*.
________________
* See Bibliography. — Note the manufacturer’s database.


Filters obestochennye in [3] or other filter medium density.

The primary Nickel GOST 849.

Nickel powder according to GOST 9722.

The Nickel solutions of known concentration.

The solution And the mass concentration of Nickel 0.0005 g/cmis prepared as follows: a portion of primary Nickel or Nickel powder in a weight 0,5000 g placed in a beaker with a capacity of 250 cm, flow 15 to 20 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 two or three times with hot distilled water. The solution is poured 20 cmof sulphuric acid diluted 1:1, evaporated to release vapors of sulfuric acid and cooled. Flow from 60 to 70 cmof distilled water, dissolve salt when heated and cooled. The solution is transferred into a measuring flask with volume capacity of 1000 cm, 50 cm pouredsulphuric acid, diluted 1:4, and adjusted to the mark with distilled water.

Solution B is the mass of Nickel concentration of 0.00005 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, and 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 cm andstand 20 cmof solution B and adjusted to the mark with distilled water.

4.3 Preparation for analysis

To build a calibration curve in a volumetric flask with a capacity of 100 cmstand 0,5; 1,0; 2,0; 4,0; 6,0; 8,0 and 10.0 cmsolution, pour distilled water to a volume of 25−30 cm, 10 cmsolution Vinokurova potassium-sodium, 10 cmof sodium hydroxide solution, 10 cmof a solution of ammonium naternicola 10 cmdimethylglyoxime solution in sodium hydroxide, adjusted to the mark with distilled water and take measurements of the absorption solution in accordance with 4.4.6.

The mass of Nickel in the calibration solutions is 0,000005; 0,000010; 0,000020; 0,000040; 0,000060; 0,000080 and 0,000100 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.

4.4 analysis

4.4.1 Sample the sample weight 0,500 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, the solution is evaporated to a volume of 5 to 6 cm.

4.4.2 When the mass fraction of Nickel is not more than 0,020% of the solution 4.4.1 poured from 100 to 120 cmof distilled water, 5 cmof a solution of sodium citrate, 5 to 6 g of ammonium chloride, 20 cmof ammonia, 4 cmof hydrogen peroxide and boil for 8−10 min. the Solution was cooled, neutralized with hydrochloric acid diluted 1:1, to pH 8−9 by universal indicator paper and transferred to a separatory funnel with a capacity of 500 cm. Pour distilled water to a volume of 200 cm, 120 cmdimethylglyoxime solution in ethyl alcohol, 20 cmof chloroform, extracted for 1 min and then carry out the analysis in accordance with 4.4.5.

4.4.3 When the mass fraction of Nickel from 0.02% to 0.20% of the solution 4.4.1 go from 60 to 70 cmof distilled water, heated to boiling, cool, transfer the solution into volumetric flask with a capacity of 250 cm, adjusted to the mark with distilled water. Aliquot part of the solution of volume 25 cmwas transferred to a beaker with a capacity of 250 cm, poured with distilled water to a volume of 70 to 80 cm, 5 cmsolution of sodium citrate, 2 to 3 g of ammonium chloride, 15 cmof ammonia solution, 2 cmof hydrogen peroxide and boil for 8−10 min. the Solution was cooled, neutralized with hydrochloric acid diluted 1:1, to pH 8−9 by universal indicator paper and transferred to a separatory funnel with a capacity of 250 cm. Pour 50 cmof the solution dimethylglyoxime in ethyl alcohol, 20 cmof chloroform, extracted for 1 min and then carry out the analysis in accordance with 4.4.5.

4.4.4 If the mass fraction of Nickel in excess of 0.20% of the solution 4.4.1 go from 60 to 70 cmof distilled water, heated to boiling, cool, transfer the solution into volumetric flask with a capacity of 500 cm, adjusted to the mark with distilled water. Aliquot part of the solution volume of 5 cmwas transferred to a beaker with a capacity of 100 cm, poured with distilled water to a volume of 20 cm, 5 cmsolution of sodium citrate, neutralized with ammonia to pH 8−9 by universal indicator paper, transferred to a separatory funnel with a capacity of 100 cm, flow 15 cmdimethylglyoxime solution in ethyl alcohol, 20 cmof chloroform and extracted with 1 min.

4.4.5 the Lower organic layer decanted into a separating funnel with a capacity of 100 cm, water phase poured 20 cmof chloroform and repeat the extraction. The organic phase is poured into the same separatory funnel, and the aqueous phase discarded.

The organic phase is washed until discoloration of the solution, priliva 15, 10 and 5 cmof ammonia, diluted 1:19, separatory funnel and shaking 10−15 times.

To the washed organic phase poured 15 cmof hydrochloric acid, diluted 1:24, separatory funnel and shake for 1 min. the Organic phase was drained into another separatory funnel, and the aqueous phase in a beaker with a capacity of 100 cm. The Stripping is repeated using 15 cmof hydrochloric acid, diluted 1:24, the aqueous phase is poured into the same beaker, the organic phase is discarded.

To the aqueous phase poured 5 cmof sulphuric acid diluted 1:1 add two to three drops of 0.5 cmof nitric acid for the destruction of residues of organic compounds, and then again evaporated to release vapors of sulfuric acid. To the cooled residue is poured from 10 to 15 cmof distilled water, heated to dissolve the salts, again cooled.

4.4.6 Solution is transferred to a volumetric flask with a capacity of 100 cm, flow 10 cmsolution Vinokurova potassium-sodium, 10 cmof sodium hydroxide solution, 10 cmof a solution of ammonium naternicola 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. As a solution comparison, using a solution prepared in accordance with 4.3 without introducing a solution containing Nickel.

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

4.5 Processing the analysis results

Fraction of total mass of Nickel in sample X, %, calculated by the formula:

, (1)

where Mis the mass of Nickel in sample solution, g;

Mis the mass of Nickel in solution in the reference experiment, g;

K — dilution factor of sample solution;

M — weight of sample, g.

4.6 accuracy Control analysis

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

The regulations control the precision (limits of repeatability and reproducibility) and the rate control accuracy (expanded uncertainty) of the results of the analysis are shown in table 1.


Table 1 — Requirements of control precision (limits of repeatability and reproducibility) and the rate control accuracy (expanded uncertainty) of the results of the analysis at a confidence probability P=0,95

Percentage

5 Atomic absorption method

5.1 Method of analysis

The method is based on measuring absorption at a wavelength of 232,0 or the amount of 231.1 nm resonance radiation by atoms of Nickel, the resulting fiery atomization when spraying the sample solution in flame acetylene-air.

5.2 measurement Means, auxiliary devices, materials, reagents and solutions

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

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

Acetylene gas according to GOST 5457.

Filters obestochennye in [3] or other filter medium density.

Nitric acid according to GOST 4461, if necessary, purified by distillation, or according to GOST 11125, diluted 1:1 and 1:19.

Cobalt GOST 123 or standard sample of cobalt, for example, [4] pre-installed (certified) mass fraction of Nickel not more than 0,001%.

Nickel powder according to GOST 9722 or primary Nickel GOST 849.

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 were placed in a glass or flask with a capacity of 250 cm, 20−25 cm pournitric acid, diluted 1:1, dissolved by heating, boil for 3−5 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 two or three times with hot distilled water. The solution was cooled, transferred to a measuring flask with volume capacity of 1000 cm, 50 cm pournitric acid, diluted 1:1, and 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 10 cmof nitric acid, diluted 1:1, and adjusted to the mark with distilled water.

5.3 Preparation for assay

5.3.1 To construct a calibration chart 1 in determining the mass fraction of Nickel is not more than 0,010% of the sample of cobalt or of a standard sample of composition of cobalt with a mass of 5,000 grams are placed in tumblers or flasks with a capacity of 250 cm. The number of batches must match the number of points of calibration curve, including Supervisory experience.

Sample of cobalt or of a standard sample of the composition of cobalt is dissolved by heating in a volume of 50 to 60 cmof nitric acid, diluted 1:1, evaporated to a volume of 15−20 cm, flow 50 to 60 cmof distilled water, heated to boiling, cooled, transferred to volumetric flasks with a capacity of 100 cm, transferred to them 0,5; 1,0; 2,0; 3,0; 4,0 and 5,0 cmof solution B. the flask with the solution in the reference experiment, the solution containing the Nickel, not poured, adjusted to the mark with distilled water and measure the absorbance in accordance with 5.4.

The mass of Nickel in the calibration solutions is 0,00005; 0,00010; 0,00020; 0,00030; and 0,00040 0,00050 G.

5.3.2 For the construction of calibration curve 2 in determining the mass fraction of Nickel from 0.010 to 0.050% cobalt in sample or standard sample composition of cobalt with a mass of 1,000 grams are placed in tumblers or flasks with a capacity of 250 cm. The number of batches must match the number of points of calibration curve, including Supervisory experience.

Sample of cobalt or of a standard sample of the composition of cobalt is dissolved by heating in the amount of 15 to 20 cmof nitric acid, diluted 1:1, evaporated to a volume of 5 to 7 cm, flow 50 to 60 cmof distilled water, heated to boiling, cooled, transferred to volumetric flasks with a capacity of 100 cm, transferred to them 0,5; 1,0; 2,0; 3,0; 4,0 and 5,0 cmof solution B. the flask with the solution in the reference experiment, the solution containing the Nickel, not poured, adjusted to the mark with distilled water and measure the absorbance in accordance with 5.4.

The mass of Nickel in the calibration solutions specified in 5.3.1.

5.3.3 For construction of calibration curve 3 when determining the mass fraction of Nickel of more than 0,050% in volumetric flasks with a capacity of 100 cmshift 10 cmof the solution in the reference experiment, prepared in accordance with 5.3.2, and pour 0,5; 1,0; 2,0; 3,0; 4,0 and 6,0 cmof solution B. In one of the flasks with a solution of the reference experiment a solution containing Nickel, not poured, adjusted to the mark with nitric acid, diluted 1:19, and measure absorption in accordance with 5.4.

The mass of Nickel in the calibration solutions is 0,00005; 0,00010; 0,00020; 0,00030; 0,00040 and 0,00060 G.

5.4 analysis

A portion of the sample weight in accordance with table 2 were placed in a glass or flask with a capacity of 250 cm.

Table 2 Conditions of preparation of sample solution

A portion of the sample with a mass of 5,000 g was dissolved with heating in a volume of 50 to 60 cmof nitric acid, diluted 1:1, and a mass of 1,000 g in the amount of 15 to 20 cmof nitric acid, diluted 1:1, evaporated to a volume of 15 to 20 cmor from 5 to 7 cm, flow from 40 to 50 cmof distilled water, heated to boiling and cooled. The solution was transferred to a volumetric flask with a capacity of 100 cmand adjusted to the mark with distilled water.

When the mass fraction of Nickel of more than 0,050% in a volumetric flask with a capacity of 100 cmstand aliquot part of the solution by volume in accordance with table 2 and adjusted to the mark with nitric acid, diluted 1:19.

The absorbance of the sample solution and the calibration solutions at a wavelength of 232,0 nm and slit width 0.2 nm measured at least two times, sequentially spraying them in the flame acetylene-air, spray rinsed the system with distilled water, check the zero point and the stability of the calibration curve. To check the zero point solution is used, the appropriate control experience, prepared in accordance with 5.3.

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

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

5.5 Processing of analysis results

Fraction of total mass of Nickel in sample X, %, is calculated by the formula

, (2)

where Mis the mass of Nickel in sample solution, g;

K — dilution factor of sample solution;

M — weight of sample, g.

5.6 Control of accuracy of analysis

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

The regulations control the precision (limits of repeatability and reproducibility) and the rate control accuracy (expanded uncertainty) of the results of the analysis are shown in table 1.