GOST 13047.17-2014

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  ГОСТ 13047.17-81

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

GOST 13047.17−2014

INTERSTATE STANDARD

NICKEL. COBALT

Methods of iron determination

Nickel. Cobalt. Methods for determination of iron

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 13047.17−2014 introduced as the national standard of the Russian Federation from 1 January 2016.

5 REPLACE GOST 13047.17−2002


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 iron (at mass fraction of iron from 0.001% to 1.0%) in the primary Nickel GOST 849, Nickel powder according to GOST 9722, 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 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 4204−77 Reagents. Sulphuric acid. Specifications

GOST 4461−77 Reagents. Nitric acid. Specifications

GOST 4478−78 Reagents. Sulfosalicylic acid 2-water. Specifications

GOST 5457−75 Acetylene, dissolved and gaseous. Specifications

GOST 9721−79 cobalt Powder. 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 14261−77 hydrochloric Acid of high purity. 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 415 nm of a solution of complex compounds of iron with sulfosalicylic acid in an ammonia environment, after a preliminary extraction separation of iron by isoamyl acetate from hydrochloric acid medium.

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

Spectrophotometer or photoelectrocolorimeter, providing measurements in the range of wavelengths from 400 to 430 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 3:1, 1:1 and 1:10.

Sulfuric acid according to GOST 4204, diluted 1:1 and 1:9.

Sulfosalicylic acid according to GOST 4478, solution mass concentration of 0.1 g/cm.

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

Carbonyl iron [2]* or other iron containing not less than 99.9% of the main substance.
________________
* See Bibliography. — Note the manufacturer’s database.


The iron solution of known concentration.

Solution And mass of iron concentration 0.001 g/cmis prepared as follows: a sample of iron weighing 1,0000 g were placed in a glass or flask with a capacity of 250 cm, flow 20 to 30 cmof hydrochloric acid diluted 1:1, dissolved by heating, poured 2 to 3 cmof nitric acid, diluted 1:1, and evaporated up to wet salts.

The walls of the beaker or flask is washed with distilled water, poured 30 cmof sulphuric acid diluted 1:1, evaporated to release vapors of sulfuric acid, cooled, poured 100 cm()of distilled water, dissolve salt when it is heated, cooled, transferred into a measuring flask with volume capacity of 1000 cmand adjusted to the mark with distilled water.

Solution B mass of iron concentration 0.0001 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cmtransfer 10 cmof solution A, pour 10 cmof sulphuric acid, diluted 1:9 and adjusted to the mark with distilled water.

Solution mass of iron concentration 0,00001 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cmtransfer 10 cmof a solution, pour 10 cmof sulphuric acid, diluted 1:9 and adjusted to the mark with distilled water.

4.3 Preparation for analysis

4.3.1 Before analysis used laboratory glassware is washed with hot hydrochloric acid, diluted 1:1, then with distilled water.

In the analysis of Nickel marks N-0, N-1U, N-1 and cobalt grade K-0 to remove accidental contamination of samples with iron it is recommended to handle it. A sample weight of 7 to 10 g placed in a beaker with a capacity of 400 or 600 cm, flow from 30 to 50 cmof hydrochloric acid, diluted 1:10.

The solution with the sample is stirred for 2−3 min, poured the solution by decantation and the sample was washed two or three times with distilled water for 50 cm, pouring the solution by decantation. The sample was dried with filter paper and kept in a desiccator for 10 min at a temperature of from 100 °C to 110 °C.

4.3.2 To build a calibration curve in a volumetric flask with a capacity of 100 cmtransfer 1,0; 2,0; 4,0; 6,0; 8,0 and 10,0 cmsolution, pour distilled water to a volume of 15 cm, 10 cmsulfosalicylic acid solution and then carry out the analysis in accordance with 4.4.2.

The mass of iron 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 iron to build the calibration graph, given the values of absorption of the calibration solution, is prepared without introducing a solution containing iron.

4.4 analysis

4.4.1 Sample the sample weight in accordance with table 1 were placed in a glass or flask with a capacity of 250 cm.


Table 1 Conditions of preparation of sample solution

In a glass or flask poured from 15 to 20 cmof nitric acid, diluted 1:1, is dissolved when heated, is evaporated to wet salts, the walls of the beaker or flask is washed with distilled water, repeat the steaming, pour 15 cmof hydrochloric acid, diluted 3:1, heated to dissolve the salts, and cooled.

When the mass fraction of iron in excess of 0.010% solution transferred to a volumetric flask with a capacity of 250 cmand was adjusted to the mark with hydrochloric acid, diluted 3:1.

Solution or its aliquot part of volume in accordance with table 1 is transferred to a separatory funnel with a capacity of 100 cm, flow up to 40 cmof hydrochloric acid, diluted 3:1, 20 cmof isoamyl acetate, shake for 1 min. the Aqueous phase is discarded and the organic phase poured 15 cmof hydrochloric acid, diluted 3:1, and shake the funnel 30, the aqueous phase is discarded and organic phase is again washed with 15 cmof hydrochloric acid, diluted 3:1.

To the organic phase poured 20 cmof distilled water and shake the funnel 30, the aqueous phase is poured into a glass with a capacity of 100 cm, and the organic phase poured 20 cmof distilled water and repeat the extraction. The aqueous phase is poured into the same beaker, and the organic phase discarded.

The combined aqueous solution is evaporated to a volume of 5 to 7 cm, pour 5 cmof sulphuric acid diluted 1:1, evaporated to release vapors of sulfuric acid, cooled, poured 10 to 15 cmof distilled water and transferred to a volumetric flask with a capacity of 100 cm.

4.4.2 volumetric flask pour 10 cmsulfosalicylic acid solution, the ammonia until yellow color of the solution and 5 cmand bring to the mark with distilled water. Light absorption of the sample solution and control solution experience is measured after 15 minutes on the spectrophotometer at a wavelength of 415 nm or photoelectrocolorimeter within the range of wavelengths from 400 to 430 nm, using as a comparison solution of distilled water.

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

4.5 Processing the analysis results

Mass fraction of iron in the sample X, %, is calculated by the formula

, (1)

where is the mass of iron in the sample solution, g;

 — the mass of iron in solution in the reference experiment, g;

M — weight of sample, g;

K — dilution factor of sample solution.

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 2.


Table 2 — 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 248.3 nm resonance radiation by atoms of iron, resulting from the 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 iron.

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, 1:9 and 1:19.

Hydrochloric acid according to GOST 3118, if necessary, purified by distillation, or according to GOST 14261, diluted 1:1 and 1:2.

Nickel powder according to GOST 9722 or standard sample of Nickel, for example [4], with the prescribed mass fraction of iron not more than 0.002%.

Cobalt GOST 123 or standard sample of cobalt, for example, [5], pre-installed (certified) mass fraction of iron not more than 0.002%.

Carbonyl iron [2] or other iron containing not less than 99.9% of the main substance.

The iron solution of known concentration.

Solution And mass of iron concentration 0.001 g/cmis prepared as follows: a sample of iron weighing 1,000 grams is placed in a beaker with a capacity of 250 cm, flow 25 to 30 cmof nitric acid, diluted 1:1, dissolved by heating, pour 1 to 2 cmof hydrochloric acid diluted 1:1, and the solution is evaporated to a volume of 5 to 7 cm, the side of the Cup washed with distilled water, again evaporated, pour 50 to 60 cmof distilled water, cooled, transfer the solution into a measuring flask with volume capacity of 1000 cm, flow 20 cmof nitric acid, diluted 1:1, and adjusted to the mark with distilled water.

Solution B mass of iron concentration 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, adjusted to the mark with distilled water.

5.3 Preparation for assay

5.3.1 Before analysis used laboratory glassware is washed with hot hydrochloric acid, diluted 1:1, then with distilled water.

To remove accidental contamination of samples with iron it is recommended to handle it in accordance with 4.3.1.

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

Sample of Nickel powder or cobalt or of a standard sample of composition of Nickel or cobalt is dissolved by heating in a volume of 50 to 60 cmof nitric acid, diluted 1:1. When using the Nickel powder in the slurries was filtered through a filter (red or white ribbon), washed two or three times with nitric acid, diluted 1:9, the filters are washed two or three times with hot distilled water. The solutions were evaporated to a volume of 10 to 15 cm, flow from 40 to 50 cmof distilled water, heated to boiling, cooled, transferred to volumetric flasks with a capacity of 100 cm.

In the flask is transferred 0,5; 1,0; 2,0; 3,0; 4,0; 5,0 and 6.0 cmof solution B. the flask with the solution in the reference experiment, the solution containing the iron pour, adjusted to the mark with distilled water and measure the absorbance in accordance with 5.4.

The mass of iron in the calibration solutions is 0,00005; 0,00010; 0,00020; 0,00030; 0,00040; 0,00050 and 0,00060 G.

5.3.3 For construction of calibration curve 2 in determining the mass fraction of iron in excess of 0.010% sample of Nickel powder or cobalt or of a standard sample of composition of Nickel or cobalt with a mass of 1,000 g was placed in a beaker or flask with a capacity of 250 cm. The number of batches must match the number of points of calibration curve, including Supervisory experience.

Sample of Nickel powder or cobalt or of a standard sample of composition of Nickel or cobalt is dissolved by heating in the amount of 15 to 20 cmof nitric acid, diluted 1:1, and then carry out the analysis in accordance with 5.3.2.

In volumetric flasks transfer 0,5; 1,0; 2,0; 3,0; 4,0; 5,0 and 6.0 cmof solution B. the flask with the solution in the reference experiment, the solution containing the iron pour, adjusted to the mark with distilled water and measure the absorbance in accordance with 5.4.

The mass of iron in the calibration solutions specified in 5.3.2.

5.3.4 For the construction of calibration curve 3 when determining the mass fraction of iron more than 0,050% in volumetric flasks with a capacity of 100 cmstand for 20 cmof the solution in the reference experiment, prepared in accordance with 5.3.3, poured 0,5; 1,0; 2,0; 3,0; 4,0; 5,0 and 6.0 cmof solution B. In one of the flasks with a solution of the reference experiment, the solution containing the iron pour, adjusted to the mark with nitric acid, diluted 1:19, and measure absorption in accordance with 5.4.

The mass of iron in the calibration solutions specified in 5.3.2.

5.3.5 For the construction of calibration curve 4 in determining the mass fraction of iron in excess of 0.25% of the volumetric flasks with a capacity of 100 cmtransfer 1,0; 2,0; 3,0; 4,0 and 5,0 cmof solution B. In one of the flasks with a solution of the reference experiment, the solution containing the iron pour, adjusted to the mark with nitric acid, diluted 1:19, and measure absorption in accordance with 5.4.

The mass of iron in the calibration solutions is 0,0001; 0,0002; 0,0003; 0,0004; 0,0005 g.

5.4 analysis

A portion of the sample weight in accordance with table 3 was placed in a beaker or flask with a capacity of 250 cm.


Table 3 — 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 is from 15 to 20 cmof nitric acid, diluted 1:1, evaporated to a volume of 15 to 20 cmor from 5 to 7 cm, respectively, transferred to a volumetric flask with a capacity of 100 cm, cooled and adjusted to the mark with distilled water.

When the mass fraction of iron more than 0,050% in accordance with table 3, dilute the sample solution with nitric acid, diluted 1:19 in a volumetric flask with a capacity of 100 cm.

The absorbance of the sample solution and respective solutions to construct the calibration curve at a wavelength of 248.3 or 248,8 nm, slit width 0.15 and 0.30 nm is 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.

The values of absorption of the calibration solutions and corresponding masses of iron build calibration graphs.

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

5.5 Processing of analysis results

Mass fraction of iron in the sample X, %, is calculated by the formula

, (2)

where is the mass of iron in the 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 2.

Bibliography

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* Valid on the territory of the Russian Federation.