GOST 13047.10-2014

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  ГОСТ 13047.10-2014

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

GOST 13047.10−2014

INTERSTATE STANDARD

NICKEL. COBALT

Methods for determination of copper

Nickel. Cobalt. Methods for determination of copper

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 13047.10−2014 introduced as the national standard of the Russian Federation from 1 January 2016.

5 REPLACE GOST 13047.10−2002


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 copper (at a mass fraction of copper from from 0.0002% to 2.0%) 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 859−2001 Copper. Brand

GOST 3760−79 Reagents. The aqueous ammonia. Specifications

GOST 4328−77 Reagents. Sodium hydroxide. Specifications

GOST 4461−77 Reagents. Nitric acid. Specifications

GOST 5457−75 Acetylene, dissolved and gaseous. Specifications

GOST 5845−79 Reagents. Potassium-sodium vinocity 4-water. 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 20015−88 Chloroform. 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 435 nm of a solution of complex compounds of copper diethyldithiocarbamate, extractable with chloroform at pH 3−4.

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

Spectrophotometer or photoelectrocolorimeter, which provides measurements in the wavelength range from 420 nm to 450 nm.

Nitric acid according to GOST 4461, if necessary, purified by distillation, or according to GOST 11125, diluted 1:1, 1:9 and 1:19.

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

Sodium hydroxide according to GOST 4328, solution mass concentration of 0.1 g/cm.

Potassium-sodium vinocity 4-water according to GOST 5845, solution mass concentration of 0.1 g/cm.

Lead diethyldithiocarbamate [1]*, the solution of the mass concentration of 0.0001 g/cmin chloroform.
________________
* See Bibliography. — Note the manufacturer’s database.


Paper universal indicator [2].

Chloroform according to GOST 20015 or Pharmacopoeia [3].

Copper according to the GOST 859.

Solutions of known copper concentration.

The solution And the mass concentration of copper 0,001 g/cmis prepared as follows: a sample of copper weighing 1,0000 g were placed in a glass 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, transferred into a measuring flask with volume capacity of 1000 cmand adjusted to the mark with distilled water.

Solution B mass concentration of copper 0.0001 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cmtransfer 10 cmof solution A and bring to the mark with nitric acid, diluted 1:19.

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

The solution G of the mass concentration of copper 0,000005 g/cmis prepared as follows: into a measuring flask with a capacity of 200 cmtransfer 10 cmof solution B and adjusted to the mark with distilled water.

4.3 Preparation for analysis

4.3.1 To construct a calibration chart 1 in determining the mass fraction of copper not more than 0.03% in a separating funnel with a capacity of 100 cmstand 0,5; 1,0; 2,0; 4,0; 6,0 and 8,0 cmsolution G pour 50 to 60 cmof distilled water and further analyze in compliance with 4.4.2.

The mass of copper in the calibration solutions is 0,0000025; 0,0000050; 0,0000100; 0,0000200; 0,0000300 and 0,0000400 G.

The light absorption values of the calibration solutions and corresponding mass of copper to build the calibration graph 1 given the importance of absorption of the calibration solution, is prepared without introducing a solution containing copper.

4.3.2 For the construction of calibration curve 2 in determining the mass fraction of copper in excess of 0.03% in separating funnel with a capacity of 100 cmtransfer 1,0; 2,0; 3,0; 5,0; 7,0 and 10,0 cmsolution, pour 50 to 60 cmof distilled water, add drop by drop nitric acid diluted 1:9, or ammonia, diluted 1:1, to obtain a solution pH of 3−4 by universal indicator paper and then carry out the analysis in accordance with 4.4.2.

The mass of copper in the calibration solutions is 0,00001; 0,00002; 0,00003; 0,00005; 0,00007 and 0,00010 g.

The light absorption values of the calibration solutions and corresponding mass of copper to build the calibration graph 2 given the importance of absorption of the calibration solution, is prepared without introducing a solution containing copper.

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

To the weighed samples poured from 20 to 40 cmof nitric acid, diluted 1:1, is dissolved when heated, is evaporated to a volume of 5 to 10 cm, flow 20 cmof distilled water.

When the mass fraction of copper not more than 0,008% solution transferred to a separatory funnel with a capacity of 100 cm.

When the mass fraction of copper from 0.008% to 0,300% solution transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with distilled water and taken aliquot part of volume in accordance with table 1 in the separating funnel with a capacity of 100 cm.

Allowed other dilute solutions, provided that the mass of copper in the solution placed in a separatory funnel, is within the limits of the masses of copper of the calibration graphs, constructed in accordance with 4.3.

4.4.2 the Solution in a separating funnel, top up with distilled water to 50 cm, add dropwise ammonia diluted 1:1, or nitric acid diluted 1:9, to obtain a pH in the range of 3−4 on the universal indicator paper, pour 10 cmof a solution of lead diethyldithiocarbamate funnel and shake for 2 min.

The organic phase is decanted through a funnel with a cotton swab, rinsed with chloroform in volumetric flask with a capacity of 25 m*. To the aqueous phase poured 5 cmof a solution of lead diethyldithiocarbamate, and shake the funnel for 1 min.
________________
* Dimension corresponds to the original. — Note the manufacturer’s database.


The organic phase attached to the solution in a volumetric flask, the aqueous phase repeat extraction with 5 cmof lead diethyldithiocarbamate for 30 s. the Extraction is repeated to produce the colorless organic phase, the organic phase merging into the same volumetric flask, and measure the light absorption of the solution in accordance with 4.4.4.

4.4.3 the analysis of cobalt with a mass fraction of copper not more than 0.001% organic phase after extraction of copper by diethyldithiocarbamate lead is collected in a porcelain Cup or a glass with a capacity of 100 cmand evaporated to dryness on a water bath.

The dry residue is treated with 5 cmof nitric acid, diluted 1:1, and evaporated to dryness. Salt dissolved in a volume of 3 to 5 cmof nitric acid, diluted 1:9, and the solution transferred to a separatory funnel with a capacity of 100 cm, top up with distilled water up to 50 cmand then a second extraction in accordance with 4.4.2.

4.4.4 Solution in volumetric flask was adjusted to the mark with chloroform. After 10 min. measure the light absorption of the solution on the spectrophotometer at a wavelength of 435 nm or photoelectrocolorimeter in the wavelength range from 420 nm to 450 nm, using as a comparison solution of chloroform.

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

4.5 Processing the analysis results

Mass fraction of copper in the sample of X % is calculated by the formula:

, (1)

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

 — the mass of copper 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 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 324,7 nm resonance radiation by atoms of copper 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 copper.

Acetylene gas according to GOST 5457.

Filters obestochennye in [4] 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.

Nickel powder according to GOST 9722 or standard sample of Nickel, for example [5] pre-installed (certified) mass fraction of copper not more than 0,0002%.

Cobalt GOST 123 or standard sample of cobalt pre-installed (certified) mass fraction of copper not more than 0,0002%.

Copper according to the GOST 859.

Solutions of known copper concentration.

The solution And the mass concentration of copper 0,001 g/cmat 4.2.

Solution B mass concentration of copper 0.0001 g/cmat 4.2.

Solution of the mass concentration of copper 0,00001 g/cmat 4.2.

5.3 Preparation for assay

5.3.1 To construct a calibration chart 1 in determining the mass fraction of copper of not more than 0,0020% sample of Nickel powder or cobalt or standard samples of composition of Nickel or 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 Nickel powder or cobalt or standard samples of composition of Nickel or cobalt is dissolved by heating in a volume of 50 to 60 cmof nitric acid, diluted 1:1, boiled for 2−3 min. When using Nickel powder in the solution was filtered through a filter (red or white ribbon), washed two or three times with nitric acid, diluted 1:9. The filter is washed two or three times with distilled water. The solutions were evaporated to a volume of 15 to 20 cm, flow 50 to 60 cmof distilled water, heated to boiling, cooled, transferred to volumetric flasks with a capacity of 100 cm, flow 1,0; 2,0; 4,0; 6,0; 8,0 and 10,0 cmof solution B. the flask with the solution in the reference experiment, the solution containing the copper, not poured, adjusted to the mark with distilled water and measure the absorbance in accordance with 5.4.

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

5.3.2 For the construction of calibration curve 2 in determining the mass fraction of copper from 0.002% to 0,010% sample of Nickel powder or cobalt or standard samples of composition of Nickel or cobalt with a mass of 3,000 g were placed in beakers 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 Nickel powder or cobalt or standard samples of composition of Nickel or cobalt is dissolved in accordance with 5.3.1, transfer the solutions in volumetric flasks with a capacity of 100 cmand flow 0,5; 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 copper, not poured, adjusted to the mark with nitric acid, diluted 1:19, and measure absorption in accordance with 5.4.

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

5.3.3 For construction of calibration curve 3 when determining the mass fraction of copper from 0.01% to 0.05% of the sample of Nickel powder or cobalt or standard samples of composition of Nickel or 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 Nickel powder or cobalt or standard samples of composition of Nickel or cobalt is dissolved in a volume of 15 to 20 cmof nitric acid, diluted 1:1 in accordance with 5.3.1, transfer the solutions in volumetric flasks with a capacity of 100 cmand flow 0,5; 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 copper, not poured, adjusted to the mark with nitric acid, diluted 1:19, and measure absorption in accordance with 5.4.

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

5.3.4 To build a calibration schedule 4 when determining the mass fraction of copper from 0.05% to 0.50% in volumetric flasks with a capacity of 100 cmshift 10 cmof the solution in the reference experiment, prepared in accordance with 5.3.3, and pour 0,5; 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 copper, not poured, adjusted to the mark with nitric acid, diluted 1:19, and measure absorption in accordance with 5.4.

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

5.3.5 To build a calibration chart 5 when determining the mass fraction of copper over 0.50% in the volumetric flask with a capacity of 100 cmstand 0,5; 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 copper, not poured, adjusted to the mark with nitric acid, diluted 1:19, and measure absorption in accordance with 5.4.

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

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 weight of 3,000 or 5,000 g was dissolved with heating in a volume of 50 to 60 cmof nitric acid, diluted 1:1, the hitch weight of 1,000 g was dissolved with heating 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, 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 copper of more than 0,050% in a volumetric flask with a capacity of 100 cmstand aliquot part of the sample solution with a volume in accordance with table 3 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 324,7 nm and slit width of not more than 0.4 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 mass of copper to build the calibration graph.

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

5.5 Processing of analysis results

Mass fraction of copper in the sample of X % is calculated by the formula:

, (2)

where is the mass of copper 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 2.