GOST 13047.12-2014

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  ГОСТ 13047.12-2014

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

GOST 13047.12−2014

INTERSTATE STANDARD

NICKEL. COBALT

Methods for determination of antimony

Nickel. Cobalt. Methods for determination of antimony

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 13047.12−2014 introduced as the national standard of the Russian Federation from 1 January 2016.

5 REPLACE GOST 13047.12−2002


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 antimony (in mass fraction of antimony from 0.0001% to 0,0020%) in the primary Nickel GOST 849, Nickel powder according to GOST 9722 and GOST cobalt 123 on. 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 1089−82 Antimony. Specifications

GOST 3118−77 Reagents. Hydrochloric acid. Specifications

GOST 4197−74 Reagents. Sodium atomistically. Specifications

GOST 4204−77 Reagents. Sulphuric acid. Specifications

GOST 4461−77 Reagents. Nitric acid. Specifications

GOST 5789−78 Reagents. Toluene. Specifications

GOST 6691−77 Reagents. Urea. Specifications

GOST 9722−97 Nickel Powder. Specifications

GOST 10157−79 Argon gaseous and liquid. 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

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 610 nm of a solution of complex compounds of antimony with crystal violet (indicator) after a preliminary extraction of the toluene.

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

Spectrophotometer or photoelectrocolorimeter, which provides measurements in the wavelength range from 580 to 620 nm.

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

Hydrochloric acid according to GOST 3118, if necessary, purified by distillation, or according to GOST 14261, diluted 3:1 and 1:1.

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

Sodium atomistically according to GOST 4197, solution mass concentration of 0.1 g/cm.

Tin dichloride [1]*, solution mass concentration of 0.1 g/cmin hydrochloric acid, diluted 3:1.
________________
* See Bibliography. — Note the manufacturer’s database.


Crystal violet (N, N, N', N', N», N'-Hexamethylpropylene; kristallwelt) [2], solution of the mass concentration of 0.002 g/cm.

Urea according to GOST 6691, solution mass concentration of 0.5 g/cm.

Toluene according to GOST 5789, if necessary, purified by distillation.

Antimony GOST 1089.

Solutions of known concentration of antimony.

The solution And the mass concentration of antimony 0.0001 g/cmis prepared as follows: weighed pre-crushed to a powder of antimony with a mass 0,1000 g placed in a beaker with a capacity of 600 cm, flow 15 to 20 cmof sulphuric acid, dissolved by heating, cooled, poured from 200 to 250 cmof distilled water, cooled, poured 150 cmof hydrochloric acid diluted 1:1, cooled, transferred into a measuring flask with volume capacity of 1000 cmand adjusted to the mark with distilled water.

Solution B mass concentration of antimony 0,00001 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 hydrochloric acid diluted 1:1.

Solution of the mass concentration of antimony 0,000001 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cmtransfer 10 cmof solution B and bring to the mark with hydrochloric acid diluted 1:1.

4.3 Preparation for analysis

To build a calibration curve in glasses with a capacity of 100 or 150 cmcarry 1,0; 3,0; 5,0; 7,0; 10,0 and 20,0 cmsolution, poured to a volume of 25 cmhydrochloric acid diluted 1:1 add two or three drops of solution of tin dichloride and then carry out the analysis in accordance with 4.4.2.

The mass of antimony in the calibration solutions is 0,000001; 0,000003; 0,000005; 0,000007; 0,000010 and 0,000020 G.

The light absorption values of the calibration solutions and corresponding masses of antimony building a calibration curve based on the value of absorption of the calibration solution, prepared without the introduction of a solution containing antimony.

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, is dissolved when heated, is evaporated to a volume of 5 to 10 cm, cool flow 10 cmof sulphuric acid diluted 1:1. The solution was evaporated until the termination of allocation of steams of sulfuric acid, cooled, poured 25 cmhydrochloric acid diluted 1:1, dissolved salts during the heating and cool the solution.

4.4.2 the solution add two or three drops of solution of tin dichloride, stand 1 min, pour 2 cmof a solution of sodium attestatio, kept 5 min, poured 25 cmof distilled water, 2 cmof the urea solution, stirred until the termination of allocation of gas bubbles and transferred to a separatory funnel with a capacity of 250 cm. Bring distilled water to a volume of 130 cm, flow 1.0 cmof a solution of crystal violet, 10 cmof toluene and shake the separatory funnel for 30 s. the Aqueous phase is transferred into another separatory funnel with a capacity of 250 cm, and an organic phase in a volumetric flask with a capacity of 25 cm. Repeat the extraction with toluene, the aqueous phase is discarded and the organic phase was transferred to a volumetric flask.

Light absorption of the sample solution is measured after 10−15 minutes on the spectrophotometer at a wavelength of 610 nm or photoelectrocolorimeter at a wavelength range from 580 to 620 nm, using as a comparison solution of toluene.

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

4.5 Processing the analysis results

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

, (1)

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

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

K — dilution factor of sample solution;

M — weight of sample, g.

4.6 Control of accuracy of analysis results

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 217,7 nm resonance radiation by atoms of antimony, resulting from the electrothermal atomization of the sample solution.

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

Atomic absorption spectrometer for measurements with electrothermal atomization, the correction non-selective absorption and the automated flow of the solution into the atomizer.

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

Argon gas according to GOST 10157.

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.

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

Nickel powder according to GOST 9722 or standard sample of Nickel pre-installed (certified) mass fraction of antimony is not more than 0.0001%.

Cobalt GOST 123 or standard sample of cobalt pre-installed (certified) mass fraction of antimony is not more than 0.0001%.

Antimony GOST 1089.

Solutions of known concentration of antimony.

The solution And the mass concentration of antimony 0.0001 g/cmat 4.2.

Solution B mass concentration of antimony 0,00001 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 antimony 0,000001 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cmtransfer 10 cmof solution B and bring to the mark with nitric acid, diluted 1:19.

5.3 Preparation for assay

5.3.1 To construct a calibration chart 1 in determining the mass fraction of antimony is not more than 0,0010% suspension 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.

The suspension of Nickel powder or cobalt or of a standard sample of composition of Nickel or cobalt is dissolved by heating in 15−20 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 hot distilled water. The solution is evaporated to a volume of 5−7 cm, flow from 40 to 50 cmof distilled water, heated to boiling, cooled and transferred to volumetric flasks with a capacity of 100 cm.

Flasks transfer 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 antimony, not poured, adjusted to the mark with distilled water and measure the absorbance in accordance with 5.4.

The mass of antimony in the calibration solutions is 0,000001; 0,000002; 0,000004; 0,000006; 0,000008 and 0,000010 G.

5.3.2 For the construction of calibration curve 2 in determining the mass fraction of antimony more than 0,0010% in volumetric flasks with a capacity of 100 cmstand for 20 cmof the solution in the reference experiment, prepared in accordance with 5.3.1, poured 1,0; 2,0; 4,0; 6,0; 8,0 and 10,0 cmof solution V. one of the flasks with a solution of the reference experiment a solution containing antimony, not poured, adjusted to the mark with nitric acid, diluted 1:19, and measure absorption in accordance with 5.4.

The mass of antimony in the calibration solutions is given in 5.3.1.

5.4 analysis

A portion of the sample with a mass 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, is dissolved when heated, is evaporated to a volume of 5−7 cm, cooled, transferred to a volumetric flask with a capacity of 100 cmand adjusted to the mark with distilled water.

When the mass fraction of antimony more than 0,0010% in a volumetric flask with a capacity of 100 cmstand aliquot part of the sample solution with a volume of 20 cm, adjusted to the mark with nitric acid, diluted 1:19.

The absorbance of the sample solution and the calibration solutions at a wavelength of 217,6 mm, slit width of 0.3 nm with a correction non-selective absorption in the current of argon is measured at least two times, sequentially spraying them in an atomizer. Depending on the type of spectrometer to select the optimal amount of solution injected into the atomizer, from 0.010 to 0.050 cmor optimal time of the aerosol spraying of the solution from 5 to 50 C. Washed the spray 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.

Selection of optimal temperature regimes for the atomizer is carried out individually for the used spectrometer for the calibration solutions. Recommended operating conditions of the atomizer are shown in table 2.


Table 2 — operating conditions of the atomizer

The values of absorption of the calibration solutions and corresponding masses of antimony building calibration charts.

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

5.5 Processing of analysis results

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

, (2)

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

K — dilution factor of sample solution;

M — weight of sample, g.

5.6 Control of accuracy of analysis results

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 3.


Table 3 — 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