GOST 13047.13-2014

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  ГОСТ 13047.13-2014

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

GOST 13047.13−2014

INTERSTATE STANDARD

NICKEL. COBALT

Methods for determination of lead

Nickel. Cobalt. Methods for determination of lead

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 (minutes of 20 October 2014 N 71-N)

3 ACCEPTED by the Interstate Council for standardization, Metrology and certification

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 13047.13−2014 introduced as the national standard of the Russian Federation from 1 January 2016.

5 REPLACE GOST 13047.13−2002


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 establishes the atomic absorption methods for the determination of lead (with a mass fraction of lead from 0.0001% to 0,010%) in the primary Nickel GOST 849, Nickel powder according to GOST 9722 and GOST cobalt 123 on.

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 3778−98 Lead. Specifications

GOST 4236−77 Reagents. Lead (II) nitrate. Specifications

GOST 4461−77 Reagents. Nitric acid. Specifications

GOST 5457−75 Acetylene, dissolved and gaseous. 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 22861−93 Lead 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 Atomic absorption method with electrothermal atomization

4.1 Method of analysis

The analysis method is based on measurement of absorption at a wavelength is 283.3 nm resonance radiation by atoms of lead resulting from the electrothermal atomization of the sample solution.

4.2 measuring instruments, 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 lead.

Argon gas according to GOST 10157.

Filters obestochennye [1]* other filters or medium density.
________________
* See Bibliography, here and hereafter. — Note the manufacturer’s database.


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

Lead at 3778 or GOST GOST 22861.

Lead (II) nitrate according to GOST 4236.

Nickel powder according to GOST 9722 or standard sample of Nickel pre-installed (certified) mass fraction of lead of no more than 0.0001%.

Cobalt GOST 123 or standard sample of cobalt pre-installed (certified) mass fraction of lead of no more than 0.0001%.

Solutions of known lead concentrations.

Solution mass And lead concentrations of 0.001 g/cmof lead is prepared as follows: a portion of the lead weight 0,5000 g placed in a beaker with a capacity of 250 cm, flow from 30 to 40 cmof nitric acid, diluted 1:1, dissolved by heating, boil for 2−3 min, cooled, transferred to a volumetric flask with a capacity of 500 cm, a flow of 30 to 40 cmof nitric acid, diluted 1:1, adjusted to the mark with distilled water.

Solution mass And lead concentrations of 0.001 g/cmof lead nitrate is prepared as follows: a portion of nitrate of lead weight 1,5980 g were placed in a glass with a capacity of 250 cm, flow from 40 to 50 cmof distilled water and 5 cmof nitric acid, diluted 1:1, dissolved by heating, boil for 2−3 min, cooled, transferred to a volumetric flask with a capacity of 500 cm, flow from 40 to 50 cmof nitric acid, diluted 1:1, and adjusted to the mark with distilled water.

Solution B mass concentration of lead 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 mass concentration of lead 0,00001 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.

The solution G of the mass concentration of lead 0,000001 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cmtransfer 10 cmof the solution and adjusted to the mark with nitric acid, diluted 1:19.

4.3 Preparation for analysis

4.3.1 To construct a calibration chart 1 in determining the mass fraction of lead of 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. When using the 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 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.

Flasks transfer 1,0; 2,0; 4,0; 6,0; 8,0 and 10,0 cmof the solution In the flask with the solution in the reference experiment the solution containing lead, not poured, adjusted to the mark with distilled water and measure the absorbance in accordance with 4.4.

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

4.3.2 For the construction of calibration curve 2 in determining the mass fraction of lead greater than 0.001% in a volumetric flask with a capacity of 100 cmshift 10 cmof the solution in the reference experiment, prepared in accordance with 4.3.1, poured 1,0; 2,0; 4,0; 6,0; 8,0 and 10,0 cmof the solution In one of the flasks with a solution of the reference experiment a solution containing lead, not poured, adjusted to the mark with nitric acid, diluted 1:19, and measure absorption in accordance with 4.4.

The mass of lead in the calibration solutions is given in 4.3.1.

4.4 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, was dissolved with heating in 15−20 cmof nitric acid, diluted 1:1, evaporated to a volume of 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 lead more than 0,0010% in a volumetric flask with a capacity of 100 cmstand aliquot part of the solution volume of 10 cm, adjusted to the mark with nitric acid, diluted 1:19.

The absorbance of the sample solution and the calibration solutions at a wavelength is 283.3 nm, slit width is not more than 1.0 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, aerosol spray 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 4.3.

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 given in table 1.


Table 1 — operating conditions of the atomizer

The values of absorption of the calibration solutions and their corresponding masses lead to build a calibration curve.

The value of absorbance of sample solution find the mass of lead by the calibration schedule.

4.5 Processing the analysis results

Mass fraction of lead in the sample X, %, calculated by the formula:

, (1)

where is the mass of lead in sample solution, 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 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 with flame atomization (at a mass fraction of lead from 0.002% to 0,010%)

5.1 Method of analysis

The analysis method is based on measurement of absorption at a wavelength is 283.3 nm resonance radiation by atoms of lead, the resulting fiery atomization when spraying a solution of the sample in the 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 lead.

Acetylene gas according to GOST 5457.

Filters obestochennye [1] 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 pre-installed (certified) mass fraction of lead of not more than 0,002%.

Cobalt GOST 123 or standard sample of cobalt pre-installed (certified) mass fraction of lead of not more than 0,002%.

Lead at 3778 or GOST GOST 22861.

Lead (II) nitrate according to GOST 4236.

Solutions of known lead concentrations.

Solution mass And lead concentrations of 0.001 g/cmat 4.2.

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

5.3 Preparation for assay

To build a calibration chart, a portion of Nickel powder or cobalt or of a standard sample of composition of Nickel or cobalt with a mass of 3,000 g were placed in a glass 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 25−30 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 and transferred to volumetric flasks with a capacity of 100 cm.

In the flask transfer 0,5; 1,0; 2,0; 3,0 and 4,0 cmof solution B. the flask with the solution in the reference experiment the solution containing lead, not poured, adjusted to the mark with distilled water and measure the absorbance in accordance with 5.4.

The mass of lead in the calibration solutions is 0,00005; 0,00010; 0,00020; and 0,00040 0,00030 g.

5.4 analysis

A portion of the sample with a mass of 3,000 g were placed in a glass or flask with a capacity of 250 cm, flow 25 to 30 cmof nitric acid, diluted 1:1, dissolved by heating, boil for 2−3 min, evaporated to a volume of 15 to 20 cm, flow 50 to 60 cmof distilled water, cooled, transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with distilled water.

The absorbance of the sample solution and the calibration solutions at a wavelength is 283.3 nm, slit width is not more than 1.0 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 of the solution is used in the reference experiment, prepared in accordance with 5.3.

The values of absorption of the calibration solutions and their corresponding masses lead to build a calibration curve.

The value of absorbance of sample solution find the mass of lead by the calibration schedule.

5.5 Processing of analysis results

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

, (2)

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

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 2.