GOST 13047.23-2014

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  ГОСТ 13047.23-2014

GOST 13047.23−2014 Nickel. Cobalt. Method for the determination of tellurium in Nickel

GOST 13047.23−2014

INTERSTATE STANDARD

NICKEL. COBALT

Method for the determination of tellurium in Nickel

Nickel. Cobalt. Method for determination of tellurium in nickel

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 13047.23−2014 introduced as the national standard of the Russian Federation from 1 January 2016.

5 REPLACE GOST 13047.23−2002


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 method for the determination of tellurium (if the mass fraction of tellurium from 0,00002% to 0,0010%) in the primary Nickel GOST 849.

2 Normative references

This standard uses the regulatory references to the following standards:

GOST 849−2008 Nickel primary. Specifications

GOST 4461−77 Reagents. Nitric acid. 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

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

4.1 Method of analysis

The method is based on measuring absorption at a wavelength of 214,3 nm resonance radiation by atoms of tellurium 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 tellurium.

Argon gas according to GOST 10157.

Filters obestochennye [1]* other filters or medium density.
________________
* See Bibliography. — 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.

Nickel powder according to GOST 9722 or standard sample of Nickel, for example [3] pre-installed (certified) mass fraction of tellurium is not more than 0,00002%.

Tellurium of high purity [2].

Solutions of tellurium concentration.

The solution And the mass concentration of tellurium 0,0001 g/cmis prepared as follows: a portion of the tellurium mass 0,1000 g placed in a beaker with a capacity of 100 cm, flow 10 to 15 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 cm, 50 cm pournitric acid, diluted 1:1, and adjusted to the mark with distilled water.

Solution B mass concentration of tellurium 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 tellurium 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.

The solution G of the mass concentration of tellurium 0,0000002 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cm andstand 20 cmsolution 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 tellurium is not more than 0,00010% suspension of Nickel powder or standard sample of Nickel 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.

In beakers or flasks poured from 15 to 20 cmof nitric acid, diluted 1:1 and dissolved by heating. When using the Nickel powder in the solutions were filtered through filters (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; 3,0; 4,0 and 5,0 cmof the solution In the flask with the solution in the reference experiment, the solution containing the tellurium, not poured, adjusted to the mark with distilled water and measure the absorbance in accordance with 4.4.

Mass of tellurium in the calibration solutions is 0,0000002; 0,0000004; 0,0000006; 0,0000008 and 0,0000010 G.

4.3.2 For the construction of calibration curve 2 in determining the mass fraction of tellurium more than 0,00010% suspension of Nickel powder or standard sample of Nickel with a mass of 0,500 g was 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.

The suspension of Nickel powder or standard sample composition of Nickel dissolved in accordance with 4.3.1. In a volumetric flask transfer 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 tellurium, not poured, adjusted to the mark with distilled water and measure the absorbance in accordance with 4.4.

Mass of tellurium in the calibration solutions is 0,0000005; 0,0000010; 0,0000020; 0,0000030; 0,0000040 and 0,0000050 G.

4.4 analysis

A portion of the sample with a mass of 1,000 g (with mass fraction of tellurium is not more than 0,00010%) or weighing 0,500 g (with mass fraction of tellurium more than 0,00010%) were placed in a glass or flask with a capacity of 250 cm, flow 15 to 20 cmof nitric acid, diluted 1:1, evaporated to a volume of 5 to 7 cm, transfer the solution into a volumetric flask with a capacity of 100 cm, cooled and adjusted to the mark with distilled water.

The absorbance of the sample solution and the calibration solutions at a wavelength of 214,3 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 select the optimal volume of the solution from 0.005 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 is carried out individually for the used spectrometer for the calibration solutions. Recommended operating conditions of the atomizer shown in table 1.


Table 1 — operating conditions of the atomizer

The values of absorption of the calibration solutions and corresponding masses of tellurium to build the calibration graph.

The value of absorbance of sample solution find the mass of tellurium on the appropriate calibration schedule.

4.5 Processing the analysis results

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

, (1)

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

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