GOST 13047.6-2014

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  ГОСТ 13047.6-81

GOST 13047.6−2014 Nickel. Cobalt. Method for determination of carbon

GOST 13047.6−2014

INTERSTATE STANDARD

NICKEL. COBALT

Method for determination of carbon

Nickel. Cobalt. Method for determination of carbon

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 13047.6−2014 introduced as the national standard of the Russian Federation from 1 January 2016.

5 REPLACE GOST 13047.6−2002


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 method of infrared spectroscopy determination of carbon (in mass percentage of carbon from 0,0010% to 0.50%) in the primary Nickel GOST 849, Nickel powder according to GOST 9722, cobalt GOST 123 and cobalt powder to GOST 9721.

2 Normative references

This standard uses the regulatory references to the following standards:

GOST 8.315−97 State system for ensuring the uniformity of measurements. Standard samples of composition and properties of substances and materials. The main provisions of the

GOST 123−2008 Cobalt. Specifications

GOST 849−2008 Nickel primary. Specifications

GOST 859−2001 Copper. Brand

GOST 2603−79 Reagents. Acetone. Specifications

GOST 5583−78 (ISO 2046−73) Oxygen gas technical and medical. Specifications

GOST 9147−80 Glassware and equipment lab porcelain. Specifications

GOST 9721−79 cobalt Powder. Specifications

GOST 9722−97 Nickel Powder. 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 infrared spectrometric Method.

4.1 Method of analysis

The method is based on measuring the absorption of infrared radiation by molecules of carbon monoxide (IV) after selecting it from the metal by combustion in induction high-frequency furnace in oxygen flow.

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

Carbon analyzer, based on the principle of infrared spectrometry, with high frequency induction furnace, and weights to account for the mass of sample sample.

Refractory ceramic crucible, calcined at a temperature of from 1100 °C to 1200 °C for 3−4 h.

Marshes: marshes provided by the manufacturer complete with a carbon analyzer; the copper according to the GOST 859 in the form of chips or wire; tungsten [1]*; iron carbonyl in [2] and other substances that provide combustion, and the results of the reference experiment in accordance with 4.3.
________________
* See Bibliography. — Note the manufacturer’s database.


Technical oxygen gas according to GOST 5583.

Acetone according to GOST 2603.

Standard samples according to GOST 8.315 composition of Nickel, cobalt, or alloys based on Nickel, cobalt or iron with a certified mass fraction of carbon.

4.3 Preparation for analysis

Preparing the analyzer to work and his grading is carried out in accordance with the manual. To build a calibration curve using standard samples of composition of Nickel, cobalt, or alloys based on Nickel, cobalt or iron.

A portion of the beach that mass, which is used in the analysis of samples placed to carry out control experience in the crucible and carried out the analysis in accordance with 4.4.

Allowed for the introduction of flux to use metering devices.

The result of the reference experiment is considered satisfactory, if the measured mass fraction of carbon on the digital display of the analyzer does not exceed the value of the index control accuracy (expanded uncertainty) of the method of analysis presented in 4.6 to define the mass fraction of carbon.

The negative results in the reference experiment, it is recommended to bake the crucible in accordance with 4.2, and the flux in the form of metal washed with acetone and dried at a temperature from 20 °C to 30 °C. it is allowed to use other volatile organic solvents, providing the required values in the reference experiment.

4.4 analysis

A portion of sample weighing 0.200 to 1,000 g was placed in a crucible, add the flux, the weight of which must be the same when conducting the reference experiment, the calibration and analysis, and conduct analysis in accordance with the manual of the analyzer. When poor convergence results of parallel measurements allowed before analysis to clean the sample selected in the form of chips, with acetone and dried at a temperature from 20 °C to 30 °C.

4.5 Processing the analysis results

The result of measuring the mass fraction of carbon in percentage values of the reference experiment is shown on the display or printer of the analyzer.

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

Bibliography