GOST R ISO 13898-4-2007

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  ГОСТ Р ИСО 13898-4-2007

GOST R ISO 13898−4-2007 Steel and cast iron. Determination of Nickel, copper and cobalt. Spectrometric method of atomic emission with inductively coupled plasma. Part 4. Determination of cobalt

GOST R ISO 13898−4-2007

Group B39

NATIONAL STANDARD OF THE RUSSIAN FEDERATION

Steel and cast iron

DETERMINATION OF NICKEL, COPPER AND COBALT.
SPECTROMETRIC METHOD OF ATOMIC EMISSION
INDUCTIVELY COUPLED PLASMA

Part 4

DETERMINATION OF COBALT

Steel and iron. Determination of nickel, copper and cobalt contents.
Inductively coupled plasma atomic emission spectrometric method.
Part 4. Determination of cobalt content

OKS 77.120
AXTU 0709

Date of introduction 2008−01−01

Preface

The objectives and principles of standardization in the Russian Federation established by the Federal law of 27 December 2002 N 184-FZ «On technical regulation», and rules for the application of national standards of the Russian Federation — GOST R 1.0−2004 «Standardization in the Russian Federation. The main provisions"

Data on standard

1 PREPARED AND SUBMITTED by the Technical Committee for standardization TC 145 «monitoring Methods of steel products"

2 APPROVED AND put INTO EFFECT by the Federal Agency for technical regulation and Metrology, dated 22 June 2007 N 146-St

3 this standard is identical with ISO 13898−4:1997 «Steel and cast iron. Determination of Nickel, copper and cobalt. Spectrometric method of atomic emission with inductively coupled plasma. Part 4 Determination of cobalt» (ISO 13894−4:1997 «Steel and iron — Determination of nickel, copper and cobalt contents — Inductively coupled plasma atomic emission spectrometric method — Part 4: Determination of cobalt content»).

In applying this standard it is recommended to use instead of the referenced international standards corresponding national standards of the Russian Federation, details of which are given in the Appendix With

4 INTRODUCED FOR THE FIRST TIME


Information about the changes to this standard is published in the annually issued reference index «National standards», and the text changes and amendments — in monthly indexes published information «National standards». In case of revision (replacement) or cancellation of this standard a notification will be published in a 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 spectrometer of atomic emission with inductively coupled plasma method for the determination of cobalt in unalloyed steels and cast iron.

The method is applicable for determining the mass fraction of cobalt in the range of 0.001% -0.10 percent.

2 Normative references

This standard uses the regulatory references to the following international standards:

ISO 5725−1:2002 Accuracy (trueness and precision) of methods and measurement results. Part 1. General provisions and definitions

ISO 5725−2:2002 Accuracy (trueness and precision) of methods and measurement results. Part 2. The basic method for the determination of repeatability and reproducibility of a standard measurement method

ISO 5725−3:2002 Accuracy (trueness and precision) of methods and measurement results. Part 3. Intermediate indicators the precision of a standard measurement method

ISO 13898−1:1997 Steel and iron. Determination of Nickel, copper and cobalt. Spectrometric method of atomic emission with inductively coupled plasma. Part 1. General requirements and sampling

ISO 14284:1996 Steel and iron. Selection and preparation of samples for chemical analysis

3 General requirements

General requirements — ISO 13898−1.

4 Reagents and solutions

Unless otherwise specified, use reagents of the established analytical purity, distilled water, further purified by distillation or other means.

Additional requirements for the reagents — ISO 13898−1.

4.1 Standard solution of cobalt

4.1.1 the Basic solution is 1.0 g/DMof cobalt.

Preparation of a standard solution of cobalt metal: the portion of sample weight 1,0000 g, taken with an accuracy of 0.1 mg and a purity of more than 99.99%, is placed in a beaker with a capacity of 200 cm. Add 50 cmof nitric acid (ISO 13898−1, 4.3), cover watch glass, heat gradually and boil until dissolved. Cooled to room temperature, transferred to a measuring flask with volume capacity of 1000 cm, then bring to the mark with water and mix.

1 cmstandard solution contains 1.0 mg of cobalt.

4.1.2 Standard solution corresponding to 0,020 g/DMof cobalt.

10.0 cmof a standard solution of cobalt (4.1.1) is transferred to a volumetric flask with a capacity of 500 cm, was adjusted to the mark with water and mix.

A standard solution is prepared immediately before use.

1 cmstandard solution contains 0,020 mg of cobalt.

If the calibration curve obtained is nonlinear, can be used an additional series of calibration solutions.

5 Instrument

Equipment must meet ISO 13898−1.

6 Sampling

Sampling — ISO 14284.

7 Preparation and analysis

7.1 the Hitch weight 1,000 g weighed with an accuracy of 1 mg.

7.2 the Control and experience that corresponds to the sample with zero content of cobalt, is carried out according to ISO 13898−1, 7.2.

7.3 analysis

7.3.1 Preparation of test solution — ISO 13898−1, 7.3.1.

7.3.2 Preparation of the calibration solutions

Make six chemical glasses with a capacity of 200 cmeach (1,000±0,001) g of pure iron (ISO 13898−1, 4.1), added to each 10 cmof nitric acid (ISO 13898−1, 4.3), cover with a watch glass and slowly heated until the cessation of the stormy vapors escaping. Add 10 cmof hydrochloric acid (ISO 13898−1, 4.2) and continue heating until dissolved. Cooled to room temperature and quantitatively transfer the solution into six volumetric flasks with a capacity of 200 cmeach, pre-rinsing them in a minimum amount of water. Using a pipette or burette, add to the volumetric flask standard solution of cobalt (4.1.2), the volume of which is indicated in table 1.


Table 1 — Mass fraction of cobalt from 0.001% to 0.10%

If the calibration curve will be linear, can be used additional calibration series of solutions (e.g. from table 2).


Table 2 — Mass fraction of cobalt is less than 0.010%

If you use the method of internal standard, then add 2cmof a solution of internal standard scandium (ISO 13898−1, 4.4) or 10 cmof a solution of internal standard yttrium (ISO 13898−1, 4.5). Bring to mark with water and mix.

7.4 Spectrometer measurements

7.4.1 Optimization of the device

Perform operations according to ISO 13898−1, 7.4.1.

7.4.2 measuring the intensity of radiation

Perform operations according to ISO 13898−1, 7.4.2.

7.4.3 Preparation of calibration curve

Perform operations according to ISO 13898−1, 7.4.3.

8 Processing of results

8.1 Perform operations according to ISO 13898−1, 8.1.

The result of the analysis of samples taking the average of results of two parallel measurements, if differences between them do not exceed the values of permissible differences given in table 3 or calculated according to the schedule given in Appendix V.


Table 3

Percentage

8.2 Precision

Routine testing of the present method was carried out in 26 laboratories in 12 countries, eight levels of cobalt. Each laboratory performed three determination of cobalt at each level of its content (see remarks of this subsection).

Samples used for tests are given in table A. 1 (Appendix A).

The results were processed statistically in accordance with ISO 5725−1, ISO 5725−2, ISO 5725−3 using data analysis of these samples containing eight levels of cobalt in the working range.

The data obtained showed the presence of a logarithmic relationship between the mass fraction of cobalt and a limit of repeatability (convergence) , as well as indicators of the limit of reproducibility and the limit of intermediate precision of the analysis results (see notes of this subsection) that are shown in table 3.

Graphical representation of the data is given in Appendix V.

Notes

1 Two of the three definitions was carried out under conditions of repeatability, specified in ISO 5725−1, i.e. a single operator on the same equipment at identical operating conditions, one calibration and for the minimum period of time.

2 the Third definition was made at a different time (another day) by the same operator who performed the determination, described in note 1, using the same instrument with a new calibration.

3 the results obtained on the first day, was calculated according to ISO 5725−2, the limit of repeatability (convergence) and reproducibility limit . According to the first result obtained on the first day, and the result obtained on the second day, was calculated according to ISO 5725−3 intralaboratory limit of intermediate precision .

9 test report

Test report — ISO 13898−1, section 9.

Annex a (informative). More information on international testing

Appendix A
(reference)

Data for the repeatability (convergence) and reproducibility given in table 3, were obtained based on the results of international analytical tests performed on seven samples of the steel and one sample of cast iron in 12 countries, with the participation of 26 laboratories. Graphical representation of data on test accuracy are given in Appendix B.

The analyzed samples are presented in table 1.


Table A. 1

Percentage

Annex b (informative). Graphical representation of the data for precision

The App
(reference)

;

;

,

where  — the average value of the mass fraction of cobalt, obtained in the course of one day, %;

the average value of the mass fraction of cobalt based on the data of different days, %.

Figure B. 1 — Logarithmic plot between the mass fraction of cobalt
and the limit of repeatability or reproducibility limit
and the limit of intermediate precision

Application (reference). Data on compliance with national standards of the Russian Federation the reference to international standards

Application
(reference)

Table C. 1