GOST R ISO 13898-3-2007

• gost-r-iso-13898-3-2007.pdf (330.14 KiB)
  ГОСТ Р ИСО 13898-3-2007

GOST R ISO 13898−3-2007 Steel and cast iron. Determination of Nickel, copper and cobalt. Spectrometric method of atomic emission with inductively coupled plasma. Part 3. Determination of copper content

GOST R ISO 13898−3-2007

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 3

DETERMINATION OF COPPER CONTENT

Steel and iron. Determination of nickel, copper and cobalt contents.
Inductively coupled plasma atomic emission spectrometric method. Part 3.
Determination of copper 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 145th St

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

The method is applicable for determining the mass fraction of copper in the range of 0.001% to 0.40%.

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 solutions of copper

4.1.1 the Basic solution is 0.80 g/DMof copper.

Preparation of a standard solution: the weight of metal of copper with a mass of 0.8000 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 gently 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 0.80 mg of copper.

4.1.2 Standard solution A, corresponding to 0.08 g/lof copper: 20.0 cmstandard solution of copper (4.1.1) is transferred into a measuring flask with a capacity of 200 cm, adjusted to the mark with water and mix.

Standard solution And prepared immediately before use.

1 cmstandard solution contains 0.08 mg of copper.

4.1.3 Standard solution, corresponding to 0.016 g/lof copper: 10.0 cmbasic solution of copper (4.1.1) is transferred into a measuring 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 0.016 mg of copper.

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 copper content is carried out according to ISO 13898−1, 7.2.

7.3 analysis

7.3.1 Preparation of the sample solution is carried out according to ISO 13898−1, 7.3.1.

7.3.2 Preparation of the calibration solutions

Make six chemical glasses with a capacity of 200 cmeach (1,00±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 copper And (4.1.2), the volume of which is indicated in table 1.


Table 1 — Mass fraction of copper from 0.001% to 0.40%

If the calibration curve will be linear, can be used for additional calibration series of solutions (for example from tables 2 and 3). If you apply the methodology of the 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.


Table 2 — Mass fraction of copper less than 0.008% of

Table 3 — Mass fraction of copper from 0.008% to 0,080%

7.4 Spectrometer measurements

7.4.1 Optimization of the device

Perform operations according to ISO 13898−1, 7.4.1.

7.4.2 Measurement of radiation intensity

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 Determination 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 4 or calculated according to the schedule given in Appendix V.


Table 4

Percentage

8.2 Precision

Routine testing of the present method was carried out in 26 laboratories in 12 countries. Analyzed 11 samples with copper content in the specified range. Each laboratory was performed according to three definitions in each sample (see notes 1 and 2 of this subsection). Used samples are given in table A. 1 (Appendix A).

The results obtained were processed statistically in accordance with ISO 5725−1, ISO 5725−2, ISO 5725−3 using data analysis of these samples containing 11 levels of copper in the working range.

The data obtained showed the presence of a logarithmic relationship between the mass fraction of copper and the limit of repeatability (convergence) the results of the analysis as well as indicators of the limit of reproducibility and the limit of intermediate precision (see note 3 of this subsection) that are given in table 4. More information on international tests given in Appendix A.

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 4, were obtained based on the results of international analytical tests carried out on nine samples of steel and one sample of cast iron, with the participation of 26 laboratories.

The analyzed samples are presented in table A. 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 copper obtained in one day, %;

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

Figure B. 1 — Logarithmic plot between the mass fraction of copper
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