GOST R 54153-2010

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  ГОСТ Р 54153-2010

GOST R 54153−2010 Steel. Method of atomic-emission spectral analysis

GOST R 54153−2010

NATIONAL STANDARD OF THE RUSSIAN FEDERATION

STEEL

Method of atomic-emission spectral analysis

Steel. Method of atomic emission spectral analysis

OKS 77.080.20
OKP 08 7000

Date of introduction 2012−01−01

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 DEVELOPED by Closed joint stock company «Institute of standard samples"

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

3 this standard takes into account the basic regulations of standards of ASTM Е415−08* ASTM Е1086−08* ASTM Е1009−95*
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* Access to international and foreign documents referred to here and hereinafter, can be obtained by clicking on the link. — Note the manufacturer’s database.

4 APPROVED AND put INTO EFFECT by the Federal Agency for technical regulation and Metrology of December 21, 2010 N 910-St

5 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

Introduction

This standard was developed for the first time in connection with the development of spectral equipment, expansion of analytical capabilities of the instrument, and taking into account modern requirements to the accuracy of the measurement indicators of the quality of steel in the Russian Federation.

1 Scope

1.1 this standard specifies atomic emission spectral method with photoelectric registration of spectrum to determine the steel mass fraction of elements, %:

1.2 this standard applies to the analysis of samples of steel, having a diameter sufficient to block the camera hole sparking (to ensure integrity of the camera).

2 Normative references

This standard uses the regulatory references to the following standards:

GOST R 8.563−2009 State system for ensuring the uniformity of measurements. Techniques (methods) of measurements

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

GOST R ISO 5725−6-2002 Accuracy (correctness and precision) of methods and measurement results. Part 6. The use of precision values in practice

GOST R 52361−2005 Control of the analytical object. Terms and definitions

GOST R 52781−2007 grinding and grinding. Specifications

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 12.0.004−90 System of standards of occupational safety. Organization of training safety. General provisions

GOST 12.1.004−91 System safety standards. Fire safety. General requirements

GOST 12.1.019−2009 System of standards of occupational safety. Electrical safety. General requirements and nomenclature of types of protection
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* Probably, the error of the original. Should read: GOST R 12.1.019−2009, here and hereafter. — Note the manufacturer’s database.

12.4.009 GOST-83 System of standards of occupational safety. Fire fighting equipment for protection of objects. Principal. The accommodation and service

GOST 859−2001 Copper. Brand

GOST 6456−82 emery Cloth sanding paper. Specifications

GOST 7565−81 (ISO 377−2-89) Iron, steel and alloys. Sampling method for determination of chemical composition

GOST 10157−79 Argon gaseous and liquid. Specifications

GOST 21963−2002 cutting wheels. 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 published annually by the information sign «National standards» published as on January 1 of the current year and related information published monthly indexes published in 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 Terms and definitions

This standard applies the terms and definitions GOST R ISO 5725−1, GOST 8.563*, MI 1317 [1], RMG 61 [2], RMG 29 [3], RMG 91 [4], P 50.2.056−2007 [5], as well as the following terms with respective definitions:
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* Probably, the error of the original. Should read: GOST R 8.563. — Note the manufacturer’s database.

3.1 measurement procedure (MVI): the Set of operations and rules, which provide the results of measurements with the set characteristics of error (uncertainty).

3.2 the intensity of spectral lines: the Power emitted by a unit volume source in a wavelength interval corresponding to the full width of the spectral lines.

3.3 standard sample material (material): Material (substance), one or more properties of which are mounted metrological reasonable procedures, to which was appended a document issued by the competent authority containing the values of these properties, specifying the characteristics of the errors (uncertainties) and a statement of traceability.

3.4 state standard sample: a Standard sample of the material (substances) that are recognized by the Federal body of Executive power of the Russian Federation, carrying out functions in the sphere of technical regulation and Metrology.

3.5 factory standard sample: a Standard sample of the material (substances) that are recognized by management.

3.6 analytical signal: the Signal contains quantitative information about the size, functionally associated with the content item, and recorded in the analysis.

3.7 calibration characteristics: Functional dependence of analytical signal from the content of the element expressed as a formula, graph or table.

3.8 characteristic error of the results of the analysis: limit of the interval in which the measurement error is with confidence probability of 0.95.

3.9 accuracy rate of the results of the analysis: Values of characteristics of the error (uncertainty) set for any result of the analysis obtained in compliance with the requirements and rules of this method in its implementation in a particular laboratory (corresponds to expanded uncertainty with coverage factor 2).

3.10 measurement uncertainty: a Parameter associated with the result of a measurement and characterizes the dispersion of values which can be attributed to the measurand.

3.11 standard uncertainty: Uncertainty of measurement expressed as a standard deviation.

3.12 the expanded uncertainty: the Amount determined by the interval around the expectation of measurements covering a large fraction of distribution of values that could reasonably be attributed to the measurand.

3.13 precision: the Degree of closeness to each other of independent results of measurements obtained in a particular regulated conditions.

3.14 repeatability (precision): Precision under conditions in which the measurement results obtained by one method, using the same equipment, on one surface of the sample in the same laboratory, same operator, and almost at the same time.

3.15 inter-laboratory precision: Precision under conditions in which the measurement results obtained by variation of all the factors shaping the variability in the application of specific techniques in the laboratory.

3.16 reproducibility: Precision under conditions in which the measurement results obtained by one method on identical test items in different laboratories.

3.17 the limit of repeatability (convergence):it is Allowed acceptance probability of 0.95 is the difference between the largest and smallest results of two individual measurements, obtained in conditions of repeatability.

3.18 critical range: Acceptable for the accepted probability of 0.95, the discrepancy between the results of individual measurements, obtained in conditions of repeatability.

3.19 limit intralaboratory precision: Permitted for the acceptance probability of 0.95 discrepancy between the two measurement results obtained in terms of the intralaboratory precision.

3.20 reproducibility limit: the Permissible for the acceptance probability of 0.95 discrepancy between the two analysis results obtained under conditions of reproducibility.

3.21 the ratio of control: a Numeric value that is a criterion for the recognition of the monitored indicator of the quality of the measurement results relevant (or not relevant) requirements.

4 Symbols and abbreviations

This standard applies the following symbols and abbreviations:

WITH a standard sample;

GSO is the state standard sample;

SOP — standard sample of the enterprise;

 — the value of the mass fraction of the element;

 — the limit of repeatability (convergence) measurement results for two parallel definitions;

 — critical range of measurements for three parallel measurements;

 — standard stability control calibration characteristics;

that the standards of accuracy control of measurement results;

limit intralaboratory precision;

 — the limit of reproducibility;

 — the characteristic error of the result of analysis of 0.95;

 — the uncertainty of the measurement result;

 — the expanded uncertainty of the measurement result;

enrolment rate.

5 the essence of the method

The method is based on excitation of atoms of the elements of sample material with the electric discharge, the decomposition of radiation of atoms of elements in the spectrum, measurement of analytical signals proportional to the intensity or the logarithm of the intensity of spectral lines and subsequent determination of mass fractions of elements using the calibration characteristics.

6 Sampling and sample preparation

Sampling and sample preparation — according to GOST 7565. The surface of the sample intended for the sparking, sharpen on the plane. On the surface are not permitted shells, slag inclusions, color tint and other defects.

7 measuring instruments, auxiliary equipment and materials

When performing measurements using the following measuring instruments and other technical means:

— atomic-emission spectral installation of individual calibration with photoelectric registration of spectrum for the analysis of monolithic steel specimens regardless of the method of excitation spectrum;

— Steel according to GOST 8.315 with the certified value of the mass fraction of elements in accordance with section 1 of this standard with an accuracy of less than ±0.3 mm (in special cases ±0,5) value accuracy specifications of the methodology;

abrasive — cutting machines;

— grinding and polishing machines;

— cutting wheels according to GOST 21963;

— grinding wheels for grinding GOST R 52781;

— sandpaper sanding paper according to GOST 6456;

— argon gas of the highest grade according to GOST 10157.

In the case of vacuum atomic-emission spectral units use permanent electrodes are rods of silver, copper and tungsten with a diameter of from 4 to 6 mm or a tungsten wire with a diameter of 1 to 2 mm, length not less than 50 mm in accordance with the manual.

Air for atomic emission spectral installations using copper bars marks M00, M1, M2 according to GOST 859 and coal terminals brand C3 with a diameter of 6 mm and a length of not less than 50 mm.

Allowed the use of other measuring instruments, auxiliary equipment and materials ensuring the accuracy of the analysis required by this standard.

8 Algorithm measurement

The execution of measurements involves the spectral training set to work, selection of conditions for analysis of samples of steel, the construction of calibration characteristics, analysis.

9 Operation preparation for measurements

9.1 Preparing the system and the measurements carried out in accordance with the maintenance manual and operation of the facility.

9.2 conditions of analysis of atomic emission spectral units are given in Appendix B (tables B. 1, B. 2).

9.3 the wavelengths of spectral lines and ranges of values of mass fractions of elements are given in Appendix B (table B. 3).

9.4 Primary spectral calibration of the setup is carried out experimentally in the implementation of MWI with the use of SLAs, SOPS or similar samples analyzed by standardized or certified methods.

9.5 To obtain the calibration characteristics it is recommended to use at least three samples.

9.6 the Procedure of calibration is performed in accordance with the instructions for the software of atomic-emission spectral setup.

9.7 Calibration characteristics are used to determine the mass fraction of the controlled elements, either directly or with the influence of the chemical composition and physico-chemical properties of the object.

9.8 When using the spectral installations that do not have the software, the calibration is carried out in accordance with the manual. Calibration characteristics expressed in the form of a graph, formula or table.

9.9 When working on atomic emission spectral units needed daily, and after repairs, check the position of the calibration characteristics (drift correction). The procedure for drift correction should be regulated by the manual of the device or other documents.

9.10 introduction to the measurement results of the amendments, taking into account the influence of the chemical composition, structure and other physico-chemical parameters of the analyzed samples.

10 the stability Control calibration parameters

10.1 stability Control calibration parameters is carried out at least once per shift for upper and lower limits of the measuring range with or WITH homogeneous samples. Allowed to control only the upper (lower) limit or mid-range.

For (samples) carry out two measurements in terms of repeatability and test acceptability of the results of measurements in accordance with paragraph 10.2.

10.2 If the results are acceptable, calculate the mean value and the difference according to the formula

, (1)

where the value of the mass fraction in THE (sample) obtained when building calibration characteristics.

10.3 If exceed the permissible value in accordance with Appendix A, table A. 1, the measurement is repeated. If duplicate measurements exceed the permissible value, carry out the recovery of the calibration characteristics.

11 performance measurement, verification of acceptability of results

11.1 Perform two measurements of the mass fraction of elements in the sample under conditions of repeatability.

11.2 Absolute difference obtained under paragraph 11.1 of the measurement results is compared with the limit of recurrence in accordance with Appendix A, table A. 1.

If the absolute difference between the two measurements does not exceed the limit

, (2)

results recognize acceptable and as finally given result should be the arithmetic mean value of two measurements.

11.3 If condition (2) fails, conduct another measurement and calculate the difference between the maximum () and minimum () of the measurement results. The obtained value is compared with the critical range defined by the formula (3), in accordance with Appendix A, table A. 1.

If the absolute difference between the results of the three measurements does not exceed the limit defined by the formula (3),

, (3)

where is the maximum value of the three measurements

 — the minimum value of the three measurements

the results recognize acceptable and as finally given result should be the arithmetic mean value of three measurements.

11.4 If the condition (3) is not performed, the measurement results are arranged in series of ascending () and as a final result take the value of the second smallest measurement (), followed by identifying and eliminating the reasons of high scatter of results.

11.5 Numerical value of the result of the analysis must end with the same number of discharges, and the corresponding value characteristics error of the result of the analysis is given in Appendix A, table A. 1.

12 quality Control of measurement results

12.1 Control of correctness of analysis results

12.1.1 Control of the correctness is carried out by selective comparison of the results of spectral analysis of samples results of chemical analysis performed on standardized or certified methods. The standard controls presented in Appendix A, table A. 1.

12.1.2 In case of impossibility of implementation of paragraph 12.1.1 in full methods of chemical analysis can be performed control of the correctness of the measurement results of reproduction of the certified values of mass fractions of elements in GSO or SOP. The standard controls presented in Appendix A, table A. 1.

12.1.3 the Number of results in the control of accuracy must be not less than 0.3% of the total number of definitions for a controlled period.

12.1.4 measurement Accuracy is considered satisfactory if the number of mismatches results in excess of the allowable value or is not more than 5% of the number of monitored results.

12.2 Control intralaboratory precision of the measurement results

12.2.1 order to control intralaboratory precision results of measurements performed to determine the mass percentage of the elements in the previously analyzed samples, changing the influencing factors (different times, different operators, etc.).

12.2.2 the Number of repetitions should be at least 0.3% of the total number of measurements over a controlled period.

12.2.3 inter-Laboratory precision of the measurement results is considered satisfactory if the number of discrepancies between the results of primary and repeated tests exceeding the permissible value given in Annex A, table A. 1 is not more than 5% of the number of monitored results.

12.3 subject to the conditions of sections 11 and 12 feature error (extended uncertainty) of measurement result shall not exceed the values given in Appendix A, table A. 1.

13 Making measurements

The results of the measurements draw up a Protocol, a journal entry or record in electronic media.

Together with the results of measurements represent the characteristics of error (extended uncertainty ) and are in the form of

, (4)

where is the result of the measurement item in the sample;

 — value characteristics error of the measurement result (an expanded uncertainty).

Note — Instead of specifying the characteristics of the error (extended uncertainty) is allowed to accompany the result with reference to this standard.

14 Control the admissibility of the results of measurements obtained under conditions of reproducibility

The results obtained in two laboratories to recognize acceptable if the absolute difference between them does not exceed the limit of reproducibility , given in Appendix A, table A. 1.

15 the Requirements for staff qualifications

Performance measurement can produce operator, skilled at working on atomic emission spectral setup.

16 safety Requirements

When performing measurements, observe the following safety requirements:

— electrical safety when working with electrical installations according to GOST 12.1.019 [5];

— organizaciey training working safety according to GOST 12.0.004 [6]*;

— the laboratory must comply with the fire safety requirements according to GOST 12.1.004 [7]* and have fire-extinguishing equipment according to GOST 12.4.009 [8]*;
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* The text of the document matches the original. In the Bibliography document no NTD under these numbers. — Note the manufacturer’s database.

— the regulations on labor protection and industrial safety (Oh & s) operating in the laboratory.

Annex a (mandatory). Values for the limits of repeatability, reproducibility, and standards control

Appendix A
(required)

Table A. 1

Percentage

Appendix B (recommended). The conditions of analysis of atomic emission spectral units are shown in tables B. 1-B. 3

Appendix B
(recommended)

Table B. 1

Table B. 2

Table B. 3

Bibliography