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GOST R ISO 7530-1-2016

GOST R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample

GOST R ISO 7530−1-2016

NATIONAL STANDARD OF THE RUSSIAN FEDERATION

NICKEL ALLOYS

Spectrometric method of atomic absorption in the flame

Part 1

General requirements and dissolution of the analyzed sample

Nickel alloys. Flame atomic absorption spectrometric analysis. Part 1. General requirements and sample dissolution

OKS 77.120.40*

AXTU 0709

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* According to the official website of Rosstandart OKS 77.080.20,

here and further. — Note the manufacturer’s database.

Date of introduction 2016−11−01

Preface

1 PREPARED by Federal state unitary enterprise «Central research Institute of ferrous metallurgy them.And.P.Bardin," on the basis of their own authentic translation into the Russian language of the international standard indicated in paragraph 4

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

3 APPROVED AND put INTO EFFECT by the Federal Agency for technical regulation and Metrology of March 15, 2016 N 145th St

4 this standard is identical to international standard ISO 7530−1:1990* «the Alloys of Nickel. Spectrometric analysis by the method of atomic absorption in the flame. Part 1. General requirements and sample dissolution» (ISO 7530−1:1990 «Nickel alloys — Flame atomic absorption spectrometric analysis — Part 1: General requirements and sample dissolution»).

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* Access to international and foreign documents referred to here and hereinafter, can be obtained by clicking on the link to the site shop.cntd.ru. — Note the manufacturer’s database.

The name of this standard changed with respect to names specified international standard for compliance with GOST R 1.5−2012 (subsection 3.5).

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

5 INTRODUCED FOR THE FIRST TIME

Application rules of this standard are established in GOST R 1.0−2012 (section 8). Information about the changes to this standard is published in the annual (as of January 1 of the current year) reference index «National standards» and the official 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 upcoming issue of 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 (www.gost.ru)

1 Scope

This standard specifies General requirements for the method of atomic absorption in the flame, the preparation and dissolution of the test sample, method of calculation and the methods used to assess the repeatability and reproducibility of the results for individual methods given in the standards of ISO 7530 on control methods Nickel alloys spectrometry of absorption with flame.

2 Normative references

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

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* The table of conformity of national standards international see the link. — Note the manufacturer’s database.

ISO 385−1:1984 laboratory Glassware glass. Burette. Part 1. General requirements. (ISO 385−1:1984, Laboratory glassware — Burettes — Part 1: General requirements) GOST R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample

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GOST R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample Valid ISO 385:2005 «laboratory Glassware glass. Burettes».

ISO 648:1977 laboratory Glassware glass. Pipettes with one mark (ISO 648:1977, Laboratory glassware — One-mark pipettes) GOST R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample

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GOST R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample Valid ISO 648:2008 «laboratory Glassware glass. Pipette with one mark».

ISO 1042:1983 laboratory Glassware glass. Flasks volumetric with one mark (ISO 1042:1983, Laboratory glassware — One-mark volumetric flasks) GOST R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample

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GOST R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample Valid ISO 1042:1998 «oils. Volumetric flask with one mark».

ISO 5725:1986 Precision of test methods. Determination of repeatability and reproducibility of a standard method by interlaboratory tests (ISO 5725:1986, Precision of test methods — Determination of repeatability and reproducibility for a standard test method by inter-laboratory tests) GOST R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample

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GOST R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample Are: ISO 5725−1:1994, ISO 5725−2:1994, ISO 5725−3:1994, ISO 5725−4:1994, ISO 5725−5:1998, ISO 5725−6:1994.

3 the essence of the method

This method is based on dissolving a measured sample in acid, evaporating the excess acid and dissolving the salts, and adding, if necessary, ionization buffer for suppression of ionization and diluted to the desired volume. Obtained the analyzed solution, if necessary after secondary dilution is sprayed in air-acetylene or denitrated-acetylene flame atomic absorption spectrometer. Perform a spectrometric measurement of the absorption at the resonance line spectrum of the element and compare with the value of the absorbance of the calibration solutions of the same element.

4 Reagents

In the analysis, unless otherwise stated, use only reagents established analytical grade and only distilled water or water of equivalent purity.

4.1 high-purity metals with a mass fraction of metal not less than 99.9%.

4.2 Nitric acid (HNOГОСТ R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and the dissolution test sample), GOST R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample=1,41 g/smost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample.

4.3 Nitric acid (HNOГОСТ R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and the dissolution test sample), GOST R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample=1,41 g/smost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of a test sample diluted 1:1.

4.4 Hydrochloric acid (HCI), GOST R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample=1.18 g/smost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample.

4.5 Hydrochloric acid (HCI), GOST R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample=1.18 g/smost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of a test sample diluted 1:1.

4.6 Mixture of nitric and hydrochloric acids

Carefully mix 1 part of nitric acid (4.2) and 3 parts of hydrochloric acid (4.4). This mixture should be prepared just prior to use.

Warning — This mixture of acids is unstable and is an aggressive solvent. During its preparation at the time of mixing is released poisonous gas (chlorine). Mix the acid in a fume hood, the mixture should not be kept in a tightly closed container.

4.7 Standard solutions for calibration graphs, 1 g/dbhost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample of the metal

The solutions were prepared separately for each item according to the series of ISO 7530.

5 Instrument

Use conventional laboratory equipment and the following equipment.

5.1 Atomic absorption spectrometer

5.1.1 Atomic absorption spectrometer used for measurements, should have operational characteristics that ensure the reproduction of the required values of the instrumental parameters is given in Appendix A.

5.1.2 the Instrument shall be fitted with a burner head, suitable for air-acetylene and dinitramide-acetylene flame types.

5.1.3 When using single-element lamps hollow cathode or electrodeless discharge lamp of the spectrometer must be operated at the currents recommended by the manufacturer of the device.

5.2 Volumetric glassware

5.2.1 Graded burette with a capacity of 50 smost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of a test sample with a scale division of 0.1 smost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolving a test sample in accordance with ISO 385−1, class A.

5.2.2 Pipette, corresponding to the requirements of ISO 648, class A.

5.2.3 Volumetric flasks, appropriate to the requirements of ISO 1042, class A.

6 Sampling and sample preparation

6.1 Sampling and preparation of laboratory samples and perform the standard agreed-upon methods or, in case of disagreement, to the appropriate standard.

6.2 laboratory sample is Typically prepared by milling or drilling samples, and further sample preparation is required.

6.3 If there is an assumption about the contamination of laboratory samples with oil or grease left in the process of milling or drilling sample, the sample should be cleaned by washing in ultra-pure acetone, and then air dry.

6.4 laboratory If the sample contains particles or pieces of material with widely varying sizes, sample preparation can be carried out with a file.

7 Method

7.1 Preparation of the test solution. General method

7.1.1 Select, to the nearest 0.001 g, weighed sample mass of 1.00 g and place it in a clean, untreated glass with a capacity of 600 smost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample. Add 20 smost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of a test sample of a mixture of nitric and hydrochloric acids (4.6). Heated at a temperature sufficient to initiate dissolution and to maintain the reaction until complete dissolution of the sample. For insoluble alloys may require additional variation in the acid mixture. To do this, in a glass dissolve the suspension was further added in portions of 1 simhost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of a test sample with hydrochloric acid (4.4) and heating was continued until complete dissolution of the sample.

7.1.2 At weak heating, the solution was evaporated to dryness, without sintering. Cool to approximately 50 °C, add 25 smost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of a test sample of hydrochloric acid (4.4) and repeat the evaporation.

7.1.3 Cool the contents of the beaker to about 50 °C, add 5 smost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of a test sample of hydrochloric acid (4.4) and 20 smost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample of water, then heated to dissolve the salts.

7.1.4 continue to perform operations in accordance with other standards of ISO 7530.

Notes

1 Certain alloys with high copper content can be dissolved in nitric acid, diluted 1:1. For some alloys, the more preferable mixture of acids, containing 30 smost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of a test sample of hydrochloric acid and 2 simhost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of a test sample of nitric acid.

2 This General method of dissolving sample of the alloy can be changed in accordance with the established procedure in other standards of ISO 7530.

3 If the presumably inhomogeneous sample, it is possible to select for analysis from 10 to 50 g. However, aliquota part taken from such a solution should correspond to 1 g of sample and the analysis must be performed in accordance with this procedure.

7.2 Blank

Blank perform a parallel definition for the same method using the same quantities of all reagents, with the exception of the designated component.

7.3 Preparation of calibration solutions

Calibration solutions prepared in accordance with other standards of ISO 7530.

7.4 Calibration and determination

7.4.1 Atomic absorption measurements

7.4.1.1 Spectral (resonance) lines used to determine the particular element, specified in the relevant standard of ISO 7530.

7.4.1.2 Necessary instrumental parameters should be consistent with the recommendations of the manufacturers of the devices. Light the burner and spray water into the flame before the establishment of thermal equilibrium. The characteristics of the flame will change depending on the analyzed element. Set the zero reading of the spectrometer.

7.4.1.3 it is Desirable that the device meets the requirements of the instrumental parameters is given in Appendix A. the Optimal setting of parameters controlled may vary for different types of devices. For the definition of indications may be used scale of the extension.

7.4.1.4 it is Desirable that the calibration solutions and analyzed (e) solution (s) did not differ in temperature more than 1 °C.

7.4.1.5 Zero reading spectrometer installed by water spraying.

7.4.1.6 Atomize the calibration solutions and analyzed (e) solution (s), note the reading of the spectrometer, determining the approximate concentration of the element in the analyzed solution.

7.4.1.7 Sprayed water to return the readings of the spectrometer to the starting position. If necessary, set the zero reading.

7.4.1.8 Spray calibration and analyze the solutions in order of increasing analytical signal, starting from the zero solution. When you get a stable signal value and the recorded indication. Wash the system, spraying water between each (to be analyzed or the calibration) solution.

7.4.1.9 Repeat the measurement of a complete set of calibration solutions and analyzed at least two times and record the data.

Warning — the manufacturer’s Recommendations to be implemented, special attention should be paid to the following safety rules:

a) to take into account the explosive nature of acetylene and follow the rules for the work with acetylene;

b) to protect operator’s eyes from UV radiation by using filters;

c) periodically clean the burner head of carbon, because when poorly purified the burner may occur overshoot of the flame;

d) check the filling liquid syphon with water;

e) spraying with distilled water in between spraying the analyzed solutions, blank solutions experience and/or calibration.

7.4.2 Construction of calibration graphs

On the chart is applied to the data of the average values of the readings of absorbance relative to the concentration of analyte in the calibration solutions for each series of measurements. Perform calculations as specified in section 8.

Note — Some devices may show the results of the determination directly in the concentration units of analyte. When plotted in the coordinates: the analytical signal is the concentration you should verify the accuracy of the readings.

7.5 the Number of definitions

Perform at least two definitions.

8 Processing of results

8.1 Calculation of results

8.1.1 Determine the concentration of analyte in the sample solution according to the relevant calibration chart was of the readings (measurements of each of the three series).

8.1.2 calculate the analyte content, % mass, in the analyzed sample according to the following formula

GOST R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample (1)

where is the GOST R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample, the concentration of the analyte (after deduction of blank values) in the sample solution, mg/dbhost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample;

V — volume of initial solution, smost R ISO 7530−1-2016 Nickel Alloys. Spectrometric method of atomic absorption in the flame. Part 1. General requirements and dissolution of the analyzed sample

F — the dilution factor upon repeated dilution;

m — mass of sample, g.

Note — the Average values of the results of the three readings taken for a single result. Three results give an idea of the precision of atomic absorption measurements.

8.2 Precision

8.2.1 Laboratory tests

Methods described in other standards of ISO 7530, were tested in the framework of interlaboratory tests. The samples were analyzed twice on different days.

8.2.2 Statistical analysis

8.2.2.1 Results obtained during the interlaboratory test were processed in accordance with the requirements of ISO 5725. Data were checked for homogeneity using the criteria of Cochran and Dixon according to the method of assessment described in ISO 5725.

8.2.2.2 the Principle of Cochran criterion is the comparison of several dispersions for evaluation of the homogeneity of the results submitted by a number of sample cases and their suitability for cooperative aggregation. If all sample variance meet the requirements of the Cochran criterion, they can be considered estimates of the same underlying population. The Dixon criterion is used if the mean value of the results obtained in one laboratory is significantly different from the values obtained in other laboratories. Check according to the criteria of Cochran and Dixon used with a confidence level of 95%.

8.2.2.3 Repeatability and reproducibility were calculated in accordance with the requirements of the standard ISO 5725 with a confidence level of 95%. The results of the statistical analysis that includes values for intralaboratory and interlaboratory standard deviations, are presented for each item in the relevant standard methods for monitoring of Nickel alloys by spectrometry of atomic absorption in the flame.

9 test report

The test report shall contain:

a) a reference to the method used;

b) test results;

c) the number of independent repeated definitions;

d) unusual features of the operations indicated to perform the analysis;

e) any operation not included in the relevant part of standard ISO 7530, or any optional operations that may affect the test results.

Annex a (mandatory). Check the instrumental parameters of the spectrometer

Appendix A

(required)

A. 1 Introduction

The operating characteristics of atomic absorption spectrometers of the same or different manufacturers may vary. Therefore, it is necessary to establish that the characteristics of a particular device meets specific requirements before using it for measurements of absorption in the methods regulated in the standards of ISO 7530.

A. 2 Initial adjustment of the device

A. 2.1 Atomic absorption spectrometer must be equipped with odnoschelevye burner for air-acetylene or denitrated-acetylene mixture, providing a laminar flow of fuel in accordance with the manufacturer’s instructions.

A. 2.2 as the excitation source for the designated item, you use one-element lamps with hollow cathode single-element electrodeless discharge or other suitable single-element lamp. Spend the alignment of the lamps in accordance with manufacturer’s recommendations.

Note — the Use of multielement lamps, in General, is not recommended, although some lamps with cathodes from binary alloys give a more stable radiation than single-element lamps.

A. 2.3 set Fire to flames and spray water to establish thermal equilibrium.

A. 2.4 Spray a medium solution from the calibration series of solutions and carry out tuning of the instrument to obtain the optimal values of the analytical signal. Use a specific wavelength recommended for the designated element in the relevant standard of ISO 7530, the slit width or bandwidth set based on the manufacturer’s recommendations for each of the element. If necessary, use the scale of the expansion.

A. 2.5 wash the system of the burner, spraying hydrochloric acid, diluted 1:19, set the readings of the spectrometer to zero and proceed to check the instrumental parameters, as shown in A. 3.2-A. 3.4.

A. 3 Verification of tool settings

A. 3.1 performance Verification solutions

The standards of ISO 7530 describes the construction of the calibration graphs, which are usually built using a series of five calibration solutions with the inclusion of the zero solution. To check the instrumental parameters you choose two pairs of the calibration solutions covering the upper and lower region of calibration curve to the concentration range between the two calibration solutions with a higher concentration was equal to the interval between the reference solution and the calibration solution with the lowest concentration.

A. 3.2 Readability (clarity)

A. 3.2.1 Spray two of the calibration solution with a higher concentration of the element than in the sample solution, record the readings and calculate the difference between the readings.

A. 3.2.2 Divide the resulting difference by 20. The readability of the readings considered acceptable if the result of the division will be no less than the minimum effective interval, which can be read or identify in reading.