GOST 17261-2008

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  ГОСТ 17261-2008

GOST 17261−2008 Zinc. Methods of atomic-emission spectral analysis

GOST 17261−2008

Group B59

INTERSTATE STANDARD

ZINC

Methods of atomic-emission spectral analysis

Zinc. Methods of atomic-emission spectral analysis

ISS 77.120.60

Date of introduction 2016−11−01

Preface

Goals, basic principles and main procedure of works on interstate standardization have been established in GOST 1.0−2015 «interstate standardization system. Basic provisions» and GOST 1.2−2015 «interstate standardization system. Rules of development, adoption, renewal and cancellation"

Data on standard

1 DEVELOPED by the Interstate technical Committee for standardization MTK 504 «Zinc, lead», a subsidiary of the state enterprise «Eastern scientific-research mining-metallurgical Institute of nonferrous metals» (DGP «VNIItsvetmet») of the Republic of Kazakhstan and Republican state enterprise «Kazakhstan Institute of standardization and certification"

2 INTRODUCED by Committee on technical regulation and Metrology of the Ministry of industry and trade of the Republic of Kazakhstan

3 ACCEPTED by the Interstate Council for standardization, Metrology and certification by correspondence (minutes dated 30 December 2008, N 35)

The adoption voted:

4 by Order of the Federal Agency for technical regulation and Metrology of April 7, 2016 245 N-St inter-state standard GOST 17261−2008 introduced as a national standard of the Russian Federation from November 1, 2016.

5 REPLACE GOST 17261−77


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 (www.gost.ru)

1 Scope

This standard applies to zinc and establishes methods of atomic-emission spectral analysis with the excitation spectrum of the arc discharge and inductively coupled plasma for the determination of iron, cadmium, copper, tin, lead and antimony in zinc brands CV0, CV, C0A, C0, C1, C2, C3, aluminum zinc brands CV0, CV, CSC, C0, C1, C2 according to GOST 3640 in the following range mass fraction, %:

2 Normative references

This standard uses the regulatory references to the following international 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 12.1.004−91 System safety standards. Fire safety. General requirements

GOST 12.1.005−88 standards System of labor safety. General hygiene requirements for working zone air

GOST 12.1.007−76 System of standards of occupational safety. Harmful substances. Classification and General safety requirements

GOST 12.1.016−79 System of standards of occupational safety. The air of the working area. Requirements for measurement techniques of concentrations of harmful substances

GOST 12.1.019−79 System of standards of occupational safety. Electrical safety. General requirements and nomenclature of types of protection

GOST 12.1.030−81 System of standards of occupational safety. Electrical safety. Protective grounding, neutral earthing

GOST 12.2.007.0−75 System safety standards. Products electrical. General safety requirements

GOST 12.3.019−80 standards System of labor safety. Test and measurement electrical. General safety requirements

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

GOST 12.4.021−75 System safety standards. System ventilation. General requirements

GOST 195−77 Reagents. Sodium sanitarily. Specifications

GOST 859−2001 Copper. Brand

GOST 860−75 Tin. Specifications

GOST 1089−82 Antimony. Specifications

GOST 1465−80 Files. Specifications

GOST 1467−93 Cadmium. Specifications

GOST 1770−74 laboratory Glassware measuring glass. Cylinders, beakers, flasks, test tubes. General specifications

GOST 2424−83 grinding wheels. Specifications

GOST 3640−94 Zinc. Specifications

GOST 3778−98 Lead. Specifications

GOST 4160−74 Reagents. Potassium bromide. Specifications

GOST 4221−76 Reagents. Potassium carbonate. Specifications

GOST ISO 5725−1-2003* Accuracy (trueness and precision) of methods and measurement results. Part 1. General provisions and definitions
________________
* 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.


GOST ISO 5725−3-2003 Accuracy (trueness and precision) of methods and measurement results. Part 3. Intermediate indicators the precision of a standard measurement method

GOST ISO 5725−6-2003 Accuracy (trueness and precision) of methods and measurement results. Part 6. The use of precision values in practice

GOST 5817−77 Reagents. Acid wine. Specifications

GOST 6709−72 distilled Water. Specifications

GOST 9849−86 iron Powder. Specifications

GOST 10157−79 Argon gaseous and liquid. Specifications

GOST 11125−84 nitric Acid of high purity. Specifications

GOST 19627−74 Hydroquinone (paradoxians). Specifications

GOST 22180−76 Reagents. Oxalic acid. Specifications

GOST 24104−2001 laboratory Scales. General technical requirements

GOST 25086−87 non-ferrous metals and their alloys. General requirements for methods of analysis

GOST 25336−82 Glassware and equipment laboratory glass. The types, basic parameters and dimensions

GOST 25664−83 Metol (4-methylaminophenol sulfate). Specifications

GOST 28165−89 Instruments and apparatus laboratory glass. The distiller. The evaporators. The installation of distillation. General technical requirements

GOST 29227−91 (ISO 835−1-81) oils. Pipettes are graduated. Part 1. General requirements

GOST 30331.3−95 (IEC 364−4-41−92)/GOST R 50571.3−94 (IEC 364−4-41−92) electrical Installations of buildings. Part 4. Requirements for security. Protection against electric shock

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 Terms and definitions

This standard applies the terminology according to GOST ISO 5725−1 and recommendations [1], as well as the following terms with respective definitions:

3.1 accuracy: the Degree of closeness of measurement results to the accepted reference value. The present includes a combination of random components of error (precision) and a common systematic error (correctness).

3.2 the accepted reference value: a Value that serves as a consensus for comparison with the test result. For the purposes of this standard certified values of standard samples (CO) coincide with the notion of «accepted reference value».

3.3 systematic error: the difference between the expectation of test results and the true value*
_______________
* In this standard, the concept of «true value» coincides with the concept «adopted by reference certified value».

3.4 correctness: the Degree of closeness of the average value obtained on the basis of a large series of test results to the accepted reference value*.
_______________
* In this standard, the concept of «accepted reference value» coincides with the concept of «certified value of the standard designs».

3.5 precision: the Degree of closeness to each other independent of the test results obtained in specific regulated conditions. Extreme cases of such conditions are conditions of repeatability and reproducibility conditions.

3.6 repeatability of the analysis: The degree of closeness to each other independent test results obtained under conditions of repeatability with the same method on identical objects in the same laboratory by the same operator using the same equipment within a short period of time.

3.7 the limit of repeatability : a value Such that the absolute difference between two test results obtained under repeatability would be less than or equal to him with a probability of 95%.

3.8 repeatability of results of the analysis: the Degree of closeness to each other independent test results obtained under reproducibility by the same method on identical objects in different laboratories by different operators using different equipment.

3.9 limit of repeatability : a value Such that the absolute difference between two test results obtained under reproducibility would be less than or equal to him with a probability of 95%.

4 General requirements

4.1 General requirements for methods of analysis GOST 25086.

4.2 the analysis used a measuring laboratory glassware is not below 2nd class of accuracy.

4.3 Sampling is carried out according to GOST 3640. Samples prepared in the form of cast electrodes of round crosssection with a diameter of 10 mm and a length of 50−100 mm.

From the zinc ingots average sample is taken in the form of chips, is melted in a pre-heated crucible at a temperature of 430°C-450°C and cast into a mold in the form of electrodes of specified diameter or other dimension, depending on the size of the used standard samples.

4.4 Mass fraction of iron, cadmium, copper, tin, lead, antimony and aluminium is determined in parallel on two batches.

4.5 the differences in the assessment of the quality of zinc used atomic emission method of analysis with the excitation spectrum in the arc source.

5 safety Requirements and environmental protection

5.1 the analysis of zinc, all work in the laboratory should be carried out on appliances and electrical installations, the relevant rules [2] and requirements of GOST 12.2.007.0.

5.2 When using electrical appliances and electrical installations in the process of analysis of zinc should comply with the requirements of GOST 12.3.019, GOST 30331.3, rules [3] and [4].

5.3 All equipment and installations should be equipped with devices for grounding corresponding to GOST 12.2.007.0 and GOST 12.1.030.

5.4 Analysis carried out in rooms equipped with General dilution ventilation system according to GOST 12.4.021.

5.5 To prevent contact with the air, ozone, nitrogen oxides, aerosols of metals and their oxides, metals emitted in the sources of spectra excitation and harmful effects on the body working, in quantities exceeding maximum permissible concentration according to GOST 12.1.005, and also for protection from electromagnetic radiation and prevent sunburn by ultraviolet rays, each a source of excitation spectra should be placed inside of the device, equipped with an integrated exhaust air inlet and the protective screen according to GOST 12.1.019.

5.6 the analysis of zinc use of chemicals with harmful effects on the human body. When working with chemicals, you must follow the safety requirements outlined in the regulations for their manufacture and use.

5.7 the Content of harmful substances in working area air (acid vapors, aerosols, chemicals and other substances) generated in the course of the analysis shall not exceed the maximum allowable concentrations according to GOST 12.1.005.

5.8 Monitoring of content of harmful substances in the air of working zone — according to GOST 12.1.005, GOST 12.1.007, GOST 12.1.016.

5.9 the use and operation of compressed, liquefied and dissolved gases in process analysis is required to observe the rules of safe operation of vessels working under pressure, approved by the relevant national authorities.

5.10 When performing analysis of zinc is necessary to observe the basic rules of safe work in chemical laboratories* approved according to established procedure.
________________
* On the territory of the Russian Federation the document is not valid. Acts PND f 12.13.1−03. — Note the manufacturer’s database.

5.11 the Disposal, deactivation and destruction of hazardous wastes from the tests should be carried out in accordance with the sanitary rules and norms [5].

5.12 To ensure that fire safety should comply with the requirements of GOST 12.1.004. The laboratory room must have a means of extinguishing according to GOST 12.4.009.

5.13 laboratory Personnel must be provided with premises and devices according to the construction norms and rules [6] for the group the production processes of IlIa.

5.14 laboratory Personnel must be provided with workwear and other PPE in accordance with standard industry regulations of free issue of workwear, footwear and protective equipment to workers and employees of enterprises, approved in the prescribed manner.

6 the Method of atomic-emission spectral analysis with the excitation spectrum of the arc discharge

6.1 the essence of the method

The basis for determining the mass fraction of components in the zinc on the method of «three standards» with the excitation spectrum in the arc of an alternating current power of 5 A.

6.2 measuring instruments, materials, reagents and solutions

The quartz spectrograph medium dispersion, allowing for a single exposure to the range of 230 to 380 nm, or a diffractive-type DFS-8 with three-lens Achromat illumination system of the slit and with the three-step attenuator. Allowed to use devices with photoelectric registration of spectrum.

The generator is activated the arc AC.

Microphotometer of any type, allowing to measure the density of the blackening of analytical lines.

Laboratory scales according to GOST 24104.

Laboratory electric furnace, mine for alloying of zinc shavings, allowing the temperature to 500 °C.

Mold for casting electrodes of round crosssection with a diameter of 10 mm and a length of 50−100 mm, or other sizes, made of cast iron, steel and graphite.

Crucibles, graphite, graphite-chamotte and chamotte.

Files N 3 and N 4 according to GOST 1465.

Grinding wheel rotating according to GOST 2424 or machine KP-35 for sharpening electrodes.

Glasses with a capacity of 1000 cmaccording to GOST 25336.

Spectrographic plates of the type II sensitivity 13−15 units or type of ES sensitivity 10, SFC-02, the SFC-03, NT-2SV.

Distilled water according to GOST 6709.

Developer metalhydrogen: mix solutions 1 and 2 in the ratio 1:2.

Solution 1: 60 g potassium carbonate according to GOST 4221 dissolved in 1 DMof water.

A solution of 2: 6 g metol according to GOST 25664,15 g of hydroquinone according to GOST 19627, 90 g of anhydrous sodium semitecolo according to GOST 195, 6 g of potassium bromide according to GOST 4160 dissolved in 2 DMof water.

Allowed to use other contrast-working developers, the composition of which is specified in the normative documents on fabrication.

Fixer is acidic.

Standard samples of composition of zinc, corresponding to requirements of GOST 8.315.

Allowed to use other equipment and reagents from the technical and metrological characteristics not worse the specified.

6.3 analysis

6.3.1 Sample and standard samples, having the form of electrodes, sharpen on the «roof» (sharpened on two sides under an angle of 45° with the subsequent sharpening of the upper part of the electrode on the horizontal rectangular area with a width of 2−2,5 mm) and strengthen the tripod so to avoid shielding of the discharge. Allowed the sharpening of both electrodes on the hemisphere or on the lower plane and upper hemisphere.

When performing analysis on the instruments with photoelectric registration of spectrum allowed the use of samples, standard samples of a different shape and a different size.

On the end surface of electrodes should not be visible to the eye scratches, pits and other defects.

The distance between the electrodes is 2−3 mm.

The source of spectra excitation — arc alternating current power of 5 A.

6.3.2 Spectra photographed on a quartz spectrograph medium dispersion or diffraction-type DFS-8 (the 600 lines/mm). The width of the slit of a spectrograph — 0,015−0,020 mm front gap is installed a three-tier reliever. Are being used or other illumination system of the slit. Intermediate diaphragm — round.

When using devices with photoelectric registration of spectrum, you must first choose the optimal conditions of excitation of spectra, allowing to obtain the necessary sensitivity and accuracy of analysis results.

The exposure time is 20−40 s depending on the sensitivity of the photographic plates.

To determine the mass fraction of components in zinc uses pairs of lines shown in table 1.


Table 1

6.4 Processing of results

6.4.1 two spectrum of standard samples and four samples of the spectrum photographed on the same photographic plate. With microphotometer measure the blackening of analytical lines of the designated component and line comparison and calculate the difference . The results of the photometry of the standard samples to build calibration graphs for each component you define in the coordinates: .

While the axis of ordinate delay difference pucherani line components and comparison lines, and on the x — axis is the logarithms of the concentrations of the respective components in the standard samples.

According to calculated values

and

according to the schedule determine the mass fraction of components in the sample. Get the results of two parallel measurements.

Allowed for constructing the calibration graphs to use semilog paper to plot data in coordinates:

,

where the readings of the output of the measuring device, is proportional to the logarithm of the intensity of the lines defined by the component, and lines of comparison;

 — mass fraction of components in the reference sample.

6.4.2 the result of the analysis take the average of results of two parallel measurements obtained on the same photographic plate on the two spectrograms each, with photographic registration of spectrum and the average of results of two parallel measurements (three measurements each) and (2) with photoelectric registration, if the difference between them does not exceed the limit of repeatability in table 2.

6.4.3 Upon receipt of the results of parallel measurements with a discrepancy of more than permitted analysis of samples is repeated.

6.4.4. If the discrepancy between the results of parallel measurements once again exceeds the limit value of the frequency of occurrence , studying the causes of the deviations from the technical point of view. If you need to obtain some reasonable values and in case of exceeding the limit of repeatability, act in accordance with GOST ISO 5725−6 (subsection 5.2).

6.4.5 the discrepancy between the analysis results obtained in two laboratories (2), shall not exceed the limit of reproducibility . If this condition is acceptable both analysis and as a final result of using their overall average. The value of the reproducibility are shown in table 2.

If you exceed the limit of reproducibility study of the causes of the deviations and use methods for assessing the acceptability of the results of the analysis according to GOST ISO 5725−6 (paragraphs 5.3.2−5.3.4).

6.4.6 the results of the analysis represent a numeric value, which must end with a digit of the same category as the numeric value of the error guaranteed by the method of analysis specified in this standard (table 2).

6.5 Characteristics of error analysis

This method provides obtaining of analysis results with an error, the value of which does not exceed the values given in table 2.


Table 2 — Values of parameters and limits of repeatability, reproducibility, and error (at confidence probability of 0.95)