By visiting this site, you accept the use of cookies. More about our cookie policy.

GOST 20996.0-2014

GOST 33729-2016 GOST 20996.3-2016 GOST 31921-2012 GOST 33730-2016 GOST 12342-2015 GOST 19738-2015 GOST 28595-2015 GOST 28058-2015 GOST 20996.11-2015 GOST 9816.5-2014 GOST 20996.12-2014 GOST 20996.7-2014 GOST P 56306-2014 GOST P 56308-2014 GOST 20996.1-2014 GOST 20996.2-2014 GOST 20996.0-2014 GOST 16273.1-2014 GOST 9816.0-2014 GOST 9816.4-2014 GOST P 56142-2014 STATE STANDARD P 54493-2011 GOST 13498-2010 STATE STANDARD P 54335-2011 GOST 13462-2010 STATE STANDARD P 54313-2011 GOST P 53372-2009 GOST P 53197-2008 GOST P 53196-2008 GOST P 52955-2008 GOST P 50429.9-92 GOST 6836-2002 GOST 6835-2002 GOST 18337-95 GOST 13637.9-93 GOST 13637.8-93 GOST 13637.7-93 GOST 13637.6-93 GOST 13637.5-93 GOST 13637.4-93 GOST 13637.3-93 GOST 13637.2-93 GOST 13637.1-93 GOST 13637.0-93 STATE STANDARD 13099-2006 GOST 13098-2006 GOST 10297-94 GOST 12562.1-82 GOST 12564.2-83 GOST 16321.2-70 GOST 4658-73 GOST 12227.1-76 GOST 16274.0-77 GOST 16274.1-77 GOST 22519.5-77 GOST 22720.4-77 GOST 22519.4-77 GOST 22720.2-77 GOST 22519.6-77 GOST 13462-79 GOST 23862.24-79 GOST 23862.35-79 GOST 23862.15-79 GOST 23862.29-79 GOST 24392-80 GOST 20997.5-81 GOST 24977.1-81 GOST 25278.8-82 GOST 20996.11-82 GOST 25278.5-82 GOST 1367.7-83 GOST 26239.9-84 GOST 26473.1-85 GOST 16273.1-85 GOST 26473.2-85 GOST 26473.6-85 GOST 25278.15-87 GOST 12223.1-76 GOST 12645.7-77 GOST 12645.1-77 GOST 12645.6-77 GOST 22720.3-77 GOST 12645.4-77 GOST 22519.7-77 GOST 22519.2-77 GOST 22519.0-77 GOST 12645.5-77 GOST 22517-77 GOST 12645.2-77 GOST 16274.9-77 GOST 16274.5-77 GOST 22720.0-77 GOST 22519.3-77 GOST 12560.1-78 GOST 12558.1-78 GOST 12561.2-78 GOST 12228.2-78 GOST 18385.4-79 GOST 23862.30-79 GOST 18385.3-79 GOST 23862.6-79 GOST 23862.0-79 GOST 23685-79 GOST 23862.31-79 GOST 23862.18-79 GOST 23862.7-79 GOST 23862.1-79 GOST 23862.20-79 GOST 23862.26-79 GOST 23862.23-79 GOST 23862.33-79 GOST 23862.10-79 GOST 23862.8-79 GOST 23862.2-79 GOST 23862.9-79 GOST 23862.12-79 GOST 23862.13-79 GOST 23862.14-79 GOST 12225-80 GOST 16099-80 GOST 16153-80 GOST 20997.2-81 GOST 20997.3-81 GOST 24977.2-81 GOST 24977.3-81 GOST 20996.4-82 GOST 14338.2-82 GOST 25278.10-82 GOST 20996.7-82 GOST 25278.4-82 GOST 12556.1-82 GOST 14339.1-82 GOST 25278.9-82 GOST 25278.1-82 GOST 20996.9-82 GOST 12554.1-83 GOST 1367.4-83 GOST 12555.1-83 GOST 1367.6-83 GOST 1367.3-83 GOST 1367.9-83 GOST 1367.10-83 GOST 12554.2-83 GOST 26239.4-84 GOST 9816.2-84 GOST 26473.9-85 GOST 26473.0-85 GOST 12645.11-86 GOST 12645.12-86 GOST 8775.3-87 GOST 27973.0-88 GOST 18904.8-89 GOST 18904.6-89 GOST 18385.0-89 GOST 14339.5-91 GOST 14339.3-91 GOST 29103-91 GOST 16321.1-70 GOST 16883.2-71 GOST 16882.1-71 GOST 12223.0-76 GOST 12552.2-77 GOST 12645.3-77 GOST 16274.2-77 GOST 16274.10-77 GOST 12552.1-77 GOST 22720.1-77 GOST 16274.4-77 GOST 16274.7-77 GOST 12228.1-78 GOST 12561.1-78 GOST 12558.2-78 GOST 12224.1-78 GOST 23862.22-79 GOST 23862.21-79 GOST 23687.2-79 GOST 23862.25-79 GOST 23862.19-79 GOST 23862.4-79 GOST 18385.1-79 GOST 23687.1-79 GOST 23862.34-79 GOST 23862.17-79 GOST 23862.27-79 GOST 17614-80 GOST 12340-81 GOST 31291-2005 GOST 20997.1-81 GOST 20997.4-81 GOST 20996.2-82 GOST 12551.2-82 GOST 12559.1-82 GOST 1089-82 GOST 12550.1-82 GOST 20996.5-82 GOST 20996.3-82 GOST 12550.2-82 GOST 20996.8-82 GOST 14338.4-82 GOST 25278.12-82 GOST 25278.11-82 GOST 12551.1-82 GOST 25278.3-82 GOST 20996.6-82 GOST 25278.6-82 GOST 14338.1-82 GOST 14339.4-82 GOST 20996.10-82 GOST 20996.1-82 GOST 12645.9-83 GOST 12563.2-83 GOST 19709.1-83 GOST 1367.11-83 GOST 1367.0-83 GOST 19709.2-83 GOST 12645.0-83 GOST 12555.2-83 GOST 1367.1-83 GOST 9816.3-84 GOST 9816.4-84 GOST 9816.1-84 GOST 9816.0-84 GOST 26468-85 GOST 26473.11-85 GOST 26473.12-85 GOST 26473.5-85 GOST 26473.7-85 GOST 16273.0-85 GOST 26473.3-85 GOST 26473.8-85 GOST 26473.13-85 GOST 25278.13-87 GOST 25278.14-87 GOST 8775.1-87 GOST 25278.17-87 GOST 18904.1-89 GOST 18904.0-89 STATE STANDARD P 51572-2000 GOST 14316-91 GOST P 51704-2001 GOST 16883.1-71 GOST 16882.2-71 GOST 16883.3-71 GOST 8774-75 GOST 12227.0-76 GOST 12797-77 GOST 16274.3-77 GOST 12553.1-77 GOST 12553.2-77 GOST 16274.6-77 GOST 22519.1-77 GOST 16274.8-77 GOST 12560.2-78 GOST 23862.11-79 GOST 23862.36-79 GOST 23862.3-79 GOST 23862.5-79 GOST 18385.2-79 GOST 23862.28-79 GOST 16100-79 GOST 23862.16-79 GOST 23862.32-79 GOST 20997.0-81 GOST 14339.2-82 GOST 12562.2-82 GOST 25278.7-82 GOST 20996.12-82 GOST 12645.8-82 GOST 20996.0-82 GOST 12556.2-82 GOST 25278.2-82 GOST 12564.1-83 GOST 1367.5-83 GOST 25948-83 GOST 1367.8-83 GOST 1367.2-83 GOST 12563.1-83 GOST 9816.5-84 GOST 26473.4-85 GOST 26473.10-85 GOST 12645.10-86 GOST 8775.2-87 GOST 25278.16-87 GOST 8775.0-87 GOST 8775.4-87 GOST 12645.13-87 GOST 27973.3-88 GOST 27973.1-88 GOST 27973.2-88 GOST 18385.6-89 GOST 18385.7-89 GOST 28058-89 GOST 18385.5-89 GOST 10928-90 GOST 14338.3-91 GOST 10298-79 GOST P 51784-2001 GOST 15527-2004 GOST 28595-90 GOST 28353.1-89 GOST 28353.0-89 GOST 28353.2-89 GOST 28353.3-89 STATE STANDARD P 52599-2006

GOST 20996.0−2014 Selenium technical. General requirements for methods of analysis


GOST 20996.0−2014


INTERSTATE STANDARD

SELENIUM TECHNICAL

General requirements for methods of analysis

Selenium technical. General requirements for methods of analysis


ISS 77.120.99

Date of introduction 2015−09−01


Preface

Goals, basic principles and main procedure of works on interstate standardization have been established in GOST 1.0−92 «interstate standardization system. Basic provisions» and GOST 1.2−2009 «interstate standardization system. Interstate standards, rules and recommendations on interstate standardization. Rules of development, adoption, application, renewal and cancellation"

Data on standard

1 DEVELOPED by the Technical Committee for standardization TC 368 «Copper"

2 recorded by the Interstate technical Committee for standardization MTK 503 «Copper"

3 ACCEPTED by the Interstate Council for standardization, Metrology and certification (Protocol No. 67-P dated 30 may 2014)

The adoption voted:

     
Short name of the country
MK (ISO 3166) 004−97
Country code
MK (ISO 3166) 004−97
Abbreviated name of the national authority for standardization
Armenia
AM The Ministry Of Economic Development Of The Republic Of Armenia
Belarus
BY Gosstandart Of The Republic Of Belarus
Kyrgyzstan
KG Kyrgyzstandard
Russia
EN Rosstandart
Tajikistan
TJ Tajikstandart
Uzbekistan
UZ Uzstandard

4 by Order of the Federal Agency for technical regulation and Metrology dated 26 November 2014 N 1779-St inter-state standard GOST 20996.0−2014 introduced as the national standard of the Russian Federation from September 1, 2015.

5 REPLACE GOST 20996.0−82


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

1 Scope


This standard establishes General requirements for methods of analysis of technical selenium and safety requirements when performing analyses.

2 Normative references


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

GOST 8.010−99* State system for ensuring the uniformity of measurements. The techniques of measurements. The main provisions of the

_____________________

* On the territory of the Russian Federation GOST R 8.563.


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 12.1.005−88 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 12.1.010−76 System of standards of occupational safety. No danger of explosion. General 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 12.1.030−81 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

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

GOST 12.4.011−89 System safety standards. Means of protection of workers. General requirements and classification

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

GOST 12.4.068−79 System of standards of occupational safety. PPE dermatological. Classification and General requirements

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

GOST 4212−76 Reagents. Methods of preparation of solutions for colorimetric and nephelometric analysis

GOST 4517−87 Reagents. Methods for the preparation of accessory reagents and solutions used in the analysis

GOST 4919.1−77 Reagents and highly purified substances. Methods of preparation of solutions of indicators

GOST 4919.2−77 Reagents and highly purified substances. Methods for the preparation of buffer solutions

GOST 6709−72 distilled Water. Specifications

GOST 9147−80 Glassware and equipment lab porcelain. Specifications

GOST 10298−79 Selenium technical. Specifications

GOST 24104−2001* laboratory Scales. General technical requirements

_____________________

* On the territory of the Russian Federation GOST R 53228.


GOST 25086−2011 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 25794.1−83 Reagents. Methods for the preparation of titrated solutions for acid-base titration

GOST 25794.2−83 Reagents. Methods for the preparation of titrated solutions for redox titration

GOST 25794.3−83 Reagents. Methods for the preparation of titrated solutions for titration by precipitation, non-aqueous titration and other methods

GOST 27025−86 Reagents. General instructions for testing

GOST 29169−91 (ISO 648−77) oils. Pipette with one mark

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

GOST 29228−91 (ISO 835−2-81) oils. Pipettes are graduated. Part 2. Pipettes graduated without a set timeout

GOST 29229−91 (ISO 835−3-81) oils. Pipettes are graduated. Part 3. Pipettes graduated with a standby time of 15 s

GOST 29251−91 (ISO 385−1-84) oils. Burette. Part 1. General requirements

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

___________________

** On the territory of the Russian Federation GOST R ISO 5725−1.


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

___________________

*** On the territory of the Russian Federation GOST R ISO 5725−6.


ST SEV 543−77 Number. Record rules and rounding

Note — When using this standard appropriate to test the effect of reference standards for the sign «National standards» drawn up as of January 1 of the current year and related information signs, 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, abbreviations,

3.1 this standard applies the terminology according to GOST 25086, GOST, ISO 5725−1.

3.2 this standard applies the following abbreviations:

ACE — certified mixture;

GC calibration characteristics;

OK — a sample for inspection;

WITH a standard sample;

khch — chemically pure;

C. D. a — net for analysis.

4 General provisions


The measurement procedures used to determine quality indicators technical selenium must comply with the requirements of GOST 8.010, GOST, ISO 5725−1, GOST ISO 5725−6 and of this standard.

5 requirements for the selection and preparation of samples


The selection and preparation of samples technical selenium is carried out according to GOST 10298.

6 Requirements for laboratory buildings

6.1 Analytical work must be performed in special laboratory premises.

6.2 Laboratory premises should be provided with natural iskusstvennoi General dilution ventilation and local ventilation system according to GOST 12.4.021.

The air of the working area and laboratory facilities on the content of harmful substances must meet the requirements of GOST 12.1.005 and GOST 12.1.007.

6.3 desktops, workers and fume hoods, designed to work with flammable and explosive substances must be covered with fireproof materials, but when working with acids, alkalis and other chemically active substances — materials resistant to their effects.

6.4 Coverage of laboratory facilities must conform to [1].

6.5 In the workplace when performing the measurement process when working with solutions, weighing samples, conducting operations on the filter setting of the mass concentration of solutions should be ensured normal conditions, corresponding to sanitary norms [2].

7 Requirements for measuring instruments, auxiliary equipment, materials

7.1 When measured use laboratory scales according to GOST 24104. The class of accuracy of scales must be specified in the measurement technique.

The mass of test portions analyzed samples of substances for the preparation of solutions of known concentration, bulk precipitation gravimetric method of measurement is determined with an accuracy to the fourth decimal place after the comma.

7.2 For the measurement of time intervals less than 5 min used an hourglass or a stopwatch, 5 min, timers or clocks of any type.

7.3 are used For drying laboratory ovens, providing a heating temperature of not less than (250±3)°C. For dissolution and evaporation of solutions used electric stoves with a closed heating element for the heating temperature to 400 °C.

7.4 For the decomposition of samples is allowed to use the microwave decomposition of samples of any brand or use other systems of decomposition, providing a complete conversion of analyte into the solution.

7.5 For measurements use a measuring laboratory glassware not lower than 2nd accuracy class according to GOST 1770, 29169 GOST, GOST 29227, 29228 GOST, GOST 29229, GOST 29251, utensils and equipment according to GOST 25336, crockery and equipment (crucibles, boats, inserts for desiccators, etc.) according to GOST 9147.

7.6 methods Used in the measurement of the measuring instrument must have certificate of verification and/or calibration certificates. Test equipment required for testing must be certified.

7.7 allowed to use along with the equipment specified in the method of measurement, other measuring instruments, test equipment, auxiliary devices, providing measurements with the set in particular the method error (uncertainty).

8 Reagents and solutions

8.1 reagents Used should have the qualification «pure for analysis» (h. d. a.). Allowed the use of the reagents lower qualifications provided that their metrological characteristics of the measurement results, normalized to the measurement technique. Mandatory application of reagents a higher qualification stipulated in the measurement procedure.

8.2 For each unit of consumer packaging of chemical reagents and especially pure substance should be attached label indicating the name of the reagent/substance, to the designation of the appropriate normative document for the chemical/substance, qualification, date of manufacture, shelf life of the reagent.

8.3 verification of the fitness for use of laboratory reagents with the expired period of storage should be carried out in accordance with the recommendations of [3] or the procedure provided in the lab.

If necessary:

— the label should be affixed indicating the special storage conditions reagent/substance;

— the label must be protected from external influences.

8.4 For the preparation of analyte solutions and reagents solutions used distilled water according to GOST 6709 or water for laboratory analysis of the 2nd grade.

The necessity of more clean water set in the measurement technique.

8.5 For the preparation of solutions of known concentration are used metals or reagents qualification not less than «chemically pure» (khch), with a mass fraction of basic substance is no less than 99.9%. The required accuracy of weighing and volume measurement result in the measurement technique. Unless otherwise specified, the mass of the substance measured with an accuracy of four decimal places.

The mass concentration of the solution C, g/cmГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа(mg/cmГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, µg/cmГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, g/DMГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаmg/DMГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа) is calculated by the formula

ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, (1)


where m is the mass of the component (metal) or compounds (oxide, salt), taken to prepare the solution, g (mg, mcg);

K is the conversion factor of the substance taken for preparation of a solution of the compound (component), which is used to calculate the concentration of the solution (if the composition of these compounds is the same, then K=1);

V — solution volume, cmГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа(DMГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа).

Allowed for the preparation of solutions of known concentration to use WITH, certified for this component. The error of establishing the mass fraction of component in the standard sample shall not exceed one-third of the error of the used measurement techniques.

The mass concentration of the solution C, g/cmГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа(mg/cmГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, µg/cmГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, g/DMГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаmg/DMГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа) in this case is calculated by the formula

ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, (2)


where m is the mass of standard sample, g (mg, mcg);


A — certified value mass fraction of component, %;

V — solution volume, cmГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа(DMГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа).

8.6 Mass concentration of a solution defined by a component set not less than three batches of a substance (if the technique is not laid different number of batches) and expressed in grams of matter 1 cmГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаof solution (g/cmГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа). For the mass concentration of the solution take the arithmetic mean value obtained from the n results of the titration. The calculated values are rounded to the fourth decimal digit after comma.

8.7 To establish the mass concentration of the solution used:

— metals or chemicals — training not less than «chemically pure» (H. h), with a mass fraction of basic substance is no less than 99.9%;

— Composition of the certified to the designated component;

— aliquots of solutions of known concentration;

— AC, prepared according to [4].

8.8 Solutions of chemical reagents prepared in accordance with GOST 4212, GOST 4517, 4919.1 GOST, GOST 4919.2, 25794.1 GOST, GOST 25794.2, 25794.3 GOST, GOST 27025.

8.9 taking measurements and preparation of solutions after each addition of the reagent the solution was stirred.

8.10 the Degree of dilution of acids and solutions point to the formula A: B (e.g., 1:1), where the letter «a» means the volumetric part of the dilute concentrated solution, the letter «B» is the volume of the solvent.

If the methodology does not specify the concentration of the acid or an aqueous solution of ammonia, then use concentrated acid or ammonia solution.

8.11 the Terms related to the degree of heating of water (solution) and the duration of the operations — according to GOST 27025:

— «the solution at room temperature» — a solution has a temperature from 15 °C to 25 °C;

— «moderately warm solution» — a solution has a temperature from 25 °C to 40 °C;

warm solution has a temperature of from 40 °C to 75 °C;

— «hot water» (solution) means that the water (solution) has a temperature of above 75 °C.

The term «cooling» means cooling to a temperature of from 15 °C to 25 °C.

The term «heating» means the heating is to a temperature of above 75 °C.

8.12 Storage of solutions and reagents in accordance with GOST 4212, unless otherwise indicated:

the solutions of reagents must be stored at temperature from 15 °C to 25 °C in tightly closed plastic or glass container (bottles, flasks) with pritertymi or tightly closed tubes, in places protected from direct sunlight. The containers must have labels which indicate: the name, concentration, date of preparation and expiry date;

the solutions of decomposing under the action of light, kept in jars of dark glass or bottle of colorless glass with a light coating or wrapped in lightproof film (paper);

the solutions of the mass concentration of the element or ion of the substance 1 mg/cmГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаstore one year;

the solutions of the mass concentration of 0.1 mg/cmГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа — 3 months;

the solutions of the mass concentration of the element, ion or substance 0.01 mg/cmГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаand more diluted using freshly prepared (freshly prepared solution — a solution made of no more than 8 hours before using it).

In case if the storage solution appeared haze, flakes of the precipitate, the solution replaced by freshly prepared.

8.13 the Solutions of indicators should be prepared in accordance with the requirements of GOST 4919.1 and specific measurement techniques.

9 Requirements for performance measurement

9.1 Mass fraction of each component in the sample is determined in parallel (or independently) in two batches, unless otherwise noted in the measurement procedure, with the exception of the mass fraction of selenium (determined in three batches) Simultaneously with the measurements in the same conditions is carried out the control (blank) experience for an amendment to the measurement results.

9.2 Calculation of the mass fraction of the component is carried out using calibration characteristics (GC) — dependence of analytical signal on the concentration of analyte. In accordance with [5] RX can be represented by a table, a graph (built with smoothing or without smoothing); formula (in analytical form).

Note — depending on the kind of expression used GC combinations: a calibration table, calibration curve, calibration function.


The method and the conditions of constructing GC (choice of analytical signal, the number of points needed to construct a calibration curve, etc.) indicated in the specific standard for the measurement method.

9.3 To build the GC uses different calibration samples: SB, as, solutions of mass (molar) concentration.

Note — Variations of the calibration are calibration sample solution and the calibration mixture.

9.4 Calibration curve built in the system of rectangular coordinates: the abscissa shows the delay numeric value of mass fraction or mass of analyte, and the axis of ordinates the value of the analytical signal or the function from it.

9.5 For the construction of calibration curve requires at least three calibration points, each of which is based on the arithmetic mean of the results of two parallel measurements, unless otherwise noted in the measurement technique. The calibration points should be evenly distributed across the measuring range to cover the desired interval definitions.

9.6 Calibration solutions and the calibration mixture prepared in accordance with the method of measurement.

9.7 is allowed to carry out the construction of the calibration graphs and the calculation of the measurement results with the help of software of measuring instruments.

9.8 is allowed to pre-plotting, in the presence of their stability in time and periodic checks OK.

9.9 the Number of measurements of the analytical signal of the investigated solution is determined by the requirements of specific measurement techniques. The number of measurements of the analytical signal can vary depending on the business need (analysis, stability measurements, etc.).

9.10 permitted to conduct sequential or parallel measurement of different methods several components from one sample of the sample after decomposition, if you do not need to change the further course of the analysis and ensured the achievement of the metrological characteristics specified in specific standards for measurement methods.

9.11 Analytical instrumentation prepared to work according to the instructions for their use.

9.12 When using instrumental methods of measurement, it is necessary to choose optimal conditions of measurement of the analytical signal provides the necessary sensitivity and accuracy depending on the method applied, the type of device, defined by the component and its mass fraction in the sample.

9.13 When you use photometric methods of measurements of the thickness of the absorbing layer of the cell are selected such as to provide measurements in an optimal optical densities for the applied means of measurement.

9.14 in determining the method of atomic absorption wavelength, the composition of the gas flame, a reducing or oxidizing action of the flame, turn the burner and other conditions of measurement are selected in such a way as to achieve the optimal values of measurements of the sensitivity and accuracy of the corresponding component and use of the device.

9.15 When using spectral measurement techniques subject to the achievement of the metrological characteristics specified in the standards on methods of measurement that allowed:

— to use when measuring the absorption of other resonance spectral line;

— use automated build system calibration charts, measurements in automated mode with the results of the measurements on paper or electronic media;

— consistently determine multiple components in one test portion of the sample after decomposition and appropriate dilution of the sample solution so that the mass concentration (mass) detectable component therein was in the range of mass concentrations (mass) calibration curve.

9.16 allowed to apply along with the means of measurement specified in the measurement procedure, other measurements of this type, providing metrological characteristics of the measurement results.

10 Requirements for processing and representation of measurement results

10.1 For the results of the measurements take the average value (arithmetic mean value or median) of the results of parallel measurements. The number of parallel measurements, to be averaged when calculating the measurement point in the measurement technique.

The numerical value of the measurement result must end with the digit the same category as the value of the index exactly indicated in the measurement technique.

10.2 the Discrepancy between the highest and lowest results of parallel measurements when measuring samples at a confidence probability P=0.95 does not exceed the limit of repeatability r (n=2) or CRГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа(n>2), the value of which is contained in the measurement technique.

If the discrepancy between the highest and lowest results of parallel measurements exceeds the value rГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, the measurement procedure is repeated. If necessary, the eligibility check is carried out according to the method of measurement or can be used methods for testing the acceptability of the results of parallel measurements and establishing the final result in accordance with GOST, ISO and GOST 5725.6 25086 (Appendix A).

Allowed to introduce rГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаto some public shares with the expectation values rГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаfor the intermediate mass fraction by linear interpolation.

It is allowed to insert rГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаin the form of equations or tables that includes the whole interval of the mass fraction of the designated component to be mounted in the measurement technique and divided into subintervals within which the appropriate values rГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаcan be assumed constant.

Note — If determination is performed in terms of a type of intermediate precision, limit of repeatability rГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаshould be replaced by the limit of intermediate precision.

10.3 Rounding of the measurement results is carried out in accordance with the requirements of the CMEA CT 543.

11 Methods of verification of admissibility of the results of measurements obtained in conditions of repeatability and reproducibility

11.1 checking the admissibility of the results of parallel measurements obtained in conditions of repeatability, carry out in the preparation of each measurement result of the working samples.

11.2 procedure for checking the admissibility of the results of parallel measurements involves comparing the absolute differences between the highest XГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаand lowest XГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаand n is the number of single measurements (definitions) rГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, made in accordance with the method of measurement, limit of repeatability r.

If the condition

ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, (3)


for the measurement result taking arithmetic mean value of n single measurements XГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа(i=1, …, n).

If the condition (3) is not satisfied, then perform the procedure given in 11.3.

11.3 Receive m parallel definitions. In this case m=n if the measurement procedure is not costly, and m=1 if the measurement procedure is expensive.

For the outcome measurements take the average value of n+m single measurements under the condition of

ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, (4)


where XГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаis the maximum result of n+m single measurements;

XГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа — the minimum result of n+m single measurements;

CRГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа(n+m) — the critical range for the number of single measurements n+m.

The value of the critical range CRГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа(n+m) is calculated by the formula

ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, (5)


where Q (P, n+m) — coefficient, which depends on the number n+m of single measurements obtained under conditions of repeatability and confidence level of R. the values of the coefficient Q (P, n+m) for the acceptance probability of P=0.95 is given in table 1;

ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаstandard the standard deviation (SD) of repeatability calculated by the formula

ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, (6)


where r is the repeatability limit;


Q (R, n) is a coefficient which depends on the accepted probability P and the number of parallel definitions n. The values of the coefficient Q (P, n) are given in table 1 for the acceptance probability of P=0,95.

11.4 If the condition (4) is not satisfied, then you must find out the causes resulting in unacceptable measurement results, and take action to correct the final measurement result can be accepted by the median ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаof the single measurements.


Table 1 — values of the coefficient Q (P, n) for a confidence probability P=0,95

   
n or (n+m) Q (R, n)
2 2,8
3 3,3
4 3,6
5 3,9
6 4,0

11.5 the Divergence between the results of measurements obtained in two laboratories, should not exceed the limit of reproducibility. If this condition is acceptable both measurement and as a final can be used their common arithmetic mean value.

If you exceed the limit of reproducibility can be used methods for assessing the acceptability of the results of measurements according to GOST ISO 5725−6.

11.6 the test results of the two measurements obtained by one method of measurement with different values of precision (if the interval representation), limit of repeatability r, R intermediate precisionГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаand repeatability R is calculated according to the formulas:

ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, (7)


where rГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаand rГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа — limits of repeatability corresponding to the values determined by the component in the sample;

ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа,* (8)


where RГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаand RГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа — limits intermediate precision;
_____________________

* Formula and explication to it correspond to the original. — Note the manufacturer’s database.

ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, (9)


where RГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаand RГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа — indices of reproducibility.

12 accuracy Control of measurement results in the laboratory

12.1 accuracy Control of measurement results within a laboratory exercise for measurement procedures with established indices of accuracy (correctness and precision) and approved for use in the prescribed manner in accordance with GOST 8.010.

12.2 During the implementation of the measurement methods in the laboratory provide operational control of the measurement procedure and control of stability of measurement results.

Algorithm for operational control procedures measurement result in the internal documents of the laboratory.

Control procedures stability measurements reglamentary in the documents of the laboratory.

12.3 as a means of control can be used:

— samples for control (s): standard samples (SS) according to GOST 8.315 or certified mixture (AC) [4];

— working samples with known additive detectable component;

— working samples of a stable composition;

— work samples, diluted in a specific ratio;

— other methods of measurement with the established indices of accuracy (control of measurement).

12.4 measurement procedures with the use of OK is to compare the result of the control determining the certified properties of the specimen to control ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаwith the certified value in [6]. At the same time OK must be adequate to the analyzed samples (possible differences in the compositions of the analyzed samples should not contribute to the measurement results statistically significant error). The error of the certified value of CR should be not more than one-third of the accuracy specifications of the measurement results.

If during the inspection, apply the OK, which are not used for establishing the measure of the accuracy of measurement results in case of exceeding the error of the OK one third of the error of measurement allowed to calculate the control ratio K according to the formula

ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, (10)


where ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа — error certified value is OK;


ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа — the indicator of the accuracy of measurement results corresponding to the certified value approx.

Method for permanent calibration schedule feature to recognize is stable under the condition:

ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, (11)


where X is found according to the calibration schedule, the value of the mass concentration of the component in the calibration sample;

C — certified value of the mass concentration of the component in the calibration sample;

KГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа — value of the standard stability control calibration curve established in the laboratory by construction of calibration curve.

12.5 Operational control procedures measurement using the method supplements test method of measurement method or sample dilution implemented in accordance with the algorithms given in [6].

In the implementation of operational control procedures measurement with the use of the addition method under the condition XГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, if XГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаis the mass fraction determined by impurities in the sample, ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаthe lower limit is determined by the concentration, the amount of additives should be 2−3 times the value WithГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа.

Monitoring is carried out by comparing the results of control treatments KГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаwith standard control K.

The result of the control procedure, KГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаis calculated by the formula

ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа, (12)


where X is the mass fraction of impurities determined in the sample with the additive;


WithГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаvalue Supplement;

±ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа) — value characteristics error of the measurement result corresponding to the mass fraction of impurities determined in the sample to the lower limit of the concentration detected in the sample (the sample with the additive, respectively).

If the result of the control procedure that satisfies the condition:

ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа,


the procedure of measurements confirmed to be satisfactory.

Allowed to use other methods of operational control of the measurement procedure.

12.6 To check the stability of the measurement results within the lab using the control procedure according to GOST ISO 5725−6 [6].

12.7 the Choice of control method depends on the analyzed objects and indicators, measurement techniques, cost and duration of measurements, etc.

13 Making measurements


The results of measurements are in the form X±ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа(at confidence probability P=0,95), where X is the result of measurement, %;

±ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализаis a measure of the accuracy (error) of measurement, %.

The values «±ГОСТ 20996.0-2014 Селен технический. Общие требования к методам анализа» is given in a particular method of measurement.

Note — If the final result of the measurement take the median values of critical difference and accuracy specifications calculated in accordance with GOST ISO 5725−6.


Rounding of the measurement results is carried out in accordance with the requirements of ST CMEA 543.

14 security Requirements

14.1 Preparation of samples for measurements, the measurements (dissolution in acids, alkalis etc.) and all the operations of chemical analysis related to the release of toxic fumes or gases should be performed in fume cupboards or boxes equipped with local suction device according to GOST 12.4.021.

In laboratory premises allowed to store chemicals in a Cabinet, equipped with a ventilation system with corrosion-resistant coating in accordance with the requirements of GOST 12.4.021.

14.2 Laboratory areas should be equipped with General dilution ventilation system according to GOST 12.4.021.

14.3 When performing measurements in workplace air can be harmful substances, maximum permissible concentration (MPC) in air of working zone should correspond to GOST 12.1.005 and hygienic standards [7].

14.4 Control of content of harmful substances in the air of working zone should be carried out in accordance with the requirements of GOST 12.1.005, GOST 12.1.007 and GOST 12.1.016.

14.5 Laboratory facilities which perform work on the chemical analysis of the investigated material must meet fire safety requirements according to GOST 12.1.004 and rules [8]. The means and methods of fire suppression should be applied according to the GOST 12.4.009 depending on the origin and nature of the fire.

14.6 When working with flammable and explosive gases should comply with the requirements of GOST 12.1.004 and GOST 12.1.010. When you use gases in cylinders must comply with the regulations [9]*.
________________
* See Bibliography. — Note the manufacturer’s database.

14.7 Electrical instrumentation and laboratory equipment, and the terms of use must comply with the requirements of GOST 12.1.030, GOST 12.2.007.0. Grounding shall conform to the requirements of regulation [10].

14.8 Organization of the training and testing of knowledge of requirements of labour safety — according to GOST 12.0.004.

14.9 the Staff of the laboratory should be provided with special clothing, special footwear and other means of individual protection in accordance with GOST 12.4.011, GOST 12.4.068, rules and regulations in the territory of the CIS.

14.10 laboratory Personnel must be provided with sanitary-household premises in the group production processes 3A in accordance with [11].

14.11 When transferring bottles with acids, alkalis and ammonia must be provided reliable protection of the container against damage (crates, baskets with shavings).

14.12 When using source materials that have hazardous properties must comply with safety requirements, regulated by the normative documents of the relevant reagents.

14.13 Waste acid and alkali should be collected separately in special containers; after neutralizing, drain into the sewer or in accordance with local conditions in the designated place.

14.14 When performing chemical analyses with the use of solvents or chlorine derivatives of hydrocarbons it is necessary to use personal protective equipment, taking account of the ways of penetration of these substances into the body (e.g., through the skin, respiratory tract).

14.15 Illumination of workplaces must comply with the requirements of sanitary rules and norms on the territory of the CIS.

Bibliography

     
[1] Sanitary norms and rules
SanPiN 2.2.½.1.1.1228−2003
Hygienic requirements to natural, artificial and combined lighting of residential and public buildings
________________
* Probably, the error of the original. Should read: SanPiN 2.2.½.1.1.1278−03. — Note the manufacturer’s database.
[2] Sanitary norms and rules
SanPiN 2.2.4.548−98*
Hygienic requirements to microclimate of industrial premises
________________
* Probably, the error of the original. Should read: SanPiN 2.2.4.548−96. — Note the manufacturer’s database.
[3] Recommendations on interstate standardization
RMG 59−2003
State system for ensuring the uniformity of measurements. Verification of fitness for use in laboratory reagents with the expired period of storage method of laboratory control of precision of the measurement
[4] Recommendations on interstate standardization
RMG 60−2003
State system for ensuring the uniformity of measurements. Mix certified. General requirements for the development
[5] Methodological manual
MI 2175−91
State system for ensuring the uniformity of measurements. Recommendation. Calibration characteristics of means of measurement. Methods of construction. Estimation errors
[6] Recommendations on interstate standardization
RMG 76−2004
State system for ensuring the uniformity of measurements. Internal quality control of results of quantitative chemical analysis
[7] Hygienic standards
GN 2.2.5.1313−03*
Chemical factors of production environment. The maximum permissible concentration (MPC) of harmful substances in the air of working zone
[8] Rules of fire prevention regime in the Russian Federation (UTV. decree of the RF Government of 25 April 2012 N 390*
[9] PB 03−576−03* Rules of arrangement and safe operation vessels working under pressure**, approved. by the resolution of Gosgortekhnadzor of the Russian Federation from June, 11th, 2003 N 91
________________
* On the territory of the Russian Federation the document is not valid, became invalid on the basis of the order of Rostechnadzor dated 25 March 2014 No. 116. There are Federal rules and regulations in the field of industrial safety «Rules of industrial safety of hazardous production facilities that use equipment operating under excess pressure». — Note the manufacturer’s database.
[10] Rules of arrangement of electrical installations, approved. The Ministry of energy of the Russian Federation Order No. 204 dated July 8, 2002.*
[11] A set of rules
SP 44.13330.2011*
SNiP 2.09.04−87 Administrative and domestic buildings revised edition
____________________
* Valid on the territory of the Russian Federation.



_____________________________________________________________________

UDC 669.776:543.06:006.354 ISS 77.120.99

Key words: selenium technical measurement, calibration characteristics, measuring instruments, accuracy