The importance of wastewater treatment systems is undeniable. No building that is used by man can do without them. New ones are constantly emerging manufacturing enterprises, gas stations, bars and restaurants, other establishments from the service sector, apartment buildings or country houses, and the problem of high-quality wastewater treatment remains relevant. To solve it, enterprises, local authorities, owners of residential real estate are building local treatment systems of various types.

The concept of VOC

Devices, structures, complexes of structures with various engineering communications and various combined systems, the main purpose of which is the complete or ultra-deep purification of household, industrial, rain and other sewage, are called local treatment facilities (VOCs).

Many people equate VOCs with autonomous sewage - this is not true, since autonomous sewage is one of the types of VOCs that function independently and exist separately from the central sewer line.

Interesting to know. most main task what such structures, structures and their complexes should solve is the purification Wastewater to the level described in legislative rules and standards of relevant services, guaranteeing the absolute safety of the surrounding flora and fauna, health and life of people.

VOC types

Local facilities for the purification of sewage water can be divided into the following types by location:

1. Treatment systems that are part of the municipal central sewerage system, which, after processing wastewater, send it to the city sewer network;
2. Cleaning systems that serve buildings or building complexes separately from the central sewer line, as they are removed at a decent distance from it or without the possibility of connecting to it (autonomous sewerage).

VOC of the centralized sewerage

The first group mainly consists of large-scale systems, which include a number of large-scale treatment facilities that form an automatic complex for the processing of large volumes of industrial effluents from factories, industrial production, plants and domestic effluents from cities, towns, and other settlements.

Such sewer systems are usually built outside the city line. The territory allocated for their construction and operation is a sanitary zone where it is forbidden to live and hold various recreational activities.

They are maintained by specially trained personnel, and they operate through special devices and equipment, control panels and automation systems.

Independent VOCs

Autonomous VOCs have smaller dimensions. Installed to purify industrial wastewater from small production organizations and factories, as well as effluents from economic activity person. They have a simpler design and cleaning technology with lower power and throughput.

Often, local sewage treatment systems of an autonomous type serve service industries, small villages and individual residential buildings that are far from the municipal sewage treatment network.

How does the LOS work?

The vast majority of local treatment facilities operate on a multi-level method of wastewater treatment, which consists in their passage of the following stages:

• mechanical (rough);
• bacterial (biological);
• chemical-physical.

Rough cleansing

As a result of mechanical treatment, household and fecal waters are passed through various filter systems that trap large inclusions in them. The stage at which the effluents pass through the first filter system is called rough cleaning. After this stage, the wastewater passes the next set of filters, designed to remove smaller inclusions from the drains. Upon completion of the passage through the filters, the water enters specialized storage tanks, where the process of clarification takes place.

Chemical cleaning

Since wastewater is affected by various chemical reagents, inorganic and organic compounds that have a detrimental effect on the state environment, then before the discharge of such waters into a reservoir or river, it is required to carry out the process of their chemical neutralization. This process is based on oxidation-reduction reactions. For example, if you want to get rid of impurities in the water caused by alkaline solutions, you need to treat the liquid with various acids, and vice versa.

Bacterial cleansing

This stage consists in the purification of wastewater from various organic contaminants by means of special bacteria, which, processing such contaminants, start the process of their decomposition with further removal from the VOC. This cleaning step can take place in an anoxic or oxygen environment, against which a distinction is made between anaerobic and aerobic cleaning.

Varieties of autonomous treatment systems

Autonomous local treatment systems include the following types of facilities:

• septic tanks with sedimentation tanks;
• biofilters;
• aerotanks.

These systems differ from each other in design features and the method of wastewater treatment.

Important! Any of the above facilities must necessarily be equipped with filtering installations or facilities, since on their own they will not be able to organize a full processing cycle, in which water will be purified by 97-100%.

Septic tanks

Constructions for organizing sewage, consisting of accumulation tanks, divided into chambers for cleaning and settling waste inclusions, are called septic tanks. They can include several storage tanks in their design. The most popular for organizing a sewer system in summer cottages and personal plots, as they have a low cost and a high level of practicality.

Septic tanks are small in size and contain all the necessary devices for organizing the processing of sewage water.

Such septic tanks are produced on an industrial scale mainly from high-strength plastic. This material is light in weight, which makes the installation of a septic tank quick and easy. Such systems perfectly withstand sharp temperature fluctuations, exposure to various aggressive environments, onslaughts and mechanical loads.

The construction of a septic tank can be carried out from concrete and other materials.

Note! Septic tanks are not able to treat wastewater by 100%, as they are part-cycle VOCs. Be sure to create special filter fields together with them, which contributes to almost complete soil purification.

On the market of local treatment systems, you can find ultra-deep cleaning stations, which are a kind of septic tank, where all kinds of filtering devices and other cleaning agents have already been installed. Such devices have compact dimensions and provide almost one hundred percent purification of sewage water.

Aerotanks

Specialized open storage tanks in the shape of a rectangle, where the filtration process and the sedimentation of abrasive wastewater fractions are carried out, are called aerotanks.

Aerotanks have an elongated shape, reminiscent of water channels, through which household fecal liquid moves, mixing with activated sludge (a community of protozoa) with the help of air pressure, which is responsible for their processing.

Various substances appearing on the surface, for example, oil products, fatty inclusions, can also be removed in aeration tanks.

These structures do not exist in isolation, but are part of a complex of municipal sewer systems or, in a reduced form, are built into a septic tank with settling tanks and ultra-deep cleaning stations.

Design for biological treatment

Biofilters are special containers or structures that serve for deep purification of wastewater with the help of colonies of certain bacteria launched into them. Just like in aerotanks, they are part of municipal sewer systems or, in a reduced and simplified version, are built into septic tanks.

In addition to microorganisms, filter materials are placed in biofilters, which provide mechanical wastewater treatment, for example, expanded clay.

VOC for industrial enterprises

Local treatment facilities for industrial enterprises operate according to a progressive and more complex structure for processing wastewater with more complex pollution.

Wastewater treatment systems serving large or complex technology enterprises, in their structure contain:

• Mechanical cleaning line. The waste liquid enters the storage tank, from which it is distributed to biofilters, getting rid of large inclusions;
• Simultaneous processing of industrial effluents by the chemical method. After getting rid of large fractions, effluents enter various sedimentation tanks containing certain chemicals and solvents that bind to organic and inorganic water pollutants, forming feathers or lumps that settle at the bottom of the tank;
• Specialized greenhouses with aerotanks that contain activated sludge and water hyacinth, which rids the water of organic fractions;
• Biological ponds for post-treatment of wastewater, in which the last stage of work with fractions takes place by exposing them to special microorganisms;
• Disinfection station for sewage treatment by means of ultraviolet radiation.

Typically, each stage of wastewater treatment industrial type is carried out in a separate building or room, which makes it possible to avoid the release of polluting compounds or substances from these sewage into the atmosphere, as well as to comfortably control the entire technological process.

VOCs in this structure provide processing of sewer lines at the following enterprises:

• poultry farms;
• meat processing plants;
• factories for the production of glass and other products from it;
• canning factories;
• car washes;
• factories of fat-containing products and vegetable oils;
• and other industrial enterprises.

VOC for rain (storm) runoff

Systems for the processing of storm water have their own characteristics in terms of structure and treatment methods, which is due to the presence in their composition of a significant content of suspensions of natural origin, chemical compounds and large particles.

These VOCs can successfully function for the treatment of storm water from the following facilities:

• car washes;
• factories;
• territories of industrial enterprises;
• large parking lots and car parks;
• adjacent territories to business centers and shopping facilities;
• household plot.

So a standard storm sewer system should contain the following elements:

• sump;
• trap of sand and other abrasive particles;
• trap of oil-containing substances (oil trap);
• absorbent filter;
• UV disinfection system;
• control container for approbation of the purified liquid.

VOCs for storm sewer systems have a high level of wastewater treatment (up to 98%) and productivity, as they must be ready to process a large volume of liquid, for example, during prolonged rains.

In the design of such sewer systems, there are sedimentation tanks, where effluent is separated from large fractions such as branches, street litter, glass, cobblestones and other particles washed up with water from melting snow or rain.

VOCs for storm drains must contain sand and oil traps in their system, as storm drains contain a large number of abrasive substances and refined petroleum products emitted by cars and gas stations.

The final stage of purification of such effluents is their disinfection by means of ultraviolet rays, after which the purified liquid can be sent to natural reservoirs.

In local treatment facilities for sewage of any type, those technological solutions, which reliably provide high-quality wastewater treatment without negative impact on the state of the environment, making human life easier and more comfortable.

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INTERSTATE COUNCIL FOR STANDARDIZATION, METROLOGY AND CERTIFICATION

INTERSTATE COUNCIL FOR STANDARDIZATION, METROLOGY AND CERTIFICATION

GOST

INTERSTATE

STANDARD

31991.1-

(ISO 11890-1:2007)

PAINT MATERIALS

Determination of volatile organic content

compounds (LOS).

difference method

(ISO 11890-1:2007, MOD)

Official edition

Standartinform

Foreword

The goals, basic principles and procedure for carrying out work on interstate standardization are established by GOST 1.0-92 “Interstate standardization system. Basic Provisions” and GOST 1.2-2009 “Interstate Standardization System. Interstate standards, rules and recommendations for interstate standardization. Rules for the development, adoption, application. updates and cancellations

About the standard

1 PREPARED by the Technical Committee for Standardization TC 195 "Paint and varnish materials". OJSC "Scientific and Production Company "Spektr LK" based on an authentic translation into Russian of the standard specified in paragraph 4, which was made by FSUE "STANDART-INFORM"

2 INTRODUCED by the Technical Secretariat of the Interstate Council for Standardization, Metrology and Certification

3 ADOPTED by the Interstate Council for Standardization, Metrology and Certification (Minutes of December 3, 2012 No. 54-P)

4 This standard has been modified from international ISO standard 11890-1:2007 Paints and varnishes - Determination of volatile organic compound (VOC) content - Part 1: Difference method

Additional words, phrases included in the text of this standard to meet the needs national economy and features of national standardization are in italics.

Table 1 "Results of the interlaboratory test", containing reference data, has been excluded from section 10.

This standard has been prepared on the basis of GOST R 52485-2005 (IS011890-1:2000) “Paint-and-lacquer materials. Determination of the content of volatile organic compounds (VOC). Difference method”, taking into account the requirements of ISO 11890-1:2007.

The international standard was developed by the Standardization Committee TC 35 "Paints and varnishes".

Translation from of English language(ep).

Compliance degree - modified (MOD)

5 By order of the Federal Agency for Technical Regulation and Metrology dated August 7, 2013 No. 482-st, the interstate standard GOST 31991.1-2012 (ISO 11890-1:2007) was put into effect as a national standard Russian Federation since July 1, 2014

6 INTRODUCED FOR THE FIRST TIME

Information about changes to this standard is published in the annual information index "National Standards", and the text of changes and amendments - in the monthly information index "National Standards". In case of revision (replacement) or cancellation of this standard, a corresponding notice will be published in the monthly information index "National Standards". Relevant information, notification and texts are also placed in information system general use - on the official website of the Federal Agency for Technical Regulation and Metrology on the Internet

© Standartinform. 2014

In the Russian Federation, this standard cannot be fully or partially reproduced. replicated and distributed as an official publication without the permission of the Federal Agency for Technical Regulation and Metrology

GOST 31991.1-2012 (ISO 11890-1:2007)

INTERSTATE STANDARD

PAINT MATERIALS

Determination of the content of volatile organic compounds (VOC).

difference method

paint materials. Determination of volatile organic compound (VOC) content. Difference method

Introduction date - 2014-07-01

1 area of ​​use

This International Standard specifies a method for the determination of the content of volatile organic compounds (VOCs) in paints and varnishes and their raw materials. This method is used for the expected mass fraction VOC more than 15%. If the expected mass fraction of VOCs is from 0.1% to 15%. use the method according to GOST 31991.2.

The method is based on the assumption that the volatile substance is water or an organic compound. If other volatile inorganic compounds are present in the material, their content is determined by another more suitable method and the results of such determination are taken into account in the calculations.

2 Normative references

This standard uses Normative references to the following interstate standards:

GOST 9980.2-86 (ISO 842-84, ISO 1512-74, ISO 1513-80) Paintwork materials. Sampling for testing (ISO 842:1984 Raw materials for paints and varnishes - Sampling. MOD: ISO 1512.1974 "Paints and varnishes - Sampling". MOD: ISO 1513:1980 "Paints and varnishes - Inspection and preparation of test samples" .MOD)

GOST 14870-77 Chemical products. Methods for the determination of water (ISO 760:1978 "Determination of water - Karl Fischer method (general method). NEQ)

GOST 29317-92 (ISO 3270-84) Paint-and-lacquer materials and raw materials for them. Temperature and humidity conditions for conditioning and testing (ISO 3270:1984 "Paints, varnishes and their raw materials. Temperature and humidity conditions for conditioning and testing". MOD)

GOST 31939-2012 (ISO 3251:2008) Paint and varnish materials. Determination of the mass fraction of non-volatile substances (ISO 3251:2008 "Paints, varnishes and plastics - Determination of the content of non-volatile substances". MOD)

GOST 31991.2-2012 (ISO 11890-2:2006) Paint and varnish materials. Determination of the content of volatile organic compounds (VOC). Gas chromatic method (ISO 11890-2:2006 "Paints and varnishes - Determination of volatile organic compounds (VOCs) - Part 2: Gas chromatic method". MOD)

GOST 31992.1-2012 (ISO 2811-1:2011) Density determination method. Part 1: Pycnometric method

Official edition

Note - When using this standard, it is advisable to check the validity of reference standards in the public information system - on the official website of the Federal Agency for Technical Regulation and Metrology on the Internet or according to the annual information index "National Standards", which was published as of January 1 of the current year, and on issues of the monthly information index "National Standards" for the current year. If the reference standard is replaced (modified), then when using this standard, you should be guided by the replacing (modified) standard. If the referenced standard is canceled without replacement, then the provision in which the reference to it is given applies to the extent that this reference is not affected.

3 Terms and definitions

8 of this standard, the following terms are used with their respective definitions:

3.1 volatile organic compound; VOC: Any organic compound having an initial boiling point less than or equal to 250°C. measured at normal pressure

NOTE The properties and number of compounds to be taken into account depend on the application of the coating material. For each field of application, limit values ​​and methods for determining or calculating such compounds are established in regulatory (ND) or technical (TD) documents for paintwork material (LKM).

3.3 ready-to-use paintwork material: Paintwork material after it has been mixed, if necessary, with other components and diluted with appropriate solvents and/or thinners in accordance with RD or TD. suitable for application by the appropriate staining method.

4 Essence of the method

After preparing the sample, the mass fraction of non-volatile substances is determined according to GOST 31939. Then the water content is determined according to GOST 14870. After that, the VOC content in the sample is calculated.

5 Required additional information

For any particular application, the test method specified in this International Standard. must be supplemented with the necessary information. Scroll additional information is given in Appendix A.

6 Sampling

Take an average sample of the material for testing (or each material in the case of a multilayer system) according to GOST 9980.2.

Control and preparation of each sample - according to GOST 9980.2.

7 Testing

7.1 Preparation of the paint sample for testing

For testing, a sample of paintwork materials is used. ready for use (3.3).

7.2 Number of determinations and test conditions

Two parallel tests are carried out at a temperature (2312) * C and relative humidity (5015)% (GOST 29317). unless otherwise specified.

7.3 Determining parameters

Determine the parameters necessary for the calculation (8.2-8.4), as required by the requirements of 7.4 and 7.5. Some parameters can be determined by the difference of their values ​​depending on the nature of the compounds. present in the sample.

7.4 Density

If required for calculation (b.3.8.4). determine the density of the sample according to GOST 31992.1. Density determination is carried out at a temperature of (2312) °C, unless other conditions are specified.

7.5 Mass fraction of non-volatile substances

Determine the mass fraction of non-volatile substances in a sample ready for use, according to GOST 31939.

6 in the case of one-component coatings, the mass fraction of non-volatile substances in the sample, ready for use. determined according to GOST 31939.

In the case of determining the mass fraction of non-volatile substances in a sample ready for use of multicomponent systems, thoroughly mix the components in accordance with the manufacturer's instructions. Samples are immediately weighed in accordance with GOST 31939. Samples for analysis are kept in cups. in which weighing was carried out, for 1 hour at a temperature of (23 ± 2) ® C and atmospheric pressure. unless otherwise specified. Then the determination is carried out according to GOST 31939.

If any unusual phenomenon occurs during heating (decomposition or destruction), then, by agreement between the parties concerned, it is possible to use a time and (or temperature) other than those recommended in GOST 31939.

7.6 Mass fraction of water

The mass fraction of water in percent according to GOST 14870 is determined by choosing the reagents so that they do not interfere with the analysis of the compounds contained in the sample. If the composition of such compounds is unknown, they are subjected to qualitative analysis, for example, according to GOST 31991.2.

Notes

1 Typical connections that may interfere with the penetration. are ketones and aldehydes. For right choice reagents should be guided by the information provided by the manufacturer.

NOTE 2 If the properties of the material to be tested are precisely defined and it is known that it does not contain water, then the determination of the water content in it can be omitted, assuming it to be zero.

The composition of the Fisher reagent is indicated in the ND or TD for a specific paintwork material.

8 Calculation

8.1 General provisions

Calculate the VOC content according to the method specified in the RD or TD for the material. If a specific method is not specified in the ND or TD, then the VOC content is calculated according to method 1.

Method 1 is the preferred calculation method because it provides the best precision of the results by eliminating the density operation, which is a potential source of additional errors.

8.2 Method 1: Mass fraction of VOCs. %. in a ready-to-use material is calculated by the formula

VOC = 100 - NV - m w . (one)

where VOC is the mass fraction of VOC in the material ready for use. %;

NV - mass fraction of non-volatile matter (7.5), %; m. is the mass fraction of water (7.6). %.

8.3 Method 2: Mass concentration of VOCs. g / dm 3, in a material ready for use, is calculated by the formula

VOC = (100 - NV 10. (2)

where VOC is the mass concentration of VOC in the material ready for use, g / dm 3:

NV - mass fraction of non-volatile matter (7.5), %; m w - mass fraction of water (7.6),%:

p t is the density of the sample at a temperature of (23 ± 2) X (7.4). g/cm3:

10 - conversion factor.

8.4 Method 3: VOC content. g/dm 3 , in a ready-to-use material, except for water. calculated according to the formula

where LOS,. - content of VOC 6 in the material ready for use, with the exception of water, g / dm 3: NV - mass fraction of non-volatile substance (7.5). %; mw is the mass fraction of water (7.6). %;

p, is the density of the sample at a temperature of (23 ± 2) °C (7.3). g/cm3:

P i is the density of water at a temperature of 23 ° C. g/cm 3 (p w - 0.9975 g/cm 3);

1000 - conversion factor.

9 Processing results

If the results of two parallel tests differ by a value greater than that specified in 10.2. the test is repeated.

Calculate the average of the two valid replicate results and report the result to the nearest 1%.

10 Precision

10.1 Limit of repeatability of results r

The repeatability limit r is the value below which the absolute value of the difference between the results of two separate tests, each of which is the average of the results of two parallel determinations obtained on identical material by one operator in one laboratory within a short period of time on one standardized test, is expected to be test method.

The repeatability of the results for five repeated determinations by this method, expressed as a coefficient of variation in repeatability, is 1%.

10.2 Reproducibility limit R

The reproducibility limit R is the value below which the absolute value of the difference between the results of two tests, each of which is the average of the results of two replicate determinations obtained on identical material by operators in different laboratories, using the same standardized test method, is expected to fall.

the reproducibility of the results by this method, expressed as the reproducibility variation coefficient, is 2%.

11 Test report

The test report must contain:

b) information necessary to fully identify the material being tested (manufacturer's name, trademark, lot number, etc.);

c) supplementary information items referred to in Annex A:

e) the test results of Clause 8, the calculation method used (8.2, 8.3 or 8.4);

0 any deviation from this method tests:

e) the date of the test.

Annex A (mandatory)

Required Additional Information

In order to be able to use the method of this International Standard, additional information specified in this appendix must be provided.

The necessary information should preferably be agreed between the interested parties, using as its source, in whole or in part, the relevant international or national standard or other technical document relevant to the product under test.

c) Organic compound(s), the content of which(s) should be determined [if it(they) are known^)).

b) Analytical methods to be used to identify these compounds.

c) Calculation method used (section c).

UDC 667.64.001.4:006.354 MKS 87.040 MOD

Key words: paints and varnishes, volatile organic compound (VOC), mass fraction, mass concentration, difference method

Editor L I Nakhimova Technical editor Е.8. Baeprozvainap Proofreader M.v Buinaya Computer airstaa V.I. Grishchenko

Handed over to the set 07/09/2014.

Signed and stamped 27.00.2014. Format 60>S4 "/ I. Headset Ariel. Coin. medical sheet 1.40. Account. Nod. sheet 0.70. Circulation 62 eq. For * 3612.

Published and printed by JSC FSUE STANDARTINFORM. 123995 Moscow. Garnet lane.. 4.

To reduce the amount of pollutants and runoff from roads directly on the carriageway, the following measures are taken:

• Collection of storm water from roads through catchment trays and pre-curb recesses for further discharge to wastewater treatment plants.
• Prevention of erosion of earthen slopes and roadside areas, timely cleaning of drainage ditches, roadsides and slopes.
• Regular cleaning of the road surface, cleaning of drainage systems.
• Timely repair of the roadway.
• Use control de-icing reagents.
• A ban on the dumping of snow removed in winter into water bodies or onto the ice surface.
• Selection of environmentally friendly road marking materials.

Pollutants and particles of asphalt material accumulate on the road sections with broken pavement, which spread in the form of a suspension during rain and enter the surface sewage. In order to prevent polluted construction effluents - for example, during the repair of the roadway - from falling into water collection devices, it is necessary to organize the removal of polluted effluents into a specially arranged infiltration trench.

Minimize the use of de-icing agents to reduce harmful effects on the environment is possible with the correct calculation of the rate of use of reagents. If the road passes near a reservoir, it makes sense to install special barriers that divert polluted effluents from the water body. Screens made of polymeric materials are the most promising for this.

The search for new anti-icing products that combine efficiency, cost-effectiveness and environmental safety - actual problem today.

Engineering wastewater treatment

The storm and melt runoff collected from the surface of the road in the most favorable variant is directed to the treatment plant. When choosing the type of treatment plant, it is necessary to take into account its interface with the road drainage system.

The choice of treatment plant design depends on the climatic and hydrological characteristics of the area, as well as on the characteristics of pollutants.

Pollutants are classified according to their physical state (soluble, insoluble, colloidal systems) and chemical composition. An important characteristic of suspended particles that affects the choice of treatment equipment is dispersion (particle size and shape).

Types of treatment facilities

At the treatment plant, all or several of the following stages of wastewater treatment are sequentially implemented: mechanical treatment, chemical treatment, physical-chemical and biological treatment.

Mechanical wastewater treatment from pollutants is carried out using mechanical gratings, sand traps, settling tanks, oil traps, hydrocyclones, filters, plant strips, etc.

Mechanical treatment facilities open the way for effluents entering the treatment facilities. Mechanical cleaning removes large debris from wastewater, significantly reduces the content of suspended solids and prepares wastewater for further treatment stages.

Next view - chemical wastewater treatment. Chemical methods are used after mechanical treatment and before effluents enter biological treatment, or are used as the final stage of post-treatment (chlorination, ozonation).

Neutralization (for acidic or alkaline effluents) and oxidation are used as chemical treatment methods on an industrial scale.

Physical and chemical cleaning methods belong to the deep cleaning stages. These are methods of flotation, coagulation (clarification), adsorption, ion exchange, extraction, etc. The use of these methods allows you to remove most of the toxic chemical compounds that are in dissolved form from the water.

For the cleaning big expenses wastewater using the adsorption method, the following types of structures are used: free-flow adsorbers, infiltration trenches, drainage wells.

Biochemical cleaning methods based on the ability of some microorganisms to process dissolved chemical compounds.

Biological cleaning methods have their own characteristics associated with the normal functioning of microorganisms - it is necessary that the concentration chemical substances were within the specified limits, and that there were no heavy metals. Biological treatment can be aerobic (with active air access) and anaerobic (oxygen-free).

Aerobic treatment is carried out in treatment facilities the following types: aeration tanks, oxygen tanks, biofilters, biological ponds.

Anaerobic purification (methane fermentation or fermentation) is carried out without air access in specially equipped reactors (methane tanks, septic tanks, anoxicators) and allows biological processing of even the most difficult-to-oxidize chemical compounds.

The combination of aerobic and anaerobic treatment methods gives the greatest effect of improving water quality.

If the installation of treatment facilities near the road is not possible, structures in the form of reinforced concrete shield fences should be installed.

For the treatment of surface runoff from roads and bridges, the most promising is the installation of complex treatment facilities that give the maximum effect on the treatment of polluted effluents.

Paint industry. GOST R 52485-2005: Paint and varnish materials. Determination of the content of volatile organic compounds (VOC). difference method. OKS: Paint and varnish industry, Paints and varnishes. GOSTs. Paintwork materials. Definition of content.... class=text>

GOST R 52485-2005

Paintwork materials. Determination of the content of volatile organic compounds (VOC). difference method

GOST R 52485-2005 (ISO 11890-1:2000)
Group L19

NATIONAL STANDARD OF THE RUSSIAN FEDERATION

Paintwork materials

DETERMINATION OF VOLATILE ORGANIC COMPOUNDS (VOC)

difference method

paint materials. Determination of volatile organic compound (VOC) content.
Difference method

OKS 87.040
OKSTU 2309

Introduction date 2007-01-01

Foreword

The goals and principles of standardization in the Russian Federation are established federal law dated December 27, 2002 N 184-FZ "On technical regulation", and the rules for the application of national standards of the Russian Federation - GOST R 1.0-2004 "Standardization in the Russian Federation. Basic provisions"
About the standard

1 PREPARED by Spektr-Lakokraska Research and Production Company LLC, Technical Committee for Standardization TC 195 "Paints and varnishes" based on an authentic translation of the standard specified in paragraph 4, which was made by VNIIKI. Registration number: 1080 / ISO

2 INTRODUCED by the Technical Committee for Standardization TC 195 "Paint and varnish materials"

3 APPROVED AND PUT INTO EFFECT by Order of the Federal Agency for Technical Regulation and Metrology dated December 30, 2005 N 511-st

4 This International Standard is modified from ISO 11890-1:2000, Paints and varnishes — Determination of volatile organic compounds — Part 1: Difference method (Paints and varnishes — Determination of volatile organic compound). (VOC) content - Part 1: Difference method"). However, it does not include references to international standards: ISO 2811-2:1997 "Paints and varnishes. Density determination. Part 2: Immersed body (plummet) method", ISO 2811-3:1997 "Paints and varnishes. Density determination. Part 3. Oscillatory method, ISO 2811-4:1997 "Paints and varnishes. Determination of density. Bowl pressure method", which are not used in the state standardization of the Russian Federation.
The name of this standard has been changed relative to the name of the specified international standard to bring it into line with GOST R 1.5-2004 (subsection 3.5).
Phrases, indicators, their meanings included in the text of this standard to take into account the needs of the national economy of the Russian Federation are in italics

5 INTRODUCED FOR THE FIRST TIME

Information about changes to this standard is published in the annually published information index "National Standards", and the text of changes and amendments - in the monthly published information indexes "National Standards". In case of revision (replacement) or cancellation of this standard, a corresponding notice will be published in the monthly published information index "National Standards". Relevant information, notification and texts are also posted in the public information system - on the official website of the Federal Agency for Technical Regulation and Metrology on the Internet

1 area of ​​use

1 area of ​​use

This International Standard is part of a series of standards for sampling and testing coatings.
This standard specifies a method for the determination of volatile organic compounds (VOCs) in paintwork materials and raw materials. This method is used for the expected mass fraction VOC over 15%. If the expected mass fraction VOC from 0.1% to 15%, use the method according to GOST R 52486.
The method is based on the assumption that the volatile substance is water or an organic compound. When other volatile inorganic compounds are present in the coating material, their content is determined by another more suitable method and the results of such determination are taken into account in the calculations.

2 Normative references

This standard uses normative references to the following standards:
GOST R ISO 5725-1-2002 Accuracy (correctness and precision) of measurement methods and results. Part 1. Basic provisions and definitions
GOST R ISO 5725-2-2002 Accuracy (correctness and precision) of measurement methods and results. Part 2: Basic method for determining the repeatability and reproducibility of a standard measurement method
GOST R 52486-2005 Paint and varnish materials. Determination of the content of volatile organic compounds (VOC). Gas chromatographic method
GOST R 52487-2005 Paint and varnish materials. Determination of the mass fraction of non-volatile substances
GOST 9980.2-86 Paintwork materials. Sampling for testing
GOST 14870-77 Chemical products. Water determination methods
GOST 28246-2005 Paint and varnish materials. Terms and Definitions
GOST 28513-90 Paint and varnish materials. Density determination method
GOST 29317-92 Paintwork materials and raw materials for them. Temperature and humidity for conditioning and testing
Note - When using this standard, it is advisable to check the validity of reference standards in the public information system - on the official website of the Federal Agency for Technical Regulation and Metrology on the Internet or according to the annually published information index "National Standards", which was published as of January 1 of the current year , and according to the corresponding monthly published information signs published in the current year. If the reference document is replaced (modified), then when using this standard, you should be guided by the replaced (modified) document. If the referenced document is canceled without replacement, then the provision in which the link to it is given applies to the extent that this link is not affected.

3 Terms and definitions

In this standard, the following terms are used with their respective definitions:

1 The properties and number of compounds to be taken into account depend on the area of ​​application of the coating material. For each field of application, limit values ​​and methods for determining or calculating such compounds are established by regulations or agreement.
2* According to some government legislative acts the use of the term VOC is limited to only those compounds that exhibit photochemical activity in the atmosphere. Any other compound is then defined as being photochemically inactive.
[adapted, GOST 28246-2005]
________________
* Note 2 is for reference only and is not applicable in the Russian Federation.

3.3 photochemically inactive compound: An organic compound that does not participate in atmospheric photochemical reactions (3.2 Note 2).

3.4 ready to use: The state of a material after it has been mixed in the correct proportions in accordance with the manufacturer's instructions and diluted, if necessary, with the appropriate solvents so that the material is ready for use by the approved method.

4 Essence of the method

After sample preparation, determine mass fraction non-volatile substance according to GOST R 52487, then the water content is determined according to GOST 14870. If necessary, the content of photochemically inactive compounds is determined according to GOST R 52486. After that, the VOC content in the sample is calculated.

5 Required additional information

To be applicable, the test method specified in this International Standard shall be supplemented with the necessary information. A list of additional information is given in Appendix A.

6 Sampling

Take away average sample material for testing (or each material in the case of a multilayer system) according to GOST 9980.2.
Carry out control and prepare each sample for testing to the state of "ready for use" in accordance with GOST 9980.2.

7 Testing

7.1 Number of determinations and test conditions
Unless otherwise indicated, two parallel tests are carried out at a temperature of (23 ± 2) °C and relative humidity (50 ± 5)% (GOST 29317).

7.2 Determining parameters
Determine the parameters necessary for the calculation (8.2-8.5), in accordance with the requirements of 7.3-7.6. Some parameters can be determined by the difference in their values ​​depending on the nature of the compounds present in the sample.

7.3 Density
If required for the calculation (8.3-8.5), determine the density of the sample according to GOST 28513. Density determination is carried out at a temperature of (23 ± 2) °C.

7.4 Mass fraction non-volatile substances
Unless otherwise specified, the definition mass fraction non-volatile substances are carried out according to GOST R 52487.

7.5 Mass fraction of water
Determine the mass fraction of water in percent according to GOST 14870, choosing reagents so that they do not interfere with the analysis of the compounds contained in the sample. If the composition of such compounds is unknown, they are subjected to a qualitative analysis, for example, according to GOST R 52486.
Notes

1 Typical compounds that may interfere with analysis are ketones and aldehydes. For the correct choice of reagents, one should be guided by the information that is usually published by manufacturers.

NOTE 2 If the properties of the material to be tested are well defined and it is known that it does not contain water, then the determination of the water content in it can be omitted, assuming it to be zero.

The composition of Fisher's reagent is indicated in normative document for a specific coating material.

7.6 Photochemically inactive compounds(only if national legislation applies)

7.6.1 If the sample contains unknown organic compounds, they should be subjected to a qualitative analysis, for example, according to GOST R 52486.

7.6.2 Determine the content of photochemically inactive compounds in the sample according to GOST R 52486.

7.6.3 Determine the density of photochemically inactive compounds by the method given in 7.3 or by using published reference data.

8 Calculation

8.1 General
Calculate the VOC content according to the method specified in regulatory document for a specific paintwork material. If no specific method is specified in the RD, then the VOC content is calculated according to method 1.
Method 1 is the preferred calculation method due to the fact that it provides high precision results due to the absence of a density determination operation (which is a potential source of additional errors).

8.2 Method 1: mass fraction VOC, %, in the material, "ready to use", calculated according to the formula

Where - mass fraction VOC in the material, "ready to use",%;
- mass fraction
- mass fraction water (7.5), %.

8.3 Method 2: mass concentration VOC , g/dm, in "ready to use" material calculated according to the formula

Where - mass concentration VOC in "ready-to-use" material, g/dm;
- mass fraction non-volatile substance (7.4), %;
- mass fraction water (7.5), %;
g/cm;
- conversion factor

8.4 Method 3: mass concentration VOC , g/dm, in a "ready-to-use" material, with the exception of water, calculated according to the formula

Where - mass concentration VOC in "ready-to-use" material, excluding water, g/dm;
- mass fraction non-volatile substance (7.4), %;
- mass fraction water (7.5), %;
is the density of the sample at a temperature of (23 ± 2) °C (7.3), g/cm;
g/cm; (0,997537 g/cm);
- conversion factor

8.5 Method 4: Mass concentration of VOCs, g/dm, in a "ready-to-use" material, excluding water and photochemically inactive compounds (used only if national legislation applies), calculated according to the formula

Where - mass concentration VOCs in "ready-to-use" material, excluding water and photochemically inactive compounds, g/dm;
- mass fraction non-volatile substance in the sample (7.4), %;
- mass fraction water in the sample (7.5), %;
- mass fraction-th photochemically inactive compound (7.6), %;
- density of the sample at a temperature of (23 ± 2) °C (7.3), g/cm;
is the density of water at a temperature of 23 °C, g/cm; (0,997537 g/cm);
is the density of the i-th photochemically inactive compound (7.6.3), g/cm;
- conversion factor.

9 Processing results

If the results of two replicate tests differ by more than that specified in 10.2, the test is repeated.
Calculate the average of the two valid replicate results and report the result to the nearest 1%.

10 Precision

10.1 General
The precision of the test method was determined from the results of an interlaboratory test conducted in accordance with GOST R ISO 5725-1 and GOST R ISO 5725-2. Three different materials were tested in 5-7 laboratories. Some of the obtained results were not taken into account when calculating the precision of this method, because they went beyond the scope of its application (Table 1, footnote a). Mass fraction The VOC for these materials was less than 15%, but they were only tested for better comparison with the level of precision provided by the GOST R 52486 test method.

Table 1 - Results of the interlaboratory test

10.2 Limit of repeatability
The repeatability limit is the value below which the absolute value of the difference between the results of two separate tests, each of which is the average of the results of two parallel tests performed on identical material by the same operator in the same laboratory within a short period of time, according to one standardized method, is expected to fall. .
The repeatability of the results for five repeated determinations by this method, expressed as a coefficient of variation in repeatability, is 1%.

10.3 Reproducibility limit
The reproducibility limit is the value below which the absolute value of the difference between the results of two tests, each of which is the average of the results of two replicate tests, obtained on identical material by operators in different laboratories using the same standardized method, is expected to fall.
The reproducibility of the results by this method, expressed as the reproducibility variation coefficient, is 2%.

11 Test report

The test report must contain the following data:

b) all information necessary to fully identify the material being tested (manufacturer's name, trademark, lot number, etc.);

c) supplementary information items referred to in Annex A;

e) the test results of Clause 8, the calculation method used (8.2, 8.3, 8.4 or 8.5);

f) any deviation from the specified test method;

g) the date of the test.

Annex A (mandatory). Required Additional Information

Annex A
(mandatory)

In order to be able to use the method specified in this International Standard, the additional information listed in this annex must be provided.
The necessary information should preferably be agreed between the interested parties, using as its source, in part or in whole, the relevant international or national standard or other technical document relevant to the product under test.

a) Organic compound(s) to be determined (if known).

b) Analytical methods to be used to identify these compounds.

c) Organic compounds (listing a) which are photochemically inactive (7.6).

d) Calculation method used (clause 8).

Annex B (informative). Information on the compliance of reference international standards with the national standards of the Russian Federation used in this standard as normative references

Annex B
(reference)

Table B.1

Bibliography

GOST R 52486-2010
(ISO 11890-2:2006)

Group L19

NATIONAL STANDARD OF THE RUSSIAN FEDERATION

Paintwork materials

DETERMINATION OF VOLATILE ORGANIC COMPOUNDS (VOC)

Gas chromatographic method

paint materials. Determination of volatile organic compound (VOC) content. Gas-chromatographic method

OKS 87.040
OKSTU 2309

Introduction date 2011-07-01

Foreword

The goals and principles of standardization in the Russian Federation are established by the Federal Law of December 27, 2002 N 184-FZ "On Technical Regulation", and the rules for the application of national standards of the Russian Federation - GOST R 1.0-2004 "Standardization in the Russian Federation. Basic provisions"

About the standard

1 PREPARED BY JSC "Scientific and Production Company "Spektr LK" on the basis of an authentic translation into Russian of the standard specified in paragraph 4, which was carried out by FSUE "STANDARTINFORM"

2 INTRODUCED by the Technical Committee for Standardization TC 195 "Paint and varnish materials"

3 APPROVED AND PUT INTO EFFECT by Order of the Federal Agency for Technical Regulation and Metrology dated November 30, 2010 N 796-st

4 This standard is modified from the international standard ISO 11890-2:2006 * "Paints and varnishes - Determination of volatile organic compounds (VOC) - Part 2: Gas chromatography method" (ISO 11890-2:2006 "Paints and varnishes - Determination of volatile organic compound (VOC) content - Part 2: Gas-chromatographic method"). At the same time, additional words and phrases included in the text of this standard to take into account the needs of the national economy of the Russian Federation and the peculiarities of Russian national standardization are highlighted in bold italics with a solid horizontal underline.
________________
* Access to international and foreign documents can be obtained by clicking on the link. - Database manufacturer's note.

Table 1 "Results of the interlaboratory test" containing reference data is excluded from section 12

5 INSTEAD OF GOST R 52486-2005 (ISO 11890-2:2000)


Information about changes to this standard is published in the annually published information index "National Standards", and the text of changes and amendments - in the monthly published information indexes "National Standards". In case of revision (replacement) or cancellation of this standard, a corresponding notice will be published in the monthly published information index "National Standards". Relevant information, notification and texts are also posted in the public information system - on the official website of the Federal Agency for Technical Regulation and Metrology on the Internet

1 area of ​​use

1 area of ​​use

This International Standard specifies a gas chromatographic method for the determination of volatile organic compounds (VOCs) in paintwork materials (LKM) and raw materials. This method is used for the expected mass fraction VOC from 0.1% to 15%. If the intended mass fraction VOC more than 15%, apply the method according to GOST R 52485.

The method is based on the assumption that the volatile substances are organic compounds or water. When in LKM volatile inorganic compounds are present, their content is determined by another method and the results obtained are taken into account in the calculations.

2 Normative references

This standard uses normative references to the following standards:

GOST R 52485-2005 (ISO 11890-1:2000) Paintwork materials. Determination of the content of volatile organic compounds (VOC). difference method (ISO 11890-1:2000 Paints and varnishes — Determination of volatile organic compounds (VOCs) — Part 1: Difference method, MOD)

GOST R 53654.1-2009 (ISO 2811-1:1997) Density determination method. Part 1. Pycnometric method (ISO 2811-1:1997 "Paints and varnishes - Determination of density - Part 1: Pycnometric method", MOD)

GOST 9980.2-86 (ISO 842-84, ISO 1512-74, ISO 1513-80) Paintwork materials. Sampling for testing (ISO 842-84 "Raw materials for the manufacture of varnishes and paints - Sampling", MOD; ISO 1512-74 "Paints and varnishes - Sampling", MOD; ISO 1513-80 "Paints and varnishes - Inspection and preparation of test samples" , MOD)

GOST 14870-77 Chemical products. Water determination methods (ISO 760:1978 Determination of water — Karl Fischer method (general method), NEQ)

Note - When using this standard, it is advisable to check the validity of reference standards in the public information system - on the official website of the Federal Agency for Technical Regulation and Metrology on the Internet or according to the annually published information index "National Standards", which was published as of January 1 of the current year , and according to the corresponding monthly published information signs published in the current year. If the reference standard is replaced (modified), then when using this standard, you should be guided by the replacing (modified) standard. If the referenced standard is canceled without replacement, the provision in which the reference to it is given applies to the extent that this reference is not affected.

3 Terms and definitions

In this standard, the following terms are used with their respective definitions:

3.1 volatile organic compound; VOC: Any organic compound having an initial boiling point less than or equal to 250°C, measured at normal pressure of 101.3 kPa.

3.3 paintwork material ready for use: paintwork after mixing it, if necessary, with other components and diluting with appropriate solvents and / or thinners in accordance with regulatory (ND) or technical documents(TD) , ready to be applied by the appropriate staining method.

4 Essence of the method

In sample LKM, ready for use, VOCs are separated by gas chromatography. Use a hot or cold sample injection system, depending on the type of material being tested. A hot sample injection system is preferred.

Once compounds have been identified, their amounts are calculated from peak areas using an internal standard.

Depending on the type of chromatograph, the water content can be determined.

Then calculate the total content of VOC in paintwork ready for use.

5 Required additional information

For the method specified in this International Standard, the additional information given in Annex A is necessary.

6 Equipment

6.1 Gas chromatograph

The instrument is installed and used in accordance with the manufacturer's instructions. All parts of the instrument that come into contact with the test sample shall be made of a material (e.g. glass) that is resistant to the sample, i.e. from a material that will not enter into a chemical reaction with it.

6.2 Sample introduction system

6.2.1 General

One of two types of input is used - according to 6.2.2 or 6.2.3.

6.2.2 Split hot sample injection system (preferred system)

The instrument shall have an evaporator, the temperature of which shall be controlled to the nearest 1 °C, and a flow divider. It is necessary to be able to regulate and control the division of flows. The flow divider liner must contain silane-treated glass wool to retain non-volatile components. The design of the appliance shall provide for the possibility of cleaning the liner and filling it with new glass wool packing or, if necessary, replacing it with a new one. This is due to the need to exclude errors caused by the accumulation of a film-forming substance or pigment (ie adsorption of compounds). The appearance of adsorption is indicated by the appearance of peak tails, which are especially pronounced in the case of low-volatile components.

6.2.3 Cold sample introduction system with flow divider

The cold sample introduction system shall be provided with a temperature programmed heater ranging from ambient temperature to 300 °C and shall have an inlet in the flow divider made of an inert material such as glass. The flow divider shall be packed with silane treated glass wool and maintained as specified in 6.2.2. It is necessary to be able to regulate and control the flow division.

The precision of the method can be improved if the sample injection system, especially in the case of hot injection, is connected to an automatic pipette. Follow the instrument manufacturer's instructions when using an automatic dispenser.

6.2.4 Selecting the sample introduction system

The choice between hot and cold sample introduction systems depends on the type of material being tested. The cold injection system must be used for materials that release substances at high temperatures that cause peaking.

The progress of the cleavage or decomposition reactions can be determined by changes in the chromatogram (eg appearance of unknown peaks and increase or decrease in peak size) at various evaporator temperatures.

The Hot Sample Injection System covers all sample volatiles, degradation products of film formers and additives. Cleavage products of film-forming agents or additives that are identical to the material components can be separated using a cold inlet system, since they are eluted later as a result of a programmed increase in the temperature of the evaporator.

The sample injection system must be specified in the RD or TD for a specific coating.

6.3 Thermostat

The thermostat must provide heating to a temperature of 40 °C to 300 °C both in isothermal mode and under conditions of programmable temperature change. It must maintain the temperature within ±1 °C. The end temperature of the heating program must not exceed the maximum operating temperature of the column (6.5).

6.4 Detector

Any of the following three detectors, or other detectors suitable for VOC detection, may be used.

6.4.1 Flame ionization detector (FID), operating at temperatures up to 300 °C. To prevent condensation, the temperature of the detector must be at least 10°C above the maximum thermostat temperature. Detector gas supply, sample injection volume, split ratio, and gain control must be optimized so that the signals (peak areas) used for calculation are proportional to the amount of substance.

6.4.2 Mass spectrometer, graduated and a tuned or other mass selective detector.

6.4.3 Fourier IR spectrometer, calibrated according to the manufacturer's instructions .

6.5 Capillary column

The column should be made of glass or fused silica.

It has been proven that columns of sufficient length, with a maximum internal diameter of 0.32 mm, coated with a film of polydimethylsiloxane or polyethylene glycol of appropriate thickness have a good separation capacity for the separation of VOCs.

The stationary phase and column length should be chosen to provide the desired separation (Appendix B, examples).

The combination of column length, temperature program, and labeling agent is chosen so that the boiling points of the VOC in the sample are below the boiling point of the labeling agent, i.e. VOCs should elute before the label substance, and non-VOC compounds after the label substance. If a polar stationary phase is used for VOC determination, it is recommended to use the tracers given in 7.4 in combination with a DB-1301 column or equivalent, at least 60 m long, 0.32 mm internal diameter and 1 µm film thickness.

The length, internal diameter of the column and the film thickness must be specified in the RD or TD for a specific coating.

6.6 Apparatus for qualitative analysis

Where separated components are identified using a mass selective detector or Fourier IR spectrometer, these instruments should be connected to a gas chromatograph and operated according to the manufacturer's instructions.

6.7 Injection syringe

The capacity of the syringe must be at least twice the volume of the sample being injected into the gas chromatograph.

6.8 Recorder

Compensation recorders are used to record the chromatogram.

6.9 Integrator

Peak areas are measured using electronic system data processing (integrator or computer). The integration parameters for calibration and analysis must be identical.

6.10 Sample containers

Use containers (flasks, test tubes, bottles), made of chemically resistant materials, such as glass, which must be tightly closed.

6.11 Gas filters

The connecting tubes of the gas chromatograph should contain filters to adsorb residual impurities in the feed gases (6.12).

6.12 Gases

6.12.1 Carrier gas: dry, oxygen-free helium, nitrogen, or hydrogen with a purity of at least 99.996% vol.

6.12.2 Gases for powering the detector: hydrogen with a purity of at least 99.999% vol. and air free from organic compounds.

6.12.3 Auxiliary gas: nitrogen or helium of the same purity as the carrier gas.

7 Reagents

7.1 Internal standard

The internal standard should be a substance that is not present in the sample and completely separates from other components in the chromatogram. It must be inert with respect to the components of the sample, stable over the required temperature range, and of known purity. Determined that for many coatings compounds such as isobutanol and diethylene glycol dimethyl ether are suitable. Usually the internal standard is selected experimentally. .

The internal standard must be specified in the ND or TD for a specific paintwork.

7.2 Connections for calibration

Compounds used for calibration must be at least 99% pure by weight. or be of known purity.

The connection for calibration must be indicated in the RD or TD for a specific material.

7.3 Thinner

An organic solvent is used to dilute the sample. It must have a purity of at least 99% of the mass. or be of known purity. The solvent must not contain compounds that give peaks that overlap in the chromatogram. The solvent is always tested separately to detect contamination and possible peak overlap, especially when analyzing trace substances. The solvent must be specified in the ND or TD for a specific paintwork .

NOTE Solvents such as methanol and tetrahydrofuran have been found to meet these requirements.

7.4 Label substance

For the determination of VOCs, it is necessary to use a label substance of known purity and a boiling point equal to the maximum limit of (250 ± 3) °C.

EXAMPLE The following can be used as a labeling substance: for non-polar systems - tetradecane, having a boiling point of 252.6 ° C; for polar systems - diethyl adipate having a boiling point of 251 °C.

8 Sampling

Take away average sample of coatings (or each material in the case of a multilayer system) according to GOST 9980.2.

Control and preparation of each sample - according to GOST 9980.2.

9 Testing

9.1 Density determination

The density of the test sample is determined according to GOST R 53654.1, if required for the calculation (10.3, 10.4). Density determination is carried out at a temperature of (23 ± 2) ° C, .

9.2 Determination of the mass fraction of water

The mass fraction of water is determined as a percentage according to GOST 14870 (method 2), choosing the reagents so that they do not interfere with the analysis of the compounds contained in the sample. If the connections are unknown, then they are determined qualitative analysis (9.4).

Notes

1 Typical compounds that may interfere with analysis are ketones and aldehydes. For the correct choice of reagents, one should be guided by the information provided by the manufacturer.

NOTE 2 If the properties of the material to be tested are well defined and it is known that it does not contain water, then the determination of the water content of this material can be omitted, assuming it to be zero.


The Fisher reagent* used must be specified in the RD or TD for a specific material.
_________________
* The text of the document corresponds to the original. - Database manufacturer's note.

9.3 Conditions for performing a gas chromatographic determination

9.3.1 The conditions for performing a gas chromatographic determination of VOCs depend on the material being tested and should be optimized each time using a known calibration mixture (see Annex B for examples of conditions used for hot and cold injection systems).

9.3.2 Sample injection volume and split ratio should be coordinated so as not to exceed column capacity and remain within the linear range of the detector. Asymmetric peaks indicate an overload of the gas chromatographic system.

9.4 Qualitative analysis of the product

9.4.1 If the organic compounds in the material are not known, they are determined by qualitative analysis. The most preferred for this purpose is a gas chromatograph connected to a mass selective detector or Fourier IR spectrometer (6.6) programmed with the same settings as given in 10.3.

9.5 Graduation

9.5.1 If the appropriate compounds are available, the correction factor is determined by the following procedure.

9.5.1.1 Weigh into the container (6.10), to the nearest 0,1 mg, the organic compounds determined in 9.4 in quantities which shall correspond to their content in the test sample.

Weigh the same amount of the internal standard (7.1) into a container, dilute the mixture with the solvent (7.3) and introduce it into the chromatograph under the same conditions as the test sample.

9.5.1.2 Optimize instrument settings in accordance with 9.3.

9.5.1.3 Re-introduce the required amount of calibration mixture into the gas chromatograph. Correction factors are calculated for each of the compounds according to the formula

where is the mass of the th compound in the calibration mixture, g;

- peak area of ​​the internal standard;

- mass of the internal standard in the calibration mixture, g;

is the peak area of ​​the i-th compound.

9.5.2 If the resulting peaks cannot be identified or compounds are not available, then the correction factors should be assumed to be 1.0.

9.6 Preparation of a paint sample ready for use

From 1 to 3 g of the sample is weighed into the container with an accuracy of 0.1 mg and the internal standard in an amount that should correspond to the content of the test material in the container is diluted with the appropriate amount of solvent, the container is carefully closed and the contents are mixed.

NOTE Samples containing pigments or other components that interfere with the test may be separated by centrifugation.

9.7 Quantification of VOC content

9.7.1 Set the chromatograph settings as during calibration optimization.

9.7.2 Using a separate gas chromatographic analysis, determine the retention time of the tracer. This retention time defines the summation cut-off point for calculating the VOC content from the chromatogram. Use a column that gives elution times related to the boiling point.

9.7.3 Introduce 0.1 to 1 mm of the test sample into the gas chromatograph and record the chromatogram. Peak areas are determined for all compounds with a retention time less than the label substances.

Calculate the mass of each compound, g, present in 1 g paintwork , according to the formula

where is the correction factor for the i-th connection (9.5.1.3);

Peak area of ​​the th compound;

Mass of the internal standard in the test sample (9.6), g;

Mass of the test sample (9.6), g;

Peak area of ​​the internal standard.

NOTE Some solvents, such as naphtha, will give multiple peaks when eluted. With most recording integrators, the total area of ​​the peaks can be summed and treated as a single peak, as long as no other compounds are eluting in that range. If the design of the integrator does not provide for such an operation in automatic mode, then the total area is summed up manually. Then the above formula can be used to determine the amount of solvent in the test sample.

9.7.4 Carry out two parallel determinations.

10 Calculations

10.1 General

Calculate the average value of the VOC content as the arithmetic mean of the two results of parallel determinations according to the method established in ND or TD for a specific paintwork . If in ND or TD no specific method is specified, the VOC content is calculated according to method 1.

Method 1 is the most preferred due to the fact that it provides high accuracy of results due to the absence of a density determination operation (which is a potential source of additional errors).

10.2 Method 1 Mass fraction VOC, %, in LKM , ready to use calculated according to the formula

100 is a conversion factor.

10.3 Method 2 Mass concentration VOC, g/dm , in paintwork , ready to use calculated according to the formula

where 1000 is the conversion factor;

is the mass of the i-th compound in 1 g of the test sample (9.7.3), g;

unless otherwise specified (9.1), g/cm .

10.4 Method 3 Mass concentration VOC, g/dm , in LKM , ready to use, with low water content, calculated according to the formula

where is the mass of the i-th compound in 1 g of the test sample (9.7.3), g;

The density of the test sample at a temperature of (23 ± 2) ° C, unless otherwise specified (9.1), g/cm ;

Mass of water in 1 g of the test sample (9.2), g;

The density of water at a temperature of (23 ± 2) ° С (0.997537 g/cm ), if other conditions are not specified, g/cm ;

1000 - conversion factor;

The density of the test sample at a temperature of (23 ± 2) ° C, if other conditions are not specified (9.1), g/cm .

11 Processing results

If the results of two parallel tests differ by more than that specified in 12.2, the test is repeated.

Calculate the mean of the two valid replicate results. If the values mass fraction more than 1%, then they are indicated in the protocol with an accuracy of 0.1%. If the values mass fraction less than or equal to 1%, then they are indicated in the protocol with an accuracy of 0.01%.

12 Precision

12.1 Limit of repeatability

The repeatability limit is the value below which the absolute value of the difference between the results of two separate tests, each of which is the average of the results of two parallel tests performed on identical material by the same operator in the same laboratory within a short period of time, according to one standardized method is expected to fall. tests.

The limit of repeatability of results for five repeated determinations by this method, expressed as a coefficient of variation in repeatability, ranges from 1% to 8%.

12.2 Reproducibility limit

The reproducibility limit is the value below which the absolute value of the difference between the results of two tests, each of which is the average of the results of two replicate tests, obtained on identical material by different operators in different laboratories using the same standardized test method, is expected to fall.

The limit of reproducibility of results by this method, expressed as a coefficient of reproducibility variation, ranges from 2% to 11%.

13 Test report

The test report must contain:

b) information needed to identify the material being tested (manufacturer's name, trademark, lot number, etc.);

c) supplementary information items referred to in Annex A;

e) the test results of Clause 9, the calculation method used (10.2-10.4);

f) any deviation from the specified test method;

g) the date of the test.

Annex A (mandatory). Required Additional Information

Annex A
(mandatory)

The application of this test method is possible only when using items a) to d) given in this annex.

The necessary information may be subject to agreement between the interested parties, or may be obtained in part or in whole from this International Standard or other documents relevant to the material being tested.

a) Organic compound(s) to be determined (Section 9).

b) Conditions under which the test should be carried out (clause 9).

c) The labeling substance used (7.4).

d) Calculation method used (clause 10).

Annex B (informative). Examples of conditions for conducting gas chromatographic determinations

Annex B
(reference)

B.1 Hot injection of waterborne material

B.2 Cold injection of waterborne material

B.3 Hot injection of water-free material

B.4 Cold injection of water-free material

Electronic text of the document
prepared by Kodeks JSC and verified against:
official publication
M.: Standartinform, 2011