Packaging - Evaluation of the ultimate aerobic biodegradability of packaging materials under controlled composting conditions - Method by analysis of released carbon dioxide

This European Standard specifies a method for the evaluation of the ultimate aerobic biodegradability of packaging materials based on organic compounds under controlled composting conditions by measurement of released carbon dioxide at the end of the test. This method is designed to resemble typical aerobic composting conditions for the organic fraction of mixed municipal solid waste. The packaging material is exposed in a laboratory test to an inoculum which is derived from compost. The aerobic composting takes place in an environment where especially temperature, aeration and humidity are closely monitored and controlled. The test method is designed to yield a percentage and rate of conversion of carbon of the test material to released carbon dioxide.
The conditions described in this European Standard do not necessarily always correspond to the optimal conditions allowing the maximum degree of biodegradation to occur.

Verpackung - Bestimmung der vollständigen aeroben biologischen Abbaubarkeit von Packstoffen unter kontrollierten Kompostierbedingungen - Verfahren mittels Analyse des freigesetzten Kohlenstoffdioxids

Diese Europäische Norm legt ein Verfahren zur Bestimmung der vollständigen aeroben biologischen Abbaubarkeit von Verpackungsmaterial fest, welches auf organischen Bestandteilen basiert. Das Verfahrensprinzip beruht auf kontrollierten Kompostierungsbedingungen und Messung des freigesetzten Kohlenstoffdioxids bis zum Ende der Prüfung. Dieses Verfahren ist in seinen Bedingungen einer typischen aeroben Kompostierung der organischen Fraktion von gemischtem, festem Siedlungsabfall ähnlich. Das zu prüfende Verpackungsmaterial wird in der Laborprüfung einem Kompostinokulum ausgesetzt. Die Bedingungen der aeroben Kompostierung, insbesondere Temperatur, Belüftung und Feuchtigkeit, werden genau aufgezeichnet und kontrolliert. Das Verfahren liefert als Ergebnis die prozentuelle Umsetzung des Kohlenstoffes aus dem Prüfmaterial in freigesetztes Kohlenstoffdioxid.
Die in dieser Europäischen Norm beschriebenen Bedingungen sind nicht notwendigerweise gleich jenen, die zum Erreichen der maximalen Umsetzungsrate in Kohlenstoffdioxid führen.

Emballage - Evaluation de la biodégradabilité aérobie ultime et de la désintégration des matériaux d'emballage dans des conditions contrôlées de compostage - Méthode par analyse du dioxyde de carbone libéré

Embalaža – Vrednotenje končne aerobne biorazgradljivosti in razkroja embalažnih materialov pod nadzorovanimi pogoji kompostiranja – Metoda z analizo sproščenega ogljikovega dioksida

General Information

Status
Published
Publication Date
30-Jun-2003
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-Jul-2003
Due Date
01-Jul-2003
Completion Date
01-Jul-2003

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.L]RVerpackung - Bestimmung der vollständigen aeroben biologischen Abbaubarkeit von Packstoffen unter kontrollierten Kompostierbedingungen - Verfahren mittels Analyse des freigesetzten KohlenstoffdioxidsEmballage - Evaluation de la biodégradabilité aérobie ultime et de la désintégration des matériaux d'emballage dans des conditions contrôlées de compostage - Méthode par analyse du dioxyde de carbone libéréPackaging - Evaluation of the ultimate aerobic biodegradability of packaging materials under controlled composting conditions - Method by analysis of released carbon dioxide55.040SDNLUDQMHPackaging materials and accessories13.030.99Drugi standardi v zvezi z odpadkiOther standards related to wastesICS:Ta slovenski standard je istoveten z:EN 14046:2003SIST EN 14046:2003en01-julij-2003SIST EN 14046:2003SLOVENSKI
STANDARD



SIST EN 14046:2003



EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14046March 2003ICS 13.030.99; 55.040English versionPackaging - Evaluation of the ultimate aerobic biodegradabilityand disintegration of packaging materials under controlledcomposting conditions - Method by analysis of released carbondioxideEmballage - Evaluation de la biodégradabilité aérobieultime et de la désintégration des matériaux d'emballagedans des conditions contrôlées de compostage - Méthodepar analyse du dioxyde de carbone libéréVerpackung - Bestimmung der vollständigen aerobenbiologischen Abbaubarkeit und Desintegration vonPackstoffen unter kontrollierten Kompostierbedingungen -Verfahren mittels Analyse des freigesetztenKohlenstoffdioxidsThis European Standard was approved by CEN on 27 December 2002.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and UnitedKingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2003 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14046:2003 ESIST EN 14046:2003



EN 14046:2003 (E)2ContentspageForeword.31Scope.42Normative references.43Terms and definitions.44Principle.55Test Environment.56Reagents.67Apparatus.67.1Composting vessels.67.2Air circulation system.67.3Apparatus for the determination of carbon dioxide.67.4Gas tight tubes.67.5pH meter.67.6Analytical instruments.67.7Balance.67.8Analytical instruments (optionally).68Procedure.78.1Preparation of the inoculum.78.2Preparation of the test material and the reference substance.78.3Start-up of the test.88.4Incubation period.88.5Termination of the test.99Calculation and expression of results.99.1Calculation of the theoretical amount of carbon dioxide.99.2Calculation of the percentage of biodegradation.109.3Calculation of weight loss.109.4Expression of results.1010Validity of results.1011Test Report.11Annex A (informative)
Principle of a test system with released carbon dioxide.12Annex B (informative)
Example of a carbon dioxide release and a biodegradation curve.13Annex C (informative)
Example of weight loss determination.15Annex D (informative)
Information - Ring test.18Annex E (informative)
Example of form sheets.19Bibliography.22SIST EN 14046:2003



EN 14046:2003 (E)3ForewordThis document (EN 14046:2003) has been prepared by Technical Committee CEN/TC 261 "Packaging", thesecretariat of which is held by AFNOR.This European Standard shall be given the status of a national standard, either by publication of an identical text orby endorsement, at the latest by September 2003, and conflicting national standards shall be withdrawn at thelatest by September 2003.This document has been prepared under a mandate given to CEN by the European Commission and the EuropeanFree Trade Association.This document contains annexes A, B, C, D and E, which are informative.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal,Slovak Republic, Spain, Sweden, Switzerland and the United Kingdom.SIST EN 14046:2003



EN 14046:2003 (E)41 ScopeThis European Standard specifies a method for the evaluation of the ultimate aerobic biodegradability of packagingmaterials based on organic compounds under controlled composting conditions by measurement of released carbondioxide at the end of the test. This method is designed to resemble typical aerobic composting conditions for theorganic fraction of mixed municipal solid waste. The packaging material is exposed in a laboratory test to an inoculumwhich is derived from compost. The aerobic composting takes place in an environment where especially temperature,aeration and humidity are closely monitored and controlled. The test method is designed to yield a percentage andrate of conversion of carbon of the test material to released carbon dioxide.The conditions described in this European Standard do not necessarily always correspond to the optimal conditionsallowing the maximum degree of biodegradation to occur.2 Normative referencesNot applicable.3 Terms and definitionsFor the purposes of this European Standard, the following terms and definitions apply.3.1test materialpackaging materials made from organic compounds normally tested in compact forms at a suitable size3.2ultimate biodegradation of a test materiallevel of biodegradation achieved when the test material is utilised by micro-organisms resulting in the production ofcarbon dioxide, water, mineral salts and new microbial cellular constituents (biomass)3.3total dry solidsamount of solids obtained by taking a known amount of test material or compost and drying at about 105 °C toconstant weight3.4volatile solidsamount of solids obtained by subtracting the residues of a known amount of test material or compost afterincineration at about 550 °C from the total dry solids content of the same sample. The volatile solids content is anindication of the amount of organic matter3.5theoretical amount of formed carbon dioxide (ThCO2)theoretical maximum amount of carbon dioxide formed after oxidising a chemical compound completely, calculatedfrom the molecular formula; expressed in this case as mg carbon dioxide per mg or g test compound3.6lag-phasetime from the start of a test until adaptation and/or selection of the degrading micro-organisms are achieved andthe biodegradation degree of a chemical compound or organic matter has increased to about 10 % of the maximumlevel of biodegradation, recorded in days3.7maximum level of biodegradationmaximum biodegradation degree of a chemical compound or organic matter in a test, recorded in per cent, abovewhich no further biodegradation takes place during the testSIST EN 14046:2003



EN 14046:2003 (E)53.8biodegradation phasetime from the end of the lag phase of a test until about 90 % of the maximum level of biodegradation has beenreached, recorded in days3.9plateau phasetime from the end of the biodegradation phase until the end of the test, recorded in days4 PrincipleThe test method is designed to be an optimised simulation of an intensive aerobic composting process anddetermines the ultimate biodegradability of a test material under controlled aerobic composting conditions. Theinoculum consists of stabilised and mature compost if possible derived from composting the organic fraction ofmunicipal solid waste.The test material is mixed with the inoculum and introduced into a static composting vessel where it is intensivelycomposted under optimum oxygen, temperature and moisture conditions for a test period of usually 45 or more days.During the aerobic biodegradation of the test material, carbon dioxide, water, mineral salts and new microbialcellular constituents (biomass) are the ultimate biodegradation products. The carbon dioxide produced iscontinuously monitored or measured at regular intervals in the test and blank vessels and integrated to determinethe cumulative carbon dioxide production. The percentage of biodegradation is obtained by comparing the carbondioxide produced from the test material to the maximum amount of carbon dioxide which could be derived from thetest material and which is calculated from its measured total organic carbon (TOC). This percentage ofbiodegradation will not include the amount of carbon converted to new cell biomass which is not in turn metabolisedto carbon dioxide during the course of the test.Additionally at the end of the test the weight loss of test material may be determined.5 Test EnvironmentIncubation shall take place in the dark or in diffused light in an enclosure which is maintained at a constanttemperature of 58 °C ± 2 °C and which is free from vapours inhibiting to micro-organisms.SIST EN 14046:2003



EN 14046:2003 (E)66 ReagentsUse only reagents of recognised analytical grade.Use as reference substance for a positive test control cellulose for thin-layer chromatography with a particle size ofless than 20 m.7 Apparatus7.1 GeneralEnsure that all glassware is thoroughly cleaned and, in particular, free from organic or toxic matter.7.2 Composting vesselsGlass flasks or bottles allowing an even gas purge in an upwards direction.NOTEA minimum volume of 2 l should fulfil the prerequisites mentioned in 8.2 and 8.3. For screening purpose, depending onthe test material also smaller volumes may be used. If the weight loss of the test material is determined weigh each emptycomposting vessel.7.3 Air circulation systemCapable of supplying each composting vessel with dry or humidified, if required carbon dioxide free, air at a pre-setflow rate which shall be high enough to provide truly aerobic conditions during the test (example see annex A).7.4 Apparatus for the determination of carbon dioxideDevice for direct carbon dioxide determination or after complete absorption in a basic solution and determination ofthe dissolved inorganic carbon (DIC) (example see annex A). If the exhausted air is directly be measured e.g. with acontinuous infrared analyser or a gas chromatograph an exact dosing or measurement of the gas flow is required.7.5 Gas tight tubesWhich prevent diffusion of oxygen and carbon dioxide to connect the composting vessels with air production andcarbon dioxide determination system.7.6 pH meter7.7 Analytical instrumentsFor determination of dry solids (at 105 °C), volatile solids (at 550 °C), total organic carbon (TOC) or elementalanalysis of compact material and dissolved inorganic carbon (DIC) in the case of DIC measurement.7.8 BalanceTo measure the weight of test vessels including compost and test material which is normally in a range between3 kg and 5 kg.7.9 Analytical instruments (optionally)For the optional determination of oxygen in the air, moisture, volatile fatty acids and total nitrogen (e.g. by the Kjeldahlmethod ISO 5663).SIST EN 14046:2003



EN 14046:2003 (E)78 Procedure8.1 Preparation of the inoculumTake as inoculum well aerated compost from a properly operating aerobic composting plant.NOTE 1It is recommended that compost from a plant composting the organic fraction of municipal solid waste is used in orderto get a sufficient range of micro-organisms which may be adapted to packaging materials. The age of the compost should bepreferably between 2 and 4 months. If such a compost is not available also compost from plants treating green or yard waste ormixtures of green waste and municipal solid waste (bio-waste) may be used. Such a compost may be less adapted to packagingmaterial.The compost inoculum should be homogeneous and as free from larger inert materials such as glass, stones ormetals. Remove them manually and then sieve the compost on a screen of about 0,5 cm to 1 cm.NOTE 2It is recommended to use compost with sufficient porosity to enable as aerobic conditions as possible. Addition ofstructural material such as small wood particles or persistent or poorly biodegradable inert material may avoid sticking together andclogging of the compost during the test.Determine the total dry solids and the volatile solids content of the compost inoculum. The total dry solids contentshould be between 50 % and 55 % of the wet solids and the volatile solids more than about 15 % of the wet or30 % of the dry solids. Adjust the water content, if necessary, before the compost is used by adding water or gentlydrying, e.g. by aerating the compost with dry air.Prepare a mixture of 1 part of compost inoculum with 5 parts of de-ionised water. Mix by shaking and measureimmediately the pH value which should be between 7,0 and 9,0.NOTE 3For further characterisation of the compost inoculum suitable parameters such as the content of total organic carbon,total nitrogen or fatty acids can be determined at the beginning and the end of the test (optionally).Check the activity of the compost inoculum during the test by means of a biodegradable reference substance (see 6)and by measuring the carbon dioxide evolution in the blank vessels. The reference substance should be degraded at> 70 % at the end of the test (see 10). The inoculum in the blank control should produce between 50 and 150 mg ofcarbon dioxide per g of volatile solids over the first 10 days of the test (see 10). If the production of carbon dioxide istoo high, the compost should be stabilised by aeration for several days before it is used in a new test. If the activity istoo low an other compost inoculum should be used.8.2 Preparation of the test material and the reference substanceDetermine the total organic carbon (TOC) of the test material and the reference substance cellulose (see 6), usinge.g. ISO 8245 and indicate it preferably as g TOC per g total dry solids. Alternatively, if the materials do not containinorganic carbon it is possible to determine the carbon content by elemental analysis. The test material shall havesufficient organic carbon to yield carbon dioxide in an amount suitable for the determination. Normally a minimum of50 g total dry solids containing 20 g TOC per vessel is required.Determine the total dry solids of the test material and the volatile solids if the weight loss shall be determined (seeNote hereafter).NOTEThe loss of test material and reference substance during the test can be determined optionally as an additionalinformation. In the example given in annex C the amount of volatile solids of the test material is determined and compared with theamount at the end of the test.Investigate the test material in the form of films, formed articles like
tensile bars, granules or powder. The maximumsurface area of a compact test material used should be about 2 cm ´ 2 cm. In case the original test material is larger,reduce it in particle size.SIST EN 14046:2003



EN 14046:2003 (E)88.3 Start-up of the testSet up a sufficient number of composting vessels (7.2) so that the test includes at least the following:a) 3 vessels for the test material ;b) 3 vessels for the reference substance ;c) 3 vessels for the blank control.The amount of the test mixture, containing compost inoculum and test material, used in the test depends on thequality of the test material (see 8.2) and the size of the composting vessels (see 7.2). The relation between the dryweight of compost inoculum and dry weight of test material should be about 6 : 1. Be sure that the same amount ofcompost is in each vessel. Inert material if added is not considered in this relationship (see Note 2 in 8.1). About 3/4 ofthe volume of the compost vessel should be filled with the test mixture. Sufficient of headspace is required in order toprovide enough space for manual shaking of the test mixture.In a typical case prepare composting vessels which have a volume of about 3 l, weigh out 600 g of total dry solidsof inoculum (7.2) and 100 g dry solids of the test material and mix well. The test mixture should have the samewater content of about 50 % as the inoculum (see 8.1). It should feel somewhat sticky and have some free wateravailable when gently pressed by hand. Adjust the moisture content of the mixture, if required, by adding water.Introduce the mixture into the vessels.NOTE 1It is recommended that the ratio between organic carbon and nitrogen (C/N-ratio) of the test mixtures is optimised soas to ensure a good composting process. The C/N ratio for the test mixture should be between 10 and 40, it may be adjusted withurea, if necessary. The organic carbon content can be calculated from the TOC of the compost inoculum and the test material. The
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