Astm d6400

ASTM STANDARDS PERTAINING TO THE
BIODEGRADABILITY AND
COMPOSTABILITY OF PLASTICS
Sponsored by Subcommittee D20.96 on Environmentally

Degradable Plastics
1999
Stock #: COMPOST
ASTM
100 Barr Harbor Drive,
West Conshohocken, PA 19428-2959
Editorial Staff
Director, Technical Publishing Services: Editors:

Roberta A. Storer Robert F. Allen Patricia A. McGee
Nicole C. Baldini Kathleen A. Peters
Manager, Standards Publications: Patricia E. Donofrio Susan Sandler
Joan L. Cornillot Elizabeth L. Gutman Todd J. Sandler
Paula C. Fazio-Fluehr Eleanor Keefe Richard F. Wilhelm
Senior Indexer: Joanne G. Kramer
Editorial Assistants:
H. Joel Shupak Christine M. Leinweber
Audrey Lewandowski
Vernice A. Mayer
Emilie A. Whealen
Library of Congress Cataloging-in-PublicationData
American Society for Testing and Materials.

ASTM standards pertaining to the biodegradability and
compostability of plastics / sponsored by Subcommittee
D20.96 on Environmentally Degradable Plastics.
p. cm.
Includes bibliographical references.
“ASTM Stock #: COMPOST.”
ISBN 0-803 1-2720-0
1. Plastics-Biodegradation-Standards. 2. Plastic
scrap-Deterioration. 3. Compost. I. ASTM Subcommittee D20.96 on
Environmentally Degradable Plastics. 11. Title.
TD798.A47 1999 99-35158
620.1‘923234~21 CIP
COPYRIGHT 0 1999 AMERICAN SOCIETY FOR TESTING AND MATERIALS, West Conshohocken, PA. All rights reserved. This
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Printed in Philadelphia, PA
July 1999
FOREWORD
This book is a compilation of the key documents that were developed by Subcommittee D20.96 on Environmentally Degradable Plastics for the
testing and identification of plastics that will biodegrade and compost satisfactorily. These standards are based on the work initiated by Interna-
tional Standards Research at the request of ASTM as well as leading scientists in the U.S. and other parts of the world. The key standard is Spec-
ification D 6400-99. The other standards are referenced in Specification D 6400-99 and are necessary to meet the criteria listed in Specification D
6400-99.
This compilation contains the following standards:
D 6400-99, Specification for Compostable Plastics, which ( I ) identifies plastics and products made from plastics designed to be composted in
municipal and industrial aerobic composting facilities, and (2) determine if plastics and products made from plastics will compost satisfacto-
rily, including biodegrading at a rate comparable to known compostable materials.
D 6002-96, Guide for Assessing the Compostability of Environmentally Degradable Plastics, which outlines the recommended criteria, proce-
dures, and a general approach to establish the compostability of plastics.
D 5338-98, Test Method for Determining Aerobic Biodegradation of Plastic Materials Under Controlled Composting Conditions, which deter-
mines the degree and rate of aerobic biodegradation of plastic materials on exposure to a controlled-composting environment under labora-
tory conditions.
D 6340-98, Test Methods for Determining Aerobic Biodegradation of Radiolabeled Plastic Materials in an Aqueous or Compost Environment,
which are applicable for determining the degree and rate of aerobic biodegradation of plastics whose biodegradation rate is slow and requires
test periods for as long as 365 days. These test methods require radiolabeling the selected carbon of the plastic polymer materials and monti-
toring the conversion of the radiolabeled carbon of the polymer to C02.
Suggestions and comments regarding this compilation are welcome and should be addressed to Product Manager, Publications, ASTM, 100Barr
Harbor Dr., West Conshohocken, PA 19428-2959.
ASTM
ASTh4, founded in 1898, is a developer and publisher of technical information designed to promote the understanding and development of tech-
nology and to ensure the quality of commodities and services and safety of products.
ASTM’s primary mission is to develop voluntary full consensus standards for materials, products, systems, and services. It provides a forum for
producers, users, ultimate consumers, and those having a general interest (representatives of government and academia) to meet on common
ground to write standards that best meet their needs.
iii
ASTM Standards: Page:
D 6400-99 Specification for Compostable Plastics 1
D 6002-96 Guide for Assessing the Compostability of Environmentally Degradable Plastics 4
D 5338-98 Test Method for Determining Aerobic Biodegradation of Plastic Materials Under Controlled Composting
Conditions 10
D 6340-98 Test Methods for Determining Aerobic Biodegradation of Radiolabeled Plastic Materials in an Aqueous or
Compost Environment 16
Committee D-20 Membership Application 23
V
[Tb Designation: D 6400 - 99
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohccken. PA 19428
Reprinted from the Annual Book of ASTM Standards. Capyright ASTM
Standard Specification for

Compostable Plastics‘
This standard is issued under the fixed designation D 6400, the number immediately following the designation indicates the year of .
.. _______
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 2.3 Association Francaise de Normalisation (CEN) Stan-

1.1 This specification covers plastics and products made dard:5
from plastics that are designed to be composted in municipal CEN/TC 261/SC 4 N 99 Packaging-Requirements for
and industrial aerobic composting facilities. Packaging Recoverable through Composting and
1.2 This specification is intended to establish the require- Biodegradation-Test Scheme and Evaluation Criteria for
ments for labeling of materials and products, including pack- the Final Acceptance of Packaging (WI 261 236)
aging made from plastics, as “compostable in municipal and 2.4 I S 0 Standard:5
industrial composting facilities.’’ IS0 14855 Evaluation of the Ultimate Aerobic Biodegrad-
1.3 The properties in this specification are those required to ability and Disintegration of Plastics under Controlled
determine if plastics and products made from plastics will Composting Conditions-Method by Analysis of Evolved
compost satisfactorily, including biodegrading at a rate com- Carbon Dioxide
parable to known compostable materials. Further, the proper- 2.5 Government Standard:6
ties in the specification are required to assure that the degra- 40 CFR Part 503.13 Standards for the Use or Disposal of
dation of these materials will not diminish the value or utility Sewage Sludge
of the compost resulting from the composting process. 3. Terminology
1.4 The following safety hazards caveat pertains to the test
methods portion of this standard This standard does not 3.1 Dejinitions-Definitions appearing in this specification
purport to address all of the safety concerns, ifany, associated are found in Terminology D 883, unless otherwise noted.
with its use. It is the responsibility of the user of this standard 3.1.1 biodegradable plastic-a degradable plastic in which
to establish appropriate health and safety practices and to the degradation results from the action of naturally occurring
determine the applicability of regulatory limitations prior to microorganisms such as bacteria, fungi, and algae.
use. 3.1.2 compostable plastic-a plastic that undergoes degra-
dation by biological processes during composting to yield CO’,
Nom 1-No equivalent IS0 specifications exist for this standard. water, inorganic compounds, and biomass at a rate consistent
2. Referenced Documents with other known compostable materials and leave no visible,
distinguishable or toxic residue.
2.1 ASTM Standards: 3.1.3 composting7-a managed process that controls the
D 883 Terminology Relating to Plastics’ biological decomposition and transformation of biodegradable
D 5338 Test Method for Determining Aerobic Biodegrada- materials into a humus-like substance called compost: the
tion of Plastic Materials Under Controlled Composting aerobic mesophilic and thermophilic degradation of organic
Conditions3 matter to make compost; the transformation of biologically
D 6002 Guide for Assessing the Compostability of Environ- decomposable material through a controlled process of biooxi-
mentally Degradable Plastics3 dation that proceed through mesophilic and thermophilic
2.2 Organization for Economic Development (OECD) phases and results in the production of carbon dioxide, water,
Standard:4 minerals, and stabilized organic matter (compost or humus).
OECD Guideline 208 Terrestrial Plants, Growth Test 3.1.3.1 Discussion-Composting uses a natural process to
stabilize mixed decomposable organic material recovered from
municipal solid waste, yard trimmings, biosolids (digested
‘This specification is under the jurisdiction of ASTM Committee D-20 on
sewage sludge), certain industrial residues and commercial
Plastics and is the direct responsibility of Subcommittee D20.96 on Environmen- residues.
tally Degradable Plastics.
Current edition approved April 10, 1999. Published May 1999.
Annual Book of ASTM Stanaizrds, Vol08.01.
’Available from American National Standards Institute, 11 W. 42nd St., 13th
Floor, New York, NY 10036.
Annual Book of ASTM S r a h d s , Vol08.03. Code of Federal Regulations, available from U.S.Government Printing Oilice,
Available from Organization for Economic Development, Director of Informa- Washington, DC 20402.
tion, 2 rue Andre’ Pascal, 75775 Paris Cedex 16, France. ’Composr Facility Operating Guide, Composting Council, Alexandria, VA,
1995.
1
(b D6400
3.1.4 degradable plastic-a plastic designed to undergo a should be tested in the same form as they are intended to be
significant change in its chemical structure under specific used. For products that are made in multiple thicknesses or
environmental conditions, resulting in a loss of some properties densities, such as films, containers and foams, only the thickest
that may be measured by standard test methods appropriate to or most dense products need to be tested as long as the
the plastic and the application in a period of time that chemical composition and structure remains otherwise the
determines its classification. same. It is assumed that thinner gages and lower densities will
3.1.5 plastic-a material that contains as an essential ingre- also compost satisfactorily. Similarly,if additives are present in
dient one or more organic polymeric substances of large test samples that pass testing, lower levels of the same
molecular weight, is solid in its finished state, and, at some additives are similarly passed.
stage in its manufacture or processing into finished articles, can 6.2 A plastic product is considered to have demonstrated
-
be shaped by flow. satisfactory disintegration if after controlled laboratory-scale
3.1.6 polymer-a substance consisting of molecules charac- composting, found in 7.2.1 of Guide D6002, no more than
terized by the repetition (neglecting ends, branch junctions, 10 % of its original dry weight remains after sieving on a
other minor irregularities) of one or more types of monomeric 2.0-mm sieve.
units. 6.3 A plastic product must demonstrate a satisfactoryrate of
biodegradation by achieving one of the following ratios of
4. Classification conversion to carbon dioxide found in 6.3.1, 6.3.2 or 6.3.3,
4.1 The purpose of this specification is to establish stan- within the time periods specified in 6.3.3.1 or 6.3.3.2, using
dards for identifying products and materials that will compost Test Method D 5338 as outlined in 7.3.1 and 7.3.3 of Guide
satisfactorily in commercial and municipal composting facili- D 6002:
ties. Products meeting the requirements outlined below are 6.3.1 For products consisting of a single polymer (ho-
appropriate for labeling as “compostable” in accordance with mopolymers or random copolymers), 60 % of the organic
the guidelines issued by the Federal Trade Commission.* carbon must be converted to carbon dioxide by the end of the
test period (see 6.3.4), when compared to a known reference
5. Basic Requirements material as outlined in 7.3.2 of Guide D 6002.
5.1 In order to compost satisfactorily,a product or material 6.3.2 For products consisting of more than one polymer
must demonstrate each of the characteristics found in 5.1.1- (block copolymers, segmented copolymers, blends, or addition
5.1.3, and which are quantified in Section 6. of low molecular weight additives), 90 % of the organic carbon
5.1.1 Disintegration During Composting-A plastic prod- must be converted to carbon dioxide by the end of the test
uct or material will disintegrate during composting such that period (see 6.3.4), when compared to a known reference
any remaining plastic residuals are not readily distinguishable material as outlined in 7.3.2 of Guide D 6002.
from the other organic materials in the finished product. 6.3.3 For products consisting of more than one polymer,
Additionally, the material or product must not be found in
each individual polymer component, present at more than 1 %
significant quantities during screening prior to final distribution
concentration, must achieve the 60 % specification for ho-
of the compost. mopolymers, as described in 6.3.1.
5.1.2 Inherent Biodegradation-A level of inherent biodeg-
radation shall be established by tests under controlled condi- 6.3.3.1 For materials that are not radiolabeled, the test
tions, that are comparable to known compostable materials. period shall be no greater than 180 days.
5.1.3 No Adverse Impacts on Ability of Compost to Support 6.3.3.2 If radiolabeled materials are used, then the test
Plant Growth-The tested materials shall not adversely impact period may be as long as 365 days.
on the ability of composts to support plant growth, when Nom 3-While the end points of biodegradation may include incorpo-
compared to composts using cellulose as a control, once the ration into biomass or humic substances as well as carbon dioxide, no
finished compost is placed in soil. Additionally, the polymeric recognized standard test methods and specifications exist to quantify these
products or materials must not introduce unacceptable levels of outcomes. When these tests and specifications become available, this
heavy metals or other toxic substances into the environment, standard will be revised.
upon sample decomposition. 6.4 A plastic product can demonstrate satisfactory terrestrial
NOTE>For a better understandingof why these criteria are important, and aquatic safety if it fulfills the following requirements:
the reader should consult Guide D6002 Compost Facility Operating 6.4.1 The plastic or product shall have concentrations of
Guide? and CEN/TC 261/SC 4 N 99. heavy metals less than 50 % of those prescribed in 40 CFR Part ~
6. Detailed Requirements 503.13, and

6.4.2 The plastic or product shall fulfill the requirements of
6.1 In order to be identified as compostable, products must the tests found in 7.5.2.2 and 7.5.2.3 of Guide D 6002,
pass the requirements of 6.2,6.3, and 6.4 using the appropriate including the cress seed test for plant germination and a plant ~
laboratory tests, representative of the conditions found in growth test following OECD Guideline 208.
aerobic composting facilities. Products and finished articles
7. Sampling
‘Guidelines for thc Use of Environmental Marketing Claims, Federal Trade 7.1 Sampling shall be conducted as indicated in the speci-
Commission. Washington, DC, 1992. fied test method.
2
8. Specimen Preparation 10. Keywords
8.1 SpeCh" Preparation shall be in accordance With the 10.1 biodegradable; compostable plastic; composting; de-
specified test method. gradable plastics; labeling
9. Marking and Labeling
9.1 Marking and labeling shall conform to national and
local regulations.
TheAmerican Society for Testingand Materials takes no position respecting the validity of anypatent rights assededin connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent fights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your commentsare invited either for revision of this standard or for additionalstandards
and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your
views known to the ASTM Committee on Standards, 100 Ban Harbor Drive, West Conshohocken, PA 19428.
3
Designation: D 6002 - 96
Standard Guide for

Assessing the Compostability of Environmentally Degradable
Plastics’
This standard is issued under the fved designation D 6002; the number immediately following the designation indicates the year of
1. Scope E 1440 Guide for an Acute Toxicity Test with the Rotifer
I. 1 This guide covers suggested criteria, procedures, and a Brachionus’
general approach to establish the compostability of environ- E 1720 Test Method for Determining Ready, Ultimate,
mentally degradable plastics. Biodegradability of Organic Chemicals in a Sealed
1.2 This standard does not purport to address all of the Vessel COz Production Test5
safety concerns, if any, associated with its use. It is the G22 Practice for Determining Resistance of Plastics to
responsibility of the user of this standard to establish appro- Bacteria6
priate safety and health practices and determine the applica- 2.2 ORCA Document:
bility of regulatory limitations prior to use. Guidelines for the Evaluation of Feedstock for Source
Separated Biowaste Composting and Biogasification’
2. Referenced Documents 2.3 OECD Guidelines?‘
OECD Guideline 207 Earthworm, Acute Toxicity Tests
2.1 ASTM Standards: OECD Guideline 208 Terrestrial Plants. Growth Test
D 638 Test Method for Tensile Properties of Plastics’
D 882 Test Methods for Tensile Properties of Thin Plastic
Sheeting2 3. Terminology
D 883 Terminology Relating to Plastics’ 3.1 Definitions:
D 3593 Test Method for Molecular Weight Averages/ 3.1.1 biodegradableplastic-a degradable plastic in which
Distribution of Certain Polymers by Liquid Size-Ex- the degradation results from the action of naturally occurring
clusion Chromatography (Gel Permeation Chromatog- microorganisms such as bacteria, fungi, and algae. D 883
raphy (GPC)) Using Universal Calibration3 3.1.2 compostable-capable of undergoing biological de-
D 5 152 Practice for Water Extraction of Residual Solids composition in a compost site as part of an available
from Degraded Plastics for Toxicity Testing4 program, such that the material is not visually distinguish-
D 5209 Test Method for Determining the Aerobic Biodeg- able and breaks down into carbon dioxide, water, inorganic
radation of Plastic Materials in the Presence of Munic- compounds, and biomass, at a rate consistent with known
ipal Sewer Sludge4 compostable materials.
D 5247 Test Method for Determining the Aerobic Biode- 3.1.3 composting-a managed process that controls the
gradability of Degradable Plastics by Specific Micro- biological decomposition and transformation of biodegrad-
organisms4 able material into a humus-like substance called compost;
D 5338 Test Method for Determining Aerobic Biodegrada- the aerobic mesophilic and thermophilic degradation of
tion of Plastic Materials Under Controlled Composting organic matter to make compost; the transformation of
Conditions4 biologically decomposable material through a controlled
D5509 Practice for Exposing Plastics to a Simulated process of bio-oxidation that proceeds through mesophilic
Compost Environment4 and thermophilic phases and results in the production of
D 55 12 Practice for Exposing Plastics to a Simulated carbon dioxide, water, minerals, and stabilized organic
Compost Environment Using an Externally Heated matter (compost or humus). Composting uses a natural
Reactor” process to stabilize mixed decomposable organic material
D 595 1 Practice for Preparing Residual Solids Obtained recovered from municipal solid waste, yard trimmings,
After Biodegradability Standard Methods for Plastics in biosolids (digested sewage sludge), certain industrial residues,
Solid Waste for Toxicity and Compost Quality Testing4 and commercial residues (l).9
D 5988 Test Method for Determining the Aerobic Biodeg- 3.1.4 degradable plastic-a plastic designed to undergo a
radation in Soil of Plastic Materials or Residual Plastic significant change in its chemical structure under specific
Materials after Composting4
5 Annual Book of ASTM Standards, Vol I 1.05.

This guide is under the jurisdiction of ASTM Committee D-20 on Plastics and 6 Annual Book ofASTM Standards, Vol 14.02.
is the direct responsibility of Subcommittee D20.96 on Environmentally Available from Organic Reclamation and Composting Association, Avenue E.
Degradable Plastin. Mounier 83, Box I , B- I200 Brussels, Belgium.
Current edition approved Aug. IO, 1996. Published October 1996. 8 Available from Organization for Economic Development, Director of Infor-
Annual Book of ASTM Standards, Vol08.0 I. mation, 2 rue Andre’ Pascal,75775 Paris Cedex 16, France.
3 Discontinued-See 1992 Annual Book of ASTM Standards, Vol08.03. 9 The boldface numbers in parentheses refer to the list of references at the end
Annual Book of ASTM Standards, Vol08.03. of this guide.
4
## D6002
environmental conditions, resulting in a loss of some prop- formed, under mesophilic conditions, to obtain information
erties that may be measured by standard methods appro- unavailable from literature review. The objectives are as
priate to the plastic and the application in a period of time follows:
that determines its classification. D 883 6.1.1 To determine whether biodegradation of polymeric
3.1.5 mesophilic phase-the phase of composting that materials and other organic components in the plastic
occurs between 20 and 45°C (68 and 113°F) (1). product can occur. Biodegradation is based on carbon
3.1.6 plastic-a material that contains as an essential dioxide production. ~ --
ingredient one or more organic polymeric substances of large 6.1.2 To expand understanding of the degradation mech-
molecular weight, is solid in its finished state, and, at some anism.
stage in its manufacture or processing into finished articles,
can be shaped by flow. D 883 NOTE4-A positive result in Tier 1 tests is not required to
demonstrate the compostability of product components. Components
3.1.7 polymer-a substance consisting of molecules char- which fail Tier 1 tests might prove successful in Tier 2 composting tests.
acterized by the repetition (neglecting ends, branch junc- If a component fails Tier 1, but is still considered promising, it should
tions, and other minor irregularities) of one or more types of advance to Tier 2. Likewise, a promising component could enter the test
monomeric units. D 883 strategy directly at Tier 2.
3.1.8 thermophilic phase-the phase in the composting NOTE5-Chemical analysis, (for example, regulated heavy metals) of
process that occurs between 45 and 75°C (1 13 and 167°F);it product component may be appropriate prior to initiation of testing.
is associated with specific colonies of microorganisms that 6.2 The following test methods are suggested for initial
accomplish a high rate of decomposition (1).
screening of polymeric materials, monomeric subunits of the
polymer, and other organic components.
4. Summary of Guide 6.2.1 Test Method D 5209 (Sturm Test)-This aqueous
4.1 This guide uses a tiered criteria-based approach to test method uses a fresh sample of activated sewage sludge
assess the compostability of environmentally degradable that has been aerated, homogenized, and settled. The super-
plastic products (processed material containing polymeric natant is used as the inoculum. It contains primarily a mixed
materials, processing additives, and other additives required bacterial population that promotes rapid biodegradation
to meet performance requirements). under mesophilic conditions. The metabolism of test mate-
4.1.1 This guide includes methods that simulate rials produces CO,, which is trapped in alkali solution and
mesophilic and thermophilic conditions that are representa- quantitated by titration. The test length is typically 30 days,
tive of composting processes and compost end use. but it can be extended if the medium is reinoculated. A
4.1.2 The tiers progress from rapid screening of polymeric positive result (recovery of 60 % + of theoretical CO,)
materials and other organic components to relatively long- usually indicates that the material will also biodegrade in a
term, more complex/higher cost evaluations. This guide will composting environment. A negative result should be con-
allow one to focus the correct level of resources on materials firmed by a laboratory thermophilic composting test such as
of greatest interest and potential. Test Method D 5338. The contribution of nonmicrobial
4.1.3 Each tier in this guide includes objectives and a degradation can be quantified by including sterile or poison
summary that presents potential test methods, method controls and comparing changes in molecular weight or
principles, test duration, implication of results, and suggested mass.
priority. 6.2.2 Soil Contact Test (Test Method D 5988)-This
NOTE1-The availability of other test methods appropriate for this static test uses a defined sand/soil/mature compost matrix to
guide is acknowledged. provide a consortium of mesophilic and thermophilic bac-
NOTE2-See Fig. I for a description of this guide in flow-chart form. teria and fungi. Biodegradation is measured in a manner
similar to the Sturm test, based on the amount of material
5. Significance and Use carbon converted to gaseous carbon (CO,). Readily biode-
5.1 Plastics that are designed to degrade after use have gradable materials can be screened in 30 to 60 days. A
been developed. These materials are intended to enhance negative result should be confirmed under thermophilic
existing solid waste landfill diversion programs by allowing composting conditions (Test Method D 5338).
difficult to recycle materials to be collected and processed in 6.3 The following test methods can be used to obtain
alternative solid waste disposal systems. Composting has additional information regarding the inherent biodegrad-
emerged as a viable approach to process these materials and ability or degradability of materials.
the organic fraction of municipal solid waste (MSW). A 6.3.1 Test Method D 5247 (Specific Microbe Test)-This
comprehensive testing program is needed to establish the aqueous test method uses pure microbial cultures to assess
compostability (for example, fragmentation rate, biodegrada- the biodegradability of materials under mesophilic condi-
tion rate, and safety) of these materials. tions, based on weight loss or molecular weight changes. The
5.2 This guide can be adapted to generate product-specific test duration is 7 to 14 days. Microbes indigenous to the
evidence for the substantiation of compostable claims to composting or soil environment can be evaluated with this
obtain classification as a compostable product. test method.
6.3.2 Practice G 22 (Bacteria Growth Resistance)-With
NOTE3-State and local regulations should also be considered. this test, solid materials are placed in inoculated molten agar,
and the extent of microbial growth is rated. The test duration
6. Tier 1: Rapid Screening Tests is approximately 14 days. A positive result indicates that the
6.1 In this tier, rapid screening level studies are per- test material is potentially biodegradable.
5
#) D6002
6.3.3 Clear Zone Assays-Opaque test material is dis- 7.1.4 To obtain additional evidence with regard to a
persed into solid agar. A given quantity of microorganisms is plastic product's or component's environmental safety using
applied to form a lawn. Degradation of a material is compost obtained from laboratory-scale studies.
indicated by the formation of clear zones in the solid 7.1.5 To establish the degradation rate of a plastic product
medium. The test duration is 3 to 14 days. A positive result or finished article under pilot scale composting conditions
indicates that the test material is potentially biodegradable. prior to the full-scale composting studies described in Tier 3.
Microbes indigenous to the composting or soil environment 7.2 The following test methods are suggested for estab-
can be evaluated with this test method. The biodegradability lishing the degradation rate of polymeric materials or plastic
of nonopaque organic materials can be assessed by adding products under laboratory-scale composting conditions.
the indicator 2,3,5-triphenyl-tetrazoliumchloride (TTC) to 7.2.1 The degradation rate of test materials under labora-
the media. If microbial colonies can oxidize the material, tory thermophilic composting conditions may be obtained
their electron transport pathways will reduce the TTC. by performing Test Method D 5338 without the CO, trap-
Reduced TTC is detected by its deep red color, whereas ping component. The test materials are exposed to an
oxidized TTC is colorless (2). inoculum that is derived from stabilized compost from
6.3.4 Sealed Vessel Test (Test Method E 1720)--Ready municipal solid waste.
aerobic biodegradability of organic materials is assessed in 7.2.1.1 Aerobic composting occurs in an environment in
small, sealed vessels inoculated with sewage microbes. Gas- which temperature, aeration, and humidity are monitored
eous CO, is monitored by head space analysis. This test and controlled closely. The degradation rate of materials
method represents a simpler approach relative to Test may be established with the current Test Method D5338
Method D 5209 (Sturm). A positive result (60 % +) usually temperature profile or constant 58"C, which has been
indicates that the material will also biodegrade in a adopted by the European standards organization, CEN. The
composting environment. test duration is 45 days, but it may be extended to simulate
6.4 If it appears that a material is being colonized or used field conditions. At various time intervals, materials may be
as a growth substrate by microorganisms, a more funda- removed from the compost, cleaned, and dried.
mental understanding of the degradation process can be 7.2.1.2 Changes in material chemical structure may be
obtained. This typically involves the preparation of purified quantitated based on molecular weight distribution (Test
microbial cultures capable of using the material as a carbon Method D 3593). More sophisticated techniques such as
source. The pure cultures can then be used for the isolation Fourier transform infrared (FTIR) and nuclear magnetic
and characterization of cellular enzyme systems contributing resonance may also be appropriate (4).
to degradation of the material (3). 7.2.1.3 Loss of material integrity due to material degrada-
6.5 The potential effect of materials on plant germination tion may be quantitated by using Test Methods D 882 for
may be assessed with the cress seed test. This step may be thin films or Test Method D 638 for sheet. Material degra-
especially valuable for screening processing additives used at dation may also be established based on weight loss. Surface
1 9% or less in the plastic. Soils from the above soil contact damage may be evaluated using tools such as Scanning
test (6.2.2) may be evaluated at the beginning and end of the Electron Microscopy (SEM).
test to establish the potential effect of microbial degradation 7.2.1.4 Degradation rates of materials may also be estab-
products. In the cress test, soil or compost is extracted with lished using simulated MSW matrixes in externally heated
water and filtered. The supernatant is used for the germina- and self-heating controlled laboratory-scale composting envi-
tion test. Various dilutions of the supernatant are prepared, ronments in accordance with Practices D 5509 and D 5512.
and aliquots are added to petri dishes lined with filter paper. 7.2.1.5 Sieve analysis can be included in the above tests to
Cress seeds are placed on the wet paper and left to germinate obtain additional fragmentation information. Compost con-
in the dark over 4 days at room temperature. The percentage taining fragmented material may be passed through a U.S.
of germinated seeds is determined after 4 days and compared Standard Sievelo with a %-in. (9.51-mm) opening. This
to a water control. Soils containing test materials should not simulates the final screening step used to produce high-
be significantly different from the blank soil at 95 % confi- quality compost products. National, state, and local regula-
dence interval. tory requirements should also be consulted.
NOTE6-Agitation from compost turning equipment at full-scale
7. Tier 2: Laboratory and Pilot Scale Composting Assess- facilities may give faster fragmentation rates relative to laboratory-scale
ment methods.
7.1 The objectives of this tier are as follows: 7.3 The following test methods are suggested for estab-
7.1.1 To establish the degradation rate (change in chem- lishing the biodegradation rate of a plastic product, poly-
ical structure, decrease in mechanical strength, fragmenta- meric materials in the product, and other organic compo-
tion, or weight loss) of the polymeric material or plastic nents in a composting environment.
product under laboratory-scale thermophilic composting 7.3.1 Test Method D 5338 is suggested for establishing the
conditions. biodegradability of organic components in a plastic product
7.1.2 To confirm the biodegradability of the plastic in a composting environment. Material biodegradability is
product and other organic components in the product under based on the amount of material carbon recovered as gaseous
laboratory scale thermophilic composting conditions. carbon (CO,) relative to the amount of material carbon
7.1.3 To determine whether organic residues continue to
biodegrade in a laboratory-scale simulation of compost-
amended soil. lo Available from W. S. Tyler Co., Cleveiand, OH
6
4m D6002
originally added to the compost. Product organic compo- with Practice D 5152 or D 5951 prior to performing
nents, at levels of 1 % or less, generally do not require ecotoxicity tests.
retesting in this step if a positive result was obtained in Tier 1 7.5.2 The following ecotoxicity tests are suggested as a
(6.2). This test can be performed separately or concurrently minimum prior to proceeding to pilot and full-scale testing:
with (7.2). Biodegradation rates or end points should meet 7.5.2.1 Aquatic toxicity test with rotifer Brachionus in
national, state, or local regulations or be compared to the accordance with Guide E 1440. The test duration is one day.
reference materials described in 7.3.2. 7.5.2.2 Plant germination as described by the cress seed
7.3.1.1 If a negative result is obtained, check the controls test in 6.5. The test duration is four days.
described in the test method or repeat the test method with a 7.5.2.3 Plant growth test as described by OECD Guideline
lower dose closer to field-use levels (assuming that an 208. This procedure determines phytotoxicity by mixing the
acceptable signaknoise ratio is possible). compost containing the material with soil. The plant emer-
7.3.2 Products or components may be compared under gence survival and growth is evaluated. Three plant species
identical conditions to natural reference materials known to are generally tested. The test duration is approximately 1
be biodegradable in a composting environment (for example, month. The results from compost containing material are
cellulose or starch (see Guidelines for the Evaluation of compared to compost without material and a soil control.
Feedstock for Source Separated Biowaste Composting and 7.5.2.4 Earthworm test in accordance with OECD Guide-
Biogasification)). Other materials regarded as biodegradable line 207. This procedure determines possible toxicity by
in a composting environment are oak, maple, and corn mixing the compost containing the material with a specified
leaves and kraft paper (5). Unmodified polyethylene film, soil. The earthworm weight change and survival are mea-
typically used to collect yard trimmings, is generally consid- sured. The results from compost containing material are
ered a negative reference material. compared to compost without material and soil controls.
7.3.3 The recovery of all material carbon as gaseous 7.6 Pilot-scale investigations are intended to confirm the
carbon (CO,) may be impractical due to the incorporation of results from laboratory-scale composting tests. These tests
material carbon into microbial biomass or stable humic may be used to evaluate the practical processibility, at
substances. I4Carbon labelled materials may allow carbon to anticipated field use levels, of a plastic product or full-sized
be partitioned into C0,-C, residue-C, water soluble-C, and article by simulating larger-scale operating conditions (see
microbial biomass-C to obtain a complete mass balance. The Guidelines for the Evaluation of Feedstock for Source
use of radio-labelled materials allows testing at field-use Separated Biowaste Composting and Biogasification). Pilot-
levels in composts with high background C02. However, scale tests may also be used to establish the impact of
these definitive studies are comparatively expensive. different waste matrixes on the degradation of a material (6).
NOTE 7-An ASTM standard method for 14C-labelledmaterials is 7.6.1 A standard ASTM pilot-scale test method has not
not available. been developed. Pilot-scale systems ranging from relatively
7.3.4 The effect of a material on compost microorganisms simple to complex have been constructed by industry (6) and
commercial testing laboratories. Some systems include ro-
may be evaluated as described by Schwab, et a1 (6).
tating drums (manual or mechanical) to simulate full-scale
7.4 The following test methods are suggested for estab-
lishing the rate at which plastic product organic components feedstock homogenization and composting process initia-
continue to biodegrade in compost conditioned soil. tion. Some systems control feedstock aeration and tempera-
7.4.1 If incomplete biodegradation is indicated in 7.3, the ture. Vessel sizes range from 30 to 200 L. All systems are
biodegradability of product or component residue in soil self-heating. The duration of the thermophilic composting
may be established with the soil contact method cited in phase ranges from a few days to a few weeks.
6.2.2. The test duration should be a minimum of 6 months 7.6.2 Externally heated pilot-scale systems may be re-
quired to simulate thermophilic conditions characteristic of
or until a regulatory specification is attained or results
full-scale processes.
support the calculation of a rate as indicated by the lack of a
plateau. 7.6.3 Product degradation, safety, and microflora changes
7.4.2 Materials from 7.3.2 can also be evaluated in soil to may be measured with the techniques described in 7.2, 7.3.4,
and 7.5.
obtain additional comparative data.
7.7 In addition to ecotoxicity, a product may not have a
7.4.3 Composts should be prepared in accordance with
the Bridging Practice of Practice D 5951 prior to the soil negative effect on the quality of the compost based on
studies. standard chemical and physical tests. National, state, and
7.5 The plastic product should not cause any negative local regulation should be consulted.
7.7.1 The quality of pilot-scale composts containing de-
ecotoxilogical effects on the resulting compost. The following
graded plastic should be compared to pilot-scale plastic-free
terrestrial and aquatic ecotoxicity tests are suggested for
composts based on chemical analysis. Suggested analyses
obtaining evidence regarding product effects on plant and
include Environmental Protection Agency (EPA) 503 heavy
animal life. National, state, and local regulatory require-
metals, pH, compost maturity, density, porosity, and con-
ments should be considered.
ductivity as described in Refs (1, 7).
NOTE 8-The test material dose specified in laboratory methods,
such as Test Method D 5338, is much higher than levels expected to be
released into the environment. Ecotoxicity is concentration dependent. 8. Tier 3: Field/Full-Scale Assessment
If a negative effect is observed, additional testing is suggested based on 8.1 In this tier, the compostability of products in the field
predicted exposure levels. is established based on full-scale composting studies and
7.5.1 Compost from 7.3 should be prepared in accordance backyard composting environments. The backyard studies
7
Tier 3-Field/Full
Screening Tests Scale Assessment
05338-7 1 (product degradation/fragmentation

I I in compost)
[-’ 1 Sturm 05209-6.1 1 I 05338-7 2 (product biodegradation in compost)

\I (biodegradahon of
polymeric materials and I Soil Contact Test-7 3 (product biodegradation in
Full Scale Exposure-8 1
(Range of technologies)
/I
organic components)
Soil Contact Test-

6 1 2 (biodegradation of
tI -+ soil conditioned with compost)
Environmental Safety of Product-7 4 (aqueous

and terrestrial ecotoxicity tests )
Backyard Composting-8 2
-
D5247 (Specific Microbe)-6.2.1
G22 (Bacteria Resistance)-6.2.2
Clear Zone Assays-6.2.3
Sealed Vessel-6.2.4
w
05512 and 05509 (degradahon in
simulated MSW. externally and self-
heating environments)-7.1.1.2
Sieve Analysis 01 Product

-
Track Product Decompositton In
Microbial Isolates/Enzyme Assays-6.3 Residue-7.1.1.3 P W h
Screening Ecotoxicity (Cress Seed)-6.4 D5338 (reference materials)-7 2.3
140-7.2.3 Lmited Plant Growth Field Tests
Microflora profiles-7.2.4
FIG. 1 Flow-Chart of Guide D 6002
have been included in response to current Federal Trade placement of fiberglass pouches containing the product in
Commission (FTC) marketing guidelines (8). the feedstock. The pouches may be removed periodically to
8.2 The field assessment of products in full-scale systems measure the fragmentation rate and quantify product degra-
should include a range of technologies. Technologies range dation as described in 7.2.
from unmanaged piles (municipal yard waste) to turned 8.2.2.1 A full-scale procedure that includes use of the
aerated static piles with temperature control to tunnel/ pouches has been developed by the ASTM Institute for
agitated bay systems with temperature control. Consult Ref Standard Research Degradable Polymer Advisory Com-
mittee. The procedure may be submitted to ASTM for
(9) to obtain descriptions of facility technqlogies in the standardization.
United States. The need for full-scale assessment may be 8.2.3 Limited plant growth studies are also suggested
reduced as composters, solid waste managers, and degradable using compost containing degradable products. The intent of
plastic product suppliers gain experience with their products. these studies is to confirm previous laboratory/pilot-scale
8.2.1 Ideally, product should be added to the feedstock at results.
anticipated exposure levels and be exposed to the entire 8.3 According to the FTC marketing guidelines (8), an ~
process to establish the compatibility with turning equip- unqualified compostable claim is considered deceptive if the
ment and to ensure that the product is not screened off early product is not compostable in a “home” or “backyard”
in the process. Other goals are to ensure that the product environment.
does not have an adverse effect on the process (that is, 8.3.1 The compostability of products in backyard ~
biological activities, litter, odor, pH, etc.) and that the composting environments can be established if desired. The
product is not visually distinguishable after curing and final composting process tends to be slower due to a relatively
short thermophilic composting phase. Loss of heat due to the
processing is completed.
relatively small pile or bin size is a significant factor. The
8.2.2 A useful technique for quantitating the degradation approach described in 7.6 and 7.7 will probably provide
rate in full-scale systems that do not grind feedstock is the sufficient evidence.
8
8.3.2 The compostability of products should be estab- three tiers. The report should contain a conclusion regarding
lished in both bins and freestanding piles based on typical the compostability (fragmentation, biodegradation, and
home composting practices. safety) of the product based on the “weight of evidence.”
NOTE 9-Guidelines for best management practices under backyard
composting environments can be obtained from the Composting
Council (1). 10. Keywords
9. Report 10.1 biodegradation; compostable; composting; degrad-
9.1 The report should summarize the results from all able; Plastic; Polymer; Strategy; toxicity
REFERENCES
(1) Compost Facility Operating Guide, Composting Council, Workshop on Biodegradability, Institute for Local Self-Reliance,
Alexandria, VA, 1995. Washington, DC, 1992.
(2) Skipper, H. D., et al, “Microbial Degradation of Herbicides,” (6) Schwab, et al, “Characterization of Compost from a Pilot Plant-
Research Methods in Weed Science, 1989, pp. 457-462. Scale Composter Utilizing Simulated Solid Waste,” Waste Man-
(3) Jendrossek, D., et al, “Degradation of Poly(3-hydroxybutyrate), agement and Research, Vol 12, 1994, pp. 289-303.
PHB, by Bacteria and Purification of a Novel PHB Depolymerase (7) Recommended Test Methods for the Examination of Compost and
Composting, Composting Council, Alexandria, VA, 1993.
from Comamonas sp.,” Journal of Environmental Polymer Degra- (8) Guidelines for the Use of Environmental Marketing Claims,
dation, Vol I , 1993, pp. 53-63. Federal Trade Commission, Washington, DC, 1992.
(4) Seal, K. J., “Test Methods and Standards for Biodegradable ( 9 ) US.Solid Waste Composting Facility Profiles, Vol 11, National
Plastics,” Chemistry and Technology of Biodegradable Polymers, Composting Program, United Conference of Mayors, Washington,
G. L. Griffin, ed., Blackie Academic and Professional, DC,1993.
Bishopbriggs, Glasgow, 1994, pp. 116- 134. (10) Zucconi, et al, “Cress Seed Germination Bioassay,” Bicycle,
(5) “Toward Common Ground,” Proceedings of the International March/April 198I .
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additionalstandards
technical committee, which you may attend. If yo0 feel that your comments have not received a fair hearing you should make your
views known to the ASTM Committee on Standards, 100 Barr Harbor Drive, West Conshohocken, PA 19428.
9
($/b Designation: D 5338 98 - An American National Standard
Standard Test Method for

Determining Aerobic Biodegradation of Plastic Materials
Under Controlled Composting Conditions'
This standard is issued under the fixed designation D 5338; the number immediately following the designation indicates the year of
superscript epsilon (E) indicates an editorial change since the last revision or reapproval. \
1. Scope Water by Aqueous-Injection Chromatographys

1.1 This test method determines the degree and rate of D 3590 Test Methods for Total Kjeldahl Nitrogen in Wate?
aerobic biodegradation of plastic materials on exposure to a D 4129 Test Method for Total and Organic Carbon in Water
controlled-composting environment under laboratory condi- by High-Temperature Oxidation and Coulometric Detec-
tions. This test method is designed to yield reproducible and tion6
repeatable test results under controlled conditions that re- E 260 Practice for Packed Column Gas Chromatography7
semble composting conditions. The test substances are exposed E 355 Practice for Gas Chromatography Terms and Rela-
to an inoculum that is derived from compost from municipal tionship~~
solid waste. The aerobic composting takes place in an envi- 2.2 APHA-A WWA-WPCF Standards:
ronment where temperature, aeration and humidity are closely 2540 D Total Suspended Solids Dried at 103 to 105"C8
monitored and controlled. 2540 E Fixed and Volatile Solids Ignited at 550°C8
1.2 This test method is designed to yield a percentage of 2.3 I S 0 Standard:
conversion of carbon in the sample to carbon dioxide. The rate I S 0 14852 Plastics-Evaluation of the Ultimate Aerobic
of biodegradation is monitored as well. Biodegradability and Disintegration Under Controlled
1.3 This test method is designed to be applicable to all Composting Conditions-Method by Analysis of Re-
plastic materials that are not inhibitory to the microorganisms leased Carbon Dioxideg
present in aerobic composting piles. 3. Terminology
1.4 The values stated in SI units are to be regarded as the
standard. 3.1 Definitions-Definitions of terms applying to this test
1.5 This standard does not purport to address all of the method appear in Terminology D 883.
safety concerns, if any, associated with its use. It is the 4. Summary of Test Method
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 4.1 This test method consists of the following:
bility of regulatory limitations prior to use. Specific hazard 4.1.1 Selection of plastic material for the determination of
statements are given in Section 8. the aerobic biodegradability in a controlled-composting sys-
1.6 This test method is equivalent to I S 0 14852. tem,
4.1.2 Obtaining an inoculum from composted municipal
2. Referenced Documents solid waste,
2.1 ASTM Standards: 4.1.3 Exposing the test substances to a controlled aerobic
D 618 Practice for Conditioning Plastics and Electrical composting process in conjunction with the inoculum,
Insulating Materials for Testing2 4.1.4 Measuring carbon dioxide evolved as a function of
D 883 Terminology Relating to Plastics' time, and
D 1293 Test Methods for pH of Water3 4.1.5 Assessing the degree of biodegradability.
D 1888 Test Methods for Particulate and Dissolved Matter, 4.2 The percentage of biodegradability is obtained by de-
Solids, or Residue in Water4 termining the percentage of carbon in the test substance that is
D 2908 Practice for Measuring Volatile Organic Matter in converted to CO, during the duration of the test. This percent-
age of biodegradability will not include the amount of carbon
converted from the test substance that is converted to cell
I This test method is under the jurisdiction of ASTM Committee D-20 on Plastics
and is the direct responsibility of Subcommittee D20.96 on Environmentally ' Annual Book of ASTM Standards, Vol 1 1.02.
Degradable Plastics. Annual Book of ASTM Standards, Vol 1 1.04.
Current edition approved July 10, 1998. Published September 1998. Originally 'Annual Book of ASTM Standards. Vol 14.02.
published as D 5338 - 92. ' Standard Methods for the Examination of Water and Wastewater, 17th Edition.
Annual Book of ASTM Standards, Vol 08.01. 1989. American Public Health Association, 1740 Broadway, New York. NY 19919.
' Annual Book of ASTM Standards, Vol 1 1.01. ' Available from American National Standards Institute. 1 I W. 42nd Sr.. 13th
Discontinued; see 1 Y Y f Annual Book of ASTM .Standard.\, Vol I I .01. Moor. New York. NY 10036.
10
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polymer is inherently non-biased since radioactivity is a direct 15.2 Data on the precision and bias of these test methods
measure of the polymer carbon. However, an accurate true between laboratories are being determined by a round-robin
value is determined only when detection efficienciesare high, test, and will be available on or before December 2003.
interferences are avoided, and proper calibration is performed.
This can be accomplished routinely with present scintillation
counting techniques.
TheAmerican Society for Testingand Materials takes no position respecting the validity of any patent rights asserted in connection
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additionalstandards
views known to the ASTM Committee on Standards, 100 Barr Harbor Drive, West Conshohocken, PA 19428.
22
10. Test Method A-Aqueous Environment extended depending upon the objectives of the experiment.
10.1 Prepare incubation flasks by adding 75 mL of limited 11.5 In order to test whether the oxidation of the carbon in
BAM, 2 to 5 mL of inoculum and 50 to 100 mg (>500 000 the plastic could occur chemically under these composting
dpm) of the radiolabeled plastic sample to a 125-mL Erlenm- conditions, it may be necessary to use a sterile control. This is
eyer flask. not necessary if the chemistry of the compound being tested is
10.2 Pass oxygen through the water flask and the incubation well documented and it is known that chemical oxidation does
-
flask (each maintained at 58 t 5°C) at a rate of 15 mL/min t not occur under these composting conditions.
2 mL/min. 12. Calculation
10.3 Shake the flasks at 100 t 10 rotationsloscillationsper
min. 12.1 Total dpm in a composting vessel at the start of the test
10.4 The gasses leaving the incubation flask pass through (ST, dpm) is calculated as follows:
the acid trap and then through the C02 absorption column ST,dpm = (SA)(LP) (1)
containing 4 to 5 mL of methoxyethyl amine cooled to >15"C
or through a column containing 8 to 10 mL of methoxyethyl where:
SA = specific activity in dpdmg, and
amine without cooling. LP = mg of labeled plastic added to the vessel.
10.5 Switch the gas flow to another absorption column in 12.2 To calculate the quantity of radioactivity (dpm) de-
intervals from 4 to 8 h, depending on the objectives of the tected in C02 absorbent, measure the volume of methoxyethyl
experiment and the methoxyethyl amine from the original
amine drained from the absorption column. Then, measure the
column is drained into a scintillation vial.
radioactivity in a 2-mL aliquot. Employ the following equa-
10.6 Add 10 to 15 mL of scintillation cocktail to the
tion:
scintillationvial and count the sample in the liquid scintillation
counter set to measure the beta radiation of carbon- 14. C, dpm = [(Al - B ) /Cv]/2 (2)
11. Test Method B-Compost Environment where:

C, dpm = total dpm per collection,
11.1 Uniformly distribute the radiolabeled plastic sample, A1 = dpm in the 2-mL aliquot,
cut in pieces approximately 2 cm2(for film), in approximately B = background dpm, and
300 g of compost as the compost vessel is filled. Addition of cv = millilitres from each column collection.
200 to 300 mg of plastic is sufficient for each composting 12.3 Calculate the cumulative percent production of
vessel. Comparative samples should have similar surface areas. carbon-14 carbon dioxide (14C02) or percent of plastic bio-
11.2 Partially fill acid traps with concentrated sulfuric acid logically oxidized (Px, %) using the following equation:
so as to accommodate the water removed from the airflow.
11.3 Keep the compost vessel and humidifying trap in a 58 Px, %= X,-,(C,dpdST, dpm) 100 (3)
? 5°C chamber. Record the temperature of each composter 13. Interpretation of Results
daily and ensure that it is within 5°C of the chamber. Raise the 13.1 The I4CO2measured in these test methods are a direct
temperature of the air to 58°C by passing it through a coil in the indication of the oxidation of the sample. However, the extent
heated chamber prior to entering the water trap (humidifying and the rate of oxidation are related to the compost mixture
trap). Bypass these humidifying traps during the first 2 to 3 made for that individual test and the form of the sample.
days due to the production of large amounts of metabolic water. Although different batches of compost can produce different
Sample the composters at 3 days and weekly thereafter to results, the compost formula for the simulation of MSW in
determine the percent moisture of the compost. If the percent these test methods will generally give repeatable results. This
moisture drops to 50 % pass the incoming air through the water is due to the selection of common feed ingredients that are
traps. Control moisture in the compost at 50 to 60 %. standardized in the trade and tend to have a consistent
11.4 Fill the C02 absorption columns with >200 mL of composition. Depending upon the objectives of the test, it is
methoxyethyl amine. Drain and measure the volume, and place generally wise to include within each test series a standard
a 2-mL aliquot in a scintillation vial with 15-mL scintillation preparation of known degradation rates and to make test
fluid. Count in a Beta counter calibrated to count carbon-14. comparisons.
NOTE1-It is important in the early days of the composting process to 14. Report
monitor the viscosity of methoxyethyl amine by observing the bubble
flow. The large quantity of CO, evolving during this period can cause the 14.1 Report the following information:
methoxyethyl amine to solidify. Usually a daily collection and refill of 14.1.1 Data regarding compost temperature and moisture,
methoxyethyl amine will be sufficient. In order to reduce the volatility of 14.1.2 Daily (or periodic) production of 14C02,
this short-chain amine, the column can be cooled by circulating refrigerant 14.1.3 Cumulative periodic summation of 14C02,
at temperatures< 15°C through the jacket of the column. If the absorption
column is not cooled, an additional 20 % of the absorbant must be used.
14.1.4 Graphic display of 14C02summation data comparing
Generally, absorption columns are completely drained and refilled once a treatments, and
day. 14.1.5 Average and standard deviation of replicates if there
NOTE 24ccasionally two phases develop due to larger quantities of are sufficient numbers.
water trapped in the methoxyethyl amine, and these two phases can be
blended into one by the addition of several millilitres of methanol. During 15. Precision and Bias
prolonged composting trials (over 20 days) the sampling interval can be 15.1 Measurement of radioisotope labeled (carbon-14)
21
Sclntillation
Cocktail
_____. ++
-
......... , ............ '.! ............ -I 1
Power Supplies
Relays
FIG. 4 Fully Automated I4C COPCollection System for Sixteen Units (MP = metering pump, v = valves, 16Wv = sixteen way valves)
Vent
.I I
- .,I
Air- -
Ne-dle
Valve
Flow
Meter
I
I
c02
Absorption
Column
Acid
trap
Cornposter
Oven
FIG. 5 Automated Radiochemical Composting Apparatus
lies in the ability to detect and distinguish that carbon-14 polymer intended for commercial production.
isotope from a virtual sea of carbon-12 in the compost. This 9.2 Thickness of polymer film can be an important variable
ability to follow or trace that carbon due to its radioactivity for any biodegradation test. Thus, the thickness should be
requires that the radiochemical purity of the compound be measured by a micrometer and included with any data describ-
established, that is, verify that only the compound of interest is ing biodegradation rates of polymeric material. Further, in the
labeled and no label is present in any other material. This preparation of such films, take care to produce a film of
verification requires an analytical technique that can separate uniform thickness.
the polymer and determine that the radioactivity resides solely 9.3 The radiolabeled plastic should be prepared with an SA
in the polymer, and that the structure (NMR analysis) and of at least 7000 dpdmg. ASA of 10 000 d p d m g provides
molecular weight distribution (see D 5296) are the same as the sufficient counts for extended test.
20
!-. --- ing activities) was used in an ASTM-ISR study4 and has the
I following composition on a dry matter basis (made up to 55 to
j V
60 % moisture for testing): wood chips (brush), 41.4 %;
chapped leaves, 25.4 %; grass clippings, 25.8 %; aged com-
post, 7.3 %. Different compost preparations can produce dif-
ra--------
-
-
1-
L
L ___.
ferent rates of biodegradation. A yard and garden waste
compost can, with certain plastics, result in slower rates of
degradati~n.~
7.2 The compost is made up to 55 to 60% moisture by
measuring the moisture content of each component, calculating
the moisture content of the mix, and adding water to bring the ~
Cooled mix to near target moisture percentage. The moisture content

Chamber can be checked by taking a sample of the compost, weighing it,
drying it, reweighing it, and calculating the moisture from the
difference in weight. Water can then be added as needed.
During the experiment, testing of the moisture content should
be checked weekly and maintained at 55 to 60 % by humidi-
fying (bubbling the air through water) the air as needed.
Input from 7.3 Liquid culture inoculum are prepared from the target
Culture Flask/ aqueous environment. They can be used directly, that is,
Acid Trap sewage sludge or waste water treatment sludge, or eluant from
---- c. _"--
compost, or they can be enriched by growing the mixed culture
on the carbon source of interest.
7.4 Media used for liquid culture is related to the environ-
9- I
ment being simulated. For waste water or sewage sludge, a
limited basal media (BAM broth minus glucose) is prepared
according to the Handbook of Microbial Media.s This media
--F
relies on the plastic for the major source of carbon bond energy.
Auto Positioning Rack 7.5 The carbon dioxide absorber, methoxyethyl amine6 is
FIG. 3 Single Unit from an Automated 14CCOPCollection System used to capture CO, in the scrubbing columns.
(V = valve and MP = metering pump) 7.6 A liquid scintillation cocktail designed for counting
carbon-14 is required. Any commercial scintillation cocktail
in series and insuring that no radioactivity is trapped in the reagent that is compatible with the CO, absorber is accept-
second column. able.'
6.3.1.7 The COz absorbent must not interfere with the
accurate measurement of radioactivity in the liquid scintillation 8. Hazards
counter by incompatibility with any other reagent. 8.1 Compost presents well-known health risks that can be
avoided by the use of appropriate protective equipment such as
7. Reagents and Materials gloves and masks.
7.1 Compost for this testing may be made up in accordance 8.2 Strong bases used for C02 absorption are particularly
with either of the following recipes, municipal solid waste hazardous and instructionsin Material Safety Data Sheets must
(MSW) or woody compost, or obtained from an active munici- be followed.
pal solid waste or yard waste composting center. 8.3 Radioactive carbon-14 compounds must be handled in
7.1.1 Compost, designed to stimulate municipal solid waste accordance with federal and state regulations.
(MSW) organic matter, is prepared by combining the following
materials (on a dry matter basis): alfalfa meal, 35.7 %; shred- 9. Radiolabeled Preparations
ded newspaper, 27.2 %; garden soil, 13.2 %; poplar sawdust, 9.1 The utility of tagging the carbon in a molecule or a
10.4 %; cottonseed meal, 6.4 %; cow manure, 1.6 %; calcium portion of the molecule with the radioactive isotope of carbon,
carbonate; 5.3 %; sodium bicarbonate, 0.2 %. The mixture is
designed to contain the biochemical ingredients found in MSW ISR Degradable Polymeric Materials Program, Compilation of ISR Contractor
(lignified cellulose (newspaper, poplar sawdust and alfalfa Compos! Tes! Repor!, ASTM, 1993.
meal), protein (cottonseed meal and alfalfa meal), natural R.M. Atlas, Handbook of Microbiological Media, CRI Press, Inc., 1993, p. 113.
inoculum (garden soil and cow manure); soluble carbohydrates Carbosorb" (Packard Instrument Co.) is a strongly basic short-chain amine is
a highly efficient CO, absorber and is compatible with many scintillation cocktails.
and buffering capacity sufficient to maintain a neutral to Other organic bases can be used for trapping CO, but they generally lack the
slightly basic pH). The particle size of the components of the efficiency of methoxyethyl amine. Inorganic bases have several disadvantages for
compost mix are sized to pass through a 6-mm screen. example, they are strong quenching agents, produce severe color or turbidity
interference, and have low trapping capacities.
Moisture content should be adjusted (see 7.1.3) to 55 to 60 ?k 'Although the manufacturer of Carbosorb", recommends their product Perma-
for testing. flour E+", other scintillation cocktails are also compatible, including the Beckman
7.1.2 An alternate compost (used to simulate yard compost- Environmental Cocktail Ready Safe".
19
k m
cukumnrJJ
Md Tmp
- J
Add Tmp \.--

&r-.--===-==-=-=-.
- ----- -1
-1
fiun
Cul(um f l u w
--
Add Tmp I
FIG. 2 Semlautomated I4CCO, Collection System for Eight Units Over Six Sampling Periods
controlled temperature chamber, a sulfuric acid trap, and a C 0 2 6.2.6 A liquid scintillation counter, capable of counting the
absorption column. low-energy beta emitted by the radioactive isotope carbon-14
6.2.2 The composting vessel is a 1-L borosilicate glass is used to measure the quantity of radioactivity in the trapped
reaction kettle with a glass flange tooled to receive an “0” ring, CO,. An instrument that can automatically measure counting
clamped against an inert plastic surface. Pressurized air, efficiency and correct for quenching is preferred.
controlled by a needle valve, is passed through a flow meter 6.2.7 It is important to test the system for leaks and insure
and then either through a water trap, maintained at the same that the radioactive CO, does not escape from the apparatus
temperature as the compost, or directly to the compost (25 2 both for accurate results and safety of personnel.
3 cc/min). The composting vessel is fitted with a central hollow 6.2.8 Vent columns to a radiochemical hood.
stainless steel shaft that protrudes through a perforated dis- 6.2.9 Place check valves, that will allow the air flow to
tributor plate at the bottom of the vessel (Fig. 5). The air is travel in only one direction, between the test flasks and the acid
passed down the shaft to the space below the distributor plate and between the acid and absorber.
and then passes up through the compost to the top of the 6.3 Alternate Composting Apparatus:
compost where it exits from the vessel. The shaft contains rods 6.3.1 Alternative compost apparatus can be used if it con-
projecting perpendicular from the shaft in a radiating fashion. forms to the following requirements:
The shaft is connected to a motor that turns the shaft at rate of
6.3.1.1 Although compost vessels can be larger than 1-L, it
about 6 r/min. The mixing motion is designed to mix, break up
is generally not practical to exceed 1-L, due to the large volume
clumps and convey the compost upward. The resultant action
of CO, that is produced and must be completely absorbed.
tends to circulate the compost in the composting vessel and
maintains an even flow of air through the compost. 6.3.1.2 The compost temperature must be controlled.
6.2.3 As air exits the composting vessel, it passes through a 6.3.1.3 The air supply flow must be controlled and humidi-
check valve and then proceeds through a sulfuric acid trap. The fied.
trap dehydrates the air and insures that the CO, stays in the gas 6.3.1.4 The air must be stripped of moisture prior to
phase. scrubbing to eliminate the two phases that occur when the
6.2.4 The air then passes into a glass column filled with scintillation cocktail is added to CO, absorber that has accu-
glass helixes and a commercial CO, absorber, methoxyethyl mulated too much water.
amine. The glass helixes break up the gas bubbles and provide 6.3.1.5 The scrubbing column must be designed to permit
greater surface area for the absorption (scrubbing) of CO,. enough aidliquid contact to completely capture the CO,.
6.2.5 The column is jacketed (has an outer glass chamber) 6.3.1.6 The efficiency of the absorption column must be
where a refrigerant (propylene glycol) is circulated. verified. This can be accomplished by placing another column
18
4. Summary of Test Method over a chosen period of time can be sampled by collecting the
4.1 Test Method A involves the characterization of the test CO, absorbent from the column at the end of each period by
material, the preparation of the natural mixed culture inoculum, hand, or by automating the CO, collection.
the control of the culture environment, the collection and 6.1.2 Fig. 2 illustrates an eight-unit system with a semi-
measurement of radioactive carbon dioxide (CO,) over time, automated CO, collection system based on a timed, automated
and the calculation and interpretation of the results. The results six-way valve. The gas effluent from the culture flask and acid
may be compared to those obtained from Test Method D 5209. trap is continuously passed through an absorption column and ~
4.2 Test Method B involves the characterization of the test periodically switched to the next column. Just before the sixth
material, the preparation of the compost matrix, the control of column is due to switch, the five columns are drained and
the composting process, the collection and measurement of refilled. Soon after the sixth column switches, it is drained and
radioactive CO, over time, and the calculation and interpreta- refilled.
tion of the results. The results may be compared to those 6.1.3 Fig. 3 represents a single unit from a fully automated
obtained from Practice D 5512 as well as Test Method D 5338. CO, collection system where two absorption columns are
alternately used to capture the CO,. While one column is
5. Significance and Use collecting CO, from the effluent, the other is drained into a
5.1 These test methods can provide direct and unequivocal scintillation vial, scintillation cocktail is added to the vial, and
evidence of aerobic biodegradability. This requires that the the column is refilled with the CO, absorbent automatically.
radiochemical purity of the plastic is verified using Test 6.1.4 Fig. 4 is a diagrammatic representation of a sixteen-
Method D 5296. unit, fully automated system. The system is controlled by a
5.2 These methods also provide the opportunity to deter- personal computer and an 1/0 microprocessor. Valves and
mine the rate of biological oxidation in a complete composting metering pumps are powered by electronically-controlled
environment or aqueous environment by frequent periodic power supplies and relays. Reservoirs of C 0 2 absorbent and
sampling of carbon dioxide. scintillation cocktail serve all sixteen units. The scintillation
5.3 These methods provide biodegradation data at use levels vials are in a rack that positions the vials for each sampling
of the plastic in a full cycle composting process or an aqueous period.
system.
6.1.5 Alternative apparatus can be used if it has the capa-
6. Apparatus bility of maintaining the appropriate temperature, controlling
the oxygen flow, humidification of gas flow, and complete
6.1 Liquid Culture Apparatus:
collection of CO,.
6.1.1 Fig. 1 is a diagrammatic representation of a single unit
for measuring the carbon-14 carbon dioxide (CO,) production 6.1.6 Alternate apparatus can be manually operated or
from the biodegradation of a labeled polymer in aqueous controlled by computer interface.
culture. It consists of a fine needle valve for the sensitive 6.2 Composting Apparatus:
control of oxygen flow, a water and culture flask in a controlled 6.2.1 Fig. 5 is a diagrammatic representation of the radio-
temperature environment, a trap to remove water from the gas chemical composting apparatus. The radiochemical compost-
stream and to insure the carbon monoxide (CO) stays in the gas ing apparatus consists of a glass composting vessel capped by
phase, and a CO, absorption column: Periodic CO, production an inert plastic surface, a controlled humidified air flow, a
CONTROL OF
TEMPERATURE AND AQlTATlON
0,-- = = =
FINE
NEEDLE COLUMN
VALVE COOLED
co2
ABSORPTION
HP CULTURE COLUMN
FIG. 1 Single Unit for Measuring ‘‘C COPProduction from the Biodegradation of a I4C-LabeledPolymer
17
#Tb Designation: D 6340 98 -
Standard Test Methods for

Determining Aerobic Biodegradation of Radiolabeled Plastic
Materials in an Aqueous or Compost Environment'
This standard is issued under the fixed designation D 6340; the number immediately following the designation indicates the year of
1. Scope conform to all the regulatory requirements, specifically those

1.1 These test methods directly determine the rate and that relate to the Use Of Open radioactive Sources.
degree of biological oxidation of carbon in plastic materials l a 9This standard does not Purport to address all Of the
when placed in a composting environment containing simu- safety concerns, if any, associated with its use. It is the
lated municipal solid waste or an aqueous environment under responsibility of the user of this standard to establish appro-
laboratory conditions. priate safety and health practices and determine the applica-
1.2 Test Method A utilizes a mixed culture derived from the bility Of regUzutorYlimitations Prior to use.
target environment (waste water, sewage sludge, compost 2. Referenced Documents
eluant, and other environmental sources). Temperature, mix-
ing, and aeration are monitored and controlled. 2.1 ASTM Standards:
1.2.1 This method has the sensitivity to determine biodeg- 883 to
radation at concentrations commonly found in these environ- D 5209 Test Method for Determining the Aerobic Biodeg-
ments. radation of Plastic Materials in the Presence of Municipal
1.3 Test Method B starts with fresh compost and proceeds Sewage Sludge3
through the normal composting process to an early mature D 5296 Test Method for Molecular Weight Averages and
stage. Temperature, aeration; and moisture are monitored and Molecular Weight Distribution of Polystyrene by High
controlled. Performance Size Exclusion Chromatography3
1.3.1 This method can determine biodegradation at levels of D 5338 Test Method for Determining Aerobic Biodegrada-
the plastic commonly expected in municipal solid waste. tion of Plastic Materials Under Controlled Composting
1.4 These test methods require that the target component of Conditions3
the plastic material be synthesizedusing the radioactive isotope D 5512 Practice for Exposing Plastics to Simulated Com-
carbon-14. Depending upon the objective, either a portion of post Environment Using an Externally Heated Reactor3
the components of the plastic or all of the carbon can be 3. Terminology
uniformly labeled with carbon-14. The test method will deter-
mine how that labeled portion will be metabolized and bio- 3.1 Dejinitions-For definitions of terms used in these test
logically oxidized by the microorganisms in the system tested. methods as they relate to composting, see Terminology D 883.
1.5 These test methods can be applied to any carbon-14 3.1.1 specijc activity, SA, n-refers to the quantity of
labeled compound as well as for plastic materials that have radioactivityper mass unit of compound (polymer, etc.), that is
been formulated to biodegrade in a natural aerobic environ- dpmh%.
ment. 3.2 Acronyms:
1.6 The synthesis and preparation of the radiolabled plastic 3.2.1 Bq, n-becquerel; SI unit where 1 curie (Ci) = 3.7 .
is beyond the scope of these methods. Carbon-14 labeled 10" Bq.
polymers may be purchased from a number of commercial 3.2.2 dpm, n-disintegrations per minute, used to measure
labs. the quantity of radioactivity.
1.7 There are no I S 0 test methods that are equivalent to the 3.2.2.1 Discussion-The measure dpm is derived from
test methods in this standard. counts per minute (cpm) where dpm = cmp-bkgdcounting
1.8 The safety problems associated with compost and radio- efficiency. There are 2.2 lo6 dpm/pCi.
activity are not addressed in this standard. It is the responsi- 3.2.3 mCi, n-millicurie; 1/1OOOth of a curie (standard
bility of the user of this standard to establish appropriate safety unit).
and health practices. It is also incumbent on the user to 3.2.4 ,uCi, n-microcurie; 1/1OOOth of a millicurie.
3.2.5 MSW, n-municipal solid waste (organic matter).
' These test methods are under the jurisdiction of Committee D20 on Plastics and
are the direct responsibility of Subcommittee D20.96 on Degradable Plastics. 'Annual Book of ASTM Standards, Vol 08.01.
Current edition approved Nov. 10, 1998. Published February 1999. 'Annual Book of ASTM Standards, Vol 08.03.
16
D5338
The American Society for Testingand Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standardare expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own respnsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed evety five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
views known to the ASTM Commjttee on Standards, 100 Barr Harbor Drive, West Conshohocken, PA 19428.
15
260 v 263 7- I
/,- I
0
0 10 20 IO 40
DO". Doll
FIG. 3 Cumulative CO, Production from Inoculum FIG. 4 Cumulative CO, Production from Inoculum Plus Cellulose
0
0 0 0
20 D0"S 30
FIG. 5 Net Cumulative CO, Production from Cellulose

15. Precision and Bias
activity (CO, production in the first ten days), date of collec- 15*1 The precision and bias of the procedure in this test
tion, storage, and handling. method is being determined.
14.1.2 Carbon content of the plastic materials, positive and 15s2 for within-laboratoq
negative control, and calculation of the theoretical maximum testing using a conuoued composting set-up with gas tho-
cabon dioxide production. Report specific information on the matograph are presented in Table 1. These data represent three
size, shape, volume, and of the plastic materials different determinations of the degradation of cellulose as a
tested, along with the form of the plastic that is, sheet, positive reference. The average degradation of cellulose after
powder, pe!let, etc., 45 days of composting at a constant temperature of 50°C
14.1.3 Weight of vessels with contents before and at the end (+2"C) was 75.3 %, with an average standard deviation of
of the test, 2.5 % and an average 95 % confidence limit interval of 5 %.
14.1.4 Cumulative carbon dioxide evolution and oxygen All three runs were carried out within a seven-month period by
consumption over time and display graphically. Report appa- the same operators. Figures 3, 4, and 5 represent a graphical
ratus used for carrying out the test method, view of the third run in which a biodegradability of 78.9 % was
14.1.5 Percentage of aerobic biodegradation for each plastic obtained as the mean for the three replicates containing
cellulose as the positive control, with a standard deviation of
material tested, the standard deviation and 95 % confidence
0.3 % and a 95 % confidence limit interval of 2 %. The graphs
interval for each material or control substance tested for the
represent the results from three replicates for the inoculum only
percent of biodegradation,
as the blanks (see Fig. 3), the cellulose as the positive control
14.1.6 Percentage of biodegradation relative to the positive
(see Fig. 4) and the net CO, production per gram of cellulose
reference (cellulose = 100 %),
added (see Fig. 5).
14.1.7 Temperature range of test, and
14.1.8 pH of compost inoculum and pH of final residues.
Volatile fatty acids concentration for vessels with a final pH of 16.1 aerobic biodegradation; biodegradation; composting ;
less than 7. plastics
14
dry conditions are observed, that will severely slow down the measurements of flow rate and gas composition and after
breakdown process, add moisture. During the whole course of recalculation to STP (standard temperature and pressure)
the test, make adjustments to ensure proper composting con- conditions.
ditions. If adjustments are made, then CO, and 0, concentra- 12.2.3 Calculate the amount of cumulative gaseous-carbon
tions must be monitored closely during the following 72 h and produced by each reactor.
measured at least twice daily with a time interval of more than 12.2.4 Determine the mean (of the three replicates) net
6 h. gaseous-carbon production by controlled composting of the
11.4 End of the Test: test substances by subtracting the mean gaseous carbon pro-
11.4.1 At the end of the test, weigh the vessels with the duction of the control (three replicates) containing only the
contents and determine the dry solids concentration remaining inoculum.
in the composted material. 12.3 Calculate the percent of biodegradation by dividing the
11.4.2 Measure the pH in conformance with Test Methods average net gaseous-carbon production of the test compound
D 1293.If the pH is less than 7,measure the volatile fatty acids by the original average amount of carbon in the test compound
spectrum to indicate souring of the contents in the composting and multiplying by 100:
vessel in accordance with Practice D 2908.Measure the pH by mean C,(test) - mean C,(blank)
diluting the sample on a 5:l w/w ratio of distilled water to % biodegradation = x 100
Cl
compost inoculum or residue, mix by shaking manually and
measure immediately. where:
11.4.3 If more than 2 g of volatile fatty acids per kilogram Cg = amount of gaseous-carbon produced, g, and
of dry matter in the composting vessel is formed, the test must Ci = amount of carbon in test compound added, g.
be regarded as invalid. 12.4 Calculate the standard error, se, of the percentage of
biodegradation as follows:
12. Calculation S, = SQRT((s;,Jnl) + (siW/n2)) X 100/Cl
12.1 Determine the total carbon content of the test material
by elemental analysis or by calculation if the chemical com- nl and n2 are the number of replicate test and control digesters
position is well established. This allows the theoretical quantity respectively; s is the standard deviation of the total gaseous
of carbon dioxide evolution to be calculated as follows: carbon produced.
12.5 Calculate the 95 % confidence limits as follows:
material = w % carbon
95 % CL = % biodegradation 2 ( t X s,)
w/lOO X g of material charged = Y g carbon charged to
Where t is the t-distribution value for 95 % probability with
compost vessel = C ,
(nl + n2 - 2) degrees of freedom; thus n = 3 + 3 - 2
c + 0 2 + coz = 4.
12 g C yields 44 g C 0 2
13. Interpretation of Results
44 x Y
Y g C yields 7g COz 13.1 Information on the toxicity of the plastic material may
be useful in the interpretation of inhibitive effects.
12.2 Determine the cumulative CO, production (in grams) 13.2 In most instances when investigating a plastic material,
from the test substances. a reference or control substance known to biodegrade is
12.2.1 Determine the amount of CO, produced by the necessary in order to check the activity of the inoculum. If
difference, in millilitres of titrant, between the test substance sufficient biodegradation (a minimum of 70 % for cellulose
and blank Ba(OH), traps. Perform the titration with 0.05 N within 45 days) is not observed with the positive reference, the
HC1. test must be regarded as invalid and should be repeated, using
12.2.1.1 When CO, enters the absorber bottles, it reacts in new inoculum.
the following manner:
14. Report
Ba(OH), + C 0 2+ BaC03 + H20
14.1 Report the following data and information:
12.2.1.2The BaCO, formed is insoluble and precipitates. 14.1.1Information on the inoculum, including source, per-
Determine the amount of Ba(OH), remaining in solution by cent dry solids, percent volatile solids, total Kjeldahl nitrogen,
end-point titration with HCl using phenolpthalein as an indi-
cator according to the following equation:
TABLE 1 Results from Within-Laboratory Testing for the
Ba(OH)z + 2 HC1- BaC12 + 2 H20 Aerobic Biodegradability of Cellulose as a Positive Control
Under Controlled Composting Conditions
12.2.1.3From the above two equations, it can be seen that
95 %
the number of mmol of CO, produced is: Biodegradability Standard
after 45 days, % Deviation, % Confidence
Limit, %
m o l e s HCl
mmoles of COz = mmoles of Ba(OH)* at start - Run 1 76.7 4.9 8.2
2
Run 2 70.3 2.4 4.8
12.2.2 For the option with gas chromatography, the cumu- Run 3 78.9 0.3 2.0
Mean of Three Runs 75.3 2.5 5.0
lative. CQ2 production (in grams) is determined from the
13
7.2 Analytical-Grade Cellulose, for thin-layer chromatogra- 11.1.1 Obtain an inoculum from a properly operating aero-
phy with a particle size of less than 20 k m as positive bic composting plant treating municipal solid waste, or the
control." organic fraction thereof. If required, further stabilize the
7.3 Polyethylene, as a negative control. It should be in the inoculum at the laboratory in order to obtain a low CO,
same form as the form in which the sample is tested (polyeth- production (see 9.1 .).
ylene film for film samples, polyethylene pellets in case 11.1.1.1 Screen the inoculum to less than 10 mm and
sample is in the form of pellets, etc.). manually remove and discard any large inert items (pieces of
glass, stone, wood, etc.). Determine volatile solids, dry solids
8. Hazards
and nitrogen content according to Test Methods D 3590,
8.1 This test method requires the use of hazardous chemi- ,D 1888, and APHA Test Methods 2540 D and 2540 E.
cals. Avoid contact with the chemicals and follow manufac- 11.1.2 Determine volatile solids, dry solids and carbon
turer's instructions and Material Safety Data Sheets. content of all the test substances according to APHA Test
8.2 The compost inoculum may contain sharp objects. Take Methods 2540 D and 2540 E and Test Method D 4129.
care when handling it. 11.1.3 Weigh out roughly 600 g of dry solids of inoculum
8.3 The composting vessels are not designed to withstand
and mix with about 100 g of dry solids coming from the
high pressures. The system should be operated at close to
sample. Adjust the dry solids content of the mixture in the
ambient pressure. vessel to approximately 50 % with distilled water. Add ammo-
9. Compost Inoculum nium chloride if the C/N ratio is more than 40. Weigh vessels
9.1 The compost inoculum should be two to four months old with all of the contents immediately before initiation of the
well-aerated compost coming from the organic fraction of composting process.
municipal solid waste and sieved on a screen of <10 mm. If 11.1.4 The blank consists of the inoculum only, containing
such a compost is not available, compost from plants, treating about 600 g of dry solids. As references, use thin-layer
green, or yard waste, or mixtures of green waste and municipal chromatography cellulose as a positive control and polyethyl-
solid waste may be used. It is recommended that the compost ene as a negative control.
inoculum produces between 50 and 150 mg of CO, per gram of 11.2 Start-up Procedure-Initiate aeration of the compost-
volatile solids over the first ten days of the test, and has an ash ing vessels with air-flow rates that are sufficiently high to
content of less than 70 % and a pH between 7 and 8.2. Total ensure that oxygen levels do not drop below 6 % in the exhaust
dry solids should be between 50 and 55 %. air. Oxygen levels should be closely controlled during the first
9.2 The compost inoculum should be as free from larger week and measured at least twice daily. Adjust air-flow rates as
inert materials (glass, stones, metals, etc.) as possible. These needed.
items should be removed manually as much as possible to 11.3 Operating Procedure:
produce a homogeneous compost inoculum. 11.3.1 The composting vessels are incubated in the dark for
9.3 It is recommended to use compost of sufficient porosity a period of 45 days. Initially, keep the incubation temperature
to enable conditions to be as aerobic as possible. Addition of at 35°C (+2"C) for a period of one day to simulate a
structural material, such as small wood particles, or persistent mesophilic start-up phase. Subsequently, raise the temperature
or poorly biodegradable inert material may prevent the com- to 58°C (t2"C) for a period of four days. After this sanitizing
post from sticking. period, reduce the temperature to 50°C (+2"C) for optimum
10. Test Specimens composting conditions and maintain until day 28. Reduce the
temperature then to 35°C (22°C) for the remainder of the test
10.1 The test specimen should have sufficient carbon to period to simulate a mesophilic curing phase. The incubation
yield carbon dioxide that can be adequately measured by the time of 45 days may be extended until no significant CO,
trapping apparatus or CO, measurements. production in excess of the inoculum is recorded for a period
10.2 All basic composting parameters, such as C/N, oxygen of one week.
in the composting vessel, porosity, and moisture content should
11.3.2 Check CO, and 0, concentrations in the outgoing air
be optimized so as to make a good composting process
at least daily with a minimum time interval of 6 h after the fist
possible. The C/N ratio should preferably be between 10 and
week for the remainder of the test.
40 for both the inoculum and test substance combined. Oxygen
levels in the composting vessel should be at least 6 % at all 11.3.3 Check air flow daily before the composting vessels
times and no free-standing water nor clumps of material should and at the outlets, ensuring that no leaks are present in the
be present. complete system. Adjust air flow to maintain a CO, concen-
10.3 Test specimens may be in the form of films, formed tration of at least 2 % volume over volume to allow accurate
articles, dog bones, granules, powder, or other, and conform to determination of CO, level in the exhaust air.
Practice D 618. 11.3.4 Ensure proper composting conditions. Shake the
composting vessels weekly to prevent extensive channelling,
11. Procedure provide uniform attack on the test specimen and provide an
11.1 Preparation of the Samples: even distribution of moisture. In case excessive moisture levels
are observed, such as free-standing water in the vessels or
lo For development of this test method, Avicel, available from EM Chemicals, clumping due to high moisture content, remove excess liquid
Inc., Hawthome, New York, was used. by injecting dry air, or by drainage via air inlet. If excessively
12
CONTROLLED-COMPOSTING 810DEGRADABILITY
FIG. 2 Optional Set-Up Using a Gas Chromatograph
biomass and that is not, in tum, metabolized to CO, during the

course of the test. 6.1.4 Suitable devices for measuring oxygen and CO,
4.3 The disintegration of a compact test material is visually concentrations in the exhaust air of the composting vessels,
determined at the end of the test. Additionally, the weight loss such as specific sensors or appropriate gas chromatographs.
of the test material may be determined. 6.2 Carbon Dioxide-Trapping Apparatus for Each Com-
posting Vessel:
5. Significance and Use 6.2.1 At least three 5000-mL bottles fitted with gas sparging
5.1 Biodegradation of a plastic within a composting unit is and containing Ba(OH)2 carbon-dioxide scrubbing solution.
an important phenomenon because it will affect the decompo- 6.2.2 Flexible Tubing, nonpermeable to carbon dioxide.
sition of other materials enclosed by the plastic and the 6.2.3 Stoppers, equipped with gas-sampling parts.
resulting quality and appearance of the composted material. 6.3 Miscellaneous:
Biodegradation of plastics will also allow the safe disposal of 6.3.1 Analytical Balance, (50.1 mg) to weigh test speci-
these plastics through solid-waste composting plants. This men.
procedure has been developed to permit the determination of 6.3.2 100-mL Burette.
the rate and degree of aerobic biodegradability of plastic 6.3.3 0.05 N HC1.
products when placed in a controlled composting process. 6.3.4 pH Meter.
5.2 Limitations-Because there is a wide variation in the 6.3.5 Suitable devices and analytical equipment for measur-
construction and operation of composting systems and because ing dry solids (at 105"C), volatile solids (at 55OoC), volatile
regulatory requirements for composting systems vary, this fatty acids by aqueous-injection chromatography, total
procedure is not intended to simulate the environment of any Kjeldahl nitrogen and carbon concentrations.
particular composting system. However, it is expected to 6.4 Optional-The carbon dioxide-trapping apparatus and
resemble the environment of a composting process operated titration equipment can be replaced by a gas flow meter plus a
under optimum conditions. More specifically, the procedure is gas-chromatograph, or other apparatus equipped with suitable
intended to create a standard laboratory environment that will detector and column(s), for measuring CO, and O2 concentra-
permit a rapid and reproducible determination of the aerobic tions in the exhaust air of each vessel. Take care to analyze
biodegradability under controlled composting conditions. CO, concentration on a sufficiently frequent basis in order to
produce a reliable cumulative CO, production over the course
6. Apparatus of the test (for example, every 3 to 6 h). A standard gas should
6.1 Composting Apparatus (see Fig. I ) : be injected to internally standardize the gas-chromatograph on
6.1.1 A series of at least twelve composting vessels (one test a continuous basis over the course of the test. Operate the gas
substance, one blank, one positive and one negative control, all chromatograph in conformance with Practices E 260 and E 355
in three replicates) of 2 to 5 L of volume. For screening (see Fig. 2).
purposes, depending upon the test material, a smaller volume 6.5 Ensure that all glassware is cleaned thoroughly and free
also may be used. from organic matter.
6.1.2 Water Baths, or other temperature controlling means
capable of maintaining the temperature of the composting 7. Reagents and Materials
vessels at 58°C (22°C). 7.1 Barium Hydroxide Solution, approximately 0.024 N and
6.1.3 Pressurized-AirSystem, that provides C0,-free, H,O- then standardized, prepared by dissolving 4.0 g Ba(OH), per
saturated air to each of the composting vessels at accurate litre of distilled water. Filter through filter paper and store
aeration rates. If using a direct measurement of CO, (6.4). then sealed as a clear solution to prevent absorption of CO, from the
normal air may be used. air.

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ASTM STANDARDS PERTAINING TO THE

Sponsored by Subcommittee D20.96 on Environmentally

Director, Technical Publishing Services: Editors:

Library of Congress Cataloging-in-PublicationData

American Society for Testing and Materials.

Standard Specification for

1. Scope 2.3 Association Francaise de Normalisation (CEN) Stan-

6. Detailed Requirements 503.13, and

Standard Guide for

5 Annual Book of ASTM Standards, Vol I 1.05.

05338-7 1 (product degradation/fragmentation

[-’ 1 Sturm 05209-6.1 1 I 05338-7 2 (product biodegradation in compost)

Soil Contact Test-

Environmental Safety of Product-7 4 (aqueous

Sieve Analysis 01 Product

FIG. 1 Flow-Chart of Guide D 6002

Standard Test Method for

1. Scope Water by Aqueous-Injection Chromatographys

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Annual Fee $350.00*t $65.00*t

Membership Benefits include:

member, or the new official representative of an organizational membership.

NOTE: Membership benefits are subject to change.

SCOPE: The development of test methods, specifications, recommended practices,

CHAIRMAN: Paul E. Sample, Samples, Inc., 308 Walden Rd., Wilmington, DE

VICE-CHAIRMAN Barbara J. Furches, Dow Chemical Co., Engrg Thermoplastics TS&D,

VICE-CHAIRMAN Stephen B. Driscoll, The University of Massachusetts at Lowell, Plastics

VICE-CHAIRMAN Gary Lynn Williams, Owens-Corning Science & Technology Center,

VICE-CHAIRMAN Debra R. Wilson, Union Carbide Corp., Westhollow Research Center,

SECRETARY: Deborah M. Oates, Underwriters Laboratories, Inc., 333 Pfingsten Rd.,

STAFF MANAGER: Katharine E. Morgan (610-832-9721)

11. Test Method B-Compost Environment where:

FIG. 5 Automated Radiochemical Composting Apparatus

Cooled mix to near target moisture percentage. The moisture content

Add Tmp \.--

Standard Test Methods for

1. Scope conform to all the regulatory requirements, specifically those

FIG. 5 Net Cumulative CO, Production from Cellulose

FIG. 2 Optional Set-Up Using a Gas Chromatograph

biomass and that is not, in tum, metabolized to CO, during the

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