Astm D-5338 PDF

Download as pdf or txt
Download as pdf or txt
You are on page 1of 6

Designation: D 5338 – 98 (Reapproved 2003)

Standard Test Method for


Determining Aerobic Biodegradation of Plastic Materials
Under Controlled Composting Conditions1
This standard is issued under the fixed designation D 5338; 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 Solids, or Residue in Water3


1.1 This test method determines the degree and rate of D 2908 Practice for Measuring Volatile Organic Matter in
aerobic biodegradation of plastic materials on exposure to a Water by Aqueous-Injection Chromatography
controlled-composting environment under laboratory condi- D 3590 Test Methods for Total Kjeldahl Nitrogen in Water
tions. This test method is designed to yield reproducible and D 4129 Test Method for Total and Organic Carbon in Water
repeatable test results under controlled conditions that re- by High-Temperature Oxidation and Coulometric Detec-
semble composting conditions. The test substances are exposed tion
to an inoculum that is derived from compost from municipal E 260 Practice for Packed Column Gas Chromatography
solid waste. The aerobic composting takes place in an envi- E 355 Practice for Gas Chromatography Terms and Rela-
ronment where temperature, aeration and humidity are closely tionships
monitored and controlled. 2.2 APHA—AWWA—WPCF Standards:
1.2 This test method is designed to yield a percentage of 2540 D Total Suspended Solids Dried at 103 to 105°C4
conversion of carbon in the sample to carbon dioxide. The rate 2540 E Fixed and Volatile Solids Ignited at 550°C4
of biodegradation is monitored as well. 2.3 ISO Standard:
1.3 This test method is designed to be applicable to all ISO 14852 Plastics—Evaluation of the Ultimate Aerobic
plastic materials that are not inhibitory to the microorganisms Biodegradability and Disintegration Under Controlled
present in aerobic composting piles. Composting Conditions—Method by Analysis of Re-
1.4 The values stated in SI units are to be regarded as the leased Carbon Dioxide5
standard. 3. Terminology
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 3.1 Definitions—Definitions of terms applying to this test
responsibility of the user of this standard to establish appro- method appear in Terminology D 883.
priate safety and health practices and determine the applica- 4. Summary of Test Method
bility of regulatory limitations prior to use. Specific hazard
statements are given in Section 8. 4.1 This test method consists of the following:
1.6 This test method is equivalent to ISO 14852. 4.1.1 Selection of plastic material for the determination of
the aerobic biodegradability in a controlled-composting sys-
2. Referenced Documents tem,
2.1 ASTM Standards: 2 4.1.2 Obtaining an inoculum from composted municipal
D 618 Practice for Conditioning Plastics for Testing solid waste,
D 883 Terminology Relating to Plastics 4.1.3 Exposing the test substances to a controlled aerobic
D 1293 Test Methods for pH of Water composting process in conjunction with the inoculum,
D 1888 Test Methods for Particulate and Dissolved Matter, 4.1.4 Measuring carbon dioxide evolved as a function of
time, and
4.1.5 Assessing the degree of biodegradability.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics 4.2 The percentage of biodegradability is obtained by de-
and is the direct responsibility of Subcommittee D20.96 on Environmentally termining the percentage of carbon in the test substance that is
Degradable Plastics.
Current edition approved December 1, 2003. Published January 2004. Originally
approved in 1992. Last previous edition approved in 1998 as D 5338 - 98e1. 3
Discontinued.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 4
Standard Methods for the Examination of Water and Wastewater, 17th Edition,
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM 1989, American Public Health Association, 1740 Broadway, New York, NY 19919.
Standards volume information, refer to the standard’s Document Summary page on 5
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
D 5338 – 98 (2003)
converted to CO2 during the duration of the test. This percent- aeration rates. If using a direct measurement of CO2(see 6.4),
age of biodegradability will not include the amount of carbon then normal air may be used.
converted from the test substance that is converted to cell 6.1.4 Suitable devices for measuring oxygen and CO2
biomass and that is not, in turn, metabolized to CO2 during the concentrations in the exhaust air of the composting vessels,
course of the test. such as specific sensors or appropriate gas chromatographs.
4.3 The disintegration of a compact test material is visually 6.2 Carbon Dioxide-Trapping Apparatus for Each Com-
determined at the end of the test. Additionally, the weight loss posting Vessel:
of the test material may be determined. 6.2.1 At least three 5000-mL bottles fitted with gas sparging
and containing Ba(OH)2 carbon-dioxide scrubbing solution.
5. Significance and Use 6.2.2 Flexible Tubing, nonpermeable to carbon dioxide.
5.1 Biodegradation of a plastic within a composting unit is 6.2.3 Stoppers, equipped with gas-sampling parts.
an important phenomenon because it will affect the decompo- 6.3 Miscellaneous:
sition of other materials enclosed by the plastic and the 6.3.1 Analytical Balance, (60.1 mg) to weigh test speci-
resulting quality and appearance of the composted material. men.
Biodegradation of plastics will also allow the safe disposal of 6.3.2 100-mL Burette.
these plastics through solid-waste composting plants. This 6.3.3 0.05 N HCl.
procedure has been developed to permit the determination of 6.3.4 pH Meter.
the rate and degree of aerobic biodegradability of plastic 6.3.5 Suitable devices and analytical equipment for measur-
products when placed in a controlled composting process. ing dry solids (at 105°C), volatile solids (at 550°C), volatile
5.2 Limitations—Because there is a wide variation in the fatty acids by aqueous-injection chromatography, total
construction and operation of composting systems and because Kjeldahl nitrogen and carbon concentrations.
regulatory requirements for composting systems vary, this 6.4 Optional—The carbon dioxide-trapping apparatus and
procedure is not intended to simulate the environment of any titration equipment can be replaced by a gas flow meter plus a
particular composting system. However, it is expected to gas-chromatograph, or other apparatus equipped with suitable
resemble the environment of a composting process operated detector and column(s), for measuring CO2 and O2 concentra-
under optimum conditions. More specifically, the procedure is tions in the exhaust air of each vessel. Take care to analyze
intended to create a standard laboratory environment that will CO2 concentration on a sufficiently frequent basis in order to
permit a rapid and reproducible determination of the aerobic produce a reliable cumulative CO2 production over the course
biodegradability under controlled composting conditions. of the test (for example, every 3 to 6 h). A standard gas should
be injected to internally standardize the gas-chromatograph on
6. Apparatus a continuous basis over the course of the test. Operate the gas
6.1 Composting Apparatus (see Fig. 1): chromatograph in conformance with Practices E 260 and E 355
6.1.1 A series of at least twelve composting vessels (one test (see Fig. 2).
substance, one blank, one positive and one negative control, all 6.5 Ensure that all glassware is cleaned thoroughly and free
in three replicates) of 2 to 5 L of volume. For screening from organic matter.
purposes, depending upon the test material, a smaller volume
also may be used. 7. Reagents and Materials
6.1.2 Water Baths, or other temperature controlling means 7.1 Barium Hydroxide Solution, approximately 0.024 N and
capable of maintaining the temperature of the composting then standardized, prepared by dissolving 4.0 g Ba(OH)2 per
vessels at 58°C (62°C). litre of distilled water. Filter through filter paper and store
6.1.3 Pressurized-Air System, that provides CO2-free, H2O- sealed as a clear solution to prevent absorption of CO2 from the
saturated air to each of the composting vessels at accurate air.

FIG. 1 Set-Up Using Carbon Dioxide-Trapping Apparatus FIG. 2 Optional Set-Up Using a Gas Chromatograph

2
D 5338 – 98 (2003)
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 µm as positive control.6 bic composting plant treating municipal solid waste, or the
7.3 Polyethylene, as a negative control. It should be in the organic fraction thereof. If required, further stabilize the
same form as the form in which the sample is tested (polyeth- inoculum at the laboratory in order to obtain a low CO2
ylene film for film samples, polyethylene pellets in case sample production (see 9.1.).
is in the form of pellets, etc.). 11.1.1.1 Screen the inoculum to less than 10 mm and
manually remove and discard any large inert items (pieces of
8. Hazards
glass, stone, wood, etc.). Determine volatile solids, dry solids
8.1 This test method requires the use of hazardous chemi- and nitrogen content according to Test Methods D 3590,
cals. Avoid contact with the chemicals and follow manufactur- D 1888, and APHA Test Methods 2540 D and 2540 E.
er’s instructions and Material Safety Data Sheets.
11.1.2 Determine volatile solids, dry solids and carbon
8.2 The compost inoculum may contain sharp objects. Take
content of all the test substances according to APHA Test
care when handling it.
Methods 2540 D and 2540 E and Test Method D 4129.
8.3 The composting vessels are not designed to withstand
high pressures. The system should be operated at close to 11.1.3 Weigh out roughly 600 g of dry solids of inoculum
ambient pressure. and mix with about 100 g of dry solids coming from the
sample. Adjust the dry solids content of the mixture in the
9. Compost Inoculum vessel to approximately 50 % with distilled water. Add ammo-
9.1 The compost inoculum should be two to four months old nium chloride if the C/N ratio is more than 40. Weigh vessels
well-aerated compost coming from the organic fraction of with all of the contents immediately before initiation of the
municipal solid waste and sieved on a screen of <10 mm. If composting process.
such a compost is not available, compost from plants, treating 11.1.4 The blank consists of the inoculum only, containing
green, or yard waste, or mixtures of green waste and municipal about 600 g of dry solids. As references, use thin-layer
solid waste may be used. It is recommended that the compost chromatography cellulose as a positive control and polyethyl-
inoculum produces between 50 and 150 mg of CO2 per gram of ene as a negative control.
volatile solids over the first ten days of the test, and has an ash 11.1.5 The test material may be in the form of films, formed
content of less than 70 % and a pH between 7 and 8.2. Total dry articles such as dog bones, granules, or powder. The maximum
solids should be between 50 and 55 %. surface area of a compact test material used should be about 2
9.2 The compost inoculum should be as free from larger by 2 cm. In case the original test material is larger, reduce it in
inert materials (glass, stones, metals, etc.) as possible. These particle size.
items should be removed manually as much as possible to 11.1.6 No more than about 3⁄4 of the volume of the test
produce a homogeneous compost inoculum. vessel should be filled with test mixture. Sufficient headspace
9.3 It is recommended to use compost of sufficient porosity is required in order to provide enough space for manual
to enable conditions to be as aerobic as possible. Addition of shaking of the test mixture.
structural material, such as small wood particles, or persistent 11.2 Start-Up Procedure—Initiate aeration of the compost-
or poorly biodegradable inert material may prevent the com- ing vessels with air-flow rates that are sufficiently high to
post from sticking together and clogging during the test. ensure that oxygen levels do not drop below 6 % in the exhaust
10. Test Specimen air. Oxygen levels should be closely controlled during the first
week and measured at least twice daily. Adjust air-flow rates as
10.1 The test specimen should have sufficient carbon to
needed.
yield carbon dioxide that can be adequately measured by the
trapping apparatus or CO2 measurements. 11.3 Operating Procedure:
10.2 All basic composting parameters, such as C/N, oxygen 11.3.1 The composting vessels are incubated in the dark or
in the composting vessel, porosity, and moisture content should in diffuse light for a period of 45 days in an enclosure that is
be optimized so as to make a good composting process free from vapors toxic to microorganisms. The temperature is
possible. The C/N ratio should preferably be between 10 and maintained at 58°C (62°C). In special cases, for example,
40 for both the inoculum and test substance combined. Oxygen when the melting point of the test material is low, another
levels in the composting vessel should be at least 6 % at all temperature may be chosen. This temperature should be
times and no free-standing water nor clumps of material should constant during the test and kept in a range of 62°C. The
be present. change of temperature should be justified and clearly indicated
10.3 Test specimens may be in the form of films, formed in the test report.
articles, dog bones, granules, powder, or other, and conform to 11.3.2 Check CO2 and O2 concentrations in the outgoing air
Practice D 618. at least daily with a minimum time interval of 6 h after the first
week for the remainder of the test.
11. Procedure
11.3.3 Check air flow daily before the composting vessels
11.1 Preparation of the Samples: and at the outlets, ensuring that no leaks are present in the
complete system. Adjust air flow to maintain a CO2 concen-
6
For development of this test method, Avicel, available from EM Chemicals, tration of at least 2 % volume over volume to allow accurate
Inc., Hawthorne, New York, was used. determination of CO2 level in the exhaust air.

3
D 5338 – 98 (2003)
11.3.4 Ensure proper composting conditions. Shake the Ba~OH!2 1 CO2 → BaCO3 1 H2O
composting vessels weekly to prevent extensive channelling, 12.2.1.2 The BaCO3 formed is insoluble and precipitates.
provide uniform attack on the test specimen and provide an Determine the amount of Ba(OH)2 remaining in solution by
even distribution of moisture. In case excessive moisture levels end-point titration with HCl using phenolpthalein as an indi-
are observed, such as free-standing water in the vessels or cator according to the following equation:
clumping due to high moisture content, remove excess liquid
Ba~OH!2 1 2 HCl → BaCl2 1 2 H2O
by injecting dry air, or by drainage via air inlet. If excessively
dry conditions are observed, that will severely slow down the 12.2.1.3 From the above two equations, it can be seen that
breakdown process, add moisture. During the whole course of the number of mmol of CO2 produced is:
the test, make adjustments to ensure proper composting con- mmoles HCl
ditions. If adjustments are made, then CO2 and O2 concentra- mmoles of CO2 5 mmoles of Ba~OH!2 at start 2 2
tions must be monitored closely during the following 72 h and
12.2.2 For the option with gas chromatography, the cumu-
measured at least twice daily with a time interval of more than
lative CO2 production (in grams) is determined from the
6 h.
measurements of flow rate and gas composition and after
11.3.5 At the weekly shaking and at the end of the test,
recalculation to STP (standard temperature and pressure)
record visual observations with regard to compost structure,
conditions.
moisture content and color, fungal development, smell of the
exhaust air, and sample disintegration. 12.2.3 Calculate the amount of cumulative gaseous-carbon
11.3.6 The incubation time of 45 days may be extended if produced by each reactor.
significant biodegradation of the test substance is still being 12.2.4 Determine the mean (of the three replicates) net
observed. 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. Volatile solids may be determined if 12.3 Calculate the percent of biodegradation by dividing the
weight loss is to be calculated. average net gaseous-carbon production of the test compound
11.4.2 Measure the pH in conformance with Test Methods by the original average amount of carbon in the test compound
D 1293. If the pH is less than 7, measure the volatile fatty acids and multiplying by 100:
spectrum to indicate souring of the contents in the composting mean Cg~test! 2 mean Cg~blank!
% biodegradation 5 3 100
vessel in accordance with Practice D 2908. Measure the pH by Ci
diluting the sample on a 5:1 w/w ratio of distilled water to
compost inoculum or residue, mix by shaking manually and where:
measure immediately. Cg = amount of gaseous-carbon produced, g, and
Ci = amount of carbon in test compound added, g.
11.4.3 If more than 2 g of volatile fatty acids per kilogram
of dry matter in the composting vessel is formed, the test must 12.4 Calculate the standard error, se, of the percentage of
be regarded as invalid. biodegradation as follows:
Se 5 SQRT~~s2test/n1! 1 ~s2blank/n2!! 3 100/Ci
12. Calculation n1 and n2 are the number of replicate test and control digesters
12.1 Determine the total carbon content of the test material respectively; s is the standard deviation of the total gaseous
by elemental analysis or by calculation if the chemical com- carbon produced.
position is well established. This allows the theoretical quantity
12.5 Calculate the 95 % confidence limits as follows:
of carbon dioxide evolution to be calculated as follows:
95 % CL 5 % biodegradation 6 ~t 3 se!
material 5 w % carbon
w/100 3 g of material charged 5 Y g carbon charged to Where t is the t-distribution value for 95 % probability with
(n1 + n2 − 2) degrees of freedom; thus n = 3 + 3 − 2 = 4.
compost vessel 5 Ci
C 1 O2 → CO2 13. Interpretation
12 g C yields 44 g CO2
13.1 Information on the toxicity of the plastic material may
44 3 Y be useful in the interpretation of inhibitive effects.
Y g C yields 12 g CO2
13.2 In most instances when investigating a plastic material,
12.2 Determine the cumulative CO2 production (in grams) a reference or control substance known to biodegrade is
from the test substances. necessary in order to check the activity of the inoculum. If
12.2.1 Determine the amount of CO2 produced by the sufficient biodegradation (a minimum of 70 % for cellulose
difference, in millilitres of titrant, between the test substance within 45 days) is not observed with the positive reference, the
and blank Ba(OH)2 traps. Perform the titration with 0.05 N test must be regarded as invalid and should be repeated, using
HCl. new inoculum. If the deviation of the percentage of biodegra-
12.2.1.1 When CO2 enters the absorber bottles, it reacts in dation of the positive reference is greater than or equal to 20 %
the following manner: at the end of the test, then the test shall be regarded as invalid.

4
D 5338 – 98 (2003)
14. Report 14.1.11 Results on weight measurements of compost vessels
14.1 Report the following data and information: at the start and at the end of the test, and test material weight
14.1.1 Information on the inoculum, including source, per- loss, if determined.
cent dry solids, percent volatile solids, total Kjeldahl nitrogen,
activity (CO2 production in the first ten days), date of collec- 15. Precision and Bias
tion, storage, and handling. 15.1 The precision and bias of the procedure in this test
14.1.2 Carbon content of the plastic materials, positive and method is being determined.
negative control, and calculation of the theoretical maximum 15.2 Preliminary results for within-laboratory repeatability
carbon dioxide production. Report specific information on the testing using a controlled composting set-up with gas chro-
size, shape, volume, and thickness of the plastic materials matograph are presented in Table 1. These data represent three
tested, along with the form of the plastic material, that is, sheet, different determinations of the degradation of cellulose as a
powder, pellet, etc., positive reference. The average degradation of cellulose after
14.1.3 Weight of vessels with contents before and at the end 45 days of composting at a constant temperature of 50°C
of the test, (62°C) was 75.3 %, with an average standard deviation of
14.1.4 Cumulative carbon dioxide evolution and oxygen 2.5 % and an average 95 % confidence limit interval of 5 %.
consumption over time and display graphically. Report appa- All three runs were carried out within a seven-month period by
ratus used for carrying out the test method, the same operators. Fig. 3, 4, and 5 represent a graphical view
14.1.5 Percentage of aerobic biodegradation for each plastic of the third run in which a biodegradability of 78.9 % was
material tested, the standard deviation and 95 % confidence obtained as the mean for the three replicates containing
interval for each material or control substance tested for the cellulose as the positive control, with a standard deviation of
percent of biodegradation, 0.3 % and a 95 % confidence limit interval of 2 %. The graphs
14.1.6 Percentage of biodegradation relative to the positive represent the results from three replicates for the inoculum only
reference (cellulose = 100 %), as the blanks (see Fig. 3), the cellulose as the positive control
14.1.7 Temperature range of test, (see Fig. 4) and the net CO2 production per gram of cellulose
14.1.8 pH of compost inoculum and pH of final residues. added (see Fig. 5).
Volatile fatty acids concentration for vessels with a final pH of
less than 7, 16. Keywords
14.1.9 Results on the visual observations of the compost
inoculum and the test material during and at the end of the test, 16.1 aerobic biodegradation; biodegradation; composting;
such as moisture content, fungal development, structure, color, plastics
and smell,
14.1.10 Describe qualitatively the disintegration of the test
material in the case of a compact test material. Add further
information, such as photographs or measured physical values,
if these are available, and

TABLE 1 Results from Within-Laboratory Testing for the Aerobic


Biodegradability of Cellulose as a Positive Control Under
Controlled Composting Conditions
95 %
Biodegradability Standard
Confidence
after 45 days, % Deviation, %
Limit, %
Run 1 76.7 4.9 8.2
Run 2 70.3 2.4 4.8
Run 3 78.9 0.3 2.0
Mean of Three Runs 75.3 2.5 5.0
FIG. 3 Cumulative CO2 Production from Inoculum

5
D 5338 – 98 (2003)

FIG. 5 Net Cumulative CO2 Production from Cellulose


FIG. 4 Cumulative CO2 Production from Inoculum Plus Cellulose

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, 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 comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International 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, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or [email protected] (e-mail); or through the ASTM website
(www.astm.org).

You might also like