Determining Biodegradability of Materials Exposed To Source-Separated Organic Municipal Solid Waste Mesophilic Composting Conditions by Respirometry

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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D5929 − 18

Standard Test Method for


Determining Biodegradability of Materials Exposed to
Source-Separated Organic Municipal Solid Waste Mesophilic
Composting Conditions by Respirometry1
This standard is issued under the fixed designation D5929; 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 (´) indicates an editorial change since the last revision or reapproval.

1. Scope 2. Referenced Documents


1.1 This test method covers the biodegradation properties of 2.1 ASTM Standards:2
a material by reproducibly exposing materials to conditions D513 Test Methods for Total and Dissolved Carbon Dioxide
typical of source-separated organic municipal solid waste in Water
(MSW) composting. A material is composted under controlled D1129 Terminology Relating to Water
conditions using a synthetic compost matrix and determining D1293 Test Methods for pH of Water
the acclimation time, cumulative oxygen uptake, cumulative D2908 Practice for Measuring Volatile Organic Matter in
carbon dioxide production, and percent of theoretical biodeg- Water by Aqueous-Injection Gas Chromatography
radation over the period of the test. This test method does not D6247 Test Method for Determination of Elemental Content
establish the suitability of the composted product for any use. of Polyolefins by Wavelength Dispersive X-ray Fluores-
1.2 This test is performed at mesophilic temperatures. Some cence Spectrometry
municipal compost operations reach thermophilic temperatures E1621 Guide for Elemental Analysis by Wavelength Disper-
during operation. Thermophilic temperatures can affect the sive X-Ray Fluorescence Spectrometry
biodegradation of some materials. This test is not intended to 2.2 APHA-AWWA-WEF Standard Method:3
replicate conditions within municipal compost operations that 2540G Total, Fixed, and Volatile Solids in Solid and Semi-
reach thermophilic temperatures. solid Samples
1.3 The values stated in both inch-pound and SI units are to
3. Terminology
be regarded separately as the standard. The values given in
parentheses are for information only. 3.1 Definitions—Definitions of terms applying to this test
method appear in Terminology D1129.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 3.2 Definitions of Terms Specific to This Standard:
responsibility of the user of this standard to establish appro- 3.2.1 acclimation time, n—the time required for the oxygen
priate safety, health, and environmental practices and deter- uptake to reach 10 % of the total measured cumulative oxygen
mine the applicability of regulatory limitations prior to use. uptake.4
1.5 This international standard was developed in accor- 3.2.2 inoculum, n—a mixture of organic substances in
dance with internationally recognized principles on standard- varying degrees of biodegradation to provide microbial-rich
ization established in the Decision on Principles for the substrate in which to perform biodegradation testing.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. 2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
1 3
This test method is under the jurisdiction of ASTM Committee D34 on Waste Available from American Public Health Assoc., 1015 15th Street, NW,
Management and is the direct responsibility of Subcommittee D34.03 on Treatment, Washington, DC 20005, Standard Methods for the Examination of Water and Waste
Recovery and Reuse. Water, 18th ed., 1992.
4
Current edition approved Feb. 1, 2018. Published February 2018. Originally Tabak, H. H. and Lewis, R. F., “CEC/OECD Ring Test of Respiration Method
approved in 1996. Last previous edition approved in 2009 as D5929 – 96 (2009). for Determination of Biodegradability,” U.S. Environmental Protection Agency, pp.
DOI: 10.1520/D5929-18. 1–3.

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

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D5929 − 18
3.2.3 oxygen uptake, n—the cumulative oxygen consumed 5.2 This test method provides a simulation of the overall
by the organisms during the test. compost process while maintaining reproducibility. Exposing
3.2.4 theoretical carbon dioxide production (ThCO2P), the test material with several other types of organic materials
n—the maximum carbon dioxide that can be produced by a that are typically in MSW provides an environment which
material as calculated by the carbon content of the material. provides the key characteristics of the composting process,
including direct measurement of organism respiration.
3.2.5 theoretical oxygen uptake (ThOU), n—the maximum
oxygen consumption required to fully oxidize a material based
6. Apparatus
on the elemental content of the material.
6.1 Compost Respirometry Apparatus (see Fig. 1):
3.2.6 virgin newsprint—nonprinted newspaper roll stock.
6.1.1 A minimum of six reactors, 2 to 6-L volume, with the
test material in triplicate and the controls in triplicate. The
4. Test Method
reactors should be surrounded with efficient insulation to
4.1 This test method consists of the following: minimize heat loss and be gastight. Insulation should be 8 cm
4.1.1 The test samples are prepared by cutting or forming of urethane foam or equivalent. A temperature-controlled water
the material into the form it would most likely be seen in the bath may be used as an alternative to insulating the vessels.
waste stream. A theoretical maximum carbon dioxide produc- 6.1.2 Tubing, with high resistance to gas permeation.
tion and oxygen uptake are determined from an elemental 6.1.3 Peristaltic Pump, to control and maintain gas flow
analysis. through each reactor.
4.1.2 An inoculum is obtained from a source-separated 6.1.4 4-L Scrubber Vessel, for each reactor fitted with a
organic MSW or yard waste compost facility. It is procured scrubber solution sampling port.
from compost that has been composting for at least two 6.1.5 Differential Pressure Switch, for each reactor that
months. actuates between 2 and 5 in. (51 and 127 mm) of water.
4.1.3 The synthetic organic MSW is prepared from virgin 6.1.6 Solenoid and Mass Flowmeter, to control and measure
newsprint, pine bark or wood chips, corn starch, corn oil, the addition of pure (99.997+) oxygen to system.
bovine casein, and urea. A buffer/dilution water is prepared 6.1.7 Temperature Probe, situated in the middle of the
from magnesium, calcium, iron, and a phosphate buffer. compost.
4.1.4 The test material, synthetic compost, inoculum, and 6.1.8 Data Acquisition and Control System, for the measure-
dilution water are combined and placed in a temperature- ment of temperature and the control and measurement of the
controlled reactor which monitors oxygen consumption and oxygen addition.
temperature and captures all evolved carbon dioxide.
6.2 Miscellaneous:
4.1.5 The system is monitored, and oxygen uptake rates,
6.2.1 Temperature Control Room, water bath, or hood to
temperature profiles, and total carbon dioxide produced are
maintain the external temperature of the apparatus at 40 6
recorded.
2 °C.
4.1.6 The total oxygen uptake and carbon dioxide produced
6.2.2 Flow Meter, to measure recirculation flow in each
are compared with the theoretical values obtained from the
reactor (optional).
elemental analysis, and a percent of biodegradation is calcu-
6.2.3 Computer Control of Peristaltic Pump, for automatic
lated. Possible negative effects of the material are evaluated by
recirculation flow control (optional).
observing the acclimation time of the synthetic MSW and
evaluating the oxygen uptake rate. 6.3 Suitable devices for the measurement of pH, dry solids
(105 °C), elemental analysis of material, carbon dioxide con-
5. Significance and Use tent of scrubbers, weight, and volume of the final compost
material.
5.1 MSW composting is considered an important compo-
nent in the overall solid waste management strategy. The NOTE 1—All apparatus components should be made of nonreactive and
volume reduction achieved by composting, combined with the nonabsorbing material.
production of a usable end product (for example, compost as a
soil amendment), has resulted in municipalities analyzing and 7. Test Materials
selecting source-separated organic MSW composting as an 7.1 The test materials can be in any form as long as their
alternative to landfill disposal of biodegradable organic mate- dimensions do not exceed 3 by 3 by 12 cm. The test materials
rials. This standard provides a method to analyze and deter- should be in the form that they would be present in the waste
mine the effect of materials on the compost process and the stream. A representative sample must be obtained by using
performance, utility, and feasibility of the composting process appropriate ASTM methods or other documented method.
as a method for managing organic solid waste material.5 Using 7.2 Analyze the test materials for carbon, hydrogen,
this method, key parameters of process performance, including nitrogen, oxygen, phosphorus, sulfur, and any other elements
theoretical oxygen uptake (ThOU) and theoretical carbon that are suspected to be present at a level to affect microbial
dioxide production (ThCO2P) are determined. metabolism and oxygen uptake. The ThOU must be calculated
for each material.
7.2.1 Guide E1621, Test Method D6247, or other reliable
5
The Biocycle Guide to Composting Municipal Wastes, JG Press, Inc., 1989. methods may be used for elemental analysis.

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D5929 − 18

Constituent Chemical Used Dry Weight, %

Cellulosics shredded, virgin newsprint 41


Inerts pine bark or wood chips 39
Carbohydrates corn starch 5.2
Lipids corn oil 5.4
Proteins bovine casein 2.0
Organic nitrogen urea 1.4
Buffer/Nutrient as listed 5.8
8.4 Polyethylene, or another non-biodegradable material is
the negative control material. It should be in the same form as
the test materials to provide the same physical conditions in all
reactors. The synthetic MSW acts as a positive control to verify
the viability of the inoculum, see 13.4 for requirements.

9. Hazards
9.1 This test method requires the use of hazardous chemi-
NOTE 1—The compost respirometer features a 4-L reactor vessel (A) cals. Avoid contact with the chemicals and follow the manu-
insulated with 8 cm of urethane foam. (A water bath may be used to facturer’s instructions and Safety Data Sheets.
control temperature as an alternative to insulation.) The atmosphere is
drawn through the reactor by a peristaltic pump (B) to maintain aeration.
9.2 This test method does not address all of the health and
The effluent gases are passed through a 4-L scrubber vessel (C) containing safety issues related to its use. It is the responsibility of the user
1.5 L of 5 M NaOH to remove any carbon dioxide from the effluent gas to establish appropriate safety measures.
stream. Samples are drawn from this scrubber solution during the
evaluation to determine the carbon dioxide released by the compost. As
9.3 High-purity, high-pressure gases can be dangerous if not
the microorganisms consume the oxygen in the system, a pressure drop handled correctly. Follow all safety precautions and monitor
occurs and is detected by a highly sensitive pressure switch (D). This the system often to ensure proper operation.
signals the data acquisition and control system (G) and the oxygen is
replaced with pure bottled oxygen by a solenoid (E) and the amount added 10. Inoculum
is measured by a mass flowmeter (F). The gases are then returned to the
reactor. A thermocouple (H) is centered in the test reactor to monitor the 10.1 The inoculum should be obtained from MSW or yard
temperature of the compost. The system is sealed to prevent interference waste that has properly composted for two to four months. The
from barometric fluctuations. compost should be screened with a <3-mm screen.
FIG. 1 Compost Respirometer Functional Diagram
10.2 The compost can be stored at room temperature for up
to 48 h before use. It should not be allowed to dry.
7.3 Calculate the ThCO2P from the carbon content of the
test material. See 12.2 for this calculation. 11. Procedure
7.4 The nitrogen content of the synthetic MSW should be 11.1 This procedure is for twelve 4-L reactors with 4-L
increased if the C/N ratio of the parent mixture is greater than scrubber vessels. Other configurations will need to adjust
40:1. This is accomplished by adjusting the urea content of the weights and volumes to maintain proportional liquid-to-solid
synthetic MSW. The synthetic MSW has adequate nitrogen to ratios of components.
support the addition of up to 35 g of carbon before the ratio 11.2 Synthetic Municipal Solid Waste:
exceeds 40:1. If the urea content is adjusted, all reactors 11.2.1 Dilution Water—Weigh out the ingredients for
including controls must contain the same concentration of urea. 3600 mL of dilution water. This will make enough dilution
water for 13 reactors:
8. Reagents and Materials Compound Quantity per Reactor Per 3600 mL
8.1 Scrubber Solution, containing 3.25 N NaOH in distilled
KH2PO4 1.87 g 24.5 g
water. Store in a gastight plastic container. Add 30 mg of Na2HPO4·7H2O 15.29 g 200 g
phenolphthalein to the solution to indicate scrubber exhaustion. MgSO4 0.003 g 0.039 g
CaCl22H2O 0.0076 g 0.099 g
8.2 Dilution/Buffer Solution, containing the following: FeCl3 0.0002 g 0.003 g
Chemical Purpose Concentration, g/L Urea 4.0 g 52 g
11.2.2 Dry Ingredient Preparation:
KH2PO4 phosphate buffer 6.8
Na2HPO4·7H2O phosphate buffer 55.6
11.2.2.1 Weigh out 120 g of shredded virgin newsprint and
MgSO4·7H2O nutrient 0.0225 place in a sealed plastic bag. Mark each bag with the actual
CaCl2 nutrient 0.0275 weight of newsprint.
FeCl3·6H2O nutrient 0.00025
11.2.2.2 Weigh out 115 g of 2.5 by 2.5 by 0.6-cm (approxi-
8.3 Synthetic Municipal Solid Waste, containing the mately) fresh wood chips or pine bark into a 1-L plastic beaker
following:6,7
7
U.S. Environmental Protection Agency, Office of Solid Waste and Emergency
6
Clark, C. S., et al., “Laboratory Scale Composting: Techniques,” Journal of the Response, “Characterization of Municipal Solid Waste in the United States, 1960 to
Environmental Engineering Division-ASCE, Vol 103, 1977, pp. 896–906. 2000,” (update 1988), EPA/530-SW-88-033, 1988.

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D5929 − 18
with 15.1 g of corn starch and 5.95 g of bovine casein. Repeat 11.8 End of Run:
until twelve sets of dry ingredients are prepared. 11.8.1 Sample the scrubber vessels in duplicate and analyze
11.2.3 Inoculum Preparation: for carbon dioxide content.
11.2.3.1 Obtain approximately 1 kg of mature compost from 11.8.2 Determine the total weight of the compost material
a municipal MSW or yard waste compost facility. and determine the dry solids concentration.
11.2.3.2 Screen compost with 3-mm wire mesh screen and 11.8.3 Measure the pH by diluting 10 g of sample with
retain the <3-mm portion that is used as the inoculum. 50 mL of distilled water (refer to Test Methods D1293). Shake
11.2.3.3 Weigh out 12 g of inoculum into each of twelve and measure pH immediately. If the pH of the compost is
weighing trays. below 7, determine the volatile fatty acids (VFA) content of the
11.3 Sample Preparation: compost (see Practice D2908). If the VFA is >2g/kg, the
11.3.1 Determine the dry solids of the test materials and reactors have soured and the results are invalid.
obtain the elemental analysis. Calculate the amount of test
material required to provide 50 g of ThOU. 12. Calculation
11.3.2 Prepare the control samples by using polyethylene as 12.1 Calculate the theoretical oxygen uptake (ThOU) from
the material and form or cut it into the same physical size and the percent by weight of each of the elements:
shape as the test material.
ThOU ~ mg O 2 /mg! 5 C/37.51H/12.51N/29.2 (1)
11.4 Reactor Loading:
11.4.1 Mix the shredded newsprint and the dry ingredients 1P/48.41S/66.7 2 O/100
and add the dilution water. Thoroughly mix until there are no 12.2 The theoretical carbon dioxide production (ThCO2P) is
clumps of paper or chemical. also determined from the elemental analysis and is calculated
11.4.2 Add 15.8 g of corn oil by dispensing directly to the as follows:
mixture. Mix the ingredients until the oil is evenly distributed.
ThCO 2 P ~ mg CO2 /mg! 5 ~ % by weight carbon! ~ 3.667! (2)
11.4.3 Add control or test product and mix until products
are evenly distributed. 12.3 Calculate the oxygen uptake due to the test material by
11.4.4 Add inoculum and thoroughly mix into compost. subtracting the mean of the control reactors from each of the
Load into reactor, taking care not to compact the compost test reactors at each data point.
mixture. 12.4 Calculate the total carbon dioxide produced by sub-
11.5 Scrubber Preparation: tracting the mean of the control analytical results from each of
11.5.1 Fill the scrubber vessels with 1.5 L of 3.25 N NaOH the test reactors.
solution. 12.5 Calculate the percent of theoretical total oxygen uptake
11.5.2 Add 30 mg of phenolphthalein indicator to the and carbon dioxide by dividing the measured totals by the
scrubber solution. calculated ThOU or ThCO2P and multiplying by 100.
11.5.3 Seal the scrubber vessel to minimize atmospheric
carbon dioxide absorption. 12.6 Calculate the standard deviation (Sd) of the triplicate
samples:
11.6 Run Startup:
11.6.1 Assemble test reactor system and allow system to
reach ambient temperature and stabilize. σ5 Œ 1 N
( ~x 2 µ!2
N i51 i
(3)
11.6.2 Sample the scrubber vessels and analyze for carbon
dioxide content by using Test Methods D513 or other suitable where:
method. xi = each individual sample, and
11.6.3 Set the recirculation pump to 100 mL/min or at a N = the number of samples.
level that will allow adequate aeration without excessive heat 12.7 Indicate the level of uncertainty based upon any known
loss. If the test reactor temperatures exceed 42 °C, increase the or observed limitations/precision of the test apparatus, includ-
aeration to keep the reactor temperature below 42 °C. ing measuring devices.
11.7 Run Operation: 12.8 The acclimation time for the test material and compost
11.7.1 The reactors are operated for a period of 45 days. matrix can be determined at the point when the oxygen uptake
Maintain ambient temperature at 40 °C. exceeded 10 % of the total oxygen uptake for that reactor.
11.7.2 Set the computer data acquisition system to collect
and store the temperature and oxygen uptake data a minimum 12.9 If the test materials’ oxygen uptake curve shows a
of once every 2 h. negative slope at the beginning of the curve, the test material
acclimation time is calculated at the point where the slope of
11.7.3 To prevent channeling, shake the reactors vigorously
the oxygen uptake curve becomes positive for a minimum of
once a week.
24 h.
11.7.4 There must be NO leaks in the system. The tubing
and fittings must be checked thoroughly at the beginning of the
test and after each shaking with a soap solution. Any leaks 13. Interpretation of Results
must be corrected immediately. The test apparatus should be 13.1 The acclimation time can provide valuable information
monitored daily to ensure proper operation. on the toxicity or inhibition effects of the test material.

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D5929 − 18
13.2 The percent of theoretical oxygen uptake is an excel- 14.1.3 Test material physical characterization including
lent measure of the biodegradability of the test material since size, shape, weight, dry weight, initial and final reactor
it represents the mineralization of carbon in addition to all observations, and sampling technique used.
other oxidative reactions. 14.1.4 Percent of ThOU and ThCO2P for each test material.
13.3 The percent of theoretical carbon dioxide production 14.1.5 Total oxygen uptake and oxygen uptake versus time
can be used to measure biodegradability (with limitations) and plots for entire reactors and test materials only. Rate plots if
can be used to correlate results with other carbon dioxide-based applicable.
test methods. 14.1.6 Acclimation times for test materials.
14.1.7 Total carbon dioxide produced and carbon dioxide-
13.4 To ensure an active and viable inoculum, the total versus-time plots if multiple samples were analyzed during the
oxygen uptake for the control reactors should exceed 80 g. If test.
this is not observed over the 45 days, then the test must be 14.1.8 Temperature plots of each reactor.
regarded as invalid and should be repeated with new inoculum. 14.1.9 Total weight loss of reactor contents and dry weight
13.5 If the standard deviation of the blank triplicate renders of end reactor contents.
a negative result when referenced to the mean of the triplicate, 14.1.10 Final pH of compost, investigative results if pH is
the test is invalid and should be repeated with new inoculum. below 7.
14.1.11 Full description of test apparatus and documenta-
14. Report tion of any variations from this test method.
14.1 Report the following information and data with stan-
dard deviations and 95 % confidence intervals when appropri- 15. Precision and Bias
ate: 15.1 Typical oxygen uptake and temperature plots are pre-
14.1.1 Information on source, dry solids, storage conditions, sented in Figs. 2 and 3. Within-test reproducibility from three
and age of the inoculum. different test runs are presented in Table 1. Run 1 is the control
14.1.2 The ThOU and ThCO2P of test materials with el- reactors with pine bark, Run 2 is with fresh wood chips, and
emental analysis results. Run 3 is with previously used wood chips.

FIG. 2 Typical Control Reactor, Test Reactor, and Net Test Reactor

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D5929 − 18

FIG. 3 Typical Temperature Plots, Ambient Set at 37 °C

TABLE 1 Within-Test Reproducibility for Three Synthetic MSW


Compositions
O2 Uptake, Standard CO2 Standard
g Deviation, % Produced, g Deviation,%
Run 1, pine bark 131 2.4 111 6.2
Run 2, new chips 134 0.82 115 4.0
Run 3, used chips 115 0.87 91.4 3.7

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