coupling a respirometer and a pycnometer, to study the biodegradability of solid organic wastes...
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B I O S Y S T E M S E N G I N E E R I N G 9 7 ( 2 0 0 7 ) 7 5 – 8 8
1537-5110/$ - see frodoi:10.1016/j.biosys
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Research Paper: SE—Structures and Environment
Coupling a respirometer and a pycnometer, to study thebiodegradability of solid organic wastes during composting
L. Berthea, C. Druilhea,�, C. Massianib, A. Tremiera, A. de Guardiaa
aCemagref, Livestock and Municipal Waste Management Research Unit, 17 av. de Cucille CS 64427-35044 Rennes Cedex, FrancebUniversite de Provence, Laboratory of Chemistry and Environment, 3 pl. Victor Hugo-13331 Marseille Cedex, France
a r t i c l e i n f o
Article history:
Received 5 August 2006
Accepted 31 January 2007
Available online 11 April 2007
nt matter & 2007 IAgrE.temseng.2007.01.013
thor.: celine.druilhe@cemagr
A new method, coupling a respirometer and a pycnometer, to follow the biodegradation of
solid organic wastes is presented. The pycnometer was used to observe the development of
the free air space in the sample during the respirometric experiments and verified that this
parameter remained favourable to the substrate oxygenation. To test this new method,
respirometric experiments were conducted on four solid waste samples (a mixture of
agrofood sludge and pine bark chips, a mixture of urban sludge with new and reused pine
bark chips collected before and after 21 days of composting, and a mixture of household
wastes).
The respirometer is based on a 10 l reactor filled with the sample. It was designed to
allow the control of operating conditions: temperature, moisture and aeration. During
respirometric experiments, the material temperature was constant and homogeneous.
However, large variations in the moisture content were measured between the beginning
and the end of respirometric tests. Moreover, the development of moisture variability
throughout the substrate was observed. The aeration regime was characterised as a
perfectly mixed phase considering the results of retention time-distribution studies and
the free air space values measured with the pycnometer. The pycnometer accuracy was
confirmed by low differences between experimental and theoretical free air space values
for water and spherical glass beads. Moreover, it was verified that this measurement had no
influence of respirometric responses.
Applying the proposed method to the four substrates demonstrated the interest in
mixing the material during the respirometric tests, when the oxygen uptake rate rO2 fell to
a low and stable value. Indeed, in some cases, such mixing stimulated the restart of rO2 that
confirmed the presence of residual biodegradable organic matter. The major effect of
mixing was to restore favourable moisture content throughout the substrate. The results
revealed that a small mixing impact corresponded to either a low substrate biodegrad-
ability or a high initial moisture content. The pycnometer measurements demonstrated the
influence of a low free air space. It appeared that the absence of oxygen uptake restart after
mixing, in the presence of residual organic matter, could be due to a low free air space.
These results demonstrated the need (i) to mix the samples to quantify all its
biodegradable organic matter and (ii) to control the moisture, temperature and aeration to
ensure favourable conditions of biodegradation.
& 2007 IAgrE. All rights reserved. Published by Elsevier Ltd
All rights reserved. Published by Elsevier Ltdef.fr (C. Druilhe), [email protected] (C. Massiani).
ARTICLE IN PRESS
Nomenclature
C(t) concentration of methane at time t, ppm
C0 initial concentration of methane, ppm
n moles of gas in the system, mol
na0 initial moles of gas in the additional cell, mol
nr0 initial moles of gas in the reaction cell, mol
na1 intermediate moles of gas in the additional cell,
mol
nf final moles of gas in the reaction and additional
cells, mol
P system pressure, Pa
Pa0 initial pressure in the additional cell, Pa
Pa1 intermediate pressure in the additional cell, Pa
Pf final pressure in the additional and reaction cells,
Pa
Pr0 initial pressure in the reaction cell, Pa
Qe inlet airflow rate, l h�1
Qr recirculation airflow rate, l min�1
R gas constant, J K�1 mol�1
S free air space, %
Sexp experimental free air space, %
Sth theoretical free air space, %
T gas temperature, K
Ta0 initial gas temperature in the additional cell, K
Ta1 intermediate gas temperature in the additional
cell, K
Tc water-bath temperature, 1C
Tr0 initial gas temperature in the reaction cell, K
Tf final temperature in the additional and reaction
cells, K
t time in retention time distribution experiments, s
t0 beginning of respirometric tests, h
t1 time of the first mixing, h
t2 time of the second mixing, h
t3 time of the third mixing, h
tf end of the respirometric tests, h
V system volume, m3
Va volume of the additional cell including pipes, m3
Vg volume of the whole sample including solid and
voids, m3
Vr volume of the reaction cell including pipes, m3
VRTD system volume during retention time distribution
experiments, l
Vs volume of solid sample without free air space, m3
Vs,exp experimental volume of solid sample without free
air space, l
Vs,th theoretical volume of solid sample without free
air space, l
s2reduced variances
t residence time, s
m time of passage, s
B I O S Y S T E M S E N G I N E E R I N G 9 7 ( 2 0 0 7 ) 7 5 – 8 876
1. Introduction
The production of wastes is continuously increasing [e.g.
627 Mt year�1 in France in 2002; Ademe (2006)] and efficient
ways to treat and recycle them are needed. For organic wastes,
about 450 Mt (Ademe, 2006), composting appears as one of the
most promising options since the wastes could be converted
into useful agricultural products. However, the development of
composting often encounters limitations due to poor compost
quality resulting from a lack of treatment management.
Indeed, the quality of compost depends on the method of
preparing the initial material and the management of the
reactions occurring during the process. Composting, as an
aerobic treatment process, comprises three interdependent
phenomena: mass transfer, heat transfer and biological
processes (Haug, 1993). The mass and heat transfer operations
are closely linked to the kind of process applied, whereas the
biological reactions mainly depend on both substrate charac-
teristics (such as the amount and type of biodegradable organic
matter) and environmental conditions (such as temperature,
aeration level and moisture content) (Moletta, 2006). Thus, the
development of methods to study the processes of biodegrada-
tion, and to quantify and identify the biodegradable organic
matter content of samples, appears as a key step to achieve a
well-managed composting process (the optimisation of the
initial mixture, the composting time, the airflow rate).
The biological reactions—the use of the organic matter by
microorganisms—induce the consumption of oxygen and the
production of carbon dioxide. Therefore, the methods for
monitoring these parameters, called respirometric methods,
could be considered as a direct measure of biological activity.
For this reason, respirometric measurement is accepted as
being the more suitable method to study organic matter
biodegradation (Adani et al., 2006). Nevertheless, the respiro-
metric methods that monitor only the carbon dioxide
production could induce a misunderstanding of biological
processes and an underestimation of sample biodegradability.
Indeed, carbon dioxide results from both aerobic and
anaerobic reactions and, even if composting is an aerobic
treatment, the development of local zones with anaerobic
conditions could be observed (Haug, 1993; Epstein, 1997).
Therefore, methods based on oxygen uptake rate were
preferred to estimate the biodegradability potential of solid
organic wastes at the beginning, during and at the end of
composting.
Numerous methods based on oxygen uptake have been
proposed in the past. They are divided into static and
dynamic methods on the basis that oxygen uptake measure-
ment is made in the absence (static) or in the presence
(dynamic) of continuous aeration of the biomass (Adani et al.,
2004). Static methods induce limitation of oxygen transfer
through the biomass layers and into bacterial cells that
reduce or inhibit the aerobic biological processes (Adani et al.,
2002; Paletski & Young, 1995). In this condition, sample
biodegradability may be greatly underestimated. The dy-
namic methods have the advantage of minimising the
limitation of oxygenation. In these systems, the respirometric
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B I O SYS T EM S E NG I NE E R I N G 97 (2007) 75– 88 77
reactor filled with the studied sample is continuously
supplied with oxygen to ensure its diffusion in the whole
matter and aerobic conditions.
In addition to the dependency on the aeration level, the
biological processes are also linked to the structure, tempera-
ture and moisture of samples (Haug, 1993). To take into
account the sample physical structure [moisture, granulome-
try, porosity, free air space (FAS)] and its consistency, the
respirometric test has to be performed on substrates repre-
sentative of those in the compost system. However, most
existing dynamic respirometers cannot be used as they work
with small sample quantities, at best 1.5 l (Aguilar-Juarez,
2000) but commonly 10–100 g (Gomez et al., 2006; Ianotti et al.,
1994; Paletski & Young, 1995). Four respirometric systems
have been identified to provide a reaction volume permitting
work with raw materials: (1, 2) the Dynamic Respiration Index
design with two size of reaction volume (Adani et al., 2004,
2006) and (3, 4) the respirometers developed by Tremier et al.
(2005b) and Gea et al. (2004). The systems proposed by Adani
et al. (2004, 2006) have a sample reactor of 124 or 30 l. The one
presented by Gea et al. (2004) was set up with a reaction cell of
100 l and a reaction volume of 10 l is used in the system of
Tremier et al. (2005b). Compared to the others, the last
apparatus has two main advantages. First, its aeration system
includes a recirculation of a part of the exhaust air that
ensures a more homogeneous oxygen diffusion to the
biomass than a single forced aeration method. Thus, oxygen
is not limiting to biodegradation (Tremier et al., 2005b).
Second, in this system, the smaller reaction cell and its
immersion in a water-bath help to achieve good maintenance
and homogeneity of temperature and moisture anywhere in
the substrate and throughout the tests. In these conditions,
analysis and comparison of respirometric profiles are easier.
The preliminary experiments carried out on this respirom-
eter revealed a limitation of this tool since all biodegradable
organic matter was not degraded during the main peak of
oxygen uptake rate rO2 typically observed in respirometry. The
presence of residual biodegradable organic matter was
illustrated by a second peak of rO2 (representing between
23% and 37% of the total oxygen consumed) after a manual
material turning. This mixing was realised after the first peak
when the rO2 fell to a low and stable value, usually due to the
absence of biodegradable organic matter and considered as
the endogenous respiration. There were two possible reasons
for the presence of residual biodegradable organic matter.
First, the moisture variability throughout the material,
visually observed, during respirometry resulted in local zones
of the material with limiting moisture content for biodegra-
dation. Second, the limitation of biodegradation resulted from
an insufficient sample FAS that implied oxygen diffusion
problems. Indeed, the material moisture and the FAS are
known as being limiting factors of biodegradation (Haug,
1993). The operation of mixing re-homogenised the sample
and helped to restore favourable conditions of moisture and
FAS in the whole sample. Therefore, biodegradation of the
organic matter was restarted, which generated a new peak of
oxygen uptake rate. To follow the variation in FAS during
respirometric tests by in situ measurement, a specific device
was designed and combined with the respirometer. An air
pycnometer was used rather than other methods such as
specific gravity bottle, water retention apparatus, mercury
porosimetry and nitrogen absorption, paraffin wax method,
and water pycnometers (Agnew et al., 2003). The main
advantage of the air pycnometer is the possibility of measur-
ing precisely the material FAS during respirometric tests
without modifying the sample filling the respirometric cell.
The air pycnometer provides indirect space measurements by
relating the system’s pressures and volumes using the ideal
gas law.
The objective of this paper is to present the method,
coupling a respirometer and a pycnometer, developed to
study the aerobic biodegradation of solid organic wastes. The
respirometric method was chosen and then modified to
ensure efficient control of the environmental conditions
(temperature, moisture and aeration) and to allow the
measurement of sample FAS. The control of temperature
and moisture was studied by following these parameters
during respirometric experiments. The matter oxygenation
quality was controlled by the measurement of FAS all along
the respirometric tests and was specifically characterised
with retention time-distribution (RTD) experiments. The
validity and impact of the FAS measurements were studied
before applying this method during respirometric tests.
The FAS measurements and the respirometric profiles,
obtained for four substrates [a mixture of agrofood sludge
and pine bark chips, a mixture of urban sludge with new and
reused pine bark chips collected before and after 21 days of
composting, and a mixture of household wastes (HW)], were
used to prove the advantages of coupling respirometry and
pycnometry.
2. Materials and methods
2.1. Respirometric device
The respirometric device (Fig. 1) was set up on the basis of the
apparatus developed by Tremier et al. (2005b). This comprised
a 10 l hermetically closed glass reactor with a grid floor filled
with the sample under investigation. Ambient air is fed
through the bottom along with recirculation air to provide
homogeneous aeration conditions. The temperature was
controlled by a water-bath. Humidification of the inlet air
and condensation of the exhaust gas on the sample are used
to control the matter moisture content. This system was
modified to optimise the control of operating conditions
(temperature and moisture) and to adapt it to FAS measure-
ments. A 10 l cell made of stainless steel replaced the glass
reactor. The cell was made of stainless steel to resist the
compression required for FAS measurement. The cell was
filled with the sample put on a 3 mm round mesh grid placed
70 mm above the cell bottom. The system was supplied from
the bottom via a diffuser with compressed air instead of
ambient air to minimise the entering gas characteristic
variations (temperature, moisture, composition). Moreover,
the inlet airflow rate Qe increased from 50 to 60 l h�1 and the
recirculation airflow rate Qr from 4–5 to 6 l min�1.
To increase the temperature control in terms of homo-
geneity and stability, the respirometric cell was completely
immersed in a water-bath and was supplied with preheated
ARTICLE IN PRESS
Comair counter
Serpentine (Air preheating)
Sample respirometric cell
B
A
Compressed Gas volume
FlowmeterFlowmeter
Flowmeter
Pump
ThermostatWater bath
Sample Stainless steel
Pt100
Temperature and moisture probe
Air diffuserAir moisture saturation
Analyser
Insulation
Condenser bottle
B
A
Methane injection
Methane injection
point B
point A
Fig. 1 – Respirometric device after modifications to improve environmental parameter control.
B I O S Y S T E M S E N G I N E E R I N G 9 7 ( 2 0 0 7 ) 7 5 – 8 878
air at water-bath temperature Tc. The air was preheated by
passing through a copper serpentine placed in the water-bath
(diameter of 10 mm; thickness of 2 mm; length of 2 m). As in
the original apparatus, the matter temperature is measured
with a Pt100 temperature probe placed in the sample centre.
The moisture-controlled system was completely modified.
The inlet gas was saturated in humidity at the water-bath
temperature by passing through two glass bottles filled with
water. The bottles were immersed in the water-bath and filled
daily with water. The exhaust air was condensed out of the
cell, in specific bottles placed at ambient temperature.
Condensation of the exhaust air outside the cell limited the
possibility of localised water falling back on the sample.
The oxygen uptake rate was obtained by measuring oxygen
concentrations with a paramagnetic oxygen gas analyser
(Multor 710, Maihak, Hamburg, Germany) in the inlet and
exhaust gas.
2.2. Optimisation of the aeration conditions
The distribution of oxygen concentration in the studied
material has to be homogeneous and provided in sufficient
quantity to create favourable aeration conditions for biode-
gradation. Aeration was characterised by the hydrodynamic
of the gas phase and was influenced by the material FAS.
The gas flow distribution was studied through the RTD
measurement method (Roustan, 2003). This method consists
of determining the time passed by each molecule in the
circuit and of quantifying them in the exhaust gas. Practically,
a gas tracer was injected in the circuit and the concentration
of this particular gas was monitored in the outlet gas.
Methane was chosen as a gas tracer after having verified
that there was no significant methane production during
the respirometric experiments and it was not noxious for
microorganisms. Moreover, its hydrodynamic characteristics
were similar to those of air. The concentration of methane in
the exhaust gas was measured every 2 s using the gas
analyser (Multor 610, Maihak, Hamburg, Germany). The
injection of the gas tracer was a pulse type of 10 ml of pure
methane at point B of the respirometric circuit (Fig. 1).
The variation in methane concentration in the whole circuit
was monitored for an inlet airflow rate of 55 l h�1 and 0, 2, 4, 6
and 7 l min�1 as recirculation flow rates. The substrate
studied was composed of pine bark chips (global volume of
5 l; FAS of 64%). The tracing trials were duplicated for the
same recirculation airflow rate. The RTD curves were
obtained as the ratio between the concentration C(t) in
methane at each time t in the outlet gas and the concentra-
tion in methane in the inlet flow C0. Methane recovery rate
was estimated as the difference between the injecting
quantity of this component (10 ml) and the volume of
methane recovered in the exhaust flow.
To interpret the tracings carried out on the whole circuit,
the flow in the analytical device was characterised during
previous tracing experiments by the injection of methane at
point A (Fig. 1). This has shown that the hydrodynamic of the
analytical circuit was of a plug type that induced a delay in
the response and non deformation. The absence of methane
losses was also checked in these experiments.
The interpretations of the curves concerned: (i) the repeat-
ability of tracing; (ii) the determination of methane recovery;
(iii) the comparison of residence time t and the time of
passage m; (iv) the estimation of the reduced variances s2 and
(v) the comparison between the experimental RTD and the
RTD of a perfectly mixed phase (Roustan, 2003):
t ¼VRTD
Qe, (1)
m ¼
RtCðtÞdtRCðtÞdt
¼
PtCðtÞPCðtÞ
, (2)
s ¼
Rðt�mÞ2CðtÞ dtR
CðtÞ dt
m2¼
Pt CðtÞPCðtÞ� m
� �
m, (3)
where t is the time in s; C(t) is the methane concentration in
ppm of the exhaust gas at time t; VRTD is the system volume in
l; and Qe is the inlet airflow rate in l h�1.
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B I O SYS T EM S E NG I NE E R I N G 97 (2007) 75– 88 79
In our case, for all parameters the sums replaced the
integrals because the experimental data were registered at
regular and small time intervals (every 2 s).
2.3. Measurement of free air space
2.3.1. Pycnometer deviceAir pycnometer (Fig. 2) provides indirect FAS measurements
by relating the system’s pressures and volumes using the
ideal gas law:
P V ¼ n R T, (4)
where P is the pressure in Pa; V is the volume in m3; n is the
gas mole amount in mol; R is the gas constant in J K�1 mol�1;
and T is the gas temperature in K.
The sample is placed in one chamber while a second
chamber is supplied with compressed air to a specific
pressure. The air is allowed to equilibrate between the two
chambers and the resulting pressure is used to calculate the
air space volume in the sample (Agnew et al., 2003).
The pycnometer consisted of two stainless-steel cells (25 l
additional cell and 10 l reaction cell), a three-way control
valve, an absolute pressure transducer (Druck, 0–3.5 absolute
bar, Asnieres, France) and two Pt100 temperature probes (one
in each cell). An absolute pressure transducer was preferred
to a gauge to measure a pressure independent of atmospheric
pressure. The valve was used to connect or isolate the cells
between them and to supply the additional cell with
compressed air. To realise in situ measurement of FAS during
respirometry, the respirometric cell filled with the sample was
used as the reaction cell of the pycnometer. Thus this system
allowed to follow the variation in FAS of the sample during
the respirometric test due to biodegradation activity and
variation in physical structure of the matter.
The gas temperature was measured during all the FAS
measurements, so it was possible to correct the gas volume as
a function of the temperature. The volumes of cells and tubes
were precisely measured by filling these items with a known
volume of water.
Additional cell
Reaction cell(respirometric cell)
Sa ple
TT
Three-way control valve
P
Compressed air
Sample
Fig. 2 – Air pycnometer device: T, Pt100 probe; P, pressure
transducer.
The FAS measurement was divided into three parts. First,
after being placed at atmospheric pressure, the two cells were
connected between them and isolated from the atmosphere.
The equilibrium state was described by
Pr0ðVr � VsÞ ¼ nr0 R Tr0, (5)
Pa0 Va ¼ na0 R Ta0, (6)
where Pa0 and Pr0 are the pressures of the additional and
reaction cells in equilibrium condition in Pa; Va and Vr are the
volumes of additional and reaction cells (including the
volume of pipes) in m3; Vs is the volume of the solid sample
(not including the FAS) in m3; na0 and nr0 are the moles of gas
in the additional and reaction cells in mol; Ta0 and Tr0 are the
gas temperature in the additional and reaction cells in K.
Then, the reaction cell was isolated and the additional cell
was connected to the compressed air. The additional cell was
supplied with compressed air until the internal pressure
reached a value between 2500 and 2800 absolute pascal. This
range of pressures optimises the measurement accuracy
(Agnew et al., 2003; Oppenheimer et al., 1997). After the
pressure and temperature stabilisation (approximately
6 min), the state of the additional cell was described by the
following:
Pa1 Va ¼ na1 R Ta1, (7)
where Pa1 is the pressure of the additional cell in Pa; na1 is the
moles of gas in the additional cell in mol; and Ta1 is the gas
temperature in the additional cell in K.
Finally, the reaction cell was progressively connected to
the additional cell. After the stabilisation of pressure and
temperature (approximately 6 min), the equilibrium state was
characterised by
Pf ðVa þ Vr � VsÞ ¼ nf R Tf , (8)
where Pf is the pressure of the system in Pa; nf is the moles of
gas in the system in mol and Tf is the gas temperature in the
system in K.
The combination of these previous equations led to the
volume of solid sample Vs and then to the sample FAS S:
Vs ¼ Va
Pf �Pa1 Tf
Ta1
Pf �Pr0 Tf
Tr0
þ Vr, (9)
S ¼ 1�Vs
Vg
� �100, (10)
where S is the FAS in %; and Vg is the volume of the whole
sample (solid and void) in m3.
2.3.2. Pycnometer calibrationThe pycnometer calibration consisted of a comparison
between the theoretical and experimental FAS values for
two experiments.
The first test was on a respirometric cell loaded with 5.988
and 3.940 l of water (theoretical FAS of 0). The second test was
carried out on 0.999 l of spherical glass beads (diameter of
5 mm; theoretical FAS of 36.86%) placed in the reaction cell.
The first measurements with the pycnometer indicated a
deformation of the additional and reaction cells with an
increase in pressure. In this condition, the volume of these
cells (Vr and Va) had to be corrected as a function of the
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B I O S Y S T E M S E N G I N E E R I N G 9 7 ( 2 0 0 7 ) 7 5 – 8 880
pressure applied in the system. This correction was made
following specific experiments conducted to determine the
deformation coefficients. These experiments consisted of
measuring the weight variation of cells filling with water
until the pressure reached 3 absolute bar. The pressure
applied covered the range of pressures used during FAS
measurement. The volume variation was identical to the
mass variation since water was assumed to be an incom-
pressible fluid in the range of pressures studied. The volume
of the cells varied linearly with pressure. The coefficients of
deformation were evaluated during both the compression
and the decompression phases.
2.3.3. Influence of free air space measurement onrespirometric responseThe pycnometer device was developed to measure the
material FAS throughout the respirometric trials. As this
measurement required the pressurisation of gas filling
the voids between solid particles, a specific experiment was
carried out to evaluate the influence of pycnometer measure-
ment on respirometric response. Indeed, the pressurisation
could stress microorganisms, cause leaching and increase
oxygen solubility. The influence on leaching could be
observed immediately after FAS measurement and at the
end of the respirometric test by quantifying the leachates.
Two respirometric cells were filled with the same sample, a
mixture of sludge and pine bark chips. The moisture of this
sample was about 53% and the dry weight ratio between pine
bark chips and sludge was equal to 1.7 for a favourable
biodegradation.
The cells were studied in respirometry in the same
operating conditions (Tc ¼ 40 1C, Qe ¼ 60 l h�1, Qr ¼ 6 l min�1).
The FAS for the sample placed in a respirometric cell
was measured with the pycnometer whereas no measure-
ment was performed on the sample filling another respiro-
metric cell. The comparison of the respirometric curves
helped to reach a conclusion about the influence of the FAS
measurement.
2.4. Validation of the new respirometric device
2.4.1. Respirometric runsIn order to study sample biodegradation, the respirometric
measurements had to depend only on the intrinsic para-
meters of the microbial activity: biodegradable organic matter
quantity and species of microorganisms. The variation in
environmental conditions (temperature, moisture and aera-
tion) must not influence the biodegradation process during
measurement. Hence, three respirometric tests were carried
out on different organic materials to study the oxygen supply,
temperature and moisture control, and the repeatability of
respirometric responses.
The first test was conducted on a mixture of agrofood
sludge and pine bark chips (test A, mixture A). The second
test was carried out on mixtures of urban sludge with new
and reused pine bark chips collected before and after 21 days
of composting (test B, mixtures B0 and B21). The last test was
realised on household wastes (HW) (test C, mixture C).
For all tests, the water-bath temperature was equal to 40 1C,
the inlet airflow rate was 60 l h�1 and the recirculation airflow
rate was 6 l min�1 (value optimised in the RTD experiments).
The material was mixed when the oxygen uptake rate fell to a
low and stable value. The material mixing operations were
repeated until no significant restart of the oxygen uptake rate
was detected.
In test A, the sludge came from an agrofood industry and
the pine bark chips were dried at 80 1C and calibrated
(lengtho5 cm). The initial moisture of this sample was equal
to 49.7% with a dry mass ratio of 1.7 between the pine bark
chips and sludge. Four respirometric cells loaded with this
mixture were started at the same time. For these experi-
ments, three material mixings were necessary before they
had no significant influence on rO2 profile. These mixings
occurred after 691, 1050 and 1194 h of respirometry (test A). At
each mixing, one of these cells was stopped.
The second experiment (test B) was realised on mixtures of
urban sludge and bulking agent collected after 0 and 21 days
of composting (test B—mixtures B0 and B21). The composting
treatment was carried out in an airtight 300 l insulated
stainless steel cylindrical reactor (Tremier et al., 2005a). The
initial moisture of the samples (B0 and B21) was about 60%. As
for test A, the material was mixed when rO2 reached a low and
constant value until no significant restart of the oxygen
uptake rate was detected. Only one mixing was necessary for
B21 (after 260 h of test) and two mixings for B0 (after 260 and
580 h of experiment).
The test C was conducted on HW collected on an industrial
site after 4 days of fermentation in a bioreactor and after
mechanical separation to keep out the inert material. The HW
were sampled immediately after the last mechanical separa-
tion device, a flip-flow Liwell sieve with a square mesh of
10 mm. The initial moisture content of this sample was about
60%. A first mixing was carried out at 676 h and a second at
1000 h of respirometry with introduction of pine bark
chips—ratio between HW and pine bark chips of 0.88 in wet
mass—in order to modify the material structure.
2.4.2. Study of the respirometric response repeatabilityThe repeatability of the respirometric responses, studied
by comparison of the four cells of test A, was validated
(i) for respirometric curves visually identical and (ii) for
variation coefficients of maximum rO2 and amount of
oxygen uptake lower than 10%. As all cells were not stopped
at the same time, the study of repeatability concerned
four cells on the first part (0–691 h), three cells on the
second part (691–1050 h) and two cells on the third part
(1050–1194 h). The quantity of oxygen uptake corresponded
to the total oxygen uptake deducted by the endogenous
oxygen consumption. It was chosen to deduct the endogen-
ous oxygen in order to compare, in terms of organic
matter quantity, these results to others obtained for
different substrates. The endogenous respiration was
estimated as the mean value of rO2 during the last 48 h of
respirometry.
2.4.3. Study of temperature stability and homogeneityTemperature stability during tests A, B and C was evaluated
by measuring the variation coefficient of the Pt100 tempera-
ture probe data. The stability, in terms of time, was efficient
when this coefficient of variation was under 7% (arbitrary
ARTICLE IN PRESS
B I O SYS T EM S E NG I NE E R I N G 97 (2007) 75– 88 81
choice). The spatial homogeneity of matter temperature was
studied for test A by the association between the Pt100
temperature probe data and the measurements from some
thermobuttons (DS1922L, Maxim, France) placed in different
points of the sample (at a mean of three sample). The
thermobuttons were placed at several heights and radii. The
thermobuttons were similar to a clock pile and measured
temperature with a precision of 0.5 1C. Homogeneity was
validated for a difference between two points at maximum
equal to 3 1C (arbitrary choice).
2.4.4. Study of the moisture stability and homogeneityThe moisture homogeneity for tests A, B and C was visually
evaluated at each mixing and at the end of respirometry but
not quantified because of technical limits. The global
moisture stability was estimated by measurement and
comparison of material moisture (obtained after drying at
80 1C until the variation of dry mass was inferior to 0.5% in
24 h) at the beginning and at the end of respirometry for the
tests A, B and C. It was considered efficient if the variation in
moisture was inferior less than 4% (arbitrary choice).
2.4.5. Variation of free air space during compostingTo identify a possible limitation of biodegradation due to the
FAS, the sample FAS was measured at the beginning and at
the end of respirometry, and before and after each mixing
during tests A, B and C. It was measured with the pycnometer
described previously.
3. Results
3.1. Optimisation of the aeration conditions
The results of RTD experiments characterised the gas phase
hydrodynamic as the methane recovery rate was at minimum
93% and the repeatability effective (coefficient of variation
CVo4% for the reduced variance s2, the mean of residence
time m, and the rate of methane recovery) (Table 1).
The results obtained (Table 1) were in concordance with
the theory since the higher the recirculation airflow rate, the
higher was the reduced variance s2 (Roustan, 2003). The
reduced variance s2 increased sharply (from 0.24 to 0.85)
Table 1 – Results of gas-phase characterisation by tracing met
Recirculation airflow rate,l min�1 (duplicatemeasurements)
0 2
Time of passage t, s 713.08 765.3
Mean of residence time m, s 730.16 790.6
CV for m, % 2.2 1.6
(t–m)/t, % �2.4 �3.3
Mean of reduced variance s2 0.24 0.74
CV for s2, % 1.7 3.5
Mean of methane recovery rate, % 99.04 96.23
CV for CH4 recovery rate, % 0.97 0.99
CV, coefficient of variation.
between 0 and 4 l min�1 of recirculation airflow rate Qr. On
and after 4 l min�1, the reduced variance s2 increased more
slowly to reach 0.90 for the recirculation airflow rate of
7 l min�1. This last value did not reflect a perfectly mixed
phase because in this case the reduced variance s2 is
theoretically equal to 1 (Roustan, 2003). Nevertheless the
experimental RTD curves and the one for a perfectly mixed
flow were very close for the value of Qr of 6 and 7 l min�1. The
curves for these two recirculation airflow rates differed from
the theoretical profile only during the first 100 s of the
experiment (Fig. 3).
Moreover, the low difference between the passage and
residence times (o 5%) proved the absence of significant dead
zones and preferential ways (Roustan, 2003).
For the recirculation flow rates of 6 and 7 l min�1, the gas
phase was considered as perfectly mixed because (i) the
reduced variance was closed to the theoretical one of a
perfectly mixed flow, (ii) of the correspondence between
experimental and theoretical RTD profiles after 100 s and (iii)
of the absence of dead zones and preferential ways. Under
these conditions, the respirometric samples were supplied
with homogeneous and sufficient oxygen flow. A recirculation
airflow rate of 6 l min�1 was retained for the respirometric
experiments.
3.2. Pycnometer validation
3.2.1. Pycnometer accuracyThe results of tests 1 and 2 showed the accuracy and
repeatability of the pycnometric measurements (Table 2).
The repeatability was validated even if the coefficients of
variation obtained for the FAS of test 1 were greater than 10%.
For this test, the null porosity of water-induced high error that
revealed a limitation of the tool. The pycnometer accuracy
was confirmed by the low differences calculated between the
experimental and theoretical values measured for the solid
volume Vs and the FAS S. Among all tests, the highest
differences between theoretical and experimental Vs were
3.3% (test 2—Table 2) and 1.2% (test 1—Table 2). In the same
way, the experimental Sexp differed from the theoretical value
Sth at most by 5.4% (test 2—Table 2). Taking into account the
errors due to instruments, volume determination and cell
hod
4 6 7
1 765.31 765.31 765.31
8 781.10 796.42 785.90
0.5 0.2 1.4
�2.1 �4.1 �2.7
0.85 0.89 0.90
2.4 1.6 3.2
93.70 96.43 94.26
0.66 0.03 1.87
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0
0.0002
0.0004
0.0006
0.0008
0.001
0.0012
0.0014
0.0016
0.0018
0.002
0 500 1000 1500 2000 2500
Time, s
Ret
entio
n tim
e di
stri
butio
n
Fig. 3 – Theoretical retention time distribution (RTD) of perfectly mixed flow and experimental RTD curves obtained at
different values of recirculation airflow rate Qr: , Qr ¼ 0 l min�1; , Qr ¼ 2 l min�1; , Qr ¼ 6 l min�1; x, Qr ¼ 4 l min�1;
n,Qr ¼ 7 l min�1; , theoretical RTD.
Table 2 – Calibration of the pycnometer
Test Vs,th, l Vs,exp, l 1�Vs;expVs;th
;% Sth, % Sexp, % 1�SexpSth
; %
1 (water) 5.988 5.960 0.5 0 0.64 —
5.956 0.5 0 0.70 —
5.935 0.9 0 1.04 —
(CV ¼ 0.23%) (CV ¼ 27.2%)
3.940 3.943 �0.1 0 �0.08 —
3.892 1.2 0 1.21 —
3.939 0.1 0 0.02 —
(CV ¼ 0.73%) CV ¼ 187.2%)
2 (spherical
glass beads)
0.999 1.008 �0.9 36.86 36.37 1.3
1.032 �3.3 36.86 34.88 5.4
1.006 �0.7 36.86 36.53 0.9
0.986 1.3 36.86 37.82 �2.6
(CV ¼ 1.87%) (CV ¼ 3.3%)
Vs,th, theoretical volume of solid; Vs,exp, experimental volume of solid; Sth, theoretical free air space; Sexp, experimental free air space; CV,
coefficient of variation.
B I O S Y S T E M S E N G I N E E R I N G 9 7 ( 2 0 0 7 ) 7 5 – 8 882
deformation, the pycnometer could be considered as a
reliable tool to measure FAS.
3.2.2. Influence of free air space measurement onrespirometric responsesThe respirometric responses obtained from the experiments
carried out to observe the influence of FAS are illustrated on
Fig. 4. The comparison of these curves, visually and with
reproductibility criteria, did not demonstrate any significant
influence of the FAS measurement. The curves were similar
and the criteria of reproductibility were validated (CV on
maximum rO2 of 3.2%; CV on oxygen uptake of 4.2%). No
leachate was obtained after the FAS measurement or at the
end of respirometry that confirmed the absence of significant
influence of pycnometer measurement on respirometry.
3.3. Respirometer validation
3.3.1. Description and repeatability of respirometric curvesThe profiles of respirometric curves (test A on Fig. 5, test B on
Fig. 6 and test C on Fig. 7) were typical. After a short time lag,
the oxygen uptake rate increased quickly due to biodegrada-
tion of the most easily biodegradable substrate. Then,
when all of this matter has been degraded, a break in the
ARTICLE IN PRESS
0
50
100
150
200
250
300
0 20 40 60 80 100 120 140 160Time, h
r O2,
mm
ol [
O2]
kg−
1 [D
Mi]
h−1
Fig. 4 – Influence of the free air space measurement on respirometric responses rO2: , cell without free air space
measurement; �, cell with free air space measurement; DMSi, initial dry matter of sludge (rO2).
0
10
20
30
40
50
60
70
80
90
100
110
0 200 400 600 800 1000 1200 1400Time, h
r O2,
mm
ol [
O2]
kg−
1 [D
Mi]
h−1
0
5
10
15
20
25
30
35
40
45
50
Tem
pera
ture
, ˚C
t0
Mixing 1
Temperature profiles
Respirometric profiles
Mixing 2 Mixing 3
t1 t2 t3 tf
Fig. 5 – Respirometric responses rO2 of test A carried out on agrofood sludge and pine bark chips: DMi, initial dry matter
mixture; t0, start of the test; tf, end of the test; thick lines, respirometric profiles of cells 1–2–3–4; fine lines, temperature
profiles of cells 1–2–3–4 obtained with PT100 probes.
B I O SYS T EM S E NG I NE E R I N G 97 (2007) 75– 88 83
exponential growth was observed. The oxygen consumption
rate decreased regularly down to the complete disappearance
of all the biodegradable substrates. During this decrease in
oxygen uptake rate, the slowly biodegradable organic matter
was hydrolysed before being consumed by microorganisms.
These phenomena induce the consumption of all biodegrad-
able organic matter if no limitation of temperature, moisture
and aeration occurs. The operation of mixing realised during
tests A, B and C did or did not lead to a restart of oxygen
consumption. During test A, the more numerous the previous
mixing operations, the lower was the restart (Fig. 5). The
mixing of materials studied in test B had no influence (Fig. 6).
For test C, the first mixing had no influence on the oxygen
uptake rate profile whereas the second, after addition of pine
bark chips, led to a restart of oxygen uptake rate (Fig. 7). The
study of environmental conditions (temperature, moisture,
aeration, and FAS) was used to understand the presence or
absence of oxygen consumption restart after mixing.
The repeatability of respirometric responses was confirmed
with test A. The coefficients of variation obtained for
maximum rO2 and the amount of oxygen uptake were less
than 10% during the three phases studied (Table 3). Moreover,
the curves were identical (Fig. 5).
3.3.2. Stability and homogeneity of temperatureThe Pt100 probe temperature was close to the water-bath
temperature (40 1C) throughout the experiments, even if
during the peak of rO2 the temperature could be slightly
higher (Table 4, Figs. 5–7). Except during this short period, the
difference between the mean Pt100 value and water-bath
temperature value was at the maximum 2.2 1C. Moreover, the
temporal stability of temperature was confirmed by the low
ARTICLE IN PRESS
0
20
40
60
80
100
120
140
160
180
200
0 200 400 600 800 1000 1200 1400
Time, h
0
10
20
30
40
50
60
Tem
pera
ture
, ˚C
Mixing 1
Mixing 2 - Addition of bulking agent
r O2,
mm
ol [
O2]
kg−1
[DM
i] h
−1
Fig. 7 – Respirometric response of test C carried out on household wastes until the second mixing and on a mixture of
household wastes and pine bark chips from the 2nd mixing to the end: DMi, initial dry matter of household wastes; ,
respirometric profile; , temperature profile.
0102030405060708090
100110120130140150
0 100 200 300 400 500 600 700 800Time, h
0
5
10
15
20
25
30
35
40
45
50
Tem
pera
ture
, ˚C
Mixing 1 Mixing 2
r O2,
mm
ol [
O2]
kg−1
[DM
i] h
−1
Fig. 6 – Respirometric responses (rO2) of test B carried out on urban sludge and pine bark chips: DMi, initial dry matter of
mixture; , respirometric profile for B0; , temperature profile for B0; , respirometric profile for B21; ,
temperature profile for B21.
Table 3 – Repeatability of respirometric responses duringtest A (mixture of agrofood sludge and pine bark chips;initial moisture of 49 . 7%)
rO2,max , mmol[O2] kg�1[initial dry
matter] h�1
O2 uptake, mmol[O2] kg�1[initial dry
matter]
t0–t1 t1–t2 t2–t3 t0–t1 t1–t2 t2–t3
Mean 86 29 11 9751 2640 495
CV, % 0.7 3.1 8.9 1.9 5.0 9.1
rO2,max, maximum of oxygen uptake rate; O2 uptake, oxygen
consumed; CV, coefficient of variation; t0, start of the test; t1,t2,t3,
time of mixings.
B I O S Y S T E M S E N G I N E E R I N G 9 7 ( 2 0 0 7 ) 7 5 – 8 884
variation coefficient of P100 probe data for the majority of
trials (CVo7% for all tests except the cell filled with HW).
The spatial temperature homogeneity was effective during
test A as the difference of temperature between the two
points of measurement remained under 3 1C.
In these conditions, the respirometric device seems useful
to conduct experiments at a preset temperature.
3.3.3. Evolution of free air space during respirometric runsThe objective of studying the FAS of the sample during
respirometry was to verify whether this parameter became
limiting during the biodegradation processes. The FAS
considered optimum varies among authors. It must be in
excess of 30% and 35%, respectively, for Haug (1993) and
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Table 4 – Control of temperature and moisture for tests A, B and C
Experiments Time, h Tmean, 1C CVT, % DTmax, 1C Hi, % Hf, % HfHi� 1
Test A (agro food sludge and pine bark chips)
Cell 1 0–1316 41.02 3.3 1.3 49.7 58.2 +16.9
Cell 2 0–1194 41.07 3.7 2.01 49.7 55.2 +10.9
Cell 3 0–1050 41.36 3.8 2 49.7 45.4 �8.7
Cell 4 0–691 41.62 2.9 2.6 49.7 44 �11.6
Test B (urban sludge and pine bark chips)
B0 0–713 40.5 3.6 — 60.3 66.2 +8.9
B21 0–713 39.7 5.7 — 57.5 61.9 +7.1
Test C (Household wastes)
Until the second mixing 0–1000 42.2 9.7 — 60.2 73 +21.3
Test C (Household wastes and pine bark chips)
From the second mixing to the end 1000–1220 40.3 1.7 — 62.0 65.6 +5.8
Tmean, mean of Pt100 probe measurements; CVT, coefficient of variation on Pt100 probe data; DTmax, maximum variation of temperature in the
sample; Hi, initial moisture content; Hf, final moisture content.
Table 5 – Variation in free air space during tests A, B and C
Experiment Free air space, %
Initial Mixing 1 Mixing 2 Mixing 3 Final
Before After Before After Before After
Test A (agrofood sludge and pine bark chips)
Cell 1 67 66 66 64 67 64 66 61
Cell 2 68 62 67 65 69 64 ** **
Cell 3 67 66 70 * ** ** ** **
Cell 4 69 69 ** ** ** ** ** **
Mean 68 66 68 65 68 64 66 61
CV, % 1.6 4.2 3.5 1.9 2.1 1.0 — —
Test B (urban sludge and pine bark chips)
B0 54 48 55 46 49 *** *** 40
B21 64 53 59 *** *** *** *** 50
Test C (only household wastes until second mixing and then adding of pine bark chips)
41 24 23 10 58 *** *** 50
* Absence of measurement for experimental reason; ** No measurement (test ended); *** No material mixing.
B I O SYS T EM S E NG I NE E R I N G 97 (2007) 75– 88 85
Keener et al. (2002) whereas Epstein (1997) proposed a range
between 30% and 35% and Madejon et al. (2002) between 32%
and 36%. According to Mohee et al. (1998), the FAS must be
between 30% and 60%. They specified that to ensure a
favourable FAS in maturation, an initial FAS of 60% is
desirable.
The measurements performed during test A showed that
the FAS varied between 61% and 70% (Table 5). During this
test, the FAS remained in excess of 30%, so it was never
limiting to the biological processes according to the literature
data. The FAS determination at the beginning and at the end
of respirometry, and also at each mixing, did not reveal a clear
profile for this test. The variation in FAS remained within the
precision of the method.
The FAS measured on test B (Table 5) showed that this
parameter decreased between each mixing. After mixing
the matter, FAS was higher than before, which confirmed
the beneficial effect of this treatment to obtain the complete
biodegradation of samples. As for test A, the FAS measured
during test B was never limiting to the biodegradation (430%).
ARTICLE IN PRESS
Table 6 – Total oxygen consumed and oxygen uptakeafter the first mixing for tests A and B
Experiment O2 uptake,mmol
[O2] kg�1[initialdry matter]
O2 uptake afterthe first
mixing, %
Test A (agrofood sludge and pine bark chips)
Cell 3 12 643 21.1
Cell 2 12 635 20.1
Cell 1 12 975 19.1
Test B (urban sludge and pine bark chips)
B0 4767 o 1
B21 1849 o 1
B I O S Y S T E M S E N G I N E E R I N G 9 7 ( 2 0 0 7 ) 7 5 – 8 886
For test C, the FAS variation during respirometry differed
from the variation in tests A and B. The initial FAS of HW
(41%) was not limiting to biodegradation but was lower than
the one for the substrates of the previous tests, which
contained a bulking agent. Before the first mixing, the
FAS became limiting (24%) and remained at the same value
after mixing (23%). Therefore, the pycnometer makes it
possible to highlight the fact that material mixing had no
effect on the FAS and to adapt the experimental conditions to
the type of the wastes. For the second mixing, pine bark chips
were added to the HW in order to modify the material
structure and increase its FAS up to a more favourable value
(58%). Until the end of respirometry, the FAS of this new
mixture (HW and bulking agent) remained favourable to
biodegradation.
3.3.4. Stability and homogeneity of moistureMoisture control was difficult as its stability throughout the
trials was not effective (Table 4). Moreover, the development
of moisture variability throughout the substrate was observed
during respirometric tests.
The initial moisture for test A was equal to 49.7% and the
relative variations were from �11.6% to +16.9% between the
beginning and end of respirometry. The global moisture
content after 1194 and 1316 h of respirometry (respectively,
before the third mixing and at the end of the experiment)
was not limiting for biodegradation with values of 55.2%
and 58.2%. Nevertheless, at 691 and 1050 h (respectively,
before mixing 1 and 2), global moisture contents were very
low (44% and 45.4%) and moisture heterogeneities were
observed. Therefore, it could be assumed that local zones in
the material with a limiting moisture content for biodegrada-
tion (o45%) appeared. As the FAS was not limiting during
this test, the effect of mixing was mainly to rehumidify
zones with limiting conditions of moisture. Thus, the
biodegradation could restart, mainly after 691 and 1050 h of
respirometry.
The material moisture was more stable for test B with
variations of +8.9% and +7.1% after 713 h of respirometry. The
initial moisture was higher than the one of test A (about 60%
for mixtures B0 and B21 against 49.7% for mixture A) and the
moisture remained high with 61.9% and 66.2% at the end of
respirometry. Thus, instead of the development of moisture
heterogeneity, the material probably remained with favour-
able conditions of moisture throughout the substrate. Similar
results were obtained by Adani et al. (2001). During their
respirometric tests, the material mixings and the addition of
water implied an increase in biological activity. The authors
concluded that these operations helped to restore favourable
conditions for biodegradation.
The variation in moisture during test C was equal to +21.3%
until the second mixing at 1000 h (no moisture measurement
for the first mixing at 676 h) and equal to +5.8% during the
study of the HW and bulking agent mixture from 1000 h to the
end of respirometry. At the second mixing, the high moisture
(73%) could induce a limitation of biodegradation by reducing
the matter aeration potential. The addition of bulking agent
at this moment decreased the moisture content to 62% and
increased the FAS up to 58%, restoring favourable environ-
ment for biodegradation.
4. Discussion
The presence and absence of an rO2 peak after material
mixing could be explained by differences in waste biodegrad-
ability and/or by the establishment of limiting environmental
conditions (temperature, moisture and aeration). The study of
matter temperature proved that it could not explain the rO2
profiles after mixing because it was stable and homogeneous
throughout all tests.
During test A, the matter mixings induced peaks of rO2.
These peaks decreased with the number of mixings. There-
fore, the modifications realised on the respirometer do not
suppress the restart of oxygen uptake after matter mixing.
The oxygen consumed after the first mixing represented 20%
of the total oxygen consumed (including the endogenous
respiration) against 23–37% for the original system (Table 6).
The restarts were probably not due to an aeration problem as
the RTD experiments proved that the gas phase was perfectly
mixed. The RTD experiments were conducted on separate
trials but the conclusion remained valid in this case because
samples were similar mixtures of sludge and pine bark chips
and because their values for FAS were similar. Moreover, the
FAS of mixture A was favourable to biodegradation through-
out respirometric experiments (values between 61% and 70%).
In contrast, the variations in global moisture content ranged
between �11.6% to +16.9% and the substrate moisture was
sometimes quite limiting to biodegradation (44% and 45.4%,
respectively, before the first and second mixings). These low
moisture contents associated with the development of
moisture heterogeneity probably led to local zones with
limiting conditions of moisture. Therefore, the two first
mixings should rehumidify these zones that stimulated the
restart of biodegradation processes. After the third and last
mixings during test A (1194 h), no peak was observed under
favourable conditions of moisture, temperature and aeration.
Thus it was assumed that all biodegradable organic matter
was consumed.
The material mixings realised during test B did not cause a
restart of oxygen uptake whereas the development of
moisture variability throughout the substrate was observed.
The FAS was not limiting, between 40% and 64%, and the
ARTICLE IN PRESS
B I O SYS T EM S E NG I NE E R I N G 97 (2007) 75– 88 87
global moisture content remained favourable (57–66%). There-
fore, there are 2 possible reasons to explain this absence of
peak after mixing. The first one was that the variability in
moisture was not sufficient to create local zones with limiting
moisture. Thus, the high initial moisture of samples B0 and
B21, in comparison to the one of mixture A (60% versus 49.7%),
helped to retain favourable moisture content to biodegrada-
tion anywhere in the sample. The second reason to explain
the absence of peak, for test B, was the difference of
biodegradability between samples of tests A and B. The test
A took 1300 h against 761 h for test B because of the lower
biodegradability of samples B0 and B21 (4767 and 1849 mmol
[O2 consumed] kg�1[initial dry matter] for B0 and B21 against
at mean 12 751 mmol [O2 consumed] kg�1[initial dry matter]
for mixture A—Table 6). Indeed, the time of respirometry for
test A helped to increase the development of moisture
heterogeneity. So the effect of mixing seemed more impor-
tant for samples with high quantity of biodegradable organic
matter because they need a longer time of respirometry,
which helped the development of moisture heterogeneity and
limitation. In spite of the respirometer modifications, the
material moisture remained heterogeneous that implied the
necessity of material mixings. The influence of this operation
on the respirometric profile depends on the nature of the
tested sample.
During test C, the first mixing on the HW did not imply an
oxygen uptake restart whereas a peak was observed after the
second mixing with addition of pine bark chips. Indeed, the
absence of peak after the first mixing was due to a limitation
of matter aeration caused by a low value of FAS (24–23%) and a
high moisture content (4 60%). This was confirmed by the
restart after the addition of bulking agent, which increased
the FAS (58%) and reduced the moisture content (62%). This
restart proved the presence of residual biodegradable organic
matter and confirmed the interest to follow moisture content
and FAS during respirometry to quantify the substrate
biodegradability.
5. Conclusion
The pycnometer developed to measure the free air space (FAS)
during respirometry appeared to be a reliable tool. The FAS
obtained for water and spherical glass beads were close to
theoretical values instead of the variation in cell volume due
to the compression. It allowed in situ measurements without
perturbing biodegradation.
The respirometric apparatus was validated in terms of
temperature and aeration. The temperature was stable and
homogeneous during all trials. The measurement of the FAS
at the beginning and end of respirometry and at each mixing
allowed to demonstrated a possible limitation of biodegrada-
tion due to this parameter.
The control of moisture could not be validated as in most
tests the stability and homogeneity of this parameter was not
effective. The development, in course of respirometry, of
zones with limiting moisture content could lead to a restart of
oxygen consumption after material turning. In similar con-
ditions of FAS, the effects of mixing seemed to be more
important for matrix with a large quantity of slowly
biodegradable organic matter and with a low initial moisture.
In the case of high moisture content, a low FAS could imply an
absence of biodegradation whereas all biodegradable organic
matter was not consumed. Indeed, a material with a low FAS
was difficult to aerate, and bulking agents were necessary.
In the objective to quantify the whole biodegradable organic
matter of wastes, the application of mixings until they had no
effect on oxygen uptake rate seemed necessary, mainly to
rehumidify local zones with low or limiting moisture con-
tents, which potentially appeared in material during respiro-
metry. Moreover, the added control of the FAS at each mixing
was essential and demonstrated that the absence of oxygen
uptake restart was effectively due to the absence of biode-
gradable organic matter and not due to aeration problems.
The new device, associating respirometric measurements in
controlled environment and in situ measurements of the FAS,
was perfectly adapted to the study of the biodegradability of
organic waste of various origins and of different degrees of
evolution.
Acknowledgements
This study was conducted within the frame of a PhD project
funded by the ADEME (French Agency for Environment and
Energy Management) and the Cemagref laboratories (Agricul-
tural and Environmental Engineering Research Institute).
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