Biofltration of Concentrated

Mixtures of Hydrogen Sulfide and

Methanol
V.S. Sologar, Zijin l u, and D. Grant Allen
Department of Chemical Engineering and Applied Chemistry, and Pulp & Paper Centre, University of Toronto, Toronto, Ontario,
M5S 3E5, Canada; allendgachem-eng,utoronto.ca (primary author)
To date, little research has addressed biofiltration of
volatile organic compound (VOC) and reduced sulfur com-
pound (RSC) mixtures at the relatively high concentrations
(0 to 450ppmJ of interest to the pulp and paper industry.
The objectives of this study were to assess the impact of
cotreatment on the biofiltration of air emissions containing
mixtures of RSCs and VOCs, and to develop models of the
processes. Expmments were conducted at various concen-
trations (1 6 s EBRO using hydrogen sulfide as a model RSC
(0-45OppmJ and methanol as a model VOC (0-400ppmJ.
Reaction-limited and biofilm models showed that hydrogen
sulfide degradation followed Monod kinetics, while
methanol removal was first order. The maximum hydrogen
sulfide removal rate obserued during the first three months
of operation was 144g H$/m3 bed/h. However, this de-
clined to 85-95g HS/ m3 bedh in subsequent months. The
methanol removal rate was 7040% of the applied load
(maximum 480 g methanoYm3 be&) for single component
and mixture treatment. The results indicate that methanol
and hydrogen sulfide removal in biofilten are independent
and that co-treatment is an attractive option.
INTROWCTION
Air emissions from the forest products industry
tend to be complex mixtures of compounds. The
impact of the interactions between compounds and
their effects on biofilter operation and performance
must be characterized in order to develop good mod-
els for design and scale-up.
Reduced sulfur compounds (RSCs) emitted from
Kraft pulping include hydrogen sulfide (HzS), methyl
mercaptan (MM), dimethyl sulfide (DMS), and
dimethyl disulfide (DMDS). In the Kraft process, RSCs
are emitted from smelt dissolving tanks, washer hood
and seal tank vents, lime kiln exhausts, lime slaker
vents, and black liquor oxidation systems 11, 21.
Methanol and terpenes, two of the most common
volatile organic compound (VOC) emissions from the
Kraft process, are released from multiple effect evapo-
rators, brown stock washers, and pulp storage tanks
[l, 31. Other gaseous organic pollutants include alco-
hols, phenols, ketones, and acids [41.
A review of the literature suggests that biofiltration of
hydrogen sulfide and methanol mixtures are feasible at
low concentrations and low loading rates (Table 1).
However, the feasibility of cotreatment at concentrations
relevant to pulp and paper industry emissions has not
been addressed. Furthermore, the interaction effects
between RSCs and VOCs, and the impact of mixture
treatment on biofilter operation and performance has
not been addressed under controlled conditions, and no
attempts have been made to model mixture biofiltration
of RSCs and VOCs. Cox and Deshusses [91addressed
biofiltration of the highest concentrations of hydrogen
sulfide and toluene mixtures, but the narrow range of
loading rates studied precludes modeling of interaction
effects. Thus, biofiltration of RSC and VOC mixtures at
the high concentrations (0-500 ppmv) found in many
pulp and paper industry emissions has not been investi-
gated prior to this study.
Theobjectives of this study were to model the biofil-
tration of air emissions containing hydrogen sulfide, a
representative RSC, and methanol, a representative
VOC, in order to identlfy interaction effects between the
two classes of compounds, and to assess the feasibility
of co-treatment. Two biofilter models, one based on the
reaction-limited model presented by Hirai, et ul. [lo1 and
the other on the biofilm model for biofiltration of VOC
mixtures presented by Mohseni and Allen [ill, were
modified for application to the biofiltration of hydrogen
sulfide and methanol mixtures.
MATERIALS AND METHODS
Operating conditions for the single component
and mixture biofiltration studies were selected based
on the nature of pulp and paper air emissions, and
typical biofilter operating characteristics. The target
concentration ranges for hydrogen sulfide and
July 2003 129
Environmental Progress (V01.22, No.2)
Table 1. Reduced sulfur compound/volatile organic compound mixture biofiltration studies.
I source I Compounds
1 Studied
I VOCs, HzS Webster et al.
1999 [6]
Other VOCs
[ 71
Allen and Ellis I M S
2000 [8]
Cox and
Deshusses Toluene
2000 [9]
Concentration
Range (ppmv)
1 - 10 ppm HzS
26 ppm VOCs
0.i'- lppm vocs
1.5 - 3.8 ppm H2S
on avg.
8 - 12 ppm H2S
8 - 12 ppm MT
8 - 12 ppm DMS
8 - 12 ppm DMDS
MeOH
0 - 170 ppm H2S
0 - 600 ppm Tol.
30 - 80 ppm
Loading Ranges Studied and Removal Rate
Obtained
V- IOW VOC and H2S loadings
.O g H ~ S /m3 bed/h was created.
>99% H2S removal
Loading: 0.64 g H2S / m3 bed / h,
0.67 g MeOH / m3 bed / h.
91.7% H2S removal, 98.3% combined removal
Two stage biofiltration for H2S pre-treatment.
>91% removal of H2S in Stage 1 of Acid Gas
Biofilter (AGB)
Loadings:
2 - 12 gH2S / m3 bed/ h
9.1 - 9.3 g MeOH / m3 bed/ h
100 YO H2S, MT removal
90 - 95% MeOH removal
Loadings:
0-24.1 gH2S/m3bed/h
0 - 225 g Tol. / m3 bed / h.
Removal Rates:
100% for H2S <7gl m3 bed/ h
70 - 80% H2S removal at 24p/m3 be&.
Figure 1.
A T
Schematic of the experimental apparatus.
methanol were identified as 0-450 ppm, and 0-400
ppm,, respectively. In addition, biofiltration experi-
ments were conducted at neutral pH, to reflect the
general pH optima for VOC degrading microorgan-
isms, and at 30" C, which is in the optimum temper-
ature range for mesophilic microorganisms. Nova
InertB, a porous inflated glass packing material ( 5
to 7 mm particle diameter), was selected to prevent
complications arising from bed compaction and
aging over the experimental period, and to allow
continuous control of nutrient availability. Nutrients
were delivered via a recirculating nutrient solution
that also controlled pH, and provided continuous
removal of sulfate ions from hydrogen sulfide degra-
dation. A schematic of the experimental apparatus is
shown in Figure 1.
Three identical biofilters, operating in parallel at
30" C and neutral pH, were employed over one year to
study the biofiltration of hydrogen sulfide and
methanol, as single components and in mixtures. The
glass biofilter columns were 9.0 cm in diameter and 45
cm in height. Preliminary experiments were conducted
with single-stage biofilters filled with 40 cm of continu-
ous packing. Themajority of the experiments were con-
ducted using staged biofilters in which each reactor
contained three packed sections, each 11 cmin height.
Concentration measurements were performed
using a gas chromatograph (Varian Star 3400 CX, Mis-
sissauga, ON, Canada) equipped with a pulsed flame
photometric detector for hydrogen sulfide detection,
and a flame ionization detector for methanol detec-
tion. A 16-port auto-sampler with a 50 pL sample loop
was used for the majority of the experiments. Manual
130 J uly 2003
Environmental Progress (V01.22, No.2)
sampling was used in the last three months of experi-
mental work due to a malfunction in the auto-sam-
pler. Inlet concentrations were measured at the begin-
ning and at the end of the sampling to ensure that the
rotameter flow had not changed over the sampling
period.
MODEL DEVELOPMENT
Two modeling approaches were evaluated. The
first was a reaction-controlled, lumped parameter
approach for a well-mixed biofilm, as per Hirai, et al.
[lo]. The second was the VOC mixture biofiltration
model presented by Mohseni, et al. [I l l , which
accounts for reaction rate and mass transfer processes
in biofilters, and was extended to treat hydrogen sul-
fide and methanol. In both cases, the contribution of
the liquid trickling solution to the mass transfer and
reaction rates was assumed to be negligible.
Reaction-Limited Model
Wani, et al. [121extended a lumped parameter model,
first proposed by Hirai, et al. [lo], to RSC mixtures. In
this study, the model is applied to RSC and VOC co-
treatment as a simple method of assessing interaction
effects between the compounds in biofilter operations.
The model is based on a substrate mass balance across
the reactor, Monod reaction kinetics, and a well-mixed
biofilm. For the methanol and hydrogen sulfide system,
the elimination capacity (EC) for the reaction-limited
model can be expressed as follows:
where k is the first order rate constant (s-l), A is the
biofilter cross-sectional area (m2), H is the biofilter
height (m), and Q is the air flow rate through the biofil-
ter (m3/s>.
Biofllm Model
Mohseni and Allen I l l 1 developed a model for the
co-treatment of a-pinene and methanol based on the
Ottengraf and van den Oever [131biophysical model
for biofilms. The model is based on the following
assumptions: Monod kinetics, plug flow operation
with no axial dispersion, uniform biofilm growth over
the packing medium, and the presence of all growth
factors other than the substrates being tested in
excess. An adapted version of Mohseni and Allen's
model applicable to a methanol and hydrogen sulfide
system is given below.
The steady-state biofilm mass balances for the two
components are given by:
( 6)
d2sMeOH =p . 'MeOH p=. Me OH S MeOH
dx2 'MeOH Km, MeOH +'MeOH
De,MeOH
ECH2, =a 'max,H,S Ch, H2S
Km, H, S +'ln.H2S
'max, MeOH * ' 1, MeOH
Km, MeOH +Cln,MeOH
ECMeOH =P
(3)
where Vmax is the maximum substrate removal rate
(g/m3/h), Km is the Monod constant (g/m3), C is the
gas phase substrate concentration (g/m3), and a and
p are empirically determined interaction parameters. If
interaction is significant, then the functional form of
these parameters could be complex and would
depend on the nature of any observed interactions.
The model can also be solved for first order kinet-
ics, which apply to the methanol removal kinetics in
the range of study. For first order kinetics, the elimina-
tion capacity at a constant empty-bed retention time
can be described in terms of the mass loading rates:
EC =LO&( 1 - e-uH' Q)
where Deis the effective diffusion coefficient (m2/h),
S is the substrate concentration in the biofilm (g/m3),
x is the dimension across the biofilm (m), X is the
biofilm density (kg/m3), Y is the biofilm yield coeffi-
cient Wg), pmax is the maximum specific rowth rate
(h-l), and Km is the Monod constant (g/m 8 1.
The boundary conditions are:
(7)
' H2S
mH2S mMeOH
SHZs =-and S,,, =-
.-,
dsH S
2 =0 at x =
dx
where m is the air-water partition coefficient and 6 is
the biofilm thickness (m).
The gas phase mass balances on methanol and
hydrogen sulfide in the biofilter are:
x=o
(9)
(10)
' s Oe, MeOH [ 7 1 dsMeOH
x=o
Environmental Progress (V01.22, No.2) July 2003 131
Table 2. Model parameters for the biofiltration of hydrogen sulfide and methanol.
(1) Shl v#f dan ct al. 1993; (2) Mohseni (1998); (3) WiUcc-Chang oomlation in Geanlroplis 1993; (4) Pary end &em 1997
where Ug is the gas velocity (m/h) and As is the
biofilm surface area (m2).
The boundary conditions are:
(11)
MeOH = MeOHj n
H,S =H,S,in at h=O
The system of four nested nonlinear differential
equations can be solved using Matlab@ (The Math-
Works Inc, Release 12); however, the Km, X, Y, and
pmax values for each component must first be deter-
mined, either with experimental data or by parameter
fitting. The X/Y* pmax terms can be lumped in the
parameter r because they appear as a multiplicative
group in the mass balance equations. The kinetic
parameters r and K, can be fitted to the experimental
data using a nonlinear least-squares approach.
For the case of first order kinetics, the biofilm
model can be solved analytically:
(12)
7 .-I
Model Parameters
In order to facilitate data analysis and modeling,
we had to estimate a number of physical properties
for the substrates and the biofiltration system. These
parameters may be estimated using the system prop-
erties, and physical property data and biofilm charac-
teristics from the literature. The parameters used in
the modeling exercises and their sources are summa-
rized in Table 2. The interaction parameters a and p
were set to 1, which assumes no interaction effects.
The form of the interaction parameters will depend
upon the nature of the interactions. That is, whether
the interactions are chemical, physical, or biological,
and whether they are concentration-dependent, will
determine the functional forms of a and p. In this
study, no significant interaction effects were observed.
Therefore, there was no need to address the form of
the interaction parameters.
RESULTS AND DISCUSSION
Hydrogen Sulfide Bioflltration
Preliminary experiments on single component
hydrogen sulfide biofiltration performed using single-
stage biofilters indicated that very high removal rates,
up to 144 g H2S/m3 bed/h, can be achieved initially.
This is comparable to the 136-147 g H2S/m3 bed/h
removal rate obtained by Wani, et al. [2, 41for hydro-
gen sulfide removal using hog fuel biofilters. Howev-
er, after 100 days of operation, the maximum removal
rates decreased to 85-95 g H2S/m3 bed/h. Through-
out the study, deposition of elemental sulfur in the
biofilter packing material was observed, and the rates
of deposition increased with biofiltration loading. The
reduction in bed porosity and changes in packing sur-
face properties caused by sulfur deposition, as well as
biofilm aging, are the most likely causes for the dete-
rioration in maximum removal rate over time.
The presence of methanol had no significant effect
on the hydrogen sulfide removal rate (See Figure 2).
The removal rate was plotted as a function of the log
mean concentration difference to facilitate compari-
son between the experimental data and predicted
removal rates using the reaction-limited model. The
model predictions are shown with 95% confidence
132 J uly 2003
Environmental Progress (V01.22, No.2)
_ _ ~-
-
Hydrogen Sulfide Biofiltration
Hydrogen Sulfide Biofiltration in the
Pre, ence of Methanol
m
1
_ _ _ _ _
Vmax (g H2S/m3 W h )
K, (PPmy>
BF1 BF2 BF1 BF2
66f 19 56* 10 1 2 f 16 17f 11
63 f 20 59 f 14 66+44 28f 19
I
__. - .___
. _ -~
Hydrogen Sulfide Biofiltration
Hydrogen Sulfide Biofiltration in the
Presence of Methanol
Log M#n C o n c ~ c n Di fl mnce, C I 0 0
Figure 2. Comparison of experimental results and
reaction-limited model predictions for single compo-
nent and mixture hydrogen sulfide biofiltration in BF2
at 30" C, pH 7, and an EBRT of 16 seconds.
r (kg H2S/m3 biofihdh)
BF1 BF2 BF1 BF2
64 47 1.2 2
57 50 125 10
K, (mg/m3 biofllm)
-__
bounds for the estimated parameters, Vmax and Km.
Analysis of the 95% confidence bounds for the reac-
tion-limited model indicates that the difference
between the two data sets is not significant. However,
gas short-circuiting and sulfur accumulation in the
packing were reduced during mixture treatment, indi-
cating increased reactor stability.
Figure 2 also shows that the reaction-limited model
with Monod kinetics described the biofiltration of
hydrogen sulfide in the presence and absence of
methanol well despite the fact that mass transfer and
biofilm properties are not taken into account. The fit-
ted values and associated uncertainties at a confi-
dence level of 95% for the kinetic parameters Vm and
K, are given in Table 3. The uncertainties in the esti-
mated parameters are large, and indicate significant
variability in the reactor performance throughout the
experiments.
+
*
o 20 40 60 ao l o o 120 140 180 180 200
Figure 3. Comparison of experimental results and
biofilm model predictions for single component
hydrogen sulfide biofiltration at 30" C, pH 7, and an
EBRT of 16 seconds.
The biofilm model, solved for Monod kinetics,
was also used to model hydrogen sulfide removal in
the presence and absence of methanol (Figure 3,
Table 41, and, overall, the results indicate that
methanol had no significant impact on the hydrogen
sulfide removal rate. The value of Km was increased
in the presence of methanol, indicating that per-
formance at low loading rates may have been some-
what reduced, particularly in BF1. In order to fit the
model to the experimental data, a very thin biofilm,
10 pm in depth, was required. This suggests that
hydrogen sulfide biofilms are very thin and very
active, or that the system is strongly diffusion limit-
ed. The biofiltration literature indicates that VOC
degrading biofilms are several hundred microns in
depth [3, 14, 151. However, no research on the
depth or properties of RSC, and, specifically H2S,
degrading biofilms has been presented.
Environmental Progress (V01.22, No.2)
_ ~_ - ~ ~ _ _
Table 5. First order rate constants for methanol removal
Overall, the hydrogen sulfide biofiltration experi-
ments indicate that co-treatment of RSCs and VOCs in
biofilters is attractive, and may even stabilize the
biofilter. In terms of modeling, there is no need to
include any interaction parameter (i.e., a =1.0)
Methanol Biofiltration
The maximum methanol removal rate was 380 g
methanoVm3 bed/h (80% removal). This removal rate
is much higher than the maximum removal rates
reported in the literature, which range from 50-250 g
methanoUm3 bed/h [ 3 , 14-171. Furthermore, the
methanol removal rate increased linearly with the
loading rate throughout the study, which suggests that
other nutrients (e.g., oxygen) were not rate limiting in
this study.
Methanol biofiltration, in the presence and absence
of hydrogen sulfide, was found to be more stable than
hydrogen sulfide biofiltration. That is, methanol removal
rates reached steady state in one to two days, as com-
pared to more than one week for hydrogen sulfide. The
methanol biofiltration results were also more repeatable
than those of hydrogen sufide. However, slime accumu-
lation in the reactors occurred on several occasions, sug-
gesting that there was some conversion of methanol to
extracellular polymeric substances (EPS).
Methanol removal rates were linearly dependent on
concentration (or the inlet loading rate, at constant
EBRT). Thus, first order kinetics were used to model
methanol biofiltration (See Figure 4).
Linear regression was used to determine the slopes
of the lines in Figure 4, and from these slopes, the first
order rate constants for both the reaction-limited and
biofilm models were determined. For first order kinet-
ics, the rate constants for the two models are directly
proportional to one another and differ only in the
degree of isolation of the kinetic parameter from the
biofilm and mass transfer properties. The first order
rate constants for the reaction-limited and biofilm
models are given in Table 5.
The rate constants for methanol removal for both
models have overlapping confidence bounds for BF2 in
the presence and absence of methanol. However, the
rate constant for methanol removal in the presence of
hydrogen sulfide in BF1 is significantly lower than for
single component methanol biofiltration. The hydrogen
sulfide removal rate during mixture treatment was also
lower than in BF2, which suggests that the reduced
removal rate may be due to operating problems in BF1
rather than the impact of methanol. Therefore, it
appears that the impact of hydrogen sulfide on the
134 J uly 2003
0 1W 200 3W 400 500
Load (0 MaOH I ma bod I h)
Figure 4. Methanol removal rate as a function of inlet
loading for BF1 and BF2 in the presence and absence
of hydrogen sulfide at 3OoC, pH 7, and an EBRT of 16
seconds.
methanol removal rate is negligible within the experi-
mental error and so there is no justification for including
an interaction parameter (i.e., p =1). The absence of a
decline in methanol removal over time during mixture
biofiltration suggests that the pH cycling and sulfur
accumulation in the packing material do not inhibit
methanol removal. Therefore, co-treatment of VOCs and
RSCs in biofilters appears to be feasible and attractive for
the pulp and paper industry.
CONCLUSIONS
Experiments with biofilters degrading hydrogen sul-
fide and methanol singly and in mixtures have shown
the following:
1. The interaction effects between hydrogen sulfide
and methanol in biofiltration are negligible. No sig-
nificant differences were observed between the
removal rates or efficiencies during single compo-
nent and mixture treatment.
2. Hydrogen sulfide removal is best described by
Monod kinetics.
3. The methanol removal can be describe with a first
order model.
4. Both reaction-limited and biofilm-based models
describe hydrogen sulfide biofiltration well, given
the simple first-order to zero-order transition
observed. However, a very thin (10 pm) biofilm
was required in order to fit the model to the data.
5. The reaction-limited and biofilm models for
methanol biofiltration fitted the experimental data
identically, and the rate constants for the two mod-
els were directly proportional to each other.
Environmental Progress (V01.22, No.2)
ACKNOWLEDGMENTS
The authors would like to thank the National Sci-
ences and Engineering Research Council of Canada,
and members of the Research Consortium on Mini-
mizing the Impact of Pulp and Paper Mill Discharges
2000-2003, including: Aracruz Celulose SA, Domtar,
Inc., EKA Chemicals, Inc., Georgia-Pacific Corpora-
tion, Irving Forest Services Ltd., J apan Carlit Co. Ltd.,
Potlatch Corporation, Sterling Pulp Chemicals Ltd.,
Tasman Pulp & Paper Co. Ltd., and Tembec, Inc., for
their financial support.
NOMENCLATURE
AS
A
C
Cln
De
EC
h
H
Km
k
Load
m
Q
r
S
ug
Vmax
X
X
Y
Biofilmsurface area per unit volume of the
biofilter m2.m-3
Cross-sectional area of the
biofilter m2
Substrate concentration in the air stream
ppmv or g.m-3
Log mean concentration difference
ppmv or g.m-3
Effective diffusivity of substrate in the biofilm
m2.h-l
Elimination capacity g.m-3 h-l
Distance from the biofilter
inlet m
Total height of the biofilter m
Half saturation constant in Monod kinetics
ppm 0rg.m-3
First order reaction rate constant s-
Inlet mass loading rate of substrate
g.m-3 h-l
Aidbiofilm partition coefficient -
Volumetric air flow rate m3/s
Macro-kinetic growth rate
constant Kg.m-3. h-l
Concentration of substrate in the biofilm
g . m-3
Velocity of air through the
biofilter m.h-l
Maximum substrate removal rate
(reaction limited model) g.rn3.h-l
Dimension across the biofilm m
Dry cell density of the microbial community
Biomass yield coefficient g / g
v1
Kg.m-3
DMS
DMDS
EBRT
MeOH
MM
RSC
DMDS
voc
H2S
Dimethyl sulfide
Dimethyl disulfide
Hydrogen sulfide
Methanol
Methyl mercaptan
Reduced sulfur compounds
Dimethyl disulfide
Volatile organic compound
Empty bed retention time S
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