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Emission of H2S and mass balance of

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Emission of H2S and mass balance of sulfur in anaerobic

Water Science and Technology Vol 48 No 2 pp 227234 IWA Publishing 2003

ponds
J. Paing*, B. Picot* and J.P. Sambuco**
* Dpartement Sciences de lEnvironnement et Sant Publique, Universit Montpellier I, BP 14491, 34093
Montpellier cedex 5, France
(E-mail: jpaing@yahoo.fr; Bernadette.Picot@pharma.univ-montp1.fr)
** CEREMHER, Zone de Recherche du Lagunage, B.P. 118, 34140 Mze, France
(E-mail: jpsambuco@yahoo.fr)

Abstract Anaerobic ponds are highly efficient at removing BOD from wastewater with a reduced land area
requirement. However, their use is often limited because of the problem of odor release, primarily due to the
emission of hydrogen sulfide (H2S). The experiments were conducted on full scale anaerobic ponds used for
the primary treatment of urban wastewater under Mediterranean climatic conditions (south of France). A
model was developed to estimate the emission of H2S from water characteristics (temperature, pH and
sulfides concentration). The emission rate from anaerobic ponds varied between 20 and 576 mg-S/m2.d,
leading to concentrations of H2S in the surrounding atmosphere between 0.2 and 5.2 ppm. These
concentrations risked creating odor nuisances for nearby inhabitants. The whole of the results and the
analysis of sulfur species in sludge permitted the production of a complete mass balance for sulfur. Methods
of reducing the emission of odorous compounds were tested on a large scale. The recirculation of
secondary effluent and the use of impermeable or permeable covers appeared to be the most interesting
solutions.
Keywords Anaerobic pond; emission; hydrogen sulfide; odor control; odor nuisance

Introduction
Anaerobic ponds are a cost-effective and practical way to treat domestic, agricultural and
industrial wastewater. They are so efficient at removing BOD that their inclusion substan-
tially reduces the land area required by a waste stabilization pond system. However, the use
of anaerobic ponds with open surfaces is often limited due to the release of malodorous gas
creating nuisances to neighbors. Those odors are primarily due to the emission of hydrogen
sulfide H2S, which has a very low odor detection threshold, between 0.001 and 0.1 ppm
amongst different authors (Parsons et al., 2000). In anaerobic treatments, the presence of
sulfide is principally due to the dissimilatory reduction of sulfate by sulfate-reducing bacte-
ria such as Desulfuvibrio (Pescod, 1996).
According to Mara and Pearson (1998), odor problems in anaerobic ponds can be
avoided if the recommended design loadings are not exceeded (100 gBOD/m3.d at 10C
and 350 gBOD/m3.d at 20C) and if the sulfate concentration in the raw wastewater is less
than 300 mgSO4/l. However, the H2S emission rate from anaerobic ponds has never been
determined, only the concentration of sulfides in pond water was sometimes reported.
The first aim of this study was to measure the H2S emission rate and the resulting con-
centration of H2S in the atmosphere. With these measures, a predictive model to estimate
the emission of H2S from the characteristics of wastewater was defined. The second aim
was to use this model to discuss the recommendations for avoiding odor problems and the
solutions for reducing the odor emission. This work was performed on anaerobic ponds
used for the primary treatment of urban wastewater under a Mediterranean climate (south
of France). 227
 Materials and methods
The experimental site was the large-scale research waste stabilization pond of Mze on the
French Mediterranean coast (033506 E, 432510 N), shown in Figure 1. This system
had been enlarged in 1998 by the addition of two primary anaerobic ponds in parallel (mean
characteristics: volume 5,000 m3, depth 3.1 m, retention time 4.6 days, organic loading
83 gBOD/m3.d, population 13,800) and of 4 facultative ponds with step-feeding and
recirculation (Sambuco et al., 2002). Those ponds have been investigated for a two year
J. Paing et al.

period from their start up (05/98). The mass balance of sulfur has been carried out for one
complete year of operation (10/9810/99).
The characteristics of the influent and effluent were determined with twice monthly
composite 24 h samples for the influent and individual samples for the effluent. The follow-
ing parameters were measured according to Standard Methods (APHA,1995): suspended
solids (SS), chemical oxygen demand (COD), dissolved COD, sulfides by the iodometric
method (SII), sulfate by the turbidimetric method (650 nm). Bicarbonate and volatile fatty
acids (expressed as acetic acid) were determined by an alkalimetric method.
The accumulation of sludge was measured according to a protocol described in Picot et
al. (2003). Different forms of sulfur present in the peat were analyzed with methods com-
monly used in the analysis of sediments (described in Picot et al., 2001): FeS (ferrous
monosulfide), FeS2 (pyrite), SO42, org-S (organic sulfur) and total sulfur. These analyses
were performed on 9 sludge samples.
The production of biogas was measured with 4 gas collectors specially developed for
this study. They were made with a circular plexiglass cap with a bottom area of 0.3848 m2.
The daily biogas production rate (Ebiogas in l/m2.d) was measured weekly and the biogas
was sampled in a Tedlar bag and analyzed rapidly. H2S concentration ([H2S]biogas) was
measured by bubbling the biogas into a solution of 0.1M zinc acetate and then analyzing the
precipitated sulfides.
The concentration of H2S in the atmosphere surrounding the anaerobic ponds ([H2S]atm)
was measured using a method adapted from LeCloirec et al. (1988), with a detection limit of
0.02 ppm. Air was pumped for 5 hours at a flow rate of approximately 60 l/h and bubbled into
100 ml of 0.1 M zinc acetate solution. Eight bubbling chambers were positioned all around
the anaerobic ponds once a week, on the banks at 1 m from the water, in order to measure a
mean concentration of H2S. Nine bubbling chambers were also positioned according to
Figure 1, in order to determine the principal sources of odors in this treatment plant.

Pre-treatment

INLET
L1
RAW WASTEWATER

A1
 A2

R1 Effluent
L2  Recirculated effluent
 R2
R3 A = anaerobic pond
L3 R = facultative pond with
 R4 recirculation and step-feeding
L = facultative pond

F1
N F = maturation pond

F2
 Analysis of [H2S]atm
OUTLET

228 Figure 1 Schematic of the waste stabilization pond system of Mze (France)
Results and discussion
As soon as the anaerobic ponds were started up, a number of complaints about odors
occurred from residences surrounding the treatment works (the first houses were 200 m
East of the ponds). These odors were emitted principally by the two anaerobic ponds, as
shown by the analysis of the H2S concentration in Figure 2. An analysis by gas chro-
matography of the biogas produced by these ponds revealed that hydrogen sulfide was the
principal odorous compound, at a concentration of 2,400 mg/m3. Methylmercaptan was

J. Paing et al.
also detected but only at 4.8 mg/m3. Amines and organic acids were not detectable. Those
results showed that investigations of odor emissions could thus be limited to the study of
H2S emission from the anaerobic ponds, related to the production of sulfides.

Wastewater characteristics
The raw wastewater was principally from domestic sources, except for some winery waste-
water (Table 1). The change in the parameters between the influent and effluent showed the
anaerobic activity of the pond with a reduction of pH, an increase in the volatile fatty acids,
an increase in the bicarbonate, and an increase in sulfides resulting from the reduction of
sulfate by sulfate-reducing bacteria. It should be noted that the raw wastewater was already
anoxic, as shown by the presence of sulfides and volatile fatty acids. The sulfides concen-
tration (3.8 mgS/l) was considered as moderate by the classification of Hvitved-Jacobsen
and Nielsen (2000). Sulfides created problems in the network (concrete corrosion, odor
emissions), so that control measures had been installed in 2001 by the municipality (ferrous
salts addition).

Sulfide production
The presence of sulfides in anaerobic ponds is principally due to the dissimilatory reduction
of sulfate, but also to the anaerobic degradation of organic sulfur and to the presence of
sulfides in the raw wastewater. In the anaerobic ponds of Mze, the mean rate of the sulfate
reduction was 63%. The quantity of the removed sulfate (monthly mean expressed in

2,0
[H2S] atm (m g-S/m 3)

1,5

1,0

0,5

0,0
1 2 3 4 5 6 7 8 9
Figure 2 H2S concentration at different sampling points in the waste stabilization pond system

Table 1 Annual mean characteristics for the influent and effluent of the anaerobic pond. Mean, minimum,
maximum and standard deviation (n=22)

Parameters Raw wastewater Effluent

mean min. max. mean min. max.

Temperature (C) 18.6 12.2 25.3 4.1 17.3 8.1 25.8 5.7
pH 7.4 6.1 8.4 0.8 7.1 6.7 7.4 0.2
Suspended solids (mg/l) 256 151 404 73 114 60 217 39
Total COD (mgO2/l) 589 356 960 150 462 278 614 85
Dissolved COD (mgO2/l) 332 160 641 122 302 158 456 58
Bicarbonate (mgCaCO3/l) 321 121 477 77 380 214 487 61
Volatile fatty acids (mg ac.ac./l) 41 14 115 19 75 33 111 24
Sulfides (mgS/l) 3.8 0.0 8.8 2.3 19.2 3.2 36.4 8.3
Sulfate (mgSO4/l) 165 96 222 30 57 3 123 33
229
 kgS/d) was dependent on temperature with a linear relationship (RSO4 = 2.091T + 2.532, r2
= 0.7045, n = 12). However, the quantity of produced sulfides was not obviously dependent
on temperature. Their concentration seemed to be controlled by other mechanisms and
influenced by several parameters such as pH, organic loading and retention time. In this
study, the mean ratio between the sulfides concentration in anaerobic ponds and the sulfate
concentration in the raw wastewater (SII/S-SO4) was 0.35, in accordance with the ratio of
0.28 calculated by Toprak (1997) with a similar anaerobic pond. Almasi and Pescod (1996)
J. Paing et al.

found ratios of 0.4 (10C) and 0.6 (25C) at pilot scale.

Model for the H2S emission

The principal mechanisms governing the emission of volatile compounds in the
atmosphere are volatilization at the surface and gas stripping. In the case of anaerobic
ponds, the production of biogas, which is released by bubbling to the atmosphere, is a major
mechanism. Stating the hypothesis that the surface volatilization is less important than the
emission by bubbling with the biogas, the H2S emission rate can be calculated from the H2S
concentration in the biogas ([H2S]biogas) and the biogas emission rate (Ebiogas). A model
was developed to calculate those parameters from data measured in the pond water:
temperature, pH and sulfides concentration (Figure 3).
On the one hand, the measured values of [H2S]biogas were compared to theoretical values
of the H2S concentration ([H2S]biogas,eq), calculated at equilibrium from Henrys law and
the H2S concentration in the aqueous phase ([H2S]aq). A linear relationship was obtained,
indicating the biogas was over-saturated in H2S. On the other hand, the biogas emission
rate was found to be strongly dependent with temperature with a non-linear relationship
(Picot et al., 2001). All these theoretical and statistical equations allowed the calculation of
the H2S emission rate. Finally, the atmospheric concentration of H2S around the anaerobic
ponds ([H2S]atm) measured with bubbling chambers was compared to the H2S emission
rate. A linear relationship was obtained indicating that the H2S emission rate explained
73.3% of the variation in [H2S]atm. Indeed, this parameter could also be influenced by other
factors like wind speed and meteorological conditions. In summary, this model showed that
the H2S emission rate was principally dependent on temperature which influenced the bio-
gas production and the transfer of H2S in the gaseous phase. The pH and the sulfide concen-
tration were also important factors.

+
[H ] [S -II]
[H 2 S]aq = +
T, pH, S-II K + [H ] T
K = constant, f(T)
WATER Ebiogas = 4.8451 e
0.1203T

[H2 S]aq [H 2S]biogas,eq = H [H2S]aq

H = Henrys law constant, f(T) r2 = 0.9200, n=16

[H2 S]biogas ,eq [H 2S]biogas = 1.89 [H 2S]biogas,eq

r2 = 0.9284, n=20
BIOGAS
[H2 S]biogas  Ebiogaz

H 2S emission rate [H 2S]atm* = 0.012 EH2S

r2 = 0.7375, n=23

ATMOSPHERE [H2 S]atm * measured at 1 m from the water

Odor nuisances
Figure 3 Predictive model for the emission of H2S (SII and [H2S]aq in mgS/l; [H2S]biogas and [H2S]atm in
230 mgS/m3; Ebiogas in l/m2.d; H2S emission rate in mgS/m2.d)
Seasonal variations
Figure 4a shows the annual variations for the sulfides concentration measured in pond
water and for the calculated emission rate of biogas. Figure 4b shows that the concentration
[H2S]atm calculated with the model exhibited high values in summer, between June and
September, when water temperatures were greater than 20C. In winter, even if the concen-
tration of sulfides was high, the H2S emission rate was limited because the production of
biogas was low.

J. Paing et al.
Table 2 shows the mean annual values of the measured and calculated parameters. The
mean concentration of H2S in the biogas was 3,390 mg-S/m3 and the mean emission rate of
H2S was 172 mgS/m2.d. The concentration of H2S around the anaerobic ponds varied
between 0.2 and 6.9 mgS/m3, equivalent to 0.2 and 5.2 ppm. [H2S]atm was then always
greater than the odor detection threshold equal to 0.005 ppm according to Parsons et al.
(2000). The limit of 5 ppm (6.6 mgS/m3) considered unsafe for working with 8 hours expo-
sure, seemed to have been reached occasionally.

Mass balance of sulfur

For a complete mass balance of sulfur, the different forms of sulfur were analyzed in the
sludge. The concentration of total sulfur was 9,890 gS/g dry weight. Organic sulfur was
predominant, accounting for 70%, due to the large amount of organic matter. The forms of
reduced inorganic sulfur FeS and FeS2 accounted respectively for 16 and 13%. The amount
of sulfate was not significant. The presence of FeS could result from the precipitation of
Fe2+ with sulfides.
All of the results together allowed the complete mass balance of sulfur shown in Figure 5
to be carried out. The concentration of organic sulfur in the wastewater was estimated to be
5 mgS/l (Parker, 1979). The annual emission of H2S was calculated to be 0.28 kgS/d for a
surface emission of 1,615 m2. The accumulation in sludge was estimated to be 0.26 kgS/d,
with a rate of sludge accumulation equal to 0.017 m3/capita.year or 26 kgDS/d (Picot et al.,
2002). The loss of H2S in the atmosphere and the accumulation in sludge were thus very
low compared to the flow arriving with the influent. It should be noted that this mass

(a) 40 sulfides 120 (b) 6

[H2S]atm
biogas emission rate (l/m2.d)

biogas emission rate

35
100 5
sulfides (mgS/l)

[H2S]atm (ppm)

30
80 4
25
20 60 3
15 2
40
10
20 1
5
0 0 0
10/98
11/98
01/99
02/99
03/99

04/99
05/99
06/99
07/99
08/99
09/99
10/98
11/98
01/99
02/99
03/99
04/99
05/99
06/99
07/99

08/99
09/99

Figure 4 Annual variations of: (a) the sulfides concentration and the biogas emission rate, (b) the H2S con-
centration in the atmosphere around the anaerobic ponds

Table 2 Mean annual characteristics of anaerobic pond AP1 (n = 22)

Temp. pH SII [H2S]aq [H2S]biogas Biogas H2S emission [H2S]atm.

(C) (mgS/l) (mgS/l) (mgS/m3) emission rate (mgS/m3)
rate (l/m2.d) (mgS/m2.d)

mean 17.3 7.1 19.2 9.5 3,390 49 172 2.0

min. 8.1 6.7 3.2 1.2 510 13 20 0.2
max. 25.8 7.4 36.4 22.4 8,640 108 576 6.9
5.7 0.2 8.3 5.1 1,960 32 172 2.0
231
 H2 S: 0.3
total sulfur: 67 AT MOSPHERE total sulfur: 47
sulfate: 57 sulfate: 21
sulfides: 20
sulfides: 4
org-S: 6
org-S: 6
Stripping WATER
INFLUENT Sulfato-
2-
reduction EFFLUENT
SO4 S-II H2 S BIOGAS
J. Paing et al.

Precip itation
FeS
SLUDGE

total sulfur: 0.3

org-S, FeS, FeS2

Figure 5 Annual mass balance of sulfur in the anaerobic pond (flow expressed in kgS/d)

balance was not equilibrated with 67 kgS/d entering the anaerobic pond and 47.6 kgS/d
outgoing. This could be explained by the under-estimation of the H2S emission rate or by
errors in the estimation of sulfur species in wastewater.

Solutions to reduce odor emission

In the case of the waste stabilization pond system of Mze, the H2S emission from
anaerobic ponds involved a risk of odor nuisances all the year for neighboring inhabitants.
Indeed, [H2S]atm measured around the anaerobic ponds could be interpreted like a
maximum concentration that risked being smelt by close inhabitants because the effects of
dilution and dispersion could be insignificant with particular meteorological conditions.
The limit for nuisances could be fixed at 0.05 ppm of H2S (10 odor units/m3 according to
Parsons et al., 2000) and was then always exceeded. The odor nuisances appeared, despite
the recommendations of Mara and Pearson (1998) which were followed with an organic
loading less than 100 gBOD/m3.d and a mean sulfate concentration in the raw wastewater
less than 300 mgSO4/l. These limit values were then not sufficient in the case of very close
residences (200 m in this study).
In that case, measures to reduce the odor emissions should be undertaken. Possible
solutions are listed in Table 3. Addition of FeCl3 should not be attempted because of the
toxicity risk for algal biomass in secondary ponds. Liming, surface aeration and recircula-
tion were tested at full scale on the anaerobic pond A1, A2 served as reference. Liming was
efficient with a reduction of H2S emission rate of 66% for a pH increase from 7.0 to 7.7
(addition of lime: 200 kg/d for 5,000 m3). The efficiency should be greater with a higher pH
(92% for pH 8.5), but it could be toxic for anaerobic bacteria and other odorous compounds
like ammonia or amines could appear. The surface aeration was not efficient because of the
impossibility of obtaining a stratification of the pond water and the aeration power installed
(4 0.35kW) was not sufficient to aerate the whole pond. The recirculation of the effluent
from the facultative pond L2 with ratios R/Q = 1 and R/Q = 2 reduced H2S emission rate by
80%. The efficiency was due to the dilution effect and to the production of oxidizing condi-
tions from photosynthetic activity. Indeed, chlorophyll a and bacteriochlorophyll a were
detected, the latter represented photosynthetic sulfur bacteria like Chromatium and
Thiocapsa (Almasi and Pescod, 1996). However, the effect on removal performances in the
long term was not determined.
The installation of an impermeable cover like a geomembrane is very efficient for odors
and allows the reuse of the biogas to produce energy. However, this radical solution is
relatively expensive and needs additional maintenance. Finally, the use of a synthetic or
232 biological permeable cover was recently developed and showed a good efficiency with
Table 3 Possible solutions to reduce the emission of odors from anaerobic ponds

Solution type Action mode References

Addition of FeCl3 Complex the sulfides in insoluble ferrous

sulfides (FeS or FeS2)
Liming Increase the pond pH to reduce the Parker, 1979
proportion of [H2S]aq
Surface aeration Increase the redox potential at the pond Zhang et al., 1997 (pilot scale)

Recirculation
Impermeable cover
Synthetic or biological
permeable cover
J. Paing et al.
surface for the oxidation of sulfides to Schulz and Barnes, 1990
sulfate (agri. waste)
Combined action of the injection of: Shelef et al., 1977
water with high pH
algal biomass able to bring up the redox
potential by photosynthesis
additional flow for the renewal of water
and dilution of the sulfides
Isolate the emission of odorous gas DeGarie et al., 2000
Collect and treat the produced gas Shelef and Azov, 2000
Isolate the emission of odorous gas Zahn and Dispirito, 1999
Fix and oxidize this gas in a porous Hudson et al., 2001(pilot scale)
structure Picot et al., 2001 (pilot scale)

lower costs. The use of a biological cover consisting of a floating peat bed with plants was
tested at laboratory scale and showed an excellent efficiency with a 96% reduction of H2S
emission rate (Picot et al., 2001).

Conclusion
This work permitted the development of a predictive model for the estimation of H2S
emission from anaerobic ponds from water characteristics (temperature, pH and sulfides
concentration). In the case of this study, the H2S emission rate varied between 20 and 576
mgS/m2.d, leading to a concentration between 0.2 and 5.2 ppm of H2S in the surrounding
atmosphere. These concentrations risked creating odor nuisances for nearby houses. The
use of dispersion models with the H2S emission rate could indicate the minimum distance
between anaerobic ponds and habitations to avoid odor problems. Solutions to reduce the
emission of odorous compounds could also be envisaged. The impermeable cover for gas
collection and treatment is the more radical solution but its installation and maintenance is
relatively expensive. This solution allows the reuse of the biogas to produce energy. The
recirculation of a secondary effluent rich in oxygen and algae is efficient and less expensive
but the long term effect on removal performances should be further determined. The use of
synthetic or biological permeable covers seemed also to offer interesting possibilities.

Acknowledgements
The authors would like to thank the Agence de lEau RMC, the Conseil Gnral de
lHrault and the Ecosite de Mze for their financial support during this research project.

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