Research Article

Adsorption Science & Technology

Low-temperature H2S 2017, Vol. 35(1–2) 120–136
! The Author(s) 2016
removal for solid oxide fuel Reprints and permissions:
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cell application with metal DOI: 10.1177/0263617416672664

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oxide adsorbents
Christof Weinlaender, Raphael Neubauer
and Christoph Hochenauer
Institute of Thermal Engineering, Graz University of Technology, Austria

Abstract
The desulfurization of biogas is essential for the successful operation of solid oxide fuel cells.
H2S is one of the main components in biogas. In order to feed a solid oxide fuel cell,
the contaminated gas has to be reduced to a certain degree. In this work, different parameters
onto the desulfurization performance of commercially available desulfurization adsorbents
were investigated. The experiments were carried out using a custom made lab-scale unit.
Synthetic biogas was passed through the sorbent bed and the outlet H2S concentration was
measured. Experimental runs in a fixed bed reactor were conducted to monitor H2S removal
efficiency of a zinc oxide adsorbent, an adsorbent based on a mixture of manganese and copper
oxide and a zeolite adsorbent. H2S removal efficiency was monitored under various operating
conditions such as different temperatures, space velocities and inlet concentrations. This work
provides useful data for adsorption tower design and process optimization.

Keywords
Desulfurization, hydrogen sulfide, zinc-oxide, copper-oxide, manganese-oxide

Submission date: 1 September 2016; Acceptance date: 13 September 2016

Introduction
This paper focuses on the low-temperature H2S removal for solid oxide fuel cell (SOFC)
application with metal oxide sorbents. SOFCs offer some important benefits and their high
efficiency contributes to a diminution of CO2 emission per unit electric power. SOFCs have
the advantage of higher fuel flexibility compared to other fuel cells types (Lo Faro et al.,
2012; Sasaki and Teraoka, 2003). The application of SOFCs instead of heat engines will lead
to 10–20% higher efficiency in electrical power generation (Van herle et al., 2004).

Corresponding author:
Christof Weinlaender, Institute of Thermal Engineering, Graz University of Technology, Inffeldgasse 25/B, A-8010 Graz,
Austria.
Email: christof.weinlaender@tugraz.at
Weinlaender et al. 121

Sulfur content in fuel varies from 10 ppmw in ultralow commercial gasoline to 3000 ppmw
in military fuels such as JP-5 and JP-8 and 10,000 ppmw for naval distillate (Alprekin et al.,
2008). Kurkela et al. (1996) expects sulphur in biogas to be predominately present as H2S. In
biogas, the content of hydrogen sulfur spans from 10–30 to 500–2000 ppm (Liu et al., 2015).
Furthermore, the H2S concentration in natural gas grids is typically limited to a few ppm
to avoid facility corrosion, unnecessary production of by-products, and possible public
exposure and complaints (Cosoli et al., 2008; Namgung et al., 2012). After reforming, the
sulphur concentration is typically in the range of several ppmv to several hundred ppmv.
Therefore, efficient sulfur removal is important for a fuel cell that uses biogas, liquefied
petroleum gas or gasoline to prevent downstream sulphur poisoning of catalysts in the fuel
processor and in the fuel cell anode. Even at minor quantities, the sulfur compounds can cause
severe poisoning of catalysts or in fuel cell anodes (Gong et al., 2007). In order to use biogas as
a fuel for a SOFC, several of its components have to be reduced to a certain degree. Among
those components are, apart from H2S, particulate matter, tar, hydrogen chloride, alkali metal
species and nitrogen containing compounds such as ammonia (Aravind, 2007; Aravind et al.,
2008). The influence of H2S on the performance of SOFCs has been analysed in depth.
Rasmussen and Hagen (2009) studied the influence of H2S on the catalytic activity of a
Ni/YSZ (yttrium-stabilized zirconia) electrode. After mixing the CH4 containing fuel with
H2S in the concentration from 2 to 24 ppmv, the cell voltage decreased significantly.
Matsuzaki and Yasuda (2000) reported that a H2S concentration as low as 0.05 ppmv
resulted in performance loss of a SOFC with a Ni/YSZ electrode. Veyo (1998) concluded
that the impurity of 1 ppmv H2S led to a 60 mV cell voltage drop.
There are numerous techniques available for H2S removal from gas streams which can
be classified as biological and physical–chemical processes. Biological treatments are cost
effective and environmentally friendly processes. H2S can be severed through the oxidation
of microorganisms of the species thiobacillus. This oxidation requires a certain amount of
oxygen which can be achieved by adding air. Furthermore, the oxidation can be carried out
either in a digester or in an external scrubbing column. The biological system is able to emit
large quantities of H2S from the biogas, however, the systems’ disadvantage is its poor
adaptability to fluctuating H2S contents (Allegue and Hinge, 2014).
Physicochemical processes can be classified as reactive (chemical oxidation), absorption
(caustic washing), and adsorption (metal oxides, activated carbon) techniques. The most
widely used technology now is the Claus process, which recovers elemental sulfur from
sulfur-containing gas. Because of thermodynamic limitations, efficient removal of H2S from
the gas is difficult and 3–5% of the H2S is left in the tail gas (Zhang et al., 2015). Another used
technology is chemical absorption. The water solubility of the H2S is enhanced by making the
water alkaline or by its oxidation to more water-soluble compounds. The crucial disadvantage
of the absorption is that usually eliminates a problem with a contaminated gas stream only to
create a contaminated liquid stream or a more concentrate gas liquid stream. Besides that,
there are high initial investment costs as well as high consumption of chemicals. Advantages
are high efficiency removal and ability to handle a wide range of pollutant concentrations.
Another process based on chemical absorption is the catalytic oxidation with chelated iron salt
solutions. Beside the advantage that removal efficiencies of 99.99% or higher can be reached,
H2S gets converted into elemental sulfur in this process. On the other hand, reports about
plugging and foaming problems refer to a complex process control (Allegue and Hinge, 2014).
Adsorption systems are typically suitable for low gas flow rates and low H2S
concentrations. Among the available adsorbents, metal oxides are contemplated
122 Adsorption Science & Technology 35(1–2)

to be a valuable choice for H2S elimination. The reaction taking place using metal oxides for
sulfur removal proceeds according to the following equation:
Mex Oy þ yH2 S ! Mex Sy þ yH2 O ð1Þ

Desulfurization of fuel gas can be achieved by using metal oxide sorbents that form stable
sulfides. Elseviers and Verelst (1999) analysed the purification performance of different metal
oxides between 350 K and 923 K, and ranked Cu, Zn, Co and Mo as being the most useful.
ZnO has been widely used to remove H2S at moderate low temperatures because of its
high equilibrium constant and high sulfur capacity in this temperature spectrum. Even if
zinc oxide seems favourable for desulfurization among metal oxide based sorbents, its
fundamental disadvantage is the limited feasibility of regeneration. For such cases, upon
breakthrough, the adsorbent bed is replaced with a fresh batch of ZnO and the sulfur
removal continues. CuO has an extremely high equilibrium sulfidation constant that
allows an extremely low equilibrium constant even at high temperatures (Patrick et al.,
1989). Due to the fact that little or no data on copper–manganese-oxide and the copper-
oxide doped zeolite are present, this paper provides useful data for process optimization and
adsorption tower design.
In this analysis, three commercially obtainable extrudates were evaluated for H2S removal
under various conditions. Those extrudates are ZnO, a mixture of MnO and CuO, and a
CuO doped zeolite. The sulfur uptake of the different sorbents was evaluated by varying the
reaction temperature and space velocity. In addition, two H2S inlet concentrations (200 and
1000 ppmv) were used to simulate different biogas feedstocks and cover the average and
maximum H2S load of biogas from conventional biogas plants. Breakthrough behaviour of
an adsorbent is also important for the adsorption process to be scaled up. As part of this
research, the studies on breakthrough behaviour of the adsorbents under various operating
conditions were carried out in hope that the research will lead to an optimized adsorption
process being established. The goal of this study is to determine the influence of H2S inlet
concentration, reaction temperature and space velocity of three different sorbents mentioned
before on sulfur uptake. The data gathered will be useful for adsorption tower design.

Experimental
Sorbents
The physical characteristics of the three different sorbents are listed in Table 1.

Table 1. Physical characteristics of zinc oxide sorbent, manganese and copper

oxide mixture sorbent, copper oxide doped zeolite.

Sorbent ZnO CuO–MnO Zeolite

3
Bulk density (kg/m ) 1090 650 500
Pellet size (mm) 4.5 1.6 1.6
ZnO content (mass%) 87–93 0 0
CuO content (mass%) 0 >25 <25
MnO content (mass%) 0 >25 0
Aluminosilicate content (mass%) 0 0 >75
Weinlaender et al. 123

Figure 1. Schematic diagram of the experimental apparatus (A: reactor; B: heating; C: valves; D: gas
analyser; E: thermocouples; MFC: mass flow controller).

Figure 2. Effect of reaction temperature on H2S outlet concentration of ZnO adsorbent. Space velocity
4000 h1; H2S inlet concentration 200 ppmv.
124 Adsorption Science & Technology 35(1–2)

Synthetic biogas
In order to simulate different biogases, test gases with different H2S content were used. The
gases were mixed and bottled by AirLiquide. H2S content of 200 and 1000 ppmv in nitrogen
was used to simulate two different synthetic biogas feedstocks. These H2S inlet
concentrations cover the average and maximum H2S load of biogas from conventional
biogas plants. As the influence of steam content was investigated by Kim et al. (2007),
only dry gas was used for the test runs. Novochinskii et al. (2004) reported that an
increase of steam concentration had a negative influence on the H2S capture capacity of
the ZnO sorbent. The accuracy of the certified mixtures was 3 ppmv H2S for the 200 ppmv
gas mixture and 30 ppmv H2S for the 1000 ppmv gas mixture.

Test rig
The custom-made lab-scale unit to perform desulfurization experiments included the
following parts: a mixed and certified test gas with 200 and 1000 ppmv H2S in nitrogen,

Figure 3. Effect of reaction temperature on H2S outlet concentration of CuO–MnO adsorbent. Space
velocity 4000 h1; H2S inlet concentration 200 ppmv.
Weinlaender et al. 125

a mass flow controller, a reactor with bypass valves, a programmable gas preheating unit
and a gas analyser. A flowsheet of the test rig is represented by Figure 1. The feed gas is
dosed with a mass flow controller (red-y series hi-performance, accuracy 0.3 % of full scale,
þ0.5% of reading). The reactor consists of two stainless steel pipes made of 1.4401 stainless
steel in the following dimensions: 26.9 mm outer diameter; 21.6 mm inner diameter; each
400 mm long and connected with a union connection. The upper part of the reactor is used as
a gas preheating zone. Two electric heating tapes coupled to proportional-integral derivative
(PID) controllers and type K thermocouples (mounted on the outer surface of the upper and
lower reactor part) ensure gas preheating. The lower reactor part contains the test cell
(material: 1.4401, 21.6 mm outer diameter; 18 mm inner diameter and 150 mm length)
which is suitable for taking up different sorbents. The H2S concentration in the reactor
exhaust stream was continuously monitored with an ABB AO 2000 gas analyser
(accuracy 0.05 ppmv). The built-in calibration cell of the gas analyser allows calibration to
be undertaken without the use of test gas bottles. SO2 was monitored to check undesired
reactions leading to SO2 formation. The control of the mass flow controller and the two

Figure 4. Effect of reaction temperature on H2S outlet concentration of zeolite adsorbent. Space velocity
4000 h1; H2S inlet concentration 200 ppmv.
126 Adsorption Science & Technology 35(1–2)

programmable heating tapes is achieved with the aid of LabVIEW software. Furthermore,
the LabVIEW program was used for recording relevant process data such as temperatures
and outlet H2S concentration.

Test procedure
Different types of experiments have been performed using the ZnO sorbent, the MnO–CuO
mixture sorbent and the CuO doped zeolite. At different temperatures and different Gas
Hourly Space Velocities (GHSV; the quotient of the entering volumetric flow rate of the
reactants divided by the catalyst bed volume), 200 and 1000 ppmv synthetic biogas was
passed through the sorbent bed and the outlet H2S concentration was measured for a
30 minutes steady state period. This investigation was carried out to find out the
maximum sulfur reduction achievable from the three sorbents under different conditions.
During typical test runs, sorbent pellets were loaded into the test cell and reactor, and
reactor temperature was varied. The space velocity was varied through the amount of

Figure 5. Effect of space velocity on H2S outlet concentration of ZnO adsorbent. Reaction temperature
293 K; H2S inlet concentration 200 ppmv.
Weinlaender et al. 127

sorbent pellets, or in other words, through the height of the reactor. While the reactor was
heated up to the desired temperature, the reactor was purged with nitrogen. After reaching
the operating temperature, the synthetic biogas was fed into the reactor and data logging
started. Before entering the gas analyser, the gas stream passed a sample gas cooler
consisting of a temperature controller, a heat exchanger and a peristaltic pump.
Due to the fact that except for the ZnO sorbent few or no data is available, experiments to
characterize the maximum sulfur capture capacity had to be carried out. Since sulphur
saturation can take an extremely long time, 1000 ppmv H2S in nitrogen was used to
characterize the sulfur capacity of the sorbents. For those experiments, 1 g of sorbent
sample has been flowed through at 293 K and a space velocity of 4000 h1 for 24 hours.
The sulfur capture capacity of the sorbent samples was calculated using the following
formula, which has been used by Novochinskii et al. (2004) and Kim et al. (2007).
In addition, the results were cross checked by analytical chemistry.
Rt  
FR  0 CH2 Sin  CH2 Sout dt  32  104
Scap ¼ ð2Þ
Vmol  msample

Figure 6. Effect of space velocity on H2S outlet concentration of CuO–MnO adsorbent. Reaction
temperature 293 K; H2S inlet concentration 200 ppmv.
128 Adsorption Science & Technology 35(1–2)

Nomenclature

Symbol Units Description

FR L/h gas flow rate

T h experiment time
Vmol L/mol gas molar volume
CH2 Sin ppmv H2S inlet concentration
CH2 Sout ppmv H2S outlet concentration
msample g sorbent sample weight
32 g/mol molar weight of sulfur

Figure 7. Effect of space velocity on H2S outlet concentration of zeolite adsorbent. Reaction temperature
293 K; H2S inlet concentration 200 ppmv.
Weinlaender et al. 129

Scap describes the sulfur capture capacity in (g of S)/(100 g of sorbent). The other symbols
shown in equation (2) are explained in the nomenclature.

Results and discussion

Effect of the reaction temperature
Experiments were conducted at different temperatures to determine the optimum
temperature providing the highest adsorption performance. Inlet H2S concentration as
low as 200 ppmv was selected to simulate a biogas feedstock with average sulfur content.
The technical data for the used pellets is given in Table 1. The results of adsorption
experiments showing the effect of temperature are shown in Figures 2 to 4. Figure 2
shows the effect of reaction temperature on H2S outlet concentration of ZnO adsorbent.
Figure 3 shows the effect of reaction temperature on H2S outlet concentration of CuO–MnO
adsorbent and Figure 4 shows the results for zeolite. The H2S outlet concentration for all

Figure 8. Effect of H2S inlet concentration on ZnO adsorbent on H2S outlet concentration. Reaction
temperature 293 K; space velocity 4000 h1.
130 Adsorption Science & Technology 35(1–2)

sorbents decreases when the temperature is increased. The sulfur removal efficiency of the
sorbent used is defined as the amount of H2S adsorbed at the sorbents surface related to the
H2S concentration at the outlet. An increase of the reaction temperature from 293 K to
473 K led to a decreased H2S concentration at the reactor outlet. In numbers, the
efficiency increased from 91.93% to 98.72% for ZnO, from 94.26% to 98.71% for the
CuO–MnO sorbent and from 98.28% to 99.42% for zeolite.
The sulfur removal efficiency for ZnO extrudates observed in this study is in line with the
literature (Kim et al., 2007). The fact that the sulfur removal efficiency is not as high as in the
cited literature might be to the result of the following reason: The reaction of ZnO with H2S
is favoured kinetically as the temperature increases. Kim et al. (2007) achieved a sulphur
removal efficiency of 99.99% at 636 K. Due to the fact that there was no data available, the
sorbent based on CuO and MnO in combination with zeolite could not be compared with
literature.

Figure 9. Effect of H2S inlet concentration on CuO–MnO adsorbent on H2S outlet concentration.
Reaction temperature 293 K; space velocity 4000 h1.
Weinlaender et al. 131

Effect of space velocity

Figure 5 shows the effect of the space velocity upon H2S breakthrough on ZnO extrudates.
All test runs were carried out with synthetic biogas with 200 ppmv H2S concentration and at
a reaction temperature of 293 K. Increasing space velocity from 4000 h1 to 8000 h1
elevated the H2S outlet concentration dramatically from 20 ppmv to 70 ppmv after the
monitored 30 minutes. Increasing the space velocity from 8000 h1 to 12,000 h1 had little
impact and only slightly increased the H2S outlet concentration from 70 ppmv to 80 ppmv
after the monitored time span of 30 minutes. These results propose that Scap of zinc oxide is
restricted by the contact between gas and sorbent in the fixed bed reactor at higher space
velocities.
Figure 6 exhibits the obtained test results for the CuO–MnO sorbent. It was found that
the impact of the space velocity is minor, compared to the experimental runs with ZnO
extrudates. Doubling the space velocity from 4000 h1 to 8000 h1 elevated the H2S outlet
concentration from 12.5 ppmv to 13 ppmv after 30 minutes. Increasing the space velocity up

Figure 10. Effect of H2S inlet concentration on zeolite adsorbent on H2S outlet concentration. Reaction
temperature 293 K; space velocity 4000 h1.
132 Adsorption Science & Technology 35(1–2)

to 12,000 h1 only slightly increased the outlet concentration by about 1 ppmv. Comparing
the curves in Figure 6, indicates that the gas solid contact has no limiting effect at the tested
space velocities.
The results for the zeolite tested under various space velocities can be found in Figure 7.
Comparing to the other sorbents, the zeolite achieved the best H2S outlet concentrations
under all monitored space velocities. Doubling the space velocity from 4000 h1 to 8000 h1
increased the outlet concentration from 3 to 6 ppmv. The sulfur removal efficiency of tested
sorbents at different space velocities changes as follows: An increase of the space velocity
from 4000 h1 to 12,000 h1 led to a decreased sulfur removal efficiency from 91.93% to
70.77% for ZnO. Increasing the space velocity from 4000 h1 to 12,000 h1 for the
CuO–MnO adsorbent slightly decreased the sulphur removal efficiency from 94.26% to
93.28%. The zeolite sulfur removal efficiency dropped from 98.28% to 95.58%. It can
be seen that the space velocity has a greater influence on the ZnO sorbent than on the
CuO–MnO sorbent and the zeolite.

Figure 11. Sulfur capture capacity. Reaction temperature 293 K; space velocity 4000 h1; H2S inlet
concentration 1000 ppmv.
Weinlaender et al. 133

Table 2. Sulfur capture capacity in (mg of sulfur)/(g sorbent). Reaction

temperature 293 K; space velocity 4000 h1; H2S inlet concentration
1000 ppmv.

Sorbent ZnO CuO–MnO Zeolite

Sulfur capture 46.3 180.1 31

capacity (mg/g)

Effect of inlet H2S concentration

Figures 8 to 10 show the effect on H2S outlet concentration for synthetic biogases with
200 and 1000 ppmv H2S inlet concentration. Increasing the inlet concentration from
200 2to 1000 ppmv on the ZnO extrudates had major impact on the H2S outlet
concentration. In numbers, the H2S outlet concentration increased from 18 ppmv to
270 ppmv after 30 minutes. On the other hand, Figure 9 shows the impact of increasing
the inlet concentration on the CuO–MnO extrudate. The increase of the H2S inlet
concentration resulted in an increase of the outlet concentration from 12 ppmv to
68 ppmv. As the zeolite is concerned, the H2S outlet concentration increased from 4 ppmv
to 51 ppmv. This can be seen in Figure 10. Comparing the outlet concentrations of the
experiments indicates that the zeolite works best at high inlet concentrations. It can be
seen that CuO–MnO reaches a steady state after 5–6 minutes while ZnO and the zeolite
still show an increase after 30 minutes. In numbers, the sulfur removal efficiency for ZnO
decreases from 91.93% at 200 ppmv H2S inlet concentration to 82.46% at 1000 ppmv H2S
inlet concentration. For CuO–MnO sorbent it decreases from 94.26% to 93.52% and for the
zeolite it decreases from 98.28% to 96.83%.

Maximum sulfur capacity

All the tests carried out under different operating conditions for 30 minutes give an idea how
the modification of one parameter affects the H2S outlet concentration. Long time
experiments at 293 K and a space velocity of 4000 h1 were performed to characterize the
maximum sulfur capture capacity of the sorbents. The results can be seen in Figure 11
and Table 2. Scap of the sorbents was calculated by equation (2) and cross checked by
analytical chemistry. The CuO–MnO sorbent showed the best sulfur capture capacity with
180.1 (mg sulfur/g adsorbent). The zeolite achieved 31 and the ZnO was measured and
calculated at 46.3 (mg sulfur/g adsorbent).

Conclusion
The desulfurization of biogas is essential for the successful operation of SOFCs. H2S
adsorption on three different extrudates, one based on ZnO, one based on a mixture of
MnO and CuO, and a copper doped zeolite were evaluated at low temperatures in a fixed
bed reactor under various conditions. The sulfur capture capacity Scap, a value for the extent
134 Adsorption Science & Technology 35(1–2)

of sorbent utilization for sulfur removal, was evaluated. This experimental study on
low-temperature H2S adsorption, using different sorbents, has led to the following
conclusions:

1. With the inlet temperature increasing from 293 to 373 to 473 K, Scap increased for
all sorbents. The increase of the temperature slightly improved the performance of
CuO–MnO and the zeolite, and had a major impact on ZnO. The authors are aware
of the fact that ZnO works best at elevated temperatures, but decided to use it because it
is well known and studied and may provide a comparison to the other tested sorbents.
The efficiency of sulfur removal is kinetically favoured at higher temperatures, while its
equilibrium is restricted to lower temperatures. The operating temperature influences
both the diffusion rate and the thermodynamic equilibrium. This is consistent with the
reports in the literature.
2. Decreasing the space velocity from 12,000 to 8000 to 4000 h1 led to the following results
for the ZnO sorbent. At the space velocities 8000 h1 and 12,000 h1, the H2S outlet
concentration dramatically increased compared to the test runs obtained at 4000 h1.
The test at a space velocity of 4000 h1 resulted in the lowest H2S outlet concentrations
due to the increased contact time between gas and sorbent inside the reactor. The
sorbent based on a mixture of CuO and MnO as well as the zeolite were monitored
the same way. The test runs at 12,000 h1, 8000 h1 and 4000 h1 resulted in only a small
difference in the H2S outlet concentration.
3. The inlet H2S concentration was increased from 200 to 1000 ppmv to simulate two
different biogas feedstocks. All tested sorbents showed an increased sulfur capture
rate. This demonstrates that the extent of sorbent utilization was improved by the
sulphur content of the synthetic biogas. Increasing the H2S concentration from 200 to
1000 ppmv had major impact on the H2S outlet concentration of the ZnO extrudates
compared to the CuO–MnO sorbents and the zeolite.
4. Even if the zeolite shows very good results at the tested temperatures, space velocities
and inlet concentrations its maximum sulfur capacity is very low. This results in big
adsorbers compared to CuO–MnO sorbent.

Of all the experiments conducted the conclusion is that operating the zinc oxide sorbent
around a temperature of 473 K and a space velocity of 4000 h1 leads to the best results for
the H2S removal from synthetic biogas. For the sorbent based on a mixture of manganese
and copper oxide, the working temperature should be elevated. The space velocity has no
major impact. The zeolite achieved the best H2S outlet concentrations and the lowest sulfur
capture capacity. Direct comparison between the monitored sorbents shows that CuO–MnO
has the highest sulfur capture capacity and should be considered as a desulfurization
material at lower temperatures. In a future step, the interference of hydrogen chloride on
the sorbents will be investigated.

Declaration of Conflicting Interests

The author(s) declared no potential conflicts of interest with respect to the research, authorship, and/or
publication of this article.
Weinlaender et al. 135

Funding
The author(s) disclosed receipt of the following financial support for the research, authorship, and/or
publication of this article: The authors would like to thank the Austrian Research Promotion Agency
(FFG) for funding this project. The project title is SOFCool (grant number 843835).

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