IPA16-151-E
PROCEEDINGS, INDONESIAN PETROLEUM ASSOCIATION
Fortieth Annual Convention & Exhibition, May 2016
PERFORMANCE EVALUATION OF H2S ADSORBENT IN SINGA FIELD: CASE STUDY OF
ADSORBENT PIMIT-B1
Moh. Nurdin Ardianto*
Heru Wijaya Pamungkas*
Subagjo**
ABSTRACT
Medco E&P Lematang (MEPL) attempts to optimize
operation performance and chemical expenses by
sourcing alternative H2S Adsorbent. PIMIT-B1 is
high local content H2S licensed under ITB & PIM
adsorbent. It is a new iron oxide based solid
adsorbent for H2S removal. PIMIT-B1 was initially
produced for the purpose of removal of H2S from
natural gas feedstock in Ammonia Plants. Later,
PIMIT-B1 was proposed to be applied in oil and gas
upstream industries.
This paper presents the results of performance
evaluation of PIMIT-B1 in its use as H2S Scavenger
adsorbent in Singa Central Processing Plant (CPP).
PIMIT-B1 was placed in a tower that allows residue
gas containing H2S from membrane unit to flow
downward from the top section of the tower to its
bottom section. For evaluation its performance, the
sample gas was taken to measure H2S concentration
in three sampling points along the tower, as well as
inlet residue gas was taken on daily basis. These data
are then processed to show the trends in which the
H2S from residue gas are being adsorbed. These
trends will show the breakthrough point, shape of
breakthrough curve, and sulfur loading at any given
time that are used to evaluate the performance of
PIMIT-B1.
From the data gathered until day 180 of adsorbent
usage, with average flow of feed natural gas and
average concentration of H2S 9.01MMscfd and
60.19ppmv respectively, the calculated breakthrough
point of the bottom of the adsorbent bed is at the day
77. Prediction of the time when the bed becomes
saturated based on the trends is day 266-269 and
sulfur loading at the time is approximately 0.25. It
was concluded that PIMIT-B1 can be implemented
for further operation and be more economical in
Singa CPP.
* Medco E&P Indonesia
** Institute of Technology Bandung
INTRODUCTION
Medco E&P Lematang (MEPL) operates Singa
Central Processing Plant (CPP) in Singa Field,
Lematang block. CPP is located about 230 km
southwest of Palembang, South Sumatra (Figure 1).
Singa CPP has sour gas treatment facility, configured
in two parallel acid gas removal systems. The acid
gas removal consists of Amine Unit with Methyl Di-
Ethanol Amine (MDEA) solvent and Membrane
Unit.
Two gas wells with High Temperature & High
Pressure (HTHP) characteristic were produced as
feed for CPP and to be processed into sales gas.
Singa CPP commenced production in April 2010,
with 40 BBTUD sales gas delivered to gas buyer.
SINGA CPP OVERVIEW
Acid gas removal unit in Singa CPP consists of two
systems, Amine unit and Membrane unit, were
designed to anticipate 38 percent mole CO2 and 350
ppm H2S in raw gas. To produce the sales gas with
specification of 4%vol CO2 and 4 ppmv H2S,
Membrane unit will separate hydrocarbon gas from
acid gas (CO2 & H2S) and moisture content.
Membrane output flow (residue gas) is not capable to
achieve 4 ppm H2S due to design restriction (acid
permeation). Thus, H2S Scavenger unit (2x50%)
containing adsorbent solid bed was installed
downstream of Membrane unit to purify the gas
stream from H2S.
According to block diagram in Figure 3, the raw gas
flows to CPP trough dedicated flowlines and collects
in one manifold. The process begins with a series of
steps to separate produced water (PW) from the raw
gas while lowering its temperature. The PW is then
flowed to H2S Stripper to remove H2S content and
further processing in Produced Water Treatment
(PWT).
Once passed through the gas filter, sour gas is then
processed further in the AGRU, which consists of
Amine System and Membrane System. A major
quantity of gas is processed in Amine Unit while the
remaining is processed in the Membrane Unit. These
processes produce sweet gas and residue gas at a
lower CO2 and H2S content. Moisture content in the
sweet gas from Amine system is removed in the
dehydration system, meanwhile the residue gas from
Membrane system which contains H2S to be purified
in H2S Scavenger Unit
Membrane Unit which depends on physical
permeation separates hydrocarbon from acid gas and
moisture content in the feed gas to produce residue
gas. As per design, membrane output is 18 ppmv
where will not achieve H2S as per sales gas
specification (4 ppmv). Therefore, a H2S Scavenger
unit 2 x 50% containing H2S adsorbent solid bed was
installed at downstream Membrane Unit (Figure 2).
This unit is designed to remove H2S in residue gas up
to 4 ppm.
As the feed gas passes through the membrane tubes,
the gas is separated into a high-pressure methane-
rich gas (residue), and a low pressure gas stream
concentrated in carbon dioxide (permeate). Because
H2S content at residue gas outlet of membrane unit
was still too high, two parallel of H2S Scavengers
were installed to reduce H2S content.
BACKGROUND
The consumption of chemical H2S adsorbent used in
Singa CPP is up to 60 metric ton per year. This was
significant for operations costs. During initial
operation, MEPL attempted to optimize the
requirements for chemical consumption and to obtain
more efficient chemicals for gas processing.
MEPL attempted to optimize operation performance
and chemical expenses by sourcing alternative H2S
Adsorbent. Institut Teknologi Bandung (ITB)
promoted PIMIT-B1, a new iron-oxide based H2S
adsorbent, jointly researched and produced with PT
Pupuk Iskandar Muda (PIM) Aceh. PIMIT-B1
adsorbent is high local content and licensed under
ITB & PIM. PIMIT received its patent from
Direktorat Jenderal HKI RI in 2009.
After several technical discussions and considering
plant availability and configuration, MEPL decided
to conduct the field trial in full scale basis to observe
the PIMIT-B1 adsorbent performance. This activity
also will promote the utilization of material with high
local content (TKDN) where regulated by
Government of Indonesia by Permen ESDM No. 15
/ 2013.
OBJECTIVE
A field trial was conducted in full scale basis with 15
tons PIMIT-B1 adsorbent in one vessel, with
minimum 180 days trial operation to conclude the
performance. The objective of this study is to publish
the performance data of PIMIT-B1, including
process data (pressure drop, H2S content etc), sulfur
removed per adsorbent weight (lbs/lbs) and
breakthrough time (days). Thus the field trial result
to be compared with adsorbent design data
HYDROGEN SULPHIDE REMOVAL
SYSTEM
H2S Scavengers are used to remove small quantities
of sulfur compound. It has relatively high operating
cost per weight of sulfur removed and is suitable for
treatment of low H2S. H2S Scavenger processes are
typically batch operations. The reactive material is
brought into contact with sour gas stream until the
sweet gas sales requirements can no longer be met.
Then reactive material must be replaced and
removed as waste and disposed of in an
environmentally acceptable procedure.
Numerous commercial scavenger units are available
on the market. They can generally be categorized
into two different groups as follows:
Dry Sorption Processes
The reactants in this process are solid without free
water and thus are called dry. Some of the
compounds may require a hydrate form of the basic
reactant in order to precipitate in the treating
reaction. In addition there must be some water
available either with gas feed or moisture on the dry
solid to initiate the reaction. Once started, the
reaction will produce of mole of water with each
mole of H2S removed. Several processes in the dry
sorption are classified based on metal type such as
Iron Oxide base, Zinc Oxide base and Alkaline base.
Liquid Absorption Processes
The reactants in this process are liquid in form of
either aqueous or slurry. Gas-Liquid Contactors are
used to increase contact surface and maximize gas
contact time (Wang, 2011). Several process
technologies are available and classified as slurry
process, zinc oxide slurry, oxidizing solution, etc.
Table 1 lists the process technology available for H2S
Scavenger.
Considering the amount of H2S present in residue gas
is less than 1% v/v, MEPL chose dry sorption process
using solid scavenger.
MONITORING OF H2S REMOVAL
PERFORMANCE
Wang (2008) explained the breakthrough curve
which gives an indication of an adsorbate (H2S) is
distributed within a fixed bed when a gaseous stream
containing a percentage of the adsorbate passes
through a fixed until the adsorbate emerges in the
exit stream. Figure 4 shows a typical breakthrough
curve and Figure 5 shows the concentration of
adsorbate in the gas phase at any given point
(location) in the bed as a function of time.
The adsorbent quickly becomes saturated at the inlet
of the bed and the adsorbate concentration falls off
rapidly along the bed forming a concentration profile
along the bed which is called the transition zone.
In Figure 5, t1 shows the initial formation of the
concentration profile, t2 shows one at some
intermediate time, and tb shows another just before
breakthrough. The point at which the adsorbate H2S
is first detected at the exit stream. After
breakthrough, the adsorbate concentration in the
effluent stream rises steeply up to the value of the
inlet concentration during the time interval between
tb and tc as shown in Figure 4.
Break through time is the time where the break
through point occurs. While sulfur loading is the
amount of sulfur sequestered by the adsorbent at a
certain time. Equation (3) is modified equation for
calculating sulfur loading by Wang (2008) on the
breakthrough time.
, of this adsorbent is up to 40 percent. Therefore,
(1)
Where
VH2S = feed molar velocity, kmol/h
tb = breakthrough time, h
CA,in = H2S Concentration, ppmv
MWs = Weight Molecule of Sulfur = 34 kg/kmol
Wfb = bed weight, kg = A x Z x ρb
A = adsorbent-bed surface area, m2
Z = height of adsorbent-bed, m
ρb = bulk mass-density of adsorbent, kg/m3
CONFIGURATION OF H2S SCAVENGER
H2S Scavenger Unit installed in Singa CPP has two
parallel vertical vessels 35-MBA-187 A/B size 1525
mm OD x 8895 mm S/S. It was designed for 1315
psig at 150F and capable of handling 25 MMscfd
residue gas arising from gas-gas exchanger. It has
bed height of 8.050 m.
The H2S Scavenger vessel was designed with criteria
max H2S concentration at outlet flow 4 ppm,
allowable pressure drop max 2 psi, dry gas moisture
content and 0.2 lb/lb adsorbent sulfur loading.
There are three nozzles spread evenly above all the
packing with the distance between the nozzle and the
top and base of packing more than 2 m. The top
nozzle is Nozzle 9, as far as 2.001 m from the top of
the packing, followed by Nozzle 10 as far as 2.099 m
below it, and the Nozzle 11 as far as 2.000 m from
the Nozzle 10 and 1.950m from the bottom of the
packing adsorbent.
Residue gas enters at the top section of the vessel via
a pipe distributor and flows downwards through
distributor plate and top section ceramic ball,
adsorbent bed, bottom section ceramic ball then
exiting from bottom of vessel. As the residue gas
passes down the adsorbent bed.
ADSORBENT PIMIT-B1
PIMIT is used for absorption to remove the sulfur
(H2S) contained in natural gas and other gaseous
hydrocarbons. PIMIT has operating temperature in
range 20-60°C. This product has been licensed under
ITB & PIM, Patent Certificate No. P00200200732
from Direktorat Jenderal HKI RI.
Based on local content calculation, the local content
PIMIT-B1 has the highest local content of H2S
Adsorbent ever used in MEPL. PIMIT-B1 also has
been used in PT Pertagas Sumbagut for trial H2S
adsorption (5 ton) and delivered the expected result.
PIMIT-B1 is an ironoxide based H2S Scavenger to
react with adsorbed H2S. The reaction of sulfur
removal using iron oxide adsorption (Wang, 2008)
is:
H2S (g) + Fe2O3  Fe2S3(s) + H2O (l)
∆H = -22 kJ (25 °C and 1 atm)
The reaction is exothermic, which means the
adsorption of H2S may increase the temperature of
internal vessel and require special attention. The
reaction is best performed at room temperature.
Therefore, the gas temperature should be monitored
and maintained to prevent overheating.
PIMIT-B1 is produced in pellet shape with dark red
color, detail specifications are listed in Table 2.
TRIAL AND EVALUATION METHOD
To perform the field trial in full scale, the operating
procedure for catalyst change out has been developed
to ensure the adsorbent was safely loaded into the
vessel. The new adsorbent PIMIT-B1 with weight
32,000 lbs is loaded into the vessel H2S Scavenger,
which includes the ceramic balls and support
equipment. After removing the oxygen in the vessel,
the gas is introduced from the outlet of Membrane
into the inlet H2S scavenger vessel.
To evaluate its performance, H2S concentration was
sampled on daily basis at three points along the tower
as well as inlet residue gas. These data are then
processed to show the trends in which the H2S from
residue gas are being adsorbed. The trends will
shows the breakthrough point, shape of breakthrough
curve, and sulfur loading at any given time that are
used to evaluate the performance of PIMIT-B. The
other data such as inlet gas flowrate, bypass flowrate
and the vessel pressure drop to be recorded and
monitored closely.
H2S Scavenger performance data have been
collected. It represents various operating conditions
of H2S Scavenger from December 2013 till October
2014. The processed data were taken daily from the
first day usage up to 180 days using H2S detector.
Data from the initial concentration of H2S in natural
gas into the vessel and daily H2S concentration data
were observed at each position of the nozzle,
calculated percent H2S adsorbed and the ratio
between the concentrations of H2S in a certain
position with the inclusion concentration. Both data
sets are presented in graphical form to illustrate the
trend of decrease in the amount of H2S that can be
adsorbed by the adsorbent PIMIT.
The equation to calculate percentage H2S adsorbed is
as follows:
% 100% (2)
Where:
C0= H2S inlet (scfd)
Cn= H2S at nozzle n (scfd), n= 9, 10, 11
From the data that has been collected, break through
time to point at Nozzle 9, 10, and 11 can be seen
clearly. To estimate the break through time on the
basis of packing we used approach through piles of
sulfur loading PIMIT. From the break through time
and the break through curve tendency to reach a point
where no further adsorption can occur, the lifetime
of the adsorbent PIMIT can be estimated. Further, the
calculated lifetime and sulfur loading were compared
with PIMIT-B1 specification.
TRIAL RESULT AND EVALUATION
H2S Concentration
The Figure 8 chart represents daily residue gas
flowrate from gas/gas exchanger to H2S Scavenger
Vessel and residue gas flowrate which was bypassed.
During this observation period (12 Des 2013 – 12
Oct 2014), average residue gas flowrate entering H2S
Scavenger is 9.01 MMscfd.
It is noted that residue gas flowrate to H2S Scavenger
tended to decrease over time, since CO2 content of
residue gas from Membrane tended to increase over
time. Therefore residue gas must be decreased in
flowrate prior to mixing with sweet gas from amine
unit, so that the mixed gas meets sales gas
specification. Refer to the profile of H2S content
Figure 8, residue gas for 180 days observation
contains 60.19 ppmv H2S average.
The Figure 9 chart represents the H2S concentration
(Ca) in Nozzle 9, 10 and 11 at H2S Scavenger Vessel.
The H2S concentration at these nozzle tended to
increase due to adsorbent saturation.
Breakthrough Curve
Figure 10 represents the comparison of H2S content
at the outlet and the inlet during the trial days.
According to the chart at Figure 10, in the early days
of usage PIMIT adsorbent, the gas passing through
the Nozzle 9, 10 and 11 have been completely
cleaned and no longer contain H2S. On the 23th day
break through times of the Nozzle 9 and 10 began to
register slight H2S. As it passes through the gas is
cleaned in the packing that exists between the Nozzle
10 and 11. On the 41st day, a breakthrough time
occurred for Nozzle 11.
From the graph it can be seen that the break through
curve formed at Nozzle 10 and 11 show similarities,
but deviation occurs at breakthrough curve formed
by Nozzle 9. Based on this deviation, the data on the
position of the Nozzle 9 will no longer be used for
the next observation. Correlations for position of
Nozzle 10 and 11 were obtained with a value of R
0.7625 and 0.787 respectively. Correlation for the
position of Nozzle 11 was selected to determine a
time when the H2S inlet rate equaled the H2S outlet,
which means that at that time, adsorbent packing
above Nozzle 11 is no longer able to adsorb H2S.
Correlation of Nozzle 11 gives R value that is closer
to1and apposition that is closer to the bottom of the
packing. Smaller interval data provides a better
alignment with what is happening on the basis of
packing. According to this correlation, adsorbent has
no longer time to adsorb H2S at day 269, or 228 days
from breakthrough time until complete saturation
point.
Table 3 summarizes the breakthrough time and the
calculated sulfur loading based on the position of
sampling point. Equation (1) is used to calculate the
sulfur loading.
At the position of Nozzle 11, the sulfur loading is
0.18grams/gram of adsorbent. By assuming that in
the event of a breakthrough at the bottom of the
packing, distribution H2S adsorbed is same with a
breakthrough on the position of the Nozzle 11, the
sulfur loading that occurs also can be assumed to
have a value equal or close. The break through time
for the bottom of the packing is on the 77th day. So
that the life time of the adsorbent packing PIMIT
obtained is 302-305 days or approximately 10.1
months.
Sulfur loading calculated at the time of complete
saturation is reached at 0.25 gram H2S/gram
adsorbent. Sulfur loading slightly exceeds the ability
of sulfur loading of 0.24 gram H2S/gram adsorbent
provided by the manufacturer due to the different
residue gas flow rate used. With smaller gas flow,
ability of adsorbent to adsorb H2S could rise further
as the contact time increases and provide more
opportunities for equilibrium between the adsorbate
in the gas and in the adsorbent.
CONCLUSION AND RECOMMENDATION
Based on full scale field trial, it can be concluded:
 The breakthrough curve with comparison of H2S
content predicted 58 days breakthrough time at
bottom vessel.
 The lifetime of adsorbent PIMIT-B1 in H2S
Scavenger vessel in Singa CPP with flowrate and
concentration of H2S in the first 6 months of use
is 302-305 days.
 Sulfur loading PIMIT in H2S Scavenger
adsorbent vessel Singa CPP at complete
saturation point is 0.25 gram H2S/gram
adsorbent
Based on the conclusions, MEPL should continue the
collection of data for monitoring and comparing with
other adsorbents. Meanwhile, the operator should
monitor the H2S content at outlet vessel closely after
passing the breakthrough time at bottom vessel.
PIMIT-B1 also can be used for further operations for
H2S removal system in Singa CPP.
REFERENCES
Lili Dj., Subagjo, Susanto T.P., Edy H.P., 2012,
Adsorben Sulfur PIMIT-B1 Sebuah Pengembangan
Produk Hasil Kerjasama antara Industri dan
Perguruan Tinggi, Seminar Nasional Teknik Kimia
Soebardjo Brotohardjono IX, page C.5-1 – C.5-4
Subagjo, 2015, Restorasi Semangat Membuat Baju
dari Batu: Peranan ITB dalam Pembuatan Katalis
Nasional, Pidato Ilmiah pada Peringatan Dies
Nataliske 56, Institut Teknologi Bandung, page 5-8
– 5-12
Wang, H., Wang D.M., and Chuang K.T., 2011, A
Sulfur Removal and Disposal Process through H2S
Adsorption and Regeneration: Breakthrough
Behavior Investigation, Process Safety and
Environment Protection
Wang D.M, 2008, Breakthrough Behavior of H2S
Removal with an Iron Oxide Based CG-4 Adsorbent
in a Fixed-Bed Reactor, Department of Chemical
Engineering University of Saskatchewan
 TABLE 1

H2S SCAVENGER PROCESS TECHNOLOGY

Iron Sponge Process

Iron Oxide Basis Process
Sulfa Treat Process

Sorption
Zinc Oxide Basis Process ICI Low Temp Zinc Process
Dry
Alkaline Solid Softnolime RG Process
H2S Scavenging Process Technology

Slurry Process Iron Oxide Process

Zinc Oxide Slurry ChemSweet ; Slurry Process
Permanganate / Dichromate
Oxidizing Solution
Processes
Oxidizing Chlorine Based
Liquid Absorption

Diklor Processes
Solution
Sulfa Check Processes
Oxidizing Nitric Solution
Hondo HS-100 Process
Aldehyde Based Processed
Polyamine Based Process Sulfa Srub
Sulfa Guard
Alkylamine Gas Treat 114 Process
Process Sulfa Check
Caustic Scrubbing NaSH Process

TABLE 2

SPECIFICATION OF PIMIT-B1 ADSORBENT

Specification Unit Description

Color - Dark red
Size mm 5x8
Shape - Pellets
pH - 8–9
Fe2O3 (dry basis) % 78,08
Moisture % 3 -4
Crushing Strength Kgf 4-9
Bulk Density Kg/l 0.90 – 1.051
Surface Area m2/gr 83 - 101
Absorption Capacity Kg/kg 0.24

TABLE 3

BREAKTHROUGH TIME AND SULFUR LOADING

Position Breakthrough Time Sulfur Loading

Nozzle 10 24 days 0.10
Nozzle 11 41 days 0.18
Bottom of Vessel 58 days 0.25
Figure 1 – Location of Singa CPP in Lematang Block

Figure 2 - Membrane unit in Singa CPP

 Figure 3 - Block diagram of Singa CPP

Figure 4 - Breakthrough curve from the breakthrough point, tb, to the complete saturation point, tc.

Figure 5 - Development and progression of a transition zone along the bed: transition zones at different time
t1, t2 and breakthrough time tb
Figure 6 - H2S Scavenger vessel 35-MBA-187 A/B

Figure 7 – PIMIT-B1 in pellet shape

Figure 8 - Gas flow rate and H2S concentration in inlet of H2S scavenger vessel during PIMIT trial

Figure 9 - H2S concentration in nozzle 9, 10 and 11 of H2S scavenger vessel during PIMIT trial
Figure 10 - Breakthrough curve comparison from each nozzle