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UOP.indd 1 11/03/2024 10:12:27
 ptq gas
PETROLEUM TECHNOLOGY QUARTERLY

2024
www.digitalrefining.com
3 LNG accelerating the low-carbon energy transition
Rene Gonzalez

5 Dryout design considerations for cryogenic gas plants: Part 1

Scott A Miller, David A Jelf, J A Anguiano and Joe T Lynch
Honeywell UOP

11 Optimise sulphur recovery plant emissions during unit upset conditions

Jochen Geiger, Michael Gaura and Anantha Kukkuvada
AMETEK Process Instruments

17 ‘On the fly’ vs high-performance H₂S selective solvent

Ashraf Abufaris BASF Middle East Chemicals LLC
Blake Morell BASF Corporation

21 Steam methane reformer tube lifecycle improvement best practices

Richard D Roberts and Grant Jacobson
Becht

28 Testing and effects of pipeline chemicals on gas processing facilities

David Engel and Scott Williams
Nexo Solutions

32 Hydrogen recovery from refinery off-gas – Part 1: An overview

Zach Foss
Divigas

Cover
From LNG liquefaction facility projects to advances in hydrogen production technology, bankable
investments reflect the gas industry’s role in the transition to net zero emissions by 2050.
Photo courtesy of Joshua Sun

©2024. The entire content of this publication is protected by copyright full details of which are available from the publishers.
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supplements the publisher cannot be held responsible for any statements, opinions or views or for any inaccuracies.

ed com.indd 1 08/03/2024 15:48:50

 Energy Transition
is in the air

Discover our Discover our

Gas Products Gas Processes

Untitled-5 1 14/03/2024 14:17:53

 ptq
LNG accelerating
the low-carbon
energy transition
PETROLEUM TECHNOLOGY QUARTERLY

Editor
Rene Gonzalez
editor@petroleumtechnology.com
tel: +1 713 449 5817
Managing Editor
Rachel Storry
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Register to receive your regular copy of
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PTQ (Petroleum Technology Quarterly) (ISSN No:
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and is distributed in the US by SP/Asendia, 17B
South Middlesex Avenue, Monroe NJ 08831.
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D
emand for liquefied natural gas (LNG) is expected to continue beyond 2040.
China has overtaken Japan to become the world’s largest LNG importer, while
demand from other Asian countries is also growing, even as domestic gas
production in some of these countries is decreasing. Significant infrastructure projects
are required to be able to import LNG from the Middle East and other exporting
countries. High capital investments needed for regasification terminals do not
guarantee secure supply when considering disruptions due to geopolitical conflicts.
All this must be factored into the industry’s long-term planning for using LNG to
provide grid stability while facilitating a higher share of renewables in the market.
In the medium term, potential demand, such as from India, is set to consume new
supply coming onto the market by 2025. The question is, who are the exporters
that growing markets can depend on, especially when committing to long-term con-
tracts? The big winners are the dominant exporters from the Middle East and Russia.
This begs the question that as the top global natural gas producer and exporter, the
US’s exports of LNG play a vital role in supporting global energy security. Following
Russia’s invasion of Ukraine, the US has become the primary supplier of LNG to
Europe. However, to what extent will the perceived flexibility and reliability of US
LNG in global markets last?
With the current US Administration enforcing a moratorium on planned LNG
exports to non-Free Trade Agreement countries, compelling postponement or can-
cellation of new liquefaction projects, Russia stands to win big by not only influenc-
ing Europe and China’s LNG market but elsewhere throughout the globe. Against
this backdrop, the US was again the largest supplier of LNG to Europe in 2023,
accounting for nearly half of total LNG imports, according to data from Cedigaz. In
parallel, Southeast Asia is increasing LNG imports to backfill domestic gas declines.
The US EIA Short-Term Energy Outlook (6 February) expected the US benchmark
Henry Hub natural gas spot price to average higher in 2024 and 2025 than in 2023 but
remain lower than $3.00 per MMBtu. The forecast seems to be based on increases in
natural gas prices as demand grows faster than supply in 2024. Developers advanced
several LNG projects to the construction phase in 2023, following the signing of sale
and purchase agreements (SPA), contracts specifying the terms and conditions of
LNG supplies between seller and buyer, underpinning the projects.
Developers signed contracts with buyers for almost 22 million metric tons per year
of LNG last year, or about 3 Bcf/d of natural gas, according to data from the US
Department of Energy (DOE) and company websites. However, the volumes con-
tracted in 2023 totalled 52% less than the contracted volumes in SPAs signed in
2022. On 16 January 2024, a record high of 141.5 billion cubic feet (Bcf) of natural
gas was consumed in the US Lower 48 states due to the ‘Polar Vortex’, exceeding
the previous record set on 23 December 2022, according to estimates from S&P
Global Commodity Insights.
LNG’s dominance in the transition to net zero emissions and energy security will
be enhanced with a range of technologies incorporating advanced analytics, the
Internet of Things, and artificial intelligence to enhance efficiency, safety, overall
operational performance, and ultimately capacity, including increased ammonia and
hydrogen production, such as blue hydrogen. For example, blue hydrogen’s future,
as discussed in this issue of Gas 2024, is expected to become clearer by the end of
the year, as the US DOE awards the first billion-dollar subsidies for demonstration
projects and the Treasury Department issues guidance for companies that want to
claim new tax credits for low-carbon hydrogen production.

Rene Gonzalez

Gas 2024 3

ed com.indd 3 07/03/2024 17:44:54

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p4 becht.indd 1 07/03/2024 16:40:58

 Dryout design considerations for
cryogenic gas plants: Part 1
A well-conducted cold plant dryout will help plant commissioning and ensure
start-up goes smoothly and does not last any longer than necessary
Scott A Miller, David A Jelf, J A Anguiano and Joe T Lynch
Honeywell UOP
A
cryogenic plant dryout is a critical step during
start-up, but it often does not receive proper atten-
tion early in the project that would allow successful
execution. For this discussion, ‘cold plant’ refers to a cry-
ogenic turboexpander plant for natural gas liquids (NGLs)
recovery, which recovers liquids comprised of either ethane
and heavier components (often referred to as C₂+ liquids or
NGLs) or propane and heavier components (often referred
to as C₃+ liquids or liquefied petroleum gas [LPG]).
A cold plant dryout can be executed correctly the first
time. The owner/operator can be confident that the cold
plant is dry prior to cooling down when proper design
features are implemented, and guidelines are followed. All
gas processors know that water must be removed from the
cold plant. However, knowing the best method for remov-
ing water; how much water has been removed during the
dryout period; and when dryout is complete, can be chal-
lenging. Far too often, a dryout is stopped before the cold
plant is completely dry.
Hydrate problems
The solid that forms when water is present in a hydrocar-
bon stream is not ‘ice’, but a crystalline structure known as
a hydrate. Hydrates can form at conditions where solids
would not be expected and will form above the freezing
point of water. They are a physical combination of water
and other chemical constituents, like those found in natural
gas processing, which have an ‘ice-like’ appearance.1
Hydrates form when enough water is present at the
right combination of temperature and pressure and tend to
favour systems with low temperature and high pressure.2
For gas plant owners/operators, this means that when the
plant begins to cool down, hydrates will form in process
areas where sufficient water is present, restricting or com-
pletely obstructing process flow.
It is not uncommon to see hydrates obstructing flow
through heat exchanger passes or the strainers that pro-
tect the heat exchanger from construction dirt and debris.
Hydrates can cause enough pressure drop to rip apart
strainers, allowing dirt and debris to enter and damage the
downstream heat exchanger. In the case of thermosyphon
reboilers and side heaters, hydrate formation may restrict
the flow through the exchanger and reduce the amount of
www.digitalrefining.com
UOP.indd 5
heat input to the column enough to prevent achieving the
bottoms liquid product purity specification.
Hydrates may also form on the cold plant fractiona-
tion column trays and packing. The result is a decrease in
efficiency, causing low product recovery and potentially
off-specification liquid product. Hydrates are also known to
plug control valves and plant instrumentation.
Water can enter the plant equipment through rain or con-
densation from open piping during construction and through
water left after hydrostatic testing. The single most impor-
tant step that can be taken prior to the start-up of a cold
process plant is to drain and blow out as much free water as
possible from the piping and equipment. Eventually, all the
water must be removed from the cold plant to the parts per
million (ppm) level for the cold plant to operate safely and
efficiently. Not all of the water can be removed simply by
draining low points. The remaining water must be removed
by a combination of moving the water to a low point where it
can be drained and absorbing the water in a vapour stream
so it can be removed from the cold plant equipment and pip-
ing. Several options for eliminating this remaining water are
presented in the next section.
Dryout options
The following options are common approaches to drying
out a cold plant prior to cooldown. A description of each
option is given, discussing its advantages and disadvan-
tages, in order from the least cost-effective to the most
cost-effective option.
Option 1 involves pressure cycling with nitrogen. In this
approach, sections of the cold plant are isolated to be pres-
surised and depressurised multiple times using nitrogen.
This method requires no piping design considerations other
than properly locating low-point drains and ensuring the
drains are of sufficient number and size to remove water
from the system.
This dryout approach requires a large quantity of nitro-
gen to be available and can be very expensive because of
the amount of nitrogen consumed. This dryout option is
less likely to be successful if large quantities of free water
(puddles of water) are still present in the system. It is more
difficult to determine the amount of water remaining in the
cold plant after nitrogen purging and whether all water has
Gas 2024 5
08/03/2024 09:47:20

To sales,
reinjection,
or flare
A A
Cold plant
Inlet gas
B B
Dust filters
Dehydrators
Liquid
Dryout flow path Off-line product
Figure 1 Once-through dryout
been removed from the system compared to the other dry-
out approaches. Water content readings must be taken at
many more locations to get an accurate assessment of the
amount of water remaining in the system.
Option 2, the once-through dryout approach flows
warm, dehydrated inlet gas through the cold plant, equip-
ment, and then to the flare stack, reinjection, or a sales gas
pipeline. The dryout path is operated at as low a pressure
as possible. The pressure drop through the cold plant is
minimised to prevent any Joule-Thomson (J-T) expansion
that would cool down the process while drying the plant.
The flow rate should be maintained to move any free water
to the low-point drains, or to absorb the water in the vapour
stream and remove it from the process. A pressure-reduc-
ing device (such as a temporary flow orifice or valve) must
be included to take the pressure drop upstream of the cold
section of the plant. Figure 1 illustrates the main process
flow path for this dryout method.
Keep in mind that the dryout flow rate may be limited by
the flare system’s tolerance for flaring or reinjection system
capacity. If the wet gas is sent to a sales gas pipeline, the
gas water content should be monitored to ensure it remains
below the maximum amount specified. The once-through
dryout is an effective approach and has been used on many
projects. However, the dryout flow rate can be limited by
the flare system or reinjection capacity. For this scenario,
the dryout period will most likely be longer in order to
remove all the water in the cold plant.
Option 3, the closed-loop re-circulation approach, recir-
culates warm, dehydrated gas in a closed loop through
the cold plant back to the dehydration system inlet using a
residue gas compressor. The dryout loop is operated at as
low a pressure as possible without shutting down the res-
idue compressor. The pressure drop is minimised through
the cold plant to prevent any J-T expansion that would cool
down the process while drying the plant. Again, the goal
is to minimise pressure drop through the cold plant but
maintain a high enough flow rate to ‘sweep’ free water to
low-point drains or carry the water away in the gas to be
removed by the front-end dehydrators.
A recirculation line is required that connects the residue gas
line downstream of the residue gas compressors to the inlet
gas piping upstream of the dehydrators to make the ‘closed
loop’. A pressure-reducing device (such as a temporary orifice
6 Gas 2024
UOP.indd 6
Air cooler Residue gas compressor
To sales
A A
Cold plant
Inlet
gas
B B
Dust filters
Dehydrators
Liquid
Dryout flow path Off-line product
Figure 2 Closed-loop recirculation dryout
or valve) must be included in the dryout design to take the
pressure drop upstream of the cold plant. Figure 2 illustrates
the main process flow path for this dryout method.
The closed-loop recirculation approach is our recom-
mended approach, as it achieves a proper dryout in the
shortest time. This dryout option removes both free water
and ambient condensation. It does so without excessive
amounts of nitrogen, as with nitrogen pressure cycling, or
excess flaring, as with a once-through dryout with dehy-
drated inlet gas. Nitrogen cycling is only effective at remov-
ing ambient condensation within the cold plant and does
a poor job of moving free water to the low points where it
can be removed from the system. The once-through dryout
option must have a location to discharge the wet dryout
gas after passing through the cold plant.
Monitoring dryout progress using closed-loop recircula-
tion is relatively straightforward. Once dryout is complete,
transitioning to cooldown can be done quickly with min-
imal effort simply by shifting the pressure drop from the
dryout pressure-reducing device to the J-T valve. If desired,
cooldown can commence using the dryout recirculation gas
prior to introducing fresh inlet gas.
A well-executed dryout begins during the detailed design
phase by determining the dryout features required for a spe-
cific cold plant design. A dryout procedure should be prepared
prior to dryout, including any cold plant design limitations as
well as the specific steps to follow for removing water and
monitoring the cold plant water content during dryout.
Cold plant design features: Executing dryout
Several design features should be considered during the
detailed design phase for the cold plant to be included as
part of the cold plant design package. Although some of the
features listed in this section are required specifically for dry-
out, many will be used for alternative purposes as well (such
as depressurisation and venting hydrocarbons from process
equipment prior to maintenance or repair, isolating equip-
ment, and monitoring the dehydrator outlet water content).
These features are:
• Recirculation piping
• Pressure-reducing device and location
• Drain valves
• Provisions for stagnant process areas
• Location to monitor cold plant water content.
www.digitalrefining.com
08/03/2024 09:47:21
 Air cooler Residue gas compressor Residue gas compressor
To sales To sales Air cooler

Location 1
Location 2
A A A A
Inlet Inlet
gas gas
Cold plant Cold plant

Recirculation B B
B B
piping
Dust filters Dust filters
Dehydrators Dehydrators
Liquid Liquid
Dryout flow path Off-line product Dryout flow path Off-line product

Figure 3 Recirculation piping Figure 4 Possible locations of pressure-reducing devices

Recirculation piping
A recirculation line connecting the residue gas line down-
stream from the residue gas compressor(s) to the inlet gas
piping upstream of the dehydrators should be included to
complete the closed loop. For designs that include a cold
plant bypass, the plant bypass can also be designed to
function as the recirculation line during dryout. Figure 3
shows the typical recirculation piping connection points.
Pressure-reducing device and location
The location of the pressure-reducing device to take the
plant pressure drop upstream of the cold plant is dependent
on the dehydrator regeneration system design and source
of regeneration gas.
When selecting the pressure-reducing device location,
the cold plant designer must be mindful of the location cho-
sen for dehydrator regeneration gas supply and return to
ensure the regeneration compressor has enough compres-
sion head to return the wet regeneration gas to the plant.
For example, in plant designs that use inlet gas for regen-
eration, the pressure-reducing device must not be located
between the dehydrators and the piping take-off for the
regeneration gas supply. The regeneration gas compres-
sor will not be able to overcome the pressure difference.
Figure 4 shows possible locations to consider.
Typically, a temporary flow orifice, manual valve, or auto-
mated valve is used as the pressure-reducing device. For
example, if a temporary orifice is to be installed at Location
2 in Figure 4, the temporary orifice can be installed down-
stream of one of the molecular sieve dust filters inside its
isolation valves (see Figure 5). Typically, two full-flow dust
filters (one filter in service and one spare filter) are included as
part of the dehydrator design package, allowing easy orifice
installation and removal. The orifice plate should be of suffi-
cient thickness to handle the pressure drop, which in many
cases will exceed 500 pounds per square inch (psi) or 35 bar.
The pressure-reducing device should be sized to take the
full plant pressure drop at the maximum dryout flow rate.
The maximum dryout flow rate is set by the maximum flow
the cold plant J-T valve can pass when fully open with a
pressure drop of ~30 psi (2 bar).
The dryout gas flow rate will end up being approxi-
mately 30% of the cold plant nameplate capacity without
for dryout
introducing too much pressure drop across the fully open
J-T valve. Typically, even a single full plant rate residue
compressor can be operated on its surge control line at
reduced speed to provide a pressure rise of less than the
normal operating pressure rise.
The pressure-reducing device can then be sized for
the expected pressures when running the compressor at
reduced speed on its surge line. The surge control valve
will then remain in control in parallel with the dryout loop
flow for the duration of the dryout procedure. If multiple
machines are used, it may be possible to use one machine
with its surge control valve closed during dryout.
The closed-loop operating pressure on the residue com-
pressor suction side must be high enough to clear the
low-pressure shutdowns for the compressor. The discharge
pressure will be determined by the permissible operating
point for the compressor.
Drain valves
During the model review, identify all low points around
major process equipment and add drain valves as required.
Hard pipe all low-point drains to a closed-drain system.
Design the low-point drains to be easily accessible. The
low-point drains will be used periodically to drain any col-
lected free water from the system. A one-inch drain is the
minimum size recommended. There must not be any inter-
nal projection at the drain connection.
The turboexpander and booster compressor low points
are always inside the machines’ isolation valves and, there-
fore, are not available to drain free water during dryout. As
a result, the lowest spot around both machines may move
Temporary orifice in place
of blind flange spacer
Dust filter To cold plant
Figure 5 Detail for temporary orifice

www.digitalrefining.com Gas 2024 7

UOP.indd 7 08/03/2024 09:47:24

 Subcooler
Residue gas
to compression
Booster
Expander
Gas/gas
Inlet Cold
gas sep.
J–T valve
Demethaniser
Reboiler
passes
Stagnant piping and equipment Liquid product
Figure 6 Ethane recovery plant (main dryout path and
stagnant areas)
just outside the isolation points during dryout. In this situa-
tion, ensure low-point drains are installed at these locations
to drain any free water that may collect during dryout.
Provisions for stagnant process areas
The following process flow diagrams (PFD) are examples
of two typical cold plant designs: one designed for ethane
recovery (see Figure 6) and one designed for propane
recovery (see Figure 7). Each PFD identifies major pro-
cess equipment and control valves and highlights the main
recirculation flow path through the cold plant as well as the
stagnant flow areas during dryout.
Several piping and equipment loops and the lower sec-
tion of the fractionation column below the expander outlet
feed are stagnant (no dryout flow). Unless a flow is intro-
duced, these areas of the cold plant will remain wet. Design
provisions must be included to introduce flow into each
stagnant area.
A source of dryout gas is located downstream of the
dehydrator dust filters (also downstream of the pressure-
reducing device used for dryout), but upstream of the cold
plant should be selected to provide dryout flow to each
stagnant area. As an example, for a 200 million standard
cubic feet per day (MMSCFD) or 5.4 x 106 normal cubic
metres per hour (Nm³/hr) cold plant, a 4in minimum pipe
size is recommended from the dryout gas source to provide
adequate flow of dryout gas to multiple stagnant areas at
once. As the cold plant nameplate capacity increases, scale
up the dryout gas source pipe size accordingly to ensure
adequate flow at the recommended 30 psi allowable J-T
valve pressure drop during dryout.
Part 2: Closed loop dryout method and monitoring
UOP Ortloff has witnessed many cold plant dryouts dur-
ing commissioning and initial start-up over the years. A
well-conducted cold plant dryout will help plant com-
missioning and ensure start-up goes smoothly and does
not last longer than necessary. There are multiple dryout
options which can remove water from the system, as dis-
cussed in Part 1 of this two-part article. However, there are
8 Gas 2024
UOP.indd 8
Condenser
Reflux
Residue gas accum.
to compression Booster
Expander
Reflux
Gas/gas pump
Inlet Cold
gas sep.
J–T valve
Deethaniser
Reboiler
Stagnant piping and equipment Liquid product
Figure 7 Propane recovery plant (main dryout path and
stagnant areas)
drawbacks to some of them. The closed-loop recirculation
dryout effectively removes water from the system while
easily monitoring dryout progress This allows for a quick
transition to plant cooldown after dryout is completed.
Some of the design challenges, the method for implement-
ing a closed-loop recirculation dryout, and monitoring pro-
gress will be discussed in further detail in PTQ Q2 2024.
References
1 Engineering Data Book, 12th ed., Gas Processors Suppliers
Association, Tulsa, OK, 2004, Section 20, pp.9.
2 Carrol J, An Introduction to Gas Hydrates, 2008, [Online] Retrieved
May 13, 2010, www.telusplanet.net/public/jcarroll/HYDR.HTM.
3 Engineering Data Book, 12th ed., Gas Processors Suppliers
Association, Tulsa, OK, 2004, Section 20, pp.19.
4 Engineering Data Book, 12th ed., Gas Processors Suppliers
Association, Tulsa, OK, 2004, Section 20, pp.23.
Scott A Miller is a Principal Process Engineer with Honeywell UOP,
supporting Ortloff Cryogenic Gas Processing Technologies. He has
more than 23 years of experience in the petrochemical and gas pro-
cessing industries, of which 15 are in the design and operation of NGL/
LPG recovery plants. Email: scott.a.miller@honeywell.com
David A Jelf is a Principal Instrument and Controls Engineer with
Honeywell UOP, supporting Ortloff Cryogenic Gas Processing
Technologies. He has more than 40 years of experience in the design
and operation of NGL/LPG recovery plants.
J A Anguiano is a former Engineering Manager with Honeywell UOP,
previously supporting Ortloff Cryogenic Gas Processing Technologies.
He has more than 25 years of experience in the design and operation
of NGL/LPG recovery plants.
Joe T Lynch is a retired Engineering and Licensing Manager from
Honeywell UOP, previously supporting Ortloff Cryogenic Gas
Processing Technologies. He has more than 45 years of experience in
the design and operation of NGL/LPG recovery plants.
www.digitalrefining.com
11/03/2024 12:09:39
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 Optimise sulphur recovery plant
emissions during unit upset conditions
Knowledge, understanding, and awareness training are essential to maintain
process instrumentation for optimal information gathering

Jochen Geiger, Michael Gaura and Anantha Kukkuvada

AMETEK Process Instruments

W
orking conditions for refineries are changing, and
such changes might be challenging. In several
geographical areas, the historical supplier of crude
oil has changed, resulting in new crude oil compositions.
The method of supply may also have changed from pipe-
lines, with stable composition, towards ocean vessel sup-
ply, with different compositions.
Regardless, final product quality from refineries needs to
be stable, and quantities need to be ever increasing. At the
same time, environmental impacts are being more strictly
regulated, increasing monitoring and reporting require-
ments. Emissions always need to be reduced. In summary,
more flexibility from refiners is required.
All of this puts more load and attention on sulphur recov-
ery units (SRUs), which are expected to operate continu-
ously and in an optimised manner. As discussed in several
papers, such SRUs require some special attention with
regard to safety and operational monitoring.
On its own, elemental sulphur is not an issue. It is one
of the most common elements (by mass) on earth and is
essential to life. Sulphur is present in living organisms,
including humans, and can be used in fertiliser production. It
even has medicinal applications. However, sulphur can also
be harmful to both humans and the environment. Hydrogen
sulphide (H₂S) concentrations of just a few parts per million
(ppm) in ambient air can lead to illness and death at sus-
tained levels greater than 100 ppm. Sulphur dioxide (SO₂)
is also toxic to humans at very low concentrations but has
received significant attention based on its negative impacts
on the environment. Specifically, it can destroy vegetation
and wildlife and contribute to the production of acid rain.
The basic chemistry of sulphur recovery has been known
for more than 90 years. In today’s world, the capacity of
modern SRUs can range from tens to thousands of tons of
sulphur production per day. The most significant improve-
ments have been made to the overall recovery efficiency.
Although it was sufficient to operate at 80-85% in the
1970s and between 95% and 99% in the 1990s, the cur-
rent requirement is to operate at recovery efficiency rates
of 99.9+%.
Considering that we rely on the same chemistry as 90
years ago, except for tail gas clean-up units, such efficiency
improvements only became possible using reliable process
instrumentation (see Figure 1).

Stack gas
Claus sulphur recovery unit emissions monitoring AT7
SO2 No x (mass flow)
Tail gas treating unit
Absorber outlet
Acid gas feed forward Quench column H2 H2S (COS)
Total hydrocarbons off-gas
H2S NH3 CO2
Claus tail gas H2 H2S AT5 AT6
H2S SO2
Temperature (COS CS2)
AT1
Reduction
AT3 gas Cobalt molybdenum
Air Converters
& condensers generator reduction reactor

Thermal oxidiser

Reactor furnace &

Waste heat exchanger AT4
Quench Absorber &
Reduction column stripper
reactor off-gas columns
Sulphur pit
H2 SO2
sweep gas AT2 Sulphur pit
H2S SO2

Figure 1 Claus SRU

www.digitalrefining.com Gas 2024 11

Ametek.indd 11 07/03/2024 17:10:20


Ratio of O₂ needed per mole HC compared to moles of H2S
Compound moles O₂ per mole HC Ratio of O₂ needed
per mole HC compared
to mole of H₂S
Methane 2 4
Ethane 3.5 7
Propane 5 10
Butane 6.5 13
Pentane 8 16
Hexane 9.5 19
Table 1
The challenges are:
• Understanding of the environmental impact of each sin-
gle instrument.
• Knowing the potential improvement of using the best
instrument combination.
• Keeping the instruments in operational conditions.
• Mitigating upset conditions by understanding ‘unex-
pected’ instrument behaviours.
The following discussion will investigate each sample
point and review from a control aspect and the potential
environmental impact. When considering AT1 feed gas
to the Claus reaction furnace, also known as the feed gas
analyser (refer to AT1 in Figure 1), the bespoke feed gas (in
refineries) can consist of two different source streams. The
first is the acid gas stream, and the second is the sour water
stripper (SWS) gas.
While acid gas should be more stable, the SWS is known
to be a potential source of upsets. Against this backdrop,
we should not fall into the belief that no conditions can
cause upset conditions for SRUs originating from acid gas.
Refinery operating conditions
Refineries need to operate their SRUs with both acid and
SWS gas. This might not be the case for every single unit
(train), but as a general operating condition, it can be
taken as given. One of the problems of SWS gas comes
from ammonia (NH₃) as part of the SWS stream composi-
tion, requiring operation of the Claus reaction furnace at a
higher temperature (<1,200°C) in order react and destroy
the ammonia before entering the heat exchanger.
The key aspect of any feed gas measurement and control
is to mitigate upset conditions. Such upset conditions can
be caused by rapid changes in hydrocarbons in the feed
gas. We can observe such changes in both streams, acid
and SWS gas. Hydrocarbons need a significantly higher
amount of oxygen (O₂) than H₂S to react in the Claus fur-
nace, as shown in Table 1.
Depending on SRU design, the sudden occurrence (or
sudden disappearance) of hydrocarbons can cause opera-
tional issues. The potential impact can even affect bypass
recovery processing steps with potentially drastic conse-
quences. In the case where only the tail gas clean-up unit
gets bypassed, the overall sulphur dioxide (SO₂) emissions
could potentially increase by a factor of 100. Normal SO₂
concentrations after final incineration, in combination with
an amine-based tail gas treatment unit (TGTU), are 200-
400 ppmv SO₂, which will jump to 10,000/20,000 ppmv in
cases of TGTU bypass.
Even when not approaching such dramatic process con-
ditions, it can be said that a closed feed gas control loop can
reduce emissions by 10-15% of the overall emission rate.
Flaring events can be reduced by 65-95%.1 Considering
that sources of hydrocarbon upsets are caused upstream
from the SRU, another new challenge will be caused by fre-
quent changes in crude composition, with most refineries
not designed for such changes in crude composition.
A reliable understanding of the feed gas composition
(H₂S, NH₃, THC, CO₂) will make process control more effec-
tive. Fast responses to compositional changes will allow
a fast reaction on the acid gas-to-air ratio, resulting in an
overall emissions reduction.
The AT2 sulphur pit is a safety measurement where H₂S
must be maintained below the explosive limit (lower explo-
sive limit [LEL] 3.25 vol%). SO₂ should be measured to pro-
vide an early warning of sulphur fire.
A smouldering sulphur fire is not uncommon; exposed
iron pipe reacts with sulphur from pyrites, a slow but exo-
thermic reaction that can result in an ignition source. For
example, with H₂S as the fuel source and pyrophoric fire as
the ignition source, waiting only for oxygen will make the
fire triangulate.
At the AT3 tail gas analyser, also called the air demand
analyser, the entire process control of the modified Claus
process is guided by this measurement. The leading com-
ponents to be measured here are H₂S and SO₂. Their
components can be of interest but do not require process
control. Taking a step back, what does the process control

Claus beds & Tail gas

Acid gas Burner Reaction furnace To tail gas clean-up
condensers
unit or incinerator
FT- AT-
201 301

Main air Trim air

FV-101 FV-102 Sulphur

FT- FT-
101 102

Combustion air

Figure 2 Feedback plus ratio control

12 Gas 2024 www.digitalrefining.com

Ametek.indd 12 07/03/2024 17:10:22

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SO2 + 3H2 H2S + 2H2O
S + H2 H2S
H2O + CO H2 + CO2
COS + H2O CO2 + H2S
CS2 + 2H2O CO2 + 2H2S
Figure 3 Cobalt-molybdenum catalysed reactions
of a modified Claus unit look like? The process consists of
two chemical reaction steps:
3H₂S + 3/2O₂ → SO₂ + 2H₂S + H₂O
SO₂ + 2 H₂S ↔ 3Sx + 2H₂O
First is a thermal reaction (Claus furnace) followed by a
catalytical reaction. The key parameter is the air (oxygen)
flow to the thermal reactor. This setup will result in a spe-
cific H₂S-to-SO₂ ratio. For a modified Claus unit, the ratio is
described as 2:1. Depending on the tail gas treater down-
stream of the Claus unit, this ratio can be different.
As shown in Figure 2, the tail gas analyser controls the
trim air valve, which typically represents 10% of the air-
flow to the reaction furnace. The main air valve is set by the
acid gas-to-air ratio calculated on the best available infor-
mation about the gas entering the reactor. This brings us
back to the previous arguments: improved process control
by getting a reliable feed gas composition analysis. The two
measurements (feed and tail gas) in combination will result
in better process control.
Significant sulphur recovery rate
improvements in the modified
Claus plant are possible by using
modern process instruments and
combining them into a full process
control scheme
Modified Claus unit control
It is essential to understand the potential impact on the
process control scheme for each of the installed measure-
ments. ‘Nice to have’ does not make the difference; relia-
bility and safety are the key. Significant sulphur recovery
rate improvements in the modified Claus plant are possible
by using modern process instruments and combining them
into a full process control scheme.
What is important to consider with any addition of pro-
cess instrumentation, besides safety, is that all instrumen-
tation must provide data quickly and reliably. Downtime is
not acceptable.
Today’s environmental regulations do not allow sulphur
recovery rates <99%. Sulphur emissions will still be too
high. A standalone modified Claus unit will not achieve the
required sulphur conversion rates. Downstream tail gas
14 Gas 2024
Ametek.indd 14
clean-up units are therefore required. The most installed
these days are amine-based TGTUs.
The purpose of the TGTU is to convert all remaining
sulphur components carried over from the modified Claus
unit into H₂S. This happens in the catalytic section of the
TGTU process. The reduction reactor utilises a cobalt-mo-
lybdenum catalyst (also mentioned as CoMo bed). The
cobalt-molybdenum catalysed reactions are shown in
Figure 3.
The first step of the reaction does require hydrogen (H₂).
H2 can be present as a byproduct of the modified Claus
reaction but can also be generated by an inline reduction
burner or provided from an external source. To ensure that
the ‘sulphur compounds to H₂S’ reaction is complete, an
excess of H2 is required after the reduction reactor, regard-
less of the H2 source.
In the second process step, the H₂S needs to be sepa-
rated and returned to the inlet of the modified Claus reac-
tion furnace. This step is based on an amine absorber/
regenerator system.
The overall sulphur recovery efficiency (modified Claus
reaction and TGTU) is required and predicted to be at
99.9+%. This is confirmed by measuring the total mass
emission of sulphur dioxide (SO₂) at the exhaust of the final
thermal reactor or ‘stack’. Two points of interest for close
process control include the quench column and absorber
outlet.
Considering the AT5 quench tower outlet measurement
(H₂ and H₂S), since the TGTU process was first intro-
duced as the Shell Claus Off-Gas Treating (SCOT) process,
H2 measurement has been expected at this point. It was
included in the original system design. As previously men-
tioned, the purpose of measuring the H₂ here is to ensure
that excess H₂ is coming out of the CoMo reactor.
H₂S is also measured at this point so that operators and
the automated control system understand the amount of
H₂S that will be entering the absorber.
Sample gas measurements at this point of the process
are easier to handle than AT4 measurements at the quench
tower inlet because of the lower temperature of the process
gas. Any particulates will also have been removed in the
quench tower.
The primary measurement at the AT6 absorber outlet
H₂ and H₂S and carbonyl sulphide (COS)/CS₂ point was
defined as a single H₂S measurement to ensure the perfor-
mance of the amine absorber. By gaining knowledge about
the application and availability of multicomponent instru-
ments, additional measurements became interesting.
Knowing the importance of excess H2 in the TGTU and
recognising that an additional measured component does
not add significant cost to an analyser, a redundant H₂
measurement should be added at this point. By adding the
H₂ measurement, redundancy can be achieved without sig-
nificant extra costs.
The same can be said about adding a COS and/or CS₂
measurement; both can be used to determine the condition
of the CoMo bed catalyst. If the COS and CS₂ values are
increasing, the CoMo catalyst needs to be replaced, or other
operational variables such as flow rate or temperature need
www.digitalrefining.com
07/03/2024 17:10:23
 to be adjusted, or the modified Claus unit has some opera-
tional concern that needs to be addressed.
Looking into the combination of the two previously
described sample points, a redundant measurement of H₂
will ensure optimal performance of the TGTU. It should
reduce the cost of replacing contaminated amine and min-
imise downtime.
If H₂S is measured at the quench tower outlet and the
absorber outlet, it will be possible to measure and control
absorber efficiency online on a 24/7 basis. Process control
of the amine recycling/regeneration is also possible based
on the H₂S ‘IN’ and ‘OUT’ measurements.
The final quality control parameter is the SO₂ mass emis-
sion to be measured at the thermal oxidiser outlet. Only
mass emission can tell the true rate of sulphur recovery.
Knowing the H₂S entering the process and the amount
of SO₂ leaving the oxidiser will provide an accurate value.
Summary
Modern process instrumentation has the potential to help
reduce the emissions from an SRU.
The initial investment is not negligible, but the application
challenges are high with regard to measurement reliability
and safety aspects (the SRU has the most toxic gas mix-
tures of the entire refinery). Knowledge, understanding,
and awareness training are essential to maintain the instru-
ments; without the instrument signals, the emission targets
are not achievable.
To achieve such goals, technical disciplines must work
together, starting at the processing unit’s design phase.
Misunderstandings about piping can result in unsafe
installations.
Choosing the ‘wrong’ instrument may result in not achiev-
ing the best possible process performance. Untrained
local staff may result in instruments not working. Finally,
the average lifetime of an instrument installed in an SRU
is 15-20 years. Choosing a supplier under these circum-
stances can be challenging.
References
1 Molenaar, van Son – Worley, Keep your sulphur recovery unit online
and efficient, Sulphur Magazine, No. 408.
2 Design, safety and operational aspects of SRU analysers, CRU
Sulphur Magazine, No. 400.
Jochen Geiger is Director Sales and Service EMEA and India at
AMETEK Process Instruments, based in Cologne, Germany, and
specialising in industrial applications and instrumentation (process
analysers) in the chemical industry. He has provided training courses
on chemical plants, refineries, and oil and gas production sites around
the globe. He holds a Masters in electronics and is Process Analyser
Specialist. Email: Jochen.geiger@ametek.com
Michael Gaura is Senior Product Manager, USA at Ametek Process
Instruments USA/Canada. He holds a BS in biology and chemistry
from Purdue University and a Masters from Oklahoma State University.
Anantha Kukkuvada is Regional Sales Manager India, Sri Lanka,
Bangladesh and Africa, at Ametek Process Instruments India. He has
20 years of experience in sales and marketing in the field of analysers
and field instruments. He holds an MBA in business administration and
management from Indian Institute of Management Bangalore.

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 ‘On the fly’ vs high-performance H2S
selective solvent
A focus on highly selective designs in low-pressure tail gas treating units using
BASF’s proprietary technology in comparison to generic MDEA solutions
Ashraf Abufaris BASF Middle East Chemicals LLC
Blake Morell BASF Corporation
S
elective removal of hydrogen sulphide (H2S) has
become an important topic over the last two decades.
Selective designs are tailored either on maximum or
controlled H2S selectivity, depending on the application.
The reaction equilibrium in sulphur recovery units (SRU or
Claus section) prevents complete conversion of the sulphur
species in feed gas to elemental sulphur. Typically, an SRU with
two to three Claus reactors can only achieve 93-98% sulphur
recovery efficiency. However, higher recoveries of 99.8% and
above are achievable if the remaining sulphur compounds in
the SRU tail gas are hydrogenated to H2S, which is removed
in a selective amine unit (tail gas treating unit, TGTU).
Selection of the proper amine technology for the TGTU is
essential to make these projects economically and environ-
mentally viable. Use of a highly H2S selective solvent, such
as BASF’s proprietary OASE yellow, can provide benefits
by optimising the capital investment or reducing the oper-
ating cost.
Various parameters during the design phase influence
the H2S selectivity (and consequently carbon dioxide [CO2]
slip) in TGTUs, such as absorber height, amine circulation
rate, and absorber internals in the mass transfer zone.
However, one of the most effective levers is the amine tem-
perature itself. H2S selectivity of generic solvents rapidly
deteriorates once amine temperature exceeds 45°C. A key
benefit of the OASE yellow selective solvent is a maintained
H2S selectivity even in high ambient temperature environ-
ments and subsequent high lean amine temperatures of up
to 50°C. This avoids installing/operating costly chillers for
solvent cooling and makes the design reliable, robust, and
flexible for various operational scenarios.
Against this backdrop, key parameters for these selective
designs are discussed, followed by operational start-up
data from OASE yellow solvent swaps.
Design options to influence H2S selectivity
A number of factors influence H2S removal in the presence
of CO2. Adjusting these parameters plays a critical role in
unit optimisation throughout the design, commissioning,
start-up, and operation phases:
 Amine type
Historically, methyldiethanolamine (MDEA) has been
www.digitalrefining.com
GAS BASF.indd 17
widely used in H2S selective applications in the industry.
However, recent stricter sulphur dioxide (SO2) emission
targets that meet the World Bank standard of 150 mg/
Nm3 often require additional chemistry to further boost the
MDEA performance of other amines to achieve tight treated
gas H2S specifications. Besides the performance- related
characteristics, properties such as volatility, stability, acid
gas loading capacity, and of course commercial aspects are
important selection criteria.
 Lean amine temperature
Selective treatment with amine-based solvents generally
takes advantage of the rapid reaction of H2S compared to
the kinetically hindered reaction of CO2: CO2 first must react
with water to form carbonic acid before the solvent can
absorb the CO2. Thus, tertiary amines such as MDEA are
often used for selective applications as they cannot form
carbamates (the only fast reaction with CO2).
The following reactions of tertiary amines take place in
aqueous solutions:
Reaction of water and amine (fast)
R1R2R3N + H2O  R1R2R3NH+ + OHˉ
2 H2O  H3O+ + OHˉ
H2S reaction (fast)
H2S + H2O  HSˉ + H3O+
CO2 reactions (overall reaction: slow):
CO2 + 2H2O  HCO3ˉ + H3O+ (slow)
HCO3ˉ + OHˉ  H2O + CO32- (fast)
In this reaction system, CO2 co-absorption and, thus, H2S
selectivity are heavily influenced by reaction conditions. This
means higher pressure and temperature, as well as a higher
CO2/H2S ratio in the feed gas, favour CO2 co-absorption and
lower H2S selectivity, especially at lean amine temperatures
above 50°C, which are typical for the Middle East region.
The CO2 reaction accelerates and strongly competes with
the H2S reaction. As a result, a cooling system/chiller is often
part of the design in these climates to achieve H2S selectiv-
ity with an MDEA/acidified MDEA solution.
 Mass transfer
Besides lean amine temperature and feed gas pressure
Gas 2024 17
08/03/2024 09:42:42

Generic amine
H2S selectivity
MDEA
Promoted MDEA
High
Low Lean amine temperature range
Figure 1 Selective solvent performance comparison
(partial pressure), absorber internals, column height, and
liquid/gas (solvent/feed gas) ratio all strongly affect the
total mass transfer of individual components from the gas
into the liquid phase. While the mass transfer of H2S is
predominantly gas-phase driven, CO2 reaction kinetics are
mostly related to resistance in the liquid phase. Absorber
height and mass transfer surface determine vapour/liquid
contact, which directly impacts reaction selectivity. The liq-
uid/gas (solvent/feed gas) ratio itself not only impacts mass
transfer but also influences the temperature profile within
the absorber, impacting reaction kinetics.
Selecting the right solvent
While designing a TGTU, one of the most important deci-
sions is the type of amine. A typical gas sweetening amine
unit with primary or secondary amines such as monoetha-
nolamine (MEA) or diethanolamine (DEA) would require a
very high amine circulation rate, as these solvents absorb
both H2S and CO2 almost without selectivity towards H2S.
For this reason, a more H2S selective amine must be con-
sidered to reduce solvent circulation/inventory, the amount
of CO2 recycled to the SRU, and reboiler duty.
Figure 1 illustrates a comparison between generic
amines such as MDEA and acidified MDEA against propri-
etary amines offered by BASF Gas Treating (OASE yellow
and Flexsorb SE Plus).
OASE yellow was developed to enable selective removal
of H2S in both high (natural gas) and low-pressure
100
90
H2S spec treated gas (ppmv)
80
70
60
50
40
30
H2S spec
20
Amine circulation rate (%)
10
0 TGTU feed gas: H2S 1.2%v, CO2 30%v
Conversion within 72 hours
Figure 2 Case study 1 OASE yellow conversion results
18 Gas 2024
GAS BASF.indd 18
applications (acid gas enrichment or tail gas treatment). The
proprietary combination of several amines and a promoter
Proprietary amine system provides higher acid gas capture capacity and ena-
Flexsorb SE Plus
bles lower achievable treated gas H2S specifications.
OASE yellow Flexsorb SE Plus is a proprietary gas treating agent
developed by ExxonMobil Research and Engineering
Company specifically for selective H2S removal. The tech-
nology is well known in the industry for its high perfor-
Energy demand Low mance, even at high ambient temperatures. The selectivity
High advantage allows H2S removal at lower solvent circulation
rates, resulting in lower energy consumption compared to
conventional processes. The reliable and simple-to-operate
process is characterised by low corrosion and lower foam-
ing compared to conventional gas treating solvents. The
technology has a commercially proven track record since
1983, with more than 140 reference plants.
Both OASE yellow and Flexsorb SE Plus can achieve
high treated gas purity to meet the stricter SO2 emission
targets of the World Bank Standard (150 mg/Nm3). In addi-
tion, both solvents can maintain H2S selectivity at high lean
amine temperature (+50°C), which makes designs without
an expensive chiller unit possible. On the contrary, generic
amines would need high energy demand and lower lean
amine temperature to achieve the required H2S selectivity,
which increases the unit’s costs significantly.
Case study 1: Switching from MDEA to OASE yellow
In this case study, a refinery located in Germany operated a
TGTU with generic MDEA solvent, which often limited the
refinery’s operations. The feed gas to this unit includes 1.2
mol% H2S and 30 mol% CO2. The constraint encountered
at the TGTU is the environmental permit limit for SO2 emis-
sions from the thermal oxidiser. This environmental con-
straint typically occurred in the summer months due to an
increase in the lean amine temperature in the TGTU. As the
lean amine temperature approached 37.8°C, the amount of
H2S that slipped to the thermal oxidiser increased signif-
icantly, resulting in increased SO2 emissions. To mitigate
this increased emission during the summer, the overall SRU
capacity needed to be limited, even with the use of rented
chillers.
These factors warranted a review of alternative technol-
ogies and a solvent changeover. However, the refinery had
100 already passed the turnaround period, and the operation
90 team had the challenge of changing over the solvent while
the unit operated ‘on the fly’.
Amine circulation rate (%)
80
As part of this evaluation, BASF was requested to ana-
70
lyse the possibility of utilising OASE yellow in this unit to
60
reduce the treated gas H2S content during the summertime
50
from 90 ppmv to 35 ppmv. OASE connect, an in-house
40
rate-based model simulator, was used to assess the possi-
30
bility of meeting this target without any mechanical modifi-
20 cations to the existing equipment.
10 Based on the simulation results, it was concluded that
0 with the addition of the OASE yellow enhancer system to
the existing MDEA inventory, meeting the H2S target was
not only possible but also the unit could reduce the solvent
circulation rate to approximately 65% of the current oper-
ating level.
www.digitalrefining.com
08/03/2024 09:42:44
 TGTU feed gas: H2S 6.8%v, CO2 3.5%v TGTU feed gas: H2S 6.8%v, CO2 3.5%v
200 H2S spec 100 200 16
Amine circulation rate (%)
90
175 Reboiler steam (t/h) 175 14

Reboiler duty steam rate (t/h)

H2S spec treated gas (ppmv)

H2S spec treated gas (ppmv)

Amine circulation rate (%)
80 Max H2S spec
150 150 12
70
125 60 125 10

100 50 100 8
40
75 75 6
30
50 50 4
20
H2S spec
25 10 25
Reboiler steam (t/h) 2
0 0 0 0

Conversion within 26 hours Conversion Optimisation

Figure 3 Case study 2 OASE yellow conversion results Figure 4 Case study 2 optimisation

By switching from MDEA to OASE yellow, the refinery’s resulted in an annual Opex savings of approximately $1
annual average sulphur capacity increased, which allowed million for the unit.
it to run additional sour crude. In addition, it was no longer
necessary to rent chillers to cool the lean amine, leading to Conclusion
considerable operating cost savings. The selective removal of H2S has become an important
Figure 2 illustrates the actual performance test results topic over the last 20 years. With dwindling sweet gas
collected from the unit during the 72-hour swap process. reserves, H2S selective gas treatment at low pressure (acid
With the stepwise addition of the OASE yellow enhancer gas enrichment, tail gas treatment, or a combination of
system, a noticeable decrease of the H2S at the outlet of the the two) has become necessary to produce a high-quality
unit absorber (red dots) was observed. The solvent circula- Claus gas, enabling sulphur removal and monetisation of
tion rate was able to be reduced at the same time, resulting these gas fields.
in operational cost savings for the unit. Savings in energy and circulation rate (Opex), as well as
a reduction in equipment sizing (Capex), are the obvious
Case study 2: Switching from acidified MDEA to benefits of enhanced H2S selective treatment. Even more,
OASE yellow many of the newest projects require a high degree of oper-
In this case study, a refinery located in South Korea oper- ational flexibility combined with a robust operation in warm
ated a TGTU with acidified MDEA. The feed gas to this unit locations enabled by these technologies.
includes a higher H2S content compared to the previous Capacity, operational flexibility, reliability, and the ability
case, with 6.8 mol% H2S and a lower CO2 content of 3.5 to achieve specifications are all considered during BASF’s
mol%. This study aimed to reduce steam consumption technology selection process, utilising the in-house simula-
while maintaining the environmental permit limit for SO2 tion tool, OASE connect.
emissions from the thermal oxidiser. Similar to the previous OASE yellow technology utilising the most common
unit, the changeover from acidified MDEA to OASE yellow selective base amine, MDEA, allowed for smooth swaps
had a constraint to be done during the unit operation with- from generic solution to meet the stricter emission limits
out shutting down the process. and optimise the unit operational costs. The technology
BASF completed a study considering the unit’s mechani- can also be utilised in grassroots designs to achieve further
cal details and concluded that it was possible to reduce the savings on the capital investment of these projects, making
H2S content from 150 ppmv to 25 ppmv, maintaining the them economically more attractive and feasible.
current steam consumption to the unit. In turn, the steam
consumption could be reduced by 35% while still meeting OASE is a trademark of BASF, and FLEXSORB SE PLUS is a trade-
the unit’s environmental limits. mark of ExxonMobil.
Figure 3 illustrates the first step of the conversion with
the actual performance test results collected from the unit Ashraf Abufaris is Senior Technical Market Manager Middle East
during the 26-hour swap process. As the OASE yellow and gas treatment expert at BASF Middle East Chemicals LLC in Abu
enhancer system was added to the system, the treated gas Dhabi, UAE. He presented on the effectiveness of BASF’s H2S selec-
H2S content decreased even as the circulation rate was tive removal technologies in hot climates at the 28th International
reduced by 25%. Conference and Expo ‘Oil and Gas of Turkmenistan’ held in Ashgabat.
In the second step (see Figure 4), steam consumption was
reduced by 35%, allowing H2S concentration to increase to Blake Morell is Technical Market Manager at BASF Corporation in
the acceptable limit of 150 ppmv. This steam rate reduction Houston, Texas, USA.

www.digitalrefining.com Gas 2024 19

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 Steam methane reformer tube
lifecycle improvement best practices
Reformer tube life assessment can be done via online monitoring, non-destructive
testing, and tube harvesting with historical operating, monitoring, and inspection data
Richard D Roberts and Grant Jacobson
Becht
S
team methane reformers (SMRs) are an integral asset
operated globally within methanol, hydrogen, ammo-
nia, and direct reduced iron (DRI) plants. Providing
plant owners/operators with the ability to extend tube life
within the steam reformer is essential in maximising the use
of an owner’s capital investment. Most of the tube’s material
content is made up of nickel, ultimately driving the overall
economics of fabrication. The cost of purchasing and install-
ing a single reformer tube can be upwards of USD 25,000.
However, in today’s highly competitive markets, the effect of
unplanned downtime in reducing the plant on-stream factor
is far greater than the installed cost of a single reformer tube.
It is essential that plant engineers have access to highly
accurate online monitoring and inspection data, allowing
them to better manage the reformer tubes and, where cir-
cumstances allow, extend the tube life expectancy beyond
the typical prescribed life expectancy. One hundred thou-
sand operating hours is a typical design life guideline prac-
tice used by furnace design engineers.
Today, plant owners and tube manufacturers have
become accustomed to inspecting tubes with
the latest technologies, even before they ship
from the tube fabrication facility. This proactive
approach enables quick detection and quantifi-
cation of manufacturing flaws, enabling repairs
to be made if necessary. Additionally, this early
inspection approach provides plant owners with
‘baseline’ inspection data for future use over the
life of the tube.
Tube inspection instrumentation technolo-
gies often apply non-destructive testing (NDT)
methods such as laser profilometry (LT), eddy
current (ET), ultrasound (UT), radiography
(RT), and electromagnetic acoustic transducer
(EMAT). Each method has its strengths and
weaknesses. Therefore, some instruments have
coupled two or more NDT methods to maximise
the accuracy of test result outputs and inspec-
tion area coverage.
QA/QC and ‘baseline’ inspections
Both internal and external inspection approaches
(see Figure 1) can be utilised to facilitate QA/ Figure 1 Internal and external inspection methods
www.digitalrefining.com
Becht.indd 21
QC screening at the tube manufacturing facility. Internal
inspection methods tend to be preferred as they allow
the tubes to be stacked on top of one another in the hori-
zontal orientation, thus requiring a small footprint within
the facility. External methods require tubes to be spread
out to allow for adequate space around the exterior, thus
requiring a much larger space to carry out the inspections.
Both approaches often apply one or more of the previously
described NDT methods.
Conducting QA/QC inspections prior to the tubes being
shipped from the manufacturer’s facility allows necessary
repairs to be made in advance of shipping and often tight
installation deadlines. Flaws such as dimensional over-bor-
ing, machine gouges, and excessive weld-root penetration
are damages that may reduce tube life downstream if not
addressed prior to placing into service.
Data collected as part of the QA/QC inspection can also
be archived as ‘baseline’ data and applied during future rou-
tine inspections. Even tubes fabricated well within design
tolerances naturally contain variations within the internal
bore dimension. Precise bore dimensions
can be obtained and documented during
this exercise. Future routine inspections
can leverage these dimensional data rather
than applying design values. This approach
ultimately produces much more precise
creep strain monitoring over the life of the
tube, which directly impacts the accuracy of
remaining life assessment calculations.
Gas 2024 21
08/03/2024 16:18:27
 dI 2πhc2 Φobject = ε x σ x T4
R (λ,T) = = T1 = 5500˚K (sun)
dλ λ5(e hc/λkT –1) T2 = 4500˚K (Stefan-Boltzmann equation)
T3 = 3000˚K (light bulb)
1.8E14 T1 The rainbow area represents the
sensitivity of the human eye Target object Atmosphere
1.6E14
Total power P radiated from a black
object with surface area S heated to
1.4E14 temperature T is:
∞
1.2E14 P = S∫R(λ,T)dλ = σST4
R (λ,T) [W/m3]

1.0E14 2π5k4
σ= = 5.67 x 10-8 [W/m2K4]
15h3c2
(Stefan-Boltzmann law)
ε
8.0E13
T2 At any temperature T the wavelength λ max
6.0E13 corresponding to the peak is: Camera
hc 2.898 x 10-3
4.0E13 λ max = = [m] Background
5kT T
(Wien’s displacement law)
2.0E13
T3
0.0E0 Φtotal = ε x τ x Φ(T)object +(1–ε) x τ x Φ(T)background +(1–τ) x Φ(T)atmosphere
0 10-7 2 3 4 5 10-6 2 3 4 5 10-5 2 3
Wavelength λ [m]

Figure 2 Planck’s Radiant Function and Stefan-Boltzmann equations

‘Online’ monitoring techniques troubleshoot real-time performance issues. Pyrometers

Infrared (IR) technology has been used as an ‘online’ temper-
also require adherence to well-written procedures to
ature monitoring approach within steam reformers for many maintain the accuracy and consistency of the temperature
decades. IR is a non-destructive, non-intrusive, non-contact
measurements.
method for mapping thermal patterns on the surface of An effective IR program is an absolute necessity to mon-
tubes and refractory within the reformer during operation.itor the steam reformer tubes, as well as provide a wealth
Understanding the tube metal temperature defines the per- of diagnostic information that may be used to evaluate the
formance capability and inherent reliability of the reformer
performance and reliability of other reformer components
and, ultimately, the risk of a tube rupture failure. (tubes, tube supports, burners, and refractory).
IR is accomplished with two primary instrument types, Radiation signals are strong functions formed from many
such as thermal imaging cameras and pyrometers. The sources within an operating reformer. Planck’s Radiant
thermal imaging camera forms a two-dimensional ther- Function and the Stefan-Boltzmann equations set the the-
mal image of the target surface, while the pyrometer oretical foundation for these temperature measurements
provides only a single target point temperature. Each (see Figure 2). The complexity of the measurement envi-
instrument has advantages and disadvantages, and effec- ronment, coupled with differing materials that change over
tive programs will apply both to leverage the strengths. time, makes accurate temperature measurements difficult
The imaging camera provides meaningful images and but possible with technical know-how and properly applied
measurements for a historical record, which can be used measurement techniques.
to assess tube creep damage rates and long-term perfor- To confirm temperature measurements in a reformer, a
mance changes. The pyrometer should be used for accu- contact pyrometer, aka ‘Goldcup’ (see Figure 3), can be
rate field measurements to compare specific tubes and used. This water-cooled tool allows temperature meas-
urements to +/-2°C of mid-wall
temperature when properly
applied. To maintain data accu-
racy, one must be very cautious
about properly calculating the
cooling effect via shielding and
contact by the Goldcup when
in use. After a field survey of a
reformer with a Goldcup, these
in-situ temperature calibration
locations can be used to improve
the measurement accuracy of
easier-to-field tools (IR cameras
and pyrometers). With proper
procedures and training, the
basic optical pyrometers can
approach the Goldcup accu-
Figure 3 Goldcup tool for mid-wall temperature measurements racy after correction factors are

22 Gas 2024 www.digitalrefining.com

Becht.indd 22 08/03/2024 16:18:30

 4.25

Baseline - 1993 Tube A - 2000

4.20 Tube A - 2004 Tube A - 2006
Comparison location
Inside diameter (in)

4.15

4.10

4.05

4.00

3.95
0 50 100 150 200 250 300 350 400 450 500
Tube length (in)

Figure 4 NDT inspection methods

applied via the data sets obtained with the Goldcup and
proper procedures with training are implemented for the
pyrometer use.
‘Offline’ inspection methodologies
During routine plant shutdowns, ‘offline’ tube inspections
can be facilitated. Whether the catalyst is being extracted
from the tubes or not will dictate which internal or external
inspection option can be applied. The internal approach can
only be applied once the tube is fully evacuated of cata-
lyst and preferably the catalyst support cone (if present)
at the bottom of the tube, providing access to the full tube
length, top flange to bottom cone or flange, depending
upon tube design.
Inspections facilitated from the tube interior surface
while applying an internal probe mechanism often provide
more accurate test results, as the internal bore of the tube is
machined smooth with tight profile tolerances, as opposed
to the rough ‘as cast’ exterior tube surface profile. The full
tube length can also be accessed from the tube’s interior
bore. Often, many obstructions near the tube’s exterior,
such as floor and roof refractory penetrations and narrow
tunnel walls, limit an external crawler’s travel, ultimately
leaving a portion of the tube uninspected where obstruc-
tions exist.
Leveraging inspection results
The amount of inspection data collected with today’s
instrumentation technologies can be overwhelming if not
managed correctly. Complex software has become essen-
tial, allowing scrutiny of individual tubes and the ability to
combine data from all tubes into one image. Overlaying the
combined data sets onto one viewing platform is powerful
in discerning general damage patterns well in advance of
experiencing unexpected localised or broad area failures.
Producing inspection results quickly while a steam reformer
is offline enables engineers to focus on necessary repairs or
modifications quickly prior to the asset being brought back
online. For example, a partially collapsed tunnel may result
in localised elevated temperatures, ultimately accelerating

1 1. Primary creep 2 3
Macrocracking
2. Secondary creep
3. Tertiary creep

Microcracking
Strain

Steady-state Aligned cavities

creep rate

Isolated cavities

Time

Figure 5 Tube failure prediction

www.digitalrefining.com Gas 2024 23

Becht.indd 23 08/03/2024 16:18:32

 www.zwick-armaturen.de

p24 Zwick.indd 1 07/03/2024 16:46:37

 100000
10 years
10000
1 year
Life time (hours)
1000
1 month
100
1 day
10
1
1750
Metal temperature (˚F)
Figure 6 Lifetime vs metal temperature chart and illustration explaining creep damage progression through a tube wall
tube damage. As the 3D image highlights, plant engineers
can see the beginning of damage patterns and address
what is needed.
It is essential that NDT inspection methods applied
produce repeatable results, starting from the baseline to
ongoing routine inspections (see Figure 4) and from one
inspection period to the next. Repeatable results allow
data to be overlaid, enabling quantification of damage level
increases and highlighting shifting of damaged area.
Remaining tube life complexities
Provided the NDT inspection technique(s) applied can
generate adequate discrimination, the inspection test
results can also be used to determine the remaining tube
life and, therefore, decide the time at which the tubes need
replacing.
Some inspection techniques simply package test results
into A, B, C, and D type categories, which do not provide
sufficient detail nor consider the wide scatter of damage
throughout a reformer furnace with respect to tube damage.
Even ignoring the variables in the tube operating environ-
ment, some tubes will fail before the expected design life
(see Figure 5). This is primarily because the design meth-
odology utilises a probabilistic approach based on analysis
of controlled short-term destructive testing of tube sam-
ples. In most cases, 95% of tubes will exceed the design life
– this means that 5% of the tubes will not reach design life.
www.digitalrefining.com
Becht.indd 25
Maximum operating
temperature of 1750 ˚F
= 10 years life time
Never operate
above
1850 1950 2050
Unfortunately, when it comes to predicting which tube
may fail first in a reformer, variation in tube life is a fact of
life due to the following factors:
• Wall thickness variations within manufacturing specifica-
tions and design tolerances.
• Material property variation in chemistry and macrostruc-
ture between each tube section.
• Temperature variation due to reformer design, flue gas flow
plus uncertainty, and errors in temperature measurement.
The latter factor is particularly important as relatively
minor differences in temperature have a significant impact
on tube life. Typically, a 68ºF (20ºC) increase in tube tem-
perature will reduce the life by as much as 50% (see Figure
6). This continues to stress the importance of focusing on
accurate temperature measurements while online by an
owner/operator or trusted contractor.
Tube harvesting
Applying a tube harvesting approach allows plant operators
to focus replacement efforts towards those tubes where
operating life has been consumed beyond acceptable tol-
erances. In many steam reformer designs, there are cooler
regions within the firebox where tube temperatures rarely
reach material creep strain thresholds. Therefore, operating
life will exceed other tubes operated in regions of higher
temperatures. Applying a tube harvesting approach allows
plant operators to spread capital expenditures over time
Gas 2024 25
08/03/2024 16:20:57
 90

80

70

60 10 out of 352 tubes

Tube count

50

40

30

20

10

0
0
2
4
6
8
1
2
4
6
8
2
2
4
6
8
3
2
4
6
8
4
2
4
6
8
5
2
4
6
8
6
2
4
6
8
7
0.
0.
0.
0.

1.
1.
1.
1.

2.
2.
2.
2.

3.
3.
3.
3.

4.
4.
4.
4.

5.
5.
5.
5.

6.
6.
6.
6.
Percentage expansion

Figure 7 Tube harvesting graph

rather than replacing all tubes at the same time, regardless
of the severity of damage (see Figure 7).
To apply an effective tube harvesting program, the NDT
inspection method applied must produce quantitative test
results. Simply bundling the tubes into A, B, C, and D type
categories does not provide enough detail to adopt a har-
vesting strategy. Ideally, each tube should be ranked, and
then a histogram should be applied to determine where
tube replacement thresholds are set. Integrating availa-
Performing baseline QA/QC
inspections proactively at the tube
manufacturing facility provides a
means to ensure the quality of tube
fabrication prior to shipping and
installation
ble temperature measurement data into this process also
helps prioritise where to harvest and test for damage. It is
easy to perform destructive testing on the correct tube but
incorrect elevation on the tube if temperature data is not
integrated into this effort.
Conclusion
Performing baseline QA/QC inspections proactively at the
tube manufacturing facility provides a means to ensure the
quality of tube fabrication prior to shipping and installation,
in addition to collecting important baseline data for future
comparison during routine inspections once they are placed
in service. Failure to do so may result in installing tubes that
contain manufacturing flaws, in addition to reducing the
accuracy of future inspection data comparisons.
Once tubes have been installed and placed into service,
routine tube skin monitoring is critical. It is imperative that
plants develop and maintain a temperature monitoring
program. This frequently requires a combination of tech-
nologies (infrared imaging and pyrometer with Goldcup) to
verify the accuracy of temperature data.
Time interval periods between planned reformer shut-
downs are critical. Often, trends are to extend plant shut-
downs as far out as possible, mainly due to economic
drivers. For a nominal 100,000-hour (11.4 years) design life
and a shutdown cycle of four years, the tubes can only be
inspected at year zero (baseline), year four, and year eight
before some may require replacement. To plan for this, the
plant owner will only have the year four data on which to
base critical replacement decisions. Therefore, the inspec-
tion technique(s) applied must produce quantitative test
results and be sensitive enough to assess all tubes at this
early stage. Qualitative inspection techniques that produce
results report ranking tubes in ‘good’, ‘moderate’ or ‘poor’
condition (A, B, C, and D) are of little value.
Remaining life assessment approaches should have the
ability to apply historical operating, monitoring, and inspec-
tion data. Combining remaining life assessment calculation
analysis with a tube harvesting program provides plant
engineers with a step up in maximising the operating life
of tubes in addition to spreading out capital spend. Becht
partners with owner-operators to establish such programs,
ensuring online monitoring data and inspection data ben-
efits are maximised over the life of the steam reformer’s
tube network.
Richard D Roberts is Inspection and Fixed Equipment SME at Becht.
He holds a BS in mechanical engineering from Ohio State University.
Grant Jacobson is Division Manager, Fired Heater Services Division
at Becht. He holds a BS in chemical engineering from University of
Nebraska-Lincoln.

26 Gas 2024 www.digitalrefining.com

Becht.indd 26 08/03/2024 16:21:08

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 Testing and effects of pipeline
chemicals on gas processing facilities
Minimising, replacing, and properly using pipeline chemical additives causing foaming
and/or solids formation will alleviate detrimental effects in amine and glycol units
David Engel and Scott Williams
Nexo Solutions
C
hemical additives used upstream of processing facil-
ities are often a root cause of detrimental effects
in amine and glycol dehydration units, such as sol-
vent foaming, chemical poisoning, and equipment fouling,
among others. For this reason, a study was conducted to
understand the behaviour of various chemical additives
when contacted with an amine solvent.
A total of 65 commercially available pipeline and upstream
chemical additives commonly used upstream from process-
ing facilities were received and reviewed in terms of their
safety data sheet (SDS) documentation. Each chemical sam-
ple was contacted with lean amine solvent (methyldietha-
nolamine [MDEA] 50% in water) at ambient and elevated
temperatures. To assess the chemical compatibility of each
additive with the amine solvent, the outcome of a series of
tests was observed in terms of foam formation, solid forma-
tion, and colour changes.
Figure 1 shows the various chemical additive experiments
when contacted with the lean amine solvent and incubated
at 60°C for five hours under atmospheric conditions. Table
1* describes the samples as labelled, named according to
each SDS (as received), and numbered for future reference.
The observed colour of each additive and the supplier were
also listed. Compositional information was reviewed for
each sample but is not listed in this discussion because of
the extensive number of samples and components in each
chemical additive and the fact that most compositions were
proprietary and not indicated in the SDS documentation.
Bottle testing and results
Bottle testing of each chemical additive was performed by
adding 0.5 ml of each additive to 10 ml of fresh lean amine
provided in 40 ml sealed vials. This is essentially 5% con-
centration by volume. Each vial was properly mixed after
the addition of the chemical additive to the amine solvent.
Pictures were taken starting in one hour after mixing into
the tenth day. Higher chemical additive concentrations were
used to exacerbate their effects and differentiate results.
Unheated samples
Each vial was observed after 24 hours to determine if any
phase separation had occurred, and several characteris-
tics of each sample were then recorded. The results of the
28 Gas 2024
Nexo.indd 28
Figure 1 Chemical additives contacted with lean MDEA
solvent and incubated at 60°C for five hours
testing for all 65 samples are listed in Table 2.* The foaming
tendency, phase separation, solids precipitation, opacity,
and colour of each sample were recorded.
Of the 65 pipeline and upstream chemical additives
tested with lean amine solvent, 39 displayed some degree
of foaming tendency. Twenty-eight chemical additives dis-
played a significant amount of foam with stability, and 11
displayed a high to severe foaming. Twenty-nine samples
displayed some degree of liquid phase separation, as those
additives were partially or completely insoluble in the amine
solvent. Eight chemical additives exhibited solids precipita-
tion, presumably due to chemical or physical incompatibil-
ity between the formulation components and lean amine
solvent. Forty chemical additives were observed to have a
significant amount of haze present after agitation due to
emulsification and solids dispersion.
Heated samples
The chemical additives samples with the lean amine sol-
vent were then placed in a water bath and heated to 60ºC
for approximately five hours. The samples were allowed to
cool over the course of 24 hours. Each vial was observed
to determine if any phase separation occurred. During the
test, several characteristics of each chemical additive sam-
ple were recorded. The results of these 65 test samples are
in Table 3.* The foaming tendency, phase separation, solids
precipitation, opacity, and colour of each test were recorded.
Of the 65 chemical additives tested with lean amine
solvent, 43 displayed some degree of foaming tendency.
Twenty-eight chemical additives displayed a significant
amount of foam with stability, and 13 displayed a high to
severe amount of foaming. Twenty-three chemical additives
www.digitalrefining.com
07/03/2024 17:33:02
 samples displayed some degree of liquid phase
separation, as those chemical additives were
partially or completely insoluble in the lean amine
solvent. Nine samples exhibited solids precipita-
tion, presumably due to chemical incompatibility
between the formulation components and lean
amine solvent. Forty-one chemical additive sam-
ples were observed to have a significant amount
of haze present after agitation due to effects
including emulsification and solids dispersion.
The observed effects of each chemical addi-
tive sample heating (in comparison to unheated
sample characteristics and 24-hour cooling)
were not significant in most cases, as only sam-
ple characteristics changed. Solids precipitation
was observed in one additional chemical addi-
tive sample after heating. Sample opacity was Figure 2 Image analysis of lean amine solvents with various chemical
largely unchanged.However, some chemical additive samples in terms of compatibility and colour change at: left:
additive samples slightly clarified or became a lit- room temperature and right: at 60ºC for five hours. Red squares show
tle hazier. Some samples were observed to have the samples that changed colour upon heating. Samples 1, 11, 19, 21,
slightly changed foaming tendency after heat- 38, 40, and 51 showed a marked colour change upon heating
ing, but most chemical additive samples were
unchanged. The most significant change in characteristics after heating at 60°C for five hours.
was liquid phase separation; six chemical additive samples From exposure to the various process additives at room
were observed to have dissolved their discontinuous phase temperature, the colour changes in the amine solvent were
after heating and cooling time. clearly visible. The samples with an inner ring contour, grey
colour, are indicative of no changes to the transparency
Additive analysis of the amine upon addition of the process additive. Some
The complete analysis shows that about 75% of the chem- samples still show the inner ring, but there is a slight colour
ical additives tested resulted in some form of observed change. This indicates that the sample has changed colour
incompatibility. Some chemical additives displayed a but is still transparent. The other samples where the inner
greater degree of incompatibility compared to others, and ring is not visible indicate that the samples changed in colour
continued use of those products with significant incompat- and became opaque (hazy) or presented a separate phase.
ibility should be replaced. At least 12 chemical additives About 50% of the samples turned the lean amine solvent
presented moderate to severe foaming tendency of the lean opaque (30 chemical additives), and five additives changed
amine solvent (see Tables 2 and 3)* and should be recon- the solvent in colour but did not cause the mixture to become
sidered and re-evaluated for use or potentially replaced. opaque. In addition, seven samples indicated by the red
Additionally, eight chemical additive samples showed squares changed colour upon heat exposure. Samples 1,
solids precipitation when contacted with lean amine sol- 11, 19, 21, 38, 40, and 51 showed a marked colour change
vent, and 23 chemical additive samples generated liquid difference after heating. These evaluations are only visual
phase separation (see Tables 2 and 3).* All these products observations and were used in combination with the other
should be reconsidered for use or potentially replaced. Any observations, such as solids formation and foam stability.
samples with severe haziness or complete opacity should
be reconsidered for use or also potentially replaced. Foam-inducing chemical additives
A total of 42 chemical additives produced lean amine sol-
Compatibility image analysis vent foaming, as shown in Table 4.* The products marked
To gain an understating from a visual perspective of each in red generated severe foaming. Figure 4 shows the seven
chemical additive and their effect to heat exposure, chem-
ical additive samples 1-61 containing the lean amine sol-
Empty 54 45 36 27 18 9
vent and the chemical additive samples were scanned from Control 53 44 35 26 17 8
the bottom of the glass vial and analysed by their visual 61 52 43 34 25 16 7
properties (see Figure 2). The vial array codification related 60 51 42 33 24 15 6
to the various additives is indicated in Figure 3. Samples 59 50 41 32 23 14 5
58 49 40 31 22 13 4
highlighted in red in Figure 2 show a marked colour change 57 48 39 30 21 12 3
upon heating. 56 47 38 29 20 11 2
The section and colouration of the various additives when 55 46 37 28 19 10 1
contacted with the lean amine solvent are shown in Figure
2. The section on the left shows the mixtures at room tem- Figure 3 Position codification of chemical additives
perature, and the image on the right shows the mixtures contacted with lean amine solvent

www.digitalrefining.com Gas 2024 29

Nexo.indd 29 07/03/2024 17:31:56


Figure 4 Chemical additives with severe foaming. Top,
from left to right: samples 7, 23, 26, 34, 42, 50, 57 before
agitation. Bottom, from left to right: after agitation (+1 min)
samples highlighted in the table with severe foaming ten-
dency. It was recommended that these seven additives be
considered for replacement or replaced.
Foaming tendency in methanol samples
It must be noted that two out of five methanol samples were
found to have foaming tendency. Methanol-based additives
should not foam as they are used primarily as hydrate inhib-
itors and should not contain any surfactant components in
their formulation.
Methanol is used for hydrate inhibition and other applica-
tions, and in general should not produce foam. The meth-
anol-based additives with foaming tendency were Sample
11 (Indigo RSI Methanol) and Sample 17 (Methanol Indigo
17). It is recommended that these additives should be
re-evaluated before further use or replaced.
The number of process additives causing solids formation
was far lower compared to the process additives causing
foam stabilisation. Most of the solids formed were amber to
brown in colouration. The chemical additives that generated
solids upon contacting the amine solvent may cause solids
formation if they reach the amine unit. These products were
recommended to be removed prior to entering the plant or
replaced.
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30 Gas 2024
Nexo.indd 30
Figure 5 Samples with solids precipitation in lean amine
solvents (from left to right: Sample 4, 15, 18, 19, 22, 43,
51). Samples 63, 65 not shown
Solids-forming chemical additives
Table 5* describes the chemical additives that caused sol-
ids formation when contacted with the amine solvent, and
Figure 5 shows seven of the nine samples visually.
The number of process additives causing solids formation
was far lower compared to the process additives causing
foam stabilisation. Most of the solids formed were amber to
brown in colouration. The process additives that generated
solids upon contacting the amine solvent may cause solids
formation if they reach the amine unit. These products were
recommended to be removed prior to entering the plant or
replaced.
Concluding remarks
From the perspective of the chemical additives used
upstream of gas processing plants, a total of 65 products
were evaluated in terms of their lean amine solvent com-
patibility. The evaluation was partially based on colour
changes once the chemical was contacted with the amine
solvent. In addition, foaming tests and solids formation
were also verified. These tests were performed with and
without heat (60°C for five hours) and agitation. Only seven
chemical additives changed colour during heat treating.
Of the total 65 chemical additives tested, about two-
thirds (42 out of 65) caused lean amine solvent foaming in
different degrees. A total of seven chemical additives gen-
erated severe foaming and should not be used in the pro-
cess or anywhere upstream (see Figure 6). Eight products
induced solids formation when exposed to the lean amine
solvent and should also be avoided in both the process and
upstream. Most of the chemical additive products tested
were miscible in the lean amine solvent. However, 23 gen-
erated a separate phase or emulsion formation.
www.digitalrefining.com
07/03/2024 17:32:03
 Severe foaming
7 (10%)

Minimal to no foaming
23 (32%)

Foaming
42 (58%)

OUR BALL VALVES GO

BEYOND THIS DISPLAY
Figure 6 Foam tendency of the tested samples

It is generally difficult to accurately identify specific chem-

AND YOUR
...
icals that cause detrimental effects in processing facilities
such as amine or glycol units. However, minimising and
EXPECTATIONS!
properly using the products causing foaming and/or solids
formation will alleviate detrimental effects. In some cases,
total replacement is necessary.
Correct application of these products is also critical so
1/8’’ - 56 ‘‘
that no unused or excess chemical is entrained in the inlet
gas entering processing plants. In terms of mitigation, com-
plete removal of chemicals entering the process via the inlet
gas is likely not possible. Therefore, strict practices and
provisions need to be in place to ensure minimal contam-
CLASS 2500
ination ingression with the inlet gas. These practices and AND HIGHER
provisions include:
u Water wash of the inlet gas using a highly effective
water injection and extraction methods.
 Install correctly designed gas filtration for solids removal
from the inlet gas. OIL, GAS,
HYDROGEN,
 Install correctly designed liquids coalescing for liquids DISTRICT ENERGY
removal from the inlet gas. & VARIOUS
APPLICATIONS
 Use proper high-efficiency elements (internals) with
proper seals in both the inlet gas filter and coalescer.
 Test for oxygen ingression with the inlet gas and mini-
mise its presence if detected.
 Ensure proper regeneration of the amine solvent to avoid
possible cross-reaction with any contaminant entering the
process and to minimise solvent thermal degradation.
*All tables are available from the authors and included on the digital
version of the article on DigitalRefining.com.

Disclaimer
Nexo Solutions received samples and SDSs of the various chemical
additives from processing facilities for the specific objective of testing
chemical compatibility with process solvents. None of these chemicals
were tested or analysed for material composition or molecular types.

David Engel is Managing Director at Nexo Solutions. He has more than

25 years of industrial experience in various areas, including chemical
synthesis, oil and gas, analytical methods, membranes, chemical addi-
tives, process chemistry, and process separation technologies. He has
been awarded almost 21 patents and authored more than 100 papers
and seminars. He holds a PhD in organic chemistry from Indiana
University Bloomington. Email: david.engel@nexosolutions.com
Scott Williams is a Process Engineer, responsible for research and
development, engineering, marketing, and sales at Nexo Solutions
based in The Woodlands, Texas. He holds a BS in chemical and bio- www.boehmer.de
logical engineering from University of Colorado at Boulder.

www.digitalrefining.com Gas 2024 31

Nexo.indd 31 08/03/2024 16:35:28

 Hydrogen recovery from refinery
off-gas – Part 1: An overview
Using next-generation hydrogen separation membranes to recover unused
hydrogen wherever possible
Zach Foss
Divigas
M
odern refineries have adapted to exploit heav-
ier crude oils and meet ever more stringent envi-
ronmental requirements for fuel specifications,
increasing demand for hydrogen to meet the most severe
hydrotreatment needs. Increased hydrotreatment severity
has caused an increase in refinery off-gas (ROG) produc-
tion in most refineries, which frequently exceeds the pos-
sibility of sending it to other units or burning it entirely as
fuel gas.
The value of these ROG streams increases dramati-
cally when the hydrogen component can be purified and
recycled as a feed gas back to the hydrotreaters, reducing
hydrogen purchases through merchant suppliers or hydro-
gen production from the refinery itself.
With an increased focus on carbon footprint and net zero
goals by 2050, hydrogen production is a key focus area for
reducing greenhouse gas emissions. Greater than 96% of
hydrogen manufactured today is through steam methane
reforming (SMR), where natural gas is heated in the pres-
ence of steam over a catalyst to produce hydrogen and
carbon monoxide (CO). The CO can be further processed
via a water gas shift (WGS) reaction to produce additional
hydrogen as well as carbon dioxide (CO₂).
Modern refineries have adapted to meet ever more stringent environmental
requirements for fuel specifications
32 Gas 2024
Divigas.indd 32
Once the hydrogen product is separated and purified from
the CO₂ and other contaminants, most hydrogen plants
currently release the CO₂ directly into the atmosphere. This
type of hydrogen production is referred to as ‘grey’ hydro-
gen. Grey hydrogen production prices are highly variable
depending on the cost of natural gas, but a good rule of
thumb is a price of $1.50-2.00/kg.
To reduce the carbon impact of hydrogen production,
many refiners look to move to blue hydrogen, SMR pro-
duction paired with carbon capture, utilisation, and storage
(CCUS) or green hydrogen produced via electrolyser driven
by renewable electricity. These process changes have a
significant impact on the price. Blue hydrogen is estimated
to double hydrogen costs to $2.80-3.50/kg, while green
hydrogen is a staggering five times price increase up to
around $8/kg.
This cost increase of a crucial feed gas for refinery
processes has several implications, one of which is the
increased importance of recovering unused hydrogen wher-
ever possible. Most of the hydrogen supply for refiners now
comes from three locations: the refinery hydrogen plant,
which is typically an SMR unit; the catalytic reformer (CR),
which produces hydrogen as a byproduct of its reaction;
and third-party-produced hydrogen via
pipeline or other transportations meth-
ods. To reduce the need for hydrogen
from those sources, refineries look to
their ROG streams for economically
recoverable hydrogen.
Gas separation options
Hydrogen separation membranes have
been utilised in refinery operations
since the 1980s but have remained
niche in their application due to the lim-
itations of legacy membrane technol-
ogy. Divigas has developed the Divi-H
membrane, a polymeric hollow-fibre
membrane capable of separation
and purification of hydrogen even in
extreme environments. Unlike legacy
technologies, Divi-H excels at separa-
tion of hydrogen from CO₂.
www.digitalrefining.com
08/03/2024 17:14:21
 Summary of gas separation technologies

Features Adsorption Cryogenics Legacy membranes Divi-H

H₂ purity 99.9%+ 90-96% 90-98% 90-99.95%
H₂ recovery 75-92% 90-98% 85-95% 90-95%
Feed pressure 10-40 barg >5-75 barg 20-160 barg 20-160 barg
Feed temperature 50-80C <0C 20-80C 20-150C
Feed H₂ content >40% >10% >25-50% >25-80%
H₂ product pressure Feed pressure Feed/low pressure << Feed pressure < Feed pressure
H₂ capacity 1-225 K Nm³/hr 10-75+ K Nm³/hr Modular Modular
Pretreatment requirements Depends on CO₂, H₂O CO₂, H₂S, acid Minimal (liquid
adsorbent removal gas removal separation only)
Multiple products No Liquid HCs No No
Capital cost Medium High Low Low
Scale economics Moderate Good Modular Modular

Table 1

It can operate in environments rich in H₂S and acidic
gases that would cause legacy membranes to fail and
operate at temperatures up to 150°C, whereas prior tech-
nology was limited to 50-80°C. These improvements in the
performance of polymeric hydrogen separation membranes
allow for significant use-case expansion within refinery
operations. Table 1 gives a summary of the different gas
separation technologies available to refiners.
Part 1 of this article will preview sample ROG streams
produced from several types of units for their potential sep-
aration and purification via Divi-H. The membrane demon-
strates separation costs as low at $0.015/kg hydrogen
separated, with returns on investment (ROIs) exceeding
2,400% over the life of the product when compared to grey
hydrogen production. Part 2 in PTQ Q3 2024 will analyse
its effectiveness in hydrotreaters and hydrocrackers.
continuously without the need for intermittent cycles or
regeneration steps, providing a steady supply of separated
gases. The Divi-H membrane modules allow for ‘hot swap-
ping’, where a fibre cartridge is replaced within a single
module while the system continues operating.
y Simplicity and ease of operation: Membrane systems
are simple to operate and require minimal supervision. They
do not involve complex processes like cryogenic cooling or
adsorption-desorption cycles.
z Fast start-up and shutdown: Membrane systems can
quickly reach operational conditions, reducing downtime
during start-up and shutdown.
{ Versatility: ROG streams can change compositions,
flow rates, and pressures quickly. Membrane separation
can handle a wide range of gas streams with varying com-
positions and flow rates.

Membrane technology advantages

There are several qualitative benefits to leveraging mem-
brane technology for gas separation, of which not all will be
considered in the following analysis:
u Energy efficiency: Membrane separation requires sig-
nificantly lower energy consumption compared to cryo or
pressure swing adsorption (PSA) separation. The driving
force for separation is provided purely by the feed gas
pressure.
v Compact and modular design: Membrane systems
have a smaller footprint and are easily scalable, making
them suitable for applications where space is limited or
modular expansion may be required. This scalability allows
for great flexibility for ROG stream applications, as the flow
rates and composition of the ROG can change quickly and
vary greatly.
w Selectivity and design versatility: While cryogenic and
PSA separation are limited in their hydrogen purity options,
membrane systems can be designed for a massive range
of desired purities, pressure drops, and recoveries. If the
purity of the hydrogen product stream does not need to be
at 99.95%+, the economics of membrane separation are
difficult to beat.
x Continuous operation: Membrane separation operates
Membrane separation requires
significantly lower energy
consumption compared to cryo or
pressure swing adsorption separation
| Minimal maintenance requirements: Membrane sys-
tems have no moving parts, resulting in lower maintenance
and operational costs.
} Reduced environmental impact: Membrane separation
avoids the need for cryogenic fluids or chemical adsor-
bents, minimising the release of harmful substances into
the environment.
~ Cost-effectiveness: Membrane separation offers a
cost-effective solution for gas separation due to lower cap-
ital and operational expenses, shorter project lead times,
and reduced utility requirements.
ROG sources
The hydrogen balance throughout a refinery can be com-
plex, with multiple source locations, uses, and points of

www.digitalrefining.com Gas 2024 33

Divigas.indd 33 08/03/2024 17:14:22

 in today’s modern refinery. Gasoline has several specifica-
Hydrogen-containing ROG producers tions that must be satisfied to provide high performance
Unit name Operating Operating for today’s motor vehicles. Octane, however, is the most
temp. (F) pressure (bar) widely recognised specification. Molecules are reformed
Gas oil hydrotreater 600-800 130-140 into structures that increase the percentage of high-octane
Hydrocracker 650-800 105-210 components while reducing the percentage of low-octane
Kerosene hydrotreater 600-800 35-100 components. In doing so, it liberates a significant amount
Diesel hydrotreater 600-800 35-100 of hydrogen that may be used in desulphurisation and sat-
Light naphtha hydrotreater unit 400-500 25-45 uration reactions elsewhere in the refinery. Table 2 sum-
Heavy naphtha hydrotreater unit 400-500 25-45 marises the units and operating conditions for potential
Isomerisation unit 250-520 17-27 sources of hydrogen-containing ROG.
Catalytic reformer 925-975 7-25
Fluid catalytic cracker (FCC) 950-1,020 1-2 Where does membrane technology make the
most sense?
Table 2 Membrane separation technology has been closely moni-
tored for its advantages over traditional separation meth-
potential recovery. For the purposes of this analysis, the ods. Membrane separation requires no moving parts,
following sources of hydrogen-containing ROG will be dis- chemical reactions, solvents, or adsorbents. The separation
cussed in Parts 1 and 2: is driven exclusively by the pressure of the feed gas.
• Hydrotreating is a catalytic process to stabilise products While purified hydrogen is produced at a lower pressure
and remove objectionable elements like sulphur, nitrogen, than the feed gas, it can be reintroduced to units operating
and aromatics by reacting them with hydrogen. Hydrogen at lower pressure or recompressed using existing or new
reacts with oil to produce hydrogen sulphide from sulphur, hydrogen recycle compressors. The retentate – typically
ammonia from nitrogen, saturated hydrocarbons, and free containing <10% hydrogen and lighter hydrocarbons – is
metals. Metals remain on the catalyst, and other products released at near feed pressures and can be easily routed to
leave with the oil-hydrogen stream. downstream separation processes (for example, cold box)
• Isomerisation is a type of refinery process that converts or even as feed back to the SMR.
linear paraffins with low octane ratings into branched par- Due to the feed pressure requirements for membrane
affins with higher octane ratings. This process is typically separation, the units that make the most sense as ROG
used to upgrade low-quality naphtha into higher-quality feed producers are the high-pressure systems. An eco-
gasoline blending components. nomic analysis of the separation potential for Divi-H will
be conducted in Part 2, starting with the highest pressure
systems then working to the lower.
Due to the feed pressure Divigas has developed a proprietary simulator that uti-
requirements for membrane lises Aspen Hysys and Matlab to allow for simulations using
feed gas pressure, temperature, composition, and flow rate.
separation, the units that make the Results include the make-up of the permeate and retentate
most sense as ROG feed producers streams, as well as the required membrane surface area,
end hydrogen purity, and hydrogen recovery. We will ana-
are the high-pressure systems
lyse the results as follows:
• Pressure reduction and module count required for 95%,
99%, and 99.9% hydrogen purity from each potential
• The fluid catalytic cracker (FCC) is the tool refiners use to source. While currently utilised PSA technologies typically
correct the imbalance between market demand for lighter produce 99.9% or greater hydrogen, there is significant
petroleum products and crude oil distillation that produces flexibility in permeate purities with membrane technology.
an excess of heavy, high boiling range products. The FCC • Opportunities for reintroduction without additional
unit converts heavy gasoil into gasoline and diesel, cracking compression.
heavy gasoils by breaking the carbon bonds in large mol- • Recompression of purified hydrogen back to feed pres-
ecules into multiple smaller molecules that boil in a much sures, allowing recycling back into the same unit.
lower temperature range. • Cost of separation ($/kg).
• The hydrocracker is like the FCC in that it is a catalytic Several assumptions were made to simplify the analysis:
process that cracks long-chain gasoil molecules into smaller • These streams are rough approximations of ROG com-
molecules that boil in the gasoline, jet fuel, and diesel fuel position, flow rate, and conditions. For an analysis of a spe-
range. The fundamental difference is that cracking reactions cific unit case, precise data from that specific unit should be
take place in an extremely hydrogen-rich atmosphere. Two utilised.
reactions occur. First, carbon bonds are broken, followed • While the compressor duty was considered when look-
by the attachment of hydrogen. Hydrocracker products are ing at cases where the purified hydrogen was recom-
sulphur-free and saturated. pressed to feed pressures, it was assumed spare hydrogen
• Catalytic reforming is the workhorse for octane upgrade recycle compressor capacity would be available. If it is not

34 Gas 2024 www.digitalrefining.com

Divigas.indd 34 08/03/2024 17:14:23

 available, a capital expense for additional compression
should be included.
• The Divi-H membrane life is estimated at five years. All
analysis of ROI and cost/kg separated was conducted over
a five-year cycle. Longer time windows improve the eco-
nomics. The fibre replacement that would occur in year five
is cheaper than the original capital expenditure, as cartridge
housings and ancillary equipment are not included.
• Module cost for a 10in diameter, 3m length membrane
module was assumed to be $80,000. This is a rough con-
servative estimate based on current manufacturing costs
and projected savings with scale-up. Ancillary equipment,
including piping, valving, and pressure control, was esti-
mated to be 50% of total module and housing costs.
• A rate of $0.08/kWh was assumed when converting
compressor duty to cost. This is the current average indus-
trial electricity cost in the US.
Below are definitions that may be useful for understand-
ing the simulation data:
• Permeate: The gas stream that permeates through the
membrane surface, in this case hydrogen.
• Retentate: The gas stream that does not permeate
through the membrane surface.
• Permeance: How much gas permeates the membrane
per unit surface area.
• Selectivity: How many molecules of one gas will pass
through the membrane per one molecule of a different gas.
• Purity: Mol% hydrogen in the stream.
• Recovery: The percentage of feed hydrogen that ends up
in the permeate.
ac24_Decarbonisation Technology Magazine_178x125.indd 1
www.digitalrefining.com
Divigas.indd 35
• Single-stage: Membrane separation conducted with a
single-pass through membrane modules set up in parallel
flow configuration.
• Two-stage: Membrane separation conducted with two
passes through membrane modules in series.
• High-throughput fibre: Designed by Divigas to prioritise
permeance (gas throughput) over selectivity (purity).
• Balanced fibre: Designed by Divigas to balance perme-
ance and selectivity.
• High-purity fibre: Designed by Divigas to prioritise selec-
tivity over permeance.
ROG streams will be a crucial source of hydrogen in refiner-
ies as product regulations and crude processing requirements
drive increased hydrogen demands. The need will further
increase as energy companies look to limit heavy sources of
carbon within their operations to meet net zero goals by 2050.
As refiners shift from SMR produced grey hydrogen to green
or blue, costs will increase, lowering the economic barrier to
downstream hydrogen recovery and purification.
Part 2 in the Q3 issue of PTQ will review sample ROG
streams produced from several hydrotreaters, a hydroc-
racker, an isomerisation unit, and a catalytic reformer for
their potential separation and purification via Divi-H,
References will be included in Part 2.
Zach Foss is Director of Business Development for Divigas, responsi-
ble for sales, marketing, strategic initiatives, and project management.
He has 10 years of experience in the manufacturing and sale of down-
stream petrochemical and specialty products. He holds a BS in chemical
engineering from University of Texas. Email: Zach.foss@divigas.com
23.10.2023 07:52:37
Gas 2024 35
08/03/2024 17:14:25
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36 Gas 2024 www.digitalrefining.com

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