ASU-12-08-BOC

Adsorbers and Gel Traps

Adsorbers and Gel Traps

Purpose and Scope
About Cryogenic Adsorbers
Adsorber System
Essential Safety Role
Potential Hazard of Contaminants
Inherent Hazard of Cryogenic Adsorber Systems
Contaminant Removal Systems
Adsorber Vessel
Location of Adsorber
Selection of Adsorbent
Order of Adsorption
Adsorber Filters
LO Adsorbers
Adsorber Operation
Adsorber In-Service Period
Draining Liquid from the Adsorber
Regeneration (Reactivation)
Typical Regeneration Temperature Profile
Cooldown after Regeneration
Rapid Regeneration Procedure
Overview of Rapid Regeneration Procedure

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Step 1- Isolation and Draining Liquid

Step 2 - Establishing Regeneration Flow and Heating
Step 3 - Terminating Heating and Establishing Cooling with Regeneration Gas
Step 4 - Initiating and Completing Liquid Filling
Step 5 - Bringing the Adsorber Back Online
Temperature Profiles during Regeneration
Taking Adsorbers Out of Service
Adsorber Maintenance
Adsorber Cold Standby
Cold-end Gel Trap (CEGT) Operation
Common Problems

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Attachment(s):
T-G-280, Cryogenic Adsorbers
T-S-004, Gel - Liquid Phase Adsorber
T-S-008, Gel Gas Phase Adsorber

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Purpose and Scope

Purpose

This chapter explains:

The purpose of cryogenic adsorbers

The different types of adsorber and adsorbent that may be used

How adsorbers and gel traps should be operated and maintained

How to deal with common problems with adsorbers.

It also highlights the fundamental safety risks.

Scope

This chapter applies to all BOC sites worldwide that operate liquid phase (rich liquid or liquid
oxygen) or gas phase (gel trap type) cryogenic adsorbers.
The target audience is operators, managers and engineers.
This chapter does not apply to ambient temperature adsorbers, such as pre-purification units (PPUs).

About Cryogenic Adsorbers

Adsorber System
Adsorber vessel

The cryogenic adsorption system comprises one or two vessels containing silica gel adsorbent. The
system also includes filtration equipment to prevent adsorbent dust travelling down stream, a method
to circulate process flow through the adsorber and a means to provide and vent hot nitrogen
regeneration gas.
The adsorbent removes trace contaminants from a cold gas or liquid process stream. Most
commonly the adsorption is carried out on Rich Liquid (RL) passing from the HP to LP column or
on a recirculated stream of liquid oxygen at the condenser/reboiler sump. In some older plants the
adsorber may be on the cold air feed to the HP column.
It is a batch operation and the adsorber vessel must be isolated periodically from service and
regenerated (reactivated) for re-use.

Essential Safety Role

The essential safety function of cryogenic adsorbers in ASUs is to remove trace quantities of:

hydrocarbons such as acetylene, propane, ethlylene, etc.

low solubility contaminants - mainly carbon dioxide and nitrous oxide.

Hydrocarbon
safety

Potential Hazard of Contaminants

Trace levels of
contaminants

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Whatever system is used to remove air contaminants prior to entry into the cold box, trace levels of
CO2 , N2 O and hydrocarbons may remain and then reach the column system.

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Where do
contaminants
concentrate?

These contaminants are less volatile than oxygen. Therefore, they will concentrate in the column
reboiler and vaporiser sumps to a level that could cause a safety hazard.

Why these
Hydrocarbons may condense out as solids and accumulate as fuel for explosions. Carbon dioxide
contaminants are and nitrous oxide also provide a hazard because they can condense out as solids. The solids can
a hazard
block heat exchange passages, causing localised dry boiling and accumulation of hydrocarbons

around and within the solid deposit.

Accumulation of The accumulation of solids is a particular problem in a reversing heat exchanger (RHE) plant making
solids is a hazard little or no liquid oxygen. When this is the case a cryogenic adsorber system is installed to take up

the contaminants.
On rare occasions a cryogenic adsorber may be required for a plant using a PPU. This has been
necessary when removal of N2 O in the PPU has been incomplete, and a plant is designed for very
low liquid purge. See: ASU-12-02 : Cold Box Hazards and Safety

Inherent Hazard of Cryogenic Adsorber Systems

Cryogenic adsorbers create multiple concurrent hazards in their own right.

Training

Only those trained should carry out operation of adsorbers. Trained personnel need to be aware of
the risk to the plant, themselves and others nearby.

Routine
operation

Routine operation of adsorbers involves:

cryogenic liquid venting and disposal with the hazards of:

cold burns, splashing into eyes, etc.

mists creating poor visibility

oxygen enrichment with hazards of fire with incompatible materials especially people.

pressure system operation with hazards of liquid/gas release from vents/safety valves.

high temperature reactivation systems with hazards of burns and electrical safety.

flammable gas explosion issues due to hydrocarbon build up and ignition.

Contaminant Removal Systems

Partial removal

Most contaminants are at least partially removed in process steps upstream of the distillation system.
Exceptions to this are methane and ethane which remain soluble through the process and are of
lesser concern.

Modern plants

Most modern plants use adsorptive pre-purification units (PPUs) to remove H2 O and CO2 .
Depending on the adsorbent used and the quantity, varying amounts of N2 O and hydrocarbons may
pass through the PPU.

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Older plants

Older plant designs using reversing heat exchangers rely entirely on the freeze-out mechanism for
the removal of CO2 and other impurities. For reversing heat exchanger (RHE) plants, contaminant
concentrations leaving the cold end of the main heat exchanger are determined by their vapour
pressure at the exit temperature.

Adsorber Vessel
Adsorber vessel

The cryogenic adsorber is a stainless steel vessel containing silica gel adsorbent that removes trace
contamination from the gas or liquid process stream. In some designs there is an integral filter
which prevents the migration of adsorbent material to downstream equipment. The adsorber vessel
is the principal component of the Adsorber System.

Location of Adsorber
Location options

Liquid phase
adsorbers

The adsorber can be:

located in the gas phase on the cold air feed, prior to entry into the high pressure column,
or

installed on liquid streams - either the rich liquid leaving the high pressure column or
recirculating liquid oxygen.

Liquid phase adsorbers are usually fitted to RHE plants. More recent plants are equipped with PPUs
instead of RHEs. PPU plants are not equipped with adsorbers unless the plant has a very low LO
purge and is at risk from accumulation of N2 O.
The PPU removes most hydrocarbons as well as other impurities. Any hydrocarbons not removed
must be kept at low levels in solution within the plant by maintaining an adequate purge.
PPU plants that never have water present in the adsorber or regeneration gas stream may be
regenerated to a temperature of only 80C, which is sufficient to remove hydrocarbons and will give
a power saving. An IMSS exemption should be raised to obtain approval to reduce the regeneration
temperature. See: IMS-02-10 : Exemptions to IMSS Requirements.

Flow through a
liquid phase
adsorber

Limited use of
cold gas phase
adsorption

Flow through the adsorber is generated by either:

the available pressure drop for the rich liquid stream or cold air feed, or

by pumping a circulating liquid oxygen stream at the sump of the low-pressure column.

Although cold gas phase adsorption is more effective, it is normally not used. This is because it can
impose a significant pressure drop on the air circuit and would cause a power penalty, which in most
circumstances the liquid phase adsorbers do not.
A second issue is the risk of desorption of hydrocarbons if the temperature of the gas phase adsorber
increases due to a change of operating conditions.
Note:

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Gas phase adsorption has been used on oxygen and nitrogen generators.

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Selection of Adsorbent
Use of silica gel
beads

Although in principle the bulk of the contaminants could be removed by a number of different types
of adsorbents, silica gel beads are the adsorbent of choice.
This is partly due to good adsorption characteristics at low temperature, but also due to the superior
resistance to degradation caused by the severe thermal and pressure swings that result between
normal running and regeneration conditions.

Advantages of
silica gel

Silica gel has a high capacity for adsorption of carbon dioxide, nitrous oxide, acetylene, ethylene,
propane, propylene, and butane from cryogenic liquids. The high capacity makes it possible for an
adsorber to be in operation for at least a week. A pair of adsorbers is usually installed to give
continuous protection from impurities.

Recommended
choice

The recommended choice of adsorbent based on adsorption capacity and attrition tests is Sorbead R
with Sorbead WS an acceptable replacement when breakup has occurred due to moisture
contamination.

Approved
supplier

The silica gel must be purchased in accordance with a design specification from an approved
supplier. This is to ensure it meets performance criteria.
Mobil Sorbead R Tyler 4-8 mesh beads {2.4mm 4.7mm} is the typical adsorbent used. Mobil sold
the manufacturing rights and the product is now known as KC-Trockenperlen S, marketed in the UK
by Lawrence Industries. Another preferred material is Lindes Pergel W 2.8 6mm beads.
Note:

Grades of silica
gel

When these materials are not available, the adsorbent purchased must as a minimum
comply with adsorbent specifications T-S-004, Gel - Liquid Phase Adsorber (see
attachment) and T-S-008, Gel Gas Phase Adsorber (see attachment).

The two grades used are both predominantly SiO2 with some Al2 O3 as follows:

Sorbead R is 97% SiO2 and 3 % Al2 O3

Sorbead WS is 97% SiO2 and 3 % Al2 O3

Sorbead WS is much more tolerant of liquid water, which will break up Sorbead R. Sorbead
WS is used where there is a history of breakup of gel, usually as a layer of WS at each end of the
adsorber, with R in the middle. Mixed beds are more difficult to re-use as the gels tend to mix
when removed for inspection.

Breakup problem The cause of any problems with breakup of the adsorbent should be identified.

Breakup within the bed cannot be detected by inspection from the top of the bed. Samples may be
taken through the bed at different depths but then need to be sieved to establish the quantity of
particle breakup.
Most larger broken up particles fall to the bottom of the bed and the lighter dust is generally carried
through the bed to the outlet filter.
Sand like particles falling to the bottom of the bed cause the adsorber to act as a screen filter rather
than deep bed filter, which can be blocked very quickly by solid CO2 contamination. This often
occurs during a plant cold start up when large quantities of CO2 can be carried over from the process.
If the cause of the breakdown is due to high moisture levels, Sorbead WS should be considered for
the top and bottom 10% of the bed, because this is much more resistant to water, but does have
slightly reduced CO2 adsorption capacity compared with Sorbead R.

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Order of Adsorption
Liquid phase
order

In the liquid phase, silica gel has the following order of adsorption capability with acetylene being
the most strongly adsorbed and methane least strongly adsorbed.

Acetylene

Propylene

Carbon dioxide

Nitrous Oxide

Ethylene

Propane

Ethane

Methane

Adsorber Filters
Function

Filters are required to remove particulates, which generally consist of small silica gel particles that
have degraded due to thermal shock or attrition.

Design

Filters are either incorporated in the adsorber vessels or separately in the downstream circuit to trap
any adsorbent particles or powder that might contaminate downstream equipment.
Because of the significant temperature changes experienced between normal operation and
regeneration conditions, the filter design has to allow for differential contraction as well as being
leak tight where it joins the vessel and adsorption bed.
The filter is a composite of perforated metal and glass twill layers, with the glass twill undergoing
different compression forces during thermal swings.
For detailed design requirements, see: T-G-280, Cryogenic Adsorbers (see attachment).

Integral filter /
adsorber design

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In an integral filter/adsorber design the cone at the top of the bed is perforated and covered with wire
gauze. The purified liquid therefore passes through the cone and passes from the outside of the filter
into the inner part of the filter.

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LO Adsorbers
BOC design
requirements

The standard BOC design requires that a flow equal to the total oxygen make be passed through the
adsorber. To achieve this, liquid is:

taken from the sump

passed through a mechanical pump, and

returned to the reboiler bath or to storage.

In a small number of plants the circulation flow is created by partially vaporising the liquid leaving
the adsorber in a plate fin heat exchanger. This reduces the fluid density and creates a thermosyphon
effect in the LO adsorber circuit. Particular care is need with this type of plant to avoid dry boiling
in the vaporiser and special operating rules apply for inspection and maintenance. Dry boiling in the
vaporiser exchanger can lead to accumulation of trace hydrocarbons with subsequent violent reaction
with the oxygen. Explosions in this type of auxiliary reboiler have occurred in a number of plants
throughout the industry in recent years.

Adsorber Operation

Adsorber In-Service Period

Maximum inservice period

Adsorbers must not remain in service for longer than the maximum duration specified in the
operating manual, or subsequently approved operating procedures.

For liquid phase adsorbers this is generally 1 week

For gas phase adsorbers this may be exceed 1 month

Note:

Defined
regeneration
intervals

The maximum duration relates to total in-service time since last regeneration. Where plants
operate in stop/start mode, procedures must be in place to ensure that total in-service time
is monitored.

The maximum in-service periods are independent of pressure drop across the bed or results of
acetylene tests of the condenser liquid.
Adsorbers must be regenerated at the defined interval even if the pressure drop or acetylene tests
appear satisfactory.
Extending in-service time increases adsorber hydrocarbon loading (and therefore the hazard) and
may result in break through of hydrocarbons or carbon dioxide into the process without immediately
visible symptoms.

Reduced inservice period

The in-service period may need to be reduced where high atmospheric contamination, pressure drop
or acetylene buildup dictates.

Control checklist

This checklist includes recommendations for monitoring the operation of the adsorbers.

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Use a marker board to indicate adsorber number/letter and status (that is, regenerating,
cooling).

Mount the board near the absorbers or in the control room.

Record the status of the adsorbers and regeneration in the log book. Include the temperature
reached on each regeneration.
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Draining Liquid from the Adsorber

Method 1

This procedure describes one method of draining liquid from the adsorber.
Step

Action

Close the liquid outlet of the adsorber coming offline.

Allow liquid in the adsorber to vaporise (gas off). This pressure decants the
liquid into the online adsorber.

About method 1

This method recovers refrigeration by saving a large part of the liquid contained in the adsorber.

Method 2

This method of draining liquid from the adsorber is preferred if high hydrocarbon load is suspected.
Step

Action

Box in the adsorber.

Drain off the liquid.

About method 2

This method discards any heavily contaminated liquid and ensures that as the pressure falls and
hydrocarbons are desorbed, these pass into the drainage system and not back into the main plant.

Regeneration (Reactivation)
Regeneration
procedure

This table describes the normal regeneration procedure.

Step

Action

The vessels are drained of liquid. See: Draining Liquid from the Adsorber
(Page 9).

Once liquid is drained from the adsorbers, regeneration must be carried out
immediately.

A stream of ambient nitrogen is passed through the vessel for 2-3 hours.

The nitrogen heater is switched on.

Once the bed outlet temperature has reached 120C (248F), it is maintained
there for one hour.
At every fourth regeneration, the temperature must reach 130C (266F) and
be held for 3 hours.

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The vessel is then cooled using ambient nitrogen for three hours, before
cooling the bed with cold gas, if available, or liquid.

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Length of
process

The whole process is normally allowed to take 24 hours. The main reason for this is that draining the
adsorber and re-cooling the bed results in a significant increase in refrigeration requirement, which is
best spread across a relatively long but regular period. The second consideration is that too fast a
change in temperature could cause problems to both the grid and filter internals.

Need for
adequate
regeneration

Adequate regeneration temperature must be achieved to ensure complete removal of all

hydrocarbons. Whilst some hydrocarbons are easily removed, others remain adsorbed until high
temperatures are achieved. If these are not removed during regeneration, they may build up until the
bed becomes saturated. Such a high concentration of adsorbed hydrocarbons is in itself hazardous,
but may also result in breakthrough of other hydrocarbons into the process.

What to use for

regeneration

Dry nitrogen with oxygen content below 1% is preferred. Air may be used, but is inherently less
safe because of the potential for creating flammable mixtures.

Flow rate

Flow is determined by the design of a particular system. It should be adjusted to give approximately
150 180C (302 356F) adsorber inlet temperature when attempting a bed temperature of 120C
(248F).
The flow rate must be high enough to carry the total heat required for regeneration, but low enough
to reach the desired temperature from the heater.
The balance will be based on experience with the particular plant.
It is essential to maintain an adequate regeneration flow, particularly when regenerating with air, to
ensure sufficient dilution to maintain the outlet gas well below its flammable range. Different
hydrocarbons desorb at different temperatures, so it is necessary to maintain the flow throughout the
entire regeneration process.

Temperature
requirements

Reason for
temperature
increase

Regeneration temperature requirements are:

120C (248F) for one hour, measured in the regeneration gas leaving the adsorber

130C (266F) for three hours measured as above, on every fourth regeneration cycle.

The increase of temperature during the fourth regeneration is primarily to ensure the complete
removal of trace water from RL adsorbers. This may happen in a RHE plant where the water load is
unusually high. Since the water load in the RL stream is not generally known, the practice of
heating to 130C (266F) for an extended period on the fourth regeneration has been applied
generally.
Where water is known to be a problem, the regeneration temperature on every fourth regeneration
cycle should (if possible) be increased to 150C (302F) for one hour. This is particularly applicable
to RHE plants where the individual blocks/banks of the RHE are known to be out of balance.

Troubleshoot
temperature
problems

If the regeneration temperature cannot be achieved, look for faults or cold leaks (for example,
isolation valves not fully closed).
If any faults are found, maintenance to the plant equipment may be necessary (for example, valve
leaks, heater faults, etc.

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Typical Regeneration Temperature Profile

About this graph

This graph was plotted during an adsorber regeneration cycle. It shows the following at the adsorber
outlet during regeneration:

temperature variation

CO2 concentration

H2 O concentration.

In this case, the adsorber took 25 hours to regenerate. CO2 was fully desorbed after 15 hours, and
moisture after 25 hours.

During the initial stages of regeneration, all the heat goes into raising the bulk temperature of the
bed. However, this rise is not seen until the temperature front reaches the bed outlet. The
temperature then rises until enough energy is available to drive the CO2 off the bed.
At this point the CO2 is detected at the outlet. It is often accompanied by a pungent smell (probably
caused by retained aromatic hydrocarbons removed from air). No rise in temperature is apparent
until all the CO2 is regenerated. At this point the energy in the regenerating gas can now continue to
heat the bed.
Sometimes a smaller plateau occurs between 0 100C (32 212F), indicating that moisture has
been retained in the bed. Moisture causes breakup of the adsorbent. Moisture may be carried over
from the improperly balanced RHEs and will leave the column in the RL.
Moisture degradation of the sieve can occur from free water contained in the regeneration gas
stream, therefore all free water must always be removed from the regeneration gas.

Cooldown after Regeneration

Procedure

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This procedure describes how to cool down the bed after heating.

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Step

Action

Blow through the bed with unheated nitrogen until the temperature of gas
leaving the adsorber falls to 20C (36F) above ambient temperature.

Close the nitrogen supply to the bed. Crack open liquid feed and outlet. This is
to start liquid flow.
Cool the bed slowly to prevent damage to absorbents. When the bed is cold
and contains liquid, slowly increase the flow until normal operating conditions
are established.

Rationale for
slow cooling

Rapid cooling or heating of the absorbers or gel traps will cause serious damage. This damage could
lead to breakdown and dusting of the adsorbent with subsequent high pressure drops across filters
and possible distribution of dust throughout the plant.

Rapid Regeneration Procedure

Overview of Rapid Regeneration Procedure
When to use

Use this procedure if it is necessary to regenerate an adsorber on an RHE plant blocked by CO2 to
allow the ASU to remain online.
The procedure may only be followed on adsorbers filled with:

Sorbead R or WS

other equally stable bead type silica gel product.

Using this procedure for repeated cooldowns has not resulted in significant breakup, but it should
only be carried out in emergency situations (that is, to avoid shutdown).
In order to use this procedure it is necessary to establish the regeneration profile of the bed.

Pre-requisite
checks

Trials

Before following this procedure, check that:

the newly introduced adsorber has not exceeded its on-line time for hydrocarbon adsorption.

the consequences of break up of the beads have been weighed against shutting down the ASU
for complete regeneration.

Study the regeneration profile and establish by experiment the optimum time at which the heater can
be switched off and still achieve the desired bed outlet temperature (all carbon dioxide removed) as a
consequence of the thermal front moving through the bed.
The outlet temperature may just exceed the first plateau from the regeneration graph in as little as 10
hours, but trials must be carried out to establish the exact time.

Rapid
regeneration
procedure

The steps involved in the rapid regeneration of the adsorber are listed below. Further details are
given in the subsequent topics.

Step

Action

Isolation and draining liquid.

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Step

Action

Establishing regeneration flow and heating.

Terminating heating and establishing cooling with regeneration gas.

Initiating and completing liquid filling.

Bringing the adsorber back online.

Step 1- Isolation and Draining Liquid

When to use

Follow these steps to depressurise the adsorber and commence drainage when the clean adsorber is
in parallel service.

Step

Action

Close the isolation valve on the outlet of the blocked adsorber.

Close in the inlet isolation valve.

Open the bottom drain fully.

Note

The speed of drainage may be limited by the capacity of the liquid disposal system.

Step 2 - Establishing Regeneration Flow and Heating

When to use

Follow these steps to set up the regeneration circuit. This can start as soon as depressurisation and
liquid disposal have commenced.

Step

Action

Admit nitrogen as early as possible, dependent on the capacity of the liquid or

cold vapour disposal system.

Wait until flows have been established, then switch the heater on.
It is not necessary to wait for the bed to warm naturally with ambient nitrogen
because before the bed sees heat it will take up to 30 minutes for the heater to
warm:

elements

delivery pipework, and

regeneration inlet pipework.

The heating is progressive and therefore thermal shock does not occur.

Step 3 - Terminating Heating and Establishing Cooling with Regeneration Gas

When to use

Follow these steps to terminate heating and establish cooling with regeneration gas.

Step

Action

Determine the optimum time achieved during trials to attain the desired bed
outlet temperature.

Switch the heater off.

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What happens
during this step

The thermal front continues to move through the bed to achieve heating and vaporisation of CO2 .
The top of the bed now begins to cool and follows the heating profile through the bed.
Gas cooling is complete as soon as the bed outlet temperature of 200 K is achieved.

Step 4 - Initiating and Completing Liquid Filling

When to use

Follow these steps to initiate and complete liquid filling.

Step

Action

Wait for gas cooldown to finish, then introduce cryogenic liquid to speed the
cooling process.
At this stage, cooling is limited by the size of the regeneration outlet valve (this
needs to release enough vapour to allow sufficient liquid to enter and aid
further cooling).
Initially, the inlet valve is cracked to reduce potential thermal shock, but it may
be progressively opened to full over 30 minutes.

Start bottom up cooling as the outlet temperature falls. This is possible

because the falling temperature shows that most of the heat has been removed.
This is usually faster as the top vent is usually larger than the regeneration
outlet valve. This valve may be fully opened over a period of 15 minutes. It
must be opened very slowly at first, because:

the temperature at the bottom of the bed may still exceed 200 K, and

the thermal shock may damage the bottom of the bed.

Step 5 - Bringing the Adsorber Back Online

About this step

Follow these steps to initiate and complete liquid filling.

When to use

Follow these steps to bring the adsorber online after 15 minutes of liquid cooldown.
It is important at this stage not to disrupt the process or overheat the plant subcooler exchangers
because:

the maximum temperature tolerated by the subcooler exchangers is 65C (149F), and

they are vulnerable to failure as a result of thermal shock.

Step

Action

Monitor the RL subcooler inlet temperature over 10 minutes.

Note:

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Do not allow the temperature to rise by more than 10C (18F) when
proceeding with the actions below.

Crack open the adsorber outlet valve.

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Step

Action

Check the subcooler outlet temperature. This may rise slightly because it
cannot remove all heat and maintain subcooling.
If there is little or no temperature rise, progressively open the adsorber outlet
valve.
During this stage the adsorber continues to fill with liquid at a rate determined
by the rate of release of vapour.
A fall in temperature shows that the adsorber is full and most of the vapour
removed.
The liquid line may still vapour lock at this stage, because the bed may not
have cooled evenly and heat may still be trapped at the centre of the beads.

Temperature Profiles during Regeneration

Temperature
profiles during
regeneration

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The approximate times of each step in the rapid regeneration procedure, and the temperature profile
at each step, are shown in the diagram below:

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Subsequent
regeneration

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If rapid regeneration is attempted, the adsorber must be fully regenerated again within one week of
the last full regeneration.

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Taking Adsorbers Out of Service

When an adsorber is taken out of service, or the plant is shut down, adsorbed hydrocarbons may start
to de-sorb as the adsorber warms and depressurises. This may create a flammable/explosive mixture
with the oxygen and hydrocarbons. It would only require an ignition source to initiate a dangerous
event.
Flammable gas
hazard

Liquid drained safeguard

Once liquid is drained from the adsorbers, regeneration must be carried out immediately.

Liquid not
drained safeguard

If liquid is not drained, the adsorber may stand cold for a maximum of 24 hours provided a liquid
level is maintained. If the adsorber stands cold for longer than this, liquid must be drained and
regeneration carried out.
Note:

This requires a means of regeneration to be available at all times. For example, where
plants regenerate using process air or nitrogen, an alternative means of regeneration must
be available in case of major machinery failure.

Plant shutdown
safeguard

If the plant is shut down, the adsorber must not be left to evaporate the liquid to dryness. This
means that RL adsorbers must usually be reactivated. However, it may be possible to continue to
recirculate LO though the LO adsorbers, particularly if the plant has LO injection capability.

Maintenance
safeguard

Maintenance carried out on such systems must take account of this hazard and be controlled by
permit.

Adsorber Maintenance
Internal
inspection

Adsorbers should be emptied at four yearly intervals and grid supports and wire mesh inspected for
damage.
High pressure drop across filters or beds indicates adsorbent breakdown and powdering and an
earlier change may be required. A further indication of failure of adsorbent and filters is the
presence of silica gel in LO samples taken from the sump of the condenser/reboiler.
The exterior of adsorber vessels should also be inspected at the same time for possible corrosion
cracking particularly in the vicinity of vessel welds. Corrosion has been found to occur due to
water condensation and leaching of impurities from cold box insulation.

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ASU-12-08-BOC
Adsorbers and Gel Traps

Adsorbent
replacement

Adsorbent gel may only be re-used if it is in satisfactory condition, as indicated by all of the
following:

there is no evidence of excessive breakage of beads

there is no evidence of recent CO2 or hydrocarbon contamination of the reboiler sump of the
ASU

a test for the water adsorption capacity of the gel shows that it has not deteriorated

more than 70% of the adsorbent is of the original size, and

the adsorbent is not discoloured.

If the sieve fails any of these tests then the entire adsorbent charge must be replaced.
If the adsorbent is suitable for re-use, it may be carefully sieved to remove damaged adsorbent. The
adsorbent level may be topped up with fresh materials.
Replacement adsorbent must be purchased in accordance with design specification
from an approved supplier.
Adsorption capacities of suitable materials vary markedly and improper material may
not remove contaminants from the process.

Avoiding breakup

To prevent break-up of the adsorbent, the silica gel should always be charged carefully into the
vessel (for example, by use of a vertical feeder tube kept full).

Valve
maintenance

Isolation valves become contaminated with dust, and must be cleaned whenever an adsorber is
emptied.
Leaking valves can result in improper regeneration and concentration of hydrocarbons on the valve.
They must be repaired as soon as possible.
Evidence of adsorbent beads in drains (especially from the sump of the LP column reboiler)
indicates failure of bed supports. The bed will need to be removed from service for repair.

Filter
maintenance

Where filters are installed on the outlet of the adsorber to retain dust carried over from the adsorber,
they should be inspected and cleaned at six monthly intervals.

Maintenance
records

Records of the work performed on the adsorbers and filters and details of the as found condition
should be maintained for future reference.

Adsorber Cold Standby

Recommended
procedure

This procedure is recommended if the adsorber is to be cooled and stood cold ready to be put in
service.

Step

Action

Cool the adsorber slowly using liquid from the on-stream adsorber.
This is achieved by opening the outlet valve and cracking the thawing
outlet/drain with the main inlet valve shut.

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Wait until the thawing outlet/drain is fully cold, then close it.

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ASU-12-08-BOC
Adsorbers and Gel Traps

Period of cold
standby

Provided that the adsorber has been regenerated and cooled using liquid from the in-stream adsorber,
it can be left cold for up to 7 days, before being put in service.

Cold-end Gel Trap (CEGT) Operation

Application

The adsorbents can vary and with this so will the regeneration temperature requirements.
Gel traps are used on reversing heat exchanger plants to remove hydrocarbons and carbon dioxide by
adsorption (CO2 as vapour) and filtration (CO2 as solid). They are installed in the air line to the HP
column. As the primary function of the trap is to remove hydrocarbons, regeneration should take
place exactly as stipulated by the plant supplier.

Onstream time
period

The maximum length of time which gel traps are permitted to remain on stream must be stated in the
operating instructions.
In some cases this is based on pressure drop but in general it is a stated time interval.

High CO2 loading

On some plants fitted with gel traps (for example, on nitrogen generators with RHEs), high solid
CO2 loadings can occur. In these situations, very small changes in RHE cold end temperatures can
cause the deposited CO2 to re-sublime to vapour, which then moves through the process and results
in fouling elsewhere.
To overcome this problem, run the generator at a fixed output. This reduces fouling and fluctuations
in plant parameters. If this is not possible, regular thawing of the plant is required.

Before a warm
start

The gel trap (or at least one of the gel traps on twin trap plants) should always be regenerated and
cooled to ambient temperature before a warm start of the plant.

Air temperature
ex RHEs

During the initial phase of plant startup the air compressors and expansion turbine are started and air
is recycled round the RHEs. The air ex RHEs at the cold end should be down to approximately
243K (-30C and -22F) before cooling of the gel traps commences.

On small plants it is possible to cool the gel trap at the same rate as the column system. This
ensures the trap is online when the product is required from the plant.

On larger plants this is not practicable. A period of up to several days may elapse before the
gel trap bypass can be fully closed.

Blowing down gel Depressurisation must take at least 15 minutes when blowing down gel traps. This is to prevent
traps
possible damage to gel. Large plants will take much longer because of pipework constraints.

Moisture
carryover

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Where moisture has been carried over to a gel trap:

maintain the regeneration outlet temperature for an extended period of time, or

increase the regeneration temperature.

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ASU-12-08-BOC
Adsorbers and Gel Traps

Regeneration
temperature
achieved

Improving CO 2
loading capacity

When the desired regeneration temperature ex the gel trap is achieved:

switch off the heater, and

continue nitrogen flow through the gel trap bed until the gel trap is cooled to approximately
20C (68F).

Any carbon dioxide carried over from the RHEs will exist as fine particles, which can quickly block
the gel trap. A high differential pressure across the gel trap indicates high CO2 loadings.
On overloaded plants, large quantities of CO2 can be carried over, and weekly regeneration may
become necessary.
In these instances, the effectiveness of the adsorber can be improved by replacing about 25% of the
gel at the inlet with activated alumina (9/16 cylindrical), but note that the effectiveness of
hydrocarbon adsorption will be reduced. For this reason, a risk assessment should be carried to
ensure hazard controls are still effective.
In this way, the alumina traps any large particles, and fine particles flow into the bed, depositing in
the pore sites between beads, resulting in much high loading before a high differential pressure is
observed.

Before a planned
shutdown

Before a planned shutdown, the gel trap should be regenerated and cooled to ambient temperature to
ensure it is available for plant restart.

Following a plant
trip

Following a plant trip there is a risk on restart of desorbing CO2 from the gel trap bed into the plant.
For this reason the gel trap should be bypassed before the plant is brought online. Where no bypass
is fitted the immediate history and status of the gel traps will determine the technique used. On twin
gel trap plants, regeneration to provide a fresh gel trap should take place as soon as possible.

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ASU-12-08-BOC
Adsorbers and Gel Traps

Typical gel trap

arrangement

Common Problems
Leaking adsorber inlet or outlet valves are not uncommon, but represent a significant risk.
Leaking valves can result in both:

Issue leaking
valves

Mandatory
safeguard

improper regeneration, and

concentration of hydrocarbons on the cold valve and pipework.

Either of these can result in a hydrocarbon incident and this represents a high risk.

Repair leaking adsorber inlet or outlet valves as soon as possible. Depending on the severity of the
leak, the plant may need to be shut down for maintenance of the valves.
Regeneration and thawing inlet valves are installed in the reverse direction of flow so that, when
closed, the glands are not continually pressurised with cryogenic liquid.

Issue High DP
and loss of RL
flow

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RL adsorbers are likely to suffer from high DP and resultant problems with liquid flow from the
lower to the upper column. A blockage in RL adsorber may first be indicated by an opening of RL
upflow valve position to compensate for the high pressure drop across the adsorber.
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ASU-12-08-BOC
Adsorbers and Gel Traps

Safeguard

Avoid loss of RL adsorber flow for extended periods because it may put the plant at risk due to:

dry boiling in exchanger passages and

deposition of CO2 and hydrocarbons in the reboiler.

Operation with bypass should only be for very brief periods. The adsorber should be immediately
regenerated. If this does not alleviate the problem, the filter should be inspected and cleaned. If this
is not successful, the plant must be shut down and the adsorber inspected.

Issue high
pressure drop

The common causes of high pressure drop are:

CO2 in RL due to RHE problems

dust in RL filter due to breakup of the gel.

In both cases the cause should be addressed. High levels of CO2 or other contaminants in the RL are
also likely to indicate high levels of hydrocarbons, and are to be avoided.

Similar problems with LO adsorbers, while not likely to shut down the plant in itself, are likely to
put the plant at risk from fouling and potential hydrocarbon buildup.

Issue LO
adsorbers

Issue LO
adsorber
vaporisers

Plate fin vaporisers used for creating circulation through LO adsorbers are especially vulnerable to
contaminant accumulation and dry boiling. This has been an intermittent cause of explosions in LO
vaporisers for both BOC and other industrial gas company plants.

Safeguard

It is especially important to monitor for any indication of:

increased pressure drop or loss of flow in the LO adsorber circuit, and

traces of adsorbent in column sumps and drains.

Issue fouling of On some plants, the RL adsorber is placed down stream from the RL/PL subcooler. On these plants,
subcoolers
CO2 buildup is generally seen in the subcooler, creating a high pressure drop or loss of heat transfer.

Initially, fouling is indicated by an RL upflow valve operating further open than normal.

Safeguard

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Thawing is the only solution when subcooler fouling occurs.

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