Paper 3e

Failure of a Titanium Lined Vessel

due to Sudden Application of
Vacuum
The titanium liner inside a separator collapsed due to rapid vacuum formation during startup, when the
normal startup procedure was not followed.
This paper describes the initial unsuccessful attempts to repair the failed liner in situ, and its subsequent
successful replacement with a new duplex stainless steel liner. The root cause of the vacuum formation is
explained, and modifications to prevent recurrence are described.

Les Farbotko, Angus Dowrie, Steve McGuire

Incitec Pivot Limited

Introduction Modifications to prevent recurrence were in the

form of an instrumented protective system, as

I
ncitec Pivot Limited (IPL) is the largest man-
ufacturer and distributor of nitrogen products
and fertilizers on the East coast of Australia.
At the Gibson Island site in Brisbane, Queen-
sland, IPL operates a Vulcan urea plant, of na-
meplate capacity 640 MTPD, which has been de-
bottlenecked to about 900 MTPD.
well as changes to the format and structure of op-
erating procedures.
Some important lessons were learned regarding
operations culture and “blind spots” in relation to
equipment reliability risk assessment.

In late September 2007, a titanium-lined separator The CPI-Allied Urea Process

in the urea plant was observed leaking ammonia
gas from its telltales during plant startup. On in-
spection, the titanium liner was found to have col-
lapsed.
Initial attempts to repair the liner in situ were un-
successful. The vessel was removed to a work-
shop, where the titanium liner was removed and a
new duplex stainless steel liner installed.
The collapse was attributed to a vacuum forming
rapidly in the plant on startup, when the normal
startup procedure was not followed.
IPL’s urea plant is based on the CPI-Allied urea
process. It was engineered by Vulcan Cincinnati
Inc., and was commissioned in 1969.
This is a once-through process (NH3 and CO2
feeds only), with a reactor operating at 5400 psig
(37 MPag), at an NH3/CO2 ratio of about 4.6 and
an outlet temperature of 430 oF (220 C).

2009 155 AMMONIA TECHNICAL MANUAL

 NH3 Vapor

NH3 Reflux
Lean MEA
PRIMARY PRIMARY
DECOMPOSER ABSORBER
UREA
REACTOR

SEPARATOR Rich MEA

T-745 to Desorption
NH3 CO2

Urea Solution
to Evaporation

Figure 1: CPI-Allied Urea Process – Front End

Unconverted ammonia and carbon dioxide are When the system was repressurized on startup,
treated in an anhydrous MEA (monoethanola- gas was seen coming from the telltales on T-745.
mine) separation system where they are separated
and recovered. On inspection, the titanium internal liner of T-745
was found severely damaged: bulged and buckled,
After letdown, reactor contents flow through the with a number of creases, folds and tears.
steam-heated Primary Decomposer, where uncon-
verted ammonium carbamate is decomposed, and
into the Separator T-745. Here urea solution is se-
parated from the excess ammonia and uncon-
verted carbon dioxide, which are sent to the Pri-
mary Absorber of the MEA system. T-745
normally operates at about 265 psig (1830 kPag)
and 310 oF (154 C).

The Incident
The plant had been shut down three days pre-
viously to replace a rupture disc at the inlet of the
Primary Decomposer that had failed prematurely.
This required the entire synthesis section, includ- Figure 2: Bulges and creases in bottom head.
ing T-745, to be drained and depressured.

AMMONIA TECHNICAL MANUAL 156 2009

 The damage was clearly the result of application
of vacuum, followed by repressurization.
Within a matter of minutes, we had destroyed the
integrity of a liner which had provided superb
service for 38 years.
Figure 3: One of several liner tears.
The immediate challenge was to repair the vessel
as quickly as possible, however it was essential
that we also identify the root cause and implement
preventive measures.
Repairs
Vessel and Liner Details
T745 is a vertical cylindrical pressure vessel de-
signed to ASME VIII, originally fabricated by
Wyatt Industries of Houston, Texas. It has a di-
ameter of 10’0” (3.05 m) with 7’7” (2.31 m) tan-
to-tan length, semi-elliptical ends, with a design
pressure of 300 psig (2070 kPag). The vessel has a
steam jacket and a loose titanium liner to protect
the carbon steel shell from the highly corrosive
urea solution.
The titanium liner is not capable of resisting the
normal process pressure. It deforms elastically
under pressure to push against the carbon steel
shell, which is the main pressure resisting compo-
2009
nent. The pressure vessel is enclosed in a steam
jacket. The outer wall of the steam jacket is
welded to the pressure vessel at the nozzles leav-
ing an annulus for steam underneath. The vessel
has tell-tales which are designed to leak in the
event of a failure of the internal liner.
The titanium liner is 1/8” (3.2 mm) thick, and (be-
fore the incident) conformed very closely to the
shape of the pressure shell.
Figure 4: T-745 through-wall section
Internals consist of an entry pipe that provides a
tangential flow below a baffle and skirt, which fa-
cilitate disengagement of the urea solution from
the vapors. Apart from a cone at the vapor outlet,
there is no demister or other secondary liquid se-
paration device. The urea solution flows through a
heated falling-film stripping section at the bottom.
The two basic options open to us were to repair it
in situ or to remove the vessel to an external
workshop. In either case removal of the damaged
areas was required and this commenced imme-
diately.
157 AMMONIA TECHNICAL MANUAL

Inlet
Figure 5: T-745 schematic
In situ Repairs
T-745 is in a confined area of the plant, which
makes its removal a difficult and time-consuming
exercise. In the past, we had successfully repaired
another lined vessel, the Primary Absorber, in si-
tu. These two factors pushed us towards the in situ
repair option at first, although some planning ef-
fort was also spent on the remove-to-workshop
option as a back-up.
When the vessel was originally constructed, we
believe the titanium liner was fabricated first,
(with butt-weld joints), which provided full access
to both sides of the liner, allowing a back-purge
during the titanium welding process. The pressure
shell was subsequently built around the liner using
backing bars on the carbon steel shell welds. It
was not possible to duplicate this arrangement
during the in situ repair, so we had to use fillet or
lap welds, which are fundamentally weaker.
Close fitment of the repair pieces was required, as
fillet welds are inherently less able to elastically
deform. This factor was known from the start, but
our previous successes and the likelihood of a
significantly shorter repair time overcame those
concerns.
New titanium plate was sourced, cut and bent to
shape, then positioned and lap-welded to the orig-
AMMONIA TECHNICAL MANUAL
inal plate. Every effort was made to achieve a
tight fit-up, however, the liner failed at one of the
lap welds under hydrotest. Excessive deformation
under pressure was the cause, simply because the
new titanium sections did not conform closely
enough to the shell.
Several attempts were made to limit liner deflec-
tion by injecting ”Belzona” between the shell and
liner where gaps existed. This was partly success-
ful, but the method required a trial-and-error ap-
proach which took valuable time. After several
more unsuccessful hydrotests and further streng-
thening of the welds, we believed we were closer
to success; however no one could predict how
long it would take to get there.
There was also no guarantee of the robustness of
the final product – the failures under hydrotest
suggested that failures in service would be likely.
Workshop Repairs
While the in situ repair attempts were taking
place, a lot of planning was happening in the
background with regard to removing the vessel to
a workshop. Once the plan had been fully devel-
oped, the decision was taken to proceed with that
option. We accepted the likely additional down-
time that would entail, however there was greater
certainty of plant reliability down the track.
The major concerns were to ensure a robust and
reliable repair, and to carry it out in as short a
time as possible. Consultation with industry ex-
perts and previously successful application in sim-
ilar service in our plant led to us choose a duplex
stainless steel, Sandvik SAF2205, for the new lin-
er. This had advantages in availability and welda-
bility in comparison with titanium.
Stelform, a company in Newcastle (approx 500
miles or 800 km south of Brisbane) with which
IPL have a long association, were able to make
space in their workshop at short notice. The
pressed sections around the semi-elliptical ends
were provided by Wenco, a company located near
158 2009
 Perth on the opposite side of the country, so there
was a significant logistical angle to the whole re-
pair.
All of the titanium liner and internals were to be
replaced. Rather than working through a manway,
we cut the vessel in two to facilitate access for
men and materials. A lot of care was taken with
match-marking and ensuring flange stand-offs
were the same as original, since we did not want
to have to make field corrections to the connecting
steam-jacketed piping.
The duplex plate used was ¼” (6.4 mm) thick, in-
stead of the original 1/8” (3.2 mm) thick titanium
plate. This was due partly to availability, but also
to a desire to provide better vacuum capability.
The SAF2205 plates were butt welded, and also
fused to the carbon steel shell through the weld
root. The consequence of attaching the shell to
the liner was that leakage paths no longer existed.
To counter this, bridges were made in sections of
the welds to ensure there was always a leakage
path from any point on the new liner, to provide
early indication of a liner failure.
A detailed quality plan which covered all aspects
of vessel removal, transport, repairs, re-
installation and commissioning was developed
and applied to ensure a successful repair.
Total urea plant downtime from this incident was
twelve weeks.
Vacuum Capability of New Liner
The original liner clearly had negligible vacuum
capacity. (We estimated less than 1 psig or 7 kPag
of vacuum.) Ideally, the new liner would have
been rated for full vacuum, however this was not
possible with the ¼” (6.4 mm) material used. We
were able to design it for a “half-vacuum” (-7
psig, -50 kPag). Coupled with other measures
such as an instrumented protective system, this
was considered sufficient to prevent another fail-
ure at any future time. In the ordinary course of
events, the material thickness would have been se-
2009
lected to permit full vacuum (and thus design out
the problem), however this was not possible due
to time constraints and material availability.
Root Cause of the Vacuum
That we had experienced a vacuum event was un-
deniable. What was not known was when exactly
this had happened, and how?
We examined the shutting down and starting up
phases in great detail.
Procedures
Both our shutting down and startup procedures
had been in use since at least 1970. We had a
wealth of successful experience with both, and
had been confident in them, yet some aspect had
failed.
A review of the original Vulcan Operating Ma-
nual revealed that the original designers had envi-
saged the use of nitrogen to purge air from the
system on startup, however this procedure was
never used.
Shutdown Procedure
Our standard shutdown procedure for this section
requires it to be depressurised to the low-pressure
section downstream for ammonia recovery. The
last traces of ammonia are then steamed out
through the Primary Absorber top vent, the system
is finally air blown, and the vent left open.
Nothing untoward was found in the technicians’
logs or in questioning. Similarly, nothing in the
plant data trends suggested we had pulled a va-
cuum during any of these operations.
(One of the difficulties here was the fact that all of
our pressure transmitters in this part of the plant
are ranged from zero gauge pressure upwards.
159 AMMONIA TECHNICAL MANUAL
 None are calibrated to read vacuum - no one ever
expected to need to read negative pressures - so
inferences needed to be made from other process
variables, such as temperatures.)
Startup Procedure
Typical startup procedure is the reverse of shut-
ting down: Air in the system is steamed out, the
vent is closed and the system is immediately pres-
surised with ammonia vapor. Only then is MEA
circulation started, since it needs pressure in the
Primary Absorber to push the liquid level out.
Close examination found that some pressures and
temperatures had fallen part way through startup,
an unusual occurrence. Caution was needed inter-
preting the pressure transmitter readings: Ranged
0-400 psig (0-2800 kPag), how accurate would
they be at 2-3 psig (14-20 kPag)? We also found
that many temperature indicators were ranged
from 200-400 oF (93-204 C), so were out of range
during the abnormal conditions of shutdown and
startup.
By cross-referencing the changes in the process
variables that we could trust against the techni-
cians’ activities, it became evident that there had
been deviations from the usual startup procedure.
System Blocked in after Steaming
We observed that the steam purge, which had
been started on night shift, had been turned off at
about 07:30. The vent valve had been blocked in
when steam was turned off, but the system had not
been pressurised with ammonia.
This in itself had the potential to pull a vacuum,
however the thermal mass of the system is large
enough that it does not cool rapidly. We con-
cluded this did not create the damaging vacuum.
MEA Flow Started
It is normal to start an MEA flow and establish a
level of MEA in the Primary Absorber. However,
AMMONIA TECHNICAL MANUAL
this step is normally done AFTER pressurizing
the system with ammonia vapor.
By the simple reversal of these steps, we had de-
stroyed our titanium liner.
When steam purging had stopped, the system was
full of steam at near-atmospheric pressure. Start-
ing a flow of MEA across the trays of the Primary
Absorber tower created ideal conditions for rapid
condensation of the steam into the cold MEA.
With the vent valve closed, there was no opportu-
nity to draw in air to break any vacuum that de-
veloped.
How much vacuum we pulled is not certain.
Based on temperature indications in different
places, we believe it was definitely below -3 psig
(-20 kPag). There are indications it may have been
reached as low as -11 psig (-75 kPag), in less than
a minute.
Pressurization with Ammonia
When the system was finally pressurized with
ammonia vapor (almost two hours later), the dam-
age to the liner had already occurred. However, to
compound matters, the pressurization rate was
unusually rapid, which probably was responsible
for some of the tearing and creasing we found on
the titanium liner, as the deformed liner was ra-
pidly forced back against the pressure shell.
Other Consequential Damage
We needed to reassure ourselves that the vacuum
had not damaged any other equipment. Rather
than open up and inspect everything, we opted to
do a detailed desktop evaluation of all compo-
nents that may have been affected. In some cases
this required considerable engineering calcula-
tions.
The Urea Reactor was our greatest concern. Our
reactor has an inner basket of zirconium, which
contains the reaction mixture, and is surrounded
by purge water which overflows into the inner
160 2009
 basket at the top. The pressure shell itself has an
inner lining of 316L stainless steel, which is
welded at intervals to the carbon steel shell.
CS Shell
316L Liner
Steam Jacket
Zirconium
Basket
Figure 6: Reactor schematic
The vapor space connection between the inside of
the zirconium basket and the purge water annulus
allowed pressure to be equalized on both sides, so
the basket was believed safe. Calculations con-
vinced us that the stainless steel liner on the pres-
sure shell was adequately fastened to the shell, so
that it would withstand full vacuum. In any case,
the actual vacuum reached inside the reactor was
limited by the small size of the orifice in the reac-
tor letdown valve (open at the time of the inci-
dent), and boiling off of purge water in the annu-
lus.
We physically inspected the trays in the Primary
Absorber, to ensure they had not suffered any
damage.
We found no other damage.
2009
Preventing a Recurrence
Process Hazard Analysis
Having our minds focused on vacuum, we brains-
tormed all possible causes, and reviewed their li-
kelihood and potential to cause damage.
We identified two situations where deep vacuum
could be created rapidly:
1. Absorption of steam by an applied liquid
flow (MEA or water) – as had happened,
and
2. Absorption of ammonia vapor by an ap-
plied liquid flow (MEA or water).
There were also a number of other causes identi-
fied (natural cooling and condensation of blocked
in steam; rapid draining of a liquid-filled system;
cooling of a hot non-condensable gas; and exter-
nally applied vacuum) however these were either
unable to reach very low and damaging pressures,
or low pressures would only form slowly.
All of these scenarios only occur during abnormal
operating states: starting up, shutting down, or
while the plant is offline for maintenance. How do
we guard against all of them?
We considered reverting to use of nitrogen to
purge the system on startup, however this would
have added considerably to startup time and cost.
It would also not have eliminated all of the other
possible causes (e.g. ammonia absorption) or cov-
ered the other situations.
We had lost the opportunity to design out the
problem when we decided not to make the new
liner full vacuum rated. Hence we were forced to
consider add-on vacuum protection facilities.
Protective Systems
Our initial focus was on a vacuum breaker, how-
ever we soon realized that letting air into a system
that might contain hot (and flammable) MEA was
161 AMMONIA TECHNICAL MANUAL
 not the smartest move. Using nitrogen (instead of
air) would have worked, except for the large vo-
lume that would be needed in a very short time.
We finally opted for an instrumented protective
system, which, in summary, achieves the follow-
ing:
1. To prevent rapid vacuum formation:
• Shuts off the MEA flow if pressure
falls below a preset minimum (80 psig
or 550 kPag);
2. To prevent slow vacuum formation:
• If pressure is low (< 5 psig or 35
kPag) AND the vent valve is shut,
starts a steam flow to the Primary Ab-
sorber.
• If pressure goes negative, starts a
steam flow to the Primary Absorber
(irrespective of vent valve position).
These responses are activated by a 2 out of 3 vot-
ing system in a high integrity PLC, in a system
with an overall SIL rating (Safety Integrity Level)
of 1.
General Lessons
Clearly, failure to adhere to our startup procedures
was the root cause of the vacuum event; however
there are some important lessons here that are
broadly applicable.
Risk Assessment
IPL has a strong focus on equipment risk assess-
ment as a means of minimizing safety hazard and
maximizing plant reliability. Nevertheless, the
possibility of vacuum occurring and causing a ma-
jor vessel failure had never occurred to anyone.
Rule-of-thumb is that a vessel designed for 300
psig (2 MPag) will withstand full vacuum. T-745
had been designed for 300 psig (2 MPag) (and our
Reactor for 6600 psig or 45.5 MPag). How could
such vessels fail under vacuum?
AMMONIA TECHNICAL MANUAL
No one had made the mental connection that the
titanium liner was not a structural part of the ves-
sel. It was a classic blind spot that cost us dearly.
(A slightly different mental leap is the considera-
tion of applied external pressure to vessel liners
e.g. applying air pressure to a vessel’s telltale to
find an internal liner leak.)
Training, Procedures and Operating Culture
Until fairly recently, our operating workforce had
been quite stable, with average length of service
of 18-20 years, and had considerable experience.
These older operators were predominantly trained
on the job by their predecessors and therefore
many had learned to complete tasks in different
ways.
About 10 years ago, we set up our own internal
Training Group, and developed Training Guides
and Competency Testing, which were applied to
new hires and anyone learning a new plant area.
There was also a greater focus on written proce-
dures, and we had gone through various formats.
Our original procedures had evolved from the
Vulcan operating manuals, however many were
used as guidelines to achieve an outcome in the
plant, i.e. plant startup, but weren’t necessarily
prescriptive on the actions to take. Consequently,
different shifts, for example, would start the plant
in slightly different ways.
(The smaller percentage of newer employees that
had trained on the new system were generally
more consistent in following procedures.)
It is also probably fair to say that some of our key
procedures were generally wordy, with a lot of
specific cautions and detail about hazards to
avoid.
We believe that the combination of the culture of
operator discretion and the absence of a clear “DO
THIS; THEN DO THAT” message contributed to
162 2009
 the failure of T-745 when the procedure steps got
out of sequence. This was one of the root causes
of the vacuum event.

We have since introduced prescriptive procedures

that remove discretion and require signoff after
each step. These new procedures may not be de-
viated from without authorization.

Conclusions
1. Vessel liners may not have the same struc-
tural integrity as the vessel they form part
of, and need to be considered separately
and carefully in any risk assessment. In
particular, vacuum rating needs to be tak-
en into account, as well as applied exter-
nal pressure.

2. Operating procedures need to be re-

viewed, to ensure that steps taken out-of-
order will not have unwanted conse-
quences. If such situations exist, then no
discretion to deviate from the written pro-
cedure can be allowed without formal au-
thorization.

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AMMONIA TECHNICAL MANUAL 164 2009