Major Ammonia leak incident in Urea plant

Oman India Fertiliser Company was commissioned in April-2005. The performance in the first five
commercial years of operation has been very good and all the envisaged project targets have been
accomplished. Meticulous Root Cause Analysis of the problems surfaced at various stages have been
analysed by the OMIFCO engineers in close association with the vendors and the consultants and
implementation of the identified corrective measures in the shortest possible time has been the key to
the achieved success of the company.
The paper highlights about a critical Ammonia leak incident that occurred in the Urea 21 plant and
how the situation was analysed to prevent re-occurrence of similar incidents. In chemical Industry,
Careful Root Cause Analysis of the problems is very important and complacency cannot be ensured
unless the remedies identified are convincing and consistent with the findings of the Root Cause
Analysis made.

S G Gedigeri
Oman India Fertiliser Company

Introduction surplus liquid ammonia annually for export,

using natural gas. Storage facilities for Urea (2X

O
MAN INDIA FERTILIZER 75000 MT) and Ammonia (2X30000 MT) as
COMPANY S.A.O.C. (OMIFCO) was well as jetty with ship loaders are part of the
set up as a joint venture project under project.
the initiative of Government of Sultanate of
Oman and Government of India. OMIFCO is
owned 50% by Oman Oil Company, 25% by
Indian Farmers Fertilizer Co-Operative Ltd
(IFFCO) and 25% by Krishak Bharati Co-
Operative Ltd (KRIBHCO). OMIFCO was
registered in the Sultanate of Oman as a closed
joint stock company in the year 2000.

The Ammonia Urea complex comprises two

trains, each with a design capacity of 1750
MTPD Ammonia and 2530 MTPD granulated
Urea, along with all supporting Utilities. It is
designed to produce total 1.65 million tonnes of Photo-01: OMIFCO Complex-Sur, Oman
granulated Urea and 0.25 million tonnes of

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 The complex has two service Boilers of capacity
2 X 70 MT/hr and two HRSG boilers of
capacity 2 X 110 MT/hr. Also the complex has
its own captive power plant with two 30 MW
Frame 6B Gas Turbine Generators and Import
power connectivity with the national grid for
backup power.
Description of the System:
OMIFCO owns and operates two Urea Plants
designed by M/S SAIPEM, Italy (Previously
Snamprogetti). The Urea manufacturing
technology used at OMIFCO is based on the
Ammonia Stripping Process.
To HP Stripper
CO2
High Pressure
Ammonia Pump P-101
Recycle Ammonium
Carbamate solution
Figure: 01
Location of the failed pipe:
The location of the failed weld joint was on the
pipe rack in the Urea-21 unit of the OMIFCO
complex. The pipeline going from the Ammonia
booster pumps common discharge to the
common suction of the high pressure Ammonia
feed pumps has several weld joints. One of the
weld joints nearer to the location where booster
pumps common discharge pipe line joins the
pipe rack had developed leakage during the
normal running of the plant and later failed
subsequently.
AMMONIA TECHNICAL MANUAL
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As per the process steps involved for producing
Urea, feed Ammonia is fed to the reactor at
elevated pressure. In the Urea plant the liquid
Ammonia at about 15°.C (59°.F) and 23.5 Bar G
(340.84 psig) pressure is initially received in an
Ammonia receiver (V-105). Later by using an
Ammonia booster pump (P-105-A/B), liquid
Ammonia is pumped to the suction of the high
pressure Ammonia feed pumps (P-101-A/B).
The high pressure feed Ammonia pump
transfers liquid ammonia to the Urea reactor
through an ejector where the liquid Ammonia
acts as a propellant for the high pressure
Ammonium carbamate solution. (Figure-01)
SCHEMATIC DIAGRAM FOR
THE INCIDENT LOCATION
Failure Location
21-HV-1021
Ammonia
Ammonia Booster Receiver-V-105
Pump P-105
Liquid Ammonia from
Ammonia Plant
Incident Scenario of Ammonia
Leakage:
In Urea-21 unit on 17th January 2008 at 04.40
hours the weld joint on the common suction line
of HP Ammonia feed pumps P-101 A/B had
failed and caused heavy Ammonia leak.
Immediately the plant emergency shutdown was
initiated and the affected system was isolated
and depressurized. Control valve 21-HV-1021,
located at the outlet of Ammonia receiver V-
105, on the common pipeline going to the
suction of P-105-A/B pumps was closed from
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 the central control room to isolate large
Ammonia hold up equipment like Ammonia
receiver V-105, MP Absorber C-101, and
Ammonia condenser E-109 from the snapped
off pipeline. This had helped in significantly
reducing the Ammonia quantity leaked into the
Atmosphere. A Level-1 emergency was
declared and all the affected area was cordoned
off and cleared of any workforce present in that
vicinity. As all the working staff moved to a
safe location nobody had received any
Ammonia exposure.

OMIFCO’S HSE (Health, Safety & Photo-02: Weld joint with Sealing Clamp.
Environment) team and the Production staff
controlled and confined the leakage to within
the plant battery limits by using their own fire
tender and the personnel protection appliances.

On scrutiny it was found that the elbow to pipe

spool piece of the line 8”-21-P57-53A-V on the
North-South pipe rack of Urea-21 plant had
snapped off. The plant was back on stream on
19th January 2008 at 10.50 hours after the repair
and rehabilitation of the failed pipe line [Photo-
05].
Photo-03: Counterparts of Off-centred pipe.
Pre failure history of the affected
pipe:
One of the weld joints, on the elbow to pipe
spool piece of the line 8”-21-P57-53A-V on the
North-South pipe rack leaked at the 4 o’clock
position. In the first week of Sept. 2007 the
leaky joint was sealed on line by means of
clamp [Photo-02]. It again started leaking
through the clamp on 4th Jan 2008 and an on
line sealing compound was re-injected to stop
the leakage. However, on 17th Jan 2008 morning
hours this joint fully snapped off from the weld
joint leading to leakage of substantial amount of
Photo-04: Side view of the snapped pipe.
ammonia [ Photos-03 &-04].

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 Investigation and observations:
This particular butt weld joint which had failed
circumferentially was in operation for a period
of 39 months, before its failure.

After the failure and after removing the on line

sealing clamp in the Visual examination the
following were observed:
Failed Weld Joint
• Complete snapping of the pipe at the failure
Photo-05: Pipeline view after rehabilitation. location from the weld joint.
• The weld joint failed circumferentially
through the butt weld only and not cracked
Detailed specification of the pipe: from the parent metal of elbow / pipe.
Line Number: 8”-21-P57-53A-V Rust marks were seen in the area adjacent to
•
Service Class: 53A (Mean Pressure the weld of painted pipeline. (Refer Photos
Ammonia - Ammonia 03 & 04)
(First & Second ST) – ID surface of the pipe looked blackish
•
Liquid Ammonia (With brown indicating a general form of
Stress Relieving) corrosion. (Photo: 03)
Pipe Material: A333 Gr.6 SMLS Fractured surface was flat and in transverse
•
(0.3 C% & 1% Mn.) direction. At one location weld material had
Normalized & tempered peeled off.
Steel
• The counterparts of the failed joint displaced
Design: Line Size 8” (203.2 mm) off center.
Sch. 20 (6.35 mm Thick) • Circumferential corrosion damage is seen
Temp. & Pressure: (-) 45 O C (- 49 °F) and near to the failure location where the paint
43 bar, (623.66 psi) peeled off precisely at the region of clamp.
Max Hydro Test 64.6 Bar. Abs (936.94 psi) • Fracture occurred perpendicular to
longitudinal direction and in a single plane
Pressure.
from the weld / HAZ region.
Corrosion Allowance: 1.27 mm (internal)
• Fracture surface comprised of both fatigue
(0.05 Inch)
and brittle nature. (Photos: 06 & 07).
WPS: SPC.WL.ES.360
• Low magnification view confirms cracking
Welding Class: 3T both from OD and ID and in the weld zone
PWHT: Yes, (All Thickness near weld HAZ (Photo: 06)
Require PWHT for this • SEM (Scanning Electron Microscopy)
Piping Class.) analysis confirmed that the cracking is a
As per ASME Sect-II Part ‘A and ASME Sec typical fatigue damage starting both from ID
IX for above grade material: and OD and assisted by mild corrosive
atmosphere. (Photo: 06)

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Photo-06: SEM Result showing Crack initiation &
propagation under the combined influence of
corrosion and fatigue.
• Crack movement was under the combined
influence of high cycle fatigue and corrosion
mode prevailed due to the marine
environment.
• Secondary cracks of corrosion fatigue were
also noticed on the fracture surfaces along
with corrosion products. (Photo:09)
• EDS (Energy Dispersive Spectrum) Analysis
confirmed that the corrosion damage on
fracture surface was due to salt containing
moisture from marine atmosphere. (Figure:
02)
• Overall microstructure of weld metal, HAZ
and parent metal was normal and acceptable
for the service. Pitting like corrosion damage
at OD surface was also seen. (Photos: 11 &
12)
Repair and rehabilitation carried
out:
The pipe spool piece was cut from the other end
also which was welded to the downstream side
elbow. Both the elbows ends bevel edges were
prepared by means of in-situ grinding. A new
pipe spool piece was cut from the pipe of same
size and same LTCS material grade available in
warehouse.
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The bevel edge preparation at both the ends of
the pipe spool piece was done as per the
approved WPS for proper fit up. After proper fit
up of both the elbow to pipe spool piece butt
weld joints for the root and fill for both the
joints was carried out by the TIG welding
process (GTAW) using 2.4 mm (0.094 Inch)
dia. filler wire ER 70S-6 as per the Welding
Procedure Specification (WPS) approved for the
given Pipe Service Class and Welding Class.
During the welding process an inter pass
temperature of 140 oC (284 °F) was maintained
by means of digital thermometer.
Dye Penetrant tests of both the root weld and
final weld joints were carried out. No defect was
observed.
Hardness of newly made 02 nos. elbows to pipe
weld joints was also checked on the weld, heat
affected zone (HAZ) and the parent metal in the
near vicinity and found to be within the
acceptable limit of 225 BHN.
Insitu Radiography of both the butt weld joint
was carried out using IR 192 source of four Ci
strength. No significant defect was observed.
Stress Relieving (PWHT) of both the weld
joints was carried out subsequently as per the
SR Cycle prescribed in the approved WPS as
mentioned below.
PWHT:
Heating: @ 150 °C (302 °F)/ Hr after
200 °C (392 °F)
Holding Time: 2.4 Minutes/mm of
thickness @ 600 to 630 °C
(1112 to 1166 °F)
(01 Hr Min. in this case)
Cooling: @ 150 °C (302 °F)/ Hr in air to a
temperature of 300 °C (572 °F).
Subsequently natural cooling in wrapped condition.
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 Hardness: Hardness measurement at the weld,
pipe and HAZ area after the PWHT was again
carried out and found to be within the
recommended limit of 225 BHN.

Non Destructive Tests carried out:

• Tensile test was carried out on the sample
and the results met the requirements of
ASTM A 333 Gr.6 material for tensile
properties.
Photo-07: Low Magnification View at the fractured
• V notch charpy Impact test was carried out Surface. Multiple origins observed from OD & ID
on the sample drawn at -56.0°.C. (-68.8°F) surfaces.
Impact test results met the requirement of
ASTM A 333 Gr.6 material.
• General hardness was measured at different
locations and results were found to be
matching with the requirements of ASTM A
333 Gr.6 material.

Causes of Failure:
• The pipe is exposed to sea water atmosphere
and the paint had peeled off at some places
near welding and corrosion has taken place.
• The failure had taken place on account of Photo-08: Low magnification (33X) shows multiple
fatigue cracking assisted by mild corrosion origins in the form of ratchet marks.
initiated at weld and HAZ both from OD and
ID. Fatigue was due to cyclic load caused by
unexpected shutdowns, start-ups, pump
change overs and vibrations on the pipe.
• The prevailing marine atmosphere, the
vibration stresses from the pipe line while in
operation and the surface corrosion that acted
as stress concentration site, had resulted in
corrosion fatigue.
• Low Magnification Examination confirmed
multiple origins of the cracks all over the
circumference starting from both OD as well Photo-09: Presence of corrosion products observed
as ID. (Photo: 07) at the cracked surface.

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 • Optical metallography indicated pitting like
damage on the OD surface of the pipe.
(Photo: 10)

Photo-11: Indicates that fracture has taken

place at the fusion zone and perhaps moved
into the weld.

Photo-10: Corrosion entering metal due to

pitting like surface damage at weld location

• Both SEM (Scanning Electron Microscopy)

Analysis and Optical Metallography
confirmed the failure to be on account of
high cycle fatigue arising out of system’s
cyclic operations and piping vibrations,
assisted by corrosion. Photo-12: Corrosion fatigue crack moving
precisely along the fusion zone of the weld.
• The cracking has taken place in the weld and
HAZ zone as seen in WFMPI (Wet
Fluorescent Magnetic Particle Inspection)
and Optical Metallography. (Photos 11, 12,
and 13)

• All the cracks are filled with corrosion

products. Even the secondary cracks seen on
the fracture surface were having corrosion
fatigue nature. ( Photo-09)

• EDS (Energy Dispersive Spectrum) analysis

confirmed that the corrosion damage on
fracture surface was due to salt containing Photo-13: WFMPI revealed Secondary
moisture from marine environment. (Figure- transverse hairline cracks at HAZ on the weld
02) ID surface.

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 Figure-02: Results of Energy Dispersive Spectrum.

Percentage Percentage
Elements Elements
Present Present
Oxygen 37.22 Chlorine 1.07
Sodium 1.31 Calcium 0.87
Magnesium 0.87 Iron 57.74
Silicon 0.93

• Presence of Oxygen, Sodium, Magnesium,

Chlorine and Calcium confirms that the
corrosion is induced by the Salty marine
atmosphere.

• HAZ microstructure shows slight inclination

towards having some internal stresses which
is reflected from micro-hardness values.

• The surface corrosion in form of tiny pits has

provided favorable sites for stress
concentration to take place both from OD and
ID
• Micro Structure examination has also
confirmed corrosion fatigue cracking having
trans granular nature of propagation.
(Photo:14)
• Matrix has banded ferrite and pearlite with
mild branching nature. (Photo:14)
Photo-14: Corrosion Fatigue Cracking-showing
trans granular nature of propagation. Matrix is
banded ferrite and pearlite.
• Crack observed adjacent to fracture surface
on pipe indicating another origin of fatigue
crack.
• The humid salty marine atmosphere
provided the climate for corrosion to take
place.

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 • Pipe has been supported especially at elbow
joint where the change in the direction of the
Liquid Ammonia takes place.
• The prevailing vibrations on the pipe line
induced the fluctuating stresses.
Figure-03: Micro Hardness Profile Diagram.
Most Probable Cause of failure:
• This failure might be due to corrosion,
material defect and internal stresses owing to
welding joint.
• The stresses might have developed on
welding due to injection of sealing compound
and clamping
Corrective Measures taken:
• Flexibility and stress analysis of the pipe
line from Ammonia receiver (V-105) to the
Ammonia Booster pumps (P-105-A/B) and
from the discharge of the Ammonia booster
pumps to the suction of the HP Ammonia
Pumps (P-101A/B) was carried out
separately by a reputed local consultant and
a foreign consultant of International repute.
• The reports indicated no over stressing at
any point in the pipe line and no alarming
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Thus, naturally the most vulnerable site for
corrosion fatigue damage to take place is weld
and HAZ.
Micro Hardness Profile did not indicate any
severe abnormality. Values at HAZ and Weld
were slightly on higher side (Refer Figure-03).
forces and moments are noticed at the
restrained points.
• Reports also indicated that stresses are
within the allowable limits and the failure
of pipe weld joint is not due to
overstressing.
• WFMPI (Wet Fluorescent Magnetic
Particle Inspection), testing and Insitu
metallography of all other weld joints on
the affected pipe line were examined and
those weld joints which did not pass all the
tests were repaired. Radiography was
carried out for checking the ID cracking.
• One new On-Off type control valve HV-
1013 has been installed on C-101 MP
Absorber outlet Ammonia vapours line in
both the Urea plants. This will facilitate
quick isolation of C-101 in the event of any
leakage (Figure-04).
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 E-109 To flare
Ammonia Condenser Cold
Condneate
Location of new ON/OFF E-111
control valve CW
Ammonia from B/L
21-HIC-1013 C-105

V-105

From MP Ammonia To Urea

Condneser Receiver Ammonia Reactor R-101
Booster Pump

P-105
C-101
MP Absorber
P-101
H.P Ammonia feed Pump To MP Decomposer
or Flare
LP Steam
P-102
Carbamate Recycle Pump V-101
Carbamate Separator
Condenate Carbamate
HP Stripper Over head Vapors
Condenser

Figure-04: NEW CONTROL VALVE AT THE VAPORS OUTLET OF C-101

• New on line Breathing Air sets with
extendable hose of 50 meters length have
been provided inside the plant field area to
facilitate quick isolation in the event of
Ammonia leaks.
• Care is being taken for the quality of the
painting on the pipe surface particularly
near weld joints to avert peeling of paint
and subsequent underneath corrosion
damage.
• Much lower failure stresses and much
shorter failure times can occur in a corrosive
environment compared to the situation
where the alternating stress is in a non-
corrosive environment.
• OMIFCO has decided not to do online
sealing for any developed leakages of
Ammonia pipe lines.

Conclusion:
• Corrosion-fatigue is the result of the
combined action of an alternating or cycling
stresses and a corrosive environment.
• On line sealing of leakages either from pipes
or weld joints should be avoided which
otherwise might cause inadvertent additional
stresses, to the component which has been
already under the influence of some parental
residual stresses.
• Contrary to a pure mechanical fatigue, there
is no fatigue limit load in corrosion-assisted
fatigue.

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