Caustic stress corrosion cracking in

contaminated steam system in CO2 removal unit

by Hani Ibrahim M.Elbassyouni, AlexFert, Egypt

4th Uhde Fertiliser Symposium 2010

Dortmund, Germany
May 19 – 21, 2010
AlexFert Profile

AlexFert is an ammonia urea

complex with capacity of 1200
TPD ammonia Uhde design.

2000 TPD granular urea

Stamicarbon licensed.

The company was established in

2003 and by July 2006 the
constructions finished and the
commissioning of the plant
starts.
Process Description

Uhde Co2 Removal unit

is based on the
conventional Benfield
process where carbon
dioxide is absorbed by
an aqueous potassium
carbonate solution with
diethanolamine (DEA)
added as activator and
potassium metavandate
as corrosion inhibitor.
 Background

Since the start-up of the plant, many

cracks were detected in the welds in
two of the steam lines connected to
the flash drum.

12 inch line : the first leakage started

during the commissioning stage and
ended up with five cracks in the
welds.

The other line is 36 inch between the

flash drum and the desorber,
leakage started at Jan. 2007 and
ended with three leaking points from
different three welds.
Case Study

In Aug. 2008 a leak was

detected from the breathing
hole in the reinforcement pad Pad Vent
Hole
between nozzle N6A and the
shell plate of the flash drum.

A vent line was erected to

collect the leak to safe area

A mixture of gases and the Vent line

liberated steam from the

regenerated solution go
through the nozzle to the
desorber.
12 inch Defected line
Gas Cooler

Desorber

36 inch Defected line

N6
A

Flash Drum
Desorber

Filter Pump

Solution Pump
Leak propagation

Following up the propagation of

the leaking point, visual
inspection and thickness
measurements were carried Leaking points
out.

The red points

Seven leaking points were indicate the defected
detected in the body of the areas

nozzle and the reinforcement

bad as shown in the figure.
Thickness measurements

The Line Nozzle “N6A”

X4 X2

Thickness measurements
were carried out and The Pad Flash Drum Body
X3
indicated that there was no X1
reduction in the thickness
around any of the leaking
points.
Temporary Repair

A clamp was erected to Sealing components
BTFE tape
maintain the operation till the Sealing components
shutdown. Clamp P1
Jack bolts
Clamp P2

On Oct. 2009, during the
plant shutdown the nozzle
Clamp P3
was cut out and replaced by
new one. Also, the
reinforcement pad and part of
the shell were replaced.

But, during the start of the

plant, anther nozzle starts to
leak from the breathing hole
in the reinforcement pad.
Failure analysis

Shell of the Flash

Drum Nozzle

After the Shutdown on Oct. 2009, 6A
P.T was carried out for the
defected portion of the vessel
and the old nozzle, indicated
more than one crack starting from
the welding between the shell
plate and the nozzle which
propagates in the base metal of
the two parts.
Stress Corrosion
Stress Corrosion Cracks
Cracks
Specimen Details

Specimens from the defected

area were sent to the Central Chemical composition of the
Metallurgical Research & sample for both shell plate and pipe
Development Institute (CMRDI)
in Cairo, the sample contain
parts from .
• The shell, material A516-60.
• The nozzle, material A106 –B.
• The reinforcement pad A516-60.

The chemical compositions

complies to ASTM requirements.
Investigations

P.T test for the specimen

indicates a crack of about 140
mm long in the inner surface of
the shell plate (fig. c).

Another crack was found in

the inner surface of the pipe
(fig. d).

Fine crack, as shown by arrow

in (fig. d) was detected in the
inner surface of the pipe
starting also from the pipe/shell
plate joint.
Macrograph Examination

The shell plate was welded

to the pipe from both sides
as a double bevel groove
joint.

The reinforcement bad was

welded to the pipe as single pipe

bevel and fillet weld joint.

Shell

Both welds were found to

be free from porosity and
slag inclusions.
Micro-analysis

Microstructure examinations were

carried out for the pipe and shell
plate base metals as illustrated in
the fig. which shows normal (a) shell plate.

elongated ferrite (white) – pearlite

(grey) structure.

(b) pipe

To check the crack morphology
through the thickness, sample
was taken from the cracked
portion approximately normal to
the principal cracking plane
through the wall thickness.

The sample had a branched

large crack initiating from the
inner surface and extending to
a depth of approximately 90%
of the wall thickness as shown
in the fig.

There were little secondary
branches and it was very
difficult to notice the path of
the crack. However, towards
the tip of the crack, the
tendency of branching was
increased.

Higher magnification
micrographs confirmed that the
crack tended to propagate
intergranularly in the ferrite grain
boundary and in the interface
between the ferrite and pearlite
phases.

A close up view at the crack tip,

as shown in (fig. d), shows
clearly that the crack tip was not
sharp but had a blunted shape.
which indicates that these cracks
were not initiated by mechanical
loading but rather by chemical
corrosion.
Material Analyze for Crack Area

X-ray spectroscopy was used

to analyze the elements inside
the crack.

The results were mainly iron
(56 wt.%) and oxygen (32 wt.
%), and a small concentration
of manganese (0.9 wt. %),
vanadium (3.2 wt. %), carbon
(0.7 wt.%) and potassium (6.5
wt. %)

The high contents of Fe and O2
probably refers to iron oxides
(corrosion products), while the
elements K, C, V came from
the potash lye solution.
Discussions & conclusions

Based in the investigation carried out and our past Experience, we

found that:
• The medium inside the nozzle was saturated low pressure steam
with traces of Potash Lye solution (K2CO3) at temperature of 100°C
and operating pressure of 0.5 bar.
• The material is normal carbon steel.
• No reduction in thickness were found in the cracked area.
• The propagation of the crack is intergranularly in grain boundary.
• The shape of the crack excludes the mechanical stress as possible
cause.
• The result of the investigation is identical to another failure analyses
done for the 12-inch line by The Welding Education and Consulting
Center (WELDECC) in Alexandria.
Caustic Cracking

Carbon steels are known to be susceptible to a form of stress

corrosion cracking known as caustic cracking Where steels
with low carbon and low alloy content may crack if they are
exposed to concentrated caustic environments with the metal
under a tensile stress.

In caustic cracking, cracks initiate and grow along the grain

boundaries in the carbon steel. Extensive crack branching is
also a distinguishing feature of caustic cracking .

Discussing the above points we can identify our case as one of

the most commen forms of stress corrosion cracking which is
causti cracking.

Susceptibility to caustic SCC is dependent on several variables,
including alloy content, caustic concentration, temperature and
stress level.

The driving force for crack propagation is a high tensile stress

applied externally to the steel and/or residual within the steel as a
result of fabrication.

Caustic cracking of carbon steel occurs over a wide range of

caustic concentrations. The lower limit for cracking appears to be in
the range of a few percent (by weight) of caustic

In pressure vessel, we could easily realize the source of stresses
as the residual stress from welding.

The residual stress in welds is developed by the differential

contraction that occurs as welds cool under restraint during vessel
fabrication.

These residual stresses remain in the weld and the adjacent base
metal unless they are relaxed either by a stress relief or by
cracking.

In our case, bad fitting and welding techniques in the manufacturing

workshop which we experienced in many cases during our
inspection visits helped to raise the residual stresses remaining at
the weld leading to this problem.
Recommendation

To reduce the danger of caustic stress corrosion cracking, we have

to reduce the major parameters affecting the initiating of the cracks
without touching the operating condition.

Possible and applicable solution were,

• Reducing the tensile residual stresses.

• Changing to higher resistance material.

We have applied the two solutions before.

• in the 36 inch line, One was replacing the material from carbon
steel to St. St. 304L and in this case we adopted this solution
considering that This line was under investigation with Uhde during
the ITB of AlexFert and the first part of the line along with the
ejectors were changed to St. St. 304L regarding our previous
experience in other ammonia plants in Egypt.

• In the other case (12-Inch line), our choice was to apply heat
treatment after welding to reduce the tensile residual stresses.

The two solution were successful and we have no problems in both

line after two years of operation.
Action Taken

After discussion with Uhde, We decided that changing the material

will be very expensive and we choose the second solution.

Heat treatment was applied after replacing the defected nozzle N6A
as temporary solution.

complete new vessel is under manufacturing to replace the

defected one and the entire vessel will be stress relieved by heat
treatment to reduce the residual stresses regardless of the
thickness requirements.
 Finally, thanks to the contrbution of

Uhde GMBH.

The Central Metallurgical Research & Development Institute
(CMRDI) .

The Welding Education and Consulting Center (WELDECC)