High Pressure Carbamate Condenser

Leak Detection and Control

SAFCO has experienced a leak in the High Pressure Carbamate Condenser of the Urea plant, twice.
As a result, a technical in-house team has studied and developed a methodology for detecting and
monitoring the leak until it can be fixed. The developed method has helped in enabling operation of
the HPCC equipment in the first instance, for more than 14 months and in the second, for more for
10 months.

Khaled Abdul Aziz Al-Khuraimi

SAFCO

Introduction Problem Statement

S AFCO is one of the leaders in the

fertilizer sector, worldwide. It has four
urea plants - three of them are
Stamicarbon licensed with a total design
capacity of 8,700 MTPD. The SAFCO-2 urea
In June 2012, a leak was detected in the HPCC.
It was kept in service under very close
monitoring until its scheduled replacement
during the turnaround in April 2013.

plant is a Stamicarbon licensed plant built by

Chyoda. The name plate capacity of this urea
plant is 1,800 MTPD, and the normal plant load
is 108% to 111%.
The high pressure carbamate condenser (HPCC)
of SAFCO-2 has been in service since
commissioning in 1992. The total number of
on-stream time since commissioning is close to
21 years.
Process Description
The SAFCO steam/ condensate system is a
semi-closed loop, as shown in Figure 1. The
source is from extraction of steam turbine
(TS102). Steam is generated in the HPCC
(E202) steam drum vessel (V904A/B) and
condensed in the stripper (E201) steam drum
(V905), rectifying heater (E302), and evaporator
(E401) steam drum (V903). The SAFCO-2 urea
plant is the only one of the SAFCO plants that
uses condensate from the desorber as feed to the
steam drum, V-904A/B.

2013 65 AMMONIA TECHNICAL MANUAL

 Figure 1. SAFCO-2 steam/condensate circuit
Conductivity in the system is measured online
in two locations – the turbine condensate and
the desorber outlet (C802). Routine monitoring
of the system is done using the turbine
condensate meter, the desorber outlet meter, and
the steam drum, V-904A/B blowdown lab
analysis.
Background History and
Observation
The background and history can be summarized
in the following points:
 In December 2011, the hydrolyzer level
transmitter malfunctioned, resulting in
turbine and desorber conductivity increasing
above the limit of 10 and 15 μS/cm·s,
respectively (turbine condensate and
desorber conductivity are normally less than
10 and 15 μS/cm·s, respectively).
 Until May 2012, it was observed that
increasing conductivity in the turbine
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condensate had a direct relation with the
desorber outlet conductivity.
 From December 2011 until May 2012, the
turbine condensate conductivity and
desorber conductivity increased above the
limit of 15 and 20 μS/cm·s, respectively.
 On June 18, 2012, the hydrolyzer level
transmitter was replaced. The desorber
conductivity returned back to its normal
value of less than 15 μS/cm·s, however the
turbine condensate conductivity did not
decrease.
Leak Detection Methodology
All observations in the previous paragraph
indicated a leak in the system. The following
steps were taken to identify the leak:
1. List all the possible causes.
2. Trace the leak.
3. Prepare an action plan.
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 Possible Causes
All possible causes were brainstormed and
listed. The list was classified into minor and
major points. As the leak amount was small and
only slowly increasing, it was assumed that it
was from a minor point such as non-return
valves (NRV), steam jacket, the nitrogen:carbon
ratio (N/C) meter, or steam traps. It was also
considered that the leak could be from a major
source such as equipment or the feed itself.
The minor leakage points are as follows:
1. Urea melt header into the steam jacket,
2. N/C meter into the steam jacket,
3. Carbamate pump into the steam jacket, and
4. Urea solution transfer line1 steam jacket.
The major leakage points are as follows:
1. Make up water quality,
2. Tube side leak from the rectifying column,
3. Tube side leak from the evaporator,
4. Desorber outlet condensate quality,
5. Tube side leak from the HPCC, and
6. Tube side leak from the stripper.
Tracing the Leak
Leak source detection was done, starting from
the minor points, by checking the suspected area
physically, isolating the suspected source to
check the effect on the system and taking lab
analyses. The investigation was conducted as
follows:
Minor Points:
1. The health of steam jackets and N/C meter
were checked and found to be in normal
condition.
Major Points:
1. Make up water quality – Make up steam
condensate from V-905 via stripper was
analyzed for pH, conductivity, NH3, and
1
In SAFCO there is a grid connection between all urea
plants that is used for transferring urea solution in the case
of a shutdown.
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CO2. Results were normal as pH was 8.2,
conductivity was 4.6 μS/cm·s, and no NH3
or CO2 was detected.
2. Tube side leak from rectifying column –
E-302 steam inlet and condensate outlet
samples were analyzed for pH, conductivity,
NH3, CO2 and urea. Results at the inlet and
outlet were the same. Some results showed
higher NH3 at the inlet compared to the
outlet, which was due to temperature
difference. To double check, the outlet
condensate from the rectifying column was
isolated from V-903 and diverted to the
waste water tank (T-901), but conductivity,
NH3 and CO2 measured in V-903 remained
in the same range.
3. Tube side leak from evaporator – The
evaporator tube side operates under vacuum,
so in the case of a tube leakage, steam will
go into the process side diluting the urea
melt. Thus, there is no chance for urea to
come out to the shell side under normal
operation. To double check, a sample was
taken and the results showed pH,
conductivity, NH3, and CO2 were the same
as the rectifying column and no urea was
found in V-903. Also, urea melt going from
the evaporator to the granulator was normal
and there was no change in urea solution
concentration.
4. Desorber outlet condensate quality –
Desorber outlet condensate was affected to
some extent, but when the desorber
condensate supply to V-904A/B was
isolated, the conductivity reduced from 21 to
8.6 μS/cm·s and then remained constant.
5. Tube side leak from HPCC – Condensate
inlet and steam outlet were analyzed for pH,
conductivity, NH3, and CO2. Concentrations
of CO2 and NH3 in V904A/B were higher
than the other places. Repeated samples for
HPCC inlet and outlet revealed a minor leak
in the equipment.
6. Tube side leak from stripper – Make up
steam condensate coming from V-905 via
the stripper was analyzed for pH,
conductivity, NH3 and CO2. The results
67 AMMONIA TECHNICAL MANUAL
 were normal and no NH3 or CO2 was
detected.
Inspection Report
The last inspection for the HPCC was done in
November 2010. The inspection found stress
corrosion cracks in the material of the tube due
to chloride. The chloride was from upsets in the
condensate coming from utilities, which
occurred in the past, causing chloride to stay in
the crevice. A tube crack is as shown in Figures
2 and 3.
Figure 2. HPCC tube crack
Figure 3. Microscopic picture of the crack
Based on the inspection report, the leak source
was assumed to be from the following:
1. A leaking tube, caused by stress corrosion
cracking due to chloride attack.
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2. A leaking tube-to-tube sheet (TTS) weld,
caused by stress corrosion cracking due to
chloride attack.
3. A leaking welded tube plug from a
previously plugged tube.
In order to trace the source of the leak an on-line
inspection of the HPCC top and bottom tube
sheet’s outer periphery was conducted by
Stamicarbon. The inspection result was found
to be acceptable.
Impacts and Mitigation Action Plan
The following are the impacts of operating
under the conditions described above:
 Corrosion in steam and condensate circuit.
 Corrosion in the turbine.
 HPCC failure before turnaround.
Based on the existing situation and the previous
experienced with a HPCC leak in SAFCO-3, it
was agreed to operate the plant under close
monitoring and control of the conductivity and
ammonia content. The measured values of
conductivity and ammonia indicated a very
small leak, so it was believed that there was a
minor risk for corrosion and further damage.
The following action plan was developed and
implemented to manage the potential impacts:
1. Monitor the top and bottom HPCC lab
analysis for NH3 and CO2 pick-up, pH and
conductivity.
2. Monitor the turbine condensate conductivity
analyzer and lab analysis for NH3 and CO2
pick-up, pH and conductivity.
3. Divert the admission steam to vent when the
cation conductivity crossed the limit of
5 μS/cm·s.
4. An on-line inspection of the HPCC top and
bottom tube sheet’s outer periphery was
done. The inspection result was found to be
acceptable.
5. Clear limits were also agreed upon, so that a
shutdown has to be taken in case those limits
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 were exceeded. These limits were as
follows:
 A sudden change in conductivity
(increase or decrease).
 An increase in the NH3 from the HPCC
above 50 ppm (based on experience with
a high pressure scrubber leak where the
leak could not be detected below this
value).
 Keep the pH of the steam condensate
system above 8.5 (preferably above 9) to
minimize the risk for corrosion in the
steam condensate system.
 In order to save the turbine, the cation
conductivity limit was 5 μS/cm·s (also
based on experience).
6. In case the leak crossed the limit, the
equipment has to be repaired or replaced if
the new equipment was delivered (new
HPCC Top
pH Conductivity
300
250
pH & Conductivity
200
150 Normal Operation
100
50
0 0
Figure 4. HPCC leak trend after Oct 2013 crash shutdown
Conductivity had increased sharply during the
low load period due to fluctuation in the
differential pressure across the HPCC. After
increasing the plant load, the reduction in
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equipment was ordered after the crack was
found in the last inspection).
Monitoring and Control
It was agreed to operate the plant under close
monitoring and control of the conductivity and
ammonia content. The measured values of
conductivity and ammonia indicated a very
small leak, so it was believed that there was a
minor risk for corrosion and further damage.
Equipment leakage was increasing at a very
small rate, reaching a value of 60 μS/cm·s. The
leak continued in the same increasing rate until
October 2012 when a crash shutdown occurred.
After the shutdown, the leak quantity declined,
but still had the same increasing rate, as shown
in Figure 4.
NH3 CO2 Poly. (Conductivity)
250
Low Load
200
NH3 & CO2 pick up
S/U after 
unplaned S/D 150
100
50
conductivity was possibly due to presence of
corrosion products in the crevice, which
partially blocked the leak point.
69 AMMONIA TECHNICAL MANUAL
 SAFCO-3 Case Benchmarking
The HPCC leak in SAFCO-2 was the second
case of such a scenario within SAFCO plants.
Therefore, the SAFCO-2 HPCC leak case was
benchmarked with the previously experienced
leak in the SAFCO-3 plant.
The SAFCO-3 HPCC exchanger leak started on
September 9, 2010, and contaminated the entire
steam and condensate circuit. About 30 MTPH
(33 STPH) of steam was vented to atmosphere
as admission steam, while about 40-45 MTPH
(50 STPH) of desorber condensate was dumped.
Even so, the leak amount had crossed
2000 µS/cm·s and NH3 pick up across the
HPCC was more than 700 ppm. The plant load
was maintained at full load (114%).
The plant was closely monitored for pH,
conductivity, NH3 pick up from the HPCC, and
iron (Fe) content. As the leak was high but only
increasing by a small rate, the decision was
made to keep the plant running with close
monitoring for the mentioned aspects. The leak
behavior was fluctuating up and down following
the system pressure fluctuation. By the end,
equipment ran around 14 months until a planned
shutdown was taken to inspect and fix the
problem.
Based on the last inspection report, it was
expected the leak source was a leaking tube.
Even so the following scenarios were assumed:
1. A leaking tube caused by stress corrosion
cracking due to chloride attack. Chloride
analyses of steam condensate (V-904) for
the last three years remained less than
0.05 ppm, except on September 11–12,
2010, when it reached as high as 3.3 ppm
due to an upset in the utility
demineralization unit.
2. A leaking tube to tube sheet weld due to
thinning of tubes was unexpected to happen
as the tube to tube sheet weld was found to
be satisfactory.
3. A leaking tube plug.
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Regardless of the source of the leak, action
plans to fix the problem were developed as
follows:
1. On short notice until a plant shutdown,
monitor the conductivity, NH3, CO2 and Fe
in the HPCC.
2. It is not mandatory, but advisable to treat the
unit with 2% trisodium phosphate (TSP), to
slow down stress corrosion.
3. During a shutdown, pull a suspected tube for
further investigation to confirm the presence
of chloride stress corrosion cracking.
4. During a shutdown, find the leak and repair
as there is a risk of corrosion of the C-steel
tube sheet.
Results after the shutdown and repair were as
follows:
 A total number of 16 tubes were plugged
with a reduction in the heat transfer of only
0.5%.
 The vented admission steam of 30 MTPH
was recovered.
 30 MTPH (33 STPH) of desorber water
contaminated with ammonia was recovered.
 Total recovery of steam as well as process
condensate was 60 MTPH (STPH).
The main cause of the leak was the TTS weld
joint pin hole (Figure 5). Carbamate passed
through this pin hole with high pressure,
initially eroded the stainless steel layer (8 mm,
5
/16 in thick) and then corrosion started at the
carbon steel portion (475 mm, 18.7 in thick).
The cavity was up to 350 mm (13.8 in) deep and
125 mm (4.9 in) wide (Figure 6). The
remaining portion of the CS intact was only 125
mm (4.9 in).
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 TTS pinhole
leak from
tube 36 N 1W
Figure 5. Initial pinhole leak where cavity
started
Figure 6. Corroded area after grinding
The present repair (Figure 7) is only a
temporary measure. SAFCO inspection and
Stamicarbon indicate the HPCC is to be
replaced at the soonest possible time. Based on
the inspection report issued, procurement
actions have started for a new exchanger.
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Figure 7. The welded repair area
Findings and Results
The equipment in SAFCO-2 has been operating
under close monitoring with a known leak,
keeping leakage as a benchmark. The continued
operation and planning has been based on a
similar experience with the SAFCO-3 HPCC.
Unfortunately, the plant experienced a shutdown
twice during the leak period and the leak
behavior changed. Even so, the plant was kept
running until a forced shutdown was taken when
the NH3 pick up increased sharply crossing the
value of 500 ppm. This amount of ammonia
had an effect on the evaporation section vacuum
and the plant was shutdown.
Conclusion
SAFCO has good experience in plant
troubleshooting, even though each case is
unique. The monitoring and control plan
succeeded in the SAFCO-3 HPCC but it failed
in the SAFCO-2 case because two crash
shutdowns changed the leak behavior.
Fortunately, the SAFCO-2 shutdown occurred
10 days before the turnaround and the new
equipment was already on-site and turnaround
resources were simply rescheduled.
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