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NDE2019, 060, v2: ’Inspection of Ammonia Synthesis Converter’ 1

Inspection of Ammonia Synthesis Converter


Ketan Amin, Chintan Mulchandani and Hussain Vasadwala
GNFC, Gujarat, India
knamin@gnfc.in
cmmulchandani@gnfc.in
hevasadwala@gnfc.in
More info about this article: http://www.ndt.net/?id=25730

Abstract. The Ammonia Synthesis Converter is the heart of Ammonia plant and ensuring its reliable operation
is of utmost importance. Normally, operating life of Ammonia Synthesis Converter with S-200 basket remains
10-15 years in plants world over. In GNFC, it was under operation since 1992 i.e. for last 26 years. GNFC, also,
had faced problem of leakage from gas outlet nozzle in 2006 in this converter. Hence, with a view to increase
reliability as well as production, it was decided to replace old S-200 basket with new design S-300 basket.
During basket replacement project, detailed inspection of pressure shell was carried out to check its integrity for
future operation.

Meticulous planning and co-ordination among various departments helped in completion of inspection in just 5
hours. Defects were found in gas outlet nozzle which was repaired and converter with new basket was put in to
operation safely. Timely completion of inspection and repair activities resulted in scheduled plant start up
thereby minimizing production losses.

Keywords: Ammonia Synthesis Convertor, S-300 basket, NDT

1. Introduction

Ammonia Synthesis Convertor is the heart of Ammonia plant. It operates under high temperature and pressure,
and has longest run (@10~15 years) between catalyst changes. Opening of reactor in between needs catalyst
replacement, which is costly and time consuming. Therefore, convertor should operate between catalyst changes
without inspection or repair.

Ammonia Synthesis Convertor in GNFC was designed by Haldor Topsoe and utilized S-100 basket which was
installed in 1981. In 1992, S-100 basket was replaced by S-200 basket to increase process efficiency. The
normal operating life of S-200 convertor basket is about 15 years and it was operating since last 26 years.
Screen damage was observed in basket which was repaired and catalyst was replaced in 2006. Ammonia
synthesis catalyst also has life of about 10 ~15 years and catalysts were in use since last 12 years. There was an
increase in pressure drop in Ammonia Convertor in December 2017 which was due to screen damage in basket.
This resulted in substantial reduction in plant load as well as production. Looking to all these factors, it was
planned to replace S-200 basket by S-300 basket along with catalyst replacement during 2018 turnaround for
improving plant reliability as well as process efficiency using same old pressure shell. Hence, it was necessary
to check integrity of pressure shell.

2. Equipment Detail

The Ammonia Synthesis Convertor is Haldor Topsoe radial flow type


with pressure shell and S-200 basket. The basket is of two catalyst bed
sections. Each bed has center screen and screen panels. Interbed Heat
Exchanger (IHE) is placed in the center of the first catalyst bed. Lower
Heat Exchanger (LHE) is located below of second catalyst bed. A central
tube passes through the catalyst section. Equipment configuration is as
shown in Figure 1 and detail is as tabulated in Table 1.

Figure 1. Pressure shell and basket


2 NDE2019, 060, v2: ’Inspection of Ammonia Synthesis Converter’
Table 1. Detail of equipment
Convertor Type 2- bed radial flow convertor
Design pressure (max operating pressure) 260 kg/cm2 g
Normal operating pressure 229 kg/cm2 g
Hydrogen partial pressure (design) 175 kg/cm2 g
Temperature data
Design temperature Operating temperature
Cylindrical shell 300 °C 240 ~ 260 °C
Bottom forging 400 °C 320 °C
Material data
Cylindrical shell C-0.5 Mo (P1)
Bottom forging 2.25 Cr 0.5 Mo (P22)
Convertor basket SS 304

3. Possible Damage Mechanisms and associated damage risk

The heart of the process is Ammonia Synthesis Convertor where hydrogen and nitrogen react at high pressure
(130~350 atm) and high temperature (upto 650 °C) to produce Ammonia. This convertor is subjected to
following damage mechanisms [1].

 High temperature hydrogen attack (HTHA)


 Low temperature hydrogen attack (LTHA) or hydrogen embrittlement
 Nitriding
 Cracking due to mechanical loads

3.1. High Temperature Hydrogen Attack (HTHA)


HTHA is the damage of steel by reaction of hydrogen with cementite (Fe 3C) in steel to form methane gas (CH 4),
resulting in formation of micro cracks and fissures as well as decarburization in steel. HTHA susceptibility
depends on hydrogen partial pressure and type of steel. The Nelson curve in API 941 gives guidelines for
maximum recommended temperature at different hydrogen partial pressures for various carbon and low alloy
steels. All types of materials are assumed to have been selected in accordance with API 941 at the time of design
and are on the safe side of Nelson curve. The dummy and shell layers in multilayer vessels will not be exposed
to high pressure hydrogen since these parts are vented to the atmosphere by means of weep holes. Hence, the
risk of damage due to HTHA is relatively low.

3.2. Low Temperature Hydrogen Attack (LTHA)


LTHA usually takes place in carbon and low alloy steel operating with high pressure hydrogen at elevated
temperature after being cooled down to below 150 °C. In particular, LTHA may cause loss of ductility of high
strength steels or cracking in zones with high hardness e.g. due to insufficient PWHT. Cracking due to LTHA
will be surface breaking. Low risk of LTHA will exist at weld of low alloy steel parts.

3.3. Nitriding
Nitriding occurs on equipment with metal temperatures exceeding 380~400°C. Nitriding causes increase in
surface hardness and subsurface cracks may develop due to combined effect of nitriding and HTHA. Risk of
nitriding in shell, bottom head and top cover is very low since they are not exposed to temperatures above
300°C. The bottom forging is exposed to elevated temperature (470~500°C), but since it is cladded with
Inconel, risk of nitriding is relatively low.

3.4. Cracking due to mechanical loads


Cracking takes place at areas with high loads and/or stress risers such as geometric discontinuities e.g. at nozzles
and supports. Risk of cracking at nozzle connections is very low since connections are at relatively thick
sections (top flange, bottom forging) and hence stress level will be relatively low. Highest risk of cracking due
to high loads will be at basket support ring due to higher stresses at basket support ring to bottom head weld
joint.
NDE2019, 060, v2: ’Inspection of Ammonia Synthesis Converter’ 3
4. Pressure shell inspection and repair

Pressure shell was in operation for last 37 years and last inspection of pressure shell was carried out in 1992
during S-100 basket replacement. Hence, inspection of pressure shell is of utmost importance for conforming
the pressure shell integrity for uninterrupted operation.

A detailed inspection plan was prepared considering anticipated damage mechanisms. Appropriate Non
Destructive Evaluation (NDE) methods used to identify damage mechanisms. Table 2 shows damage
mechanisms and most relevant NDE methods applicable to damage mechanism.

Table 2. Damage Mechanism and appropriate NDE method


NDE methods used to identify damage
Damage mechanisms
VI PT WFMPI TM HM UT FMR
HTHA × × ×
LTHA × × × × ×
Nitriding × × ×
Mechanical cracking × × ×
Decarburization due to HTHA × ×
General metal loss × ×

Abbreviations:
VI - Visual Inspection
PT - Penetrant Test
WFMPI - Wet Fluorescent Magnetic Particle Inspection
TM - Thickness Measurement
HM - Hardness Measurement
UT - Ultrasonic Test
FMR - Field Metallographic Replication

Based on applicable NDE methods a detail inspection scope for various locations/parts of pressure shell was
prepared which is kept at Table 3. S-200 basket was removed for inspection of pressure shell from inside. An in-
house designed and fabricated inspection platform [2] (Figure. 2), lowered inside empty shell to facilitate
inspection.

Preliminary inspection of shell from inside and marking of locations for various NDE was done. All locations
were cleaned using 120 grit paper. Inspection of entire pressure shell was started by crew of various NDEs
simultaneously and it was completed in record 5 hrs. Findings of various NDE are tabulated in Table 4.

Figure 2. In-House designed and fabricated Inspection cage


4

Table 3. Scope and detail inspection plan of pressure shell

NDE methods to be performed at a given location


Locations of NDE
Visual PT WFMPI TM HM UT FMR
Shell course (spot 6”X6”)      
Nozzle A1 (North-East)     
Nozzle A2 (South-West)     
Nozzle D1 (North)     
Nozzle D2 (East)     
Nozzle D3 (South)     
Nozzle D4 (West)     
Top cover inside base metal (spot - 6”X6”)       
Top flange inside base metal (spot - 6”X6”)       
Top flange to shell weld joint      
CS joints    
LS Joints    
T Joints    
NDE2019, 060, v2: ’Inspection of Ammonia Synthesis Converter’

Basket support ring   


Shell to bottom head external joint     
Bottom head inside base metal (spot - 6”X6”)       
Bottom forging inside base metal (spot - 6”X6”)       
Bottom flange inside base metal (spot - 6”X6”)       
Nozzle B     
Gasket seating surfaces 
Gasket surfaces 
Table 4. Findings of various NDE in pressure shell

NDE findings at a given location


Locations of NDE
Visual PT WFMPI TM HM UT FMR
Shell course (spot 6”X6”) 29~30.2 135~160 -- Ferritic & bainitic structure
Nozzle A1 (North-East) 50.2
Nozzle A2 (South-West) 50.4
Nozzle D1 (North) 41.1
--
Nozzle D2 (East) 40.2 --
Nozzle D3 (South) 40.0

No Indication
Nozzle D4 (West) 40.5
No Indication

Top cover inside base metal (spot - 6”X6”) -- Bainitic structure


Top flange inside base metal (spot - 6”X6”) 331 133~151 Bainitic structure

No abnormality
Top flange to shell weld joint 135~161 Ferritic & bainitic structure
CS joints 157~183 Ferrite, acicular ferrite &

No Indication
-- --
LS Joints 158~184 bainitic structure
--
T Joints NI
Basket support ring -- -- --
Shell to bottom head external joint
Bottom head inside base metal (spot - 6”X6”) 108.1 140~157 Ferritic & bainitic structure
Bottom forging inside base metal (spot - 6”X6”) 3 Cracks in liner 304 -- Austenitic structure

No Indication
Bottom flange inside base metal (spot - 6”X6”) 358 160~180 Austenitic structure
No Indication

Nozzle B 112.5

No
Gasket seating surfaces -- --
-- -- -- --

abnormality
Gasket surfaces
NDE2019, 060, v2: ’Inspection of Ammonia Synthesis Converter’
5
6 NDE2019, 060, v2: ’Inspection of Ammonia Synthesis Converter’
A leakage was reported from weep hole of Inconel-600 liner provided in bottom forging. 3 cracks in liner were
observed in north direction in gland packing area during visual inspection after removing gland packing. Hence,
Penetrant test was carried out in entire circumferential length of gland packing region. Additional 7 cracks were
found in Penetrant test in this region (Figure. 3a). All the cracks are shown in schematic diagram in Figure 4.

(a) (b) (c)

(d) (e) (f)


Figure 3. Defects in bottom forging region before and after repair.
(a), (b), (c) Defects before repair
(d), (e), (f) Defects after repair

Liner
Shell
1 - Crack in liner to boss weld joint
Weld Boss
Overlay 1 2 - Crack in stud hole

3 2 3 - Crack in boss to weld overlay fillet weld

Elevation
N

- Crack in in liner to boss weld joint observed in VI


W E - Crack in liner to boss weld joint found in PT
- Crack in boss to weld overlay fillet weld found in HLT

Figure 4. Schematic diagram shows leakage locations


NDE2019, 060, v2: ’Inspection of Ammonia Synthesis Converter’ 7
Subsequently, gland packing ring was removed to inspect Inconel-600 weld overlay area behind gland packing
ring. Cracks were observed in 5 stud holes (Figure 3b) and at 2 locations in boss to weld overlay fillet weld joint
(Figure 3c) in east to south direction in both visual and Penetrant test which is shown schematically in Figure 4.

In view of cracks observed in Penetrant test in liner and stud holes, Helium leak test was done to check for
minor leaks in this area as Helium Leak Test has higher sensitivity than Penetrant test. Masking of stud holes, all
the leaky area and boss to weld overlay fillet weld joint was done using small length of masking tape and
covering entire circumferential length. Vacuum was created through weep hole and sprinkling of Helium was
done after removing masking tape one by one for all the masked area. Leakages were observed from additional
3 locations in boss to weld overlay fillet weld joint.

Cracks in gland packing area were repaired by cutting up to the cracked depth and welding (Figure 3d).
Leakages in boss to weld overlay fillet weld were repaired by cutting old fillet weld up to 1~2 mm depth and
welding (Figure 3f). Cracks in 05 stud holes were repaired by cutting front face and ID side of stud holes up to 3
mm, and welding. Studs were provided in these repaired stud holes and they were seal welded (Figure 3e). All
cutting was done using FF2 cutter and welding done using Inco 82 filler wire. After completion of repair
welding, Penetrant test was done. All defects observed in Penetrant test were attended and finally cleared in
Penetrant test. Subsequently, Helium Leak test was done and leakage was not observed.

5. S-200 basket inspection

The S-200 basket was in operation since 1992 i.e. 26 years which is higher than its normal operating life of
about 10~15 years. Therefore, any inspection of the basket was not required and basket can be scrapped off.
However, inspection of basket was done to keep it ready to put back it in to operation in case of emergency.
Preliminary inspection of both the beds of basket was carried out. Inspection activities and respective
observations were as below.

Visual inspection
Screen of Interbed Heat Exchanger (IHE) of 1st bed was observed damaged in bottom portion at two locations
(Fig. 5). Screen support strips at these locations were observed loose. Screen support strips were found missing
at 03~04 locations. Baffles of IHE tubes and sleeves on IHE tie-rods were observed cracked and damaged (Fig.
6). Holes were observed in outer shell screen of 2nd bed at 6~7 locations (Fig. 7). Outer shell screen was
observed lift-off by @1’’ at 02 locations.

Hardness measurement
Hardness was measured on various parts of 1st and 2nd bed. Material of various parts of basket was SS-304.
Hardness was found in the range of 325~574 BHN indicating nitriding effect.

Microstructural examination
Microstructural examination of various parts of 1 st and 2nd beds exposed to high temperature in the range of
360~550°C was carried out. Microstructure revealed metal degradation in form of carbide precipitation along
austenite grain boundaries. Nitriding up to depth of 1.8 mm was also observed in cross sectional view of IHE
baffle plate during microstructural examination (Fig. 8).

Haldor Topsoe S-200 basket was fabricated of SS-304 material and exposed to high temperatures with ammonia
concentration up to 20%. Based on study by K. Rorbo [3], nitridation rate observed in Topsoe convertors is on
an average 4 mpy. Hence, calculated nitridation thickness on various components would be about 104 mils or
2.6 mm considering operating life of 26 years of basket. The nitriding layer thickness of 1.8 mm found during
metallurgical examination is close to calculated nitridation thickness based on study. Also, hardness value of
various components of basket indicates nitriding has occurred on surface of components.

Figure 5. Damaged IHE screen of 1st bed Figure 6. Damaged baffles & sleeves Figure 7. Hole in screen of 2nd bed
8 NDE2019, 060, v2: ’Inspection of Ammonia Synthesis Converter’

(a) (b)
Figure 8. (a) Nitriding depth in baffle plate, (b) Carbide precipitation in austenitic structure

6. Conclusion

Various NDE methods were applied to evaluate damage mechanism in pressure shell. A specially designed and
fabricated inspection cage was used for pressure shell inspection. A meticulous inspection planning helped in
completing inspection in just 5 hours. Cracks were observed in liner to boss butt weld, boss to bottom forging
weld overlay fillet weld and in stud holes in boss. All defects repaired as per the prepared repair procedures. All
attended areas were inspected using relevant NDE method. New S-300 basket lowered in to pressure shell after
establishing integrity of pressure shell.

NDE methods were also applied to various parts of S-200 basket. However, on various observation like crack
observed in baffle plate and sleeves of tie-rods of IHE exchanger, nitriding up to 1.8 mm against calculated 2.6
mm and higher hardness in the range of 325~574 BHN, S-200 basket was scrapped.

References

1. Haldor Topsoe Basic Specification, Doc. No.: SP-514-EN, Recommendations for inspection of existing S-
200/S-300 ammonia convertor pressure shell.
2. P.C. Srinivasan, Ammonia Convertor Conversion to S-300 Basket at CFCL, Indian Journal of Fertilisers,
Vol. 13 (8), pp 76-81.
3. K. Rorbo, Environmental Degradation of High Temperature Materials, Series 3, No. 13, Vol 2, 1980, p 147.

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