Weld Zone Cracks in Repaired

2 1/4 Cr-1 Mo Ammonia Converter

Leaks occurred in ammonia converters in two separate plants with one converter leaking after four years of service and the other leaking after eight years. The converter
that leaked after four years was repaired by completely removing the failed weld and
rewelding. This repair weld developed cracks after nine months of service.

G.R. Prescott
Metallurgical Consultant, Newport Beach, CA 92663
B.J. Grotz
Brown and Root Petroleum and Chemicals, Alhambra, CA 91803

Background

After nine months of service, cracks were

detected in the repaired weld.

After four years of service, a hot-wall

type ammonia converter in France leaked at
the closing seam between the top head and
shell. The results of an investigation into this
problem was reported at the 1991 AIChE
Ammonia Safety Symposium and published
in the 1992 AIChE Technical Manual, Vol.

All of the aforementioned converter

welds, both the original and repair, were
made with the same agglomerated flux
combined with a low temperature
dehydrogenation heat treatment, LTDHT.
The inadequacy of the LTDHT was
established in the previous paper (1) based
on a thorough review of the development
work by Kobe (5). This welding procedure
is the common denominator unking these
converters together. It should be noted that
C F Braun prepared the specifications for the
original vessels but was not involved in
procurement and was not involved in the
metallurgical investigation of the closing
seam weld failures until after the repairs
were completed.

An almost identical failure occurred in

an ammonia converter with the same design
and service conditions at a German plant
after eight years of service. The results of an
investigation of that problem by BASF was
also published in the 1992 AIChE Technical
Manual, Vol. 32.(2)
The French converter was sent to a
fabricating shop where the failed weldseam
was completely removed and rewelded.

This combination of flux and a LTDHT

leaves a high residual amount of hydrogen in
116

the weld. When the weld is cooled the hard

heat-affected zone, HAZ, is susceptible to
hydrogen induced cracking. In the previous
paper(l), the conclusion was reached that
the procedure produced a linear array of
microcracks in the HAZ that were not
detectable by conventional inspection
methods. These microcracks, over a period
of time, developed into macrocracks that
ultimately propagated through the wall.

The extent of cracking on the interior

surface of the repair weld is shown in Figure
1. The sketch shows that cracks were
intermittent and occurred predominately on
the head side with a few short cracks on the
shell side. All cracks are located in the heataffected zone (HAZ). The cracks were
detected using ultrasonic inspection from the
outside surface. After nine months of
service, the cracks were 12 mm deep. After
21 months, the cracks had propagated to 27
mm but the growth rate had slowed
considerably.

This conclusion is supported by the

fact that eleven other converters of
essentially indentical configuration and
service conditions have been thoroughly
inspected and no cracks were found. These
converters are exposed to ammonia synthesis
gas at 400C (750F) and the hydrogen
partial pressure is in the range of 115-126
bar. The ammonia content in the synthesis
gas varies from 11 percent in the last
converter of a two converter plant to 15
percent in a three converter plant. The
service life of these converters range up to
16 years. None of these converters were
welded with this particular hygroscopic flux
combined with an inadequate LTDHT.

The sample obtained for this

examination was located in a zone free of
detectable cracks as shown by the sketch in
Figure 1. A photograph of the sample is
shown in Figure 2. The sample was obtained
as one solid piece and this photo shows some
preliminary cuts made for the purpose of
subsequent
nondestructive
testing,
metallurgical tests, and metallographic
examination. The cut sections are identified
as shown in Figure 2.
The overall plan of the investigation
included the following:

New Investigation
1. A detailed ultrasonic examination of the
solid block and the subsections was made
using various sensitivity settings in an
attempt to detect small internal cracks.

When the repaired weld developed

cracks after nine months of service, the
company ordered a replacement converter.
The new replacement converter was welded
with a revised welding procedure that
eleminated the use of a LTDHT. Instead, an
intermediate postweld heat treatment,
IPWHT, at 593C (1100F) for 1 hour was
used to remove the hydrogen. When the
original converter was removed from service,
an opportunity was presented to investigate
the cause of cracks that developed in the
repaired weld.

2. A complete metallographic examination

of the weldment was made with special
emphasis on the heat-affected zones. All
ultrasonic indications were carefully
examined.
3. Hardness traverses were made to detect
the presence and extent of nitriding on
the inside surface.
117

inside surface and microcracks were also

found in the weldmetal.

4. A scanning Auger microprobe was used

to determine the amount of nitrogen
present at various distances from the
inside surface.

Figure
6
is
a
composite
photomicrograph of the weldmetal at the
inside surface. This view is perpendicular to
the weld surface after it has been ground
down about 1/16-inch. Figure 6A is a fully
etched view of the weldmetal and some
cracks are visible. Repolishing the etched
surface clearly delineates the microcracks as
shown in Figure 6B. The technique of
polishing, etching, and repolishing is a very
useful procedure when looking for
microcracks. Figure 7 is a cross-sections of
weld sample E. This view shows the depth
and interdendritic nature of the microcracks
in the weldmetal. All of these microcracks
are below the surface.

ultrasonic

The overall objective of the ultrasonic

examination was to see if the sample
contained any type of detectable defects.
More specifically, the purpose was to
determine if microcracks, if they existed in
the heat-affected zones, were detectable by
using various techniques. The base case
utilized the minimum requirements of the
ASME Code for ultrasonic testing. Nothing
was detected using Code requirements, but
seven indications were recorded at a high
level of sensitivity. Figure 3 shows the
location of two of the indications, and Figure
4 shows the instrument settings and display.

Figure 8 is a cross-section of the weld

at the inside surface of sample D showing
extensive microcracking in the HAZ. Figure
9 is a cross-section from another location,
sample E, showing a similar group of
microcracks in the HAZ of the weld. As
mentioned previously, these microcracks
could not be detected by ultrasonic
examination over a wide range of sensitivity
settings. It is an important observation that
none of these microcracks are connected to
the surface which disproves the hypothesis
by BASF that surface nitrides are a causative
factor(2).
In addition, the microcracks
extend to a depth well below the nitride
layer. It also should be noted that this
sample of the weld did not contain any
visible or detectable cracks. As shown in
Figure 1, the sample provided for this
investigation
was
located
between
macrocracks visible on the inside surface.
This strongly suggests that the actual cracks
found in the vessel were generated in zones
where the microcracks existed in greater

Metallographie
All of the ultrasonic indications were
investigated and no cracks were found.
Apparently the indications were caused by
some microstructural aberrations such as
large grains in the HAZ. This is not unusual
at high gain settings.
Figure 5 shows a cross-section of the
weld between the top head and the shell.
Most of the weld was made from the outside
surface, followed by back chipping and
welding from the inside. The entire weld and
HAZ of each cut section was scanned
microscopically in an effort to find hydrogen
induced microcracks. Cracks were found in
the weld and HAZ near the inside surface.
No microcracks were found in the portion of
the weld or HAZ made from the outside.
Microcracks were found in the heat-affected
zone of the last weld passes made from the
118

recent sample, D, are also shown in Figure

10. After almost two years of operation, the
inside shows a moderate amount of increased
hardness up to a depth of about 0.5 mm.
The weldmetal is inherently harder than the
base metal and the inner surface does show
some increase in hardness over the bulk
sample. The pattern of hardness suggests
that the hardness gradient might be
associated with a temperature gradient
during the local PWHT.

density and extended to greater depths.

Even with more extensive microcracks, the
normal non-destructive examinations after
fabrication are not capable of detecting
micro-defects.
Nitriding
Hardness traverses and Auger analyses
were used to determine the extent of
nitriding at the inner surface. The question
of nitriding is an important consideration
since both BASF (2) and the French Welding
Institute (3) concluded that a thin layer of
nitride was instrumental in the initiation and
propagation of the failures of both the BASF
converters and the original failure in the
French converter.

Creusot-Loire (4) examined a sample

taken from the first converter and reported a
nitrogen content of 0.18 percent at a depth
of 0.1 mm from the inside surface. At 1.25
mm the nitrogen content had decreased to
0.01 percent which represents the nominal
nitrogen content of the steel. BASF (2)
reported 0.24 percent nitrogen at a depth of
0.1 mm and dropping to about 0.01 at a
depth of 1.5 mm.

As a comparison, a hardness traverse

was made on a piece of the shell course from
the original failure of the French converter.
Both the French Welding Institute (FWI) (3)
and Creusot-Loire (4) reported high
hardness values at the inside surface. The
FWI report shows maximum base metal
hardnesses on the three French converters
ranging from 223 HV to 406 HV.
Curiously, the high hardness reading was on
R101, the first converter in series, with the
lowest ammonia content. Creusot-Loire had
a sample from R101 and reported interior
surface hardnesses up to 420 HV. All of
these hard layers were about 0.5 mm deep.
BASF presented data on their converter
failure (2) that showed nitrogen enrichment
at the inside surface to a depth of 1.5 mm.
Hardness readings in this zone were as high
as 367 HV.

Auger analysis of the samples received

from the original and repaired vessel is
shown in Figure 11. At a depth of 0.1 mm,
the nitrogen content is 0.22 percent in the
original vessel surface and 0.23 weight
percent nitrogen in the repaired converter.
Both cases level off to the nominal nitrogen
content of the steel at depths between 1 and
1.5 mm. The depth of nitriding is greater in
the original surface as compared to the
rewelded surface. This could reflect the
longer time in service or variations in the
analyses, or because the degree of nitriding
varies from one location to another. As
shown in Figure 10, the maximum hardness
varies widely from one location to another.
Discussion

Our traverse on base metal from the

original vessel, shown in Figure 10, confirms
that the hardness is relatively high to a depth
of about 1.0 mm. Similar traverses on base
metal, HAZ, and weldmetal from the most

In the paper presented previously (1).

the conclusion was reached that the cause of
failure was due to the presence of
119

Other ammonia converters in four

different plants of essentially the same design
and in the same service for up to 16 years
have been carefully inspected and no cracks
were found. These other converters were
welded with either low hydrogen fused flux
and a 593C (1100F) IPWHT or were stress
relieved in a furnace. The two sets of
converters in the French plant and in the
German plant are the only ones welded with
agglomerated flux, LTDHT, and given local
stress relief of the closing seam..

microcracks in the heat-affected zone. Over

the four year period, these microcracks grew
and coalesced into macrocracks that
ultimately caused leakage. The microcracks
were caused by residual hydrogen which was
the result of using a hygroscopic
agglomerated flux, in conjunction with an
inadequate intermediate dehydrogenation
heat treatment. In order to. establish the
inadequacy of the LTDHT, the original
papers describing the development of
LTDHT were reviewed in detail and the
review proved conclusively that the LTDHT
was inadequate even for typical conditions
defined by the manufacturer of the flux. If
the flux were not stored properly, or handled
properly on the shop floor, then the
conditions would be much worse than
typical.

The portion of the weld made from the

outside is free of defects in the sample
furnished for this investigation.
The
situation in other areas of the repair weld is
obviously much worse as evidenced by the
fact that cracks were found as deep as 29
mm after two years of service. Due to the
limitations of the sample, it is not possible to
speculate with regard to future crack
propagation over an extended period of time.

Conclusions
The results of this investigation show
once again the risk of using an inadequate
dehydrogenation heat treatment on a weld
made with a hygroscopic agglomerated flux.
The LTDHT used was 280C (536F) for 2
hours. The original work (5) done to
develop a satisfactory LTDHT for this weld
would require at least 10 hours at this
temperature.
This LTDHT might be
adequate for a welding flux that imparts 1 to
2 ppm hydrogen content in the weld. It is
not adequate for a flux that typically puts 7
to 8 ppm hydrogen in the weld. Fabricators
who use LTDHT should familiarize
themselves with the correlations developed
by Kobe (5) and use the information to
design appropiate dehydrogenation heat
treatments. In addition, they should follow
the directions of the flux manufacturer with
regard to keeping the flux properly dried
during storage.

Gouging and back welding the inside

portion of the weld is quite another matter.
Maintaining a preheat of 250C (482F) with
welders inside the vessel is a problem of long
standing. The tendency is to let the preheat
cool down below the minimum requirements.
The compensatory heating is reduced
because these are the last weld passes made
in a short period of time. The weld is then
given the LTDHT and cooled to room
temperature. If the hydrogen content has not
been sufficiently reduced, the hard weld
heat-affected zone is subject to hydrogen
induced cracking on cooldown.
The
cracking can be macrocracks and/or
microcracks. The macrocracks are detected
and repaired. Microcracks are not detected
as we have shown in this investigation, and
these can eventually coalesce
into
macrocracks if the density of microcracks is
sufficient to promote propagation.
The
120

intersects a zone of internal microcracks due

to an inadequate LTDHT, the propagation
rate increases leading to ultimate failure.

microcracks found in the HAZ of the last

weld passes are the cause of toe cracks.
A contributing factor to the cracking
problem is the existence of high residual
tensile stresses at the ID of the weld and
HAZ resulting from the local postweld heat
treatment. These residual tensile stresses are
safely dissipated in sound welds by a small
amount of plastic deformation under normal
operating conditions.

Literature Cited
1. Prescott, G. R., Weld Failure in a 2
l/4Cr - IMo Ammonia Converter,
AIChE Technical Manual, Ammonia
Plant Safety, Vol. 32, 1992.
2. Wagner, G. H., Heuser, A., and Heinke,
G, Hydrogen Attack in 2 l/4Cr - IMo
Steel Below Nelson's Curve, AIChE
Technical Manual, Ammonia Plant
Safety, Vol. 32, 1992.

The cracks that were detected after 9

months of operation propagated fairly
rapidly for about 14 months, then
propagated at a slow rate for the following
year. The rate is shown below.
Date
August 1990
January 1991
July 1991
January 1992
August 1992

3. Institute de Soudure, Paris, France,

Documents 2 and 3, Rapport Technique,
March 26, 1990.

Crack Depth
12 mm - after 9
months service
25 mm - after 14
months service
27 mm - slow growth
28 mm - little or no
growth
29 mm - little or no
growth

4. Etude Mtallurgique De La Fissuration

Du Reacteur RI01 De La Boucle De
Synthese NH3 Socit Chimique De
Grande Paroisse, Rapport Technique No
89144C, Creusot Loire Liquidation,
Nov. 1989.
5. Takahashi, E. and Iwai, K., Omission of
Intermediate Postweld Heat Treatment
(PWHT) by Utilizing Low-Temperature
PWHT for Welds in Pressure Vessels,
STP 755 ASTM, 1982.

The above growth rate fits the

microcrack pattern that we observed in our
weld sample. The microcracks are adjacent
to the last weld passes made from the inside
surface. The microcracks apparently grew
and coalesced into a toe crack. The rate of
propagation slowed when it reached the end
of the zone of microcracks. If the toe crack

121

DISCUSSION
L. Gens, BASF: Mr. Prescott, I think you made it
very clear that you don't agree with the BASF theory that was presented by Mr. Wagner during the
'91 Ammonia Safety Symposium. After further
internal investigations and additional experiments
since '91 by our metallurgical department, we still
stick to our stated theory that owing to nitriding
from the surface, the material becomes in principle
sensitive to hydrogen attack within a relatively thin
layer. If sufficiently high stress is applied, cracking
must be expected. The cracking propagates slowly
since it depends upon the diffusion of the nitrogen
in the steel and on the transformation of the carbides. Commenting on your statement about other
ammonia converters in four different plants of
essentially the same design and so on, as far as we
know the other converters were all built according
to ASME code. The French followed the CODAP,
and the BASF converters were built according to
the German code A.D. Regelwerk. This really indicates an essential difference, for instance, in wall
thickness and stress level.
Prescott: Concerning your first comment on the
nitride formation and the hydrogen attack, one
problem that we have with that theory is that it's
very difficult to arrive at a mechanism or a reaction
mechanism that limits this attack to just one zone
in this entire converter. Why would it only be
occurring in weld metal or in heat-affected zones
and not in base metal? In reference to the codes, of
course, the vessels built in the U.S. were built to
the ASME code, yours were built to the German
code, the French to the French code, and NSM's or
Norsk Hydro I believe were built to the Dutch
code.
Guns: No, I believe they were all built to ASME
code, also.
Prescott: Well, they also had to meet the Dutch
code. We looked at these differences in terms of
wall thickness, stress levels and so on, and it really
didn't seem to us to be significant. And it certainly
shouldn't be significant if it were hydrogen attack.
Gnus: I think we have just a different opinion
there.
Prescott: We certainly do; we'll fight on.

S. Thomas, Pequiven: Mr. Prescott, was a hydrogen baking applied before the repair of these
welds? If not, can you explain the reasons?
Prescott: A hydrogen baking was applied, definitely, and extensively.
K. Nassauer, Babcock-Borsig: We have also experienced during fabrication or manufacturing of 2
1/4 Cr-1 Mo material hydrogen induced cracks,
and we have also done extensive tests with different kinds of sub-arc welding procedures with
agglomerated fluxes. We found, for example, that
with the so-called tandem wire AC current procedure, the hydrogen is much higher in the weld than
with the so-called single wire DC current procedure. This is due to the fact that the humidity, the
steam or the humidity, is dissociated into hydrogen,
and this is part of the weld. For 21/4 chrome material we only weld now with the so-called single
wire DC current process to avoid hydrogen
induced cracking during welding. Even if you
check the hydrogen content of the agglomerated
flux, this is only one possibility and only one point.
You also must look very carefully at the welding
procedure itself. As I mentioned, we did extensive
tests with the German "Bundes Anstalt fr Material
Prfung" or "BAMP" and found this a very important fact apart from, of course, the very extensive
Kobe research work, which did not focus much on
the welding process itself.
Preseott: While I appreciate your comment, I
believe that the purpose of the submerged-arc flux,
of course, is to protect the weld from the environment and the humidity. Secondly, all agglomerated
and bonded fluxes are not alike. Some pick up
moisture very readily or very slowly. Of course,
the ultimate flux was the original fused flux. I
describe in my paper where all the ingredients are
melted and then it's ground up into a flux, which is
totally nonhygroscopic. It's only when you get into
bonded and agglomerated fluxes that you find that
some are very or slightly hygroscopic. So, you
must look at flux as one of the principal sources of
the hydrogen. Other factors can enter into it, I
agree.
Appt Your theory does not explain that intensity
of damage or number and depth of cracks are

122

increasing with the number of converters. It's less

in converter 1 and more in converter 2. And if you
have three, it's more in converter 3. And this corresponds exactly to the increasing content of ammonia.
Prescott: You're absolutely right, and one possibility is that, as you mentioned, we found cracks in all
three converters in the French plant. You found
cracks in both of your converters, and the one
looking at the highest concentration of ammonia is
the one that leaked. And it's certainly possible that
the ammonia is participating in accelerating the
propagation of a crack once it's formed. That's
another mechanism that you have to consider, and
we don't have any experimental work to back up
either one of these.
AppI: Some work must be done to get a final clarification.
Prescott: I think so.
J.G.MacDonald, ICI Engineering: Some of your
initial slides showed that different etching characteristics were found adjacent to the crack, and also
the internal surfaces. Have you considered any
contribution to cracking by solid solution strengthening by nitrogen?
Prescott At 400C, we haven't. In our last slide,
the Auger analysis shows the nitrogen dropping off
to normal steel values at about one mm in depth.
MacDonald: Were they typical of what you would
expect for nitrogen levels?
Prescott: Yes.
S. Thomas: Mr. Prescott, those repair welds developed cracks that propagate fairly rapidly; so, we
have cracks after nine months service. If we are
talking about hydrogen attack, I have my concerns.
21/4 chrome is a more resistant material, so I don't
think that hydrogen attack can develop in such a
short time. Probably, you cannot discard hydrogen
embrittlement or the heat treatment applied as the
related cause of this failure.
Prescott: I would also like to mention that these
microcracks originate at the surface on the sample
that I showed you with no defects detectable by
normal methods. They are all below the surface
and well below the nitride layer. This tends to support our side of the argument.
C. Miola, Snamprogetti: According to your experience on this kind of weld, especially in service, the
ultrasonic attenuation method can help find out
really if there is hydrogen absorption or not.

Prescott Experts tried every possible setting on

their instrument to detect microcracks of this size
on the sample that I showed you, and they were
unable to do so.
Miola: The ultrasonic attenuation method is a very
sophisticated new method in order to detect hydrogen absorption.
Prescott: You're right. You can detect hydrogen
attack by very sophisticated methods, but these
microcracks are not detectable even by those methods, I believe. What is really important here is that
the requirements of the codes are far below the
sensitivity and settings attenuation that you're talking about. So, the U.S., German, French, and
Dutch codes do not detect these microcracks. They
could have existed at the time these vessels were
fabricated and shipped, and that's how we got into
a leaking situation.
J. Korkhaus, BASF: You showed us some slides
with macrocracks. I would like to know how you
explain the microstructural change with an obvious
decarburization along the cracks, if the mechanism
of macrocrack formation is the linking up of cold
cracks?
Prescott: All of these cracks, subcracks, and associated cracks are intergranular in nature. Of course,
when this crack opens up and becomes exposed to
the process gas which contains ammonia this is
very reactive metal -- it nitrides, just like the surface of this.
Korkhaus: It's not only nitrided, it's also decarburized.
Prescott: Well, it's nitrided. It has to be. However,
it's not hydrogen attack; it's just nitride.
Korkhaus: That's the point. It's a question of the
metallurgical reaction pattern and the velocities of
the different reactions.
Prescott: It's only a surface effect.
Korkhaus: I don't believe it.
Prescott: Well, I do. So, it goes on and on. You
have to decide whether you use a low-temperature
dehydrogenation heat treatment or a conventional
intermediate heat treatment.
Korkhaus: I have some problems with your recommendation concerning the flux. Some years ago
I made some hydrogen measurements on weld
metal molten down using different fluxes including
fused fluxes. During these measurements hydrogen
contents up to 10 ppm were found for weld metal
produced with fused fluxes. The hydrogen ingress
123

into the weld metal from the fused flux depends on

the way this flux has been produced. The use of
fused fluxes is not generally a guarantee for hydrogen contents of 2 to 3 ppm in the weld metal.
Prescott: I'm only saying that normal fused fluxes
used for Cr-Mo steels normally have 1 to 2 ppm.
This has been substantiated and supported by an
extensive amount of work done by both Kobe,
Hitachi, and Japan Steel. I don't know of any other
published paper that comes close.

Korkhaiis: The way of production is decisive for

the hydrogen ingress by fused fluxes into the weld
metal. Fused fluxes sometimes are produced by
pouring the melt into water. During this step, the
flux picks up moisture which acts as hydrogen
source and which you cannot get out.
Prescott: That goes back to what I said. Make sure
the fabricator knows what he has in the weld
before he designs his heat treatment. If he doesn't
know, he can't design one.

G.R. Prescott

B.J. Grotz

Con verier R-103 - Inside Surface

Head

Cracks

Scanning Side
Indication
Sound Path
Dist. To Ref.
Depth
Length
Angle
From Side 2

= OD
= #4&#5
= 3.1"
= 1.05"
= 2.1" to 2.3"
= .65"
= 45
= .52"

Scanning Side
Indication
Sound Path
Dist. To Ref.
Depth
Length
Angle
From Side 2

= OD
- #6 & #7
-1.5"
- 1.39"
= .9" to 1.02"
- Less Than .375'
= 45
= 1.2"

OD
Shell

Braun Sample

Figure 1. Location of cracks adjacent to

head-to-shell weld.
Head

Outside Surface

Shell

Figure 2. Overall view of weld sample.

Figure 3. Location of two indications of
microcracks.
124

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Figure 4. instrument settings and dispiay.

A-Etched

IOOX

B-Unetdied

Figure 6. Perpendicular view of weidmetai

at inside surface.

Inside Surface
2X

Figure 5 Composite photo of weld cross

section

100X

Figure 7. Two cross-sectional views of

sample E at inside surface.
125

Inside Surface

Hardness Traverses on Sample D at Inside Surface

Knoop 300-g
mm

Original
Vessel'

.05
.15
.25

238
238
241
218
215
209
197
180

260
264
260
260
253
245
234
231

287
257
249
249
253
245
231

282
264
264
264
253
257
234
203

203
203
203
197
197
199
185
182

323
282
257
234
221
221
215
215

.50

.75
1.00
2.00
3.00
70 mils deep
100X

215

'Base Metal

Figure 10. Hardness traverses on

sample D at inside surface
Knoop 300-g.

Figure 8. Cross section of HAZ of sample D

at inside surface.

NITROGEN ANALYSIS
Original Vessel

Inside Surface

X;'"v""

- < ,",.,-

i.o

i.s

msioe Surface mm

Repaired vessel

75 mils deep
100X

Figure 9, Cross section of HAZ of sample E

at inside surface.

126

Inside Surface mm

Figuren. Nitrogen analysis.