Mechanical Integrity of Primary

Reformer Hot Outlet Headers

This paper discusses mechanical integrity issues for primary reformer hot outlet headers. These are
typically welded assemblies of wrought Alloy 800H or 800HT or cast 20Cr-32Ni-Nb alloy. The typical
design and operating conditions for these headers are presented. Problems and failures that have been
reported at past Ammonia Plant Safety Symposiums are reviewed and summarized. With this
background information, recent failures of hot outlet headers are described along with the identified
causes of these failures. The most common failure mechanism is high-temperature creep but the
location and causes of creep damage vary. Creep failures have occurred both at weld joints and within
base metal. The sources of these problems are discussed and suggestions for mitigation are presented.
Based on the findings of the failure and material properties investigations, stress analysis and material
damage modeling is used to estimate remaining life.

Carl E. Jaske
Det Norske Veritas (USA), Inc., Dublin, OH USA

Greg T. Quickel
Det Norske Veritas (USA), Inc., Dublin, OH USA

in hydrogen and methanol reformers are also dis-

cussed. In all cases, the hot outlet headers operate
Introduction in the high-temperature creep range for their ma-
terial of construction, which is either a wrought

T
he purpose of this paper is to review and
discuss the primary mechanical integrity Alloy 800H or 800HT or a cast 20Cr-32Ni-Nb al-
issues that are associated with the hot out- loy. Because of the operating temperature range,
let headers of primary reformers. A number of pa- failures typically occur by high-temperature creep
pers presented at past Ammonia Plant Safety or creep-fatigue, with the fatigue damage induced
Symposiums have addressed various issues with by thermal cycling. Thus, creep strength is an im-
these hot outlet headers. To provide background portant parameter addressed in the review discus-
for recent issues with similar headers, the past sion.
work is reviewed and the various types of prob-
lems that have been encountered in the past are Following the background review, examples of
summarized. Relevant issues on similar headers recent problems with hot outlet headers are pre-

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 sented and discussed. The causes of these prob- Commonly used filler metals include Inconel 82,
lems and their relation to past problems are eva- Alloy 625, and Alloy 617. The common “match-
luated. The purpose of this evaluation is to help ing” filler metals are Thermanit 21/33, Thermanit
operators of primary reformers minimize the po- 21/33 So, and UTP A 2133 Mn. The final selec-
tential of similar problems in future operation of tion of welding material depends on the design
their units and to provide guidance for estimating and the welding technique that is used.
the safe and useful life of headers that are current-
ly in service. Such guidance will help avoid un- The primary load on outlet headers is internal
planned shutdowns and schedule repairs or re- pressure but bending loads are often induced by
placements in a timely, cost-effective manner. movement of attachments and/or restraints at sup-
ports. These system bending loads are related to
thermal expansion and complex interactions with-
Past Hot Outlet Header Issues in the manifold system, making stress analysis to
compute their magnitude difficult and adding sig-
Steam-methane reformers have either hot or cold
nificant uncertainty to the results of the calcula-
outlet headers to collect the process gas from the
tions. Furthermore, the bending loads are often
outlet of the catalyst tubes. Cold headers are made
displacement controlled so that stresses induced in
of carbon steel and insulated so that they operate
the high-temperature creep regime can relax and
at temperatures well below the creep range, while
redistribute with time at operating temperature. In
hot headers are not insulated and operate at high
contrast, internal pressure is usually maintained at
temperatures close to the reformer outlet gas tem-
a relatively constant level and is a sustained load
perature. The focus of this paper is on hot outlet
so that stresses induced by internal pressure are
headers that operate in the high-temperature creep
relatively straight forward to compute.
range of the materials from which they are con-
structed. Kawai, et al. [1] point out that there are
This section of the paper reviews hot outlet header
two basic types of hot header system designs: (1) a
issues that have been discussed in previous publi-
hot collector where the catalyst tubes are attached
cations. Issues with primary ammonia reformers
directly to the manifold by means of fittings and
as well as issues with similar components in hy-
the hot gases exit from the manifold via riser
drogen and methanol reformers are addressed. In
tubes and (2) a hot subheader with a cold transfer
comparing this information, keep in mind that
line where the catalyst tubes are attached to the
these different types of steam-methane reformers
subheader via outlet pigtails. In either case, the
operate in different ranges of temperature and
hot header or subheader is cylindrical vessel with
pressure as illustrated in Figure 1. Ammonia re-
numerous welded attachments at holes that allow
formers operate at higher pressures and lower
the hot process gas to flow into the header and
temperatures than hydrogen or methanol refor-
central tee section where the hot process gas flows
mers. This difference in operating conditions af-
out of the header.
fects the hot outlet header design. Thus, the outlet
headers in ammonia reformers usually operate at
Because the headers operate at temperatures near
higher stresses and lower temperatures than those
or greater than 800 °C, they are typically made
in hydrogen and methanol reformers.
from either wrought Alloy 800Hor 800HT or from
cast 20Cr-32Ni-Nb alloy. The fittings and tees are
also made using these same alloys. Welding of the
Performance of Header Materials
headers, tees, and fittings is done with a high-
nickel material or a “matching” material. Com- In 1963, Francis and Glass [2] reported the failure
monly used welding electrodes include Inco-Weld of outlet piping and described high-temperature
A, Inconel 182, Inconel 112, and Inconel 117. stress-rupture failures in Type 304 stainless steel

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2011 [84] AMMONIA TECHNICAL MANUAL
 piping. Avery and Valentine [3] reviewed the de- cast material and suggested that niobium-free
sired characteristics of materials for outlet mani- grades should be developed in order to avoid such
fold systems, while Harnby [4] pointed out that an in-service problems. Hoffman [9] evaluated the
outlet manifold system made of Alloy 800 had aging of 20Cr-32Ni-Nb castings after 21 months
better creep resistance than one made of the HU of service at 852 °C and found both M23C6 carbide
alloy. Later, Blackburn [5] pointed out that mani- and inter-metallic Nb-Ni silicide precipitates
folds made of Alloy 800 were less prone to crack- present in the aged material. The silicides were
ing than those made of traditional cast alloys, such mostly G phase plus some η’ phase. They are ex-
as HU, HK, and HT, because of its superior duc- pected to decrease creep resistance and promote
tility. He proceeded to note that the cast 20Cr- liquation cracking during welding.
32Ni-Nb alloy was an improvement to Alloy 800
for hot outlet header applications. These papers Hoffman and Gapinski [10] evaluated samples of
provide historical background on alloys for use in a 20Cr-32Ni-Nb cast outlet manifold that had de-
hot outlet headers. veloped fatigue cracks after it had been in service
for approximately 192 months at an outlet gas
temperature of 871 °C. In addition to carbide and
silicide precipitation, they observed carbide coa-
4 Limit of Tube lescence. The observed aging significantly de-
Metal Use graded the tensile strength, Charpy V-notch im-
pact resistance, stress-rupture strength and
Internal Pressure, MPa

weldability of the material. The carbides and sili-

3
NH3 cides were solutionized by annealing at 1093 °C.
However, complete solutionizing of secondary
precipitates and spheroidization of the primary
2 carbides required a minimum annealing tempera-
H2 ture of 1149 °C. Better stress-rupture properties
CH3OH were achieved by solution annealing at 1204 °C
1 than by solution annealing at 1093 or 1149 °C.
The cracked region of the manifold was success-
fully repaired after in-situ solution annealing at
0 1149 °C for three hours and operated successfully
700 800 900 1000 for four more years before the furnace was rebuilt.
The authors recommended keeping Si content as
Gas Temperature, °C
low as possible and maintaining a stoichiometric
Figure 1. Typical operating temperature and pres- Nb/C ratio of 7.7.
sure ranges for ammonia (NH3), hydrogen (H2), and
methanol (CH3OH) reformers, from Kawai, et al. [1].
Welding and Repairs
Shibisaki, et al. [6] found that Si, Nb, and C addi-
tions had a negative effect on the ductility of Roach and VanEcho [11, 12] found that weld-
20Cr-32Ni-Nb cast alloys while Mn had a positive ments generally have lower stress-rupture strength
effect on their ductility. Parks and Schillmoller [7] than comparable base metals. Inconel 182 weld-
indicated that Alloy 800H has a low tendency for ments had the lowest stress-rupture strength when
embrittlement but noted that the 20Cr-32Ni-Nb compared with Inconel 82, Inconel 112, and Inco-
cast alloy has higher creep-rupture strength than Weld A weldments. Several reformer operators
Alloy 800H. Thomas, et al [8] pointed out a se- [13-15] have experienced accelerated creep dam-
rious embrittlement issue with the 20Cr-32Ni-1Nb age, embrittlement, and failures with Inconel 182

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 weld metal. Failures have been attributed to a loss The beveled area is then covered using Inconel
of rupture strength caused by embrittlement. Inco- 182 electrodes, and the previously ground grooves
nel 182 is now known to exhibit a loss of rupture are filled up by welding following a stringer bead
strength and ductility at elevated temperatures. technique. The shortcoming of this repair method
is that Inconel 182 welds have poor high-
Commonly used materials for joining Alloy 800 temperature creep strength.
are the Inco-Weld A electrode and Inconel 82 fil-
ler metal. Avery and Valentine [5] specifically Pande and Swenson [22] successfully completed a
recommended filler metal Inconel 82 for Alloy preliminary repair by welding a reinforcement
800 welds. Roach and VanEcho [11, 12] indicated cone onto sound material in the tees to extend op-
that Inconel 82 weldments have higher stress- erating life. Blackburn [5] developed a method to
rupture strength than Inco-Weld A and Inconel improve weld efficiency using parent metal as fil-
182 weldments, but lower stress-rupture strength ler after completing the root weld with Inconel 82
than Inconel 112 weldments. McMillan [13] wire.
found success in using Inco-Weld A material in
place of failing Inconel 182 filler metal. Shi and Lippold [23] found that repair practices
that lead to failures often involve elevated temper-
Shibisaki, et al. [16] recommended the use of a atures throughout welding repairs leading to em-
high-nickel alloy metal (Inconel 82) for welding brittlement, which in turn gives rise to a ductility
20Cr-32Ni-Nb metals. Kobrin [15] obtained supe- dip. When the elevated temperature restraint ex-
rior results using Inconel 82, Alloy 625 filler met- ceeds the ductility minimum, failure occurs.
al, and Inconel 112 in place of Inconel 182. Or- Another common problem is the mechanism of
bons [17] suggested using Inconel 112 in place of hydrogen induced crack formation which leads to
Inco-Weld A for applications at temperatures weld failures. Pattabathula, et al. [24] noted this
above 816 °C because of its superior resistance to can be mitigated by increasing the temperature at
creep damage. Roach and VanEcho[11, 12] also the weld above dew point, by adding outside sur-
found that Inconel 112 had superior creep resis- face insulation, and by installing windshields on
tance to those of Inco-Weld A, Inconel 182, and sides of the furnace.
Inconel 82 weldments. van Wortel [18] noted that
filler metals 82 and 617 were found to be suscept- Another problem with welding operations, pointed
ible to relaxation cracking. For applications that out by Shibisaki, et al. [25], involves differences
require the highest strength and corrosion resis- between weld and base metal. The difference in
tance, Inconel 117 electrode and Alloy 617 filler thermal expansion coefficients can lead to elastic-
metal are recommended [19] for use at tempera- plastic strain of the weld material. Orbons [17]
tures above 788 °C. suggested high-temperature preheating around the
weld to prevent cracking of the base metal caused
Al-Jubeihi [20] reported making successful repair by weld shrinkage. Lobley, et al. [26] found that it
welds by grinding out cracks, depositing Inco- was necessary to bore machine and solution an-
Weld A stringer beads, and grinding out welds neal a 20Cr-32Ni-Nb cast header prior to repair
and base metal defects one bead at a time while welding because of its severe embrittlement in the
using dye penetrant tests and ultrasonic examina- aged condition, especially near the inner surface.
tions to ensure quality repairs. Another successful
repair method [21] involves grinding into through- Anderson and Bruno [27] reviewed weldability is-
wall cracks to remove 60% of the cross-section sues that they encountered during the welding of a
and grinding back the surface area by 5 mm to new cone piece to an existing tee (aged material)
prevent re-cracking associated with embrittlement. in a hydrogen reformer outlet manifold. Both

AMMONIA TECHNICAL MANUAL 86 2011

2011 [86] AMMONIA TECHNICAL MANUAL
 pieces were 20Cr-32Ni-Nb castings from the same was applied. DP inspection was performed fol-
foundry. Metallurgical analysis of samples of the lowing every second fill pass and after blend
previously installed, aged cone piece on which an grinding the cap pass.
Electrode 117 weld bead had been deposited re-
vealed both heat-affected zone (HAZ) liquation
cracking (LC) and reheat cracking. As shown in
Figure 2, the liquation cracking occurred near the
fusion zone (FZ) and was believed to be caused by
low melting point silicate precipitates that had
formed during service. The reheat cracking was
believed to have been caused by a combination of
mismatched mechanical properties and high inclu-
sion content. A full solution annealing of the aged
material was required to weld it successfully.

Figure 3. Location of cracking in aged 20Cr-32Ni-

Nb cast tee piece after welding a new cone piece to it,
from Penso and Mead [28].

Jack [29] reported cracking in a 21/33 weld be-

tween a tee and a subheader in a cast 20Cr-32Ni-
Nb outlet manifold after 14 years of service at ap-
proximately 793 °C. This cracking is shown in
Figure 4. Attempts to grind out and repair the
cracking were not successful, so tapered sleeves of
Alloy 800HT were designed and welded over the
Figure 2. Liquation cracking in heat-affected zone cracked weld and similar welds in the outlet mani-
(HAZ) of aged 20Cr-32Ni-Nb casting, from Anderson fold.
and Bruno [27].

Penso and Mead [28] discussed cracking that they

found on existing 20Cr-32Ni-Nb statically cast tee
pieces when a new centrifugally cast 20Cr-32Ni-
Nb reducer cones were welded to them. The loca-
tion of this cracking is shown in Figure 3. It was
found to be associated with intermetallic silicate
precipitates in the existing (aged) material. The
tees were cut out and solution annealed at
1150 °C, followed by machining out of all of the
cracks. Welding was done using a GTAW process
with Alloy 617 filler wire, a 50 °C preheat, and a
maximum interpass temperature of 150 °C. A but-
Figure 4. Cracking at subheader to tee weld; both
tering layer was first applied using low amperage.
are 20Cr-32Ni-Nb castings, from Jack [29].
The joints were then tack welded, and a root pass

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 Dejaeger, et al. [30] discussed cracks in an Alloy Recent Hot Outlet Header Issues
800H outlet header. In this case, the header was
manufactured using a solution annealed Alloy To highlight some recent issues with hot outlet
800H plate material that was cold formed into a headers, three case histories are reviewed. The
cylinder and then longitudinally welded with Ni- first two cases cover outlet headers from methanol
base filler. No heat treatment was applied after the reformers, while the third case is for an outlet
manufacturing process. After two years, a leak header from a hydrogen reformer.
was detected. Examination revealed the cause to
Case 1. Metallurgical Analysis of a Header
be high residual stresses from fabrication (cold-
to Bull Tee Weld from a Methanol
working/welding) or resulting from cyclic defor-
Reformer
mation and accompanying relaxation processes.
Stress relaxation cracking was controlled in the A metallurgical analysis was performed on a bull
replacement header by a stabilization heat treat- tee from a methanol reformer outlet header. The
ment at 950 °C performed before welding. After tee was connected to two header tubes and an in-
welding, a second heat treatment at 850 °C was creaser cone. The tee was removed when leaks
performed to decrease weld residual stresses. This were discovered at the girth welds after approx-
method successfully controlled the stress relaxa- imately 50,000 hours of service.
tion cracking in the Alloy 800H material. Howev-
er, this stabilization heat treatment temperature The header, tee, and increaser cone were made of
was less than the recommended value [18] of a cast alloy 20Cr-32Ni-Nb alloy. The welds used
982 °C, and the post-weld heat treatment (PWHT) to join these components were made using an In-
temperature was less than the recommended val- conel 82 root pass, Inconel 82 or Inconel 182 rein-
ue [31] of 900 °C. forcement, and Inconel 182 for the remainder of
the weld. Thus, the majority of the weld filler
Brongers and Jaske [32] evaluated an Alloy 800H metal in the joints was Inconel 182.
outlet manifold that had welds made using weld-
ing Electrode 112. It was removed from service Approach. The following steps were performed
after normal operation at approximately 870 °C for this analysis. The bull tee was visually in-
for 64,000 hours because nondestructive testing spected and photographed in the as-received con-
indicated cracks in the circumferential butt welds. dition. Liquid dye penetrant testing was performed
Creep-rupture tests were performed at stress levels on the three large diameter girth welds of the tee.
comparable to the service stress and temperatures Cross-sections were removed from cracks in the
above the design temperature were selected to ac- welds, mounted, polished, and etched. Light pho-
celerate the testing. The results showed that the tomicrographs were taken to document the mor-
base metal did not suffer significant creep damage phology of cracking and microstructures. Samples
from the prior service exposure and that the weld for chemical analysis were removed from the re-
metal had a very low resistance to creep damage. ducer cone, header tube, and tee and weld metal
Metallographic analysis of a weld sample taken between the increaser cone and tee to determine
from a comparable in-service manifold supported the chemical composition.
this conclusion, and data for new material re-
ported in the literature support the finding of rela- Results and Discussion. Figure 5 is a photograph
tively low high-temperature creep strength for of the bull tee. Pigtails extended vertically from
welds made using welding Electrode 112. The au- fittings attached to the tee and indicate the top of
thors recommended using welding Electrode 117 the tee. Girth welds attached the tee the increaser
for repairs. cone and tee to two header tubes. The outside di-
ameter (OD) of both header tubes was 345 mm.

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2011 [88] AMMONIA TECHNICAL MANUAL
 The wall thicknesses of the of the header tubes ure 8 is a photomicrograph of Mount W3 showing
were measured at the 12:00, 3:00, 6:00, and 9:00 the HAZ of the tee and the weld metal. Creep
o’clock orientations. The average wall thickness cracks are present at the grain boundaries in the
of the header tube was 21.4 mm. HAZ of the tee. Creep voids and aligned creep vo-
ids are present in the weld metal. Figure 9 is a
Reducer photomicrograph of Mount W3 showing the HAZ
cone of the header tube and weld metal. Relatively
wide, and also narrow, creep cracks are present in
Figure 6
Flow the HAZ of the header tube. This photomicro-
graph was taken just below the outside surface
where the crack-like indication shown in Figure 6
Flow was located.

Flow Polishing
Flow direction
Pigtail Header for cross-
Header
section
Figure 5. Photograph of bull tee following liquid dye
penetrant testing of the girth welds.

Figure 5 also shows the tee after performing liquid Header

dye penetrant testing of the three welds. The red Crack
dye shows the locations of indications. Four loca-
tions that contain indications were identified. The
indications were located at: 1) both header to tee
girth welds, 2) a pigtail to header tube girth weld, Figure 6. Photograph of a crack located at girth
and 3) the tee to increaser cone girth weld. weld between a header and the tee; area indicated in
Figure 5.
Figure 6 is a photograph of the crack-like indica-
tion located at the toe of a header to tee girth
weld. The indication is approximately 122 mm
Figure 9
long and present from the 1:15 to 2:30 orientation.
The liquid dye penetrant testing clearly showed
Figure 8
the locations of the crack indications at the girth
welds.
Header
tube side Tee side
Figure 7 is a photomicrograph of the mounted
cross-section (Mount W3) that was removed a
header to tee girth weld (GW 3). The dashed line
in Figure 6 indicates the location where the cross-
section was removed and the arrow indicates the
polishing direction. Cracks are present in the HAZ Figure 7. Stereo light photomicrograph of a
of the tee, HAZ of the header tube, and in the mounted cross-section removed from the girth weld
weld metal. Although difficult to see, a columnar shown in Figure 6 (Glyceriga Etchant).
microstructure is also present in the header. Fig-

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2011 [89] AMMONIA TECHNICAL MANUAL
 of primary carbides was reduced and that they are
HAZ Weld metal slightly blocky, which is also indicative of high-
temperature exposure.

The most severe creep damage was on the header

tube side rather than the tee side. The intergranu-
lar crack path is consistent with a high-
temperature creep mechanism. The finer, second-
ary carbides and blocky primary carbides are in-
dicative of high-temperature exposure.

Primary
Figure 8. Light photomicrograph of the mounted carbide
cross-section showing the HAZ and weld metal near
the tee side; mirror image of area indicated in Figure Secondary
7 (Glyceriga Etchant). carbide

Weld metal

HAZ
Figure 10. Light photomicrograph of the header
base metal microstructure (Glyceriga Etchant).

The results of the chemical composition analysis

conducted on a sample removed from the base
metal of the header are shown in Table 1. The re-
Figure 9. Light photomicrograph of the mounted sults of the analyses are consistent with the no-
cross-section showing the HAZ and weld metal near minal chemical composition specifications for the
the header tube side; mirror image of area indicated alloy at the time of its manufacture.
in Figure 7.
The results of the chemical composition analysis
conducted on a sample removed from the weld
Figure 10 is a photomicrograph of the header base metal between the increaser cone and tee are
metal microstructure. The observed microstructure shown in Table 2. Except for the nickel plus co-
is consistent with that expected for the 20Cr- balt (Ni + Co), manganese (Mn), iron (Fe), and
32Ni-Nb alloy. The figure shows primary carbides chromium (Cr) content, the results of the analysis
located at the grain boundaries and smaller sec- are consistent with specified values for Inconel 82
ondary carbides dispersed in the grains. The finer, and 182. The Mn and Cr content are consistent
secondary carbides are indicative of high tempera- with the Inconel 82 specification and not with In-
ture exposure. Although it is difficult to be certain conel 182 specification. The Ni + Co and Fe con-
since the appearance of the pre-service micro- tent are consistent with the Inconel 182 specifica-
structure is not known, it appears that the network tion and not the Inconel 82 specification.

AMMONIA TECHNICAL MANUAL 90 2011

2011 [90] AMMONIA TECHNICAL MANUAL
 Table 1. Results of chemical analysis of samples re- • Creep voids were present in the heat af-
moved from the tee, header tube, and increaser cone fected zone (HAZ) and weld metal of the
compared with the nominal chemical composition for header to tee girth weld but not in the base
the 20Cr-32Ni-Nb alloy. metal.
Increaser
Element Tee Header Cone Nominal1, • Creep cracks were present in the HAZ and
Wt. % Wt. % Wt. % Wt. % weld metal at one girth weld.
Carbon 0.12 0.15 0.14 0.10 – 0.15
• Intergranular creep cracks penetrated the
Manganese 1.05 1.01 0.77 1.50 (max) outer surface in the HAZ and weld metal,
Silicon 0.63 0.50 0.65 1.50 (max) near the toe of the girth welds.
Chromium 20.62 19.91 20.01 19 – 25 • The fine, dispersed secondary carbides are
Nickel 33.03 32.61 33.02 31 – 33 indicative of high-temperature exposure.
Niobium 1.17 1.08 1.05 0.50 – 1.50 • The microstructures of the base metals
0.050 were consistent with those expected for
Phosphorus 0.019 0.016 0.017
(max) 20Cr-32Ni-Nb cast alloy.
Iron Balance Balance Balance Balance
• Except for Ni compositions for the tee and
reducer cone of 0.03 and 0.02 weight %
Table 2. Results of chemical analysis of a sample
greater than specified, the base metal
removed from the weld between the tee and increaser
cone compared with the nominal chemical composi-
composition was consistent with specified
tion for Inconel 82 and 182. values for the alloy.
Inconel Filler Inconel Welding • The composition of the girth weld was
Weld Metal 82 2 Electrode 182 2
Element Wt. % Wt. % Wt. % consistent with that of Inconel 82 or 182,
Nickel + Cobalt 65.9 67.0 (min) 59.0 (min) and in some cases, with both specifica-
tions.
Carbon 0.037 0.10 (max) 0.10 (max)

Manganese 2.74 2.5 – 3.5 5.0 – 9.5 The cracking is consistent with a high temperature
Iron 8.52 3.0 max 10.0 max creep mechanism associated with the low creep
strength of the filler material. This type of failure
Sulfur 0.006 0.015 (max) 0.015 (max)
can be mitigated by using a filler metal with im-
Silicon 0.17 0.50 (max) 1.0 (max) proved creep strength in the weld joint such as a
Chromium 20.05 18.0 – 22.0 13.0 – 17.0 “matching” filler or and Inconel 617 filler.
Niobium + Tantalum 2.42 2.0 – 3.0 1.0 – 2.5
Case 2. Metallurgical Analysis of Outlet
Phosphorus 0.003 0.030 (max) 0.030 (max) Header from Methanol Reformer
A metallurgical analysis was performed on two
The fractional increase in Ni content would not be sections from a methanol outlet header that leaked
expected to have a substantial effect on creep re- in-service. One of the sections contained the leak
sistance. The differences in the Mn, Fe, and Cr as shown in Figure 11 and the other (non-failed)
content are likely related to dilution or enrichment was located away from the leak in the same head-
that can occur with the various passes of the Inco- er. The header samples were removed from ser-
nel 82 and 182 welding materials. vice after approximately the minimum design life
of 100,000 hours. The header tube sections were
Summary. A summary of the key observations centrifugally castings made of a 20Cr-32Ni-Nb al-
follows: loy.

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2011 [91] AMMONIA TECHNICAL MANUAL
 Approach. The following steps were performed Through-wall
for the analysis. The header tube sections were vi-
sually inspected and photographed. A ring section
was removed from the through-wall portion of the
header tube section; the other header section was
already in the form of a ring. The two ring sec-
tions were polished and light photomicrographs
were taken to document the observed creep dam-
age. The ring sections were then etched in Adlers
reagent to reveal their macrostructures and photo-
graphs were taken. A small portion of each ring
was then removed, mounted, polished, and etched Figure 11. Photograph of the header tube section
with glyceregia for detailed examination. Photo- (Header Section 1), as received.
micrographs were taken to document the micro-
structure and maximum service temperatures were Figure 12 is a photograph of the ring from Section
estimated. 1, following polishing and etching. The location
of ring Section 1 is indicated in Figure 11. A co-
Using elastic finite-element stress analysis, the lumnar dendritic macrostructure was visible on
maximum tensile hoop stress in the region of the both ring sections.
header failure was calculated to be 10.2 MPa.
Failure stresses for average stress-rupture lives of
100,000 hours (11.4 years) were computed for
header operation at various temperatures using the
manufacture’s Larson-Miller parameter relation-
ship for the 20Cr-32Ni-Nb alloy. A temperature of
963 °C was calculated to cause stress-rupture fail- Through-wall
ure in 100,000 hours. This was 73 °C above the
reported maximum header operating temperature
of 890 °C. Based on this result, it is likely that the
material was somewhat weaker than indicated by
the manufacture’s data and that it was overheated Creep
to some degree at the failure location. fissures

Results and Discussion. Figure 11 is a photo-

graph of the as-received header tube section
(Header Section 1) that failed. The figure shows
the through-wall portion of the failure. Secondary
cracks are also visible in the vicinity. The cracks
were present from the right side of the tube sec- Figure 12. Photograph of Ring Section 1 from
tion up to approximately 174 mm from the right Header Section 1; dashed lines in Figure 11 indicate
side. Also visible is a bulge in the tube where the the location of the ring (Adlers reagent).
cracks are present. The maximum diameters of the
bulged and non-bulged regions of Section 1 were Measured dimensions of the tube sections are
174.0 mm and 171.0 mm, respectively. listed in Table 3 along with reported nominal di-
mensions of the tube when it was new. The no-

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2011 [92] AMMONIA TECHNICAL MANUAL
 minal inside diameter (ID) of the new header tube ID and appeared to be more prevalent adjacent to
was not reported, so it was calculated based on the the OD. The residual life of this tube section is
reported minimum outside diameter (OD) of a approximately 70% based on metallurgical analy-
new header tube minus twice the minimum sound sis and guidelines of past studies [33] of reformer
wall thickness. The strain values of the header tubes. For 11 years of prior operation, this result
tube sections were based on calculated minimum implies approximately 26 years remaining life, as-
ID values. There was more strain at the bulge in suming that future operating conditions are the
the header tube than in Header Section 2, which same as those of the past.
was to be expected. Since baseline values of orig-
inal dimensions are not available for each tube,
the strains are only approximate because of inhe-
rent variations in the dimensions of new tubes.

Table 3. Measured dimensions of header tube sam-

ples compared to minimum values reported by client.
Description Outside Wall Thick- Inside
Diameter ness (WT) Diameter
(OD) (ID)
Strain*
mm in mm in %

Minimum 168.3 6.625 15 0.591 —

new tube
Bulge on 174.0 6.850 15.0 0.592 4.10
Header Sec- Figure 13. Light photomicrograph of Ring Section 1
tion 1 adjacent to the OD surface, near the through-wall lo-
Header Sec- 172.0 6.77 15.4 0.607 2.08 cation.
tion 2
* Strain based on ID minimum and measured values. ID
calculated based on OD and WT minimums and measured Aligned
values. creep voids

Figure 13 is a photomicrograph of Ring Section 1

adjacent to the OD surface. Relatively wide and
narrow creep cracks that appeared to follow the
dendritic columnar structure were present for the
full wall thickness. A low density of creep voids
was found in the cross-section. The density of vo-
ids was not high adjacent to the ID or OD surface.
The absence of creep voids near the cracks is evi-
dence of short-term overheating. Note that evi-
dence of austenite grains and twinning was appar-
Figure 14. Light photomicrograph of Ring Section 2
ent at the ID where the through-wall cracks were adjacent to the OD surface.
present. This suggests that the ID was cold
worked during fabrication. It is not known if this Figures 15 and 16 are photomicrographs of the
contributed to the failure. microstructures of Ring Section 1, near to and
away from a crack, adjacent to the OD. The pho-
Figure 14 is a photomicrograph of Ring Section 2 tomicrographs were taken at the same magnifica-
adjacent to the OD surface. Aligned creep voids tion. The network (cored structure) of primary
(not linked) were present adjacent to the OD and

2011 93 AMMONIA TECHNICAL MANUAL

2011 [93] AMMONIA TECHNICAL MANUAL
 carbides does not appear to be intact near the er elements met the manufacturer’s specification
crack. A cored, lacelike structure was present for 20Cr-32Ni-Nb. Higher than desired niobium
away from the crack, indicating that lower tem- content may have reduced the creep strength of
peratures were present away from the crack. Also the 20Cr-32Ni-Nb alloy. This possibility was
evident near the crack was the presence of sec- pointed out in the previous review of published
ondary carbides and nitrides. The nitrides were not investigations.
evident away from the crack, which is to be sus-
pected. Nitrides are known to form adjacent to
fracture surfaces. Figure 17 is a photomicrograph
of the microstructure from Ring Section 2. The
cored, lacelike structure and secondary carbides
are present as was shown away from the crack in
Ring Section 1.

Figure 16. Light photomicrograph of the microstruc-

ture of Ring Section 1 away from a crack and near
the OD surface (glyceregia etchant).

Figure 15. Light photomicrograph of the microstruc-

ture of Ring Section 1 near a crack and OD surface
(glyceregia etchant).

Based on the microstructures observed in the

header samples and the reference material, their
maximum service temperatures were estimated to
be:
• Ring Section 1: 870°C
• Ring Section 2: 840°C Figure 17. Light photomicrograph of the microstruc-
ture of Ring Section 2 (glyceregia etchant).
The reference material had four times as much
carbon as the header samples, which made it diffi-
Summary. A summary of the key observations
cult to estimate these values. Thus, there is uncer-
follows:
tainty regarding them.
• The metallographic evidence (wide creep
The amount of niobium (1.91 wt% compared with cracks, low density of voids) suggests that
the specified range of 0.90 to 1.35 wt%) in the Header Section 1 failed by short-term over-
header section was greater than the maximum val- heating.
ue of the specified range. The amounts of the oth-

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2011 [94] AMMONIA TECHNICAL MANUAL
 • Ring Section 2 showed metallographic evi- Results and Discussion. Figure 18 is a photo-
dence of creep damage. The remaining life of graph of Ring Section 1 following polishing. The
this section was estimated to be 70%, while ring section was approximately 220 mm in diame-
the maximum service temperature was esti- ter by14.5-mm thick by 64 mm wide. Ring Sec-
mated to be 840°C. tion 1 contained an inlet port for a pigtail, as indi-
• Using finite-element stress analysis, the max- cated in the figure. The port was approximately
imum tensile hoop stress in the region of the 31.8 mm in diameter and the wall was thicker at
header failure was calculated to be 10.2 MPa. this location, approximately 15.9-mm thick.
For this stress, a temperature of 963 °C was
calculated to cause stress-rupture failure in
100,000 hours, indicating that the material Polished
was either overheated, weaker than expected, surface
or a combination of both. Cracks

Case 3. Metallurgical Analysis of Outlet

Header a Hydrogen Reformer
Port for
During an inspection, a significant increase in di-
pigtail inlet
ameter was noted in one of two headers in a hy-
drogen reformer. The headers were made of the
cast 20Cr-32Ni-Nb alloy. The portion of the re-
former that fed gas to this header was known to Figure 18. Photograph of Ring Section 1 after po-
have been operating at higher than desired tem- lishing.
peratures. Further inspections revealed the pres-
ence of cracks in the header, especially in the Indicated and visible on the polished surface is an
around the holes where fittings for the outlet pig- OD surface breaking crack that is within the limits
tails were attached. As a result, the operator de- of the previously mentioned port. Although not
cided to replace the header and cut out two ring visible in the figure, a crack of similar size is lo-
sections for metallurgical failure analysis. Ring cated on the ID surface of the port, below the visi-
Section 1 was from the central portion of the ble crack.
header tube where the increase in diameter was
the largest and the most material damage was ex- Ring Section 2 was approximately 217 mm in di-
pected to be found. Ring Section 2 was from near ameter by 14.3 mm thick. The location of interest
the end of the header tube where the increase in on the ring had a red marking.
diameter was the smallest and the least material
damage was expected to be found. Metallographic Examination. Figures 19 and 20
are photomicrographs of Met Section 1a (removed
Approach. Ring Sections 1 and 2 were visually from Ring Section 1) taken adjacent to the OD
inspected and photographed and then were po- and ID surface, respectively. Met Section 1a was
lished and photographs were taken to document removed near the port of the pigtail inlet. The re-
the observed creep damage. Two portions from sidual life of the tube section that Ring Section 1
Ring Section 1 and two portions from Ring Sec- was removed from is approximately 20% based on
tion 2 were removed, mounted, polished, and the metallurgical analysis and guidelines of past
etched with glyceregia. Photomicrographs were studies [33]. Based on the smaller size of the indi-
taken to document the creep voids prior to etching vidual voids in the figures compared to the thicker
and to document the microstructure after etching. width of the cracks indicated in Figure 19, it ap-

2011 95 AMMONIA TECHNICAL MANUAL

2011 [95] AMMONIA TECHNICAL MANUAL
 pears that the material tore after the creep voids Met Section 1b was removed from Ring Section
aligned. This tearing of the material suggests, but 1opposite the port of the pigtail inlet. The density
does not indicate, that high-temperature creep was of the voids throughout Met Section 1b was low.
involved. A high density of voids, but no cracking Minor aligning of the creep voids was visible ad-
was observed near the ID surface. The aligning jacent to the OD surface.
and linking up of the voids appears to follow the
dendritic columnar structure adjacent to the OD Figure 21 is photomicrograph of Met Section 2a
surface. The location of the voids adjacent to the (removed from Ring Section 2) taken adjacent to
ID surface suggests an equiaxed fine-grained the OD. The residual life of the tube section that
structure. The density of the voids is higher adja- Ring Section 2 was removed from is approximate-
cent to the ID surface. ly 60% based on the metallurgical analysis and
guidelines of past studies [33]. Met Section 2b
was removed opposite from the location marked
in red on the OD surface. The density of voids in
on both met sections, throughout the wall thick-
ness, is uniform and high. The voids adjacent to
the OD surface are aligned (as shown in Fig-
ure 21) and appear to follow a dendritic columnar
structure. The location of the voids adjacent to the
Cracks/aligned ID surface suggests an equiaxed fine-grained
creep voids structure. Thus, even though Ring Section 2 had
less creep damage than Ring Section 1, it still had
a significant amount of creep damage.

Figure 19. Light photomicrograph of Met Section

1a, taken adjacent to the OD surface and near the
pigtail inlet (as polished).

Aligned
creep voids

Figure 21. Light photomicrograph of Met Section

2a, taken adjacent to the OD surface and near the
red marking (as polished).

Figures 22 and 23 are photomicrographs of the

microstructure of Met Section 1a (removed from
Ring Section 1) near the pigtail inlet. The figures
Figure 20. Light photomicrograph of Met Section show primary carbides located at the grain boun-
1a, taken adjacent to the ID surface and near the pig- daries and secondary carbides dispersed in the
tail inlet (as polished). grains. The network of primary carbides is more

AMMONIA TECHNICAL MANUAL 96 2011

2011 [96] AMMONIA TECHNICAL MANUAL
 intact near the ID surface than near the OD surface overheated since there is a severe reduction in the
which indicates that the OD surface was subjected amount of primary and secondary carbides there.
to higher temperatures than the ID surface.

Demarcation

Figure 24. Light photomicrograph of Met Section

Figure 22. Light photomicrograph of Met Section 1a, taken adjacent to the OD surface and near the
1a, taken adjacent to the OD surface and near the pigtail inlet showing the decarburized region (glyce-
pigtail inlet (glyceregia etchant). regia).

For the microstructure of Met Section 1a (re-

moved from Ring Section 1), opposite the port of
the pigtail inlet, the network of primary carbides is
less intact and more secondary carbides are dis-
persed in the matrix adjacent to the OD surface as
compared to the ID surface.

For the microstructure of Met Section 2a (re-

moved from Ring Section 2), at locations 180°
from each other, the network of primary carbides
adjacent to the OD surface at both locations is less
intact than at the ID surface. Again, the structure
of the primary carbides indicates that the OD sur-
face was subjected to higher temperatures than the
Figure 23. Light photomicrograph of Met Section ID surface. The quantity of secondary carbides
1a, taken adjacent to the ID surface and near the pig-
appears to be similar when comparing the loca-
tail inlet (glyceregia etchant).
tions adjacent to the OD and ID surface.
Figure 24 is a photomicrograph of the microstruc-
Summary. A summary of the results follows:
ture of Met Section 1a (removed from Ring Sec-
tion 1) adjacent to the OD surface. A demarcation
• For Ring Section 1, the width of the creep
is visible in the figure. There is no evidence of a
cracks near the port for the pigtail inlet suggests
network of carbides above the demarcation and
a high temperature creep mechanism. A decar-
there is a network below the demarcation. The re-
burized region near the port indicates that the
gion where the demarcation is present was likely
material was locally overheated. The creep

2011 97 AMMONIA TECHNICAL MANUAL

2011 [97] AMMONIA TECHNICAL MANUAL
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AMMONIA TECHNICAL MANUAL 98 2011

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