HTHA in Ammonia Plants.

A review of inspection
methods and gap with Nelson's curve
High-temperature hydrogen attack (HTHA) is a time-dependent damage mechanism that can occur
in process equipment exposed to hydrogen at elevated temperatures (above 200°C). In ammonia
plants, equipment and lines in the syngas generation system are typically subjected to these condi-
tions. The classic approach using API-941 Nelson's curves proved to have uncertainties, and no effect
of time is considered. Furthermore, after reviewing Nelson's curves where C- 0.5Mo has been consid-
ered equivalent to carbon steel, the re-validation of old plants operating for more than 40 years re-
sulted in several equipment falling in a non-safe area of the diagram. The combination of advanced
UT NDT (non-destructive testing) and recent development in the accuracy of these techniques gave
the possibility for a detailed monitoring of crack evolution, however, a big gap still exists with respect
to lifetime assessment. Despite JIP and API-579 announcements, an FFS and lifetime assessment
model is still unavailable in industry standards. Scope of the paper is to review the most recent devel-
opment on NDT techniques for HTHA detection. A practical case of the HTHA inspection program
applied in a recent turnaround of an ammonia plant in operation for more than 40 years will be pre-
sented.

Stefano Cavalleri, Giulio Paci

Yara International ASA

Johan Thoelen
In2mat

Introduction • Exposure time

E quipment in ammonia plants are exposed

to a variety of degradation mechanisms. In
the front-end particularly, where a combi-
nation of hydrogen and high pressure is present,
Typically, the risk of HTHA is assessed using
API-941 Nelson's curves [9]. Although this ap-
proach is useful for screening of a specific com-
ponent's susceptibility to HTHA degradation, it's
High-Temperature Hydrogen Attack (HTHA) is not adequate for a detailed assessment and a re-
present. HTHA is a well-known mechanism that sidual lifetime estimation [10].
has been the object of extensive studies in the These curves represent an interpolation of rec-
past [1]-[8]. However, several challenges are still orded failure/non-failure events for different ma-
present for plant owners/operators as the evolu- terials (C-steel and low-alloy steel), and, a certain
tion of HTHA damage is still difficult to predict margin of uncertainty is present, and no safety
and, because of the equipment aging, the risk of factor is considered. Particularly for carbon steel,
failure due to this mechanism is increasing. being part of the curves at lower hydrogen partial
HTHA is a degradation mechanism that involves pressure, i.e. below 1 MPa (150 psi) almost ver-
several parameters; the main ones are: tically, a slight variation in the hydrogen pressure
• Hydrogen partial pressure leads to a considerable difference in the limiting
• Operating temperature temperature. Hence high inaccuracy is present.
• Material of construction Furthermore, Nelson's curves account for hydro-
• Stress level gen partial pressure and temperature only as a
variable, while stress level and exposure time are opening the possibility of early-stage HTHA
not considered. It's well known that residual flaw detection. The scope of this paper is to pre-
stresses can play a considerable role in increasing sent the most recent development in NDT tech-
the susceptibility to HTHA; however, depending niques for HTHA detection and present a practi-
on the design safety margin and the geometrical cal case of an inspection program applied in a
configuration, components can experience high- recent turnaround of a Yara ammonia plant in op-
stress level although stress relieved. Forged piece eration for more than 40 years.
with geometrical notches, pipe elbows and tees
are examples of stress concentration.
Exposure time is a fundamental parameter as Advanced NDT techniques for
well for determining the risk of HTHA damage HTHA
which is not considered in the Nelson's curve ap-
proach. A typical scenario is related to old pieces HTHA inspections can be challenging as the
of equipment, i.e., having more than 35 years of early stages of attack with fissures, or even small
life, operating slightly below the Nelson's curve, cracks, can be challenging to differentiate from
which could have some risk of HTHA and need metallurgical defects, impurities, or other crack-
to be followed up. On the other side, there could ing mechanisms. The advanced stage of attack,
be upset conditions where a high temperature with considerable cracking, is much easier to de-
above the limiting curve is reached for a short pe- tect, but at that point there is already a higher
riod of time, measurable in months. For both sce- likelihood of equipment failure. For this reason,
narios in the standards and/or recommended several efforts have been carried out to develop
practices, there is no model to account for the ex- more efficient inspection ultrasonic techniques
posure time, and the risk assessment is based on with a special focus on inspection effectiveness
the engineering experience only. and the quality of the images. Effective inspec-
In the API RP 581 2nd Edition published in 2008 tion techniques for detecting early stages of
[11] a quantitative risk assessment model was HTHA involve a combination of various ultra-
proposed to quantify the HTHA susceptibility us- sonic examination techniques, including time of
ing a parameter, Pv, which was a function of the flight diffraction (TOFD), phased array ultrason-
hydrogen partial pressure (ppH2), temperature ics (PAUT) with full matrix capture (FMC), and
and time. However, this assessment has been re- total focusing method (TFM) on welds. A thor-
moved from the last revision of the API 581 [12] ough internal examination, including surface
and it's no longer applicable. preparation with abrasive blast media, visual in-
In the last years, several papers proposing possi- spection for blisters and high-sensitivity wet flu-
ble approaches to close the gap have been pub- orescent magnetic particle examination (HS
lished [13], [14] and Joint Industry Programs WFMT) on 100% of welds and any blistered or
(JIP) have been initiated to combine industry ex- bulged locations plus a radius around the blister
perience and knowledge. A chapter of API- is an effective protocol for detecting HTHA dam-
579/ASME-FFS [15] dedicated to HTHA was age. Many owners/operators are specifying in-
announced for the 2021 editions with the promise specting 100% of welds with the ultrasonic tech-
to provide a quantitative approach for assessing niques described above. API 586 section 2 [16],
HTHA damage and for the lifetime calculation currently under revision, can be used as a refer-
based on fracture mechanics and a dedicated ence for the inspection area definition and prior-
crack growth model. In the final release of the itization. Highlighted techniques may detect the
document, however, this part has not been in- early stage of HTHA, but proper calibration and
cluded, and the HTHA damage remained uncov- qualifications of both equipment and operator
ered. Nevertheless, the inspection techniques im- must be performed. Conventional backscattered
proved considerably in the last few years, UT has been a primary technique in the past.
Backscattered UT includes several sub-tech- sion study followed by an RBI program was es-
niques " outside the scope of discussion on this tablished throughout the entire ammonia plant,
paper. Nowadays, these techniques for detection including the utilities.
and characterization of HTHA are considered Lack of resources, time and due to Covid require-
less effective than the new techniques mentioned ments still in place, some inspection tasks were
above. However, backscattered UT can be con- not executed or skipped. Nevertheless, the turna-
sidered an appropriate approach for HTHA in- round was accomplished with some important
spection. Encoded UT techniques as well proved milestones reached (like the full refurbshiment of
to be effective for detecting HTHA damage. Two convection section of Primary Reformer as well
or more recommended UT techniques are often as a total refractory restoration inside the Second-
combined to overcome any single technique's ary Reformer) and can be considered as a starting
limitations. The use of the highest practical fre- point for the continuous improvement of the reli-
quency (e.g., 7.5 MHz to 10 MHz) is recom- ability of the plant.
mended to achieve maximum detection sensitiv-
ity for micro-damage detection. Selection of
frequency of equivalent wavelength to discrimi- Challenges in RBI program and
nate HTHA from metallurgical imperfections is inspection plan
recommended. For example, using a 10 MHz 0-
degree longitudinal wave combined with a 5 The corrosion study (RBI assessment) was com-
MHz transverse wave angle beam is useful to de- pleted on the ammonia plant for equipment and
termine, by comparing the two signals, the orien- piping loops with a Yara standardized methodol-
tation of a possible imperfection. The use of "typ- ogy following the API 580. The primary finding
ical" shear wave frequency in the 3.5 MHz to 5.0 derived from this study was the confirmation that
MHz range may also be included to enhance the several corrosions or integrity loops have been
characterization of coalesced or macrocracking operating close to or slightly above the API 941
associated with adjacent micro-damage. A sum- Nelson Curves for a prolonged period (>50
mary of the applicable techniques to detect years) and, as such, were considered high risk
HTHA damage with details of effectiveness and due to potential for an on-stream failure from
applicability is reported in Table 1. high-temperature hydrogen attack (HTHA).
The main reason for that is related to the usage of
C-0.5Mo material, which was believed to have a
Inspection program recently higher resistance than normal carbon steel but
applied in a Yara Plant has been removed from the Nelson's curves since
1990. Benefit of PWHT was also largely under-
Yara is expanding its business in Latin America estimated in the past, and many pieces of equip-
and, with this purpose, an ammonia plant in Bra- ment with medium-low thickness were built
zil was acquired in 2019. The new plant was then without a prescription of PWHT.
included into the Yara reliability frame as per Yara plan is to consider a replacement of the lines
other existing Yara's facilities. However, due to and equipment with the higher risk. However, a
some lack of information and different approach detailed inspection program based on the risk
in the inspection and maintenance strategies ranking has been applied as a short-term ap-
taken by the previous owner, a survey to rank the proach to assess the HTHA damage and define a
most critical assets and define a dedicated inspec- monitoring program. Table 2 summarizes the
tion plan for the coming turnarounds has been pipes and equipment object of this study, includ-
carried out by the Yara's Operational Excellence ing a criticality ranking based on the difference
team. As part of the reliability journey, a corro- between the operating temperature and the Nel-
son's curve limit.
 TOFD PAUT FMC/TFM
Reflective, diffraction and scatter based.
Longitudinal and waves. Linear and 2-D
matrix arrays. A*-, B**-, C***-, D****-
Reflective and diffraction-based. Longi-
Diffraction and time-based. Longi- scan 2/3D imaging. FMC data acquisi-
tudinal and shear waves. Linear, 2-D
tudinal-longitudinal diffraction tion scheme that involves the collection
matrix and annular arrays. A-, B-, C-, D-
mode setup of pair transducers. B- of all possible combinations of sources
, S- scan 2D imaging. Pulse-echo
Description and D-grayscale 2D image of the and receivers in an array, and TFM im-
scheme (using higher frequency sound)
digitized A-scan. Higher frequen- aging scheme that involves computation
increases capability for detection of
cies increase the capability for de- of a focused image on every point of an
HTHA in base material and weld-
tection of HTHA at weldments. imaged region (using high-frequency
ments/HAZ.
sound) to increase the capability for bet-
ter detection and sizing of HTHA in
base material and weldments/HAZ.
Usually effective: Can detect Stage Usually effective: Can detect Stage 2 Usually effective: Can detect Stage 2
Detection capabilities
2 HTHA in base metal, weld HAZ, HTHA in base metal, weld HAZ, and at HTHA: in base metal, weld HAZ, and at
effectiveness
and at weldments. weldments. weldments.
Usually effective for length and Usually adequate for length and depth
depth (location) and height sizing. Usually effective for length and depth (location), height and width sizing.
Sizing effectiveness a Not effective for precise location (location), height and width sizing when When appropriate inspection setup is
and sizing (width) perpendicular to appropriate inspection setup is used. used, better effectiveness can be
the scanning direction. achieved than PAUT.
• With a combination of these techniques, proper characterization between HTHA damage and large fabrication
flaws (e.g. lamination in base metal, LOP, LOF, slag, isolated porosity, and inclusion) can be effective through
indication location, advanced imaging and pattern recognition.
• Difficult to distinguish early-stage HTHA from inclusions/impurities.
• Difficult to distinguish HTHA-induced cracking versus cracks induced with potentially other damage mecha-
Characterization nisms from one inspection data set.
capability • Encoded data storage makes it possible to perform more reliable monitoring of indications from multiple inspec-
tions than conventional methods.
• The fundamental principles of early characterization techniques (backscatter signal pattern recognition, frequency
spectrum analysis, and velocity ratio) are still applicable to further assist in indication characterization. These
techniques can be applied on data collected from new techniques (TOFD, PAUT, and TFM) to improve capabil-
ity and confidence for characterization between HTHA and other damage mechanisms.
Higher inspection speed for a paral-
lel scan and lower inspection speed
for combined parallel and nonparal-
lel scans. — Consideration is to be
given to the blind zone created by
Greatest effectiveness was achieved in
the ID response's leading edge, Greatest effectiveness was achieved in
near field of the transducer used and us-
masking low amplitude responses the near field of the transducer used.
ing a high-density reconstruction grid.
from adjacent flaws and/or flaws lo- (Typ. Minimum of 32 elements for
Comments (Typ. Minimum of 64 elements for a
cated in the shadow zone caused by thickness 1 in./25mm and 64 for  1
typical 10 MHz transducer and 65,000-
the ID geometry. Similarly, inspec- in./25mm). Lower but practical inspec-
1,000,000 grid points). Lower but prac-
tions from the ID will create a near- tion speed.
tical inspection speed.
surface blind zone due to the lateral
wave. Supplemental techniques
such as PAUT or FMC/TFM should
be considered where damage within
the blind zones is a concern.

NOTE 1 Techniques must be developed/assessed/applied according to case-specific applications (e.g. thickness, geometry, the material of construc-
tion, access, etc.)
NOTE 2 Optimized and validated procedures to include well-tuned application-specific setups for TOFD, PAUT, and FMC/TFM.
NOTE 3 Operators should have HTHA-specific training and qualifications.
NOTE 4 Validation or progressive qualification may be conducted using scoop or boat sampling or destructive testing.
NOTE 5 Early-stage HTHA damage may not be ID surface connected.
Effectiveness is based upon Stage 2 volumetric damage. Full inspection effectiveness (versus detection capability) will be covered in future effort to
address API 581 inspection effectiveness guidance.

*
= A-scan is one dimensional presentation of time versus amplitude of UT signal
**
= B-scan reflection (cross-sectional view) from the top and bottom of the test object & flaws as the probe moves along a line (one axis)
***
= C-scan is analogous to a radiograph film. The external details of the test object are projected onto a plane that is the UT machine screen.
****
= D-scan represents the test object cross-sectional view for full-thickness

Table 1. Recommended ultrasonic techniques for HTHA

 Equipment/piping ID Material of Construction Operating T(°C) pp H2 POF

R-7003 Secondary C-0.5Mo steel field weld (not post weld

Refractory lined. Max al-
Reformer to E-7101 heat treated) in transition section between 927KPa Medium - High
lowable temp 260°C
Reformed Gas WHB Sec Reformer and RGWHB.

Carbon steel (refractory lined) C-0.5Mo

E-7101 Reformed Gas Waste
steel (outlet shell & nozzles), all post 384°C 927KPa Medium - High
Heat Boiler
weld heat treated (PWHTed)
E-7101 to D-7107 C-0.5Mo steel No PWHT 384°C 927KPa High
D-7107 Shift Converter Sepa- C-0.5Mo steel with 410SS cladding, all
384°C 927KPa Medium - High
rator PWHTed
D-7107 to R-7104A C-0.5Mo steel No PWHT 384°C 927KPa High
415°C
R-7104A Shift Converter C-0.5Mo steel PWHTed 1045KPa High
(outlet)
R-7104A to E-7108 C-0.5Mo steel No PWHT 415°C 1045KPa High
E-7108 HT Shift Exchanger – Original C-0.5Mo unit replaced by new F11 Cr-Mo exchanger in 2015
E-7108 to E-7109 C-0.5Mo steel No PWHT Approx 350°C 1045KPa Medium
E-7109 Exchanger – Original C0.5Mo unit replaced by new F11 Cr-Mo exchanger (1995?)
E-7108 to R-7104B (by-pass Carbon steel No PWHT Approx 350°C 1045KPa Low
normally closed)
E-7114 to E-7108 C-0.5Mo steel No PWHT 320°C 1740KPa Medium - High
E-7108 to R-7105 C-0.5Mo steel No PWHT 290°C 1740KPa Medium - High
310°C
R-7105 Methanator C-0.5Mo steel PWHTed 1740KPa Medium - High
(outlet)
R-7105 to E-7114 C-0.5Mo steel No PWHT 310°C 1740KPa High
Original C-0.5Mo shell found to contain network of cracks in 2013, assumed to be high tem-
E-7114 perature hydrogen attack, adjacent the inlet nozzle. Section of damaged shell replaced by new
Medium - High
Methanator Exchanger 1.25Cr-0.5Mo steel material in 2013, however section of original C-0.5Mo shell material re-
mains in service.
E-7114 to E-7115 C-0.5Mo steel No PWHT <250°C 1740KPa Low

Table 2. Summary of the equipment potentially susceptible to HTHA

All the items belong to the so called "Secondary

Reformer / Shifted Gas and Methanation" corro- Item #1: Shift converter separator D-7107
sion loops highlighted in an extraction of the pro-
cess flow diagram shown in Figure 2. Red rows This separator vessel was reportedly manufac-
represent the items for which the inspection is tured from C-0.5Mo steel in 1968 with a grade
mandatory in the 2022 turnaround; orange is for 410 stainless steel liner covering the internal sur-
the items that must be inspected in the next two face. The manufacturing drawing states that the
year. In contrast, in yellow and green, medium or vessel has been post-weld heat treated. It is as-
low-priority assets have been indicated for which sumed that this 410 SS liner intended to provide
a deferral of the inspection through to a future a barrier to reduce hydrogen absorption into the
opportunity outage or planned turnaround can be steel components. Given that the liner is a mar-
considered. Figure 1 shows the API-941 diagram tensitic stainless steel, this material will provide
with indication of the operating points (tempera- negligible benefit to reducing the hydrogen par-
ture vs. hydrogen partial pressure) for all the tial pressure at the shell's internal surface.
items operating above the reference Nelson's
curve.
 Figure 1. API-941 diagram with an indication of the items operating above the Nelson' curve

As such, when assessing the potential for HTHA, Based on the intensive scope of inspection for
the presence of this liner should effectively be ig- HTHA assessment, a specialized company was
nored. Consequently, this C-0.5Mo vessel oper- called to cover the scope for HTHA inspection.
ates well above the carbon steel Nelson Curve The company was accredited to have NDT tech-
and has been assigned to be susceptible to high- nicians with several experiences in HTHA in-
temperature hydrogen attack (HTHA). The loca- spections and in addition a Level 3 third party in-
tion on the Nelson Curve is similar to E-7101, as spector was involved on call to review the
shown in Figure 1. inspection report where doubts in findings inter-
The following inspections were recommended to pretation were encountered. As a result, the scope
be carried out during the 2022 TA. of the inspection was much more detailed from
what originally considered based on experience
• Ultrasonic examination (PAUT Angle and as summarized in the previous bullet points.
beam) on all shell circumferential welds In Figure 3 and Figure 4 respectively, the areas
and longitudinal welds for HTHA and object of inspection for vessel D-7107 (Shift
cracking. Converter Separator) with the indication of dif-
• Ultrasonic examination (PAUT Angle ferent applied techniques and a typical outcome
beam) on inlet and outlet nozzles; note of a PAUT scan are shown. As the quality of ma-
these nozzles appear to have reinforce- terials and welds was lower during equipment
ment pads which will restrict inspection manufacturing, the main challenge is distinguish-
of these welds. ing between a material impurity or weld inclu-
• Internal visual inspection to confirm in- sion and an HTHA defect.
tegrity of liner material.
All the main welds (circumferential, longitudi- 0.5Mo steel. Details of the post weld heat treat-
nal, nozzles) were inspected by applying the ad- ment procedure, namely soak temperature and
vanced UT techniques with the following results: soak period, were not known, and therefore the
procedure's effectiveness could not be ascer-
• The bottom-to-shell and upper-head to tained.
shell welds were not inspected by TOFD
as the inspection tooldidn't fit in the ac-
cessible area. They were hence inspected
by phased array and TFM
• All the inspected welds didn't point out
damage related to the early stages of
HTHA

Figure 2. PFD of Secondary Reformer / Shifted

Gas and Methanation Loop with an indication
of the assessed items (R-7103 = Sec. Ref., R-
7105 = Methanator, R-7104A = HT Shift
Coverter, D-7107 = Shift Converter Separator,
E-7106 = Synloop WHB, E-7114 = Methanator
exchanger )

The welds of nozzle 4 and nozzle 1 presented

large near OD signal in through scan. As this
could be a geometry-based indication, MT was Figure 3. D-7107, General assembly of the vessel
performed with no HTHA evidence. and detail of the inspected areas

Item #2: Inspection of methanator R-7105

This methanator vessel was reportedly manufac-

tured in 1968 with post-weld heat treated C-
 Figure 5 and Figure 6 show NDT technicians in-
volved in the inspection and an example of signal
from the weld listed and WC2 showing only in-
clusions in the base material and weld volume.

Figure 4. D-7107, example of PAUT scan with

rounded isolated indications in welds typically
associated to inclusions. No signs of HTHA

This C-0.5Mo methanator has operated above the

carbon steel Nelson Curve during its life accord-
ing to normal operating conditions and, as such,
it has also been assigned to be susceptible to
HTHA. The risk of HTHA is exacerbated by the Figure 5. NDT technicians performing the scan
potential for methanators to experience short- on R-7105 methanator welds
term temperature runaway events when CO2 slip
from the CO2 removal loop becomes excessive.
The typical initiating event is the loss of solvent
flow (often due to a pump trip), and process gas
with high CO2 content flows through to the
methanator, causing a sudden increase of temper-
ature in its catalyst. For every 1% of CO2 con-
verted, the process gas temperature can increase
to about 60°C and process gas temperatures can
quickly rise to >540°C which is the design tem-
perature of the equipment. It is known in the in-
dustry that cumulative damage from repeat tem- Figure 6. R-7105, an example of PAUT outcome
perature excursions has resulted in HTHA and for different scanning modes with rounded iso-
hydrogen embrittlement cracking in C-0.5Mo lated indications in both base and weld metal
steel methanators on other ammonia plants. It's typical sign of inclusions. No signs of HTHA
important to note that the shell of exchanger E-
7114, immediately downstream of the methana-
tor, displayed evidence of significant HTHA Conclusions
damage in 2013.
HTHA is a complex mechanism for which a
Following the same approach of other items in- proper assessment is still challenging due to a
spected for HTHA, a detailed inspection was per- lack of recognized methods for damage evolution
formed using a combination of advanced NDT and criticality ranking. Because of different ap-
techniques (like TOFD and/or PAUT) comple- proaches applied in the past and a lack of empir-
mented by TFM/FMC. Also in this case, no sign ical data, C-0.5Mo material was believed to have
of HTHA found despite the equipment operating good resistance to hydrogen degradation, which
for more than fifty years above the Nelson curve. has been largely used. Unexpected failures oc-
curred in the industry declassed this material to
the carbon steel behaviour. Hence several equip- [6] Michael W. Hester, P.E., Daniel J. Benac,
ment is currently operating in unsafe condition P.E., Elevated Temperature Failure Mecha-
according to the new approach. nisms in Ammonia Plant Equipment – re-
The screening campaign performed at Yara Bra- ducing the Risk of, AIChE 2013
zilian site was fundamental to identify the assets [7] Inspectioneering, November 2022, Asset
where the risk of HTHA was high and therefore Intelligence Report – A primer on High-
optimize an inspection plan both for short-term Temperature Hydrogen Attack
actions and long-term strategic decisions (e.g. re- [8] Daniel J. Benac, P.E., Sean Berg, Werner
placement). Ploumen, Rob Gommans, Hydrogen Dam-
Advanced UT techniques recently developed age Mechanisms Affecting Assets in the
have been applied to maximize the detection ca- Ammonia & Fertilizer Industry, AIChE
pability, and thanks to this effort, an internal pro- 2022
cedure for HTHA inspection has been developed, [9] API Recommended Practice 941. Steels for
and it will be applied to all Yara sites. Hydrogen Service at Elevated Temperatures
Results of the inspection on the most critical as- and Pressures in Petroleum Refineries and
sets pointed out that HTHA was not present, alt- Petrochemical Plants. Eighth Edition 2016.
hough the high susceptibility level was according [10] Dave Dewees, P.E., Gerrit Buchheim, P.E.,
to API-941. This result proved that some credit Jeremy Staats, P.E., Charles Becht V, P.E.,
can still be given to C-0.5Mo steel. Despite the Practical HTHA Experience and Time-
good inspection results performed in the last TA, Based Nelson Curves for Improved Equip-
a continuous monitoring program has been estab- ment Life Management, Inspectioneering
lished to re-inspect the most critical assets and Journal 2020
identify the possible evolution of the HTHA deg- [11] API Recommended Practice 581. Risk-
radation. Based Inspection Technology. Second Edi-
tion 2008.
References [12] API Recommended Practice 581. Risk-
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Miguel Nugent, Joseph Bednarz, "Fleet- and Carbon 0.50% Mo Materials, Inspec-
Wide HTHA Risk Assessment Using Latest tioneering Journal 2015
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Kowalski, Phillip E. Prueter P.E, "Fitness- tioneering journal 2015
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[5] Phillip E. Prueter P.E., Advances in High- ature Hidrogen Attack, 2022 (Draft)
Temperature Hydrogen Attack (HTHA) In-
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