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GENERAL STATEMENT ABOUT


MATERIALS OF CONSTRUCTION
(IN-45)

This document contains confidential proprietary material belonging to Axens which may only be made available
to personnel or organizations who have signed appropriate secrecy agreements.
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Introduction
The criteria for selecting equipment and piping metallurgy for this project are based on Axens
extensive experience with the field of refining units.
The primary objective in material selection is to prevent failure resulting from environment,
normal operation, and upset conditions. The material selection for this purpose is based on
mechanical design conditions.
The secondary objective is to provide adequate protection against the gradual material loss by
corrosion, to achieve the targeted design life. Equipment or piping normal operating conditions is
used for selecting the appropriate metallurgy for a targeted design life. Therefore, the selected
material for a given service should satisfy both the objectives of metallurgical stability, and
design life.

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to personnel or organizations who have signed appropriate secrecy agreements.
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1. EQUIPMENT DESIGN LIFE


Refer to Process Book Chapter 1.1.7. Equipment design basis: service life.

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2. CORROSION ALLOWANCE
Refer to Process Book Chapter 1.1.7. Equipment design basis: service life.

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3. MINIMUM DESIGN METAL TEMPERATURE (MDMT)


MDMT parameter shall be defined during material design in order to select materials capable of
resisting brittle fracture at the said Minimum Design Metal Temperature. This is purely a
mechanical design requirement (no corrosion concern).
Three different criteria may be used to establish the minimum design temperature:
- It may be based on consideration of the lowest expected operating temperature, the lowest
ambient temperature or an operational upset such as auto-refrigeration, or any kind of other
source of low temperature. A transient condition such as auto-refrigeration may be governing,
particularly if the restarting procedure does not permit warm-up before re-pressurizing,
- It may be established as the minimum exemption temperature allowed by the applicable
engineering code. For example, the ASME B31-3 piping code permits most carbon steel
piping with wall thickness of 12.7 mm or less to be exempt from impact testing if used at
temperature not colder than 29 deg. C,
- If the material of construction is impact tested, the Minimum Design Temperature is usually
taken to be the said impact test temperature (which is, for example, the case for HDT reactor).
The impact test conditions being defined as a function of the steel grade. Minimum Design
Metal Temperature for Low Alloyed Steel made reactors components is usually specified as
30 deg. C or 18 deg. C (depending on steel grade considered) unless process conditions
and/or owner requirement dictate a lower temperature.
As the same manner, suitable measures shall be taken in respect of the water temperature during
the hydrostatic test to avoid any brittle fracture.

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4. TEMPER EMBRITTLEMENT
Low alloyed steel such as 2.25Cr 1Mo, 2.25Cr - 1Mo - V and 3Cr-1Mo-V are susceptible to
temper embrittlement when operated in the temperature range of typically 350 550 deg. C (i.e.
hydrotreaters or hydrocrackers).
Under such operating conditions, embrittlement phenomena may appear in connection with the
behavior of Cr-Mo steels after long term service exposure.
Affected material can show a considerable reduction in toughness properties at ambient
temperature, and special precautions need therefore to be taken to avoid brittle fracture,
especially during transient phases (start-ups and shut-downs) and hydraulic pressure tests.
This mainly applies to the components made from steel grade specified here above for such
equipment as the reactors, associated vessels and certain HP heat exchangers. It is stressed that
temper embrittlement effects are normally much more moderate for lower alloyed steels (e.g.
1.25Cr-0.5Mo).

4.1 RESTRICTIONS TO CHEMICAL COMPOSITION


Refer to Axens Standard Material Specifications IN-42.

4.2 INCREASE OF TRANSITION TEMPERATURE


In addition to the stringent restriction of the chemical composition, most users specify a sampled
step cooling of steels coupons issued from materials used for fabrication of shell and heads
susceptible to Temper Embrittlement. Step cooling treatment, imperatively performed after
PWHT, will simulate a fraction of the increase in the ductility-brittle transition that should occur
after long-term service.
For information only, a typical step cooling sequence could be:
Heat to 595 deg. C Hold for 1 hour, cool at 6 deg. C/h max. to 540 deg. C
Heat to 540 deg. C Hold for 15 hours, cool at 6 deg. C/h max. to 525 deg. C
Heat to 525 deg. C Hold for 24 hours, cool at 6 deg. C/h max. to 495 deg. C
Heat to 495 deg. C Hold for 60 hours, cool at 3 deg. C/h max. to 470 deg. C
Heat to 470 deg. C Hold for 100 hours, cool at 28 deg. C/h max. down to 315 deg. C
and then Air cooling
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This simulated isothermal embrittlement results in a certain increase (shift) of the materials
transition temperature. The increase in transition temperature (TT54) from its original value has
become an accepted tool for the determination of temper embrittlement susceptibility. In order to
characterise a material for temper embrittlement resistance, a relationship was developed using
the original or as fabricated TT54 and the increase in TT54 (delta TT54).
After step cooling heat treatment, for impact properties (Charpy-V at 1/4 T and 1/2T material
thickness) should meet the following requirements:
TT54 + 2.5 delta TT54 lower than or equal to 10 deg. C
Where :

TT54 :

the 54 Joule transition temperature

delta TT54 :

(TT54 [step cooled] - TT54 [original value])

The method generally used to avoid brittle fracture consists in maintaining pressure at a low
level until reactor vessel exceeds the Minimum Pressurizing Temperature (in that way, resulting
stresses are then reduced below a stress value which could lead to brittle fracture propagation).
This MPT takes into account the TT54 estimated for the embrittled conditions and a safety
margin which mainly takes into account the effect of hydrogen absorbed during operation (effect
depending on wall thickness, steel quality and process conditions, it is the vessel vendor
responsibility to guaranty the MPT values for the considered equipment).
Below the MPT, the pressure should be kept not exceeding 25% of the design pressure for
equipment built per ASME Code Section VIII, Div.2 (some owners may allow higher value for
equipment built per ASME Code Section VIII, Div.1 considering the higher safety factor on
allowable stress values in that case). Any way, the MPT criteria for HP Reactors should always
be given or approved by vessel vendor.

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5. STABILIZING HEAT TREATMENT


Austenitic stainless steel can become sensitized after prolonged exposure at elevated
temperatures in the range of 425 - 850 deg. C (800 1600 deg. F). This structural transformation
during long term service at elevated temperature is due to a precipitation of chromium carbides
(generally Cr23C6). In fact, this precipitation at the grain boundaries does not affect the
mechanical properties. On the other hand, it involves sensitizing to intergranular corrosion (refer
to Polythionic acids).
Although stabilized types of stainless steels (such as 321, 347 and 316Ti) have a much higher
resistance towards sensitization than the non-stabilized ones, literature indicates that their
resistance can be further improved by stabilizing heat treatment (around 900 deg. C) of the solid
SS individual components. This procedure encourages the formation of stable carbides, formed
either from Titanium for Types 321 and 316Ti or from Niobium/Columbium for Types 347,
without chromium depletion.
Therefore such stabilization heat treatment is recommended for the furnace tubes. In addition it
could even be decided to apply such heat treatment also for (the hottest parts of) the stainless
steel piping despite its operating temperature remains somewhat lower.
Note that no fissuring corrosion experiences have been reported to Axens when using overlaid
347 SS (refer to Polythionic Acid Attack here after).

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6. METALLURGY SELECTION GUIDE DESIGN


Some of the main corrosion concerns that may be encountered within the hydrocarbon
processing units are summarized and discussed by the following.

6.1 HIGH TEMPERATURE H2 ATTACK


In services containing hydrogen, materials are selected based on their resistance to high
temperature hydrogen attack. Hydrogen attack can occur at temperature above about 220 deg. C.
Dissolved hydrogen can react with iron carbides generating methane gas (CH4) which is trapped
into the metal. As the concentration of methane gas increases, increasing pressure begins to tear
the grain boundary, causing fissures and then cracks. Simultaneously, the loss of carbides lowers
the strength of the metal.
Material recommendation is based on the Nelson curves (refer to API RP 941: Steels for
Hydrogen Service at Elevated Temperatures and Pressures in Petroleum Refineries and
Petrochemical Plants) for hydrogen resistance. The material is selected based on the maximum
operating temperature, and hydrogen partial pressure, with appropriate allowance added to each
of the variables to account for various operating modes.
As the figures considered in API RP 941 are based largely upon empirical experience, safety
margin of 28 deg. C (50 deg. F) and 3.4 bar (50psi) below the relevant curves (respectively for
Maximum Operating Temperature and Maximum Operating Hydrogen Partial Pressure) are
typically used when selecting steels.
Notes:
- The (P, T) values for Nelson Curves application shall not be compared with the
Mechanical Design Pressure and Temperature which are used for mechanical
calculation.
- If the temperature and pressure fall on one of the curves, then the higher alloy shall be
used.
There is no credit taken for a corrosion resistant stainless steel cladding, since hydrogen can still
diffuse through the cladding. Where alloy cladding is used, the base metal shall consequently be
selected for H2 Service.

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6.2 HIGH TEMPERATURE H2 / H2S CORROSION


The choice of material for services containing H2S in hydrogen rich environment is based on the
acceptable corrosion rate, to obtain the desired equipment life. At temperatures higher than
200 deg. C, the corrosion rate is estimated as a function of temperature and H2S partial pressure
for the selected material. The corrosion rate curves for the various metallurgy is based on the
original NACE data (Couper & Gorman curves), and this is considered to provide a desirable
degree of conservatism in the design.

6.3 HIGH TEMPERATURE SULPHIDE CORROSION IN H2 FREE ENVIRONMENT


The corrosion rate for services containing organic sulphur at temperatures above 260 deg. C in
hydrogen free environments (considered to be with ppH2 lower than 50psia) is obtained from
curves based on the original NACE and API data.
The estimated corrosion rates may be obtained, by using the Mc Conomy curves, as a function of
normal operating temperature and total sulphur content.

6.4 NAPHTHENIC ACID CORROSION


Naphtenic acid is the collective name given to the organic acids contained in some crude oils.
The naphthenic acid content of the raw feed is generally expressed as neutralization number, as
determined by ASTM test methods D664 or D974.
It can cause corrosion at temperatures as low as 175 deg. C (350 deg. F). However, serious
corrosion, pitting and/or grooving type, usually does not occur until the temperature exceeds
230 deg. C (450 deg. F).
Type 316L or 317L SS (SS containing at least 2.5%wt. of molybdenum) should be used when
neutralization number exceeds 1.5 mg KOH/g oil for operating temperatures above 230 deg. C.
Type 317 being preferred for severe combinations of TAN (Total Acid Number), Temperature,
and velocity/turbulence, since the molybdenum content of this grade ranges from 3.0 to 4.0 wt.
Percent.
Carbon steel metallurgy is considered to be sufficient for equipment and piping for Total Acid
Number TAN lower than 1.5 mg KOH/g and temperatures below 230 deg. C. For all other
conditions Stainless Steel specification shall be considered.

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6.5 WET H2S CORROSION


Wet sour services are common in the hydrocarbon producing and processing industries. The
major concerns for such services are the various forms of hydrogen cracking produced by wet
hydrogen sulphide corrosion.
As a matter of fact, H2S dissociation in presence of free water leads to atomic hydrogen
formation (particularly in the cold part of the reaction section after the washing water injection in
the reactor effluent, H2S amine absorbers and strippers overhead equipment are concerned), and
can cause the following:
Sulphide Stress Corrosion Cracking (SSCC).
Hydrogen blistering, Hydrogen Induced Cracking (HIC), Stress Oriented Hydrogen
Induced Cracking (SOHIC).
The susceptibility of deterioration by the above mentioned risks has to be lowered by specifying
appropriated Carbon Steel metallurgy.

6.5.1

Definition of different forms of damage

Sulfide Stress Corrosion Cracking:


Hydrogen atoms affect resistance of the steel and result in what is generally termed as hydrogen
embrittlement. SSC is very dependent on the stress level of the steel. With the usual types of
steel used in refinery, cracking is observed in the weld or HAZ in the base metal adjacent to
welds. This is where high strength / low ductility microstructures may be present and can be
identified by high hardness.
This type of corrosion can appear very quickly and is not linked to the drum thickness. In order
to limit this risk, a Post Welded Heat Treatment will temper the microstructure and then will
reduce the residual stresses. This type of treatment is mandatory
Hydrogen Blistering:
In this type of phenomena, hydrogen atoms are collected at imperfections or non-homogeneities
in the microstructure. It occurs throughout the base material and typically does not occur in the
weld metal. The interface between the inclusion and the steel matrix acts as a site for the
hydrogen atoms to combine into hydrogen gas (H2). The hydrogen molecular gas is too large to
diffuse back through the steel and is trapped. As more hydrogen gas collects at the said interface,
it builds up the pressure and can cause yielding of the surrounding steel, which yielding creating
lamination-type internal cavities parallel to steel surface.
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Hydrogen Induced Cracking:


HIC is stepwise internal cracks that connect adjacent hydrogen blisters on different planes in the
metal. No externally applied stress is necessary for the formation of HIC. It is commonly found
in steels with high impurity level that have a high density of large planar inclusions, such as
MnS, and/or region of segregated impurity and alloying elements in the steel.

6.5.2

Definition of different types of associated specifications

Typical Applicable Documents:


Axens specification has been built from IFP R&D results, from Axens experience in the field of
sour refinery services but also from different applicable documents of which the main are the
followings:
Materials resistant to Sulfide Stress Cracking in Corrosive Petroleum Refining
Environments as per Nace Standard MR0103, latest edition.
Materials and Fabrication Practices for New Pressure Vessels Used in wet H2S Refinery
Service as per NACE International Publication 8X194
Methods and Control to Prevent In-Service Environmental Cracking of Carbon Steel
Weldments in Corrosive Petroleum Refining Environments as per NACE Standard
RP0472, latest edition
Material requirements for Sulfide Stress Corrosion Cracking Resistant Metallic Material
as per NACE Standard MR01-75, latest edition.

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Axens Standard Specification

Axens Standard Specification for Carbon steel in "H2S service" or Sour Service:
(Refer to Axens Standard Material Specification IN-43)
Axens uses to consider 2 (two) different kinds of dedicated specifications, depending on service
severity, in the aim of limiting the likelihood of SSCC and HIC as well.
These specifications, following Axens standard, are defined as follows:
Wet H2S Resistant Steels which mainly calls for hardness limitations into the steel
therefore acting on the SSC phenomenon itself. This specification is applicable for both
pressure vessels plates and piping parts also.
HIC Resistant Steels shall verify the Wet H2S resistant Steel specification
supplemented by some limitation on impurities content into the steel thus leading to ultraclean steels. This specification only applies on pressure vessel plates (rolled and welded
pipes shall be considered like pressure vessel parts.

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6.6 AMINE STRESS CORROSION CRACKING


Amine solutions can cause pitting and stress corrosion cracking in carbon steels.
Amine stress corrosion cracking can attack non-stress-relieved CS piping and equipment. Hence,
stress relieving (PWHT) is recommended for all the welds and the cold formed parts of CS
equipment and piping, regardless of operating temperature. API RP-945 (Avoiding
Environmental Cracking in Amine Units) and the guides from technical committee NACE T-816 would apply to these services for equipment and lines.
Killed carbon steel is usually considered as acceptable under amines operation when fluid
velocities are limited to a maximum of 0.9 m/s (3ft/s) for rich amine and of 2.1 m/s (7ft/s) for
lean amine.
On the other hand, it is recommended to specify type 316 stainless steel for turbulence and/or
flash zone and/or high fluid velocities.
Note that it is generally preferred to use stainless steel as cladding and not as solid form on
account of possible presence of chlorides, highly dangerous for SS, in the fluid.
The recommendations outlined for the wet H2S corrosion are applicable for the amine service as
well. In particular, HIC resistant steels should be used for amine H2S absorbers.

6.7 AMMONIUM BI-SULPHIDE CORROSION


Water injection upstream of the reactor effluent coolers is required to prevent plugging from
water-soluble ammonium bi-sulphide salts. The water injection rate should be adequate for
saturating the vapor phase, and to provide about 25 % excess water as liquid phase, at the coolers
inlet. The water injection rate should also be sufficient to reduce the salt content of the sour
water to less than 4 wt %.
Axens had specified Killed CS metallurgy for this service in several of our licensed units.
Based on Axens experience, Killed CS metallurgy is sufficient for this service if the sour water
salt content is maintained at less than 4 wt%, and the total fluid velocity is kept in the range of 3
to 6 m/s. Also, it is important to control the wash water quality as recommended by Axens,
especially the oxygen (less than 15 ppbw) and chloride (less than 50 ppmw) content to minimize
corrosion.
Where severe operating conditions would be anticipated, Alloy 825 might be considered as
offering good characteristics in term of corrosion resistance.

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6.8 POLYTHIONIC ACID ATTACK


Where austenitic stainless steels have been selected, chemically stabilized types (321 SS
and 347 SS) are required for processes in which the normal maximum sustained operating
temperature exceeds 425 deg. C, because of their higher resistance to intergranular corrosion and
stress corrosion cracking caused by polythionic acid attack. This kind of attack can occur,
especially during the shutdown periods as a result of sensitization during service.
As a matter of fact, once opened to the atmosphere, the association of iron sulphides produced
during operation and air/moisture leads to formation of polythionic acids H2SxO6. The resulting
acid corrosion leads to the formation of intergranular cracks, typical of polythionic SCC
corrosion (mainly into Heat Affected Zone).
It is therefore strongly recommended to passivate the unit before contacting the equipment with
atmosphere. The NACE Standard RP0170 should also be followed as a guideline to carry out the
soda ash washing of all the zones to be in contact with atmosphere after shut-down. This
procedure is recommended in all the cases, even in the case of stabilized SS use.
Based on Axens experience, 347 SS shows a better resistance to sensitization than 321 SS, and is
recommended for severe services.
However for maximum resistance to sensitization, types 321 and 347 SS should be subjected to a
stabilizing heat treatment.

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6.9 CHLORIDE ATTACK


Aqueous chlorides provide an excellent electrolytic environment for corrosion.
Austenitic stainless steels are well known for their susceptibility to failure by chloride stress
corrosion cracking (CSCC).
This phenomenon may appear under almost any set of circumstances relative to the following
critical variables:
- Temperature: CSCC is virtually unknown for neutral pH solutions at temperature below
60 deg. C (140 deg. F)
- Chloride concentration: In evaluating the risks for CSCC, consider concentration
mechanisms such as evaporation, which can increase low contents to dangerous levels. For this
reason, vapor-liquid interfaces and crevices such as socket welds are to be avoided. Even trace of
chloride into water is sufficient to induce stress corrosion cracking.
- Stress: Stresses are usually due to the residual tensile stress caused by welding or coldwork such as U-Bending heat exchanger tubes. Stress relieving heat treatment is also sometimes
used to reduce cold forming or welding-induced residual stresses in austenitic stainless steels.
In consequence of the difficulties to guaranty the environment state in presence of chloride,
CSCC resistant alloys should be specified where CSCC is anticipated.
Increase in molybdenum content enhances resistance of austenitic stainless steel to chloride
attack (317L > 316 > 304,321). Super austenitic stainless steel (904L), or duplex alloy stainless
steel, as alloy 2205 (22Cr-5.5Ni-3Mo-N / UNS S31803) or higher nickel alloys types such as
Alloy 400 and Alloy 825 which are significantly more resistant to CSCC than austenitic 18-8 SS
should also be considered.
Notes:
- Monel , which may be specified where resistance to hydrochloric acid is required (top
section of the crude tower for example), shall not be used when ammonia is injected for
corrosion control due to its high susceptibility to stress corrosion cracking
- Water used for flushing or during hydro-tests in presence of austenitic stainless steel
materials should typically have a chloride content of 30 ppm, not exceeding 50 ppm.

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6.10 CAUSTIC SODA


Carbon steel is the basic recommended material of construction for moderate temperatures and
concentrations.
Threshold of operating limits are usually determined by using existing NACE caustic soda
services curves which indicates preferred materials at various temperatures and concentrations.
PWHT is recommended for Carbon Steel welds in services above these thresholds to minimize
the risk of stress corrosion cracking.
Austenitic stainless steels may sometimes be specified up to 120 deg. C (beyond this temperature
threshold, these alloys can be susceptible to caustic stress corrosion cracking).
However, caustics being often contaminated with chlorides, and since there are other competitive
materials choices, selection of austenitic stainless steels for caustic service is usually avoided.
For high severity services, Nickel Alloys such as Monel will be preferred.
Anyway, it is highly recommended in caustic soda services to avoid at one and the same time
piping low points where caustic could become highly concentrated, and hot spots.
Note: Systems in which carbon steel could be in contact with caustic soda carryover during
upsets should be stress relieved/post weld heat treated. If not possible, this system should be
made of appropriated alloys as defined here above.

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