NACE Paper No.

MECCOCT18-12586

Determination of the Degradation of a AISI TP321 Stainless Steel Tube

Filipe Nascimento, Paula Ferreira Gorjão, Celso Araújo

Instituto de Soldadura e Qualidade
Taguspark Oeiras, Av. Prof. Dr. Cavaco Silva, nº 33, 2740-120
Porto Salvo
Portugal

ABSTRACT

The present paper describes the failure investigation steps taken to determine the root causes of a
stainless steel tube used in a hydro-treatment line which presented several cracks on its surface.

The visual analysis and non-destructive testing showed the presence of linear indication in the surface
of the stainless steel pipe. The chemical analysis confirmed that the material used was according to the
design specification. The metallographic analysis showed that the microstructure was typical of a AISI
TP 321 and presented several cracks originating from the outer surface. It was also observed that the
cracks had several ramifications and presented mostly transgranular propagation. The energy dispersive
X-ray spectroscopy (EDS) analysis showed the presence of chloride inside the crack.

The most probable root cause of the failure was stress corrosion cracking (SCC) on the basis of the
results of the tests carried out.

Key words: stress corrosion cracking; stainless steel; failure analysis; pipes; crack propagation

INTRODUCTION

The refining industries either petrochemical or chemical need to control the corrosion and degradation of
the materials used to avoid equipment failures with possible disastrous consequences. API 571 1
summarizes the damage mechanisms that can occur in the refining industry and identifies the critical
factors related to them. One of such mechanisms is stress corrosion cracking (SCC) that act in stressed
parts when in contact with some specific type of environment. Several case studies of this type of failure
can be found in the literature and have been characterized in order to understand ways to avoid them in
the future.

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Several authors 2–5 have investigated failures in 316 stainless steel components and found the
occurrence of stress corrosion cracking. Their studies focused on the determination of the conditions that
led to the occurrence of this phenomenon. The presence of chlorides and sulfides were found to be the
most common conditions.

Meresht et.al. 6 investigated the failure causes in a high-pressure gas pipeline steel in northern regions
of Iran, after almost 40 years since its installation. The author concluded that that the applied polyethylene
tape coating on the external surface of the pipeline became opened and disbonded in the corroded area
causing external surface of buried pipeline to be exposed to wet soil around it. The SCC phenomenon
occurred due to chemical interactions and the formation of carbonate/bicarbonate solution allied with the
presence of tensile stresses. The study shows that a failure in surface coatings can expose the material
to an environment that promotes the SCC phenomenon.

Shalaby et.al. 7 studied the cracking phenomenon that occurred in a 321 stainless steel charge heater
tube which failed in a refinery unit processing heavy crude oil. It was determined that the cracking was
chloride stress corrosion cracking catalyzed by sulfur species. The authors suggested the improvement
of the desalter operation with frequent decoking and scale removal operations.

Escobar et.al. 8 characterized the SCC corrosion mechanism that occurred in a bolt of a submersible
pumping system. The authors found that the SCC occurred in a high corrosive medium. Furthermore, the
bolt material was of carbon steel instead of the specified Ni-Cu alloy.

In order to better predict the behavior of this phenomenon, experiments have been carried out to
characterize the SCC phenomenon and to determine better ways to eliminate/reduce its effects in
susceptible materials to different environments. 9,10

This paper presents the results of the analysis conducted to determine the degradation causes detected
in AISI TP 321 stainless steel tube used in a hydro-treatment line.

EXPERIMENTAL PROCEDURE

The determination of the root causes that led to the pipe failure followed a methodology based on
information gathering and destructive tests for characterization of the failure phenomenon. The steps
applied in this methodology were:

• Background history – in this stage most of the background history of the equipment was gathered
together with some specifications of the working conditions at the time of the failure identification
and any unusual that might have occurred;
• Visual analysis – in this stage the part was inspected by optical means to identify any indication
that might be related to the failure. Non-destructive techniques were applied, to highlight any
prominent indications. In this component, liquid penetrant testing was performed to highlight the
linear indications in the surface of the material;
• Metallographic testing – samples were cut from the most affected zones of the part and a
reference zone. The samples were ground using SiC abrasive papers, the polishing stage was
performed using 6 and 1µm diamond polishing paste and respective polishing cloths. The
samples were etched using an oxalic acid solution. The microstructure was observed using a
optical microscope at 50, 100, 200 and 500x;
• Chemical analysis – the chemical analysis was performed by optical emission spectroscopy 1;

1
The chemical analysis was performed using an Hilger Analytical Polyvac 2000 equipment

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 • SEM and EDS analysis – the scanning electron microscopy (SEM)2 was used to better
characterize the phenomena observed in the metallographic prepared samples. The SEM
analysis was performed with an output voltage of 20kV. An EDS was used to perform the
identification of any aggressive agents that might be related to the observed phenomenon.

RESULTS

Background History

The hydrotreatment line was working at a temperature of 316ºC and at a pressure of 62,7kg/cm2. A 2’’
pipe of this production line was made of ASTM A312 Gr. TP 321 11 and had an 80mm thick HC insulation.
This pipe failed during service due to an apparent external degradation.

The degradation was observed near a fitting weld seam. Figure 1 shows the two sections of the tube
studied in this analysis.

50 mm

Figure 1: Failed sample analyzed

Visual Analysis

The outer surface of the received samples was slightly ground and it was visible the presence of several
superficial irregularities, such as pitting and linear indications. These irregularities were only visible in the
outer surface of the tube (Figure 2.a). The liquid penetrant testing has revealed the presence of linear
indications in the outer surface of the tube (Figure 2.b).

Metallographic analysis

Samples were metallographically prepared for analysis of the observed degradation: It was observed the
presence of cracks with several ramifications with origin in the outer surface (Figure 3). The cracking
observed had essentially a transgranular propagation (Figure 4).

2
The scanning electron microscopy was performed using a JEOL 6500F equipment

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 a) b)

Figure 2: a) Superficial irregularities in the slightly grounded surface of the received samples; b)
linear indications observed after liquid penetrant testing.

a) b)

Figure 3: a) Example of a sample showing the degradation originating in the outer surface; b)
micrograph detailing the crack and ramifications.

Figure 4: Micrograph showing a transgranular propagation.

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Chemical analysis

The measured chemical composition complied with the composition of an ASTM A312 Gr. TP 321 (Table
1). The deviations of the molybdenum (Mo) and copper (Cu) do not seem to affect the material properties.

Table 1: Composition of the received sample

C (%) Si (%) Mn (%) P (%) S (%) Cr (%) Ni (%) Ti (%) Mo (%) Cu (%)

Sample 0,06 0,41 1,64 0,021 <0,005 17,5 10,6 0,29 0,54 0,47

ASTM A312
Gr. TP 321 ≥5 x C
≤0,08 ≤1,00 ≤2,00 ≤0,045 ≤0,030 17-19 9-13 -- --
specified
Máx 0,7
composition

SEM and EDS Analysis

The metallographic prepared samples were analyzed by SEM to characterize the observed phenomenon.
This analysis allowed to identify the presence of chloride (Cl) and sulfur (S) inside the cracks, namely in
a crack ramification (Figure 5). The remaining elements identified belong to the material composition iron
(Fe), chromium (Cr), nickel (Ni), manganese (Mn) and silicon (Si)).

Figure 5: EDS analysis of the secondary crack showing the presence of chlorine (Cl) and sulfur
(S).

CONCLUSIONS

The degradation phenomenon that occurred in the tube is known as stress corrosion cracking (SCC).
The cracks observed in the surface propagated through the tube section. The morphology of the crack
with its ramification, observed in the cross section of the tube, is also typical of the stress corrosion
cracking phenomenon.

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The stress corrosion mechanism occurs with the combined action of a corrosive environment and
mechanical loads. Austenitic materials are also known to be susceptible to this phenomenon especially
when exposed to chloride environments at temperatures over 49oC. Higher exposure temperatures
usually hasten this phenomenon as well higher stresses. The stresses can be external (constraints,
superficial irregularities) or residual from the manufacturing or welding operations. In fact, the stress
corrosion cracking mechanism propagation and the time it takes to the failure of the equipment depends
on the balance of these conditions.

In this case study, the stress corrosion cracking is confirmed not only by the morphology of the typical
cracking, but also for the presence of chloride inside the cracks, namely the thinner and further away
from the surface. This indicates that the chlorides are the corrosive agent. The high temperature (316ºC)
and also the presence of the insulation contributes for the development of the degradation mechanism.

The presence of the chlorides in the surface of the material could have occurred in two instances:

• Poor cleaning of the surface before introducing the insulation, leaving free chlorides in the
interface between the pipe surface and insulation
• Damage to the insulation that allowed the introduction of chlorides in the interface between the
pipe surface and insulation

ACKNOWLEDGEMENTS

The authors acknowledge the funding by the Portuguese Foundation for Science and Technology, in the
scope of the project «UID/EMS/00712/2013».

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