Failure of 321 stainless steel heater

tube in heavy crude oil

 Content

1. Background
2. Experimental details
3. Visual observations
4. Microhardness measurements
5. Analysis of deposits
6. Electrochemical reactivation test
7. Microscopic examination and analyses
8. Conclusion
 Background

A leak in a heater in a refinery unit handling heavy sour crude oil was
discovered. Eight convection tubes made of 321 SS had black oil/coke deposits
on their internal surfaces.
The leak was detected through gaps between tubes, but no leak was detected
from the radiant zone. The tubes were removed, and stud tubes were examined
using dye penetrant tests.
A circumferential crack was observed when the stud tube was lightly grounded
at the black colored area, raising the possibility of other cracks in the
remaining heater tubes.
The heavy crude charge has a gravity of 17 API, a total Sulphur content of
4.48% wt, and organic chloride content of 3 mg/kg.
 Experimental details

 A failure investigation was conducted on a cracked heater tube, involving visual examination of
surface and deposits, measurements of wall thickness and deposits, X-ray diffraction analysis of
inside deposits, pH measurement.
 Cross-sectional specimens were prepared for microhardness measurements and microscopic
examinations of the material. Microhardness measurements were conducted on a polished cross-
section using a diamond pyramid indenter at a load of 500 g. microscopic examinations were done
before and after etching using optical and scanning electron microscopy (SEM).
 The study evaluated the sensitization of tube material to intergranular corrosion using double loop
electrochemical potentiokinetic reactivation (EPR) techniques.
Visual observations

 The stud tube's circumferential cracking was found to be not linked to

bulging ( closure of the crack surfaces), suggesting stress corrosion by
polythionic acid or chloride, rather than creep, according to a visual
examination.
 The tube section was 89.0 cm long and 13.83 cm in diameter, covered with a
deposited black layer. The thickness varied significantly, with a minimum of
1.86 mm and a maximum of 4.61 mm. The maximum deposit thickness was
at the crack location. The tube also varied in wall thickness, with a
maximum reduction of about 1.04 mm, mainly at the crack location.
Microhardness
measurements

 The table shows that the average

microhardness values for a
polished cross-section cut from a
failed tube are slightly higher near
the internal and external surfaces.
 Analysis of deposits

 The XRD analysis revealed a

dense, hard black layer on the
internal tube surface, consisting
of carbon, iron sulphide, calcite,
sodium chloride, hematite, and
magnetite. The layer was
strongly adherent to the metal
surface and difficult to remove.
The water extract of the deposits
had an acidic pH of 4.8.
 Electrochemical reactivation test

 The EPR curves for service exposed and

solution annealed tube material reveal
passivity at -150 mV, with the solution
annealed specimen showing lower
passive current. Reactivation peaks were
formed for both specimens, but the
service exposed tube had a higher
reactivation peak current. The service
exposed sample had a higher Ir/Ia%
value (4.0) than the solution annealed
specimen (0.07), suggesting sensitization
during long-term service. The high Ir/Ia
% value suggests sensitization.
Microscopic examination and analyses
 Energy-dispersive spectroscopy

 The study conducted EDS analyses on the base metal, internal surface scale,
and precipitates inside a crack. The base metal exhibited peaks for iron,
chromium, nickel, and titanium. The internal surface scale showed strong Fe
and sulphur peaks. The precipitates inside the crack and branches had
similar spectra to the internal surface scale, but occasionally showed
prominent Fe, Cr, and S peaks. The Cr peak was found to be equal to Fe at
some spots and higher than Fe at others.
 These results would suggest that the internal surface scale and the
precipitates inside the crack and its branches are mostly iron sulphide.
However, the high Cr peak could be due to chromium sulphide precipitations.
conclusion

 The charge heater tube experienced chloride stress corrosion cracking,

which began in the sensitized internal surface layer as intergranular cracks.
 Salt precipitation in crude increased heater metal temperature, sensitizing
material and causing high temperature sulphuration, which obscured
chloride SCC cracks in some locations.
 The utilization of heavy crude oil rich in salts, sulphur, and H2S may have
been the catalytic factor. Thus, the problem is related to the type of feed
used.
References

 http://refhub.elsevier.com/S2213-2902(17)30023-8/sbref0005
 http://refhub.elsevier.com/S2213-2902(17)30023-8/sbref0015
 http://refhub.elsevier.com/S2213-2902(17)30023-8/sbref0040
 http://refhub.elsevier.com/S2213-2902(17)30023-8/sbref0060
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