A Failure Analysis Investigation of Pitting in Type 316L Piping PDF

NACE CENTRAL AREA
CONFERENCE 2006
Wednesday, October 4
Waterside Corrosion Session
A Failure Analysis Investigation of

Pitting in Type 316L Piping
Bearing Seawater Used for Cooling
Presented by Paul Redmond
Southwest Research Institute
NACE Central Area Conference 2006
Acknowledgments
This presentation summarized work
performed by Dr. Narasi Sridhar, Dr. Sean
Brassia, and Darrell Dunn.
Acknowledgments are also extended to
Melissa Hill, Harold Saldana, Fawn Daby,
and other members of the Materials
Applications staff.
OUTLINE
1. About the Southwest Research Insitute
2. Background of Type 316L SS installation
and startup issues
3. Timeline
4. Mitigating Issues
5. Startup
6. Analysis of pipe segments
OUTLINE (CONT.)
5. Biological Subcultures
6. Laboratory Simulations
7. Literature Review
8. Summary
9. Recommendations
10. References
Facts About
Southwest Research Institute
59 years of operation
501 (c)(3) nonprofit corporation
3,000 employees
1,200 acre facility in San Antonio, TX
>2 million ft2 of laboratories & offices
Over 700 patents
28 R&D 100 awards
SwRI Mission and Purpose

Founded in 1947 by
Thomas Baker Slick Jr.
Charter
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unbiased
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through science and
technology
Development &
transfer of technology
SwRI Today
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at SwRI
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engineering
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Mechanical and
Fluids Engineering
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Structural
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aerospace
structures
mechanical sciences
structural
systems
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design/analysis
testing/evaluation
flow measurement
rotating machinery
Background
Gas fired cogeneration plant in Puerto Rico.
A combination of Type 316L piping and
Fiberglass Reinforced Plastic (FRP) piping
at pier level.
High Density Polyethylene (HDPE) piping
installed in certain underground locations.
10
Background
Seawater pumps were made of Type 317L.
Cathodic protection of Type 317L.
Protection of pumps exterior only.
Condenser tubing and plate heat exchangers
composed of titanium.
11
Timeline for the Cooling System

Taken from the Plant Logs
System
Activity
Seawater Supply-Lines filled w/ Peerless water
-Hydrotest
-Lines filled w/ seawater
-In service
-Out of service
Seawater Make--Lines filled w/Peerless water
-Hydrotest
-Lines filled w/ seawater
-In service
-Out of service
-Biological growth evident
-Start system, found several pinhole leaks
March
April
May
June
July
August
September
October
November
Dec.
Jan,2000
?
15 20
10
7
12
3
21
?
15 20
10
7
11
21
23
Filled with Peerless potable water

Stagnant
Intermittent Flow
In service
12
Feb.
Time Line Details

Hydrotesting with well water.
During repeated hydrotests stagnant well water
was left in the system for up to 3 months.
No chlorination for the first 4 months.
Well water was gradually pushed out by seawater
and left stagnant for at least 1 week.
13
Time Line Details (cont.)

Intermittent trial operations; stagnant seawater
left in the system for up to 2 weeks.
Could not drain the system due to concerns of
collapsing FRP lines from vacuum.
Inspection of the system found an inadequate
number of drain points.
14
Mitigating Issues
Chlorination
The absence of chlorination in the system during
the first 4 months due to:
Environmental permit restrictions of
0.5 ppm max and 0.2 ppm avg daily.
Key chlorination pump was out of service.
Initial chlorination injection was only in the
cooling tower.
15
After Startup
Pitting leaks were detected in many Type 316L
piping locations within 2 weeks ( > 375 mils).
Leaks were predominantly in seawater supply
lines, but later in return lines as well.
Several patches/welds applied, but new leaks
continued to appear.
No leaks were observed in FRP and HDPE lines.
16
Photograph of a
Leaking Seawater Supply Pipe
The two bands indicate areas clamped with

patches on the outside diameter.
17
Analysis
A segment of failed Type 316 piping was sent
to Southwest Research Institute (SwRI ) for:
1. Root cause failure analysis;
2. Prognostications of future performance
of un-pitted sections (if possible).
18
Metallographic Analysis
No evidence of intrinsic material or
fabrication defects.
No evidence of intergranular precipitates,
secondary cracks, etc.
Shape and morphology of internal pitting
suggestive of MIC.
19
Overall View of a Pit from the

I.D. Surface and the Transverse
Cross-Section Across the Pit
I.D.
2 mm
1.3 mm
O.D.
20
Energy Dispersive Spectroscopy

Analysis of Solids Collected
at the Mouth of Pits
Na
Mg
8.0
3.6
Al
Si
11.0 24.9
Cl
Ca
Ti
Cr
Fe
Ni
0.3
1.7
16.5
2.0
13.3
0.7
1.3
16.1
0.7
High amounts of Si, Al (possibly from sand).

Cl, Na, Mg, and K (from seawater).
Ca (from barnacles?).
S (possibly from sulfate reducing bacteria [SRB]).
21
X-Ray Diffraction
X-ray diffraction of solids found indications
of NaCl and (gamma FeOOH).
22
Biological Subcultures
Subcultures were generated from water and
pipe deposit samples.
Barnacles within the deposits were
manually removed.
Subcultures were incubated in Marine Broth
2216 under aerobic conditions.
23
Biological Subculture Results

Marine Broth 2216 cultures tested positive
for slime.
Thick mucoid colonies were successfully
subculture on agar in aerobic conditions.
Possible third type of bacterium was
observed but unidentified.
24
Biological Subculture Results (cont.)

Deposits and water samples sub-cultured in Baars
Medium modified with 2.5% NaCl under anaerobic
conditions.
Pipe deposits tested positive for SRBs
Positive evidence of SRBs in slime.
No initial evidence of SRBs in water cultures
25
Laboratory Simulations
26
Pitting Testing of Type 316L in

Stagnant Seawater
Pipe freshly polished to 600 grit; strung between Teflon
fasteners.
Exposed to seawater collected at the plant in 200 ml flask
(roughly 20C) for 26 days.
Crevice corrosion was observed (up to 4 mils or 100 m).
No pitting was observed in non-crevice areas.
27
Open Circuit Potential Testing

Sealed water collected from three locations:
Inlet;
After Heat Exchanger; and
Return.
Machined Type 316L and Alloy C-22 cylindrical

specimens.
Solutions left open to ambient atmosphere; stirred to
mimic flow.
Open circuit potential was constantly monitored.
28
Measured Open-Circuit Potential of

Type 316L Stainless in Three Locations
o
316L SS and Alloy C-22 Open Circuit Potentials, 25 C

0.05
0.00
C-22 Fresh Seawater
Potential, VSCE
-0.05
316L Fresh Seawater
-0.10
316L Heat Exchanger Inlet
C-22 Heat Exchanger Inlet
-0.15
316L Return Water
-0.20
C-22 Return Water
-0.25
-0.30
10
15
20
25
30
35
40
Time, h
29
Observations
Open circuit potential of type of Type 316L noticeable
higher in fresh seawater.
At the inlet compared to after heat exchanger and return.
Hastalloy C-22 exhibited the same behavior over time.
Evolution of circuit potentials occurred over several days.
Can be related to establishments of thin biofilms and
changes in oxide films (Dickenson, et al., 1986).
30
Observations (cont.)
Protection potentials for Type 316L at 20C in seawater
s/b in the range of 0 mV vs. SCE.
Results suggest that after heat exchanger and return
piping would be less susceptible vs. inlet.
Such single point measurements are useful for
comparison but not for life predictions.
Protection potentials and open circuit potentials can have
a range of values in service.
31
Chlorine Measurements
1
0.9
Cl, tower
0.8
Cl, sea
Chlorine, ppm
0.7
0.6
0.5
0.4
0.3
0.2
0.1
/9
30
/9
9/
9/
28
/9
9/
26
/9
24
/9
9/
9
/9
9/
22
9/
20
/9
9
9/
18
/9
9/
16
/9
9
9/
14
/9
12
/9
9/
10
99
9/
8/
99
9/
6/
99
9/
9/
4/
99
2/
9/
/9
31
8/
8/
29
/9
Date
A sampling of chlorine analysis over a period of about

1 month, indicating relatively low residual chlorine levels.
32
Chlorine Measurements (cont.)

Noted at the plant during inspection that chlorine
monitors were not calibrated.
Unknown error in measurements.
Measurements made on seawater side and blowdown
to the helper cooling tower.
Can be inferred that chlorine levels were lower
seawater side vs. near the cooling tower.
33
Literature Review
Infant pits nucleate underneath breached oxide films.
Hydrolysis reactions:
Fe2+ + 2H2O
Cr3+ + 3H2O
Ni2+ + 2H2O
Fe(OH)2 + 2H+
Fe(OH)3 + 3H+
Ni(OH)2 + 2H+
Minimal mixing of internal/external solutions and

compromised passivity.
Crevice corrosion, oxygen depletion, lack of mixing
of pit solution with external solution.
34
Literature Review (cont.)

Natural seawater has been noted to be more
aggressive than artificial.
It has been shown that microbial organism can
increase the open circuit potential.
A process called ennoblement (Motoda, et al., 1990;
Audouard, et al., 1995).
35

SRB can also initiate localized attack.
Generation of sulfides can reduce the
protection potential encouraging localized
attack.
36

Kinetics of Localized Attack in Stagnant
Seawater Varied
Shallow Water depths <5 ft.; depths up to 230 mils
(5.8 mm) after 181 days exposure (Schumacher,
1979).
25.4 mils (0.635 mm) pit depths in seawater
cooled lube oil heat exchangers after 3 months
(Shalaby and Husain, 1992).
37

Localized Attack in Flowing Seawater
76 mils (1.9 mm) within 30 days, in flowing
seawater (0.06 m/s) at 14C (Asphahani, et al.,
1980).
20 mils in 100 days in 0.7 1.0 m/s (Shone et al
1988)
Under flowing conditions, pitting becomes less
susceptible.
However, crevice attack may still occur in flanged
joints, or under deposits or films (Lee and Tuthill,
1982; Shone, et al., 1988; Kain, 1998).
38

Temperature Effects in Seawater
Severity of attack in seawater attains a maximum at
30C.
Above 30C the open circuit potential drops due to
destabilization of biofilms (Steinsmo, et al., 1997;
Mullica et al 1989).
Does not diminish with increasing temperatures in
chlorinated seawater (1.0 ppm).
Residual chlorine sets up its own high redox potential
irrespective of biofilms (Steinsmo, et al., 1997)
39

Chlorination Effects in Seawater
Chlorination successful in mitigating macrofouling of
surfaces (Goodman, 1987).
Typical range is 0.2 ppm to 0.5 ppm for fresh water.
Levels as low as 0.1 ppm, sufficient to kill microbial slime
layers on surfaces; minimum open circuit potential in
flowing seawater (Shone, et al., 1988).
Residual chlorine can act as an oxidant and increasing
chances of localized attack.
Steinsmo, et al., 1997 measure open circuit potentials about 600 mv vs. SCE
in 22%Cr duplex stainless steel in a 1 ppm chlorinated solution.
40

Cathodic Protection in Seawater
If the opened circuit potential is depressed below the
protection potential localized attack will not continue.
Cathodic protection (galvanic coupling to iron/carbon
steel, zinc, and/or impressed current) can protect stainless
steels against localized attack in seawater (Lennox, et al.,
1983; Baptista and Pimenta, 1995; Valen, et al., 1999;
Sedriks, 1982).
Incidental protection by coupling carbon steel (Lee and
Tuthill, 1982).
41

Localized Attack in Fresh Water
Localized attack; rare but has been documented.
Kovach (1999) documented five cases of pitting in Type 316L piping
possibly due to high Mn and chlorination -> formation of
permanganeate.
Dickenson, et al., (1996) found evidence of biofilm induced
ennoblement of Type 316L in flowing freshwater.
Numerous examples of pitting of Type 316L with residual well water
being left in piping after hydrotesting (Kobrin [1986] as typical).
42
Summary
Through wall pitting in a short period of time (375 mils
in 6 weeks) was more severe than normally observed
even in stagnant water conditions.
Appeared to be almost instantaneous.
Such pitting rates were not observed in comparable
laboratory experiments.
Not attributable to metallurgical factors.
43
Summary (cont.)
Stagnant water conditions (well water)
were created during prolonged hydrotesting
(leak free joints could not be attained).
Proper draining was not attempted to avoid
collapsing fiber reinforced piping (FRP).
Early plant operations were intermittent
prolonging stagnant seawater conditions.
44
Summary (cont.)
Excess Chlorine levels (0.5 to 0.8 ppm) could cause
premature pitting; however:
Environmental restrictions on chlorine discharge;
Lack of calibrated monitoring; and
Early chlorine pump failure.
Actual chlorine levels likely seldom exceeded

0.2 ppm.
Absence of sufficient chlorination during hydrotesting/
intermittent operations, lead to the establishment of an
active microbial consortium of biofilm formers and
SRBs.
45
Summary (cont.)
SRBs can reduce the protective potential.
The presence of marine microorganisms can raise the
open circuit potential.
The two factors combine likely lead to the apparent
instantaneous local attack.
Once established even rapid flowing seawater would
be insufficient to stop localized attack.
Weld/patches over existing leaks can exacerbate
existing pitting leading to crevice corrosion.
46
Summary (cont.)
Type 317L seawater pumps were CP protected
on exteriors only.
Current flow spill over into interior components
could not be addressed.
Anode placement possibly problematic with
insufficient protection of interior components.
47
Recommendations
1. Most Type 316L segments should be replaced with
FRP.
2. Remaining Type 316L segments can be used to
provide:
a. Cathodic Protection (CP); and
b. Proper continuous through system chlorination (0.2 ppm)
is maintained.
3. Careful monitoring of the Type 317L pumps.

Reallocation of anodes S/B considered.
48
Recommendations (cont.)
4. Corrosion monitoring of remaining Type 316L
segments:
a. Potential measurements (reference electrodes); and
b. Measuring dissolved iron not useful due to dilution.
5. Increase the number of drain points in FRP.

6. Rewrite plant startup and operation procedures to
reflect lessons learned.
49
References
Asphahani, A.I., P.E. Manning, W.L. Silence, and F.G. Hodge. 1989. Highly
Alloyed Stainless Materials for Seawater Applications. Kokomo, IN: Haynes
International.
Auduard, J.P., C. Compere, N.J.E. Dowling, D. Feron, D. Festy, A. Mollica, T.
Rogne, V. Scotto, U. Steinsmo, C. Taxen, and D. Thierry, 1995. Effect of
marine biofilms on stainless steels results from a European exposure
program. Paper No. 3, 1995 International Conference on Microbially
Influenced Corrosion. Houston, TX: NACE International.
Baptista, W. and G. Pimenta. 1995. Cathodic protection against crevice
corrosion of high-alloy steel in seawater. Materials Performance. V.34. pp.
29-32.
Dickinson, W.H., Z. Lewandowski, and R.D. Greer, 1996. Evidence of surface
changes during ennoblement of type 316L stainless steel: dissolved oxidant
and capacitance measurements. Corrosion. V.52. pp. 910-920.
Kobrin, G., 1986. Reflections on microbially influenced corrosion of stainless
steels, Biologically Induced Corrosion, S.C. Dexter (ed.), Houston, TX: NACE
International. pp. 33-46.
50
References (Cont.)
Kovach, C.W., 1999. Types 304 and 316 stainless steels can experience
permanganate pitting in water-handling systems. Materials Performance.
V.38. pp. 70-75.
Lee, T.S. and A.H. Tuthill. 1982. Guidelines for the use of carbon steel to
mitigate crevice corrosion of stainless steel in seawater. Corrosion/82. Paper
No. 63. Houston, TX: NACE International.
Lennox, T.J., M.H. Peterson, and C.W. Billow. 1983. Corrosion resistance and
response to cathodic protection of advanced alloys in seawater. Materials
Performance. V.22. pp. 49-55.
Mollica, A., A. Travis, E. Traverso, G. Ventura, G. de Garolis, and R.
Dellepiane. 1989. Cathodic performance of stainless steels in natural seawater
as a function of microorganism settlement and temperature. Corrosion. V.45.
pp. 48-56.
Motoda, S., Y. Suzuki, T. Shinohara, and S. Tsujikawa. 1990. The effect of
marine fouling on the ennoblement of electrode potential for stainless steels.
Corrosion Science. V.31. pp. 515-520.
51
References (Cont.)
Schumacher, M. 1979. Seawater Corrosion Handbook. Park Ridge,

NJ: Noyes Data Corporation.
Sedriks, A.J. 1982. Corrosion resistance of austenitic Fe-Cr-Ni-Mo
alloys in marine environments. International Metals Reviews. V.27.
pp.321-353.
Shalaby, H.M. and A. Husain. 1992. Localized corrosion of electric
resistance welds of austenitic stainless steel in seawater. British
Corrosion Journal. V.27. pp. 45-49.
Shone, E.B., R.E. Malpas, and P. Gallagher. 1988. Stainless Steels As
Replacement Materials For Copper Alloys In Seawater Handling
Systems. Institute of Marine Engineers Presentation.
Steinsmo, U., T. Rogne, and J. Drugli. 1997. Aspects of testing and
selecting stainless steels for seawater applications. Corrosion. V.53.
pp. 955-964.
52
References (Cont.)
Strandmyr, O. and D. Hagerup, 1998. Field experience
with stainless steel materials in seawater systems,
Corrosion/98, Paper No. 707, Houston, TX, NACE
International.
Streicher, M.A. 1983. Analysis of crevice corrosion data
from two seawater exposure tests on stainless alloys.
Materials Performance. V.22. pp. 37-50.
Valen, S., R. Johnsen, P.O. Gartland, and J.M. Drugli.
1999. Seawater piping systems designed with AISI 316
and RCP anodes. Corrosion/99. Paper No. 321. Houston,
TX: NACE International.
53

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NACE CENTRAL AREA

A Failure Analysis Investigation of

SwRI Mission and Purpose

NACE Central Area Conference 2006

Operating Research Divisions

Chemistry & Chemical Engineering

NACE Central Area Conference 2006

Timeline for the Cooling System

Filled with Peerless potable water

NACE Central Area Conference 2006

Time Line Details

Time Line Details (cont.)

The two bands indicate areas clamped with

NACE Central Area Conference 2006

Overall View of a Pit from the

NACE Central Area Conference 2006

Energy Dispersive Spectroscopy

High amounts of Si, Al (possibly from sand).

NACE Central Area Conference 2006

Biological Subculture Results

Biological Subculture Results (cont.)

NACE Central Area Conference 2006

NACE Central Area Conference 2006

Pitting Testing of Type 316L in

Open Circuit Potential Testing

Machined Type 316L and Alloy C-22 cylindrical

Measured Open-Circuit Potential of

316L SS and Alloy C-22 Open Circuit Potentials, 25 C

316L Fresh Seawater

316L Heat Exchanger Inlet

C-22 Heat Exchanger Inlet

316L Return Water

C-22 Return Water

A sampling of chlorine analysis over a period of about

Chlorine Measurements (cont.)

Minimal mixing of internal/external solutions and

Literature Review (cont.)

Literature Review (cont.)

NACE Central Area Conference 2006

Literature Review (cont.)

NACE Central Area Conference 2006

Literature Review (cont.)

Literature Review (cont.)

Literature Review (cont.)

Literature Review (cont.)

Literature Review (cont.)

NACE Central Area Conference 2006

Actual chlorine levels likely seldom exceeded

3. Careful monitoring of the Type 317L pumps.

5. Increase the number of drain points in FRP.

NACE Central Area Conference 2006

Schumacher, M. 1979. Seawater Corrosion Handbook. Park Ridge,

NACE Central Area Conference 2006

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