Corrosion Tests and Standards

INTRODUCTION
Corrosion Fundamentals
Forms of Corrosion
CORROSION TEST & STANDARD
U if C i Uniform Corrosion
Salt Spray Test
Pitting/Cre ice Corrosion Pitting/Crevice Corrosion
Intergranular Corrosion
Stress Corrosion Cracking Stress Corrosion Cracking
Sour Corrosion
Miscellouneous Miscellouneous
2
3
()

Metallurgy in Reverse (Natural process!)

4
Cited from Fontana, M.G., Corrosion Engineering. 3rd ed. 1986, New York: McGraw-Hill.
5
a b
8
The leak caused by corrosion at this elbow started the fire
that destroyed this refinery
10
Alloying to resist corrosion (SS, cupronickel, etc.)
Metallic coatings (galvanizing) g (g g)
Organic coatings (paint, lining)
Electrochemical protection p
Cathodic protection
Anodic protection p
Corrosion inhibitors
Automotive cooling systems, cooling towers, boilers, etc. g y , g , ,
11
12
4
Uhlig, H.H. and R.W. Revie, Corrosion and Corrosion Control. 3rd ed. 1985, New York: John Wiley & Sons.
CC Technologies study March 2002
In 2000 about 3.1% of GDP spent on corrosion repair and p p
control
Total cost $276Billion!
Of industries analyzed, the cost was $137.9 Billion
Country Direct Cost Indirect Cost
USA 303.76 200 (approximately)
Japan 59.02
Former USSR 55.01
Germany 49 26 Germany 49.26
UK 8.51
Australia 7.32
Belgium 6.75
India 3.78
Poland 3.53
Canada 3.38
.....
.....
.....
Global 510.14 940 (approximately)
14
5
Bhaskaran, R., N. Palaniswamy, and N.S. Rengaswamy, Global Cost of CorrosionA Historical Review,
in Corrosion: Materials, Vol 13B, ASM Handbook. 2005, ASM International.
15
16
17
An 8" in. dia oil pipeline 225 miles long with 1 inch wall
thickness was installed with no corrosion protection system
With i t t ti l th di t ti it With appropriate protection namely cathodic protection, it
would have a thin wall thickness which would
S 3 700 t f t l ( th th illi d ll ) Save 3,700 tons of steel (worth more than one million dollar)
increase internal capacity of the pipeline by about 5%.
18
3Corrosion Doctors Website. Homepage: http://www.corrosion-doctors.org
19
Ensuring maximum life of new equipment
Preservation of existing equipment
Protecting or improving the quality of a product in order to maintain or improve g g y
a competitive position.
Avoiding costly interruptions of production.
Reducing or eliminating losses of valuable products by spillage or leaks.
Refitting of equipment withdrawn from service because of corrosion Refitting of equipment withdrawn from service because of corrosion.
Reducing hazards to life and property that might be associated with corrosion:
Explosions of pressure vessels or piping systems
release of poisonous or explosive gases or vapors release of poisonous or explosive gases or vapors
20
21
/,

Accelerated tests to demonstrate products durability
A t t t t h th t t i l t t d d Acceptance tests to show that a material meets standard
Monitoring tests to show changes in a system corrosivity
Research tests to determine mechanism of corrosion

Service life Service life

ranking
22
ASTM G48 Pitting and Crevice Corrosion Resistance
Ferric chloride (FeCl
3
), 6% solution (
3
),
72H at 22
o
C (room temperature)
Report pitting or crevice corrosion p p g
Simulates sea water attack of stainless steels
23
ASTM G69, Test of metallurgical condition of Al alloys
Measure corrosion potential, E, in salt solution
C i E Z d E Cu increases E, Zn reduces E
Heat treatment determines condition
Condition affects strength and corrosion tendencies Condition affects strength and corrosion tendencies
Solution: 1M NaCl + 2.7%H
2
O
2
, 22
o
C
Surface preparation: steel wool rub p p
1 Hour immersion
Measure potential every 5 minutes after 30 minutes against SCE
reference electrode reference electrode
Average result: -75010 mV for pure Al
Al foil is pure Al Al foil is pure Al
25
ASTM C876 Corrosion of steel rebar in concrete
Potential indicates when corrosion of steel is occurringg
Copper/copper sulfate reference cell
Chloride causes steel to corrode
Deicing salt usually reason for problem
Sea water also causes problems Sea water also causes problems
Potential > -0.20 V, rebar is not corroding Potential 0.20 V, rebar is not corroding
Potential <-0.35V, rebar is corroding
Potential in between then the rebar may be corroding Potential in between then the rebar may be corroding
27
28
Potential > -0.20 V, rebar is not corroding
Potential <-0.35V, rebar is corroding g
Potential in between then the rebar may be corroding
31
.

.

ASTM, NACE, etc.
32
Document that provides specific procedures or set of
requirements for a commercial product or process that q p p
attains a consensus of knowledgeable people.
Compliance with standards is voluntary unless mandated p y
by law.
International Society of Testing Materials 1880s
ASTM founded ~1898
NACE founded ~1948
ISO ~1960
34
ASTM (1904): Steel vs. Wrought iron in atmosphere
ASTM (1937): Salt spray test, B117
NACE th di t ti i NACE: cathodic protection issues
ASTM reorganization (1964) ASTM reorganization (1964)
Created Committee G-1 on Corrosion on Metals
Volume 03 02 Volume 03.02
NACE (~1960s)
Created Technical Practice Committee Created Technical Practice Committee
ISO (1978)
Created TC 156 on Corrosion on Metals (11 Working Groups) ( g p )
35
Corrosion is electrochemical
Potentiostats became available (1960s) ( )
Passive-active behavior of stainless steel revealed with
potentiostat. p
Issues with reliability and reproducibility.
36
430SS in 1.0N (0.5M) H
2
SO
4
aqueous solution.
Single lot of SS g
Carefully designed procedure
10mV/m from E
corr
.
corr
37
38



39


FIG.5- Potentiodynamic Polarization Plot for UNS S43000 Stainless Steel in 1 N Sulfuric
Acid at 30 C Showing Range of Data from Interlaboratory Program from ASTM G 5


40

FIG. 6- Potentiostatic Polarization Plot of UNS S43000 Stainless Steel in 1 N Sulfuric Acid at
30 C Showing Acceptable Data Range and Crevice Corrosion Affected Data Points from ASTM
G 5
First reference method
Results demonstrated reproducibility p y
Method widely used to qualify laboratories
Basis of many potentiodynamic studies y p y
Method upgraded and improved several times
41
Test method (TM)
ASTM G5
Standard practice (SP) aka RP p ( )
Specification p
ASTM G188
42
Industries dealing with corrosive situations
Engineers and designers g g
Governments specifying materials for projects
Academics teaching how to use materials in the real world g
43
44
Uniform Corrosion
Pitting/Crevice Corrosion g
Intergranular Corrosion
Stress Corrosion Crackingg
Sour Corrosion
Hydrogen Induced Cracking y g g
Sulfide Stress Corrosion
Miscellouneous
Hydrogen Induced Disbonding (HID)
Salt Spray Test, etc. p y ,
45
46


/

(alloying)
Atmospheric corrosion (rusting)
Corrosion in acid solutions
()
ASTM G31
Standard Practice for Laboratory Immersion Corrosion Testing of Metals
NACE TM0169

2000/(expected corrosion rate in mpy)

G1 Standard Practice for Preparing, Cleaning, and
Evaluating Corrosion Test Specimens1Procedure Evaluating Corrosion Test Specimens1Procedure
48
49

(instantaneous) ( )
CouponTime-corrosion rate data

/
ASTM
G59 Standard Test Method for Conducting Potentiodynamic
Polarization Resistance Measurements (LPR) ( )
G96 Standard Guide for On-Line Monitoring of Corrosion in
Plant Equipment (Electrical and Electrochemical
Methods)
50
R
p
= E/ i
app
= B/ i
corr
51
52
/

Humidity Testing y g
53

Fog density (condensation-collection rate) g y ( )
pH

Static
salt
,
Cyclic
54
ASTM B117, B368, G85
, ASTMspec. p

GM 4298/Salt Fogg
Mil Standard 810E, method 509.3
DIN 50018, ISO 9227 ,
Slat fog, acetic-acid, copper accelerated salt spray (CASS)
55
Static
salt
, 24h/day, 7 dyas/week
ASTM B117
Cyclic
,
: , RH, ,
SAE J 2334 DIN 50018/SO2 GM 9540P Ford APGE Honda SAE J-2334, DIN 50018/SO2, GM 9540P, Ford APGE, Honda
HES D6501 Sec. 3.18/3.37, CCT I, II, III, IV (Nissan), BMW CCT,
etc.
56
Designation Title
B 117 Test Method of Salt Spray (Fog) Testing
B 368 Method for Copper-Accelerated Acetic Acid Salt Spray (Fog) Testing (CASS Test)
B 735 Test Method for Porosity in Gold Coatings on Metal Substrates by Nitric Acid Vapor
B 799 Test Method for Porosity in Palladium Coatings by Sulfurous Acid/Sulfur Dioxide Vapor
D 2803 Guide for Testing Filiform Corrosion Resistance of Organic Coatings on Metal D 2803 Guide for Testing Filiform Corrosion Resistance of Organic Coatings on Metal
D 2933 Test Method for Corrosion Resistance of Coated Steel Specimens (Cyclic Method)
G 60 M th d f C d i C li H idit T t G 60 Method for Conducing Cyclic Humidity Tests
G 85 Practice for Modified Salt Spray (Fog) Testing
G 87 Practice for Conducting Moist SO
2
Tests
57
58
59
60
61
//

DIN 50021-SS
GM 4298
ISO 9227 ISO 9227


(comparative testing or ranking)
Quality audit function Quality audit function
passing or failing
outdoor.
62
NaCl
atomizingfog atmosphere
5% NaCl
NaCl reagent water(D1193)
NaCl
pH: 6.5~7.2
35 1 1 1 7
o
C 35+1.1 or -1.7
o
C
Fog: 1~2 ml/collector
24 to 5000hrs.
24 24
# of cyclesbuyerseller
Orient: 1215-30o angle (if not specified)
in-car , in car
Free-falling mist

.
Hot-dip galvanized steel
63
ISO salt spray test spec. (ISO 9227)
0.2 m
3
, 0.4m
3
,
Large Chamber (walk-in type & drive-in type)
64

: 0.25 ~ 4.5 m
3

(overcrowding)
65
Salt fog cycle Dry cycle
Controlled humidity cycle
66
Solution spray cycle
Immersion clycle
67
68
1987

SAE 1008 CS (76 x 127 x 0.8 mm)
48, 96, 168h , ,
user
69
(comparative testing or ranking)
Quality audit function y
passing or failing
70
ASTM G85 (acetic acid salt spray (fog) test)
/
, Ni-Cr, Cu-Ni-Cr, Cd , Ni Cr, Cu Ni Cr, Cd
consistency
5% NaCl + acetic acidpH(3.1-3.3)
35+1 1 or -1 7
o
C 35+1.1 or -1.7 C
16h 144 to 240h
ASTM B368 (CASS test)
(Ni Cr Cu Ni Cr Cd) (Ni-Cr, Cu-Ni-Cr, Cd)
Anodized, chromated, phoaphated Al
Automotive company
5% N Cl 1 C Cl 2H O (3 8L) ti id ( H 3 1 3 3) 5% NaCl + 1g CuCl
2
2H
2
O (3.8L) + acetic acid (pH 3.1-3.3)
49+1.1 or -1.7
o
C
6 to 720h
71
ASTM G1 Standard Practice for Preparing, Cleaning and
Evaluating Corrosion Test Specimens
ASTM G46 Guide for Examination and Evaluation of Pitting ASTM G46 Guide for Examination and Evaluation of Pitting
Corrosion
ASTM D609 Practice for Preparation of Cold-Rolled Steel
P l f T ti P i t V i h C i Panels for Testing Paint, Varnish, Conversion
Coatings and Related Coating Products
ASTM D1654 Standard Test Method for Evaluation of Painted ASTM D1654 Standard Test Method for Evaluation of Painted
or Coated Specimens Subjected to Corrosive
Environments
ASTM D610 Standard Practice for Evaluating Degree of ASTM D610 Standard Practice for Evaluating Degree of
Rusting on Painted Steel Surfaces
ASTM D714 Standard Test Method for Evaluating Degree of g g
Blistering of Paints
72



/
(salt)




(ml/80cm
2
collector)
% NaCl in water
cleaning(e.g.,
ASTM D609)
% NaCl in water
pH

edge

/


/
73
74
D714
D610
75
76
.0003/8um Zinc Nickel Black PS8955
.0003/8um Tin Zinc Clear GMW3200
.0003/8um Zinc Cobalt Black PS8955
.0002/5um Zinc Nickel Clear PS8955
.0003/8um Zinc Nickel Clear PS8955
.0003/8um Zinc Cobalt Black, Topcoat PS8955
.0002/5um Zinc Cobalt Clear PS8955
.0003/8um Zinc Cobalt Clear PS8955
.0003/8um Zinc Iron Black, Topcoat PS8955
.0002/5um Zinc Iron Clear PS8955
.0003/8um Zinc Nickel Clear, Topcoat PS8955
.0002/5um Zinc Cobalt Clear, Topcoat PS8955
.0003/8um Zinc Cobalt Clear, Tocoat PS8955
.0003/8um Zinc Iron Black PS8955
.0002/5um Zinc Iron Clear, Topcoat PS8955
.0003/8um Zinc Iron Clear, Topcoat PS8955
.0003/8um Zinc Nickel Black, Topcoat PS8955
0003/8um Zinc Clear GMW3044-N
.0003/8um Zinc Clear, Clearcoat, Wax FordS437
.0003/8um Zinc Clear, Clearcoat, Wax GMW3044-G
.0003/8um Zinc Yellow
.0005/12um Zinc Yellow
.0003/8um Zinc Iron Clear PS8955
.0002/5um Zinc Nickel Clear, Topcoat PS8955
, p
0003/8um Tin Zinc Clear PS8956
.0004/10um Tin Zinc Clear PS8956
.0005/12um Tin Zinc Clear PS8956
.0002/6um Tin Zinc Clear PS8956
.0003/8um Zinc Black
.0005/12um Zinc Black
.0005/12um Zinc Clear
.0003/8um Zinc Clear GMW3044 N
.0005/12um Zinc Clear, Clearcoat
.0003/8um Zinc Clear Clearcoat GMW3044-X
.0005/12um Zinc Clear Clearcoat Wax
.0003/8um Zinc Clear JS500
.0003/8um Zinc Clear JS600
.0003/8um Zinc Clear, Organic Topcoat S440
.0003/8um Tin Zinc Clear PS8956
0 50 100 150 200 250
Hours to White Corrosion
Zinc Alloy Finishes
RB211-524 G/H Stage 3 HPC Vanes (Rolls-Royce EAK alloy)
1 hr. 5% salt fog (ASTM B117-73)
2 h t 450C (842F) 2 hrs. at 450C (842F)
1/2 hr. cool
20 hrs in 100% relative humidity (ASTM D2247) 20 hrs. in 100% relative humidity (ASTM D2247)
5 cycles
Calla
Cor-Ban
Corrosion Inhibiting Calla
Aircraft
Appearance
Products
Corrosion Inhibiting
Compounds
Sur-Prep
Critical Surface Cleaners
& Treatments
Aero-Lube
Lubricants & Lubricating Lubricants & Lubricating
Compounds
82

SShalides (Cl
-
)
/ /

(: slag inclusion or surface defects.)
Pitting corrosion through the tube wall
83
Pitting corrosion of SS condenser tube
Specimens of various st ainless st eels aft er G 48 t est ing at 80C for 24 hours.
Standard Test Methods for Pitting and Crevice Corrosion
Resistance of Stainless Steels and Related Alloys by Use of Ferric
Chl id S l ti A F i hl id itti t t Chloride Solution, A: Ferric chloride pitting test
Shell ES/247 Revision 2, 2003
SS SS
6% FeCl
3
(, )
222 or 502C
72 hrs

/
84
Specimens of various stainless steels after G 48 testing at 80C for 24 hours.
Pit, , density
(a) Narrow & dip (b) Elliptical
( ) Wid d h ll (d) S b f
85
(c) Wide and shallow (d) Subsurface
(e) Undercutting
(f) Shapes determined by microstructural orientation
86
Specimens of various st ainless st eels aft er G 48 t est ing at 80C for 24 hours.
Ferric chloride Cl-
pit crevice p
.
SSpitting potential p g p

, chloride
87


(E ) (E
pit
)
Critical pitting potential (CPP)
scan repassivation
potential(E
rp
)
E
pit
PittingEpit=Erp
Pittinghysteresis loop.
E
rp
a. E>E
pit
: Pits nucleation occurs.
b. E
rp
<E<E
pit
: New pits can not be formed, but
the existing pits may propagate

the existing pits may propagate

c. E<E
rp
: the metal remains passive (or pits repassivate)
log i

log i
ASTM G61: Standard Test Method for Conducting Cyclic Potentiodynamic Polarization Measurements
for Localized Corrosion Susceptibility of Iron-, Nickel-, or Cobalt-Based Alloys
89
90
E
pit
= A log [Cl
-
] + B
SSCr, Mo, N content

PRE
%Cr + 3.3 (%Mo + 0.5%W) + 16~30 %N ( )
91
92
Critical pitting temperature
Pitting corrosion
CPTpitting corrosion
CPC (
o
C) = 2.5 %Cr + 7.6 %Mo + 31.9 %N 41.0
0 85
o
C 72h(C 24h/E) (5C) 0~85
o
C 72h(C, 24h/E) (5C)
93

1M NaCl
700mV
SCE
1C/min
100 A/cm
2
60
1. Cooling coil
2. Gas distributor
3 R f l t d 3. Reference electrode
4. Test specimen
5. Counter electrode
6 Temperature sensor 6. Temperature sensor
7. Immersion heater
8. Specimen holder with connection
9 Reflux cooler
94
9. Reflux cooler

1M NaCl
700mV
SCE
700mV
SCE
1C/min
100 A/cm
2
60
1. Cooling coil
2. Gas distributor
3 R f l t d 3. Reference electrode
4. Test specimen
5. Counter electrode
6 Temperature sensor 6. Temperature sensor
7. Immersion heater
8. Specimen holder with connection
9 Reflux cooler
95
9. Reflux cooler
96
E
pit
E
rp

log i
97
98
99
Simulating natural seawater
100
Supplementary technical requirements for the supply of components in 6%
Mo Austenitic, 22% Cr Duplex and 25% Cr Super Duplex Stainless Steel
Requires
Impact testing
Hardness testing
Microstructure examination and ferrite phase balance (not 6Mo)
Pitting corrosion testing (additionally, stress corrosion cracking for 25Cr if specified)
Base Metal:
ASTM G48 method A test required for each lot. Test temperature shall be 122F (50C) and the
exposure time 24 hours Corrosion test specimens shall be at same location as those for tension exposure time 24 hours. Corrosion test specimens shall be at same location as those for tension
tests. The test shall expose the external and internal surfaces in the as delivered condition
(including pickling) and a cross section surface in full wall thickness.
Weld
Corrosion test shall be performed on one sample from each of the 3 and 6 oclock welding Corrosion test shall be performed on one sample from each of the 3 and 6 o clock welding
locations in accordance with ASTM G48 method A. A sample including the root shall be taken
and be exposed to the solution. Test temperature shall be 104F (40C) and exposure time 24
hours.
No pitting at 20X magnification & weight loss shall be less than 4 0 g/m
2
No pitting at 20X magnification & weight loss shall be less than 4.0 g/m
2
.
101
Procurement Spec. for MWP
102
pitting corrosion,

Between flange joints,

Under deposits on the metal surface p
In welds with incomplete penetration
Pitting, Cl- g ,

PRE
103
Crevi ce corrosi on of Ti f l ange i n hot seawat er Crevi ce corrosi on of SS
Crevi ce corrosi on of socket wel d at gap f ormed bet ween t ype 304L pi pe
And t ype 316L val ve
Pitting corrosion(6% Ferric chloride)
crevice crevice

Rubber bend

Crevice area/exposed area

PTFE
Rubber bend
PTFE

106
ASTM G78: Standard Guide for Crevice Corrosion Testing of Iron-Base and Nickel-Base St
ainless Alloys in Seawater and Other Chloride-Containing Aqueous Environments
[0.5M FeCl
3
+ 0.05M NaCl] 30
304SS
109
ASTM G48D/F
MCACPT.

110
Specimens of various stainless steels after G 48 testing at 80C for 24 hours.
111
112
113
(grain),
(grain boundary)

2xxx AlClAl
2
Cu-depleted zone
114
SS(sensitization)
weld decay
C bid Cr carbide
SS
.
(HAZ)

weld decay.
SS650C
Cr carbide.
Production
Fabrication
Welding
Heat treatment Heat treatment
116
Fe-Cr alloy in boiling 50% H
2
SO
4
with Fe
2
(SO
4
)
3
IGCsusceptibility
1926CuSO
4
-H
2
SO
4
ASSIGC
4 2 4

()
: /
, (pH, ,
)

ASTM A262: 6 practices
117
PRACTICE TEST TEMP. TIME APPLICABILITY EVALUATION
A
Oxalic acid etch
Screening test
Ambient 1.5 m
Chromium carbide sensitization
Only (1.5A/cm
2
)
Microscopic: classification of etch
Structure (screening test)
B
Streicher
Fe
2
(SO
4
)
3
50% H
2
SO
4
Boiling 120 h Chromium carbide Weight loss corrosion rate
C
Huey
65% HNO
3
Boiling 240 h Chromium carbide and phase Weight loss corrosion rate
D
M d St
10% HNO
3
3% HF
70C 4 h
Chronium carbide in 316, 316 L,
317 d 317 L
Corrosion ratio compared to solution
l d i Mod. Strau 3% HF 317 and 317 L annealed specimen
E
6% CuSO
4
10% H SO Boiling 24 h Chromium carbide Examination for fissures after bending
Strau
10% H
2
SO
4
Metallic copper
Boiling 24 h Chromium carbide Examination for fissures after bending
CuSO
F
CuSO
4
50% H
2
SO
4
Metallic copper
Boiling 120 h
Chromium carbide in cast 316 an
d 316 L
Weight loss corrosion rate
118

1927~1930(Du Pont)
12% Cr 18% Cr
(CuSO
4
-H
2
SO
4
)


Boiled 65% HNO
3
solution
Fesh solution548h periods. p
(period)
Cr
119
Cr
.
baseline corrosion rate.
annealing g
.

Fitness-for-purpose
120
121
1930(Strau)

Huey test ()mild
Cu
(crack/fissure) ( )
122
Corrosion Potential
0.30~0.58V
SHE

~10
-1
A/cm
2
~10 A/cm
2
10
5

1 m
Cr Cr

,

, bending

123

Equivalent
DIN 50914
ASTM A262 practice E
ISO 3651/2 ISO 3651/2
bending
IGC
metallographic metallographic
examination
Cr-carbide , Sigma
124
125
Photograph showing a side view of an ASTM A262 method E
(Strauss) specimen after exposure and bending.
CRA-
, 65% nitric acid
: 240h : 240h
: 48h
+ +
screening test
Oxalic acid etch test
10% oxalic acid, 1.5, 1.0A/cm
2
10% oxalic acid, 1.5, 1.0A/cm
over-etching
(by Streicher)
St t t Step structure
Ditch structure
Dual structure
126
Step or Dual structure: passing
Ditch structure
Huey test(Practice C)
127
Step structure Ditch structure
Dual structure
128
Image Optical micrographs obtained in ASTM A262 Practice A test for 316
1958

240h(65% Nitric acid)120h 240h(65% Nitric acid)120h
Cr carbideIGC
Huey testMoinsensitive

[ferric sulfate+sulfuric acid] 5



IGC resistance IGC resistance
Plant service problemfitness-
for-service .
G28A
129
130
131
CORROSION
AUSTENITIC STEELS FERRITIC STEELS
SOLUTION
CORROSION
POTENTIAL
(E
SHE
)
AUSTENITIC STEELS FERRITIC STEELS
Cr-carbide Sigma
Carbides and Nitrides
Intermetallics
Fe-Cr-Mo(Ti)
Fe-Cr Fe-Cr-Mo
316 316L 317
65% HNO
3
1-1.25 yes
316, 316L, 317,
317L, 321
yes yes yes
F (SO ) N (321 ibl
yes
Fe
2
(SO
4
)
3
+
H
2
SO
4
0.85 yes
No (321 possible
exception)
yes yes
(not or in
unstabilised Fe
-Cr-Mo alloys)
C SO + CuSO
4
+
H
2
SO
4
0.6 yes no yes yes no
As above but with
metallic Cu
0.35 yes no yes yes no
metallic Cu
y y y
10% HNO
3
+
3% HF
0.15-0.55 yes no yes yes no
5% H
2
SO
4
-0.35 yes no no
yes
(not or in
unstabilized grades)
no
Exposure Time Criteria for passing
UNS No. Alloy Name Sensitizing Standards
Exposure Time,
h
Criteria for passing
Max. mm/month
S30400 Type 304 None Oxalic acid (A262A) 120 (a)
Ferric sulfate (A262B) - 0.1
S30403 Type 304L 1h at 675C A262A - (a)
Nitric acid (A262C) 240 0.05
S30908 Type 309S None A262C 240 0.025
S31600 Type 316 None A262A - (a)
A262B 120 0.1
S31603 Type 316L 1h at 675C A262A - (a)
A262B 120 0.1
S31700 Type 317 None A262A - (a)
A262B 120 0.1
S31703 Type 317L 1h at 675C A262A - (a)
A262B 120 0.1
S32100 Type 321 1h at 675C A262C 240 0.05
S34700 T 347 1h t 675C A262C 240 0 05 S34700 Type 347 1h at 675C A262C 240 0.05
N08835 Incoloy 825 1h at 675C A262C 240 0.075
N06690 Incoloy 690 1h at 540C A262C 240 0.025
133

(1978) ( )
boiling water(289
o
C, 0.2-8 ppm O
2
)304SS
SCC
(degree of sensitization; DOS),

[+KSCN(deactivator)]

134

[+KSCN(deactivator)] [ ( )]

Ecorr,
, cathodic
()

()DOS
: .
Pitting Pitting
135
Single loop (SL) EPR test g ( )
P : Degree of Sensitization
Q
P
a
: Degree of Sensitization
Q: Charge passed during test
GBA: Grain boundary area =A
s
[5.09544 10
-3
exp(0.34696X)
A
s
: specimen surface area
X: ASTM micrograin size number (ASTM E112)
136
GBA
Q
P
a
=

0.4<P
a
<2.0
Step/dual
(microstructure )
1. 0.01<P
a
<5.0
Ferric sulfate
EPR
2. 5<P
a
<20
Pa
3. P
a
>20
EPR,

137
SL-EPR

+300mV
(1980)
Pitting of non-grain g g
boundary
Surface-finish effect
-230mV
140m finish
SL-EPR1m

Scan rate: 6V/h

~ -400mV

I
r
: I
a
138
139
140
IGC TTC.
(according to ASTM G28, Streicher, ferric sulfate+sulfuric acid)
141
142
Cited from http://www.dandvik.com
Sensitization occurs in the range 550-850C, e.g. during
heat treatment or welding (HAZ). g ( )
Cr-carbide formation (or other types of precipitates) can
lead to Cr depletion and selective attack of a zone next to p
the grain boundaries or in the weld fusion line.
Materials with good IGC resistance g
ELC steels and Ti/Nb(Cb)-stabilized steels.
IGC testing mainly according to Strauss or Huey. g y g y
143
144
Mechanism
.

activation/passivation interaction p
Stress raisers (trench, pit)
Types yp
TGSCC
IGSCC IGSCC
145
TGSCC of SS after autoclave testing in 1000 ppm chloride solution at 250
o
C
146
S
t
r
e
s
s
SCC
No SCC
SCC
Strain
147


Materials
Environment
(Cl
-
, H
2
S, etc)

SCC
Composition
Heat Treatment
Microstructure
Surface Condition
Corrosion
Environment
Composition
Temperature
Electrode Potential
Flow rate
SCC
Acid chloride solution
Seawater
Fatigue
Corrosion-
Fatigue
SCC
Stress, Strain
Condensing steam from chloride waters
H
2
S + chloride
,
Service Stress
Fit-up Stress
Residual Stress
Strain Rate
Polythionic acid (sensitized material)
NaCl H
2
O
2
NaOH - H S NaOH - H
2
S
148
Statically loaded smooth specimen
U-bend
C-ring
bent beam
direct tension specimen
+Threshold stress(o
th
) or critical cracking stress:
- the max. stress below which SCC does not occur.
- determined from the plot of applied stress vs. time
149
to failure
ASTM G30
Standard Practice for Makin
g and Using U-Bend Stress-
Corrosion Test Specimens
150
ASTM G38
Standard Practice for Making and
U i C Ri St C i T Using C-Ring Stress Corrosion Tes
t Specimens

constant-strain(load)
151
ASTM G39
Standard practice for p
preparation and use of bent-
beam stress-corrosion test
i specimens
152
ASTM G49
Standard Practice for Preparation p
and Use of Direct Tension Stress-
Corrosion Test Specimens
153
Fracture mechanics testing

Constant loadcrack opening displacement , da/dt Constant loadcrack opening displacement , da/dt
Stress Intensity, K
ISCC
154
155
SCC(
)

SCC

(potential)
pH p


vs.
156
Cantilever beam specimen (PH13-8Mo) after SCC testing
ASTM G36
Standard Practice for
Evaluating Stress-Corrosion-
Cracking Resistance of
M t l d All i B ili Metals and Alloys in a Boiling
Magnesium Chloride Solution
42~45% MgCl 154 155
o
C 42~45% MgCl
2
, 154-155
o
C
Wrought, cast, welded ASS
Ni Ni
Chloride-SCC
157
158
ASTM G123
Standard Test Method for Evaluating Stress-Corrosion Cracking of g g
Stainless Alloys with Different Nickel Content in Boiling Acidified
Sodium Chloride Solution (25% NaCl)
U-bend specimen
ASTM G36
Standard Practice for Determining the Susceptibility of Stainless
Steels and Related Nickel-Chromium-Iron Alloys to Stress-
Corrosion Cracking in Polythionic Acids Corrosion Cracking in Polythionic Acids
As-received condition
After high-temperature service (480-815C) After high temperature service (480 815C)
159
250
s / 10 21 . 2
6
-
= c
200
304 stainless steels
50
o
C, 4 M NaCl
P
a
)
-100
0
E
pit
= -54 mV
-110 mV
-10 mV
100
150
S
t
r
e
s
s

(
M
P
Air
-300
-200
-310 mV
-210 mV
P
o
t
e
n
t
i
a
l
(
m
V
)
Erp =-250 mV
0
50
S
-10 mV
-210 mV
-230 mV -270 mV, -310 mV
No SCC SCC
10
-3
10
-2
10
-1
10
0
10
1
10
2
10
3
-500
-400
-510 mV
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
0
Strain
severe dissolution
160

smooth cross head speed(10
-5
- 10
-9
m/s) p ( )

SCC
[strain]/[Inertstrain]
161
162
ASTM G129
Standard Practice for Slow Strain Rate Testing to Evaluate the g
Susceptibility of Metallic Materials to Environmentally Assisted
Cracking
ISO 7539 7 ISO 7539-7
Corrosion of metals and alloys stress corrosion testing Part 7:
Sl St i R t T ti Slow Strain Rate Testing
Others
M difi d I d Modified Industry spec.
163
164
Oil and gas well (and/or refinery process)
Cl
-
, CO
2
, H
2
S ,
2
,
2
CO
2
CS,
chloride
Sour environment
Partial pressure of H
2
S > 0.05 psi.
Liquid water (>50ppm H
2
S, refinery, NACE 8X194)
More acidic, iron sulfide film formingg
Hydrogen embrittlement (e.g., HIC)
Sulfide stress cracking (SSC) g ( )
165
166

Hydrogen embrittlement Hydrogen embrittlement

Hydrogen blistering
Hydrogen attack Hydrogen attack
Hydride formation
167
source
Weldingg
Electroplating & pickling
2H
+
+ 2e
-
H
2
or 2H
2
O + 2e
-
H
2
+ 2OH
-
Contact with gaseous hydrogen
Corrosion (sulfide, cyanide)
168
tensile ductility
Hydrogen Induced Cracking (HIC)
Internal cracking of lower strength steels (e.g. pipeline steels) due g g ( g p p )
to high pressure hydrogen collecting at inclusions.

Hydrogen Cracking
Internal cracking of steels at higher temperatures due to reaction
of dissolved hydrogen with carbon to form methane
169
H
H
H
H
H
H
H
H
H
H
H
1 Hydrogen produced by t he cat hodic react ion 1 Hydrogen produced by t he cat hodic react ion
2 Hydrogen diffuses t o region of t ri-axial t ensile st ress
ahead of t he crack
3 Hydrogen causes britt le fracture
4 Crack blunt s by plast ic deformat ion as it runs out of 4 Crack blunt s by plast ic deformat ion as it runs out of
hydrogen
171
Cold cracking/HAZ cracking
source
M i t Moisture
Organic compounds
72 72
H
At 450F, 1 inch/hr
At 220F, 1 inch/48hr
, 2


PWHT (400-450F 1h) PWHT (400 450F, 1h)
172


5% NaCl + 0.5% acetic acid (pH 3.5) with H
2
S being continuously bubbled through th
e solution.
A synthetic seawater solution saturated with H
2
S
pH: 2.70.1
H
2
S 2300ppm
1h H S i 96h t ti 25 3C : 1h H
2
S purging + 96h testing, 253C
HIC
/
acceptance criteria
176
177
SP, CaHIC
178
Shell DEP
a.k.a., Sulfide Stress Corrosion Cracking (SSCC)
SulfideSCC
Sulfidepoisoner


Low pH
CO
2
CO
2
Stress
Amb. Temperature (-7 to 49C) Amb. Temperature ( 7 to 49C)
179
Material requirement: NACE MR0175/MR0103
, , , ,
NACE TM0177.
180
181
182

A: 5% NaCl + 0.5% Acetic acid, H
2
S saturated
A C D A , A, C, D A
B: 5% NaCl + 2.5% Acetic acid + 0.41% NaCH
3
COO, saturated with
hydrogen sulfide (for CS & low alloy steel)
C: 5mM Na NaCH COO + Cl
-
for MSS C: 5mM Na NaCH
3
COO + Cl
-
for MSS
sour /
24 3C 720h : 243C, 720h

Method AStandard Tensile Test Method A Standard Tensile Test
Method BStandard Bent-Beam Test
Method CStandard C-Ring Test
M th d D St d d D bl C til B (DCB) T t Method DStandard Double-Cantilever-Beam (DCB) Test
183
Method A
Time to failure
The chemical composition, heat treatment, mechanical properties
Method B Method B
Fail /no-fail data and pseudo stress values
Time to failure (optional)
Calculated critical stress (Sc) Calculated critical stress (Sc)
The chemical composition, heat treatment, mechanical properties
Method C
Fail / no-fail data from each stress level
Time to failure (if it is recorded)
The chemical composition, heat treatment, mechanical properties
Method D
All individual value of K for each set of specimens All individual value of K
ISCC
for each set of specimens
Arm displacement
The chemical composition, heat treatment, mechanical properties
184
185
Hydrogen induced cracking (HIC) tests
NACE TM0284-96
Sulfide stress corrosion cracking (SSCC) tests: Sulfide stress-corrosion cracking (SSCC) tests:
NACE TM0177-96, EFC 16
Constant load tensile Constant load tensile
Four-point bend
C-ring
Slow strain rate test Slow strain-rate test
Full Ring Tests: OTI 95 635
Autoclave testing of organic coatings: g g g
NACE TM0185-93
Testing of elastomeric materials:
C NACE TM0187-93, TM0296-96
186
UK HSE Offshore Technology Report, 1996
A Test Method to Determine the Susceptibility to Cracking p y g
of Linepipe Steels in Sour Service
TM0177/TM0284
Full section of pipe
, (level & direction)
F ll l Full scale

/ /
ISO 15156/ NACE MR0175option
187
188
189
190
Full ring testSSC ()
191
g ()
192
Refinery planthydroprocessing
equipment
SS SS clad or weld overlay steep
plate

Bond/fusion line
blister/delamination
High T, High pressure of hydrogen
, shutdown, start-up

ASTM G146HID &

ASTM G146
Standard Practice for
E l ti f Di b di f Evaluation of Disbonding of
Bimetallic Stainless Alloy/Steel
Plate for Use in High-Pressure,
High-Temperature Refinery
Hydrogen Service

bimetallic

hydrogen charging condition hydrogen charging condition

194

195
196
Accelerated tests to demonstrate products durability
Acceptance tests to show that a material meets standard
M it i t t t h h i t i it Monitoring tests to show changes in a system corrosivity
Research tests to determine mechanism of corrosion
Usually corrosion tests have many parameters
Corrosion tests often give results that are difficult to g
reproduce Standardization helps reproducibility
Industries dealing with corrosive situations
Engineers and designers g g
Governments specifying materials for projects
Academics teaching how to use materials in the real world g
M G F t C i E i i 3
rd
d M G Hill N Y k 1986 1. M.G. Fontana, Corrosion Engineering. 3
rd
ed., McGraw-Hill, New York, 1986.
2. Webpage of Department of Chemical Engineering, University of New Brunswick, http://www.unene.ca
3. L.L. Shreir, R.A. Jarman and C.T. Burstein, Corrosion: Metal/Environment Reactions, 3
rd
ed.,
Butterworth-Heinemann, Oxford, UK, 2000.
H H Uhli d R W R i C i d C i C l 3
d
d Wil & S N Y k 198 4. H.H. Uhlig and R.W. Revie, Corrosion and Corrosion Control. 3
rd
ed., Wiley & Sons, New York, 1985
5. R. Bhaskaran, N. Palaniswamy, and N.S. Rengaswamy, Global cost of corrosion - A historical review, in
Corrosion: Materials, Vol. 13B, ASM Handbook. ASM International., 2005
6. Corrosion Doctors Website, http://www.corrosion-doctors.org
7. www.rolledalloy.co.uk
8. Corrosion Tests and Standards, Application and Interpretation, 2
nd
ed., R. Baboian, ed., ASTM
International, PA, 2005.
9. Corrosion: Fundamentals, Testing, and Protection, Vol. 13A, ASM Handbook. ASM International., 2003 g
10. Webpage of Sumitomo Metal Technologies, Inc., http://www.smt-inc.co.jp
11. Webpage of JFE Techno-Research Corp., http://www.jfe-tec.co.jp
12. http://corrosion.kaist.ac.kr
13. http://www.sandvik.com p
14. D.R. Askeland, The Science and Engineering of Materials, 4
th
ed., Ch.22: Corrosion and Wear.
15. Product Finishing, Modern Plating Corporation, 2005.
16. R.G. Kelly, J.R. Scully, D.W. Shoesmith & R.G. Buchheit, Electrochemical Techniques in Corrosion Sc
ience and Engineering, Marcel Dekker, Inc., 2002. ience and Engineering, Marcel Dekker, Inc., 2002.
17. D.A. Jones, Principles and Prevention of Corrosion, Maxwell McMillian, New York, 1992.
18. Cf. T. Arai, M. Mayuzumi and J. Ohta, SCC Maps for Low-alloy Steels by SSRT Method, Corrison/98,
98140, NACE International, TX, 1998.
19 A test method to determine the susceptibility to cracking of linepipe steels in sour service OTI 95 635 19. A test method to determine the susceptibility to cracking of linepipe steels in sour service, OTI 95 635,
Health and Safety Exective, UK, 1996.