ASTM A262

CorrosionTesting:
Overview and Importance
By: Aaron Christie
Corrosion Testing Department
 Introduction

• The latest specification ASTM A262-15 is titled as “Standard

Practices for Detecting Susceptibility to Intergranular Attack
in Austenitic Stainless Steels”.

• It is a common IGC testing method that can quickly screen

batches of material to determine corrosion susceptibility and
incorrect processing.

• It contains five unique IGC test practices.

Intergranular Corrosion / Intergranular
Attack
IGC / IGA
• Primary Cause : Sensitization

• Primary Source of Corrosion Resistance in Austenitic SS: Chromium

(12 % min.)

• Exposure at high temperatures (425 – 815 ºC) for long periods of

time causes the grain boundaries of a material to precipitate,
creating carbide deposits and causing the material to be
susceptible to intergranular attack.

• In supplying the chromium for the carbide precipitate, the

chromium content in the immediate vicinity of these carbides drops
below a critical limit, and therefore the material becomes subject to
Schematic of IGC (Sensitization) and GB
Precipitation
 The five intergranular corrosion testing methods
within ASTM A262 are:

• The Oxalic Acid Etch Test (Practice A)

• The Streicher Test (Practice B)
• The Huey Test (Practice C)
• The Strauss Test (Practice E)
• The Copper - Copper Sulfate – 50% Sulfuric Acid Test (Practice
F)
PRACTICE A—OXALIC ACID ETCH TEST FOR
CLASSIFICATION OF ETCH STRUCTURES OF
AUSTENITIC STAINLESS STEELS
• Sometimes, a short time is a prime requirement.

• The long boiling acid tests provided the motivation for introducing and
accepting this test for screening a large number of cast and wrought
austenitic SS specimens by classifying microstructures.

• These are obtained simply by making a polished surface anodic in 10 %

oxalic acid solution for 1.5 minutes with a current density of 1.0 A/cm 2. An
alternate etching solution is used for specimens containing molybdenum
(AISI 316, 316L, 317, 317L) in which ammonium persulfate is used as an
electrolyte in place of oxalic acid.

• This results in an “over etch” which facilitates interpretation by examining

the etched structures on a metallurgical microscope at 250x to 500x for
1. Step Structure 2. Dual Structure 3. Ditch Structure (Suspect)
(Acceptable) (Acceptable)

4. Isolated Ferrite Pools 5. Interdendritic Ditches

 PRACTICE B—FERRIC SULFATE–SULFURIC
ACID TEST FOR DETECTING SUSCEPTIBILITY
TO INTERGRANULAR ATTACK IN
AUSTENITIC STAINLESS STEELS
• The ferric sulfate-sulfuric acid test, often referred to as the
Streicher test or the ferric sulfate test, was originally described
by M. A. Streicher in 1958.
• It was the first test that wasn’t derived from a plant service
problem.
• A specimen representative of the material to be evaluated is
immersed in a boiling solution of ferric sulfate and sulfuric acid
for a specified time (120 h).
• Specimens should have a total surface area of about 5 – 20 cm . 2

• The mass of the specimen is recorded prior to and after the

testing and its total surface area calculated and the mass loss is
 Millimetre per month=7305 X W / A X t X d
- (1)
t = time of exposure,
h,
A = area, cm2,
W = weight loss, g,
and
d = density, g/cm3
for chromium-nickel steels, d = 7.9
g/cm3
for chromium-nickel-molybdenum
steels, d = 8.00 g/cm3

Millimetres per month × 0.04 = inches per

month
Millimetres per month × 0.47 = inches per
year
Millimetres per month × 12 = millimetres
per year
Millimetres per month × 472 = mils per
year
Millimetres per month × 1000 × density/3
Apparatus for Ferric Sulfate – Sulfuric Acid = milligrams per square
Test decimetre per day
 PRACTICE C—NITRIC ACID TEST FOR
DETECTING SUSCEPTIBILITY TO
INTERGRANULAR ATTACK IN
AUSTENITIC STAINLESS STEELS

• The boiling 65% nitric acid test, often referred to as the Huey Test,
was first described by W. R. Huey in 1930.
• It was the second simulated service test used at the Du Pont Co.
since 1927.
• Due to the presence of hexavalent chromium ions formed through
the oxidation of Cr+3 to Cr+6 by the boiling 65% nitric acid, the test
solution volume to specimen surface area ratio should be at least
20 ml/cm2 to avoid accelerated corrosion.
• 108 mL of reagent water per litre of reagent nitric acid is used as
the test solution.
• The standard
Flask test consists of
and Condenser for five boiling
Nitric periods of 48 h each
Acid Test
with a fresh test solution being used in each period.
• A cold finger type condenser as shown in the above figure is
used in this practice. The mass of the specimen is recorded
before the test and after every test period of 48 hours and its
total surface area calculated.
• The calculated corrosion rates for the individual periods in
chronological order, as well as the average for the five test
 PRACTICE E—COPPER-COPPER SULFATE–16 %
SULFURIC ACID TEST FOR DETECTING
SUSCEPTIBILITY TO INTERGRANULAR
ATTACK IN AUSTENITIC STAINLESS STEELS

• The first widely used test for detecting susceptibility to intergranular

corrosion was an early version of the boiling acidified copper sulfate test
commonly known as the Strauss Test. The apparatus used is same as that in
test practice B.
• The volume of acidified copper sulfate test solution used should be sufficient
to completely immerse the specimens and provide a minimum of 8 mL/cm 2 of
specimen surface area.
• The test specimen should be immersed in ambient test solution, which is
then brought to a boil and maintained boiling throughout the test period.
Begin timing the test period when the solution reaches the boiling point.
• The time of the test shall be a minimum of 15 h, unless a longer time is
agreed upon between the purchaser and the producer.
 A Bent Copper–Copper Sulfate–Sulfuric Acid Test Specimen
• Bend Test: The test specimen shall be bent through 180°
and over a diameter equal to the thickness of the specimen
being bent.
• Tubular products should be flattened in accordance with the
flattening test prescribed in Test Methods and Definitions
A370.
• The bent specimen shall be examined under low (5 to 20×)
magnification. The appearance of fissures or cracks indicates
the presence of intergranular attack.
Passing Test Specimen—View of the Failing Test Specimen Bent Area
Bent Area (20× Magnification) at 20× Magnification

Traces of Intergranular Fissures and “Orange-Peel” Surface. Bent Area

Failing Test Specimen – Q 21780 Fissures on the bent
surface
• When an evaluation is questionable, the presence or absence of
intergranular attack shall be determined by the metallographic
examination of the outer radius of a longitudinal section of the
bend specimen at a magnification of 100 to 250×.
PRACTICE F—COPPER-COPPER SULFATE–50%
SULFURIC ACID TEST FOR DETERMINING
SUSCEPTIBILITY TO INTERGRANULAR ATTACK
IN AUSTENITIC STAINLESS STEELS
• A specimen representative of the material to be evaluated is
immersed in a boiling solution of copper sulfate and sulfuric
acid for a specified time. A piece of copper is also immersed
in the solution. The resulting mass loss is converted to a
corrosion rate, which is compared to a specified maximum
value to determine whether the material has the resistance to
attack expected of the grade of material being tested.

• The copper–copper sulfate–sulfuric acid test detects

susceptibility to intergranular attack associated primarily with
chromium carbide precipitate in unstabilized cast austenitic
stainless steels and in certain wrought grades.
• The test apparatus used is same as in test practices B and E.
The test specimens are prepared, each having a total surface
area of 5 to 20 cm2 and are weighed before and after the test
and their total surface area calculated.

• Continue immersion of the specimen for 120 h.

• The corrosion rate should be reported as millimetres of

penetration per month calculated using equation 1.

• In all the test practices of this specification, subject the extra

low carbon and the stabilized grades to a sensitization heat
treatment at 675 ºC for 1 h prior to testing.
Designati Test Temperat Testing Applicabil Evaluation
on ure Time ity Method
Practice A Oxalic Acid Ambient 1.5 minutes Chromium Microscopic
Etch Screening Carbide Examination,
Test Sensitizati Classification of
on Only etch structure
Practice B Ferric Sulfate – Boiling 120 h Chromium Weight loss /
Sulfuric Acid solution Carbide Corrosion rate
Test
Practice C Nitric Acid Test Boiling 240 h Chromium Weight loss /
solution Carbide Corrosion rate
and Sigma
Phase
Practice E Copper Sulfate Boiling 15 h Chromium Examination of
– 16% Sulfuric solution carbide Fissures after
Acid Test bending
Practice F Copper Sulfate Boiling 120 h Chromium Weight loss /
– 50% Sulfuric solution Carbide in Corrosion rate
Acid Test CF3M and
CF8M
 Test Solution
ASTM A262 IGC - 100 g oxalic acid (H2C2O4·2H2O) crystals + 900 mL
A reagent water OR 100 g ammonium persulfate
((NH4)2S2O8) + 900 mL reagent water as per
requirement.
ASTM A262 IGC - 400 mL reagent water + 236 mL sulfuric acid + 25
B g ferric sulphate (Fe2(SO4)3·xH2O).
ASTM A262 IGC - 108 mL reagent water + 1 L Nitric acid HNO3.
C
ASTM A262 IGC - 100 g copper sulfate (CuSO4·5H2O) + 700 mL
E distilled water + 100 mL sulfuric acid and dilute
to 1000 mL with distilled water + Copper shot or
grindings.
ASTM A262 IGC - 400 mL reagent water + 236 mL sulfuric acid + 72
F g copper sulfate (CuSO4·5H2O) + A piece of
copper metal about 3 by 20 by 40 mm. An
 Oxalic Acid
Etch Test
↓ ↓ ↓ ↓
304, 304 L, 304, 304L, 316, 304, 304L, CF3M, CF8M
CF3, CF8 316L, 317, 317L, 304H, 316,
CF3, CF8, CF3M, 316L, 316H,
CF8M 317, 317L, 321,
347
Nitric Acid Test Ferric Sulfate– Copper–Copper Copper–Copper
(240 h in boiling Sulfuric Acid Test Sulfate– Sulfuric Sulfate– 50 %
solution) (120 h in boiling Acid Test (15 h Sulfuric Acid Test
solution) in boiling Boiling Solution
solution)
Chromium carbide Chromium Chromium Chromium carbide
in: 304, 304L, CF-3, carbide in: 304, carbide in: 201, in: CF-3M, CF-8M
CF-8 Chromium 304L, 316, 316L, 202, 301, 304,
carbide and sigma 317, 317L, CF-3, 304L, 316, 316L,
phase in: 316, CF-8 Chromium 317, 317L, 321,
316L, 317, 317L, carbide and 347
321, 347, CF-3M, Application of Evaluation
sigma phase in: Tests for Detecting
CF8M End-grain in: Susceptibility
321, CF-3M, CF-to Intergranular Attack in
all grades 8M Austenitic Stainless Steels
Corrosion rates indicating susceptibility to IGA.
Corrosion rates higher than those listed indicate
grain dropping in unwelded specimens
 ASTM A262 Practice D: Nitric-
Hydrofluoric Acid Test (Obsolete)
• The nitric - hydrofluoric acid test as adopted for evaluation
purposes was first described by D. Warren in 1958.
• It consisted of two 2-hour periods in 10% HN03-3% HF
solution at 70°C (158°F) and thus requires less testing time
than any of the other methods. This method was developed
specifically to differentiate between precipitated carbides and
sub-microscopic sigma in the molybdenum bearing grades.
• HF attacks glassware, special apparatus made of PVC was
required. For this reason and the hazards involved it was not
being used widely and was removed from ASTM A262 in
1993.
 When to Evaluate for IGC?

• When 304 and 316 are used unknowingly in place of 304L and 316L.
• The final mill annealing and quenching are not effective.
• Incomplete stabilization of Ti or Nb bearing alloys because of their
inadequate amounts or ineffective stabilizing heat treatments.
• Heat is applied for unscheduled forming operations during fabrication or
installation.
• When the carbon content of extra low carbon SS exceeds the specified limit.
• In a very few cases when sensitized material is accepted knowingly to reduce
costs.
• The loss in production due to plant shutdowns can greatly exceed the costs
of new equipment. For such critical applications, it is essential that the alloys
be in their optimum metallurgical condition for resisting IGA and other forms
of corrosion associated with the precipitation at grain boundaries
 References

• Sensitization, IGA, SCC and Irradiation Effects on the

Corrosion of Fe-Cr-Ni Alloys. Paul C.S. Wu
• Corrosion Tests and Standards - Application and
Interpretation, Robert Baboian, Editor
• ASTM A262-15
• ASTM A262-02
Thank