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Standard Operating Procedure for Detecting Detrimental

Intermetallic Phase in Duplex Austenitic/Ferritic
Stainless Steels AS per ASTM A923

19/03/2019
IGTS-SOP-070

00 19/03/2019 11

FAISAL SHAIKH SEBASTIN

REV. DATE PAGES PREPARED REVIEWED APPROVED

 INDOGULF INSPECTION & TESTING SERVICES

Standard Operating Procedure for Detecting Intermetallic Phases

IGTS-SOP-070 Rev.0

Table of Contents

1 SCOPE 3

2 REFERENCES (Latest Editions) 3

3 SIGNIFICANCE AND USE. 4

4 APPRARATUS. 5

5 PROCEDURES. 5

6 METHOD A 5

7 METHOD B 9

8 METHOD C 10

9 REPORTING 11

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Standard Operating Procedure for Detecting Intermetallic Phases

IGTS-SOP-070 Rev.0

1 SCOPE

These test methods cover procedures for the determination of Intermetallic Phases in Duplex
Austenitic/Ferritic Stainless steels as per A923. Three procedures are described and identified as Methods
A, B and C.

Method A - Sodium Hydroxide Etch Test for Classification of Etch Structures of Duplex
Stainless Steels.
Method B - Charpy Impact Test for Classification of Structures of Duplex Stainless
Steels.
Method C - Ferric Chloride Corrosion Test for Classification of Structures of Duplex Stainless
Steels.

2 REFERENCES (Latest Editions)

ASTM Standard A923: Standard Test Methods for Detecting Detrimental Intermetallic Phase in
Duplex Austenitic/Ferritic Stainless Steels.
ASTM Standard A 370: Test methods and definitions for mechanical testing of steel products.
ASTM G1: Practice for Preparing, Cleaning, and Evaluating Corrosion Test Specimens
ASTM G48: Test Methods for Pitting and Crevice Corrosion Resistance of Stainless
Steels and Related Alloys by Use of Ferric Chloride Solution.
ASTM G 15: Terminology Relating to Corrosion and Corrosion Testing ASTM G 46:
Guide for Examination and Evaluation of Pitting Corrosion.

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Standard Operating Procedure for Detecting Intermetallic Phases

IGTS-SOP-070 Rev.0

3 SIGNIFICANCE AND USE

The following factors govern the application of these practices.

3.1 This test method may be used with other evaluation tests to provide a rapid method for identifying
those specimens that are free of detrimental intermetallic phases.

3.2 The Charpy impact test detects reductions in toughness from that of the optimal composition
and processing. Such reductions may be attributable to intermetallic phases or to other causes
not necessarily detectable by Test Method A. A Possibly Affected Structure is likely to be
associated with a loss of Charpy impact toughness ranging from slight to severe. An Affected
Structure is associated with

3.3 A severe loss of Charpy impact toughness. A Centerline Structure may or may not be detected
by a Charpy test, depending on the orientation of the Charpy specimen.
3.4 The ferric chloride corrosion test is a 24-h test in 10 % ferric chloride. It will detect a loss of
corrosion resistance associated with local depletion of chromium and molybdenum as a result of
the precipitation of chromium-rich and possibly molybdenum-rich phases, not limited to
intermetallic phases. An Affected Structure is associated with significant weight loss in the
corrosion test. A Possibly Affected Structure is likely to be associated with significant weight loss
in the corrosion test.

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Standard Operating Procedure for Detecting Intermetallic Phases

IGTS-SOP-070 Rev.0

 APPARATUS
The Following Apparatus are required for ASTM A923

1. Glassware, Glass Beakers 1000-mL

2. Source of Direct Current—Battery, generator, or rectifier capable of supplying approximately 15 V and
20 A.

3. Metallurgical Microscope 400X Magnification Min.

 PROCEDURES

 Method A: SODIUM HYDROXIDE ETCH TEST FOR CLASSIFICATION OF ETCHSTRUCTURES OF

DUPLEX STAINLESS STEELS
 Extract the specimen from the Sample in longitudinal or transverse section. These specimens
are mounted using epoxy resin and epoxy hardener.
 Grind and polish the specimens to a metallographic surface finish (0.05µm).
 Add 40g of reagent grade sodium hydroxide (NaOH) to 100ml of distilled water to prepare the
etching solution. Eye protection is necessary for this operation.
 A polished specimen should be etched at approximately 1 to 3V dc, for 5 to 60s.
 Note: It is to be noted that the proper etching period for the optimum results varied depending
upon SDSS alloy system. When etching is performed within the period of5 to 60s, the
intermetallic phases are revealed by yellow, then brown staining followed by staining of the
ferrite. Etching time also plays an important role. Insufficient etching will not reveal the
microstructure and over etching will result in a loss of contrast, which will cause difficulties in
distinguishing the phases.

 Following etching, the specimen should be rinsed thoroughly in hot water and in acetone or
alcohol, followed by air drying.

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Standard Operating Procedure for Detecting Intermetallic Phases

IGTS-SOP-070 Rev.0

 Observation – Examine the etched surface under a metallurgical microscope at 400x or 500x
magnification.

 Classification of Etched Structures – The etched microstructures are classified into the following
types:

 Unaffected Structure (Figure 1a &1b) – The sample has been etched and the microstructure
is without the revelation of any intermetallic phase. The austenite-ferrite boundaries are
smooth.
 Possibly Affected Structure (Figure 2a &2b) – The sample has been etched and isolated
indications of possible intermetallic phase are noted. The austenite/ferrite boundaries show

a fine waviness.
 Affected Structure (Figure 3a &3b) – The indication of an intermetallic phase is readily
revealed upon etching.
 Centerline Structure (Figure 4) – The intermetallic phase is observed as a continuous or
semi-continuous phase in the mid-thickness region of the sample, with or without the
affected structure outside of the mid-thickness region, indicative of segregation. (This
structure is only applicable to wrought materials).

FIG. 1 Unaffected Structure in S31803: (a) Longitudinal Section

And (b) Transverse Section (500×)

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Standard Operating Procedure for Detecting Intermetallic Phases

IGTS-SOP-070 Rev.0

Figure 01a 500X Figure 01b 500X

FIG. 2 Possibly Affected Structure in S31803: (a) Longitudinal

Section and (b) Transverse Section (500×)


Figure 01a 500X Figure 01b 500X



FIG. 3 Affected Structures in 8a S31803: (a) Longitudinal Section
and (b) Transverse Section (500× Magnification)

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Standard Operating Procedure for Detecting Intermetallic Phases

IGTS-SOP-070 Rev.0


Figure 01a 500X Figure 01b 500X


FIG. 4 S31803: Longitudinal Section (500× Magnification Before
Reproduction)

Figure 01 500X

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Standard Operating Procedure for Detecting Intermetallic Phases

IGTS-SOP-070 Rev.0

 Test Method B: CHARPY IMPACT TEST FORCLASSIFICATION OF STRUCTURES OFDUPLEX

STAINLESS STEELS.

 Charpy Sample Extraction

Charpy samples are extracted from the materials submitted for test. The samples should be extracted
remote from the edges (at least 3 mm away for the edges).

 Charpy Test Procedure

The Charpy Impact test should be conducted per ASTM A370, “Standard Methods and Definitions for
Mechanical Testing of Steel Products,” and ASTM E23. “Notched Bar Impact Testing of Metallic
Materials.” The test may be conducted at a temperature of -50°F because this temperature is
representative of the industry typical test temperature.

 Report the test temperature and the energy absorbed.

 ASTM A923 Test Method B Acceptance Criteria

 No acceptance criteria are stated in the ASTM A923 for Cast Super Duplex Stainless Steel.
However, from the Charpy Impact testing it was found that all solution annealed materials which
showed an unaffected structure had a toughness greater than 60ft-lbs at -50°F. Hence, this can be
taken as potentially an acceptance criterion.

 If a test specimen shows an impact value below the specified acceptance criteria, one retest of two
specimens is permitted. For acceptance, both retested specimens shall show a value at or above
the acceptance criteria.

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Standard Operating Procedure for Detecting Intermetallic Phases

IGTS-SOP-070 Rev.0

 TEST METHOD C—FERRIC CHLORIDE CORROSION TEST FOR CLASSIFICATION OF STRUCTURES

OF DUPLEX STAINLESS STEELS.

 Test Apparatus

The apparatus includes glass beaker of at least 1000ml, glass cradle to hold the Sample, water
bath Electronic Balance and Low Power Microscope.

 Procedure

 The specimens can be of various sizes and shapes.

 All the surfaces of the specimen should be ground to a uniform surface finish. Sharp edges and
corners should be rounded.

 The dimensions of the test specimens and the total exposed surface area should be calculated.

 The specimen should be weighed to the nearest 0.001g or better.

 The test solution is prepared by dissolving 100g of ferric chloride, FeCl3.6H2O, in 900ml of
distilled water (approximately 6% FeCl3 by weight). The solution is filtered into the glass beaker
using a filter paper or a glass wool to remove insoluble particles.

 The pH of the test solution should be adjusted to approximately 1.3 prior to the beginning of the
test by the addition of HCl or NaOH, as required.

 Place the specimen in the glass cradle and suspend the cradle from the stop cock into the test
solution.

 These beakers are kept in a water bath (Figure 8) at a temperature of 40°C (107°F) for 24
hours.
 At the end of 24 hours the samples should be removed and rinsed with water, scrubbed with a
soft bristle to remove corrosion products, dipped in acetone or alcohol and dried in air.

 The specimens should be again weighed to 0.001g or better.

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Standard Operating Procedure for Detecting Intermetallic Phases

IGTS-SOP-070 Rev.0

 . ASTM A923 Test Method C Acceptance Criteria

 The corrosion rate should be calculated in accordance with the weight loss and total surface
area using the equation.

Corrosion rate = Weight loss/[(Specimen Area) x (Time)]

 The calculated corrosion rate should not exceed 10milligrams/decimeter/day (mdd).

 If the specimen shows a corrosion rate in excess of 10mdd, one retest on two new specimens
from the same product is permitted. No retest specimen should exhibit a corrosion rate in
excess of 10mdd.

 REPORTING

1. Field Number
2. Field Name and Description
3. Category Sets, Values or Units
4. Sample Description
5. Sample ID
6. Dimensions (sample Length , Width and Thick)
7. Solution Details
8. Equation Details
9. Initial Weight and Final Weight
10. Photography (If required)
11. Corrosion Rate

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