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Standard ASTM Practices for Detecting Susceptibility to Intergranular Attack in Austenitic Stainless Steels

Welding Engineering.

Date: 14.04.2006
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Contents
What is corrosion?

Intergranular Corrosion
Types of ASTM Practices

Practice A
Practice B Practice C Practice E
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What is corrosion? Extractive metallurgy in reverse


Extraction
Corrosion

Fe2O3

Fe

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What is IGC?
Cr Depleted zone

Cr23C6

Grain Boundary

Grain

Sensitization Phenomena
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Types of ASTM Practices


Type Practice A Description
Oxalic acid etch test (rapid screening test) Ferric sulfate Sulfuric acid test Nitric acid test Copper Copper Sulfate 16% Sulfuric acid test Copper Copper Sulfate 50% Sulfuric acid test
Detecting susceptibility to intergranular attack in austenitic stainless steels

Used For
Classification of etch structures of austenitic stainless steels.

Practice B
Practice C Practice E

Practice F

Determining susceptibility to intergranular attack in austenitic stainless steels


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Practice A
Oxalic acid etch test Scope :

(1)

Used for acceptance of material but not for rejection of material. Used in connection with other evaluation tests. It is rapid screening test for identifying specimens that shows free of susceptibility to rapid intergranular attack in

other hot acid tests.


Specimens are Identified by means of their etch structures.
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Practice A
Applicable Materials :
All Austenitic Stainless Steels.
Note :

(2)

Extra low carbon grades and stabilized grades (e.g. 304L, 316L, 317L, 321 and 347) are tested after sensitizing heat treatments. sensitized at 675C for 1 Hr.

Applicable Tests :

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Practice A
Preparation of Test Specimens :
Cutting
Specimen size is 25 x 25 mm Sawing is preferred to shearing

(3)

Polishing

Cross sectional surfaces should be polished. Specimens containing welds should include base plate, weld HAZ and weld metal.

Polishing on successively finer emery papers.

Etching Solution 100 gm of reagent grade oxalic acid crystals (H2C2O4.2H2O) Stirring until all crystals are dissolved
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900mL of distilled water

Practice A
Classifications of Etch Structure :

(4)

Etched surface is examined on a metallurgical microscope at 250X to 500X


The etch structures are classified into the following types 1. Step Structure 2. Dual Structure 3. Ditch Structure 4. Isolated Ferrite

5. Interdendritic Ditches
6. End Grain Pitting I 7. End-Grain Pitting II
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Practice A
1. Step Structure 2. Dual Structure

(5)
3. Ditch Structure

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Practice A
4. Isolated Ferrite 5. Interdendritic Ditches

(6)
6. End Grain Pitting - I

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Practice A
7. End Grain Pitting - II

(7)

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Practice A
Advantages:
Rapid method. Use for all austenitic stainless steel.

(8)

Limitations:
It does not come on direct conclusion.

This test depends on other practices.

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Practice B
Scope : Only used for cast steel.

(1)

Ferric sulfate Sulfuric acid test

Only for predicting resistance to intergranular

corrosion.
Detects susceptibility to intergranular attack associated with the precipitation of Cr carbides not with sigma phase.
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Practice B
Applicable Materials :
304, 316, 317, 321
Note :

(2)

304L, 316L, 317L,

Extra low carbon grades and Stabilized grades (e.g. 304L, 316L, 317L and 321) are tested after sensitizing heat treatments. sensitized at 675C for 1 Hr.

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Practice B
Rapid Screening Test : (optional)

(3)

It may be used before going for ferric sulfate sulfuric acid test. This test is done in accordance with procedures described in PRACTICE A.

The use of etch structure evaluation in connection with this test is specified in table below.

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Practice B
Solution:
400ml Distilled water +

(4)

236ml reagent grade sulfuric acid(95 to 98% concentration) +


25gm of reagent grade ferric sulfate solution

Apparatus:

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Practice B
Sample size:

(5)

Specimen having surface area of 5 to 20cm recommended

Location of specimen:
Specimen containing weld should be cut with included 13mm base metal on either side.

Method:
Place specimen in glass candle. Immerse it in boiling solution. No appreciable change in acid level measured. Process continue for 120 Hr.
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Practice B
Calculation:
It is determining by weight loss of the specimen

(6)

Corrosion rate should be reported as millimeters of penetration per month


Millimeter per month = (7290 X W)/(A X t X d) Where: t : time of exposure, h, A: area per cm2,

W: weight loss, g , and


d : density, g / cm2 For Cr-Ni, d = 7.9 g / cm2 & for Cr-Ni-Mo steel< d = 8.0 g / cm3
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Practice B
Advantages:

(7)

Process accuracy is good because it is based on weight loss method.

Limitations:
It does not detect susceptibility associated with sigma phase in wrought Cr-Ni-Mo stainless ( e.g. 316, 316L, 317, 317L) It does not detect the susceptibility to end grain attack.

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Practice C
Nitric Acid Test Scope :

(1)

The test may conduct on as received material also. It is not necessarily measure the performance of material in other corrosive environment. It is also used to check the effectiveness of stabilizing elements.

This practice may be applied to wrought products, casting


& weld metal.
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Practice C
Applicable Materials : 304, 304L,

(2)

Note :

Extra low carbon grades and Stabilized grades (e.g. 304L, 316L, 317L and 321) are tested after sensitizing heat treatments. sensitized at 675C for 1 Hr.

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Practice C
Rapid Screening Test : (optional)
It may be used before going for nitric acid test.

(3)

This test is done in accordance with procedures described in PRACTICE A.

The use of etch structure evaluation in connection with this test is specified in table below.

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Practice C
Solution:

(4)

Reagent grade nitric acid added at the rate of 108ml per 1 liter of distilled water.

Apparatus:

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Practice C
Sample size:
Normally 100 Gm. Of specimen should be taken

(5)

Location of specimen:
Specimen containing weld should be cut with included 13mm base metal on either side.

Method:
Use sufficient quantity of nitric acid at least 20 ml/in2. Bring acid on hot plate and boiling throughout test period. After each test rinse the specimen with water then dried and weighed. Conduct 5 boiling period of 48 Hr For every test bring new solution.
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Practice C
Calculation:
It is determining by weight loss of the specimen

(6)

Corrosion rate should be reported as millimeters of penetration per month


Millimeter per month = (7290 X W)/(A X t X d) Where: t : time of exposure, h, A: area per cm2,

W: weight loss, g , and


d : density, g / cm2 For Cr-Ni, d = 7.9 g / cm2 & for Cr-Ni-Mo steel< d = 8.0 g / cm3
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Practice C
Advantages:

(7)

It detect susceptibility to intergranular attack associated primarily with Chromium Carbide Precipitate and with sigma like precipitates. It is used for as received material. It also detect susceptibility to IGC for stabilizing elements.

Limitations:
It does not detect susceptibility associated with sigma phase in wrought Cr-Ni-Mo stainless ( e.g. 316, 316L, 317, 317L)

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Practice E
Scope :

(1)

Copper-Copper Sulfate-Sulfuric acid test The test may conduct on as received material also.

It is also used to check the effectiveness of


stabilizing elements(e.g. Cb, Ti and so forth). It does not detect the susceptibility with sigma phase.
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Practice E
Applicable Materials :

(2)

201, 202, 301, 304, 304L, 304H, 316, 316L, 316H, 317, 317L, 321, 347

Note :

Extra low carbon grades and Stabilized grades (e.g. 304L, 316L, 317L and 321) are tested after sensitizing heat treatments. sensitized at 675C for 1 Hr.

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Practice E
Rapid Screening Test : (optional)
It is an optional test.

(3)

This test is done in accordance with procedures described in

PRACTICE A.
It may be used unless prohibited by purchaser. Testing period shall be minimum 15 Hr.

The use of etch structure evaluation in connection with this test is specified in table below.

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Practice E
Solution:

(4)

100gm Copper Sulfate(CuSo4.5H2O) + 700ml distilled water + add 100ml Sulfuric Acid(H2So4) and dilute to 1000ml with distilled water.

Copper addition:
Electrolytic grade copper shot or grinding may be used.
Sufficient quantity copper may used to cover full surface of the specimen Effective galvanic coupling may have importance.

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Practice E
Sample size:
Guideline for Specimen size given in table:

(5)

Location of specimen:
The size and area of the sample generally specified in agreement between purchaser and seller.
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Practice E
Method:

(6)

Solution should be sufficient to completely immerse the specimen Each specimen can be tested in same container It is ideal to have all specimens of same grade Solution maintain in boiling condition throughout test period. Time of test shall minimum 15 Hr unless longer time agreed upon purchaser and producer. Fresh solution not needed if test were run 48 to 72 Hr.2
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Practice E
Bend Test:

(7)

Taken out specimen from solution and then polish to remove scale

Specimen may be bent through 180 and over a dia. Equal to thickness of specimen bring bent.
Specimen having cold worked or low ductility, it is not practically possible to bend 180. That time determine the maximum angle without causing crack and bend another untested specimen of same configuration as specimen to be tested. Specimen generally bent holding in vise and bend with hammer

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Practice E
Evaluation:

(8)

Bent specimen examined under low magnification(5 to 20X) Acceptable microstructure shown in fig. 11 Appearance of fissures and cracks indicate presence of intergranular attack Non acceptable microstructure shown in fig. 12 When evaluation is questionable metallographic examination of bend specimen done.(See fig. 13) Metallographic examination at magnification of 100 to 250X

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Practice E
Acceptable microstructure:

(9)

Non acceptable microstructure:

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Practice E
Metallographic Microstructure

(10)

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Practice E
Advantages:

(11)

All wrought products and weld material of austenitic SS can be evaluated. We are able to measure corrosion by ductility test.

Limitations:
Only predict resistance to IGC but not other form of corrosion.

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