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IS 12573 (2010): Method for Macro Etch Test for Wrought

Aluminium and Aluminium Alloy Products [MTD 22:
Metallography and Heat Treatment]

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IS 12573 : 2010

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Indian Standard
METHOD FOR MACRO ETCH TEST FOR WROUGHT
ALUMINIUM AND ALUMINIUM ALLOY PRODUCTS
( First Revision )

ICS 77.120.10

BIS 2010

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
February 2010

Price Group 2

Metallography and Heat Treatment Sectional Committee, MTD 22

FOREWORD
This Indian Standard (First Revision) was adopted by the Bureau of Indian Standards, after the draft finalized
by the Metallography and Heat Treatment Sectional Committee had been approved by the Metallurgical
Engineering Division Council.
This standard was first published in 1988. The revision has been taken up in order to update the standard
in the light of experience gained in its usage and to align it with the latest practices being followed in this
field in the country.
In this revision following modifications have been done:
a) Scope has been modified;
b) Clauses on selection of sample and sampling plan have been modified; and
c) Clause on specimen preparation has been modified.
Macro etch test method is frequently used as an evaluating technique for revealing solidification structure
segregation, general distribution and size of inclusions, porosity, grain size, flow lines surface condition,
manufacturing defects and method of manufacture. It is done by etching a suitably prepared specimen and
examining it visually or at low magnification (not exceeding ten diametres). Macro etch test method provides
inspections of large area as opposed to micro etch test method.

IS 12573 : 2010

Indian Standard
METHOD FOR MACRO ETCH TEST FOR WROUGHT
ALUMINIUM AND ALUMINIUM ALLOY PRODUCTS
( First Revision )
1 SCOPE

2.3.1 Cast Billets

1.1 This standard describes the method for carrying

out macro etch testing of aluminum and aluminum
alloys and some of the widely accepted etching
solutions currently in use. The products covered by
this standard are cast billets, extruded, rolled and
drawn products, such as, bars, profiles, sheets, wires,
etc, and forgings

Discs should be cut from the ends covering entire

cross-section of billet.
2.3.2 Extrusions
Discs should be cut from the ends of the extruded
section covering the full cross-section.
2.3.3 Forgings

1.2 The macro etching technique reveals defects on

the surface etched by specific chemical and can be
classified as described in IS 15264 : 2002
Geometrical product specification (GPS) Surface
imperfections Terms, definitions and parameters.

Discs should be cut transverse to the long dimension

to reveal defects, such as, cracks, bursts, piping, etc.
For revealing flow lines, forging, should be cut
parallel to the long dimension. In complicated
forging, cutting should be done after careful study
of the anticipated flow line.

2 SELECTION OF SAMPLE

2.3.4 Sheets and Plates

2.1 Defects which are revealed in macro etch testing
may be introduced at various stages of
manufacturing. To avoid wasteful work on defective
material, sampling ought to be done at an early stage
of manufacture. However, the sample should not be
taken so early that further working can introduce
serious defects. If the part is to be sectioned,
selection of the cutting plane is determined by
directionality or fibering due to the working process,
by the suspected or known form of defects, and by
the general form or nature of the part, namely,
casting, forging, extrusion, etc.

For observing surface defects, a reasonably large

sample should be taken. Samples may be cut in small
pieces for convenience of handling. For observing
laminations, transverse section has to be prepared.
2.3.5 Tubes
Suitable drawn tube samples to be made for
checking defects along and across the drawing
direction.
3 SPECIMEN PREPARATION

2.2 While stages of examination shall depend on

agreement between the manufacturer and the
purchaser, it is commonly done at semi-finished and
finished stage and shall include the following:

f) Permissible quantum of defects preferably

portrayed photographically or schematically.

3.1 Specimen shall be extracted by sawing or any

other mechanical means suitable for the stock to be
examined. However, care should be taken to prevent
mechanical deformation/cold working during
cutting and to provide sufficient coolant to restrict
any structural change due to heating during cutting.
3.2 Machined surfaces mostly serve the purpose for
macro etching. However, machining with blunt tool
or at unfavourable speed and feed can distort the
surface and give misrepresentation of the grain
structure. The usual procedure is to take roughing cut
and finish cut. This shall provide smooth surface
finish reasonably free from cold work. A shaper or
milling machine should be preferred to a lathe,
which provides control of cutting speed on a flat
surface.

2.3 A few common methods of sampling wrought

aluminium and aluminum alloys are given as below.

3.3 Degree of surface finish to be obtained on the

specimen surface (to be examined) shall depend on

a) Stages of manufacture at which inspection

needs to be carried out;
b) Definition of batch and batch size;
c) Location and number of specimens per batch
to be examined;
d) Degree of surface preparation for macro
etching;
e) Etching solution and method; and

IS 12573 : 2010
the purpose of etching and on the severity of the
etchant. Most macro etch are aggressive enough to
bring out some details of macro structure on a rough
cut surface but the over-etching often obscures
important details In general, a smoother or highly
polished surface requires less etching to bring out
the same amount of gross details and reduces the
possibility of losing fine details.

Details of macro etchant and the method used are

furnished in Table 1.
4 VIEWING AID
Etched specimen shall be examined visually or at
low magnifications. The optimum viewing
conditions for etched surface are when the light is
oblique to the angle of viewing. Generally, high
intensity light source is not required but a low power
independent light source is essential.

3.4 For revealing fine details, a very smooth surface

finish is required. Specimen surface should be ground
by emery paper up to 0 grade to obtain a smooth
surface finish with suitable lubricant to avoid cold
working or heating.

5 INTERPRETATION OF RESULTS
Indications that may be commonly seen after macro
etching are given below:
a) Centre Defect Pipe, burst, segregation
porosity or looseness;

3.5 After surface preparation, the specimen shall be

cleaned with suitable solvent to eliminate the
possibility of producing uneven attack by the macro
etchant. Cleaned specimen should be macro etched
immediately. The acidic etch is more likely to
produce uneven etch than the caustic if the surface
is not precleaned. The caustic etch is an excellent
degreaser. Caustic etch also ensures a surface free
from smeared metal, when examining direct chill
(DC) cast billets for porosity. In case of delay in
macro etching, specimen should be stored suitably
to avoid any contamination with oil and grease.

b) Surface and Sub-surface Defect Seam,

lap, segregation, crack, coarse grain ring;
c) Miscellaneous
Defects Non-metallic
inclusions or dirt, extrusions defect;
d) Fibre pattern of forged components; and
e) Grain size, columnar grains, shell zone.
6 RECORDING OF RESULTS

3.6 Macro Etchant

The record shall contain full information on grade,
alloy composition, melt number, form, condition of
supply and location examined.

Macro etchant should be selected based on the

purpose of examination and the type of alloy grades.

Table 1 Macro Etchants

(Clause 3.6)
Sl
No.
(1)
i)

Etchant
(2)

Composition
(Parts by Volume)
(3)

Method of Etching

Alloy Types Applicable

(4)

(5)

Caustic etch

10 g sodium hydroxide
(NaOH) to 90 ml of water

Immerse specimen for

5-15 minutes in solution
heated to 50-70C, rinse
with water, dip in 50 percent
nitric acid (HNO3 ) solution
to rinse again with water and
dry

Commercially pure
aluminum and all
other alloys including
welding and brazing
joints made with this
alloy

ii)

Tuckers reagent

45 parts concentrated
hydrochloric acid (HCl)
15 parts concentrated
nitric acid (HNO3 )
15 parts hydrogen flouride
(HF) (48) percent)
25 parts water

Mix freshly, before use.

Immerse or swab specimen
for 10-15 s, rinse with warm
water and dry. If necessary
repeat as much as required
until the desired effect is
obtained

Commercially pure Al,

Al-Mg and Al-Mg-Si
alloys and many other
alloys

iii)

Hydroflouric acid

1 part HF (48 percent)

9 parts water

Requires fairly smooth,

surface. Immerse until the
desired effect is obtained.
Rinse with hot water and

Al-Si alloy

dry

IS 12573 : 2010
Table 1 (Concluded)
Sl
No.
(1)
iv)

Etchant
(2)
Poultons reagent

v)

vi)

Zeerleders reagent

Composition
(Parts by Volume)
(3)

Method of Etching

Alloy Types Applicable

(4)

(5)

12 parts HCI (conc)

5 parts HNO3 (conc)
1 part HF (48 percent)
1 part water

Etch by brief immersion

or by swabbing. Rinse in
cool water. Do not allow
etchant/specimen to heat
during etching. The solution
may be premixed and
stored for long use

Pure Al, Al-Mn, Al-Si

and Al-Mg-Si and
many other alloys

50 parts HCI (conc)

15 parts HNO3 (conc)
3 parts HF (48 percent)
5 parts FeCI3
(conc) solution

Mix freshly, before use.

Cool the solution to
10-15OC. Immerse specimen
for a few seconds, rinse in
cold water. Repeat until the
desired effect is obtained

High purity Al

10 g FeCl 3
100 ml distilled water
0.5 ml HF (40 percent)

Etch at room temperature by

immersing for few seconds

High purity Al

vii)

60 ml HCl
40 ml HNO (70 percent)

Immerse for few seconds

Al-Cu alloys
many other alloys

viii)

10 ml HCl
30 ml HNO3
(70 percent)
5g FeCI3
20 ml distilled water
20 ml HNO3
(70 percent)
20 ml HCl (38 percent)
5 ml HF (40 percent)

Mix freshly. Immerse for

few seconds in solution at
room temperature. Add
HCl last
Mix freshly. Immerse for
1-3 min

All types of
Al alloys

ix)

Kellers reagent

All types of
Al alloys, Al-Mn,
Al-Si, Al-Mg and
Al-Mg-Si

NOTES
1 Macro-etching should be carried out in containers which must be fairly resistant to the attack of etching reagents.
2 The prepared specimen should be put directly into the etching solution with surfaces to be examined either facing
or vertical to permit the gas generated to escape freely. The specimens being etched should not be too close to each
other or to the tank wall to avoid non-uniform etching. If specimens are too big to be etched by immersion, etching
should be done by swabbing.
3 If etching is required to be carried out above the room temperature, the etchant should first be heated to the required
temperature and then the specimen should be immersed in it.
4 The etching periods recommended in table are introduced only to guide. The time required to develop the desired
results may be determined by frequent examination of the specimen as etching proceeds. Actual etching time depends
on the factors which include method of manufacture, heat-treatment condition, alloy grade and surface preparation,
etc.

Bureau of Indian Standards

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Review of Indian Standards
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This Indian Standard has been developed from Doc No.: MTD 22 (4849).
Amendments Issued Since Publication
Amend No.

Date of Issue

Text Affected

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