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Disclosure to Promote the Right To Information

Whereas the Parliament of India has set out to provide a practical regime of right to
information for citizens to secure access to information under the control of public authorities,
in order to promote transparency and accountability in the working of every public authority,
and whereas the attached publication of the Bureau of Indian Standards is of particular interest
to the public, particularly disadvantaged communities and those engaged in the pursuit of
education and knowledge, the attached public safety standard is made available to promote the
timely dissemination of this information in an accurate manner to the public.

“जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 को छोड न' 5 तरफ”

Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru
“The Right to Information, The Right to Live” “Step Out From the Old to the New”

IS 7739-5 (1976): Code of Practice for Preparation of

Metallographic Specimens, Part 5: Iron and steel and their
examination [MTD 22: Metallography and Heat Treatment]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”

है”
ह
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
 IS : 7739 ( Part V I- 1976
(Reaffirmed
( ReatTirnd 2003)
1FJ6I
Indian Standard
CODE OF PRACTICE FOR PREPARATION
OF METALLOGRAPHIC SPEClMENS

PART V IRON AND STEEL AND THEIR EXAMINATION

( Third Reprirlt AUGUST 1998 )

UDC 620’182’2 : 669’1

0 Copyright 1977

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAPAR MARC3
NEW DELHI 110002

Gr 7 June 1977
 IS : 7739 ( Part V ) - 1976 :

Indian Standard
CODE OF PRACTICE FOR PREPARATION
OF METALLOGRAPHIC SPECIMENS
PART v IRON AND STEEL AND THEIR EXAMlNATlON

Metallography and Heat-Treatment Sectional Committee, SMDC 27

Chairman Representing
SARI K. V. CHINNAPPA International Nickel (India) Pvt Ltd, Bombay

ManbCrS
SHRI B. C. BISWAS
DR S. S. BHATNAQAR Nationa1 Te$%%g%cutt~aboratory
Natlonal (CSIR),
Jamsbedpur
DR D. J. CHAKRAVARTY (Alternate )
-SARIJ.NAGESH BHATT Indian Telephone Industries Lrd, Bangalore
SHRI D. LAKSHMANNA ( Alternate )
DR S. K. CHATTERJEE Guest, Keen, Williams Ltd, Howrah
S~~ZIS. K. BASU ( Alternate )
SHRI DASARATHA The Visvesvaraya Iron and Steel Ltd, Bhadravati
(Karnataka)
SHRI B. HARIDA~ACHAR(Alternate )
SHRI D. M. DAVAR Premier Automobiles Ltd, Bombay
SHRI A. T. BORATE ( Alternate )
DEPUTY DIRECTOR ( MET )-III, Ministry of Railways
RDSO, LUCKNOW
CHEMIST AND METALLURWST,
RDSO, LUCKNOW(Altera& )
SHRI S. P. DEY Hindustan Motors Ltd, Uttarpara
SHRI M. B. Dvrr Indian Aluminium Co Ltd, Calcutta
SHRI A. K. GH&H ( AJternats )
SHRI A. K. GUHA Directorate General of Supplies & Disposals (Inspec-
tion Wing), New Delhi
SHRI K. M. TANEJA ( Alternate )
SHRI M. L. KATYAL Bajaj Auto Ltd, Pune
DR D. M. LAKHIANI Indian Iron & Steel Co Ltd, Burnpur
SHRI D. R. DASCUPTA (Atemate)
SHRI J. S. LOTAY Bharat Heavy Electricals Ltd. Hardwar
SHRI LAXAMAN MISHRA Directorate General of Technical Development, New
Delhi
SHRI V. D. SHARMA ( Afternuts )
DR G. MUKHERJEE Hindustan Steel Ltd, Ranchi
SHIU D. K. BA~CHI ( Alternak )
( Continuedon pugs 2 )

@ Copyright 1977
BUREAU OF INDIAN STANDARDS
This publication is protected under the bzdian Copyright Act ( XIV of 1957 ) and
reproduction in whole or in part by any means except with written permission of the
publisher shall be doomed to be an infringement of copyright under the said Act.
ISr7739(PartV)-1976

( Contimudfiom fiage 1)
Members R@festniing
DR T. MUKHERJEB Tata Iron & Steel Co, Jamshedpur
Sari A. PADMANAEAN Ashok Leyland Ltd, Madras
Da P. S. PATTIHAL Tata Engineering & Locomotive Co Ltd, Jamrhcdpur
SHRI J. C. KAPOOR( Rltmatr)
SARIV. RAMMWAMY Ministry ot Uefence (DGI)
SHRI B. N. RAY ( Altemata 1
DR V. RAMASWAMY Hindustan Steel Ltd, Ranchi
DR K. V. SUFIBARAO (Alternate )
SHRXA. R. RANADIVB Mahindra & Mahindra Ltd, Bombay
SHRI M. K. KHANLXE ( Alfumate )
SHRIR. Ii. G. Rau Mukand Iron & Steel Works Ltd, Bombay
REPRESSNTATIVE Special Steels Ltd, Bombay
TZPPRIWNTA-I~W~ Hindustan Aeronautics Ltd, Bangalore
REPRESBNTATIVB- Kamani Metals & Alloys Ltd, Boinbay
SHRI G. G. SAHA Ministry of Defcnce (R&D)
SWRIJ. N. AQRAWAL ( Al&no& )
SHRI K. L. TANDON Ministry of Dcfence (DGOF)
&RI C. R. RAMA RAO, Director General, IS1 (Ex-ojicio Membw)
Director ( Strut & Met )

SECT&l~
SHRI B. MCIKHBRJI
Deputy Director ( Met ), IS1

2
 IS: 7739(Part V)-1976

Indian Standard
CODE OF PRACTICE FOR PREPARATION
OF METALLOGRAPHIC SPECIMENS
PART V IRON AND STEEL AND THEIR EXAMINATION

0. FOREWORD
0.1 This Indian Standard was adopted by the Indian Standards Institu-
tion on 24 December 1976, after the draft finalized by the Metallography
and Heat-Treatment Sectional Committee had been approved by the
Structural and Metals Division Council.
0.2 T e primary object of metallographic examination is to reveal the
cons 2 tuents and the structure of metals and their alloys by means of the
microscope. Because of the diversity in available equipment, the wide
variety of problems encountered, and the personal element, this standard
gives for the guidance of the metallographer only those practices which
experience has shown are generally satisfactory. This part covers the
polishing, etching and examination of iron and steel. The other parts of
this code are as follows:
Part I General features
Part II Electrolytic polishing
Part III Aluminium and its alloys and their examination
Part IV Copper and its alloys and their examination
Part VI bead and its alloys and their examination
Part VII Magnesium and its alloys and their examination
Part VIII Nickel and its alloys and their examination
Part IX Gold, silver, platinum, palladium and their alloys and their
examination
Part X Tin and its alloys and their examination
Part XI Zinc and its alloys and their examination
0.3 In the preparation of this standard assistance has been derived from:
ASTM E3-62. Standard methods of preparation of metallogra-
phic specimens. American Society for Testing and Materials.
Metals Handbook 1948. American Society of Metals.

1. SCOPE
1.1 This standard ( Part V ) covers the polishing, etching and examination
‘of iron and steel.

3
ISr7739(PartV)-1976

1.2 FDr convenience, this standard is divided in two sections, namely:

a) Macroscopic examination-In which the study is made at low
magnification ( usually 10 X or less ).
b) Microscopic examination - In which the study is made at compara-
tively high magnification and resolution.
1.3 A metallographic examination shall frequently include both a macro-
scopic and microscopic examination. However, there are many occasions
on which either the macroscopic or microscopic study alone is sufficient
to supply the desired information.

SECTION I MACROSCOPIC EXAMINATION OF STEEL

2. GENERAL
2.1 Macro-examination is an inspection procedure for revealing certain
aspects of the quality and stfucture of a metal by subjecting it to the corrosive
action of an etchant and examining it visually or at low magfication.
This is usually done on steels and may be cla.ssified into two groups of study:
one, the study of the surface characteristics of the material, and the other the
study of physical and chemical nonhomogeneity of the material, for example,
porosity, cracks, seams, segregation, scabs, laps, piping, laminations, .etc,
or the absence of this condltmn, as revealed by sections of the material.
2.2 Other applications of macro-etching in the fabrications of metals, are the
study of flaw lines of weld structure, definition of weld penetration, dilution
of filler rnetal by base metals, entrapment of flux, porosity and cracks in weld
and heat-affected zones, etc. It is also used in the heat-treatment shop to
determine location of hard or soft spots, tong marks, quenching cracks,
case depth in shallow hardening steels, case depth in carburization of dies,
effectiveness of stop off coatings in carburization, etc. In the machine shop,
it may be used for the determination of grinding cracks in tools and dies.

3. SELECTION OF SAMPLE
3.1 A representative sample shall be selected with due consideration for the
purpose of the test. The sample should usually be of a full section of the
material and should be thick enough for easy handling and subsequent
preparation. Normally, transverse cross-sectional samples in the form of
flats discs at right angle to the axis shall be taken, and the cross-sectional
dimension should not exceed 300 mm X 300 mm.
3.1.1 If necessary, stipulation should be made in material specification
regarding identity of the sample, for example, cast number, ingot number,
relative position of the sample, etc, as agreed to between the supplier and
the purchaser.

4
 IS:7739(PartV)-1976

3.2 During sample selection, consideration should be given to the stage of

mechanical working at whidh the sample is selected. When macro-etching
is used as an inspection procedure, sampling ought to be done in an early
stage of manufacturing so that if the material is faulty, no further work ‘is
done, which may prove unnecessary and wasteful. However, cars should
also be taken not to select a sample so early that further working may
introduce serious defects. For steels sample shall be taken after ingot
breakdown and after most chances of bursts or flakes occurring have passed.
Billets or blooms going into small sizes are sampled after initial break-
down. Materials for forging billets or die blocks is sampled near finish size.
Sampling may be done systematically or on a random basis.

3.3 Samples may be cut from the whole by means of a saw, abrasive cut-off
wheels or any other convenient machining operation. Gas-cutting may be
used to cut samples from large sections, but the heat-affected zone of gas-cut
samples shall be removed by machining or abrasive wheel cutting prior to
etching. Suitable coolant shall be used to prevent overheating of specimens
during abrasive cutting.

4. PREPARATION OF SPECIMENS

4.0 The required surface finish for specimens for macro-etching vary from
saw-cut or machined surface to polished surfaces.

The degree of permissible surface roughness depends on the severity

of the etchant and the type of examination being made.

4.1 If the surface characteristics of a material are under study, it is rather

unusual to have any extensive preparation of the surface prior to macro-
scopic study. The surface is usually cleaned and degreased with carbon
tetrachloride so that the subsequent etchant shall attack the surface of the
material umformally. With a hot-dipped or electroplated coating present
on the surface of the material under study it is necessary to remove the coat-
ing metal to examine the underlying base metal. These protective metals
are usually stripped by chemical solution; extreme care should be’ exercised
so that the base metal is unattacked by the stripping solution.

4.2 In the study of materials for physical and chemical nonhomogeneity,

it is usually necessary to section the material through a plane which should
reveal the area of suspected heterogeneity. The degree of surface prepara-
tion to be given to the sample is largely dependent upon the type of etch to be
used in the examination and the details to be revealed in the sample under
test. In general, the quality of the surface finish must be higher as the
severity of the etchant in chemical attack decreases. Conversely, with an
intensive etch, the quality of the surface preparation may be lowered.
Rough grinding on an abrasive wheel or belt or with coarse emery paper
is usually sufficient, and even machined surfaces may sometimes prcve

5
I&7759(-Pad’)-1976

ratisfactory for deep etching specimens for macroscopic examination.

When 1~ severe etching, such as with ammopium persulphate, is to follow,
or ia sulphur printing, a somewhat smoother finish may be desirable.

5. ETCHING FOR MACROSCOPIC RXAMINATION

5.1 Table 1 gives the etching reagents which are commonly recommended
for the macroscopic examination of iron and steel.
5.1.1 Table 2 &es the recommended methods of macroetching for
specific purposes.
5.2 In deep etching, hot solutions of hydrochloric acid, sulphuric acid,
or mixtures of these acids, are generally used. Deep etching in hot, strong
solutions of these ac& requires considerable care in the time of exposure of
the material being etched, since the attack is frequently very rapid. It is
very easy to over-etch materials and thus mask the interpretation that would
be gained from an accurately etched specimen. Likewise, the intensity of
a’ local defect should be given careful conslderatiou if viewed after deep
etching, since the chemical attack will exaggerate the original condition
tremendously. A deep etch is frequently used to disclose physical and
chemical nonhomogeneity, such as porosity, cracks, seams, segregation,
etc. Ammonium persulphate, Stead’s reagent, Fr ‘s reagent, and Humfrey’s
reagent are less drastic in attack than the deep etc &mg rea.gents and are used
for grain structure development, detection of phosphorus banding, detection
of stram lines, and dendritic segregation, Sespectively.
5.3 After etching, the sample shall be washed in warm water or running
water, using a stiff brush to remove all traces of rust. They should be dried
with alcohol and clean air, and examined immediately afterwards.
5.3.1 For photographic purposes, increased contrast is frequently ob-
tained by washing after etching and applying glycerin to the etched surface.
5.3.2 A solution of one part of syrupy phosphoric acid to one part of
water, to which a little sugar has been added, is sometimes appli.ed to the
dried face to ‘delay rusting. Dipping in an alkaline solution before drying
may be helpful. Dried surfaces may be protected with oil or grease or with
a transparent lacquer.

6. suLpHuR PRINTING
6.1 This ia a macroscopic method for revealing aulphur segregation and
the size and distribution of the sulphides.
6.2 The surface, to be tested for sulphur distribution shall be reasonably
smooth and free from foreign matter such as dirt and grease. Grind the
surf&e on No. 00 or No. 000 emery paper and wash thoroughly in water to
produce a surface satisfactory for taking a sulphur print.

6
 ISr7739(PartV).1976

Place a sheet of photographic paper ( preferably matt finish, to prevent

slipping ), which has been soaked in a 2 percent aqueous solution of sulphuric
actd for approximately 3 or 4 minutes, on the surface of the specimen and
gently smooth out with a squeeze print roller so as to eliminate all entrapped
air bubbles between the paper and the specimen surface. The paper shall
be allowed to remain in contact with the specimen surface for 1 or 2 minutes.
After that period, the paper shall be removed, rinsed, fixed in sodium
thiosulphate ( hypo ), washed and dried in the usual manner.
Yellow or brown speeks on the paper indicate the presence of sulphides
in the specimen.
6.2.1 Any surface, if once used for taking on sulphur print, shall not be
used again for taking another sulphur print. If more prints are desired from
the same section at least 3 mm of steel should be removed prior to making
another print.
6.2.2 Transparent silver bromide paper may be used to give a sulphur
print transparency from which contact prints in any number may be made
on ordinary photographic paper.
6.3 The’ specimen may also be tested by pressing for 2 to 4 minutes upon
gelatin paper which has been treated with solution No. l* and yellow cad-
mium acetate is precipitated. By immersion for 2 to 3 minutes in solution
No. 2t, this is transformed to the dark brown to black copper sulphide.

7. PHOSPHORUS PRINTING

7.1 This is a macroscopic method for revealing the distribution of

phosphorus on the surface of steel.
7.!2 The surface of the specimen shall be prepared by grinding or on
No. 000 emery .$aper and cleaned after grinding by washing in warm
‘running water and carefully drying.
7.2.1 A photographic or filter paper is first soaked in a solution conslsting
of ammonium molybdate ( 5 g per 100 ml of water ) to which 35 ml of nitric
acid ( r.d. 1.2 ) has been added. The paper is then removed from the reagent,
drained nearly free of excess solution, and applied directly to the prepared
surface of the metal, care being taken to effect intimate contact between the
paper and the surface. The paper is allowed to remain in contact with the
surface for approximately 5 minutes.
*Solution No. 1:
25 g of cadmium acetate plus 200 ml of acetic acid ( 80 percent ) to which is
added a solution of 500 ml of sulphuric acid ( r.d. 1.84 ) in 950 ml of water.
ttiolution No. 2:
120 g of copper sulphate plus 880 ml of water plus 120 ml of sulphuric acid
( r.d. l-84 ).

7
IS:7739(l%rtV)-1976

7.2.2 The print is then removed from the specimen ‘and developed for
approximately 4 minutes in a developer made up of 5 ml of saturated stan-
neous chloride solution, 50 ml hydrochloric acid, 100 ml water and 1 g alum.
7.2.3 Development of a bltie colour in the print indicates the location of
phosphorus rich areas on the surface of the metal, and by noting the relative
intensity of the blue colour, the a.mount of phosphorus present may be
estimated. The intensity of colour increases with increased amounts of
phosphorus.

8. LEAD PRINTING

8.1 This is a macroscopic method for revealing the lead distribution on the
surface of a steel specimen.
8.2 The surface of the specimen shall be prepared by grinding on No. 000
emery paper and cleaned thoroughly in running water, degreased with a
suitable solvent and dried.
8.2.1 Soak a caustic resistant filter paper in 5 percent caustic soda
solution for 2 minutes. Place the soaked filter paper over the prepared sur-
face and ensure through air-free contact between the paper and the specimen
by means of a roller sqdeezer or by suitable application of pressure.
8.2.2 Remove the filter paper after maintaining the contact for about
4 minutes and then immerse it in 5 percent sodium sulphide solution for
1 minute. Take out the filter paper and wash in distilled water.
8.2.3 The brownish to dark spots indicate lead distribution in the
examined surface.
8.3 It is difficult to preserve the lead prints, unless immediately photo_
graphed, preferably in colour.

SECTION 2 MICROSCOPIC EXAMINATION OF IRON

AND STEEL

9. PREPARATION OF SPECIMENS

9.0 Recommended methods of select& size, cutting, cleaning and

mounting of specimens are given in IS : 7739 ( Part I )-1975*. Recommen-
ded methods of electrolytic polishing are given in IS i 7739 ( Part II )-1975t.

*Code of practice for preparauon of metallographic specimens: Part I General features.

tCode of practice for preparation of metallographic specimens: Part II Electrolytic
poliing. .i ‘
 IS : 7’139 ( Part V ) - 1976

9.1 A flat surface on the specimen may be obtained by filing, machining,

or grinding on stones or motor-driven abrasive belts. In filing, the speci-
men should be pushed against the cutting edges of the file with the file in
a fixed position. The motion of the specimen against the file should be in
one direction only, since cutting action on both the forward and backward .
strokes shall tend to round the edges of the specimen. One of the most
effective and rapid methods of facing a specimen is by the use of a motoi-
driven abrasive belt. Grinding wheels are effective but require considerable
attention so that the grinding surface is true at all times. Extreme care
should be exercised during grinding so that the specimen does not become
heated and thus temper the steel which is to be examined. It has been
demonstrated that grinding may raise the temperature of the surface layer
of the specimen to 1 000°C.
9.2 The secona stage or specimen preparation is the grinding with succes-
sively finer abrasive materials until the abrasive marks produced are fine
enough to be removed readily by a final polishing operation.
9.3 The grinding operation wet or dry may be aone tither by hand or by
power driven wheels if abrasive papers are used. Emery or Carborundum
papers are used in four or five degrees of fineness of grit. The commonly
used papers are No. 2, 1, 0, 00, and 000. It is frequently not necessary to
use the coarsest or No. 2 paper, but this is determined by the degree of surface
obtained on the preliminary facing. If powder driven disks are used, the
question of revolutions per minute is encountered. Actually the cutting
speed is a function of linear speed; therefore it is impossible to name the
revolutions per minute to be used on a disk since the linear speed varies
from the centre of the disk to the peripherv. The grinding speeds of the
disks usually vary from 500 to 1 000 rev/mm. The grinding on each paper
should be done in one direction and at 90” to that of the preceding paper
or stage. ( For. details of grit number of abrasive papers, see IS : 715-1976*.
A comparative chart of grit numbers of abrasive grains is given at
Appendix A.)
9.4 The grinding operation may be done on paraffined disks or on parafhn
impregnated billiard cloth or canvas. The main advantage of using
paraffined disks or impregnated cloths is the preservation of nonmetallic
inclusions in the polished surface and the retention of graphite in cast iron.
9.5 The grinding operation may also be done by using lead or lead alloy
laps. In a lead-lapped disk, the abrasive is firmly fixed in the soft metal,
and it is claimed that there is less tendency to ‘ drag out ’ nonmetallic
inclusions.
9.6 Kough polishing, which follows grinding, may be considered as a final,
grinding operation. The success of the polishing operation may largely be

*Specificatioo for coated abrasives ( third r.wi~ion).

9
IS : 7739 ( Part V ) - 1976

$;;;;rEd by this step. This may be done by any one of the followbg
:
a) Grinding on billiard cloth or canvas with aluminium oxide of grit
No. 600,
b) Grinding on fine abrasive papers such as No. 0000 or NO. 600
grit silicon carbide, and
c) Grinding with billiard cloth impregnated with paraffin.
9.7 The final polishing technique may be determined largely by the intent
of the examination. If the type and amount of nonmetallic inclusions are
to be studied, the final polish should be done on a disk with a hard, pileless
cloth such as a good grade of heavy cotton or linen, the dull side of a heavy
silk stain, or a good flat crepe. If the st&Zture of the metal is to be studied
at high power, a surface with fewer and less severe scratches, is required.
Magnesium oxide or levigated suspension of y-aluminium oxide are the
common finishing powders. Finishing speeds are fairly slow in comparison
with grinding.
While using magnesium oxide for final polishing, a small quantity of
fresh, dry powder is applied to the lapping cloth and a thin paste is formed
by adding sufficient quantity of distilled water. The paste is then worked
into the cloth fibres with the finger tips, and after so charging the cloth and
during subsequent polishing, additional distilled water is added when
necessary to keep the lap moist.
The y-aluminium oxide, used for final polishing, should have a
uniform particle size of less than 0.1 pm, and the #H of the suspending
liquid shall be controlled between 8.3 and 10.0, by using phenolphthalein
as indicator.
9.8 The polishing of cast iron specimens in which graphite is to be studied,
and of steel specimens to be studied in the etched condition, should usually
not be considered finished until the specimens have been etched and
repolished a number of times to remove the surface layers that have been
disturbed by the previous stages of polishing. Care may be required to
avoid pitting of inclusions, if this process is repeated too often.

10. ETCHING FOR MICROSCOPIC EXAMINATION

10.1 In general, polished metal shows no trace of crystalline structure.

Etching is used to clearly delineate the structure and to produce optical
contrast among the various constituents, In Table 3 are given the etching
reagents commonly recommended for microscopic examination of iron and
steel.
10.2 The polished specimen should be thoroughly cleaned prior to etching.
(The specimen should also be rubbed with caustic soda and washed in water .)

10
 I6:7739(Part V)-1676

The cleanliness of the polished surface may be tested by immersing it in

alcohol. If the surface is completely wetted by the alcohol it shall accept
uniformly the attack of the etchant. If complete wetting of the surface is
not obtained, the specimen should be cleaned in ether or some similar oil
and grease solvent.

IO.3 The cleaned specimen is immersed in the etchant. This immersion

is frequently done by means of nickel or other corrosion-resisting tongs.
The specimen is usually immersed with the polished face up so that the
progress of the etching may be observed. During etching the specimen should
be kept in motion~to prevent gas bubbles from clinging to the surface of the
steel and thus retarding a uniform attack by the etchant. The progress of
the etching may generally be observed visually, but it should also be care-
fully timed. If the sample is not etched sufficiently on the first immersion
the process may be repeated, although re-etching frequently causes staining.
However, if the specimen is over-etched on the first immersion, or any
following immersion the specimen should be repolished and sometimes even
reground prior to etching again. Alternate polishing and etching are very
often required, especially for high-alloy steels, in order to obtain a correct
development of the microstructure.

10.3.1 Whenever the etching time is small, it is better to immerse the

polished face only and take out the sample for examination of progress of
etching. Only where the etching time is considerable, samples may be kept
immersed in the etchant.

10.4 Following the etching, the specimen should be washed in water and
immersed in alcohol and then dried in a blast of warm air. Cold water
washing should be avoided since it retards the evaporation of the alcohol
and usually tends to leave water spots on the surface of the etched specimen.
During drying,’ the specimen should never be rubbed with cotton since it is
usually fatal to the detail of the etch.

10.5 Polished and etched specimens, should be preserved if required in a

desiccator or a sterilizer cabinet where dust, dirt, and moist gases from the
atmosphere shall not collect on the surface.

10.5.1 Etched surfaces that are to be preserved for comparatively long

periods of time should be coated thinly with a suitable lacquer. Lacquer
coatings are best applied to prepared surfaces by partly immersing thes eci-
men in a thinned solution of the lacquer, allowing the excess liquid to Jr ain
for a few seconds, and then permitting the lacquer to dry with the polished
and etched surface in an up and horizontal position.

10.5.2 A thin coating of Vaseline or neutral white mineral oil over the
prepared surface is satisfactory in some cases for long time preservation,
particularly when storage is made in a desiccator.

11
 TABLE 1 ETCHING REAGENTS FOR MACROsCoPIc EXAMINATION OF IRON AND S-L

( Clau5s5.1 )
No. ETCnING COMPOSITION REMARKS
REAGENT

(1) (2) (3) (4) (5)

1. Hydrochloric HCl 50 ml Usedat to82%for 1 to60min Shows segregation, porosity,
acid Hz0 50 ml depending on the size of crack% depth of hardened
sample, type of steel, and type zone in tool steel, etc. May
of structure to be developed. produce cracks in strained
Surface .4 or B rleel
2. Mixed acid HCl 38 ml To be used as above for 15 Same as for reagent No. 1
H&Q 12 ml to 45 min. Surface B or C
Hz0 50 ml
3. Nitric acid 25 ml Used cold for large surfaces such Szd 2as for reagents No. 1
G ea 75 ml as split ingots which may not
conveniently be heated.
Surface B or C
4. Nitric acid HNOa 0.5 to 1.0 Immerse 30 to 60 s after grinding To show structure of welds
percent specimen on 240-grit emery
in Ha0 belt and thorough cleaning.
Surface B or C
5. Ammonium Surface should be rubbed with Brings out grain structure in
persulphate absorbent cotton during cases of excessive graih growth,
etching. Surface C recrystallization at welds, flow
lines, etc
6. Ammonium After grinding on No. 320 abra- Shows dendritic macrostructure
persulphate
with potas-
A. C$~h%Os
B. Sime as A, plus
1~~ I%
I.5 g
sive paper, swab for 15 min
with solution At then 10 min
of cast iron

sium iodide KI with B, then 5 mm with C, and

C. Same as B, plus 1.5 * 5 min with D, finally washing
HgClz with water and drying with
D. z~;as C, plus 15 ml alcohol
8 1
7. Stead’s reagent CuCls 2.5 g The sa% are dissolved in the Brings out phosphorus-rich areas
;$‘I 10.0 g HCI with the addition of the and phosphorus bending. May
5 ml least possible quantity of hot be used also for general
Ethyl alcohol Up to 25Oml water. Surface B or C segregation
8. Pry’s reagent CuClp 90 g Most useful for mild steel, parti- Shows up strain lines due to cold
HCl 120 ml cularly bessemer and other work
HrO 100 ml high nitrogen steel. Before etch-
ing, sample should be heated to
200 to 250°C for 5 to 30 min,
depending on the condition of
the steel. During etching
the surface should be rubbed
with a cloth soaked in the etch-
ing solution. Wash in alcohol
or rinse in HCl ( 1+ 1 ) after
etching to prevent deposition
of copper. Surface B or C
EA. Pry’s reagent CuCl* 45 g Same as for reagent No. 6, may Same as for reagent No. 6
HCl 180 ml give more contrast. Speci-
Hz0 100 ml men can be washed in water
without depositing copper.
Surface B or C
9. Nital HNOs 5ml Etch 5 min, followed by 1 set in Shows cleanness, depth of hard-
Ethyl alcohol 95 ml HCI (10 percent). Surface ening, carburiaed or decar-
B or C burized surface, etc
10. Humfrey’s Copper ammo- 120 g Slight abrasion of surface after Develops dendritic segregation
reagent nium chloride etching is recommended.
HCl 50 ml Surface B
HsO 1 000 ml
11. Sulphuric acid H&Q 25 ml Use cold 8 to 16 h. Surface B Shows dendritic pattern and
He0 75 ml flow lines

NOTE 1 - The use of concentrated reagents is intended unless otherwise specified.

NOTE 2 - Surface designations :
Surface A - Saw-cut or machined surface
Surface B - Average ground surface
Surface C - Polished surface
 TABLE 2 MACROETCIiING OF IRON AND STEEL FOR SPWbIC PURPOSES
(C1au.r.s5.1.1 )

PURPOSE COMPOWRON REMARKS USE

(1) (2) (3) (4)

Blowholes Ho% 10 ml Use cold on large sections for Shows blowholes, porosity,
H2O -90 ml 24 h. Surface B pipe and inclusions
Carburised case HIW3 3 ml Etch at room temperature. Sur- Shows depth of carburized
Ethyl alcohol 95 ml face B case
contrast Iodine lg Uyac;t;oom temperature. Sur- Produces contrast for photo-
graphing
ii;0 1% L
Cracks HNOs 5 ml Etch at room temperature. Et- Detects fatigue, service harden-
Ethyl alcohol 95 ml ches within l/2 h. Surface B ing and grinding cracks
Cracks Copper 120 g Etch first with a neutral solution Produces a strong relief effect.
ammonium to remove machine marks. Shows up dendrites and may
chloride Use cold for 20-30 min. Sur- indicate cracks
HCl 50 ml face B
z
Hz0 1000 ml
Decarburization HNOS 5 ml Etch at room temperature. Sur- The decarburized areas shall be
Ethyl alcohol 95 ml face C light. Area not decarburizcd
dark
Defects H2SO4 10 ml Use cold on large sections for Shows porosity, pipe, blowholes,
W' 90 ml 24 h. Surface B and inclusions
Defects HeSO 20 ml Use near boiling for at least Shows general structure and
HCI 10 ml l/2 h. Surface A defects
HsO 30 ml
Dendrites H2SO4 20 ml Use near boiling for at least Shows general structure and
HCl 10 ml l/2 h. Surface A defects
Hs,O 30 ml
Dendritic patterr HeSO4 25 ml Use cold, 8 to lb h.‘Surface B Shows dendritic pattern and flow
H2O 75 ml lines
Dendritic FeCls 40 g Etch first with 10 percent nitric Shows dendritic structure
structure CuCl, 3g acid. Surface B
HCl 40 ml
HxO 500 ml
 Fibre fHo(hS,o~ IO-12 g Swab on freshly made solution Shows fibre and grain contrast
90 ml for l/2 min. Surface B
Flow lines HiSO 25 ml Use cold, 8 to 16 h. Surface B Shows flow lines and dendrkic
HsG 75 ml pattern
Flow lines HCl 50 ml Use hot. Surface A Shows Row lines
H,O 50 ml
Grain contrast ~~),SzGs 10-20 g Swab on freshly made solution Shows grain contrast and fibre
90 ml for 1 to 2 min. Surface B
Grain contrast $a, l-5 g P”f’;;$ ipecimen carefully. Sur- Shows good grain contrast
HCl 30 ml a
HsG 95 ml
Ethyl alcohol 30 ml
Grain size fIN3)2S208 10-20 g Swab on freshly made solution Shows grain size especially in
2 90 ml for 1 to 2 min. Surface I3 low-carbon steels, wrought
iron, and welded sections
Hardness =W3 5 ml Etch at room temperature on Shows depth of hardness
penetration Ethyl alcohol 95 ml smooth ground surface. Sur- penetration of heat treated
face B samples
;
Hardness HCl 50 ml Use hot 2 to 5 min. To preserve Shows depth of hardening,
penetration H20 50 ml surface after etching, scrub in especially carbon steels. Pro-
running water, dip in weak duces distinct contrast between
NHIOH, dip in solution of martensitic and troostitic
soluble cutting oil, dry with a zones
rag and compressed air. Sur-
face B
Heterogeneity HCl 50 ml Immerse specimen in hot solu- Shows heterogeneity in general
H,O 50 ml tion form l/2 to 1 h. Surface A
Heterogeneity HCl - Use hot 100°C. Surface A Shows heterogeneity in 3 to 3.5
percent nickel steels
NOTE - Surface designations:
Surface A - Saw-cut or machined surface
Surface B-2 Average ground surface
Surface C - Polished surface
( Continued)
 TABLE 2 MACROETCHING OF IRON AND STEEL FOR SPECIFIC PURPOSES - Contd

PURPOSE COMPCBITION REMARKS USE

(1) (2) (3) (4)

Impurities in CuCI2 lg Etch only well polished surface Plates out copper on ferrite
ferrite SnCle 0.5 g which has been thoroughly containing impurities. Gives a
F&la 30 g dried. Surface C good even etch
HCl 30 ml
He0 500 ml
Ethyl alcohol 500 ml
Inclusions HzSOA 10 ml Use cold on large sections for Shows inclusions, porosity, pipe
Hz0 90 ml 24 h. Surface B and blowholes
Inclusions HeSO lo-20 ml Use hot. Surface A Etches sulphide inclusions
He0 80-90 ml
Pipe and porosity I-WA 10 ml Use coId on large sections for Shows pipe, porosity, blowho&
HsO 90 ml 24 h. Surface B and inclusions
z Rail sections HCl 45 ml Etch near boiling point for 2 h. Use for etchingrail sections
H2SG. 15 ml Surface A
II*0 5 ml
Segregation Picric acid 3g Etch at room temperature for Shows segregation
Ethyl alcohol 100 ml 4 to 5 h. Surface B
Segregation Picric acid lg Use hot. Surface B Shows segregation
HCl 1 drop
Ethyl alcohol 25 ml
Segregation I-IN03 lo-15 ml Etch at room temperature. Sur- Shows heavy segregation
HsO or ethyl 85-90 ml face B
alcohol
Segregation HN03 5 ml Etches within l/2 h. Surface is Shows segregation in low carbon,
HsO or ethyl 95 ml black when etched. Surface B low chromium nickel steels
alcohol
Segregation I-IN03 2-10 ml Etch first with weak acid to re- Shows segregation in ingot
Hz0 90-98 ml move machine marks and then sections and large pieca
increase concentration for
structure. Surface B
 Segregation CuCls May be used for electrolytic etch- Shows segregation
Pi& acid ing. Surface B
HCl 1.5~2.5 ml
Ha0 10 ml
Ethyl alcohol 100 ml
Segregation, HNOa 5 ml Use on a polished, longitudinal The detect carbide segregations,
carbide Ethyl alcohol 95 ml section. For hiah-sneed s&l. particularly in high-speed
etch until mat& is-darkened:
Surface C
Segregation, Copper ammonium 5 g Immerse finely ground, clean Shows phosphorus and carbon
carbon and chloride sample in solution for 1 rnin: segregation
phosphorus H2O 60 ml wash with water and rub off
copper. Surface C
S egregation, Picric acid o-5 g Etch at room temperature until Uneven staining represents phos-
phosphorus H20 100 ml staining occurs. Surface C phorus segregation
Segregation, FeCls 36 g Polish as for microscopic work, Shows phosphorus segregation
phosphorus CuCls use etch cold for 10 set to 2
c SnCla 0.: “g min. Surface C
q HCl 100 ml
H2O lOO0n-J
Segreg tion, CuCls 10 g Dissolve salts in small amount of Area not coated by copper shows
phos1 horus g&F’2 hot water then add alcohol. phosphorus segregation
:: :1 Apply solution to polished sur-
Ethyl alcohol 1000 ml face drop by drop. Surface C
Segfegation, CuCla 5g Etch for 1 mm. Surface C Shows phosphorus segregation
phosphorus Mgclz 4g
HCl 1 ml
H20 20 ml
Ethyl alcohol 100 ml

NOTE - Surface designations :

Surface A - Saw-cut or machined surface
Surface B - Average ground surface
Surface C - Polished surface
( Continued
)
 TABLE 2 MACROETCHING OF IRON AND STRlIL FOR SPRCIFIC PURPOSES - Contd

PURPOSE (hdPO2ITION RKYARKS USE

(1) (2) (3) (4)

Segregation, CuCl* Polatt cpecimen carefully. Sur- Shows phosphorus segregation

phosphorus HCl 204tll
40 ml
H&J
Ethyl alcohol 20 ml

Segregation CuCl* 1.5 g Immerse specimen for 90 set or Shows phosphorus segregation
phosphorus Ni(NWs 5g more. Surface C
FeCls gg
3320 12 ml

Segregation! H2SO4 IO-20 ml Use hot. Surface A Etches sulphide inclusions

sulphide mclusions Ha0 80-90 ml
z
Soft spots HNOa 5 ml Etch at room temperature. Non-destructive test for hardened
Ethyl alcohol 95 ml Surface B tools

SOR spots HCI 50 ml U;a;Jj on ground surface. Sur- Shows soft spots
H2O 50 ml

Strains CuCl2 90 ml Copper does not precipitate with Shows strain lines
HCl 120~ml this etch. Heat specimen to 205
Hz0 100 ml to 245°C for l/2 h, then etch
ground surface for l-3 min.
Rub with powdered cupric
chloride, then rinse with
alcohol. Surface B

Strains CuCl* gg Heat specimen to 200°C and Shows strain lines

FeCl, 6g immerse ground surface.
HCl 10 ml Surface B
Ethyl alcohol 100 ml
 3n Specimen 12 x 25 x 100 mm is To measure intergranular
10 ‘nl sensitized by actual welding, or corrosion of 18-8 corrosion
a7 ml artificially by heating to 480 resisting steel
to 700% (generally 680°C).
Immersed in the boiling cupric
sulphate solution for 72 h. Spe-
cimen is then bent 180° around
12 mm pin. Cracking indicates
disintegration has taken place
due to migration of carbides to
grain boundaries. Surface B

StNCtUrC 25 ml Etch at room temperature. Sur- Shows general structure

75 ml face B

Structure I-WA 20 ml Use near boiling point for at least Shows general structure and
HCl 10 ml l/2 h. Surface A defects
Hz0 30 ml

z Weld HCl 50 ml When testing large sections! the For testing the soundness of
examination Hz0 50 ml acid may be added by building welds
a dam with paraffin wax
around the part to be tested.
Surface A

NOTE - Surface designation:

Surface A -Saw-cut or machined surface
Surface B - Average ground surface
Surface C - Polished surface
 TABLE 3 ETCHING REAGENTS FOR MICROSCOPIC EXAMINATION OF STEELS AND IRONS
( Only reagents of analytical grade should be used )

[( Clause 10.1 )

No. ETG HIN G COMPOSITION REMARKS USE

REAGENT

(1) (2) (3) (4) (5)

Group I General Reagents for Irons and Steels ( Carbon, Low and Medium-Alloy deel)

1. Nitric acid HNOs, cofourless l-5 ml Etching rate is increased, selecti- In carbon steel, (a) to darken
(Nital) Ethyl or methyl 100 ml vity decreased, with increasing perlite colomes, (b) to reveal
alcohol, 95 percent percentage of HNOs. Reagent ferrite boundaries, (c) to
or absolute (also No. 2 ( picric acid ) usually differentiate ferrite from mar-
amyl alcohol) superior, 4 percent in amyl al- tensite. The 1 percent solution
cohol useful for grain boun- is also suitable for uses (c),
dary and contrast of low- (d), (e) and (f) noted below
carbon materials. Etching for reagent No. 2
time, a few seconds to a minute
& Picric acid Picric acid 4g More dilute solutions occasional- For all grades of carbon steels :
(Picral) Ethyl or methyl 100 ml ly useful. Does not reveal fer- (a) annealed, (b) normalized,
alcohol, 95 percent rite grain boundries as readily (c) quenched, (d) quenched
or absolute as No. 1. Etching time a few and tempered, (e) spheroidi-
(Use absolute alcohol only when seconds to a minute or more zed, and(f) austempered. For
acid contains 10 percent or more all low-alloy steels attacked
of moisture) by this reagent
3. Hydrochloric and HCl 5 ml Best results are obtained when For revealing the austenite grain
picric acid Picric acid lg the martensite is tempered for size in quenched, and
Ethyl or methyl 100 ml 15 min at 205 to 245% quenched-and-tempered steels
alcohol, 45 percent or
absolute
4. Chromic acid CrOs 10 g Used electrolytically, the speci- For various structures except
HsO 100 ml men as anode, stainless steel grain boundries of ferrite. At-
or platinum as cathode, 20 to tacks cementite very rapidly,
25 mm apart; 6 V usually austenite less rapidly, ferrite
used. Time of etching 30 to and
. .._iron phosphide
. very
90 s depending on specimen slowly lf at all
 5. Heat tinting Heat only Clean, dry, polished specimen Pearlite first to pass through a
heated face up on hot plate given colour, followed by fer-
to 205 to 87OOC. l%ne and rite; cementite. less affected,
temperature both have deci- iron phosphide still less. Es-
ded effects. Bath of sand or pecially useful for cast irons
molten metal may be used
6. Heat etching Heat only Specimen is heated 10 to 60 min For revealing austenitic grain
at 815 to 1205°C in carefully size of polished specimens
purified hydrogen and should
have no contact with scale or
reducible oxides. After
etching, specimen is cooled
in mercury to avoid
oxidation

Group II General +agents for Alloy Steels (Stainless and Highspeed Steels )

7. Ferric chloride FeCls Etch at room temperature Structure of austenitic nickel

and hydro- HCI 5: !nl and stainless steels
chloric acid He0 100 ml
8. Nitric acid HNOs (colourleas) 5 to 10 ml Etch at room temperature General structure of high-speed
(Nital) Ethyhy;;lmethyl 90 to 95 ml tool steel

(95 percent
or better)
9. Chrome regia HCl 25 ml Activity is controlled by amount Heat-treated 18 percent ch-
CrOs solution (10 5 to of chromic acid romium, 8 percent, nickel
percent) in Hz0 50 ml stainless steels. Useful elec-
trolytically, if diluted with
2 parts alcohol and 2 parts
glycerin and applied for 20 to
60 s with 6 V
10. Ferric chloride Saturated solution of FeCla in Use full strength Structure of stainless steel
and nitric HCl, to which a little UNOs
acid is added
NOTE - The use of concentrated reagents is intended unless otherwise specified.
( Continued),
&: NS - Contd :ELS AND ILWTLON OF STEpIc EXAMIN& MICRGSCG:BAGENTS FO; ETCHING R TABLE 3

=! ould be used )tical grade shgents of analy ( Obly rea

==+ION COMPOSITIING No. ETCH

:ENT REAC
(4) (3) 9 (1) 6

4 I-chromium base Structure of irom water before rarm specimen il 10 ml 9. H 11. Mixed
V and alloys, high-spest results use etching. For b0 to 30 ml I:
wed steels, glycc
steel. austenitic manate polishing method of alter
?&zzrn alloys Etches nickel-given sufficient and etching. If 10 to 30 ml ilycerin 2 C
satisfactorily totally austeni- time, shall etch 1
better results tic alloys, but
r using reagent are obtained b)
No. 10-C

gh silicon alloYsStructure of hilin may be va- mount of glycer 10 ml AtNO B. E

oe of Duriron tylal ried to suit met 20 ml IF b
!O to 40 ml Glycerin : 0

hromium-nickel,
urn - manganese,
r austenitic iron-
To etch iron aay be varied if Lmount of HCl n 10 ml
iron - chromino rapidly or
and all other results employ
reagent acts t(
slowly. For best
%pa slycerin
c. I
I

se alloys chromium barnate polishing method of alte -WZ :

and etching

tainless steels ant For austenitic sally, the speci- Jsed electrolytic’ 10 g oxalic acid : acid 12. Oxalic
tlloys. Carbide high-nickel stainless steel or men as anode, ! 100 ml -I20 ;
8tructure revealec and general shade, about 25 platinum as cat
t etching time depending od usually used. mm apart; 6 1
rbides in stain- Precipitated ca
be revealed in less steels, may
: general strut- lo to 15 s, the
min. For study ture in about 1
I to 3 V may be of carbides, 1.5
easing the etch- used, thus incr
nd improving ing time a
control of etch
 13. Ammonium per- (~4hWl3 10 B Used electrolytically like the oxa- For fast-etching stainless steels
sulphate Ha0 90 ml lit acid solution, but acts more
slowly, re uiring longer than
15switb 2 v
14. Cupric chloride C&l* 5g Used cold (Kalling’s reagent) For austenitic and ferritic steels,
and hydrochlo- HCl 100 ml the ferrite being most easily
ric acid E thy1 alcohol 100 ml attacked, and austenite at-
Hz0 100 ml tacked appreciably only when
it has begun to decompose
to martensite
15. Mixed acids and HCl 30 ml Apply by swabbing For stainless alloys and others
cupric chloride HNOZ 10\ml high in nickel or cobalt
Saturate with cupric
chloride and let stand for
20 to 30 min before use
16. Nitric and acetic HNO8 30 ml Apply by swabbing For stainless alloys and others
acids Acetic acid 20 ml high in nickel or cobalt
!z 17. Nitric and hydro- HNOS 5 ml Used cold for about 5 min For‘ revealing general structure
fluoric acids HF (48 percent) 1 ml of austenitic stainless steel with
H& 44 ml avoidance of stain markings

18. Hydrochloric and HCI 10 ml Etch 2 to 10 min To reveal the grain size of
nitric acids in HNOS 3 ml quenched, or quenched and
alcohol Methyl alcohol 100 ml tempered high speed steel

19. Hydrochloric acid HCl 10 ml Used electrolytically for 10 to For straight chromium and
in alcohol Alcohol 90 ml 30 s with 6 V; mu& be free chromium-nickel steels
from water to prevent
tarnishing
20. Lactic and hydro- Lactic acid 45 ml Used electrolytically for 10 to For chromium steels (4 to 30
chloric acida in HCl 10 ml 30 s with 6 V; does not tarnish percent chromium) or delta
alcohol Alcohol 45 ml ferrite in austenitic stainless
steels
NOTE - The use of concentrated reagents is intended unless otherwise specified.
( Continued)
 TABLE 3 ETCHING REAGENTS FOR MICROSCOPIC EXAMINATION OF STEELS AND IRONS - Contd
( Only reagewts of analytical grade should be otted )
No. Ercsrnro COMPOSTION REMARKS USE
RXAGENT

(11 (2) (3) (4) (5)

Group II General Reagents for Alloy Steels ( Stainless and High-Speed Steels )
2 1. Ferricyanide Potassium 30 g Must be fresh. Use boiling To distinguish between ferrite
solution ferricyanide and sigma phase in iron-
KOH 30 g c&mium, iron-chromium-
60 ml nickel, iron-chromium-man-
HsC
ganese and related alloys.
Colotirs : sigma phase, light
blue; ferrite, yellow
22. Cupric sulphate CUSO~ 4g Marble’s reagent Structure of stainless steels
HCl 20 ml
Hz0 20 ml
2 3. Hydrochloric HCl 5 ml Same as No. 3 To etch many steels of the
!# and picric Picric acid iron-chromium, iron-chro-
acids Ethyl or methyl l&P, mium-nickel and iron-
alcohol, 95 per- chromium-manganese types
cent or absolute
24. Heat tinting Heat only in air for 10 to Carbides remain white and aus- For austenitic stainless steel con-
60 s at about 595 to tenite darkens less rapidly taining ferrite and carbide
650% than ferrite, on sections! pre-
ferably etched first wrth a
chemical reagent

Group III Segregation, Pxiarsry end Strain Lines

25. Cupric chloride A. CuClz lg Dissolve salts in least possible For shcwing segregation of phos-
4g quantity of hot water. Etch for phorus or other elements in
MgCla
HCl 1 ml about I min repeating if neces- solid solution; copper tends
20 ml sary. Stead’s reagent to deposit first on areas low&
Hz0
A$eohol, 100 ml in phosphorus. The structure
absolute may be more clearly delineat-
ed by light hand-polishing to
remove the copper deposit
after etching
 B. CuCls 5f3 May be used cold. Etching time, To reveal strain lines and their
HCl 40 ml about 10 s. Fry’s reagent microstructure, and precipi-
He0 30 ml tation hardening in steel
Ethyl alcohol 25 ml
26. Modified ferric F&Is 30 g Oberhoffer’s reagent For showing phosphorus seg-
chloride CeCls lg regation and dendritic strut-
SnCls 0.5 g ture
HCl 50 ml
Ethyl alcohol 500 ml
H2O 500 ml
27. Alkaline chromate 18 g Add NaOH slowly, and use whel Shows oxygen segregation by
~~3(diitilkd) 145 ml not over one day old, boiling darkening martensite rapidly,
NaOH 80 g at 118 to 120JC for 7 to 20 min ferrite more slowly, and zones
of high oxygen content much
more slowly
Group IV Structwe and Detath of Case of Nitrided Steels
28. Cupric sulphate CU.GOl 1.25 g - Proportions should be accurate. For showing total depth, struc-
and cupric CuCls 2.50 g Etch by immersion to avoid ture, and various zones of
chloride MgCl, 10 g confusing edge effects nitrided chromium-vanadium
HCl 2ml steels and nitralloy
z
Hz0 100 ml
Dilute above solution to
1 000 ml with 95 percent
ethyl alcohol
29. Picric and nitric Pi&c acid 10 parts Best results are obtained when For depth of case and structure
acids (4 percent) the specimen is annealed in of nitralloy
(No. 2) lead at 800°C before etching
HNO3 (4 percent) 1 part
(No. 1)
30. Nitric acid (Nital) HNOs 2 ml Etch at room temperature For structure and depth of case
Ethyl or methyl 100 ml of nitrided steels
alcohol,
95 percent
or absolute
31. Cupric s&hate CUSO~ 4g Marble’s reagent Total depth of nitrided case
HCl 20 ml
I.320 20 ml
NOTE - ‘JIe use of concentrated reagents is intended unless otherwise specified.
 TABLE 3 ETCHING REAGENTS FOR MfCROSGGPfC EXAMINATION OF STEELS AND IRONS - Contd
( Only reagents of analytIca grade should be used )

No. ETCHING IMPOSITION REMARKS USE

REAGENT
(11 (2) (3) (4) (5)

Group V Reagents for Carbides, Phospbides, Nitrides and Tnngstides

32. Sodium picrate Sodium picrate lg US;~ LF. Etching time Shows difference between phos-
(neutral) H2O 100 ml phides and cementite; iron
(Wash salt well with al- phosphide attacked, cemen-
cohol to remove excess tite unattacked
acid or alkali)
33. Chromic acid CrOs Sg Etching in picric acid (No. 2) Distinguishes between iron phos-
and heat tint- H20 100 ml then for 1 min in chromic acid; phide and cementite in phos-
ing Followed by heat heat tint by heating face up on phide eutectic of cast iron;
tinting hot plate at about 260°C for I iron phosphide is coloured
N min darker
m
34. Sodium picrate, Picric acid 2g Use boiling, 5 to 10 min, or pre- Colours cementite, but not car-
alkaline NaOH 25 g ferably, electrolytically at bides <high in chromium. In
H2O 100 ml roum temperature; for the lat- tungst& steels, iron tungstide
ter, specimen is anode, plati- (FenW) and iron tungsten
num or stainless steel is carbide (FehW&) are colour-
cathode; with 6 V, about 40 s ed more rapidly than cemen-
is usually sufficient tite, but tungsten carbide is
unaffected. Attacks sulfides.
Delineates grain boundaries
in hypereu’ectoid steels slowly
cooled condition
35. Hydrogen per- Hz02 10 ml Should be fresh. Etching time Attacks and darkens iron-tungs-
oxide and Na0I-I 10 percent 20 ml 10 to 12 min tide in carbon-free tungs-
sodium solution in water ten alloys. When carbon is
hydroxide present this solution darkens
the compound (Few WC) in
proportion to the amount of
carbide present; tungsten
carbide is darkened
 36. Ferricyanide AK&% 1 to4g Should be freshly made; etch 15 Differentiates between carbides
solution min in boiling solution. Seven and nitrides. Cementite is
HsO 1; L grams of NaOH may be subs- blackened, pearlite turned
tituted for 10 g of K0f-I in brown, and massive nitrides
eitherAorB remain unchanged

19 g May be used cold, but preferably Darkens carbide containing ch-

19 g hot, should be freshly made, romium, carbides, and tungs-
106 ml etching time 5 to 10 min. tides in tungsten and high-
Murakami’s reagent speed steels. At room tem-
perature colours ternary car-
bides (FesWsC or FesWsC)
in a few seconds, iron tungs-
tide (FesWs) in several minu-
tes, and barely colours cemen-
tite

37. Sodium cyanide NaCN 10 g Used electrolytically, the speci- Darkens carbides without at-
Us0 90 ml men as anode, cathode, similar tacking austenite or grain
tu material; about 25 mm apart boundaries
21 6 V (not less than 5). Etching
time 5 min or more

38. Chrotic acid CrOs &tuNo. 4 in Group 1. Attacks carbides in stainless steels
HsO very rapidly, austenite less
rapidly, and ferrite very slowly
if at all. For various struc-
tures of stainless steels

39. Oxalic acid Oxalic acid See No. 12 in Group II. If strong- Reveals carbides in stainless
HsO lczl ly etched general structure is steels
revealed; therefore for study
of carbides reduced. voltage
is used for etching, giving
better control of etch

NOTE- The use of concentrated reagents is intended, unless otherwise specified.

( Continued )
 TABLE 3 ETCHING-REAOBNTS tiOR MICROSCOPIC EXAMINATION OF STEELS AND IRONS - Clmd
(ody -6ODt# Of Wdytid grade shodd be Wad )

No. ETOWIO COMPCXlTtOlS FLSYARKS Usi!

&EAOSNT
(1) (2) (3) (4) (5)

Group VI Reqgents for Detection of Tamper Embrittlommnt

40. F’icric acid Picric acid Etching time about 10 minutes. A specimen of the steel, which
I-W lOt% After etching, carefully remove appears to be temper brittled
the deposit under water by & etched with any one of the
means of a cotton wool pad reagent No. 35, 36 or 37,
simultaneously with a sample
Picric acid Dissolve picric acid in ether, of the same steel in the non-
41. Pi&c acid-Zep- hardened state. In the case of
hiran chloride* Ethyl ether 4 Ll add the water-Zephiran
chloride mixture, stir well and embrittled steel, the etch will
solution 1 N Zephiran 2ml
chloride then leave for 24 h to settle. show up the grain boundaries
e of the parent austenite by
solution For etching use only the clear
(12-8 per- part of the solution. Etching blackening them, whereas
time several minutes with the there is no such reaction on
cent)
specimen kept still. Next the non-hardened steel. All
wash in an ether-alcohol the three reagents may not
solution, rewash with water necessarily be suitable for
every type of steel
and carefully wipe the dark
deposit

42. Picric acid in Picric acid 10 g Add the alcohol immediately

xylol-ethyl Xylol 80 ml before use, filter the undissolv-
alcohol Ethyl alcohol 20 ml ed picric acid. Etching time :
30 minutes. Carefully wipe the
dark deposit

N~TE - The use of concentrated reagents is intended, unless otherwise specified.

lZephiran chloride is a high molecular plkyl dimethyi benzyl ammonium chloride.

 IS : 7739 (Part V ) - 1976

APPENDIX A
( Clause 9.3 )
COMPARATIVE CHART OF GRIT NUMBERS OF
ABRASIVE PAPERS

A-l. For designation of grain sizes, of coated abrasives only grit numbers
are recognized in IS: 715-1976*. Although grit numbers are now being
universally adopted, coated abrasive papers are also available in a graded
symbol sequence of 12/O to 4) covering the grit number range of approxi-
mately 600 to 12. There is also a special emery polishing paper for very
fine polishing, such as used in preparation of metallurgical specimens, which
is graded in a symbol sequence of 4/O to 3, covering the grit number range
of approximately 600 to 180. A comparative chart showing the relation
between grit numbers and the customary grading symbols are given below
for the guidance of users:
Grit No. S’lmbol for Silicon Symbol for Emery
Carbide Paper Polishing Paper
600 12/o 4,lo
- - 3/O
500 1110 2/O
460 1010 0
360 --
320 910 L
280 8/O -
240, 7/o 1G
220 ‘310 2
180 510 3
150 4/O -
120 3/O -
100 2/O -
80 -
60 a .-
50 1 -
40 14
36 2 -
30 29 -
24 3 -

*Specification for coated abrasives ( third revision )

29
BUREAU OF INDIAN STANDARDS
Headquarters:
Manak Bhavan, 9 Bahadur Shah Zafar Marg, NEW DELHI 110002
Telephones: 323 0131, 323 3375,323 9402
Fax : 91 11 3234062, 91 11 3239399, 91 11 3239382
Telegrams : Manaksanstha
(Common to all Offices)
Central Laboratory: Telephone
Plot No. 2019, Site IV, Sahibabad Industrial Area, Sahibabad 201010 8-77 00 32

Regional Offices:
Central : Manak Bhavan, 9 Bahadur Shah Zafar Marg, NEW DELHI 110002 32376 17
‘Eastern : l/14 CIT SchemeVII M, V.I.P. Road, Maniktola, CALCUTTA 700054 337 86 62
Northern : SC0 335-336, Sector 34-A, CHANDIGARH 160022 60 38 43
Southern : C.I.T. Campus, IV Cross Road, CHENNAI 600113 235 23 15
t Western : Manakalaya, E9, Behind Marol Telephone Exchange, Andheri (East), 832 92 95
MUMBAI 400093

Branch Offices:
‘Pushpak’, Nurmohamed Shaikh Marg, Khanpur, AHMEDABAD 380001 550 13 4s
$ Peenya Industrial Area, 1st Stage, Bangalore-Tumkur Road, 839 49 55
BANGALORE 560058
Gangotri Complex, 5th Floor, Bhadbhada Road, T.T. Nagar, BHOPAL 462003 554021
Plot No. 62-63, Unit VI, Ganga Nagar, BHUBANESHWAR 751001 40 36 27
Kalaikathir Buildings, 670 Avinashi Road, COIMBATORE 641037 21 01 41
Plot No. 43, Sector 16 A, Mathura Road, FARIDABAD 121001 8-28 88 01
Savitri Complex, 116 G.T. Road, GHAZIABAD 201001 8-71 1996
53/5 Ward No. 29, R.G. Barca Road, 5th By-lane, GUWAHATI 781003 54 11 37
5-8-56C, L.N. Gupta Marg, Nampally Station Road, HYDERABAD 500001 20 IO 83
E-52, Chitaranjan Marg, C-Scheme, JAIPUR 302001 37 29 25
117/418 8, Sarvodaya Nagar, KANPUR 208005 21 68 76
Seth’Bhawan, 2nd Floor, Behind Leela Cinema, Naval Kishore Road, 23 89 23
LUCKNOW 226001

NIT Building, Second Floor, Gokulpat Market, NAGPUR 440010 52 51 71

Patliputra Industrial Estate, PATNA 800013 26 23 05
Institution of Engineers (India) Building 1332 Shivaji Nagar, PUNE 411005 32 36 35
T.C. No. 14/1421, University P.O. Palayam, THIRUVANANTHAPURAM 695034 621 17

*Sales Office is at 5 Chowringhee Approach, PO. Princep Street, 271085

CALCUTTA 700072
TSales Office is at Novelty Chambers, Grant Road, MUMBAI 400007 309 65 28
*Sales Office is at ‘F’ Block, Unity Building, Narashimaraja Square, 222 39 71
BANGALORE 560002

Printed at Simco Printing Press, Delhi