SIST-TP CEN ISO/TR 16060:2014
(Main)Destructive tests on welds in metallic materials - Etchants for macroscopic and microscopic examination (ISO/TR 16060:2003)
Destructive tests on welds in metallic materials - Etchants for macroscopic and microscopic examination (ISO/TR 16060:2003)
ISO/TR 16060 gives a non-exhaustive list of etchants that can be used for the macroscopic and microscopic examination of welds in accordance with ISO 17639 for the following groups of materials: - carbon steels and low-alloy steels; - stainless steels; - nickel and nickel alloys; - titanium and titanium alloys; - copper and copper alloys; - aluminium and aluminium alloys.
Zerstörende Prüfung von Schweißverbindungen an metallischen Werkstoffen - Ätzungen für die makroskopische und mikroskopische Untersuchung (ISO/TR 16060:2003)
Dieser Technische Bericht enthält eine keinesfalls vollständige Liste von Ätzmitteln, die für die makroskopischen und mikroskopischen Untersuchungen von Schweißnähten in Übereinstimmung mit ISO 17639 für die folgenden Werkstoffgruppen verwendet werden können:
- Kohlenstoff- und niedriglegierte Stähle;
- nichtrostende Stähle;
- Nickel und Nickellegierungen;
- Titan und Titanlegierungen;
- Kupfer und Kupferlegierungen;
- Aluminium und Aluminiumlegierungen.
Essais destructifs des soudures sur matériaux métalliques - Réactifs pour examens macroscopique et microscopique (ISO/TR 16060:2003)
L'ISO/TR 16060:2003 donne une liste non exhaustive des réactifs pouvant être utilisés pour l'examen macroscopique et microscopique des soudures conformément à l'ISO 17639 pour les groupes de matériaux suivants:
aciers non alliés et faiblement alliés; aciers inoxydables; nickel et alliages de nickel; titane et alliages de titane; cuivre et alliages de cuivre; aluminium et alliages d'aluminium.
Porušitvene preiskave zvarov na kovinskih materialih - Jedkala za makroskopsko in mikroskopsko preiskavo (ISO/TR 16060:2003)
Standard ISO/TR 16060 podaja neizčrpen seznam jedkal, ki jih je mogoče uporabiti za makroskopsko in mikroskopsko preiskavo zvarov v skladu s standardom ISO 17639 za naslednje skupine materialov: – ogljikova jekla in malolegirana jekla; – nerjavna jekla; – nikelj in nikljeve zlitine; – titan in titanove zlitine; – baker in bakrove zlitine; – aluminij in aluminijeve zlitine.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST-TP CEN ISO/TR 16060:2014
01-november-2014
1DGRPHãþD
SIST CR 12361:1999
SIST CR 12361:1999/AC:1999
Porušitvene preiskave zvarov na kovinskih materialih - Jedkala za makroskopsko
in mikroskopsko preiskavo (ISO/TR 16060:2003)
Destructive tests on welds in metallic materials - Etchants for macroscopic and
microscopic examination (ISO/TR 16060:2003)
Zerstörende Prüfung von Schweißverbindungen an metallischen Werkstoffen - Ätzungen
für die makroskopische und mikroskopische Untersuchung (ISO/TR 16060:2003)
Essais destructifs des soudures sur matériaux métalliques - Réactifs pour examens
macroscopique et microscopique (ISO/TR 16060:2003)
Ta slovenski standard je istoveten z: CEN ISO/TR 16060:2014
ICS:
25.160.40 Varjeni spoji in vari Welded joints
SIST-TP CEN ISO/TR 16060:2014 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST-TP CEN ISO/TR 16060:2014
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SIST-TP CEN ISO/TR 16060:2014
TECHNICAL REPORT
CEN ISO/TR 16060
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
August 2014
ICS 25.160.40 Supersedes CR 12361:1996
English Version
Destructive tests on welds in metallic materials - Etchants for
macroscopic and microscopic examination (ISO/TR 16060:2003)
Essais destructifs des soudures sur matériaux métalliques - Zerstörende Prüfung von Schweißverbindungen an
Réactifs pour examens macroscopique et microscopique metallischen Werkstoffen - Ätzungen für die
(ISO/TR 16060:2003) makroskopische und mikroskopische Untersuchung
(ISO/TR 16060:2003)
This Technical Report was approved by CEN on 18 August 2014. It has been drawn up by the Technical Committee CEN/TC 121.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2014 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN ISO/TR 16060:2014 E
worldwide for CEN national Members.
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SIST-TP CEN ISO/TR 16060:2014
CEN ISO/TR 16060:2014 (E)
Contents Page
Foreword .3
2
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SIST-TP CEN ISO/TR 16060:2014
CEN ISO/TR 16060:2014 (E)
Foreword
The text of ISO/TR 16060:2003 has been prepared by Technical Committee ISO/TC 44 “Welding and allied
processes” of the International Organization for Standardization (ISO) and has been taken over as CEN
ISO/TR 16060:2014 by Technical Committee CEN/TC 121 “Welding and allied processes” the secretariat of
which is held by DIN.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
This document supersedes CR 12361:1996.
Endorsement notice
The text of ISO/TR 16060:2003 has been approved by CEN as CEN ISO/TR 16060:2014 without any
modification.
3
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SIST-TP CEN ISO/TR 16060:2014
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SIST-TP CEN ISO/TR 16060:2014
TECHNICAL ISO/TR
REPORT 16060
First edition
2003-10-15
Destructive tests on welds in metallic
materials — Etchants for macroscopic
and microscopic examination
Essais destructifs des soudures sur matériaux métalliques — Réactifs
pour examens macroscopique et microscopique
Reference number
ISO/TR 16060:2003(E)
©
ISO 2003
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SIST-TP CEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
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© ISO 2003
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or
ISO's member body in the country of the requester.
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Published in Switzerland
ii © ISO 2003 — All rights reserved
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SIST-TP CEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Contents Page
Foreword. iv
1 Scope. 1
2 Normative references . 1
3 General. 1
4 Etchants for carbon steels and low-alloy steels. 1
5 Etchants for stainless steels . 1
6 Etchants for nickel and nickel alloys . 2
7 Etchants for titanium and titanium alloys . 2
8 Etchants for copper and copper alloys . 2
9 Etchants for aluminium and aluminium alloys . 2
10 Designation. 2
Annex A (informative) Etchants for carbon steels and low-alloy steels. 3
Annex B (informative) Etchants for stainless steels. 10
Annex C (informative) Etchants for nickel and nickel alloys . 16
Annex D (informative) Etchants for titanium and titanium alloys. 18
Annex E (informative) Etchants for copper and copper alloys. 20
Annex F (informative) Etchants for aluminium and aluminium alloys. 22
Annex G (informative) List of etchants. 27
© ISO 2003 — All rights reserved iii
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SIST-TP CEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
In exceptional circumstances, when a technical committee has collected data of a different kind from that
which is normally published as an International Standard (“state of the art”, for example), it may decide by a
simple majority vote of its participating members to publish a Technical Report. A Technical Report is entirely
informative in nature and does not have to be reviewed until the data it provides are considered to be no
longer valid or useful.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO/TR 16060 was prepared by Technical Committee ISO/TC 44, Welding and allied processes,
Subcommittee SC 5, Testing and inspection of welds.
iv © ISO 2003 — All rights reserved
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SIST-TP CEN ISO/TR 16060:2014
TECHNICAL REPORT ISO/TR 16060:2003(E)
Destructive tests on welds in metallic materials — Etchants for
macroscopic and microscopic examination
1 Scope
This Technical Report gives a non-exhaustive list of etchants that can be used for the macroscopic and
microscopic examination of welds in accordance with ISO 17639 for the following groups of materials:
carbon steels and low-alloy steels;
stainless steels;
nickel and nickel alloys;
titanium and titanium alloys;
copper and copper alloys;
aluminium and aluminium alloys.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 17639, Destructive tests on welds in metallic materials — Macroscopic and microscopic examination of
welds
3 General
Where details of concentration or waters of crystallization of reagents are not defined in the annexes, Table 1
is applicable. These values should be confirmed by the suppliers of each etchant.
4 Etchants for carbon steels and low-alloy steels
The etchants for carbon and low alloyed steels are given in Annex A.
5 Etchants for stainless steels
The etchants for stainless steels are given in Annex B.
© ISO 2003 — All rights reserved 1
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6 Etchants for nickel and nickel alloys
The etchants for nickel and nickel alloys are given in Annex C.
7 Etchants for titanium and titanium alloys
The etchants for titanium and titanium alloys are given in Annex D.
8 Etchants for copper and copper alloys
The etchants for copper and copper alloys are given in Annex E.
9 Etchants for aluminium and aluminium alloys
The etchants for aluminium and aluminium alloys are given in Annex F.
10 Designation
Etchants should be designated either by names or by numbers of tables in accordance with Annex G.
Table 1 — Characteristics of components
Components Characteristics
Specific gravity Concentration Hydrate Remarks
3
g/cm %
HCl 1,18 35 to 38 —
1,16 31,5 to 33
HF 1,13 40 —
HNO 1,42 69 —
3
H SO 1,84 98 —
2 4
a
H O — 6 % W/V — Usually 20 volumes
2 2
(i.e. 20 volume available O )
2
H PO 1,70 85 —
3 4
CHCOOH 1,05 99,1 — glacial
3
HBF 1,23 35 —
4
C H O — — 2
2 2 4
FeCl — — 6
3
CuCl — — 2
2
MgCl — — 6
2
Fe(NO ) — — 9
3 3
a
W/V means weight by volume.
2 © ISO 2003 — All rights reserved
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ISO/TR 16060:2003(E)
Annex A
(informative)
Etchants for carbon steels and low-alloy steels
See Tables A.1 to A.13.
Table A.1 — Nital
Type of etchant: Macroscopic and microscopic etchant
Composition in volume and in order of mixing:
99 ml to 95 ml industrial methylated spirits*
1 ml to 5 ml nitric acid (HNO )
3
*Ethyl alcohol (C H OH), denatured with methyl alcohol (CH OH)
2 5 3
Also methyl alcohol or isoamyl alcohol [(CH ) CH(CH ) OH]
3 2 2 2
Safe shelf life: Indefinite
Surface preparation:
600 grit or finer (macroetching ≈ 5 % of nitric acid)
3 µm diamond or finer (microetching ≈ 2 % of nitric acid)
Etching temperature: Ambient
Etching time: A few seconds — check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Can increase strength to 15 % for macroetching on ground surface — reveals ferrite boundaries —
differentiates ferrite from martensite. Good general purpose etchant.
Amyl alcohol is preferable for galvanized steel.
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ISO/TR 16060:2003(E)
Table A.2 — Picral (4 %)
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml ethyl alcohol (C H OH)
2 5
4 g picric acid [C H OH(NO ) ]
6 2 2 3
[+ wetting agent (sodium dodecyl benzene sulphate) (C H NaSO ) if required]
18 29 4
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: Ambient
Etching time: A few seconds — check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Little attack prior austenite boundaries — detects carbides — good resolution with fine pearlite,
martensite, tempered martensite and bainitic structures.
Table A.3 — Picric acid solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
1 l saturated aqueous picric acid [C H OH(NO ) ]
6 2 2 3
10 ml wetting agent (sodium dodecyl benzene sulphate) (C H NaSO )
18 29 4
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: 55 °C to 60 °C
Etching time: A few seconds — check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Reveals prior grain boundaries and segregation.
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ISO/TR 16060:2003(E)
Table A.4 — Picral (15 %)
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml ethyl alcohol* (C H OH)
2 5
15 g picric acid [C H OH(NO ) ]
6 2 2 3
*Also methyl alcohol (CH OH)
3
Safe shelf life: Indefinite
Surface preparation:
2 µm diamond or finer
Etching temperature: Ambient
Etching time: A few seconds to one minute — check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Reveals general structure.
The composition given saturates the solution with picric acid.
Table A.5 — Hydrochloric picric acid solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml ethyl alcohol (C H OH)
2 5
1 ml hydrochloric acid (HCl)
4 g picric acid [C H OH(NO ) ]
6 2 2 3
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: Ambient
Etching time: 10 s to a few minutes
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Microstructural characterization of HAZ, weld and parent metal.
Especially effective for very fine structures. Less effective than Nital for the ferrite grain boundaries.
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Table A.6 — Ammonium peroxodisulphate solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml water (H O)
2
10 g ammonium peroxodisulphate [(NH ) S O ]
4 2 2 8
Safe shelf life: Limited
Surface preparation:
6 µm diamond or finer
Etching temperature: Ambient
Etching time: 2 min to 3 min
Additional precautions/requirements: nil
Comments:
Reveals extent of HAZ.
Microscopic features of multipass welds.
Table A.7 — Alcoholic hydrochloric solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml ethyl alcohol (C H OH)
2 5
1 ml to 5 ml hydrochloric acid (HCl)
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: 40 °C to 50 °C
Etching time: A few seconds to one minute
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Add HCl to C H OH.
2 5
Comments: nil
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Table A.8 — 120/10/30 etchant
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
120 ml ethyl alcohol (C H OH) or methyl alcohol (CH OH)
2 5 3
10 ml iron (III) chloride (FeCl ) (60 % W/V)
3
30 ml hydrochloric acid (HCl)
Safe shelf life: Indefinite
Surface preparation:
2 µm diamond or finer
Etching temperature: Ambient
Etching time: A few seconds by immersion —– check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Good general-purpose etchant.
Table A.9 — Cuprochloric solution 1
Type of etchant: Macroscopic etchant
Composition in volume and in order of mixing:
30 ml water (H O)
2
25 ml ethyl alcohol (C H OH)
2 5
40 ml hydrochloric acid (HCl)
5 g copper (II) chloride (CuCl )
2
Safe shelf life: 2 h
Surface preparation:
1 000 grit or finer
Etching temperature: Ambient
Etching time: 10 s to 20 s
Additional precautions/requirements:
After the etching, the specimen should be washed in order to remove copper deposits.
Usual precautions for handling and disposal of acids.
Comments:
Reveals cold working strain lines.
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Table A.10 — Magneso cuprochloric solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml ethyl alcohol (C H OH)
2 5
20 ml water (H O)
2
1 ml hydrochloric acid (HCl)
4 g magnesium (II) chloride (MgCl )
2
1 g copper (II) chloride (CuCl )
2
Safe shelf life: 2 h
Surface preparation:
3 µm diamond or finer
Etching temperature: Ambient
Etching time: 60 s
Additional precautions/requirements:
Salts should be dissolved in the smallest amount of hot water, then diluted with ethyl alcohol.
A slight polishing (1 µm) after the etching furnishes the best contrast.
Comments:
Reveals phosphorus and related segregations. The copper deposits first of all on those areas
poorest in phosphorus.
Table A.11 — Adler’s etchant
Type of etchant: Macroscopic etchant
Composition in volume and in order of mixing:
25 ml water (H O)
2
.
3 g ammonium tetra chloro diaquo cuprate (II) [(NH ) CuCl 2H O]
4 2 4 2
50 ml hydrochloric acid (HCl)
15 g iron (III) chloride (FeCl )
3
Safe shelf life: Months
Surface preparation:
320 grit or finer
Etching temperature: Ambient
Etching time: 5 s to 10 s
Additional precautions/requirements:
.
Add [(NH ) CuCl 2H O] to H O (a).
4 2 4 2 2
Add FeCl to HCl (b).
3
Mix both then add (b) to (a).
Comments: nil
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Table A.12 — Heyn’s etchant
Type of etchant: Macroscopic etchant
Composition in volume and in order of mixing:
120 ml water (H O)
2
.
10 g ammonium tetra chloro diaquo cuprate (II) [(NH ) CuCl 2H O]
4 2 4 2
Safe shelf life: Months
Surface preparation:
240 grit or finer
Etching temperature: Ambient
Etching time: 10 s to 1 min
Additional precautions/requirements:
.
Add [(NH ) CuCl 2H O] to H O.
4 2 4 2 2
Comments:
Copper deposit shall be removed.
Table A.13 — Ferric chloride solution
Type of etchant: Macroscopic etchant
Composition in volume and in order of mixing:
70 ml water (H O)
2
30 ml iron (III) chloride (FeCl ) (60 % W/V)
3
Safe shelf life: Indefinite.
Surface preparation:
1 000 grit or finer
Etching temperature: Ambient
Etching time: A few seconds
Additional precautions/requirements:
Usual precaution for handling and disposal of acids.
Comments:
1) Swab the surface;
2) Rinse with water;
3) Swab again the surface;
4) After etching, water rinse, alcohol rinse, dry.
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ISO/TR 16060:2003(E)
Annex B
(informative)
Etchants for stainless steels
See Tables B.1 to B.12.
Table B.1 — Oxalic acid solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml water (H O)
2
10 g oxalic acid (ethanedioic acid) (C H O )
2 2 4
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: Ambient
Etching time: A few seconds — check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Electrolytic 2 V to 6 V. Can reveal sensitivity to inter-crystalline corrosion.
Reveals general structure.
Reveals carbides at the grain boundaries.
Table B.2 — Thiocyanate solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
80 ml water (H O)
2
20 ml sulphuric acid (H SO )
2 4
10 g ammonium thiocyanate (NH SCN)
4
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: Ambient
Etching time: A few seconds — check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Electrolytic 1,5 V to 2,0 V.
Good general purpose etchant.
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Table B.3 — Acidified ferric chloride solution
Type of etchant: Macroscopic etchant
Composition in volume and in order of mixing:
480 ml water (H O)
2
120 ml hydrochloric acid (HCl)
50 g iron (III) chloride (FeCl )
3
Safe shelf life: Indefinite
Surface preparation:
600 grit or finer
Etching temperature: Ambient
Etching time: A few seconds to one minute — check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Good general purpose macroscopic etchant, for austenitic chromium nickel and other stainless
steels.
Table B.4 — Modified Murakami's etchant
Type of etchant: Macroscopic etchant
Composition in volume and in order of mixing:
60 ml water (H O)
2
30 g potassium ferricyanide [K Fe(CN) ]
3 6
30 g potassium hydroxide (KOH)
Safe shelf life: Fresh solution
Surface preparation:
1 µm diamond or finer
Etching temperature: Temperature of freshly prepared solution (hot)
Etching time: 20 s to 40 s
Additional precautions/requirements:
Usual precautions for handling and disposal of caustic solutions.
Comments:
Reveals σ phase from δ ferrite and carbides. Austenite matrix is not revealed.
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Table B.5 — Cuprochloric solution 2
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml water(H O)
2
100 ml ethyl alcohol (C H OH)
2 5
100 ml hydrochloric acid (HCl)
5 g copper (II) chloride (CuCl )
2
Safe shelf life: 2 h
Surface preparation:
1 µm diamond or finer
Etching temperature: Ambient
Etching time: 10 s to a few minutes
Additional precautions/requirements:
After etching, the test specimen should be washed in order to remove copper deposits.
Usual precautions for handling and disposal of acids.
Comments:
Especially for ferritic and martensitic stainless steels, an alternative to electrolytic etching.
Less effective for austenitic grain boundaries that can be attacked using longer etching times. Not
effective for carbides.
Table B.6 — Chromic acid solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml water (H O)
2
10 g chromium (VI) oxide (CrO )
3
Safe shelf life: A few days
Surface preparation:
1 µm diamond or finer
Etching temperature: Ambient
Etching time: 10 s to 1 min
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Austenitic grain boundaries. Distinguishes σ phase and carbides.
Electrolytic etching (3 V) for general purpose etchings. For the analysis of carbides, the etching is
carried out in two steps: first with 1 V and afterwards with 3 V.
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Table B.7 — Alcoholic hydrochloric solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml ethyl alcohol (C H OH)
2 5
1 ml to 5 ml hydrochloric acid (HCl)
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: 40 °C to 50 °C
Etching time: A few seconds to one minute
Additional precautions/requirements:
Add HCl to C H OH.
2 5
Usual precaution for handling and disposal of acids.
Comments: nil
Table B.8 — Hydrochloric nitric acid solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
39 ml water (H O)
2
52 ml hydrochloric acid (HCl)
9 ml nitric acid (HNO ), (concentration 65 %)
3
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: Ambient
Etching time: A few seconds to a few minutes
Additional precautions/requirements:
Always add HCl and HNO to H O.
3 2
Usual precautions for handling and disposal of acids.
Comments: nil
© ISO 2003 — All rights reserved 13
---------------------- Page: 23 ----------------------
SIST-TP CEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Table B.9 — Adler’s etchant
Type of etchant: Macroscopic etchant
Composition in volume and in order of mixing:
25 ml water (H O)
2
.
3 g ammonium tetra chloro diaquo cuprate (II) [(NH ) CuCl 2H O]
4 2 4 2
50 ml hydrochloric acid (HCl)
15 g iron (III) chloride (FeCl )
3
Safe shelf life: Months
Surface preparation:
320 grit or finer.
Etching temperature: Ambient
Etching time: 5 s to 10 s
Additional precautions/requirements:
.
Add [(NH ) CuCl 2H O to H O] (a).
4 2 4 2 2
Add FeCl to HCl (b).
3
Mix both then add (b) to (a).
Comments: nil
Table B.10 — Fluonitric acid solution 1
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
50 ml nitric acid (HNO )
3
50 ml hydrofluoric acid (HF)
Safe shelf life: Do not store after using.
Surface preparation:
2 µm diamond or finer
Etching temperature: Ambient
Etching time: 5 min to 30 min by immersion
Additional precautions/requirements:
CAUTION: When handling HF wear hand and eye protection. In the event of bodily contact,
wash off skin immediately and seek medical advice.
Use receptacles in plastic.
Usual precautions for handling and disposal of acids.
Comments:
Reveals general structure.
14 © ISO 2003 — All rights reserved
---------------------- Page: 24 ----------------------
SIST-TP CEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Table B.11 — Fluonitric acid solution 2
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml water (H O)
2
100 ml nitric acid (HNO )
3
100 ml hydrofluoric acid (HF)
Safe shelf life: Do not store after using.
Surface preparation:
2 µm diamond or finer
Etching temperature: Ambient
Etching time: 1 min to 15 min by immersion
Additional precautions/requirements:
CAUTION: When handling HF wear hand and eye protection. In the event of bodily contact,
wash off skin immediately and seek medical advice.
Use receptacles in plastic.
Usual precautions for handling and disposal of acids.
Comments:
Reveals grain boundaries.
Table B.12 — Nitric acid solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
50 ml water (H O)
2
50 ml nitric acid (HNO )
3
Safe shelf life: Indefinit
...
SLOVENSKI STANDARD
kSIST-TP FprCEN ISO/TR 16060:2014
01-junij-2014
Porušitveni preskusi zvarov na kovinskih materialih - Jedkala za makroskopsko in
mikroskopsko preiskavo (ISO/TR 16060:2003)
Destructive tests on welds in metallic materials - Etchants for macroscopic and
microscopic examination (ISO/TR 16060:2003)
Essais destructifs des soudures sur matériaux métalliques - Réactifs pour examens
macroscopique et microscopique (ISO/TR 16060:2003)
Ta slovenski standard je istoveten z: FprCEN ISO/TR 16060
ICS:
25.160.40 Varjeni spoji in vari Welded joints
kSIST-TP FprCEN ISO/TR 16060:2014 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
---------------------- Page: 2 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
TECHNICAL REPORT
FINAL DRAFT
FprCEN ISO/TR 16060
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
April 2014
ICS 25.160.40 Will supersede CR 12361:1996
English Version
Destructive tests on welds in metallic materials - Etchants for
macroscopic and microscopic examination (ISO/TR 16060:2003)
Essais destructifs des soudures sur matériaux métalliques - Zerstörende Prüfung von Schweißverbindungen an
Réactifs pour examens macroscopique et microscopique metallischen Werkstoffen - Ätzungen für die
(ISO/TR 16060:2003) makroskopische und mikroskopische Untersuchung (ISO/
DTR 16060:2014)
This draft Technical Report is submitted to CEN members for Technical Committee Approval. It has been drawn up by the Technical
Committee CEN/TC 121.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are aware and to
provide supporting documentation.
Warning : This document is not a Technical Report. It is distributed for review and comments. It is subject to change without notice and
shall not be referred to as a Technical Report.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2014 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprCEN ISO/TR 16060:2014 E
worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
FprCEN ISO/TR 16060:2014 (E)
Contents
Page
Foreword .3
2
---------------------- Page: 4 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
FprCEN ISO/TR 16060:2014 (E)
Foreword
The text of ISO/TR 16060:2003 has been prepared by Technical Committee ISO/TC 44 “Welding and allied
processes” of the International Organization for Standardization (ISO) and has been taken over as FprCEN
ISO/TR 16060:2014 by Technical Committee CEN/TC 121 “Welding and allied processes” the secretariat of
which is held by DIN.
This document is currently submitted to the Technical Committee Approval.
This document will supersede CR 12361:1996.
Endorsement notice
The text of ISO/TR 16060:2003 has been approved by CEN as FprCEN ISO/TR 16060:2014 without any
modification.
3
---------------------- Page: 5 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
---------------------- Page: 6 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
TECHNICAL ISO/TR
REPORT 16060
First edition
2003-10-15
Destructive tests on welds in metallic
materials — Etchants for macroscopic
and microscopic examination
Essais destructifs des soudures sur matériaux métalliques — Réactifs
pour examens macroscopique et microscopique
Reference number
ISO/TR 16060:2003(E)
©
ISO 2003
---------------------- Page: 7 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
© ISO 2003
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or
ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2003 — All rights reserved
---------------------- Page: 8 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Contents Page
Foreword. iv
1 Scope. 1
2 Normative references . 1
3 General. 1
4 Etchants for carbon steels and low-alloy steels. 1
5 Etchants for stainless steels . 1
6 Etchants for nickel and nickel alloys . 2
7 Etchants for titanium and titanium alloys . 2
8 Etchants for copper and copper alloys . 2
9 Etchants for aluminium and aluminium alloys . 2
10 Designation. 2
Annex A (informative) Etchants for carbon steels and low-alloy steels. 3
Annex B (informative) Etchants for stainless steels. 10
Annex C (informative) Etchants for nickel and nickel alloys . 16
Annex D (informative) Etchants for titanium and titanium alloys. 18
Annex E (informative) Etchants for copper and copper alloys. 20
Annex F (informative) Etchants for aluminium and aluminium alloys. 22
Annex G (informative) List of etchants. 27
© ISO 2003 — All rights reserved iii
---------------------- Page: 9 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
In exceptional circumstances, when a technical committee has collected data of a different kind from that
which is normally published as an International Standard (“state of the art”, for example), it may decide by a
simple majority vote of its participating members to publish a Technical Report. A Technical Report is entirely
informative in nature and does not have to be reviewed until the data it provides are considered to be no
longer valid or useful.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO/TR 16060 was prepared by Technical Committee ISO/TC 44, Welding and allied processes,
Subcommittee SC 5, Testing and inspection of welds.
iv © ISO 2003 — All rights reserved
---------------------- Page: 10 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
TECHNICAL REPORT ISO/TR 16060:2003(E)
Destructive tests on welds in metallic materials — Etchants for
macroscopic and microscopic examination
1 Scope
This Technical Report gives a non-exhaustive list of etchants that can be used for the macroscopic and
microscopic examination of welds in accordance with ISO 17639 for the following groups of materials:
carbon steels and low-alloy steels;
stainless steels;
nickel and nickel alloys;
titanium and titanium alloys;
copper and copper alloys;
aluminium and aluminium alloys.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 17639, Destructive tests on welds in metallic materials — Macroscopic and microscopic examination of
welds
3 General
Where details of concentration or waters of crystallization of reagents are not defined in the annexes, Table 1
is applicable. These values should be confirmed by the suppliers of each etchant.
4 Etchants for carbon steels and low-alloy steels
The etchants for carbon and low alloyed steels are given in Annex A.
5 Etchants for stainless steels
The etchants for stainless steels are given in Annex B.
© ISO 2003 — All rights reserved 1
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kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
6 Etchants for nickel and nickel alloys
The etchants for nickel and nickel alloys are given in Annex C.
7 Etchants for titanium and titanium alloys
The etchants for titanium and titanium alloys are given in Annex D.
8 Etchants for copper and copper alloys
The etchants for copper and copper alloys are given in Annex E.
9 Etchants for aluminium and aluminium alloys
The etchants for aluminium and aluminium alloys are given in Annex F.
10 Designation
Etchants should be designated either by names or by numbers of tables in accordance with Annex G.
Table 1 — Characteristics of components
Components Characteristics
Specific gravity Concentration Hydrate Remarks
3
g/cm %
HCl 1,18 35 to 38 —
1,16 31,5 to 33
HF 1,13 40 —
HNO 1,42 69 —
3
H SO 1,84 98 —
2 4
a
H O — 6 % W/V — Usually 20 volumes
2 2
(i.e. 20 volume available O )
2
H PO 1,70 85 —
3 4
CHCOOH 1,05 99,1 — glacial
3
HBF 1,23 35 —
4
C H O — — 2
2 2 4
FeCl — — 6
3
CuCl — — 2
2
MgCl — — 6
2
Fe(NO ) — — 9
3 3
a
W/V means weight by volume.
2 © ISO 2003 — All rights reserved
---------------------- Page: 12 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Annex A
(informative)
Etchants for carbon steels and low-alloy steels
See Tables A.1 to A.13.
Table A.1 — Nital
Type of etchant: Macroscopic and microscopic etchant
Composition in volume and in order of mixing:
99 ml to 95 ml industrial methylated spirits*
1 ml to 5 ml nitric acid (HNO )
3
*Ethyl alcohol (C H OH), denatured with methyl alcohol (CH OH)
2 5 3
Also methyl alcohol or isoamyl alcohol [(CH ) CH(CH ) OH]
3 2 2 2
Safe shelf life: Indefinite
Surface preparation:
600 grit or finer (macroetching ≈ 5 % of nitric acid)
3 µm diamond or finer (microetching ≈ 2 % of nitric acid)
Etching temperature: Ambient
Etching time: A few seconds — check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Can increase strength to 15 % for macroetching on ground surface — reveals ferrite boundaries —
differentiates ferrite from martensite. Good general purpose etchant.
Amyl alcohol is preferable for galvanized steel.
© ISO 2003 — All rights reserved 3
---------------------- Page: 13 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Table A.2 — Picral (4 %)
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml ethyl alcohol (C H OH)
2 5
4 g picric acid [C H OH(NO ) ]
6 2 2 3
[+ wetting agent (sodium dodecyl benzene sulphate) (C H NaSO ) if required]
18 29 4
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: Ambient
Etching time: A few seconds — check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Little attack prior austenite boundaries — detects carbides — good resolution with fine pearlite,
martensite, tempered martensite and bainitic structures.
Table A.3 — Picric acid solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
1 l saturated aqueous picric acid [C H OH(NO ) ]
6 2 2 3
10 ml wetting agent (sodium dodecyl benzene sulphate) (C H NaSO )
18 29 4
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: 55 °C to 60 °C
Etching time: A few seconds — check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Reveals prior grain boundaries and segregation.
4 © ISO 2003 — All rights reserved
---------------------- Page: 14 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Table A.4 — Picral (15 %)
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml ethyl alcohol* (C H OH)
2 5
15 g picric acid [C H OH(NO ) ]
6 2 2 3
*Also methyl alcohol (CH OH)
3
Safe shelf life: Indefinite
Surface preparation:
2 µm diamond or finer
Etching temperature: Ambient
Etching time: A few seconds to one minute — check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Reveals general structure.
The composition given saturates the solution with picric acid.
Table A.5 — Hydrochloric picric acid solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml ethyl alcohol (C H OH)
2 5
1 ml hydrochloric acid (HCl)
4 g picric acid [C H OH(NO ) ]
6 2 2 3
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: Ambient
Etching time: 10 s to a few minutes
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Microstructural characterization of HAZ, weld and parent metal.
Especially effective for very fine structures. Less effective than Nital for the ferrite grain boundaries.
© ISO 2003 — All rights reserved 5
---------------------- Page: 15 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Table A.6 — Ammonium peroxodisulphate solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml water (H O)
2
10 g ammonium peroxodisulphate [(NH ) S O ]
4 2 2 8
Safe shelf life: Limited
Surface preparation:
6 µm diamond or finer
Etching temperature: Ambient
Etching time: 2 min to 3 min
Additional precautions/requirements: nil
Comments:
Reveals extent of HAZ.
Microscopic features of multipass welds.
Table A.7 — Alcoholic hydrochloric solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml ethyl alcohol (C H OH)
2 5
1 ml to 5 ml hydrochloric acid (HCl)
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: 40 °C to 50 °C
Etching time: A few seconds to one minute
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Add HCl to C H OH.
2 5
Comments: nil
6 © ISO 2003 — All rights reserved
---------------------- Page: 16 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Table A.8 — 120/10/30 etchant
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
120 ml ethyl alcohol (C H OH) or methyl alcohol (CH OH)
2 5 3
10 ml iron (III) chloride (FeCl ) (60 % W/V)
3
30 ml hydrochloric acid (HCl)
Safe shelf life: Indefinite
Surface preparation:
2 µm diamond or finer
Etching temperature: Ambient
Etching time: A few seconds by immersion —– check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Good general-purpose etchant.
Table A.9 — Cuprochloric solution 1
Type of etchant: Macroscopic etchant
Composition in volume and in order of mixing:
30 ml water (H O)
2
25 ml ethyl alcohol (C H OH)
2 5
40 ml hydrochloric acid (HCl)
5 g copper (II) chloride (CuCl )
2
Safe shelf life: 2 h
Surface preparation:
1 000 grit or finer
Etching temperature: Ambient
Etching time: 10 s to 20 s
Additional precautions/requirements:
After the etching, the specimen should be washed in order to remove copper deposits.
Usual precautions for handling and disposal of acids.
Comments:
Reveals cold working strain lines.
© ISO 2003 — All rights reserved 7
---------------------- Page: 17 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Table A.10 — Magneso cuprochloric solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml ethyl alcohol (C H OH)
2 5
20 ml water (H O)
2
1 ml hydrochloric acid (HCl)
4 g magnesium (II) chloride (MgCl )
2
1 g copper (II) chloride (CuCl )
2
Safe shelf life: 2 h
Surface preparation:
3 µm diamond or finer
Etching temperature: Ambient
Etching time: 60 s
Additional precautions/requirements:
Salts should be dissolved in the smallest amount of hot water, then diluted with ethyl alcohol.
A slight polishing (1 µm) after the etching furnishes the best contrast.
Comments:
Reveals phosphorus and related segregations. The copper deposits first of all on those areas
poorest in phosphorus.
Table A.11 — Adler’s etchant
Type of etchant: Macroscopic etchant
Composition in volume and in order of mixing:
25 ml water (H O)
2
.
3 g ammonium tetra chloro diaquo cuprate (II) [(NH ) CuCl 2H O]
4 2 4 2
50 ml hydrochloric acid (HCl)
15 g iron (III) chloride (FeCl )
3
Safe shelf life: Months
Surface preparation:
320 grit or finer
Etching temperature: Ambient
Etching time: 5 s to 10 s
Additional precautions/requirements:
.
Add [(NH ) CuCl 2H O] to H O (a).
4 2 4 2 2
Add FeCl to HCl (b).
3
Mix both then add (b) to (a).
Comments: nil
8 © ISO 2003 — All rights reserved
---------------------- Page: 18 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Table A.12 — Heyn’s etchant
Type of etchant: Macroscopic etchant
Composition in volume and in order of mixing:
120 ml water (H O)
2
.
10 g ammonium tetra chloro diaquo cuprate (II) [(NH ) CuCl 2H O]
4 2 4 2
Safe shelf life: Months
Surface preparation:
240 grit or finer
Etching temperature: Ambient
Etching time: 10 s to 1 min
Additional precautions/requirements:
.
Add [(NH ) CuCl 2H O] to H O.
4 2 4 2 2
Comments:
Copper deposit shall be removed.
Table A.13 — Ferric chloride solution
Type of etchant: Macroscopic etchant
Composition in volume and in order of mixing:
70 ml water (H O)
2
30 ml iron (III) chloride (FeCl ) (60 % W/V)
3
Safe shelf life: Indefinite.
Surface preparation:
1 000 grit or finer
Etching temperature: Ambient
Etching time: A few seconds
Additional precautions/requirements:
Usual precaution for handling and disposal of acids.
Comments:
1) Swab the surface;
2) Rinse with water;
3) Swab again the surface;
4) After etching, water rinse, alcohol rinse, dry.
© ISO 2003 — All rights reserved 9
---------------------- Page: 19 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Annex B
(informative)
Etchants for stainless steels
See Tables B.1 to B.12.
Table B.1 — Oxalic acid solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml water (H O)
2
10 g oxalic acid (ethanedioic acid) (C H O )
2 2 4
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: Ambient
Etching time: A few seconds — check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Electrolytic 2 V to 6 V. Can reveal sensitivity to inter-crystalline corrosion.
Reveals general structure.
Reveals carbides at the grain boundaries.
Table B.2 — Thiocyanate solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
80 ml water (H O)
2
20 ml sulphuric acid (H SO )
2 4
10 g ammonium thiocyanate (NH SCN)
4
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: Ambient
Etching time: A few seconds — check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Electrolytic 1,5 V to 2,0 V.
Good general purpose etchant.
10 © ISO 2003 — All rights reserved
---------------------- Page: 20 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Table B.3 — Acidified ferric chloride solution
Type of etchant: Macroscopic etchant
Composition in volume and in order of mixing:
480 ml water (H O)
2
120 ml hydrochloric acid (HCl)
50 g iron (III) chloride (FeCl )
3
Safe shelf life: Indefinite
Surface preparation:
600 grit or finer
Etching temperature: Ambient
Etching time: A few seconds to one minute — check by eye
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Good general purpose macroscopic etchant, for austenitic chromium nickel and other stainless
steels.
Table B.4 — Modified Murakami's etchant
Type of etchant: Macroscopic etchant
Composition in volume and in order of mixing:
60 ml water (H O)
2
30 g potassium ferricyanide [K Fe(CN) ]
3 6
30 g potassium hydroxide (KOH)
Safe shelf life: Fresh solution
Surface preparation:
1 µm diamond or finer
Etching temperature: Temperature of freshly prepared solution (hot)
Etching time: 20 s to 40 s
Additional precautions/requirements:
Usual precautions for handling and disposal of caustic solutions.
Comments:
Reveals σ phase from δ ferrite and carbides. Austenite matrix is not revealed.
© ISO 2003 — All rights reserved 11
---------------------- Page: 21 ----------------------
kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Table B.5 — Cuprochloric solution 2
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml water(H O)
2
100 ml ethyl alcohol (C H OH)
2 5
100 ml hydrochloric acid (HCl)
5 g copper (II) chloride (CuCl )
2
Safe shelf life: 2 h
Surface preparation:
1 µm diamond or finer
Etching temperature: Ambient
Etching time: 10 s to a few minutes
Additional precautions/requirements:
After etching, the test specimen should be washed in order to remove copper deposits.
Usual precautions for handling and disposal of acids.
Comments:
Especially for ferritic and martensitic stainless steels, an alternative to electrolytic etching.
Less effective for austenitic grain boundaries that can be attacked using longer etching times. Not
effective for carbides.
Table B.6 — Chromic acid solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml water (H O)
2
10 g chromium (VI) oxide (CrO )
3
Safe shelf life: A few days
Surface preparation:
1 µm diamond or finer
Etching temperature: Ambient
Etching time: 10 s to 1 min
Additional precautions/requirements:
Usual precautions for handling and disposal of acids.
Comments:
Austenitic grain boundaries. Distinguishes σ phase and carbides.
Electrolytic etching (3 V) for general purpose etchings. For the analysis of carbides, the etching is
carried out in two steps: first with 1 V and afterwards with 3 V.
12 © ISO 2003 — All rights reserved
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kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Table B.7 — Alcoholic hydrochloric solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml ethyl alcohol (C H OH)
2 5
1 ml to 5 ml hydrochloric acid (HCl)
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: 40 °C to 50 °C
Etching time: A few seconds to one minute
Additional precautions/requirements:
Add HCl to C H OH.
2 5
Usual precaution for handling and disposal of acids.
Comments: nil
Table B.8 — Hydrochloric nitric acid solution
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
39 ml water (H O)
2
52 ml hydrochloric acid (HCl)
9 ml nitric acid (HNO ), (concentration 65 %)
3
Safe shelf life: Indefinite
Surface preparation:
3 µm diamond or finer
Etching temperature: Ambient
Etching time: A few seconds to a few minutes
Additional precautions/requirements:
Always add HCl and HNO to H O.
3 2
Usual precautions for handling and disposal of acids.
Comments: nil
© ISO 2003 — All rights reserved 13
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kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Table B.9 — Adler’s etchant
Type of etchant: Macroscopic etchant
Composition in volume and in order of mixing:
25 ml water (H O)
2
.
3 g ammonium tetra chloro diaquo cuprate (II) [(NH ) CuCl 2H O]
4 2 4 2
50 ml hydrochloric acid (HCl)
15 g iron (III) chloride (FeCl )
3
Safe shelf life: Months
Surface preparation:
320 grit or finer.
Etching temperature: Ambient
Etching time: 5 s to 10 s
Additional precautions/requirements:
.
Add [(NH ) CuCl 2H O to H O] (a).
4 2 4 2 2
Add FeCl to HCl (b).
3
Mix both then add (b) to (a).
Comments: nil
Table B.10 — Fluonitric acid solution 1
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
50 ml nitric acid (HNO )
3
50 ml hydrofluoric acid (HF)
Safe shelf life: Do not store after using.
Surface preparation:
2 µm diamond or finer
Etching temperature: Ambient
Etching time: 5 min to 30 min by immersion
Additional precautions/requirements:
CAUTION: When handling HF wear hand and eye protection. In the event of bodily contact,
wash off skin immediately and seek medical advice.
Use receptacles in plastic.
Usual precautions for handling and disposal of acids.
Comments:
Reveals general structure.
14 © ISO 2003 — All rights reserved
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kSIST-TP FprCEN ISO/TR 16060:2014
ISO/TR 16060:2003(E)
Table B.11 — Fluonitric acid solution 2
Type of etchant: Microscopic etchant
Composition in volume and in order of mixing:
100 ml water (H O)
2
100 ml nitric acid (HNO )
3
100 ml hydrofluoric acid (HF)
Safe shelf life: Do not store after using.
Surface preparation:
2 µm diamond or finer
Etching temperature: Ambient
Etching time: 1 min to 15 min by immersion
Additional precautions/requirements:
CAUTION: When handling HF wear hand and eye protection. In the event of bodily contact,
wash off skin immediately and seek medical advice.
Use receptacles in plastic.
Usual precautions for handling and disposal of acids.
Comments:
Reveals grain boundaries.
Table B.1
...
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