1、BSI Standards Publication Destructive tests on welds in metallic materials Etchants for macroscopic and microscopic examination PD CEN ISO/TR 16060:2014National foreword This Published Document is the UK implementation of CEN ISO/TR 16060:2014. It is identical to ISO/TR 16060:2003. It supersedes PD
2、6604:1997 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee WEE/2, Destructive Testing of Welds. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the nece
3、ssary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2014. Published by BSI Standards Limited 2014 ISBN 978 0 580 85861 1 ICS 25.160.40 Compliance with a British Standard cannot confer immunity from legal obligations. This Published Doc
4、ument was published under the authority of the Standards Policy and Strategy Committee on 31 August 2014. Amendments/corrigenda issued since publication Date Text affected PUBLISHED DOCUMENT PD CEN ISO/TR 16060:2014 TECHNICAL REPORT RAPPORT TECHNIQUE TECHNISCHER BERICHT CEN ISO/TR 16060 August 2014
5、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 matriaux mtalliques - Ractifs pour examens macroscopique et microscopique (ISO/TR 1606
6、0:2003) Zerstrende Prfung von Schweiverbindungen an metallischen Werkstoffen - tzungen fr die 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 th
7、e 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, Romani
8、a, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by a
9、ny means reserved worldwide for CEN national Members. Ref. No. CEN ISO/TR 16060:2014 E PD CEN ISO/TR 16060:2014CEN ISO/TR 16060:2014 (E) 2 Contents Page Foreword 3 PD CEN ISO/TR 16060:2014CEN ISO/TR 16060:2014 (E) 3 Foreword The text of ISO/TR 16060:2003 has been prepared by Technical Committee ISO/
10、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
11、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:
12、2014 without any modification. PD CEN ISO/TR 16060:2014ISO/TR 16060:2003(E) ISO 2003 All rights reserved iiiContents Page 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
13、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 (informa
14、tive) 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 PD CEN IS
15、O/TR 16060:2014TECHNICAL REPORT ISO/TR 16060:2003(E) ISO 2003 All rights reserved 1Destructive 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 micr
16、oscopic 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 followin
17、g 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 M
18、acroscopic 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 steel
19、s 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. PD CEN ISO/TR 16060:2014ISO/TR 16060:2003(E) 2 ISO 2003 All rights reserved6 Etchants for nickel and nickel alloys The etchants for nickel an
20、d 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
21、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 g/cm 3Concentration % Hydrate Remar
22、ks HCl 1,18 1,16 35 to 38 31,5 to 33 HF 1,13 40 HNO 31,42 69 H 2 SO 41,84 98 H 2 O 2 6 % W/V a Usually 20 volumes (i.e. 20 volume available O 2 ) H 3 PO 41,70 85 CH 3 COOH 1,05 99,1 glacial HBF 41,23 35 C 2 H 2 O 4 2 FeCl 3 6 CuCl 2 2 MgCl 2 6 Fe(NO 3 ) 3 9 a W/V means weight by volume. PD CEN ISO/T
23、R 16060:2014ISO/TR 16060:2003(E) ISO 2003 All rights reserved 3Annex 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 me
24、thylated spirits* 1 ml to 5 ml nitric acid (HNO 3 ) *Ethyl alcohol (C 2 H 5 OH), denatured with methyl alcohol (CH 3 OH) Also methyl alcohol or isoamyl alcohol (CH 3 ) 2 CH(CH 2 ) 2 OH Safe shelf life: Indefinite Surface preparation: 600 grit or finer (macroetching 5 % of nitric acid) 3 m diamond or
25、 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 boundar
26、ies differentiates ferrite from martensite. Good general purpose etchant. Amyl alcohol is preferable for galvanized steel. PD CEN ISO/TR 16060:2014ISO/TR 16060:2003(E) 4 ISO 2003 All rights reservedTable A.2 Picral (4 %) Type of etchant: Microscopic etchant Composition in volume and in order of mixi
27、ng: 100 ml ethyl alcohol (C 2 H 5 OH) 4 g picric acid C 6 H 2 OH(NO 2 ) 3 + wetting agent (sodium dodecyl benzene sulphate) (C 18 H 29 NaSO 4 ) if required Safe shelf life: Indefinite Surface preparation: 3 m diamond or finer Etching temperature: Ambient Etching time: A few seconds check by eye Addi
28、tional 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: Micr
29、oscopic etchant Composition in volume and in order of mixing: 1 l saturated aqueous picric acid C 6 H 2 OH(NO 2 ) 3 10 ml wetting agent (sodium dodecyl benzene sulphate) (C 18 H 29 NaSO 4 ) Safe shelf life: Indefinite Surface preparation: 3 m diamond or finer Etching temperature: 55 C to 60 C Etchin
30、g 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. PD CEN ISO/TR 16060:2014ISO/TR 16060:2003(E) ISO 2003 All rights reserved 5Table A.4 Picral (15 %) Type of etchant:
31、Microscopic etchant Composition in volume and in order of mixing: 100 ml ethyl alcohol* (C 2 H 5 OH) 15 g picric acid C 6 H 2 OH(NO 2 ) 3 *Also methyl alcohol (CH 3 OH) Safe shelf life: Indefinite Surface preparation: 2 m diamond or finer Etching temperature: Ambient Etching time: A few seconds to o
32、ne 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 Compo
33、sition in volume and in order of mixing: 100 ml ethyl alcohol (C 2 H 5 OH) 1 ml hydrochloric acid (HCl) 4 g picric acid C 6 H 2 OH(NO 2 ) 3 Safe shelf life: Indefinite Surface preparation: 3 m diamond or finer Etching temperature: Ambient Etching time: 10 s to a few minutes Additional precautions/re
34、quirements: 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. PD CEN ISO/TR 16060:2014ISO/TR 16060:2003(E) 6 ISO 20
35、03 All rights reservedTable A.6 Ammonium peroxodisulphate solution Type of etchant: Microscopic etchant Composition in volume and in order of mixing: 100 ml water (H 2 O) 10 g ammonium peroxodisulphate (NH 4 ) 2 S 2 O 8 Safe shelf life: Limited Surface preparation: 6 m diamond or finer Etching tempe
36、rature: 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 al
37、cohol (C 2 H 5 OH) 1 ml to 5 ml hydrochloric acid (HCl) Safe shelf life: Indefinite Surface preparation: 3 m 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
38、 to C 2 H 5 OH. Comments: nil PD CEN ISO/TR 16060:2014ISO/TR 16060:2003(E) ISO 2003 All rights reserved 7Table A.8 120/10/30 etchant Type of etchant: Microscopic etchant Composition in volume and in order of mixing: 120 ml ethyl alcohol (C 2 H 5 OH) or methyl alcohol (CH 3 OH) 10 ml iron (III) chlor
39、ide (FeCl 3 ) (60 % W/V) 30 ml hydrochloric acid (HCl) Safe shelf life: Indefinite Surface preparation: 2 m 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. C
40、omments: 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 2 O) 25 ml ethyl alcohol (C 2 H 5 OH) 40 ml hydrochloric acid (HCl) 5 g copper (II) chloride (CuCl 2 ) Safe shelf life: 2 h Surfa
41、ce 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 s
42、train lines. PD CEN ISO/TR 16060:2014ISO/TR 16060:2003(E) 8 ISO 2003 All rights reservedTable A.10 Magneso cuprochloric solution Type of etchant: Microscopic etchant Composition in volume and in order of mixing: 100 ml ethyl alcohol (C 2 H 5 OH) 20 ml water (H 2 O) 1 ml hydrochloric acid (HCl) 4 g m
43、agnesium (II) chloride (MgCl 2 ) 1 g copper (II) chloride (CuCl 2 ) Safe shelf life: 2 h Surface preparation: 3 m 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 eth
44、yl alcohol. A slight polishing (1 m) 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 Adlers etchant Type of etchant: Macroscopic etchant Composition in volume and i
45、n order of mixing: 25 ml water (H 2 O) 3 g ammonium tetra chloro diaquo cuprate (II) (NH 4 ) 2 CuCl 4 . 2H 2 O 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 Additi
46、onal precautions/requirements: Add (NH 4 ) 2 CuCl 4 . 2H 2 O to H 2 O (a). Add FeCl 3to HCl (b). Mix both then add (b) to (a). Comments: nil PD CEN ISO/TR 16060:2014ISO/TR 16060:2003(E) ISO 2003 All rights reserved 9Table A.12 Heyns etchant Type of etchant: Macroscopic etchant Composition in volume
47、and in order of mixing: 120 ml water (H 2 O) 10 g ammonium tetra chloro diaquo cuprate (II) (NH 4 ) 2 CuCl 4 . 2H 2 O 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 4 ) 2 CuCl 4 . 2H
48、 2 O to H 2 O. 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 2 O) 30 ml iron (III) chloride (FeCl 3 ) (60 % W/V) Safe shelf life: Indefinite. Surface preparation: 1 000
49、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. PD CEN ISO/TR 16060:2014ISO/TR 16060:2003(E) 10 ISO 2003 All rights reservedAnnex B (informative) Et
