1、BSI Standards PublicationDestructive tests on welds in metallic materials Etchants for macroscopic and microscopic examinationPD CEN ISO/TR 16060:2014National forewordThis Published Document is the UK implementation of CEN ISO/TR16060:2014. It is identical to ISO/TR 16060:2003. It supersedes PD 6604
2、:1997 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee WEE/2, Destructive Testing of Welds.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary pro
3、visions ofa contract. Users are responsible for its correct application. The British Standards Institution 2014.Published by BSI Standards Limited 2014ISBN 978 0 580 85861 1ICS 25.160.40Compliance with a British Standard cannot confer immunity fromlegal obligations.This Published Document was publis
4、hed under the authority of theStandards Policy and Strategy Committee on 31 August 2014.Amendments/corrigenda issued since publicationDate Text affectedPUBLISHED DOCUMENTPD CEN ISO/TR 16060:2014TECHNICAL REPORT RAPPORT TECHNIQUE TECHNISCHER BERICHT CEN ISO/TR 16060 August 2014 ICS 25.160.40 Supersed
5、es CR 12361:1996English 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 16060:2003) Zerstrende Prfun
6、g 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 the national standards bod
7、ies 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, S
8、pain, 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 any means reserved worldw
9、ide for CEN national Members. Ref. No. CEN ISO/TR 16060:2014 EPD 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/TC 44 “Welding and allied
10、 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 d
11、ocument 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 modifica
12、tion. 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 2 7 Etchants for titanium
13、 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
14、 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 ISO/TR 16060:2014TECHNICAL
15、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 microscopic examination of we
16、lds 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 ar
17、e 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 microscopi
18、c 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
19、 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 and nickel alloys are given
20、 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 aluminiu
21、m 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/cm3Concentration % Hydrate Remarks HCl 1,18 1,16 35 to 38
22、31,5 to 33 HF 1,13 40 HNO31,42 69 H2SO41,84 98 H2O2 6 % W/V a Usually 20 volumes (i.e. 20 volume available O2) H3PO41,70 85 CH3COOH 1,05 99,1 glacial HBF41,23 35 C2H2O4 2 FeCl3 6 CuCl2 2 MgCl2 6 Fe(NO3)3 9 a W/V means weight by volume. PD CEN ISO/TR 16060:2014ISO/TR 16060:2003(E) ISO 2003 All rights
23、 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 methylated spirits* 1 ml to 5 ml nitric acid (HNO3) *E
24、thyl alcohol (C2H5OH), denatured with methyl alcohol (CH3OH) Also methyl alcohol or isoamyl alcohol (CH3)2CH(CH2)2OH Safe shelf life: Indefinite Surface preparation: 600 grit or finer (macroetching 5 % of nitric acid) 3 m diamond or finer (microetching 2 % of nitric acid) Etching temperature: Ambien
25、t 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 etc
26、hant. 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 mixing: 100 ml ethyl alcohol (C2H5OH) 4 g picric acid C6H2OH(NO2)3 + wet
27、ting agent (sodium dodecyl benzene sulphate) (C18H29NaSO4) if required Safe shelf life: Indefinite Surface preparation: 3 m 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
28、. 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 p
29、icric acid C6H2OH(NO2)3 10 ml wetting agent (sodium dodecyl benzene sulphate) (C18H29NaSO4) Safe shelf life: Indefinite Surface preparation: 3 m diamond or finer Etching temperature: 55 C to 60 C Etching time: A few seconds check by eye Additional precautions/requirements: Usual precautions for hand
30、ling 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: Microscopic etchant Composition in volume and in order of mixing: 100 ml ethyl alcohol* (C2H5OH) 1
31、5 g picric acid C6H2OH(NO2)3 *Also methyl alcohol (CH3OH) Safe shelf life: Indefinite Surface preparation: 2 m 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 acid
32、s. 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 (C2H5OH) 1 ml hydrochloric acid (HCl) 4 g picric
33、acid C6H2OH(NO2)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/requirements: Usual precautions for handling and disposal of acids. Comments: Microstructural characterization of HAZ, weld
34、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 2003 All rights reservedTable A.6 Ammonium peroxodisulphate solution Type of etchant: Microscopic etchant Composition in vol
35、ume and in order of mixing: 100 ml water (H2O) 10 g ammonium peroxodisulphate (NH4)2S2O8 Safe shelf life: Limited Surface preparation: 6 m diamond or finer Etching temperature: Ambient Etching time: 2 min to 3 min Additional precautions/requirements: nil Comments: Reveals extent of HAZ. Microscopic
36、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 (C2H5OH) 1 ml to 5 ml hydrochloric acid (HCl) Safe shelf life: Indefinite Surface preparation: 3 m diamond or finer Etching t
37、emperature: 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 C2H5OH. 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 o
38、f etchant: Microscopic etchant Composition in volume and in order of mixing: 120 ml ethyl alcohol (C2H5OH) or methyl alcohol (CH3OH) 10 ml iron (III) chloride (FeCl3) (60 % W/V) 30 ml hydrochloric acid (HCl) Safe shelf life: Indefinite Surface preparation: 2 m diamond or finer Etching temperature: A
39、mbient 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
40、 mixing: 30 ml water (H2O) 25 ml ethyl alcohol (C2H5OH) 40 ml hydrochloric acid (HCl) 5 g copper (II) chloride (CuCl2) 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 spe
41、cimen should be washed in order to remove copper deposits. Usual precautions for handling and disposal of acids. Comments: Reveals cold working strain 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: Microscop
42、ic etchant Composition in volume and in order of mixing: 100 ml ethyl alcohol (C2H5OH) 20 ml water (H2O) 1 ml hydrochloric acid (HCl) 4 g magnesium (II) chloride (MgCl2) 1 g copper (II) chloride (CuCl2) Safe shelf life: 2 h Surface preparation: 3 m diamond or finer Etching temperature: Ambient Etchi
43、ng 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 m) after the etching furnishes the best contrast. Comments: Reveals phosphorus and related segregations. The copper deposits first
44、of all on those areas poorest in phosphorus. Table A.11 Adlers etchant Type of etchant: Macroscopic etchant Composition in volume and in order of mixing: 25 ml water (H2O) 3 g ammonium tetra chloro diaquo cuprate (II) (NH4)2CuCl4.2H2O 50 ml hydrochloric acid (HCl) 15 g iron (III) chloride (FeCl3) Sa
45、fe shelf life: Months Surface preparation: 320 grit or finer Etching temperature: Ambient Etching time: 5 s to 10 s Additional precautions/requirements: Add (NH4)2CuCl4.2H2O to H2O (a). Add FeCl3to HCl (b). Mix both then add (b) to (a). Comments: nil PD CEN ISO/TR 16060:2014ISO/TR 16060:2003(E) ISO
46、2003 All rights reserved 9Table A.12 Heyns etchant Type of etchant: Macroscopic etchant Composition in volume and in order of mixing: 120 ml water (H2O) 10 g ammonium tetra chloro diaquo cuprate (II) (NH4)2CuCl4.2H2O Safe shelf life: Months Surface preparation: 240 grit or finer Etching temperature:
47、 Ambient Etching time: 10 s to 1 min Additional precautions/requirements: Add (NH4)2CuCl4.2H2O to H2O. 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 (H2O) 30 ml iron (III)
48、chloride (FeCl3) (60 % W/V) 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)
49、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) 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 (H2O) 10 g oxalic acid (ethanedioic acid
