1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 3613:2010Metallic and other inorganiccoatings Chromateconversion coatings on zinc,cadmium, aluminium-zincalloys and zinc-aluminiumalloys Test methods (ISO3613:2010)BS E
2、N ISO 3613:2010 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 3613:2010.It supersedes BS EN ISO 3613:2001 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee STI/33, Electrodeposited and related coatings.A list of
3、 organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 65989 8ICS 25.220.20Compliance with a British Stand
4、ard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 January 2011.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 3613 December 2010 I
5、CS 25.220.20 Supersedes EN ISO 3613:2001English Version Metallic and other inorganic coatings - Chromate conversion coatings on zinc, cadmium, aluminium-zinc alloys and zinc-aluminium alloys - Test methods (ISO 3613:2010) Revtements mtalliques et autres revtements inorganiques - Couches de conversio
6、n au chromate sur zinc, cadmium et alliages daluminium-zinc et de zinc-aluminium - Mthodes dessai (ISO 3613:2010) Metallische und andere anorganische berzge - Chromatierberzge auf Zink, Cadmium, Aluminium-Zink- und Zink-Aluminium-Legierungen - Prfverfahren (ISO 3613:2010) This European Standard was
7、approved by CEN on 3 December 2010. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nat
8、ional standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own lang
9、uage and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Lat
10、via, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Bruss
11、els 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 3613:2010: EBS EN ISO 3613:2010EN ISO 3613:2010 (E) 3 Foreword This document (EN ISO 3613:2010) has been prepared by Technical Committee ISO/TC 107 “Metallic and other in
12、organic coatings” in collaboration with Technical Committee CEN/TC 262 “Metallic and other inorganic coatings” the secretariat of which is held by BSI. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest
13、 by June 2011, and conflicting national standards shall be withdrawn at the latest by June 2011. 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 pate
14、nt rights. This document supersedes EN ISO 3613:2001. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finla
15、nd, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 3613:2010 has been approved by CEN as a EN IS
16、O 3613:2010 without any modification. BS EN ISO 3613:2010ISO 3613:2010(E) ISO 2010 All rights reserved iiiForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is nor
17、mally 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
18、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 prepar
19、e 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. Attention is drawn to the possibility that som
20、e 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 3613 was prepared by Technical Committee ISO/TC 107, Metallic and other inorganic coatings. This third edition cancels and replaces the second
21、edition (ISO 3613:2000), which has been technically revised. BS EN ISO 3613:2010ISO 3613:2010(E) iv ISO 2010 All rights reservedIntroduction This International Standard specifies methods for the qualitative determination of the presence of chromate conversion coatings as well as the total chromium c
22、ontent of chromate conversion coatings. The application of very thin, colourless, practically invisible chromate conversion coatings is frequently called “passivation”, while the application of thicker, coloured chromate conversion coatings is called “chromating”. The term “passivation” is not corre
23、ct, does not comply with the ISO 2080 designation and is therefore deprecated. BS EN ISO 3613:2010INTERNATIONAL STANDARD ISO 3613:2010(E) ISO 2010 All rights reserved 1Metallic and other inorganic coatings Chromate conversion coatings on zinc, cadmium, aluminium-zinc alloys and zinc-aluminium alloys
24、 Test methods WARNING This International Standard calls for the use of substances and/or procedures that may be injurious to health if adequate safety measures are not taken. This International Standard does not address any health hazards, safety or environmental matters associated with its use. It
25、is the responsibility of the user of this International Standard to establish appropriate health, safety and environmentally acceptable practices and take suitable actions for any national and international regulations. Compliance with this International Standard does not in itself confer immunity f
26、rom legal obligations. 1 Scope This International Standard specifies methods for the determination of the presence of colourless chromate conversion coatings, the presence of hexavalent chromium in colourless and coloured coatings on zinc or cadmium or aluminium-zinc (mass fraction of aluminium: 55
27、%, within a range of 54 % to 56 % mass fraction) and zinc-aluminium (mass fraction of aluminium: 5 %) alloys, the total chromium content per unit area on zinc and cadmium, the mass per unit area of both colourless and coloured coatings, the satisfactory adhesion of chromate conversion coatings, and
28、the quality of chromate coatings. These methods are applicable to colourless and coloured chromate conversion coatings containing trivalent and hexavalent chromium in varying proportions and produced by either chemical or electrochemical processes, and only to chromate coatings that are free from an
29、y supplementary coatings, such as oil, water or solvent-based polymers or wax. 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 ref
30、erenced document (including any amendments) applies. ISO 3892, Conversion coatings on metallic materials Determination of coating mass per unit area Gravimetric methods ISO 4520, Chromate conversion coatings on electroplated zinc and cadmium coatings IEC 60068-2-30, Environmental testing Part 2-30:
31、Tests Test Db: Damp heat, cyclic (12 h + 12 h cycle) BS EN ISO 3613:2010ISO 3613:2010(E) 2 ISO 2010 All rights reserved3 Reagents Use only reagents of recognized analytical grade and distilled water or water of equivalent purity, unless otherwise specified, for analysis. 3.1 Test solution A (see 5.2
32、). Dissolve 1 g of diphenylcarbazide in a mixture of 20 ml of acetone, 60 ml of glacial acetic acid and 40 ml of distilled water contained in a beaker. Add 15 ml of concentrated hydrochloric acid ( = 1,18 g/cm3), stir and add slowly 30 ml of sodium hypochlorite solution (10 % to 15 % available chlor
33、ine). Add 5 ml of hydrogen peroxide (30 % volume fraction) slowly with continuous stirring. Leave the solution in the open beaker for 24 h in a fume cupboard, to allow excess chlorine to escape, before use. The solution does not deteriorate with age and can be kept in a bottle with a loosely fitted
34、stopper. However, there may be losses due to evaporation and the concentration may alter so it is discarded after 6 months. 3.2 Test solution B (see 5.3). Dissolve 50 g of lead acetate trihydrate (CH3COO)2Pb3H2O in 1 l of distilled water or water of equivalent purity. Ensure that the pH of the solut
35、ion is between 5,5 and 6,8 as prepared. If the pH of the solution is outside this range, discard the solution and obtain a new supply of lead acetate. Any white precipitate formed during the initial preparation of the solution may be dissolved by small additions of glacial acetic acid, provided that
36、 the pH is not reduced to a value below 5,5. Discard the stock solution if the white precipitate does not disappear. 3.3 Test solution C (see 5.5) 3.3.1 Test solution C 1 Dissolve 0,4 g of diphenylcarbazide in a mixture of 20 ml of acetone and 20 ml of ethanol (96 %). After dissolution, add 20 ml of
37、 75 % orthophosphoric acid solution and 20 ml of distilled water. Prepare this solution not more than 8 h prior to use. 3.3.2 Test solution C 2 Add 700 ml of orthophosphoric acid, of specific gravity 1,7, to 250 ml of distilled water or water of equivalent purity and make up to 1 000 ml. Dissolve 1,
38、0 g of 1,5-diphenylcarbazide in 100 ml of acetone, adding one drop of glacial acetic acid to help dissolution. Keep the solution in a dark glass bottle in the refrigerator. The solution shall be discarded after 4 weeks. For the Cr(VI) standard solution, dissolve 0,113 g of K2Cr2O7in distilled water
39、or water of equivalent purity and make up to the mark in a 1 000 ml volumetric flask. Measure 2,5 ml of this solution into a second 1 000 ml volumetric flask and make up to the mark. 1 ml of this standard solution contains 0,1 g of Cr(VI). The solution shall be discarded after 9 months. For the prep
40、aration of comparison solution, add 1 ml of phosphoric acid and 1 ml of diphenylcarbazide solution to 50 ml of standard Cr(VI) solution, and mix thoroughly. Allow the solution to stand for 10 min for the colour reaction to be completed. 3.4 Test solution D (see 5.6 and 5.7). Dissolve 0,50 g of diphe
41、nylcarbazide in 50 ml of acetone. Dilute slowly, while stirring, with 50 ml of water (rapid mixing can result in precipitation of diphenylcarbazide). For maximum stability, store the solution under refrigeration in an amber-coloured glass bottle. BS EN ISO 3613:2010ISO 3613:2010(E) ISO 2010 All righ
42、ts reserved 33.5 Sulfuric acid, diluted 1 + 3. Slowly add 1 volume of concentrated sulfuric acid ( = 1,84 g/cm3) to 3 volumes of water. 3.6 Ammonium persulfate (NH4)2S2O8. 3.7 Sodium hydroxide (NaOH), 240 g/l solution. 3.8 Silver nitrate (AgNO3), 17 g/l solution. 3.9 Potassium dichromate (K2Cr2O7),
43、standard solution. Dilute 2 ml of standard volumetric potassium dichromate solution (4,9 g/l) to 1 000 ml. 3.10 Phosphate buffer solution. Dissolve 55 g of sodium dihydrogen orthophosphate monohydrate (NaH2PO4H2O) in 100 ml of water. 4 Apparatus Use normal laboratory apparatus and the following. Cle
44、an all glassware thoroughly. It is recommended that cleaning be done by boiling the glassware with nitric acid (HNO3) of 30 % mass fraction and then rinsing thoroughly with distilled water or water of equivalent purity. 4.1 Photoelectric absorptiometer (colorimeter), with a filter having a mean tran
45、smission of 520 nm. The absorptiometer shall be used with an absorption cell having an optical path length of 10 mm. 4.2 Spectrophotometer, with wavelength set at 540 nm. The spectrophotometer shall be used with an absorption cell having an optical path length of 10 mm. 4.3 Analytical balance, capab
46、le of weighing to the nearest 0,1 mg. 5 Test methods 5.1 General The test surface, prior to the following tests, shall be free of all contaminants, finger prints and other extraneous stains. If the surface is coated with a thin oil film, this shall be removed prior to the test by degreasing using a
47、suitable solvent at room temperature (not exceeding 35 C). If it is necessary to store samples, they shall be stored at temperatures not exceeding 40 C and at a relative humidity below 70 %. For test purposes, the samples shall not be subjected to forced drying at temperatures in excess of 35 C. Tre
48、atment in alkaline solutions shall not be performed as chromate conversion coatings are broken down by alkalis. Spot tests are not always a precise means of determining the presence of chromate coatings. The test methods for a) the presence of a colourless chromate coating on zinc, cadmium and alumi
49、nium-zinc alloys, b) the presence of hexavalent chromium in both coloured and colourless chromate coatings, c) the determination of hexavalent chromium content, and d) the determination of total chromium content BS EN ISO 3613:2010ISO 3613:2010(E) 4 ISO 2010 All rights reservedare given in 5.2 to 5.7. The tests shall be carried out within the following time limits: a minimum of 24 h after the application of the chromate conversion coating for all tests (5.2 to 5.10); a maximum of 3 d for tests speci
