DIN EN ISO 3613-2011 Metallic and other inorganic coatings - Chromate conversion coatings on zinc cadmium aluminium-zinc alloys and zinc-aluminium alloys - Test methods (ISO 3613 2.pdf

1、April 2011 Translation by DIN-Sprachendienst.English price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS

2、25.220.40!$nm“1757498www.din.deDDIN EN ISO 3613Metallic and other inorganic coatings Chromate conversion coatings on zinc, cadmium, aluminium-zinc alloysand zinc-aluminium alloys Test methods (ISO 3613:2010)English translation of DIN EN ISO 3613:2011-04Metallische und andere anorganische berzge Chro

3、matierberzge auf Zink, Cadmium, Aluminium-Zink- undZink-Aluminium-Legierungen Prfverfahren (ISO 3613:2010)Englische bersetzung von DIN EN ISO 3613:2011-04Revtements mtalliques et autres revtements inorganiques Couches de conversion au chromate sur zinc, cadmium et alliages daluminium-zinc et dezinc-

4、aluminium Mthodes dessai (ISO 3613:2010)Traduction anglaise de DIN EN ISO 3613:2011-04SupersedesDIN EN ISO 3613:2002-01www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.1704.11 DIN EN ISO 3613:2011-04 2 A comma is used as the decimal

5、 marker. National foreword This standard has been prepared by Technical Committee ISO/TC 107 “Metallic and other inorganic coatings” (Secretariat: KATS, Republic of Korea) and has been adopted as EN ISO 3613:2010 by Technical Committee CEN/TC 262 “Metallic and other inorganic coatings” (Secretariat:

6、 BSI, United Kingdom) within the scope of the Agreement on technical cooperation between ISO and CEN (Vienna Agreement). The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Working Committee NA 062-01-61 AA Mess- und

7、 Prfverfahren fr metallische und andere anorganische berzge. Precision data (repeatability, reproducibility) in accordance with DIN EN ISO 4259 are not yet available for the quantitative determination of hexavalent chromium in corrosion protection coatings and must still be obtained. As a rule, mass

8、 density (dimension: g/cm3) is used instead of the dimensionless relative (specific) density used in this standard. The numerical value for the two dimensions will be identical, provided the relative specific density is related to the density of water under standard conditions (1 g/cm3). In order to

9、 ensure the accuracy of analytical results obtained using the spot test, it is recommended that the hexavalent chromium concentration in corrosion protection coatings be determined photometrically. The method of determining the total chromium content as in 5.7 is not specific to hexavalent chromium,

10、 but can also be used for other valence states of chromium. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 3892 DIN EN ISO 3892 ISO 9227 DIN EN ISO 9227 IEC 60068-2-30 DIN EN 60068-2-30 Amendments This standard differs from DIN EN ISO

11、3613:2002-01 as follows: a) Clause 6 “Test report” has been added; b) Subclause 5.5.2 “Test method employing alternative test solution C 2 (destructive)” has been added; c) the standard has been aligned with the content of DIN EN 15205:2007-02; d) the standard has been editorially revised. Previous

12、editions DIN EN ISO 3613: 1995-01, 2002-01 DIN EN ISO 3613:2011-04 3 National Annex NA (informative) Bibliography DIN EN ISO 3892, Conversion coatings on metallic materials Determination of coating mass per unit area Gravimetric methods DIN EN ISO 9227, Corrosion tests in artificial atmospheres Salt

13、 spray tests DIN EN 60068-2-30, Environmental testing Part 2-30: Tests Test Db: Damp heat, cyclic (12 h + 12 h cycle) DIN EN ISO 3613:2011-04 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 3613 December 2010 ICS 25.220.20 Supersedes EN ISO 3613:2001Englis

14、h 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 conversion au chromate sur zinc, cadmium et alliages da

15、luminium-zinc et de zinc-aluminium - Mthodes dessai (ISO 3613:2010) Metallische und andere anorganische berzge - Chromatierberzge auf Zink, Cadmium, Aluminium-Zink- This European Standard was approved by CEN on 3 December 2010. CEN members are bound to comply with the CEN/CENELEC Internal Regulation

16、s 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 national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. Th

17、is 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 language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN mem

18、bers are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain

19、, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Mem

20、bers. Ref. No. EN ISO 3613:2010: E(ISO 3613:2010) und Zink-Aluminium-Legierungen - Prfverfahren Contents DIN EN ISO 3613:2011-04 EN ISO 3613:2010 (E) 2 Page Foreword3 Introduction .4 1 Scope 5 2 Normative references 5 3 Reagents.6 4 Apparatus .7 5 Test methods7 5.1 General7 5.2 Test for the presence

21、 of a colourless chromate coating on zinc .8 5.3 Test for the presence of a colourless chromate coating on zinc and cadmium.8 5.4 Test for the presence of a colourless chromate coating on and zinc-aluminium (mass fraction of aluminium: 5 %) alloys .9 5.5 Test for the presence of hexavalent chromium

22、in both colourless and coloured chromate coatings 9 5.5.1 Test method employing test solution C 1 .9 5.5.2 Test method employing alternative test solution C 2 (destructive) .9 5.5.3 Expression of results 10 5.6 Determination of hexavalent chromium content of coloured chromate coatings 10 5.6.1 Prepa

23、ration of calibration graph 10 5.6.2 Blank test10 5.6.3 Determination.10 5.6.4 Expression of results 11 5.7 Determination of total chromium content of coloured chromate coatings .11 5.7.1 Preparation of calibration graph 11 5.7.2 Blank test11 5.7.3 Determination.11 5.7.4 Expression of results 11 5.8

24、 Determination of mass per unit area of both colourless and coloured chromate coatings by gravimetric method 11 5.9 Test for adhesion by abrasion12 5.10 Quality evaluation test of chromate layers on zinc and cadmium surfaces .12 6 Test report 12 Bibliography 13 Foreword This document (EN ISO 3613:20

25、10) has been prepared by Technical Committee ISO/TC 107 “Metallic and other inorganic 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 standar

26、d, either by publication of an identical text or by endorsement, at the latest 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

27、/or CENELEC shall not be held responsible for identifying any or all such patent 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: Austri

28、a, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, 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. En

29、dorsement notice The text of ISO 3613:2010 has been approved by CEN as a EN ISO 3613:2010 without any modification. DIN EN ISO 3613:2011-04 EN ISO 3613:2010 (E) 3 Introduction This International Standard specifies methods for the qualitative determination of the presence of chromate conversion coati

30、ngs as well as the total chromium content 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”.

31、The term “passivation” is not correct, does not comply with the ISO 2080 designation and is therefore deprecated. DIN EN ISO 3613:2011-04 EN ISO 3613:2010 (E) 4 WARNING This International Standard calls for the use of substances and/or procedures that may be injurious to health if adequate safety me

32、asures are not taken. This International Standard does not address any health hazards, safety or environmental matters associated with its use. It is the responsibility of the user of this International Standard to establish appropriate health, safety and environmentally acceptable practices and tak

33、e suitable actions for any national and international regulations. Compliance with this International Standard does not in itself confer immunity from legal obligations. 1 Scope This International Standard specifies methods for the determination of the presence of colourless chromate conversion coat

34、ings, the presence of hexavalent chromium in colourle ss and coloured coatings on zinc or cadmium or aluminium-zinc (mass fraction of aluminium: 55 %, 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 o

35、n zinc and cadmium, the mass per unit area of both colourless and coloured coatings, the satisfactory adhesion of chromate conversion coatings, and the quality of chromate coatings. These methods are applicable to colourless and coloured chromate conversion coati ngs containing trivalent and hexaval

36、ent chromium in varying proportions and produced by either chemical or electrochemical processes, and only to chromate coatings that are free from any supplementary coatings, such as oil, water or solvent-based polymers or wax. 2 Normative references The following referenced documents are indispensa

37、ble 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 3892, Conversion coatings on metallic materials Determination of coating mass per unit area Gr

38、avimetric methods ISO 4520, Chromate conversion coatings on electroplated zinc and cadmium coatings IEC 60068-2-30, Environmental testing Part 2-30: Tests Test Db: Damp heat, cyclic (12 h + 12 h cycle) DIN EN ISO 3613:2011-04 EN ISO 3613:2010 (E) 5 3 Reagents Use only reagents of recognized analytic

39、al grade and distilled water or water of equivalent purity, unless otherwise specified, for analysis. 3.1 Test solution A (see 5.2). 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 conce

40、ntrated hydrochloric acid ( = 1,18 g/cm3), stir and add slowly 30 ml of sodium hypochlorite solution (10 % to 15 % available chlorine). 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 ex

41、cess chlorine to escape, before use. The solution does not deteriorate with age and can be kept in a bottle with a loosely fitted 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 o

42、f lead acetate trihydrate (CH3COO)2Pb3H2O in 1 l of distilled water or water of equivalent purity. Ensure that the pH of the solution 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 precipita

43、te formed during the initial preparation of the solution may be dissolved by small additions of glacial acetic acid, provided that 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

44、 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 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 orthophospho

45、ric 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 1,0 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 refrigerato

46、r. The solution shall be discarded after 4 weeks. For the Cr(VI) standard solution, dissolve 0,113 g of K2Cr2O7in distilled water 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

47、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 preparation 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 sol

48、ution 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 diphenylcarbazide in 50 ml of acetone. Dilute slowly, while stirring, with 50 ml of water (rapid mixing can result in precipitation of diphenylcarbazide). For maximum stabilit

49、y, store the solution under refrigeration in an amber-coloured glass bottle. DIN EN ISO 3613:2011-04 EN ISO 3613:2010 (E) 6 3.5 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), standard solution. Dilute 2 ml of standard volumetric potassium dichromate solution (4,9 g/