SIST EN 13603:2004

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.WHKQLNRKupfer und Kupferlegierungen - Prüfverfahren zur Beurteilung von Schutzüberzügen aus Zinn auf gezogenen Runddrähten aus Kupfer für die Anwendung in der ElektrotechnikCuivre et alliages de cuivre - Méthodes d'évaluation des revetements en étain sur les fils ronds étirés en cuivre pour usages électriquesCopper and copper alloys - Test methods for assessing protective tin coatings on drawn round copper wire for electrical purposes77.150.30Bakreni izdelkiCopper products25.220.40Kovinske prevlekeMetallic coatingsICS:Ta slovenski standard je istoveten z:EN 13603:2002SIST EN 13603:2004en01-januar-2004SIST EN 13603:2004SLOVENSKI
STANDARD



SIST EN 13603:2004



EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13603March 2002ICS 25.220.40; 77.150.30English versionCopper and copper alloys - Test methods for assessingprotective tin coatings on drawn round copper wire for electricalpurposesCuivre et alliages de cuivre - Méthodes d'évaluation desrevêtements en étain sur les fils ronds étirés en cuivre pourusages électriquesKupfer und Kupferlegierungen - Prüfverfahren zurBeurteilung von Schutzüberzügen aus Zinn auf gezogenenRunddrähten aus Kupfer für die Anwendung in derElektrotechnikThis European Standard was approved by CEN on 22 February 2002.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the 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 translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2002 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13603:2002 ESIST EN 13603:2004



EN 13603:2002 (E)ContentspageForeword .3Introduction .41Scope .42Normative references .43Terms and definitions .44Thickness of the unalloyed tin coating .54.1Principle .54.2Reagents and materials .54.3Apparatus .54.4Preparation of the test piece .74.5Procedure for determining the thickness ofunalloyed tin coatings .74.6Expression of results .95Continuity of the tin coating .105.1Principle .10page5.2Test solution .105.3Reference solution .105.4Preparation of the test piece .105.5Cleaning of the test piece .115.6Immersion for testing .115.7Determination .116Adherence of the tin coating .126.1Principle .126.2Stock solution .126.3Test solution .126.4Preparation of the test piece .126.5Cleaning of the test piece .136.6Immersion for testing .136.7Examination .137Test report .13Bibliography .142SIST EN 13603:2004



EN 13603:2002 (E)ForewordThis document EN 13603:2002 has been prepared by Technical Committee CEN/TC 133 "Copper and copperalloys", the secretariat of which is held by DIN.This European Standard shall be given the status of a national standard, either by publication of an identical text orby endorsement, at the latest by September 2002, and conflicting national standards shall be withdrawn at the latestby September 2002.Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 5 "Copper forelectrical purposes" to prepare the following standard:EN 13603,
Copper and copper alloys — Test methods for assessing protective tin coatings on drawn round copperwire for electrical purposes.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countriesare bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France,Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden,Switzerland and United Kingdom.3SIST EN 13603:2004



EN 13603:2002 (E)IntroductionIn preparing this document CEN/TC 133/WG 5 agreed to study carefully existing standards and to combine the besttest methods for assessing tin coatings into a single European Standard.The following standards were considered:ISO 2177 : 1985;ASTM B 33 : 1981, clauses 7 and 8;BS 4109 : 1970, clause 14;DIN 51213 : 1970, clause 6.1
ScopeThis European Standard specifies methods for assessing the tin coating on drawn round copper wire for themanufacture of electrical conductors, e.g. according to EN 13602.Standard includes test methods for the determination of the following characteristics:a)thickness of the unalloyed tin coating;b)continuity of the tin coating;c)adherence of the tin coating.WARNING
This standard can involve the use of hazardous materials, operations, and equipment. Thisstandard does not purport to address all of the safety problems associated with their use. It is the responsi-bility of the user of this standard to establish appropriate safety and health practices and determine theapplicability of regulatory limitations prior to use.2
Normative referencesThis European Standard incorporates, by dated or undated reference, provisions from other publications. Thesenormative references are cited at the appropriate places in the text, and the publications are listed hereafter. Fordated references, subsequent amendments to or revisions of any of these publications apply to this EuropeanStandard only when incorporated in it by amendment or revision. For undated references, the latest edition of thepublication referred to applies (including amendments).EN 610,
Tin and tin alloys — Ingot tin.EN 13602,
Copper and copper alloys — Drawn, round copper wire for the manufacture of electrical conductors.NOTE
Informative references to documents used in the preparation of this standard, and cited at the appropriate places in thetext, are listed in the bibliography.3
Terms and definitionsFor the purposes of this European Standard, the following terms and definitions apply.3.1unalloyed tin coatinglayer of pure tin on the surface of tinned wire4SIST EN 13603:2004



EN 13603:2002 (E)3.2alloyed tin coatingdiffusion layer of copper and tin formed at the copper wire and tin coating interface during tinning and subsequentdrawing and annealing processes3.3total tin coatingsum of the thicknesses of the unalloyed tin coating and the alloyed tin coating3.4measuring areaarea of the surface over which a single measurement is made4
Thickness of the unalloyed tin coating4.1
PrincipleAnodic dissolution of a well-defined area of the unalloyed coating using a suitable electrolyte, followed by detectionof the virtually complete dissolution of the unalloyed coating by a rapid change in cell voltage. Calculation of theunalloyed coating thickness from the quantity of electricity (in coulombs) used, which can in turn be calculated from:a)the time interval between the start of the test and the first rapid change of cell voltage, if it is conducted atconstant current density; orb)the integrated quantity of electricity used in dissolving the unalloyed coating.4.2
Reagents and materials4.2.1
Electrolyte, either a hydrochloric acid electrolyte or an electrolyte recommended by the instrument manufac-turer.For the hydrochloric acid electrolyte dilute 170 ml of hydrochloric acid (HCl),
= 1,18 g/ml, to 1 000 ml withdeionised water.NOTE
The unalloyed tin coating dissolves anodically at an efficiency of nearly 100 %; for determination of the electrolyteefficiency, see 4.5.6.WARNING
Hydrochloric acid causes burns and is irritating to the respiratory system. Avoid breathing thevapour and prevent contact with eyes and skin.This electrolyte dissolves tin coatings at very low cell voltages at which there is no anodic attack on the substrateswhen they are exposed at the end of the test.4.2.2
Tin, tin grade in accordance with EN 610.4.3
Apparatus4.3.1
GeneralSuitable instruments may be constructed from readily available components, alternatively a proprietary instrumentmay be used.5SIST EN 13603:2004



EN 13603:2002 (E)4.3.2
Direct reading instrumentsProprietary direct reading instruments are available for use with electrolytes recommended by the manufacturer.The calculation of thickness of tin coating from current density is made electronically. The instrument shall havesome means of indicating when the unalloyed tin coating has been fully removed.4.3.3
Other instrumentsInstruments other than proprietary direct reading instruments record the quantity of electricity, in coulombs, used indissolving the unalloyed coating from the measuring area, usually in arbitrary units, from which the thickness can becalculated using factors or tables.4.3.4
Electrolytic cellThe electrolytic cell consists of a container for the electrolyte, a cathode and an anode which is the test sample. Thecontainer, if it is made of metal, for example stainless steel, can serve as the cathode. If the container is made ofinsulating material, a separate cathode is required.Also required are a device for supporting the appropriate length of test sample and an agitation mechanism.Depending on the wire diameter, the test sample may be a straight length of wire or, if necessary to obtain sufficientsurface area for smaller diameter wires, a holding device such as that shown schematically in Figure 1 is required.A magnetic stirrer or similar system shall be used to provide agitation.Key1 Tee-frame to support test piece of non-conducting material, manufactured from nylon or other plastics2
Test piece3 Test piece connection (anode)4 Cathode connection5 Electrolyte level6 Test piece length L7 Electrolyte8 Non-metallic pin9 Cathode (stainless steel or lead), container (beaker)Figure 1 — Alternative method for supporting fine wire or wire which cannot be straightened6SIST EN 13603:2004



EN 13603:2002 (E)4.4
Preparation of the test pieceSelect a suitable length of test sample in order to provide the appropriate test piece area for exposure to theelectrolyte. If necessary, clean the test surface with a suitable organic solvent (see 4.5.4.5).NOTE
Care should be taken to avoid removal of metal during the cleaning operation.4.5
Procedure for determining the thickness of unalloyed tin coatings4.5.1
GeneralIf commercial equipment is used, follow the manufacturer's instructions with respect to the operating procedure formeasurement, the electrolyte and, if necessary, calibration. Appropriate attention shall be given to the factors listedin 4.5.4. The performance of the instrument shall be checked using a reference specimen of pure tin wire. A tingrade in accordance with EN 610 shall be used. The test shall be carried out in accordance with 4.5.6.If the instrument readings or the calculation of K give an electrolytic efficiency of equal to or greater than 98 %, theinstrument may be used without further adjustment. Otherwise, the cause of discrepancy shall be remedied.Proprietary instruments shall be calibrated in accordance with the manufacturer's instructions.4.5.2
Determination of measuring areaFor the determination of the measuring area the length L of the test piece in millimetres shall be determined with anaccuracy of 1 % and the diameter d of the test piece for wires with a nominal diameter of < 0,6 mm shall be deter-mined with an accuracy of 1 % and for wires with a nominal diameter of ³ 0,6 mm with an accuracy of 0,5 %. Themeasuring area A in square centimetres is given by the equation (1):(1)NOTE
An exact area of stripping is necessary for accuracy and the main source of error is due to the meniscus and current fieldat the electrolyte surface.4.5.3
Electrolysis (Dissolution of the unalloyed tin coating)The electrolyte (4.2.1) and test piece shall be introduced into the cell so that a known area is exposed to theelectrolyte. Efforts shall be made to ensure that no gas bubbles occur on the measuring area by use of the agitationmechanism. The electrical connections shall be made and the agitator operated. Electrolysis shall be continued untildissolution of the unalloyed tin coating is complete, as indicated by a sharp change in the anode potential or cellvoltage, or by the operation of the automatic cut-out.After completion of the test, the test piece shall be removed from the cell, rinsed with water and examined to ensurethat complete removal of the unalloyed tin coating has occurred over the measuring area, see 4.5.4.9.4.5.4
Factors affecting the measuring accuracy4.5.4.1
Coating thicknessThe optimum accuracy is achieved with coating thicknesses in the range 0,2 µm up to 50 µm.4.5.4.2
Current variationFor instruments using the constant current and time measuring technique, current variation will cause errors. Forinstruments using a current-time integrator, too large a change in current can change the anode current efficiencyor interfere with the end-point, causing an error.7SIST EN 13603:2004



EN 13603:2002 (E)4.5.4.3
Area variationThe accuracy of the thickness measurement will be no better than the accuracy to which the measuring area isknown. Area variati
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