1、Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 14/05/2008 01:57, Uncontrolled Copy, (c) BSIg49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58d
2、etermine the porosity of the internal coatingICS 55.120Packaging Flexible aluminium tubes Test method to BRITISH STANDARDBS EN 15384:2007BS EN 15384:2007Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 14/05/2008 01:57, Uncontrolled Copy, (c) BSIThis British Standard was published under the au
3、thority of the Standards Policy and Strategy Committee on 29 February 2008 BSI 2008ISBN 978 0 580 55646 3Amendments/corrigenda issued since publicationDate CommentsCompliance with a British Standard cannot confer immunity from legal obligations.National forewordThis British Standard is the UK implem
4、entation of EN 15384:2007.The UK participation in its preparation was entrusted to Technical Committee PKW/0, Packaging.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 necessary provisions of a con
5、tract. Users are responsible for its correct application.EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15384November 2007ICS 55.120English VersionPackaging - Flexible aluminium tubes - Test method todetermine the porosity of the internal coatingEmballage - Tubes souples en aluminium - Mthodedess
6、ai pour dterminer la porosit du revtement intrieurPackmittel - Aluminiumtuben - Prfverfahren zurBestimmung der Porositt der InnenbeschichtungThis European Standard was approved by CEN on 30 September 2007.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the c
7、onditions 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 CEN Management Centre or to any CEN member.This European Standard exists in thr
8、ee 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 CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Aus
9、tria, Belgium, Bulgaria, 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 United Kingdom.EUROPEAN COMMIT
10、TEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15384:2007: ELicensed Copy: Wang Bin, ISO/
11、EXCHANGE CHINA STANDARDS, 14/05/2008 01:57, Uncontrolled Copy, (c) BSIEN 15384:2007 (E) 2 Contents Page Foreword3 1 Scope 4 2 Principle4 3 Apparatus .4 4 Procedure .5 5 Tolerances 7 6 Test report 8 Bibliography 9 Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 14/05/2008 01:57, Uncontrolled C
12、opy, (c) BSIEN 15384:2007 (E) 3 Foreword This document (EN 15384:2007) has been prepared by Technical Committee CEN/TC 261 “Packaging”, the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by
13、 endorsement, at the latest by May 2008, and conflicting national standards shall be withdrawn at the latest by May 2008. 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 identif
14、ying any or all such patent rights. This standard is based on the professional recommendations of the European Tube Manufacturers Association (etma). According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this Europea
15、n Standard: Austria, Belgium, Bulgaria, 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 United Kingdo
16、m. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 14/05/2008 01:57, Uncontrolled Copy, (c) BSIEN 15384:2007 (E) 4 1 Scope This standard is applicable for internally coated aluminium tubes, mainly used for the packing of pharmaceutical, cosmetic, hygiene, food or other household products. The
17、 internal coating is used as a barrier and should avoid any contact between aluminium and the product. This standard defines two alternative methods copper sulphate and sodium chloride method to detect the electrolyte conductivity as one criterion for the quality of the internal coating. NOTE The el
18、ectrolyte conductivity of the internal coating is only one criterion for evaluation of the quality of an internal coating. It does not give any information on the quantity or size of any pores or uncoated areas, nor any hint on possible reactions between the aluminium tube and the product. The elect
19、rolyte conductivity should never be used as the sole criterion for quality evaluation of the internal coating, but always with other parameters e.g. film thickness, acetone and/or ammonia resistance and of course results of enhanced stability studies. 2 Principle The electrolyte conductivity of inte
20、rnally coated aluminium tubes is tested by an enamel conductometer. The aluminium tubes are filled with an electrolyte solution up to a fixed level at its open end. One electrode is connected to the tube nozzle, the second electrode is dipped into the solution. A defined voltage is applied for a fix
21、ed time. The induced current is a measure for the quality (pores and/or film thickness) of the internal coating. NOTE In the early 80s the copper sulphate method was developed and standardized (e.g. DIN 55436-3 1). Subsequently this method became a nationally and internationally well accepted qualit
22、y criterion for the internal coating of metal tubes and cans. In the past few years a new method, the sodium chloride method, came into being, holding several advantages concerning accuracy, reproducibility and repeatability as well as on health and environmental aspects. As the changeover from the
23、copper sulphate to the sodium chloride method will require a transitional period, this standard describes both methods. It is planned to delete the copper sulphate method as a national and/or international standard in the next revision of this document. 3 Apparatus Enamel conductometer Moveable elec
24、trode Electrolyte A schematic diagram of the test equipment is given in Figure 1. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 14/05/2008 01:57, Uncontrolled Copy, (c) BSIEN 15384:2007 (E) 5 Key 1 Electrode 5 Electrolyte 2 Aluminium tube 6 electrode holder 3 Insulating spacer 7 Processor u
25、nit 4 Moveable electrode Figure 1 Test device 4 Procedure All parameters having a significant influence on the test results for the copper sulphate and sodium chloride methods are listed in Table 1. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 14/05/2008 01:57, Uncontrolled Copy, (c) BSIEN
26、 15384:2007 (E) 6 Table 1 Test conditions for the copper sulphate and the sodium chloride method Parameter Copper sulphate method Sodium chloride method Temperature 23 2 C 23 2 C Voltage and measuring interval internal resistance 4 500 mV DC 2,5 s voltmeter 20 k/V ammeter 2,5 at 100 mA 6 300 mV DC 4
27、,0 s voltmeter 20 k/V ammeter 2,5 at 100 mA Electrodes - polarity - material - diameter dipping electrode is the positive pole dipping electrode copper (a plastic cap has to be mounted on the bottom of the electrode to avoid direct contact between electrode and tube shoulder) adapter electrode stain
28、less steel 5 mm 0,3 mm for tube diameter 19 mm 10 mm 0,5 mm for tube diameter 19 mm dipping electrode is the negative pole dipping electrode stainless steel adapter electrode stainless steel 6 mm 0,3 mm for all tube sizes Electrolyte Copper sulphate solution (10,0 0,01) g Copper sulphate Pentahydrat
29、e p.a. CuSO45H2O CASa)(7758-99-8) (5,00 0,01)ml Acetic acid, 100 %, p.a., HAcb)CASa)(64-19-7) (0,05 0,01) g/l wetting agent CASa)68425-44-5 Dissolve the CuSO45H2O in deionized water, add the HAc and wetting agent and make up to (1 000 2) ml with deionized water. The electrolyte conductivity of the f
30、inished solution shall be (4,75 0,25) mS. Sodium chloride solution (10,2 0,01) g Sodium chloride p.a. NaCl, CASa)7647-14-5 Dissolve the NaCl in deionized water and make up to (1 000 2) ml with deionized water. a)CAS is Chemical Abstracts Service CAS registry numbers are unique numerical identifiers
31、for chemical compounds, polymers, biological sequences, mixtures and alloys. b)HAc is the most common abbreviation for acetic acid in the context of acid-base reactions. Depending on the method and the kind of apparatus (different apparatus are available) specific adjustments and calibrations may be
32、 necessary and should be done as described in the user manuals prior to use. To take a measurement put the tube into the adapter electrode, ensuring there is an electric circuit between the tube and electrode. Insert the dipping electrode centrally into the tube, avoiding any contact between the tub
33、e wall / tube shoulder and the dipping electrode. Fill the tube with electrolyte up to 10 mm from the end after Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 14/05/2008 01:57, Uncontrolled Copy, (c) BSIEN 15384:2007 (E) 7 inserting the electrode. Start the measurement application of voltage
34、 immediately. Read the result in mA on the display after the measuring interval. The electrolyte can be used for testing 10 tubes. The test on one tube is not repeatable for the copper sulphate method, tests for one tube can be repeated with the sodium chloride method. 5 Tolerances The tolerances gi
35、ven in this standard are based on long-term experiences and are valid only for membrane tubes. For tubes with special nozzles, e.g. without membrane or cannula, higher tolerance limits may be required. In addition, for some specific internal coatings but also depending on the product, different tole
36、rance limits may be required. Any deviations from this standard shall be agreed mutually between both parties. Tolerances for the copper sulphate method are given in Table 2: Table 2 Tolerances for the copper sulphate method Tube diameter mm Mean Value mA Single Value mA 28 25 80 28 45 35 80 45 50 4
37、5 80 Tolerances for the sodium chloride method are given in Table 3: Table 3 Tolerances for the sodium chloride method Maximum electrolyte conductivity mA Tube diameter mm Cylindrical tubes Conical tubes Mean value Single value Mean value Single value 20 10 25 15 30 20 30 15 30 20 40 30 40 20 40 25
38、50 40 45 25 50 30 60 45 50 35 80 - - Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 14/05/2008 01:57, Uncontrolled Copy, (c) BSIEN 15384:2007 (E) 8 NOTE 1 Due to several variables which can affect the result (e.g. corrosion, surface of copper electrode) the accuracy of the methods may vary b
39、y several mA. For making well-founded conclusions a representative number of tubes should always be tested. NOTE 2 Test apparatus from different suppliers may give different results. In this case comparative measurements and correlations factors may be required. 6 Test report Unless otherwise agreed
40、 between both parties the test report shall contain the following information: a) Reference to this standard and if necessary a specification for the method of sampling and acceptance of the batch, b) Complete identification of the batch and of the tubes checked, c) Description of the samples, d) Re
41、gistering number of the apparatus and the selected test parameters, e) Type of internal coating, f) Test results, g) Number of tested tubes, h) Number of defects, i) If applicable the decision for acceptance or rejection, j) All factors, that may have had an influence on the test results and which a
42、re not covered by this standard, k) Date, place and name of the inspector. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 14/05/2008 01:57, Uncontrolled Copy, (c) BSIEN 15384:2007 (E) 9 Bibliography 1 DIN 55463-3, Verpackungsprfung; Aluminiumtuben; Bestimmung der Porigkeit der Innenschutzlac
43、kierung; Elektrolytisches Verfahren 2 (Packaging test; tubes made of aluminium; disposition of porosity of the inside protective lacquer; electrolytical test) 3 EN 12374, Packaging Flexible tubes Terminology 4 EN 13046, Packaging Flexible cylindrical metallic tubes Dimensions and tolerances 5 EN 130
44、47, Packaging Flexible conical metallic tubes Dimensions and tolerances 6 ISO 2859-1, Sampling procedures for inspection by attributes Part 1: Sampling schemes indexed by acceptance quality limit (AQL) for lot-by-lot inspection Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 14/05/2008 01:57,
45、 Uncontrolled Copy, (c) BSIBS EN BSILicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 14/05/2008 01:57, Uncontrolled Copy, (c) BSI389 Chiswick High RoadLondonW4 4AL15384:2007BSI British Standards InstitutionBSI is the independent national body responsible for preparing British Standards. It pre
46、sents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter.RevisionsBritish Standards are updated by amendment or revision. Users of British Standards should make sure that they possess the latest amendments or editions.It is the constant aim of BSI
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