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1、BRITISH STANDARD BS EN 15384:2007 Packaging Flexible aluminium tubes Test method to determine the porosity of the internal coating ICS 55.120 ? Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008
2、20:57:37 MDTNo reproduction or networking permitted without license from IHS -,-,- BS EN 15384:2007 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 29 February 2008 BSI 2008 ISBN 978 0 580 55646 3 National foreword This British Standard is th
3、e UK implementation 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 provi
4、sions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. Amendments/corrigenda issued since publication DateComments Copyright British Standards Institution Provided by IHS under license with BSI - Uncon
5、trolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008 20:57:37 MDTNo reproduction or networking permitted without license from IHS -,-,- EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15384 November 2007 ICS 55.120 English Version Packaging - Flexible aluminium tubes - Test met
6、hod to determine the porosity of the internal coating Emballage - Tubes souples en aluminium - Mthode dessai pour dterminer la porosit du revtement intrieur Packmittel - Aluminiumtuben - Prfverfahren zur Bestimmung der Porositt der Innenbeschichtung This European Standard was approved by CEN on 30 S
7、eptember 2007. 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 national standards may b
8、e obtained on application to the CEN 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 language and notified to the CEN
9、Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands
10、, 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: rue de Stassart, 36 B-1050 Brussels 2007 CENAll rights of exploitation in an
11、y form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15384:2007: E Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008 20:57:37 MDTNo reproduction or networking permitt
12、ed without license from IHS -,-,- EN 15384:2007 (E) 2 Contents Page Foreword3 1 Scope 4 2 Principle4 3 Apparatus .4 4 Procedure .5 5 Tolerances7 6 Test report8 Bibliography9 Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/59107700
13、01 Not for Resale, 08/14/2008 20:57:37 MDTNo reproduction or networking permitted without license from IHS -,-,- EN 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 Standa
14、rd shall be given the status of a national standard, either by publication of an identical text or by 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 docum
15、ent 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 standard is based on the professional recommendations of the European Tube Manufacturers Association (etma). According to the CEN/CENELEC Internal Regulations
16、, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands
17、, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008 20:57:37 MDTNo reproduction or networkin
18、g permitted without license from IHS -,-,- EN 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 internal coating is used as a barrier and should avoid any
19、 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 electrolyte conductivity of the internal coating is only one
20、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 electrolyte conductivity should never be used as the sole criter
21、ion 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 internally coated aluminium tubes is tested by an enamel conduc
22、tometer. 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 fixed time. The induced current is a measure for the quality (
23、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 quality criterion for the internal coating of metal tubes and can
24、s. 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 copper sulphate to the sodium chloride method will require
25、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 electrode Electrolyte A schematic diagram of the test equipment
26、 is given in Figure 1. Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008 20:57:37 MDTNo reproduction or networking permitted without license from IHS -,-,- EN 15384:2007 (E) 5 Key 1 Electrode 5
27、Electrolyte 2 Aluminium tube 6 electrode holder 3 Insulating spacer 7 Processor unit 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. Copyright British St
28、andards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008 20:57:37 MDTNo reproduction or networking permitted without license from IHS -,-,- EN 15384:2007 (E) 6 Table 1 Test conditions for the copper sulphate and the sodiu
29、m 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 4,0 s voltmeter 20 k/V ammeter 2,5 at 100 mA Electrodes - polarity - material -
30、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 stainless steel 5 mm 0,3 mm for tube diameter 19 mm 10 mm 0,5 mm for tube diameter 1
31、9 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 Pentahydrate p.a. CuSO4 5H2O CASa) (7758-99-8) (5,00 0,01)ml Acetic acid, 100 %, p.a., HAc
32、b) CASa) (64-19-7) (0,05 0,01) g/l wetting agent CASa) 68425-44-5 Dissolve the CuSO4 5H2O 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 finished solution shall be (4,75 0,25) mS. Sodium chloride solution (10,2
33、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 for chemical compounds, polymers, biological sequences, mixtures and al
34、loys. 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 necessary and should be done as described in the user manuals prior t
35、o 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 tube wall / tube shoulder and the dipping electrode. Fill the tube with e
36、lectrolyte up to 10 mm from the end after Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008 20:57:37 MDTNo reproduction or networking permitted without license from IHS -,-,- EN 15384:2007 (E) 7
37、 inserting the electrode. Start the measurement application of voltage 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 re
38、peated with the sodium chloride method. 5 Tolerances The tolerances given 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 specif
39、ic internal coatings but also depending on the product, different tolerance 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
40、diameter mm Mean Value mA Single Value mA 28 25 80 28 45 35 80 45 50 45 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 Me
41、an value Single value 20 10 25 15 30 20 30 15 30 20 40 30 40 20 40 25 50 40 45 25 50 30 60 45 50 35 80 - - Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008 20:57:37 MDTNo reproduction or networ
42、king permitted without license from IHS -,-,- EN 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 by several mA. For making well-founded conclusions a representative number of tubes should
43、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 between both parties the test report shall contain the following information: a) Referenc
44、e 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) Registering number of the apparatus and the selected test parameters, e) Type of internal co
45、ating, 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 are not covered by this standard, k) Date, place and name of the inspector. Copyright Briti
46、sh Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008 20:57:37 MDTNo reproduction or networking permitted without license from IHS -,-,- EN 15384:2007 (E) 9 Bibliography 1 DIN 55463-3, Verpackungsprfung; Aluminium
47、tuben; Bestimmung der Porigkeit der Innenschutzlackierung; 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 13047, Packaging Flexible conical metallic tubes Dimensions and tolerances 6 ISO 2859-1, Sampling procedures for inspection by attributes Par