DIN EN 15384-2-2017 Packaging - Test method to determine the porosity of the internal coating of flexible aluminium tubes - Part 2 Copper sulphate test German version EN 15384-2 20.pdf

1、April 2017 English price group 8No 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 55.120!%dN“2654397www.din.deDIN EN

2、15384-2Packaging Test method to determine the porosity of the internal coating of flexible aluminium tubes Part 2: Copper sulphate test;English version EN 153842:2017,English translation of DIN EN 15384-2:2017-04Packmittel Prfverfahren zur Bestimmung der Porositt der Innenbeschichtung von Aluminiumt

3、uben Teil 2: Kupfersulfatverfahren;Englische Fassung EN 153842:2017,Englische bersetzung von DIN EN 15384-2:2017-04Emballage Mthode dessai pour dterminer la porosit du revtement intrieur des tubes souples en aluminium Partie 2: Essai au sulfate de cuivre;Version anglaise EN 153842:2017,Traduction an

4、glaise de DIN EN 15384-2:2017-04Together with DIN EN 153841:201704,supersedesDIN EN 15384:200801www.beuth.deDocument comprises 10 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.03.17DIN EN 15384-2:2017-04 2 A comma is used as

5、the decimal marker. National foreword This document (EN 15384-2:2017) has been prepared by Technical Committee CEN/TC 261 “Packaging” (Secretariat: AFNOR, France). The responsible German body involved in its preparation was DIN-Normenausschuss Verpackungswesen (DIN Standards Committee Packaging), Wo

6、rking Committee NA 115-02-08 AA “Tubes”. Amendments This standard differs from DIN EN 15384:2008-01 as follows: a) DIN EN 15384 has been subdivided into two parts, i. e. separate parts have been prepared for the sodium chloride test and for the copper sulphate test; b) the standard has been editoria

7、lly revised. Previous editions DIN 55436-3: 1983-10, 1992-12 DIN EN 15384: 2008-01 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15384-2 January 2017 ICS 55.120 Supersedes EN 15384:2007English Version Packaging - Test method to determine the porosity of the internal coating of flexible alumin

8、ium tubes - Part 2: Copper sulphate test Emballage - Mthode dessai pour dterminer la porosit du revtement intrieur des tubes souples en aluminium - Partie 2: Essai au sulfate de cuivre Packmittel - Prfverfahren zur Bestimmung der Porositt der Innenbeschichtung von Aluminiumtuben - Teil 2: Kupfersulf

9、atverfahren This European Standard was approved by CEN on 14 November 2016. 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 biblio

10、graphical references concerning such national 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 responsi

11、bility 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 members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republ

12、ic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE

13、 NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2017 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15384-2:2017 EEN 15384-2:2017 (E) 2 Contents Page EUROPEAN FOREWORD

14、 3 1 SCOPE . 4 2 PRINCIPLE . 4 3 APPARATUS 4 FIGURE 1 TEST DEVICE 5 4 PROCEDURE 5 TABLE 1 TEST CONDITIONS FOR THE COPPER SULPHATE METHOD . 6 5 TOLERANCES . 7 TABLE 2 TOLERANCES FOR THE COPPER SULPHATE METHOD . 7 6 TEST REPORT 7 BIBLIOGRAPHY 8 DIN EN 15384-2:2017-04 EN 15384-2:2017 (E) 3 European for

15、eword This document (EN 15384-2:2017) 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 endorsement, at the latest by Ju

16、ly 2017, and conflicting national standards shall be withdrawn at the latest by July 2017. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. This docum

17、ent supersedes EN 15384:2007. According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Repu

18、blic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 15384-2:2017-04 EN 15384-2:2017 (E) 4 1 Sc

19、ope This European Standard is applicable for internally coated cylindrical 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 contact between aluminium and the product. Th

20、is standard defines the copper sulphate method to detect the electrolyte conductivity as one criterion for the quality of the internal coating. The electrolyte conductivity of the internal coating is only one criterion for evaluation of the quality of an internal coating. It does not give any inform

21、ation 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 criterion for quality evaluation of the internal coating, but always with other parameters e.g. f

22、ilm 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 conductometer. The aluminium tubes are filled with an electrolyte solution up to a fixed level at

23、 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 (pores and/or film thickness) of the internal coating. 3 Apparatus 3.1 Enamel conductometer

24、3.2 Moveable electrode 3.3 Electrolyte NOTE A schematic diagram of the test equipment is given in Figure 1. DIN EN 15384-2:2017-04 EN 15384-2:2017 (E) 5 Key 1 electrode (negative pole) 2 aluminium tube 3 insulating spacer 4 movable electrode (positive pole) 5 electrolyte 6 electrode holder 7 process

25、or unit Figure 1 Test device 4 Procedure All parameters having a significant influence on the test results for the copper sulphate method are listed in Table 1. DIN EN 15384-2:2017-04 EN 15384-2:2017 (E) 6 Table 1 Test conditions for the copper sulphate method Parameter Copper sulphate method Temper

26、ature 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 Electrodes - polarity - material - diameter dipping electrode is the positive pole dipping electrode copper (a round insulating spacer of 5 2 mm has to be mounted on the bottom of

27、 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 19 mm Electrolyte Copper sulphate solution (10,0 0,01) g Copper sulphate Pentahydrate p.a. CuSO45H2O CASa)(7758998) (5,00 0

28、,01)ml Acetic acid, 100 %, p.a., HAcb)CASa)(64197) (0,05 0,01) g/l wetting agent CASa)68425445 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 finished solution shall be (4,75 0,25) mS. aCA

29、S is Chemical Abstracts Service CAS registry numbers are unique numerical identifiers for chemical compounds, polymers, biological sequences, mixtures and alloys. bHAc is the most common abbreviation for acetic acid in the context of acid-base reactions. Depending on the method and the kind of appar

30、atus (different apparatus are available) specific adjustments and calibrations may be 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. Inser

31、t the dipping electrode centrally into the tube until it touches the tube shoulder, avoiding any contact between the tube wall / tube shoulder and the dipping electrode. Fill the tube with electrolyte up to 10 mm from the end after inserting the electrode. Start the measurement application of voltag

32、e 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. DIN EN 15384-2:2017-04 EN 15384-2:2017 (E) 7 5 Tolerances The tolerances given in this standard a

33、re based on long-term experiences and are valid only for membrane tubes. For tubes with special conification angles and 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 to

34、lerance 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

35、 45 80 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 always be tested. NOTE 1 Test apparatus from different suppliers m

36、ay give different results. In this case comparative measurements and correlations factors may be required. NOTE 2 The tolerances given in Table 2 are only valid for standard tubes and not for tubes with additional treatment such as sterilization. 6 Test report Unless otherwise agreed between both pa

37、rties 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) registering number

38、 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 are not covered b

39、y this standard, k) date, place and name of the inspector. DIN EN 15384-2:2017-04 EN 15384-2:2017 (E) 8 Bibliography 1 EN 12374, Packaging - Flexible tubes - Terminology 2 EN 13046, Packaging - Flexible cylindrical metallic tubes - Dimensions and tolerances 3 EN 13047, Packaging - Flexible conical metallic tubes - Dimensions and tolerances 4 ISO 2859-1, Sampling procedures for inspection by attributes Part 1: Sampling schemes indexed by acceptance quality limit (AQL) for lot-by-lot inspection DIN EN 15384-2:2017-04