1、BSI Standards PublicationBS ISO 15106-7:2015Plastics Film and sheeting Determination of water vapourtransmission ratePart 7: Calcium corrosion methodBS ISO 15106-7:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 15106-7:2015.The UK participation in its pre
2、paration was entrusted to Technical Committee PRI/75, Plastics and rubber film and sheets.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 contract. Users are responsible f
3、or its correct application. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 85831 4ICS 83.140.10Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Polic
4、y and Strategy Committee on 30 April 2015.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 15106-7:2015 ISO 2015Plastics Film and sheeting Determination of water vapour transmission rate Part 7: Calcium corrosion methodPlastiques Film et feuille Dtermination du coeffi
5、cient de transmission de vapeur deau Partie 7: Mthode de la corrosion du calciumINTERNATIONAL STANDARDISO15106-7First edition2015-04-15Reference numberISO 15106-7:2015(E)BS ISO 15106-7:2015ISO 15106-7:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2015All rights reserved. Unl
6、ess otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the
7、address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 15106-7:2015ISO 15106-7:2015(E)Foreword iv1 Scope . 12 Terms and defi
8、nitions . 13 Principle 14 Test specimens 15 Conditioning 26 Apparatus, procedure, and calculation . 27 Test conditions . 28 Test result 29 Precision . 310 Test report . 3Annex A (normative) Optical measurement method 4Annex B (normative) Electrical measurement method 6Annex C (normative) Corrosion a
9、rea evaluation method . 8Bibliography .10 ISO 2015 All rights reserved iiiContents PageBS ISO 15106-7:2015ISO 15106-7:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing Internationa
10、l Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO,
11、also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1
12、. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Attention is drawn to the possibility that some of the elem
13、ents of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations receive
14、d (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adhere
15、nce to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 61, Plastics, Subcommittee SC 11, Products.ISO 15106 consists of the following parts, under the general title Plastics F
16、ilm and sheeting Determination of water vapour transmission rate: Part 1: Humidity detection sensor method Part 2: Infrared detection sensor method Part 3: Electrolytic detection sensor method Part 4: Gas-chromatographic detection sensor method Part 5: Pressure sensor method Part 6: Atmospheric pres
17、sure ionization mass spectrometer method Part 7: Calcium corrosion methodiv ISO 2015 All rights reservedBS ISO 15106-7:2015Plastics Film and sheeting Determination of water vapour transmission rate Part 7: Calcium corrosion method1 ScopeThis part of ISO 15106 specifies a method for determining the w
18、ater vapour transmission rate of plastic film, plastic sheeting, and multi-layer structures including plastics based on measurements of calcium degradation due to the reaction with water.NOTE The method provides rapid measurement over a wide range of water vapour transmission rates.2 Terms and defin
19、itionsFor the purposes of this document, the following terms and definitions apply.2.1water vapour transmission rateamount of water vapour transmitted through unit area of test specimen per unit time under specified conditionsNote 1 to entry: Water vapour transmission rate is expressed in grams per
20、square metre per 24 h g/(m224 h).2.2seal materialadhesive materials between test specimen and glass slide for protecting the calcium film from the corrosive gas2.3encapsulantencapsulation material for protecting the calcium film from the corrosive gas3 PrincipleThe calcium test method is based on me
21、asuring the rate of reaction between calcium metal and water. A calcium film is deposited on a test specimen or a glass slide and sealed or encapsulated according to one of the three procedures described in Annex A, Annex B, and Annex C. The water vapour transmission rate is determined from the chan
22、ge of calcium film properties after exposure in an environmental chamber as described in Annex A, Annex B, and Annex C.4 Test specimens4.1 The test specimens shall be representative of the material, free from wrinkles, creases and pinholes, and have uniform thickness. Each test specimen shall have a
23、 larger area than the transmission area of the cell.4.2 Three test specimens shall be tested unless otherwise specified or agreed between the interested parties.NOTE For some products, testing more than three test specimens gives a more representative result.INTERNATIONAL STANDARD ISO 15106-7:2015(E
24、) ISO 2015 All rights reserved 1BS ISO 15106-7:2015ISO 15106-7:2015(E)5 ConditioningCondition the test specimens in vacuum or inert atmosphere. The period of conditioning shall be as stated in the relevant specification for the material.NOTE For some products, heating the test specimen is effective
25、for rapid conditioning.6 Apparatus, procedure, and calculation6.1 Vacuum evaporatorThe vacuum evaporator comprises a metal evaporation source, a substrate holder, a thickness monitor, and a shutter mechanism. The calcium metal shall be evaporated at less than 102Pa. In addition, the substrate temper
26、ature shall be kept low enough to prevent heating damage of specimen. A deposition mask technique shall be used for the calcium film area control.6.2 GloveboxThe water and oxygen content shall be less than 40 ppm in the glove box. The glove box shall have the mechanism for transporting a calcium fil
27、m substrate from the vacuum chamber without exposure to atmosphere.6.3 Environmental chamberThe temperature in the environmental chamber shall be kept within 0,5 C. In addition, the relative humidity shall be within 3 %.6.4 Of the several methods available for measuring the amount of water vapour pe
28、rmeating through a specimen, three are described in the annexes. Annex A: Optical measurement method Annex B: Electrical measurement method Annex C: Corrosion area evaluation method7 Test conditionsThe test conditions shall preferably be chosen from those given in Table 1.Table 1 Choice of test cond
29、itionsTest conditions Temperature Relative humidityC %1 25 0,5 90 32 40 0,5 90 33 60 0,5 90 34 85 0,5 85 3Test conditions other than these shall be agreed upon by the interested parties.8 Test resultCalculate the test result as the arithmetic mean of the results obtained for each test specimen, roun
30、ding to two significant figures.2 ISO 2015 All rights reservedBS ISO 15106-7:2015ISO 15106-7:2015(E)9 PrecisionThe precision of this test method is not known because interlaboratory data are not available. When interlaboratory data are obtained, a precision statement will be added at the following r
31、evision.10 Test reportThe test report shall include the following information:a) a reference to this part of ISO 15106, i.e. ISO 15106-7;b) the test conditions;c) the name of the apparatus used;d) all details necessary for identification of the sample tested;e) the method of preparation of the test
32、specimens;f) the side of the test specimen which faced the supply of water vapour, if necessary;g) the transmission area of the test specimen;h) the mean thickness of the test specimen;i) the number of specimens tested;j) details of specimen conditioning;k) the test result;l) the date of the test. I
33、SO 2015 All rights reserved 3BS ISO 15106-7:2015ISO 15106-7:2015(E)Annex A (normative) Optical measurement methodA.1 ApparatusA.1.1 GeneralThe apparatus includes a test cell and a spectrophotometer.A.1.2 Test cellThe test cell structure is shown in Figure A.1. The test cell size shall typically be f
34、rom 20 mm to 100 mm. The calcium film thickness shall typically be from 10 nm to 500 nm.A.1.3 SpectrophotometerThe spectrophotometer shall measure the change of optical properties of the calcium film precisely.The device has the performance that can detect an optical transmittance. The measurement s
35、hall be carried out under conditions of the constant temperature and humidity.Key1 light source2 test specimen3 seal material4 calcium film5 substrate6 light detectorFigure A.1 Example of calcium test cell structureA.2 ProcedureA.2.1 Measure the water vapour transmission rate (WVTR) of each specimen
36、 as described in A.2.2 to A.2.5.4 ISO 2015 All rights reservedBS ISO 15106-7:2015ISO 15106-7:2015(E)A.2.2 A measurement setup is shown in Figure A.1. The deposited calcium film is applied onto the substrate. The substrate is hermetically sealed using a seal material and the test specimen (or the gla
37、ss slide) under inert atmosphere. Then, the test cell is transferred to an environmental chamber for accelerated ageing.A.2.3 The optical transmission of the test cell is measured throughout the test period using a spectrophotometer.A.2.4 The rate of calcium corrosion is calculated from change of op
38、tical transmission.A.2.5 Repeat steps A.2.3 and A.2.4 and calculate the water vapour transmission rate (WVTR) each time. When the WVTR remains constant, indicating that permeation has reached a steady state, record this value.A.3 CalculationCalculate the water vapour transmission rate of each test s
39、pecimen using Formula (A.1).WVTRHOCaCapCa2=2MMddf OdtSS()(A.1)whereWVTR is the water vapour transmission rate of the test specimen, in g/(m224 h);MHO2is the molecular weight of water, in grams per mole;MCais the molecular weight of calcium, in grams per mole;dCais the density of calcium, in grams pe
40、r cubic metre;Opis the optical transmission;fOp()is the calibration function of calcium film thickness, in metres;SCais the area of the calcium film, in square metres;S is the transmission area of the water vapour surrounded with the edge seal of the speci-men, in square metres.NOTE The calibration
41、function of the calcium film thickness is determined from the relationship between optical transmission and calcium film thickness. ISO 2015 All rights reserved 5BS ISO 15106-7:2015ISO 15106-7:2015(E)Annex B (normative) Electrical measurement methodB.1 ApparatusB.1.1 GeneralThe apparatus includes a
42、test cell and ohmmeter.B.1.2 Test cellThe test cell structure is shown in Figure B.1. The test cell size shall typically be from 20 mm to 100 mm. The calcium film thickness shall typically be from 10 nm to 500 nm.B.1.3 OhmmeterThe ohmmeter has to be able to measure the change of electrical resistanc
43、e of the calcium film precisely.Key1 ohmmeter2 test specimen3 seal material4 electrode5 calcium film6 substrateFigure B.1 Example schematic representation of calcium test setupB.2 ProcedureB.2.1 Measure the water vapour transmission rate (WVTR) of each specimen as described in B.2.2 to B.2.6.B.2.2 A
44、 measurement setup is shown in Figure B.1. The electrodes for the resistivity measurement are deposited onto the substrate. After a deposited calcium film has been applied, it is hermetically sealed under inert atmosphere using a seal material and a test specimen.6 ISO 2015 All rights reservedBS ISO
45、 15106-7:2015ISO 15106-7:2015(E)B.2.3 The test cell is transferred to an environmental chamber for accelerated ageing under a specific condition. The ohmmeter is connected to the electrode.B.2.4 The resistivity is measured throughout the test period using an ohmmeter.B.2.5 The rate of calcium corros
46、ion is calculated from a change in resistivity of the calcium film.B.2.6 Repeat steps B.2.4 or B.2.5 and calculate the water vapour transmission rate (WVTR) each time. When WVTR remains constant, indicating that permeation has reached steady state, record this value.B.3 CalculationCalculate the wate
47、r vapour transmission rate of each test specimen using Formula (B.1).WVTRHOCaCaCa2= 21MMddRdtabSS(/) (B.1)whereWVTR is the water vapour transmission rate of the test specimen, in g/(m224 h);MHO2is the molecular weight of water, in grams per mole;MCais the molecular weight of calcium, in grams per mo
48、le;dCais the density of calcium, in grams per cubic metre; is the volume resistivity, in m;d(1/R)/dt is the rate of change of the conductance, in 1/(24 h);a is the length of the calcium film, in metres;b is the width of the calcium film, in metres;SCais the area of the calcium film between electrode
49、s, in square metres;S is the water vapour transmission area surrounded with the edge seal of the speci-men, in square metres. ISO 2015 All rights reserved 7BS ISO 15106-7:2015ISO 15106-7:2015(E)Annex C (normative) Corrosion area evaluation methodC.1 ApparatusC.1.1 GeneralThe apparatus includes a test cell and a microscope.C.1.2 Test cellThe test cell structure is shown in Figure C.1. The test cell size shall typi
