1、BSI Standards PublicationBS ISO 15106-6:2015Plastics Film and sheeting Determination of water vapourtransmission ratePart 6: Atmospheric pressure ionizationmass spectrometer methodBS ISO 15106-6:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 15106-6:2015.
2、The UK participation in its preparation 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 co
3、ntract. Users are responsible for its correct application. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 85830 7ICS 83.140.10Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the a
4、uthority of the Standards Policy 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 15106-6:2015 ISO 2015Plastics Film and sheeting Determination of water vapour transmission rate Part 6: Atmospheric pressure ionization mass spect
5、rometer methodPlastiques Film et feuille Dtermination du coefficient de transmission de vapeur deau Partie 6: Mthode utilisant un spectromtre de masse ionisation sous pression atmosphriqueINTERNATIONAL STANDARDISO15106-6First edition2015-04-15Reference numberISO 15106-6:2015(E)BS ISO 15106-6:2015ISO
6、 15106-6:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2015All rights reserved. Unless 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 in
7、ternet or an intranet, without prior written permission. Permission can be requested from either ISO at the 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
8、.iso.orgPublished in SwitzerlandBS ISO 15106-6:2015ISO 15106-6:2015(E)Foreword iv1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Test specimens 26 Conditioning 27 Apparatus . 28 Test condition 39 Calibration graph . 410 Procedure. 511 Calculation 612 Test result 613 Prec
9、ision . 614 Test report . 6Bibliography 8 ISO 2015 All rights reserved iiiContents PageBS ISO 15106-6:2015ISO 15106-6:2015(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 15106-6:2015Plastics Film and sheeting Determination of water vapour transmission rate Part 6: Atmospheric pressure ionization mass spectrometer method1 ScopeThis part of ISO 15106 specifie
18、s a method for determining the water vapour transmission rate of plastic film, plastic sheeting, and multi-layer structures including plastics, using an atmospheric pressure ionization mass spectrometric detection sensor.NOTE The method provides rapid measurement over a wide range of water vapour tr
19、ansmission rates.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (inc
20、luding any amendments) applies.ISO 6145-8, Gas analysis Preparation of calibration gas mixtures using dynamic volumetric methods Part 8: Diffusion method3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1water vapour transmission rateamount of wate
21、r 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 square metre per 24 h g/(m224 h).4 PrincipleThe gas transmission cell is designed in such a way that, with the test specimen inser
22、ted, it is divided into a dry chamber and a wet chamber. The dry side of the specimen is swept by a flow of dry carrier gas such as nitrogen or argon, and water vapour permeating through the specimen from the wet chamber is carried by the carrier gas into an atmospheric pressure ionization mass spec
23、trometer. This sensor contains an ion formation region near atmospheric pressure and a mass analysis region in ultra-high vacuum. The carrier gas with the moisture is introduced into the ion formation region where the carrier gas is ionized as primary ions by corona discharge ion sources, and then,
24、an ion-molecule reaction is produced between the primary ions and water molecules contained in the carrier gas and the water molecules are ionized. These ionized water molecules are fed to the mass analysis region. Water vapour content in the range between ppt and ppb in the carrier gas can be detec
25、ted as an ion intensity of mass number (m/z) of ion species, such as H2O+at m/z 18, H3O+at m/z 19, and H+(H2O)2at m/z 37. These are produced by ionization of water in the ion source and determined using a calibration curve. The mass of the water vapour which permeates through the specimen per unit t
26、ime is calculated from the ion intensity of the water molecules.INTERNATIONAL STANDARD ISO 15106-6:2015(E) ISO 2015 All rights reserved 1BS ISO 15106-6:2015ISO 15106-6:2015(E)5 Test specimens5.1 The specimens shall be representative of the material, be free from wrinkles, creases, and pinholes, and
27、have uniform thickness. Each specimen shall have a larger area than the transmission area of the cell used for the test.5.2 Three specimens shall be tested unless otherwise specified or agreed between the interested parties.NOTE For some products, testing more than three specimens gives a more repre
28、sentative result.6 ConditioningCondition the specimens at 23 C 2 C in a desiccator to prevent moisture uptake. 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 for rapid conditioning.7 Apparatu
29、s7.1 An example of a suitable apparatus is shown in Figure 1. The apparatus includes a transmission cell with two chambers, a dry chamber and a wet chamber between which a specimen is mounted, an atmospheric pressure ionization mass spectrometer to determine the amount of water vapour transmitted, t
30、wo flow controllers, a getter (for example, a molecular sieve), and a humidity controller (water reservoir).7.2 The diameter of the water vapour transmission area shall typically be 5 mm to 200 mm. The temperature of the transmission cell shall be kept within 0,5 C of the test temperature by means o
31、f a temperature controller.The size of non-circular samples shall be agreed upon by the interested parties.7.3 The flow controller shall be capable of regulating the flow rates of the carrier gas from 500 ml to 1 000 ml per minute.7.4 The getter shall be capable of reducing the moisture contents bel
32、ow 1 ppb.2 ISO 2015 All rights reservedBS ISO 15106-6:2015ISO 15106-6:2015(E)Key1 test specimen 7 getter (for example, a molecular sieve)2 transmission cell 8 atmospheric pressure ionization mass spectrometer3 dry chamber 9 gas supply4 wet chamber 10 mass flow controller5 gas supply 11 humidity cont
33、roller with distilled or deionized water (water reservoir)6 mass flow controller 12 gas exhaustFigure 1 Example of water vapour transmission rate measuring apparatus with atmospheric pressure ionization mass spectrometric detection sensor7.5 Atmospheric pressure ionization mass spectrometerThe atmos
34、pheric pressure ionization mass spectrometer shall be able to measure the ion intensity of ion species, such as H2O+at m/z 18, H3O+at m/z 19, and H+(H2O)2at m/z 37 with an accuracy of at least 0,01 parts per billion by volume.7.6 Gas flow controllerThe gas flow controller shall be capable of maintai
35、ning the gas flow to the carrier gas passed through the dry and wet chambers and the humidity controller at a constant rate.The recommended flow rate is between 500 ml/min and 1 000 ml/min.7.7 Humidity controller (water reservoir)A humidity controller that contains distilled or deionized water is co
36、nnected to the wet chamber. The temperature of the water in the reservoir shall be kept at the temperature of the transmission cell (see Table 1). Gas shall be supplied to the humidity controller through the gas flow controller. The gas is bubbled through the water in the reservoir and becomes satur
37、ated with water vapour at the given temperature.8 Test conditionThe test conditions should preferably be chosen from those given in Table 1. ISO 2015 All rights reserved 3BS ISO 15106-6:2015ISO 15106-6:2015(E)Table 1 Choice of test conditionsTest conditions Temperature Relative humidityC %1 25 0,5 9
38、0 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.9 Calibration graph9.1 Prepare a low-level humidity standard in accordance with ISO 6145-8 (diffusion method) or by another suitable method.For example, in order to obtain a rang
39、e of water vapour concentration between ppt and ppb for the calibration gas, the standard moisture is diluted over 104times as shown in Figure 2 using a two stage dilution method. A small amount of water vapour from the humidity standard is diluted by controlling the two large volumes of dry gas by
40、MFC1 and MFC2 to obtain the calibration gas with a lower water vapour content.9.2 Inject the calibration gas with a known trace level humidity into the atmospheric pressure ionization mass spectrometer and record the relative ion intensity expressed as ratio of water ion intensity to total ion inten
41、sity. In the atmospheric pressure ionization mass spectrometer analysis, water is observed in the form of several ion species, such as H2O+at m/z 18, H3O+at m/z 19, and H+(H2O)2at m/z 37. The water ion intensity is obtained by the sum of the ion intensities of those three different ion species. Prod
42、uce a calibration graph by plotting the moisture content against the water ion intensity.4 ISO 2015 All rights reservedBS ISO 15106-6:2015ISO 15106-6:2015(E)Key1 gas supply2 getter (for example, a molecular sieve)3 mass flow controller for dilution (MFC1)4 mass flow controller for dilution (MFC2)5 g
43、eneration chamber6 mass flow controller for evacuation (MFC3)7 mass flow controller for evacuation (MFC4)8 atmospheric pressure ionization mass spectrometric detection sensor9 gas exhaust10 gas exhaustFigure 2 Example of a two stage dilution method for calibration gas with controlled water content i
44、n the ppm-ppt range10 Procedure10.1 Measure the water vapour transmission rate of each specimen as described in 10.2 to 10.6.10.2 Place the specimen between the dry and wet chambers (see Figure 1), and close the transmission cell to give a hermetically sealed assembly.10.3 Sweep the carrier gas at t
45、he specified flow rate through the dry and wet chambers to remove all the moisture from both chambers. Care is necessary, because the time it takes to exhaust the cell completely might depend on the permeability of the specimen under test.The flow rate should be specified by the manufacturer of the
46、apparatus.10.4 Inject the carrier gas passed through the dry chamber into the atmospheric pressure ionization mass spectrometer. Determine the water ion intensity of ion species, such as H2O+at m/z 18, H3O+at m/z 19, and H+(H2O)2at m/z 37 corresponding to water vapour. When the ion intensity remains
47、 constant, indicating that the leakages of water to the carrier gas from the outside of the water vapour permeation apparatus have minimized, determine from the calibration graph prepared in Clause 9 the concentration of water vapour C0in the carrier gas passed through the dry chamber. ISO 2015 All
48、rights reserved 5BS ISO 15106-6:2015ISO 15106-6:2015(E)10.5 Introduce water vapour into the wet chamber through the humidity controller in such a way that the wet chamber is kept at constant humidity. Water vapour permeating from the wet chamber to the dry chamber through the specimen is swept by th
49、e carrier gas into atmospheric pressure ionization mass spectrometric detection sensor.10.6 Monitor the water ion intensity of ion species such as H2O+at m/z 18, H3O+at m/z 19, and H+(H2O)2at m/z 37, from the atmospheric pressure ionization mass spectrometer until it reaches steady state. Determine the concentration of water vapour Cffrom the calibration graph prepared in Clause 9.11 CalculationCalculate the water vapour transmission rate of each test specimen using Formula (1):WVTR =(
