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1、INTERNATIONAL STANDARD ISO 15106-4 First edition 2008-06-01 Reference number ISO 15106-4:2008(E) ISO 2008 Plastics Film and sheeting Determination of water vapour transmission rate Part 4: Gas-chromatographic detection sensor method Plastiques Film et feuille Dtermination du coefficient de transmiss
2、ion de vapeur deau Partie 4: Mthode utilisant un dtecteur chromatographie en phase gazeuse Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 04:06:46 MDTNo reproduction or networking permitted with
3、out license from IHS -,-,- ISO 15106-4:2008(E) ii ISO 2008 All rights reserved PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to a
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6、found, please inform the Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2008 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and
7、microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland Copy
8、right International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 04:06:46 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15106-4:2008(E) ISO 2008 All rights reserved iii Contents Page 1
9、Scope 1 2Normative references 1 3Terms and definitions 1 4Principle 1 5Test specimens 1 6Conditioning . 2 7Apparatus . 2 8Test conditions 4 9Calibration graph . 4 10Procedure . 4 11Calculation . 5 12Test result . 5 13Precision . 5 14Test report 6 Bibliography . 7 Copyright International Organization
10、 for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 04:06:46 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15106-4:2008(E) iv ISO 2008 All rights reserved Foreword ISO (the International Organization for
11、 Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International 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
12、right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Internatio
13、nal Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication a
14、s an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. I
15、SO 15106-4 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 11, Products. ISO 15106 consists of the following parts, under the general title Plastics Film and sheeting Determination of water vapour transmission rate: Part 1: Humidity detection sensor method Part 2: Infrared d
16、etection sensor method Part 3: Electrolytic detection sensor method Part 4: Gas-chromatographic detection sensor method Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 04:06:46 MDTNo reproduction
17、 or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARDISO 15106-4:2008(E) ISO 2008 All rights reserved 1 Plastics Film and sheeting Determination of water vapour transmission rate Part 4: Gas-chromatographic detection sensor method 1Scope This part of ISO 15106 specifies an i
18、nstrumental method for determining the water vapour transmission rate of single-layer plastic film and sheet, as well as multi-layer structures including plastics, using a gas chromatograph. NOTEThe method provides rapid measurement over a wide range of water vapour transmission rates. 2Normative re
19、ferences The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 4593, Plastics Film and sheeting Det
20、ermination of thickness by mechanical scanning 3Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 water vapour transmission rate WVTR amount of water vapour transmitted through unit area of test specimen per unit time under specified conditions N
21、OTEWater vapour transmission rate is expressed in grams per square metre 24 hours . 4Principle A dry chamber, evacuated by a vacuum pump, is separated from a wet chamber, in which the relative humidity of a gas flow is controlled at a specified level, by a test specimen. The water vapour transmitted
22、 through the specimen is collected in a sampling loop for a certain period of time. The absolute mass of the water collected is measured using a gas chromatograph. The water vapour transmission rate is then calculated from the mass of water vapour transmitted, the period of time and the transmission
23、 area of the specimen. 5Test specimens 5.1The specimens shall be representative of the material, be free from wrinkles, creases and pinholes, and have uniform thickness. Each specimen shall have a larger area than the transmission area of the cell, and shall be hermetically mounted. 5.2Three determi
24、nations shall be made using separate specimens unless otherwise specified or agreed between the interested parties. g/(m224 h) Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 04:06:46 MDTNo repro
25、duction or networking permitted without license from IHS -,-,- ISO 15106-4:2008(E) 2 ISO 2008 All rights reserved NOTEFor some products, testing more than three specimens gives a more representative result. 5.3Unless otherwise specified, determine the thickness of each specimen in accordance with IS
26、O 4593 at three equally spaced points. 6Conditioning The specimens, whose thickness has been determined in accordance with ISO 4593, shall be conditioned at the same temperature and humidity as specified for the test for a length of time appropriate to the material under test, unless otherwise agree
27、d between the interested parties. NOTEIf the gas-chromatographic apparatus includes a test cell having an automatic conditioning system, the test specimens can be placed in the cell for conditioning. 7Apparatus 7.1General An example of a suitable apparatus is shown in Figure 1. The apparatus include
28、s a gas transmission cell with two chambers, a sampling loop for holding permeated water vapour, switching valves, a gas chromatograph, a humidity controller (water reservoir) and a vacuum pump. 7.2Transmission cell The transmission cell shall consist of a wet chamber (upper side of the cell in Figu
29、re 1) and a dry chamber (lower side of the cell). The wet chamber shall have an inlet for the water vapour and the dry chamber shall be connected to a gas chromatograph via a sampling loop. The surfaces of the transmission cell in contact with the specimen shall be smooth and flat so that leakage do
30、es not occur. The transmission area shall be from to . The temperature of the transmission cell shall be kept within of the test temperature by means of a temperature controller. The tubing system shall be kept at a higher temperature than that of the humidity controller in order to prevent the cond
31、ensation of water vapour. 7.3Gas chromatograph The gas chromatograph shall be able to measure the quantity of water vapour in carrier gas with an accuracy of at least . 7.4Gas flow controller The gas flow controller shall be capable of maintaining the gas flow to the humidity controller at a constan
32、t rate. The recommended flow rate is between and . 7.5Humidity controller (water reservoir) A humidity controller that contains distilled or deionized water is connected to the wet chamber. The temperature of the water in the reservoir shall be kept within of the temperature of the transmission cell
33、 (see Table 1). Gas shall be supplied to the humidity controller via the gas flow controller. The gas is bubbled through the water in the reservoir and becomes saturated with water vapour at that temperature. 7.6Vacuum pump The vacuum pump shall be capable of producing a vacuum lower than () in the
34、dry chamber. 0,5 cm2 100 cm20,5 C 0,05g 5 ml/min100 ml/min 0,2 C 10 Pa 0,075 mmHg Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 04:06:46 MDTNo reproduction or networking permitted without licen
35、se from IHS -,-,- ISO 15106-4:2008(E) ISO 2008 All rights reserved 3 Key 1specimen 2transmission cell 3wet chamber 4dry chamber with hydrophobic filter-paper 5gas supply 6gas controller 7humidity controller with distilled or deionized water (water reservoir) 8sampling loop 9gas chromatograph 10data
36、processor 11vacuum pump 12carrier gas for gas chromatograph 13gas exhaust 14carrier gas exhaust 15switching valve 1 16switching valve 2 Figure 1 Example of apparatus for measuring WVTR by gas chromatography Copyright International Organization for Standardization Provided by IHS under license with I
37、SO Licensee=Boeing Co/5910770001 Not for Resale, 07/25/2008 04:06:46 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15106-4:2008(E) 4 ISO 2008 All rights reserved 8Test conditions The test conditions should preferably be chosen from those given in Table 1. Test conditi
38、ons other than these, for example test conditions specified in ISO 291, shall be agreed upon by the interested parties. 9Calibration graph Prepare dilute solutions of water in alcohol at different levels of water concentration. Inject a known volume of each solution into the gas chromatograph using
39、a liquid syringe and record the chromatogram for each under the same conditions. Determine the area of the peak in the chromatogram corresponding to the injected water. Produce a calibration graph by plotting water concentration against peak area and drawing a straight line through the points. NOTEI
40、n the case of (by mass) of water in methanol, a straight line can be drawn from the origin through the point representing a measurement on this solution only. 10Procedure 10.1Spread a hydrophobic filter-paper (4 in Figure 1) having the same size as the gas transmission area over the bottom of the dr
41、y chamber. The hydrophobic filter-paper is used to support the specimen film and to ensure smooth water vapour transmission through the whole specimen area. A hydrophobic filter-paper recommended for this purpose is Polyflon1) filter-paper, which is made from polytetrafluoroethylene (PTFE). It is re
42、commended that the thickness of the filter be the same as the depth of the dry chamber. 10.2Apply a thin, uniform coating of vacuum grease on the flat edges of the two halves of the transmission cell, and mount a specimen over the dry chamber in such a way that no creasing or slackness occurs. 10.3P
43、lace a rubber sealing-ring on the specimen, then set up the upper part of the cell. Clamp the two chambers together with a uniform pressure so that the specimen is completely sealed in place. 10.4Start the vacuum pump and evacuate all the air from the dry chamber. Care is necessary here, because the
44、 time taken to exhaust the cell completely will depend on the permeability of the specimen under test. 10.5Introduce 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
45、dry chamber through the specimen is evacuated by the vacuum pump. Table 1 Choice of test conditions Set of test conditionsTemperatureRH of wet chamberRH of dry chamber 10 20 30 40 50 1)PolyflonTM is an example of a suitable product available commercially. This information is given for the convenienc
46、e of users of this part of ISO 15106 and does not constitute an endorsement by ISO of this product. C % 250,5902 380,5902 400,5902 230,5852 250,5752 1 % Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/25
47、/2008 04:06:46 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15106-4:2008(E) ISO 2008 All rights reserved 5 10.6By closing valve 2 (16 in Figure 1), start collecting the water vapour which permeates through the specimen in the sampling loop (8). After a predetermined
48、period of time , close valve 1 and sweep the water vapour which has accumulated in the sampling loop into the chromatographic column (9) with carrier gas (12). Using the integrator of the chromatograph, determine the area of the peak in the chromatogram corresponding to the water vapour. Determine, from the calibration graph prepared in Clause 9, the amount of water vapour which has accumulated in the sampling loop. It is recommend