1、 Reference number ISO/TR 19032:2006(E) ISO 2006TECHNICAL REPORT ISO/TR 19032 First edition 2006-10-01 Plastics Use of polyethylene reference specimens (PERS) for monitoring laboratory and outdoor weathering conditions Plastiques Utilisation dprouvettes de rfrence en polythylne pour lvaluation des co
2、nditions de vieillissement climatique ISO/TR 19032:2006(E) 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 and installed on the
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5、 the Central Secretariat at the address given below. ISO 2006 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 microfilm, without permission in writing from eit
6、her 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 ii ISO 2006 All rights reservedISO/TR 19032:2006(E) I
7、SO 2006 All rights reserved iii Contents Page Foreword iv Introduction v 1 Scope1 2 Background information .1 3 Material.1 3.1 Preparation of PERS1 4 Procedure.2 4.1 Method for measuring the carbonyl index of PERS.2 4.2 Round Robin Test of laboratory light-source exposure devices with PERS 3 4.2.1 X
8、enon-arc-lamp exposure.3 4.2.2 Open-flame carbon-arc-lamp exposure.3 4.2.3 Fluorescence lamp exposure.4 4.3 Outdoor exposure test of PERS.4 4.4 Consistency of laboratory light-source exposure devices .5 5 Results and discussion.6 5.1 Result of RRT of laboratory light-source exposure devices with PER
9、S6 5.1.1 Xenon-arc-lamp exposure.6 5.1.2 Open-flame carbon-arc-lamp exposure.10 5.1.3 Fluorescent lamp exposure10 5.2 Characterizing the conditions of outdoor exposure test site .11 5.3 Examples of correlation between outdoor exposure test and laboratory light-source exposure test using PERS12 5.4 C
10、ontrol limit of particular laboratory light-source exposure apparatus13 6 Conclusion.14 6.1 Results of RRT .14 6.2 Outdoor exposure of PERS 15 6.3 Correlation between outdoor and xenon-arc-lamp exposure for PERS 15 6.4 Consistency of laboratory light-source exposure devices .15 Bibliography 16 ISO/T
11、R 19032:2006(E) iv ISO 2006 All rights reservedForeword ISO (the International Organization for 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 me
12、mber 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, also take part in the work. ISO collaborates closely with the International E
13、lectrotechnical Commission (IEC) on all matters of electrotechnical standardization. International 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 ad
14、opted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. In exceptional circumstances, when a technical committee has collected data of a different kind from that
15、 which is normally published as an International Standard (“state of the art”, for example), it may decide by a simple majority vote of its participating members to publish a Technical Report. A Technical Report is entirely informative in nature and does not have to be reviewed until the data it pro
16、vides are considered to be no longer valid or useful. 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. ISO/TR 19032 was prepared by Technical Committe
17、e ISO/TC 61, Plastics, Subcommittee SC 6, Ageing, chemical and environmental resistance. ISO/TR 19032:2006(E) ISO 2006 All rights reserved v Introduction The method described in this Technical Report demonstrates the use of polyethylene reference specimens (hereafter called PERS) for monitoring cond
18、itions in weathering tests used for plastics. The PERS has double bonds in its molecular structure, which are easily oxidized to produce carbonyl groups. The change in carbonyl index of PERS is produced by the combined effects of ultraviolet (UV) and temperature. Therefore, the carbonyl groups propo
19、rtionally increase, depending on the received UV and temperature. Based on this relationship, the effect of UV radiation and temperature on PERS can be expressed quantitatively. For laboratory-accelerated exposures, PERS is also sensitive to changes in the chamber air temperature. The effect of mois
20、ture was not determined in the study. TECHNICAL REPORT ISO/TR 19032:2006(E) ISO 2006 All rights reserved 1 Plastics Use of polyethylene reference specimens (PERS) for monitoring laboratory and outdoor weathering conditions 1 Scope This Technical Report describes a method that demonstrates the use of
21、 polyethylene reference specimens (PERS) for monitoring laboratory and outdoor conditions in weathering tests used for plastics. 2 Background information Degradation of plastics in an outdoor environment is mainly influenced by the ultraviolet radiation received, environmental temperature, moisture,
22、 etc. Especially in photo-oxidation induced from ultraviolet radiation, temperature plays a very important role. Measuring the ultraviolet radiation during the exposure period is useful for comparison of the result of the exposure test, but it is not enough to compare the exposure results. Therefore
23、, it is very important to find some index that can be used to evaluate the complex effect of received ultraviolet radiation and environmental temperature. The PERS is used to characterize the level of combined effect of ultraviolet radiation and temperature, and its characteristic proportionally inc
24、reases depending on the UV radiation and temperature received. 3 Material PERS is high-density polyethylene polymerized using molybdenum dioxide as a catalyst, containing the trans- form vinylene group. Other basic properties are as follows: absorbance ratio of trans-form vinylene group to methylene
25、 group: 1,0 to 1,3; melt flow rate (2,16 kg, 190 C): 0,2 to 0,4 g/10 min; density: 950 to 965 kg/m 3 ; thickness: (0,2 0,02) mm. 3.1 Preparation of PERS After kneading for 5 min the material between two rolls whose surfaces are heated at 150 C to 170 C, cut into small pieces of 0,4 g to 0,5 g. After
26、 pre-heating for 90 s in a compression moulding machine whose surface is heated at 160 C to 180 C, compress the material for 60 s, cool in a compression moulding machine whose surface temperature is 30 C to 40 C, for 60 s, and prepare the press sheet of the thickness mentioned above. NOTE PERS can b
27、e obtained from the following organization: Japan Weathering Test Center 1-3-7 Shibakoen Minatoku Tokyo Japan ISO/TR 19032:2006(E) 2 ISO 2006 All rights reserved4 Procedure 4.1 Method for measuring the carbonyl index of PERS An infrared (IR) spectrophotometer should be used as the measuring apparatu
28、s. Measure the infrared absorption spectra after irradiation, in the range of 2 200 cm 1to 1 600 cm 1 . In this case, use for the scanning speed the same method as for a quantitative analysis. The carbonyl index is determined in accordance with the following equation, based upon infrared absorbance
29、spectra of exposed PERS. Absorbance at near 2 020 cm 1peak is employed as an internal standard to correct for sample film thickness, while absorbance at near 1 715 cm 1peak is used to indicate carbonyl group content. A typical diagram of IR absorbance is shown in Figure 1. 1715 2020 r A A A = where
30、A ris the absorbance ratio (carbonyl index); A 1 715is the absorbance at near 1 715 cm 1(I I 0 ); A 2 020is the absorbance at near 2 020 cm 1(I I 0 ); I 0is the absorbance measured by the base-line method at individual wave number; I is the absorbance at the peak of individual wave number. Key Y abs
31、orbance X wavenumber (cm 1 ) 1 peak near 2 020 cm 12 peak near 1 715 cm 1Figure 1 IR absorbance diagram showing base line and peak absorbance ISO/TR 19032:2006(E) ISO 2006 All rights reserved 3 4.2 Round Robin Test of laboratory light-source exposure devices with PERS It is well known that the degra
32、dation of plastics materials or products used outdoors will occur by the combined effect of ultraviolet radiation and temperature, or other factors. It is also recognized that the reproducibility in the laboratory light-source exposure test will vary with the change in ultraviolet spectrum distribut
33、ions and the chamber temperatures caused by deterioration of lamps and filters with operating time, even if ultraviolet radiation and black standard temperature (BST) or black panel temperature (BPT) are under constant conditions. Since the PERS can quantitatively evaluate, as carbonyl index, the co
34、mbined effect of UV radiation and temperature, the carbonyl index obtained can reflect changes in a given environment. In order to verify the repeatability and reproducibility of the specimens and exposure test, the Round Robin Test (hereafter called RRT) using the PERS by laboratory light-source ex
35、posure devices in ISO/TC 61/SC 6/WG 2 was conducted. 4.2.1 Xenon-arc-lamp exposure The test conditions were according to ISO 4892-21 . The conditions are shown in Table 1. It was not requested to control the chamber temperature, but participants were requested to report this temperature. Each partic
36、ipant was provided with 4 sets of PERS that were mounted in 150 mm 70 mm plastics holders. One set of holders consists of 3 pieces of PERS. Table 1 Exposure conditions for xenon-arc lamp Filter daylight filter Irradiance 0,5 W/(m 2 nm) at 340 nm or 60 W/m 2(300 to 400 nm) BST or BPT (65 3) C for BST
37、 or (63 3) C for BPT Chamber temperature Arbitrary Water spray 102 min of light only followed by 18 min of light plus water spray Humidity (50 5) % Period 24 h, 48 h, 72 h and 96 h 4.2.2 Open-flame carbon-arc-lamp exposure The test conditions were according to ISO 4892-42 . The conditions are shown
38、in Table 2. The chamber temperature was not specified, but participants were requested to report this temperature. Each participant was provided with 4 sets of PERS that were mounted in 150 mm 70 mm plastics holders. One set of holders consists of 3 pieces of PERS. Table 2 Exposure conditions for op
39、en-flame carbon-arc lamp Filter Type 1 (Type 1 known as Corex 7058 filter) BST or BPT (65 3) C for BST or (63 3) C for BPT Chamber temperature Arbitrary Water spray 102 min light only followed by 18 min of light plus water spray Humidity (50 5) % Period 24 h, 48 h, 72 h and 96 h ISO/TR 19032:2006(E)
40、 4 ISO 2006 All rights reserved4.2.3 Fluorescence lamp exposure The test conditions were according to ISO 4892-33 . The conditions are shown in Table 3. Irradiance was not specified at any intensity. Each participant was provided with 4 sets of PERS that were mounted in 150 mm 70 mm plastics holders
41、. One set of holders consists of 3 pieces of PERS. Table 3 Exposure conditions for fluorescent lamp Lamp type UVA340 Irradiance Arbitrary Mode Mode 1: 4 h of dry UV exposure followed by 4 h of condensation BPT (63 3) C at UV exposure and (50 3) C at condensation Period 8 h, 24 h, 32 h and 48 h After
42、 each sample had been exposed for each exposure period, the carbonyl index was determined, based upon the method described in 4.1. 4.3 Outdoor exposure test of PERS The result of the outdoor exposure test varies, even if it is conducted in the same place, because of differences due the seasonal clim
43、ate changes. Although it is useful to measure the amount of ultraviolet radiation for comparison of exposure tests, it is not enough in the comparison only to consider the amount of ultraviolet radiation, because plastics are influenced not only by ultraviolet radiation but by temperature or by mois
44、ture. Since PERS is influenced by the combined effect of ultraviolet radiation and temperature, PERS were exposed in various places where the climate was different. Six locations in different climates and different countries were selected: Sapporo, Choshi, Miyakojima (Japan), Serpong, Bandung (Indon
45、esia) and Phoenix (USA). Locations and exposure angles are shown in Table 4. Table 4 Locations and exposure angles Exposure site Exposure angle Latitude Sapporo (Japan) 45South 43 03 N Choshi (Japan) 30South 35 43 N Miyakojima (Japan) 20South 24 44 N Serpong (Indonesia) 5aSouth and north 6 15 S Phoe
46、nix (USA) 34South 33 54 N a From November to February, the samples face south; and from March to October, they face north. ISO/TR 19032:2006(E) ISO 2006 All rights reserved 5 The conditions of the outdoor exposure test are based on ISO 8774 . Three pieces of PERS were exposed for 1 month. By replaci
47、ng exposed PERS with new ones, the exposure test was repeated in the following months successively. The exposure test was repeated successively for more than 24 months. The practical procedure of the outdoor exposure test is shown below. 1) The conditions of the outdoor exposure test are based on IS
48、O 877. 2) Prepare a minimum of three PERS and expose them for 1 month. It is desirable to expose them at the beginning of a calendar month, in order to evaluate the condition of the month. 3) By replacing exposed PERSs with new ones, the exposure test is repeated in the following months successively
49、. 4) The exposure test is repeated successively for at least 12 months. 5) The accumulated value of the carbonyl index for each month will be adopted for the index of combined effect of UV radiation and temperature at the site of exposure. 4.4 Consistency of laboratory light-source exposure devices It is recognized that changes in the characteristics of lamps and filters with time, and changes in the chamber temperature of laboratory light-sourc
