1、October 2014 Translation by DIN-Sprachendienst.English price group 9No 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
2、 83.080.01!%;tl“2248173www.din.deDDIN EN ISO 11358-1Plastics Thermogravimetry (TG) of polymers Part 1: General principles (ISO 11358-1:2014);English version EN ISO 11358-1:2014,English translation of DIN EN ISO 11358-1:2014-10Kunststoffe Thermogravimetrie (TG) von Polymeren Teil 1: Allgemeine Grunds
3、tze (ISO 11358-1:2014);Englische Fassung EN ISO 11358-1:2014,Englische bersetzung von DIN EN ISO 11358-1:2014-10Plastiques Thermogravimtrie (TG) des polymres Partie 1: Principes gnraux (ISO 11358-1:2014);Version anglaise EN ISO 11358-1:2014,Traduction anglaise de DIN EN ISO 11358-1:2014-10Supersedes
4、DIN EN ISO 11358:1997-11www.beuth.deDocument comprises 14 pagesIn case of doubt, the German-language original shall be considered authoritative.09.14 DIN EN ISO 11358-1:2014-10 2 A comma is used as the decimal marker. National foreword This document (EN ISO 11358-1:2014) has been prepared by Technic
5、al Committee ISO/TC 61 “Plastics” (Secretariat: SAC, China) in collaboration with Technical Committee CEN/TC 249 “Plastics” (Secretariat: NBN, Belgium). The responsible German body involved in its preparation was the DIN-Normenausschuss Kunststoffe (DIN Standards Committee Plastics), Working Committ
6、ee NA 054-01-03 AA Physikalische, rheologische und analytische Prfungen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 291 DIN EN ISO 291 ISO 472 DIN EN ISO 472 ISO 11357-1 DIN EN ISO 11357-1 Amendments This standard differs from DIN
7、EN ISO 11358:1997-11 as follows: a) Clause 2 “Normative references” has been updated to include ISO 472 and ISO 11357-1 and Clause 3 “Terms and definitions” has been revised; b) apparatus specifications have been revised; c) Annex A relating to standard reference materials for calibration purposes h
8、as been deleted. Previous editions DIN EN ISO 11358: 1997-11 National Annex NA (informative) Bibliography DIN EN ISO 291, Plastics Standard atmospheres for conditioning and testing DIN EN ISO 472, Plastics Vocabulary DIN EN ISO 11357-1, Plastics Differential scanning calorimetry (DSC) Part 1: Genera
9、l principles EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11358-1 July 2014 ICS 83.080.01 Supersedes EN ISO 11358:1997English Version Plastics - Thermogravimetry (TG) of polymers -Part 1 : General principles (ISO 11358-1:2014) Plastiques - Thermogravimtrie (TG) des polymres -Partie 1: Pr
10、incipes gnraux (ISO 11358-1:2014) Kunststoffe - Thermogravimetrie (TG) von Polymeren - Teil 1: Allgemeine Grundstze (ISO 11358-1:2014) This European Standard was approved by CEN on 28 June 2014. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions
11、for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical 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 th
12、ree official versions (English, French, German). A version in any other language made by translation under the responsibility 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 b
13、odies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia,
14、 Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved worl
15、dwide for CEN national Members. Ref. No. EN ISO 11358-1:2014 EContents PageForeword .31 Scope .42 Normative references . 43 Terms and definitions 44 Principle . 55 Apparatus 56 Test specimen preparation . 56.1 General 56.2 Test specimens from finished products 66.3 Test specimen conditioning 66.4 Te
16、st specimen mass . 67 Calibration 67.1 Mass calibration 67.2 Temperature calibration 68 Procedure 78.1 General 78.2 Temperature scanning mode . 78.3 Isothermal mode 89 Expression of results . 89.1 Graphical representation 89.2 Determination of increase in mass . 89.3 Determination of loss in mass 91
17、0 Test report . 112DIN EN ISO 11358-1:2014-10EN ISO 11358-1:2014 (E)3Foreword This document (EN ISO 11358-1:2014) has been prepared by Technical Committee ISO/TC 61 “Plastics” in collaboration with Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by NBN. This European Stand
18、ard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by January 2015, and conflicting national standards shall be withdrawn at the latest by January 2015. Attention is drawn to the possibility that some of the elements of t
19、his document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 11358:1997. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following count
20、ries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Pol
21、and, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 11358-1:2014 has been approved by CEN as EN ISO 11358-1:2014 without any modification. DIN EN ISO 11358-1:2014-10 EN ISO 11358-1:2014 (E) 1 ScopeThis part of ISO
22、11358 specifies general conditions for the analysis of polymers using thermogravimetric techniques. It is applicable to liquids or solids. Solid materials may be in the form of pellets, granules or powders. Fabricated shapes reduced to appropriate specimen size may also be analysed by this method.Th
23、ermogravimetry can be used to determine the temperature(s) and rate(s) of decomposition of polymers, and to measure at the same time the amounts of volatile matter, additives and/or fillers they contain.The thermogravimetric measurements may be carried out in dynamic mode (mass change versus tempera
24、ture or time under programmed conditions) or isothermal mode (mass change versus time at constant temperature).Thermogravimetric measurements may also be carried out using different testing atmospheres, e.g. to separate decomposition in an inert atmosphere from oxidative degradation.2 Normative refe
25、rencesThe 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 (including any amendments) applies.IS
26、O 291, Plastics Standard atmospheres for conditioning and testingISO 472, Plastics VocabularyISO 11357-1, Plastics Differential scanning calorimetry (DSC) Part 1: General principles3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 472 and the following
27、apply.3.1dynamic mass-change determinationtechnique for recording the variation of the mass of a test specimen with temperature T which is changing at a programmed rate3.2isothermal mass-change determinationtechnique for recording the variation of the mass of a test specimen with time t at constant
28、temperature T3.3Curie temperaturetemperature at which a ferromagnetic material passes from the ferromagnetic state to the paramagnetic state or vice versa4DIN EN ISO 11358-1:2014-10EN ISO 11358-1:2014 (E)4 PrincipleA test specimen is heated at specified rates with a controlled temperature programme,
29、 and the change in mass is measured as a function of temperature. Alternatively, the specimen is kept at a given constant temperature and the change in mass is measured as a function of time over a given period.During measurement the test specimen is held in a controlled inert or oxidising atmospher
30、e.In general, the reactions which cause the mass of a test specimen to change are decomposition or oxidation reactions or the volatilisation of a component. The change in mass is recorded as a thermogravimetric (TG) curve.The change in mass of a material as a function of temperature and the extent o
31、f this change are indicators of the thermal stability of the material. TG data can therefore be used to evaluate the relative thermal stability of polymers of the same generic family and polymer-polymer or polymer-additive interactions, using measurements made under the same test conditions.NOTE TG
32、data may be used for process control, process development and material evaluation. Long-term thermal stability is a complex function of service and environmental conditions. TG data alone may not be able to describe the long-term thermal stability of a polymer.5 ApparatusA number of commercial instr
33、uments suitable for thermogravimetric measurements are available. The basic apparatus consists of the following.5.1 Thermobalance, meeting the following requirements: capability to generate constant heating and cooling rates suitable for intended measurements; capability to maintain the test tempera
34、ture constant (to within 0,3 K or less for the duration of measurement); capability to maintain a constant purge gas flow rate controllable to within 10 % over a range of flow rates (e.g. 10 ml/min to 150 ml/min); temperature and mass range in line with experimental requirements; recording device ca
35、pable of automatically recording the measured curve of mass versus temperature and time; measurement of temperature signals with an accuracy of 2 K or better; measurement of time with an accuracy of 1 s or better; measurement of mass with an accuracy of 20 g or better.5.2 Purge gas, dry air or oxyge
36、n (oxidizing conditions) or a suitable inert gas with an oxygen content of 0,001 % by volume or less (non-oxidizing conditions). In either case, the water content of the purge gas shall be less than 0,001 % by mass.6 Test specimen preparation6.1 GeneralTest specimens may be liquids or solids. Solids
37、 may be in the form of powders, pellets, granules or cut pieces. For finished products, the test specimen shall be in the form normally found in use.5DIN EN ISO 11358-1:2014-10 EN ISO 11358-1:2014 (E) 6.2 Test specimens from finished productsCut the test specimen to appropriate size for the specimen
38、 holder. Microtomes or razor blades are suitable for this purpose.NOTE Test specimen size and shape are generally dependent on the sample holder. Surface area affects the overall results. For instance, in comparing a test specimen of large surface area with a test specimen of smaller surface area, b
39、oth having the same mass, the smaller surface area test specimen normally changes at a slower rate.6.3 Test specimen conditioningUnless otherwise specified in a material specification or product standard, test specimens shall be conditioned, prior to measurement, at one of the standard atmospheres s
40、pecified in ISO 291, or by any other method specified by agreement between the interested parties.6.4 Test specimen massPreferably, the mass of the test specimen shall be in the range of 10 mg to 100 mg.7 Calibration7.1 Mass calibrationWithout any gas flow through the thermobalance (to prevent any d
41、isturbance through buoyancy and/or convection effects), calibrate the thermobalance as follows, using calibrated masses in the range of 10 mg to 100 mg:Record the temperature at which the mass calibration was carried out.Zero the thermobalance. Place the calibration weight on the thermobalance and m
42、easure the corresponding mass change. If necessary, adjust the thermobalance so that the measured mass is equal to the calibration mass.If mass calibration is done by procedures included in the instrument control software or by external service providers a valid calibration certificate may be accept
43、able to demonstrate adequate mass calibration.7.2 Temperature calibrationCarry out the temperature calibration using the same atmosphere, rate of gas flow and heating rate as shall be used in the procedure specified in Clause 8.If the thermobalance is not coupled with another thermoanalytical method
44、, use the following procedure.a) Choose two or more calibration materials with a Curie temperature near the temperature range to be examined. If possible, choose the calibration materials in such a way that the temperature range to be examined lies between the Curie temperatures of two of them.b) St
45、art heating at the same heating rate as will be used in the procedure specified in Clause 8 and carry out a calibration based on the start temperature TA, mid-point temperature TCand end temperature TBfor the Curie temperature transition.NOTE 1 The Curie point is the temperature at which a ferromagn
46、etic material becomes paramagnetic on heating. The effect is reversible. Applying a magnetic field (e.g. by placing a strong magnet below the furnace) exerts a downward force on the ferromagnetic sample. This creates an apparent increase of weight which is lost upon heating the sample above its Curi
47、e temperature.NOTE 2 Certified calibration materials traceable to metrology laboratories should be preferably used. Suitable calibration materials may be available via instrument manufacturers or National Metrology Institutes. 6DIN EN ISO 11358-1:2014-10EN ISO 11358-1:2014 (E)If the thermobalance is
48、 combined with a DSC (differential scanning calorimetry) detector, it is recommended that the thermobalance is temperature-calibrated using procedures specified in corresponding standards, e.g. ISO 11357-1 for DSC.NOTE 3 The melting point of a calibration material is defined as the intercept of the extrapolated baseline and the tangent to the slope of the endotherm at the point of inflection of the curve (the so-called onset temperature).NOTE 4 Calibration is the most critical stage in obtaining reliable t
