1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 18280:2010Plastics Epoxy resins TestmethodsBS ISO 18280:2010 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 18280:2010. Itsupersede
2、s BS ISO 18280:2005 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PRI/42, Fibre reinforced thermosetting plastics andprepregs.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not pu
3、rport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2010ISBN 978 0 580 65167 0ICS 83.080.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStand
4、ards Policy and Strategy Committee on 30 September 2010.Amendments issued since publicationDate Text affectedBS ISO 18280:2010Reference numberISO 18280:2010(E)ISO 2010INTERNATIONAL STANDARD ISO18280Second edition2010-09-01Plastics Epoxy resins Test methodsPlastiques Rsines poxydes Mthodes dessai BS
5、ISO 18280:2010ISO 18280:2010(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 computer performing the edi
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9、ither 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 2010 All rights reservedBS ISO 18280:2010ISO
10、 18280:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Normative references1 3 Description of test methods.2 3.1 Physical properties .2 3.1.1 Determination of the melting range.2 3.1.2 Determination of the softening point 3 3.1.3 Determination of density 3
11、 3.1.4 Determination of refractive index 4 3.1.5 Determination of viscosity4 3.1.6 Determination of tendency to crystallize 4 3.1.7 Determination of overall volume shrinkage4 3.1.8 Determination of the flash point 5 3.1.9 Estimation of colour5 3.2 Chemical properties 5 3.2.1 Determination of epoxy e
12、quivalent5 3.2.2 Determination of chlorine content.5 3.2.3 Determination of 1,2-glycol content 6 3.2.4 Determination of the electrical conductivity of aqueous resin extracts6 3.2.5 Determination of ash.7 3.2.6 Determination of primary, secondary and tertiary amine group nitrogen content in amine epo
13、xy hardeners7 3.2.7 Determination of free acid in acid anhydride hardeners and accelerators.8 3.2.8 Non-volatile-matter content8 Annex A (informative) List of test methods for each property.9 Bibliography10 BS ISO 18280:2010ISO 18280:2010(E) iv ISO 2010 All rights reservedForeword ISO (the Internati
14、onal 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 member body interested in a subject for which a technical committee has been
15、 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 Electrotechnical Commission (IEC) on all matters of electrotechnical standa
16、rdization. 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 adopted by the technical committees are circulated to the member bodies for
17、voting. Publication as 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
18、such patent rights. ISO 18280 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials. This second edition cancels and replaces the first edition (ISO 18280:2005), which has been revised to include the following additional test methods: determination of t
19、he softening point (see 3.1.2); determination of the 1,2-glycol content (see 3.2.3); determination of the electrical conductivity of aqueous resin extracts (see 3.2.4). BS ISO 18280:2010ISO 18280:2010(E) ISO 2010 All rights reserved vIntroduction The purpose of this International Standard is to pres
20、ent an overview of ISO test methods for characterizing epoxy resins. Those test methods that are suitable and necessary for characterizing epoxy resins prior to polymerization are listed, along with brief explanations of the principles involved. Because of the specificity of thermosetting resins lik
21、e epoxy resins, a distinction is made between the presentation of properties before crosslinking (characteristics which are useful for processing) and after crosslinking (intrinsic characteristics). Procedures for determining intrinsic characteristics of crosslinked (or cured) epoxy resins are given
22、 in ISO 3673-2. BS ISO 18280:2010BS ISO 18280:2010INTERNATIONAL STANDARD ISO 18280:2010(E) ISO 2010 All rights reserved 1Plastics Epoxy resins Test methods 1 Scope Epoxy resins are a family of synthetic resins, including products, which range from viscous liquids to high-melting solids. The resin mo
23、lecule contains as reactive sites one or more oxirane or epoxy groups, usually in the form of a glycidyl group. The most commercially important resin is the glycidyl ether of bisphenol A, produced by the condensation of epichlorohydrin and diphenylpropane (bisphenol A). Epoxy resins with different c
24、haracteristics are also produced commercially by reacting epichlorohydrin with other materials. To be of use, the resins must be crosslinked with a curing agent or hardener. The choice of curing agent is of importance in designing an epoxy resin system for a given application. The major reactive gro
25、ups in the resin, the epoxy and the hydroxyl groups, react with many other groups so that many types of chemical substance can be used as curing agents. These include acid anhydrides, aliphatic and aromatic amines and polyaminoamides. Some curing agents will crosslink the resin at ambient temperatur
26、es while others require the application of heat. This International Standard provides an overview of the ISO test methods used to characterize epoxy resins. The listed property to be determined in any given case depends on agreement between the supplier and customer. 2 Normative references The follo
27、wing 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 1523, Determination of flash point Closed cup equilibr
28、ium method ISO 1675, Plastics Liquid resins Determination of density by the pyknometer method ISO 2555, Plastics Resins in the liquid state or as emulsions or dispersions Determination of apparent viscosity by the Brookfield Test method ISO 2592, Determination of flash and fire points Cleveland open
29、 cup method ISO 3001, Plastics Epoxy compounds Determination of epoxy equivalent ISO 3146:2000, Plastics Determination of melting behaviour (melting temperature or melting range) of semi-crystalline polymers by capillary tube and polarizing-microscope methods ISO 3219, Plastics Polymers/resins in th
30、e liquid state or as emulsions or dispersions Determination of viscosity using a rotational viscometer with defined shear rate ISO 3251, Paints, varnishes and plastics Determination of non-volatile-matter content ISO 3451-1:2008, Plastics Determination of ash Part 1: General methods ISO 3521, Plasti
31、cs Unsaturated polyester and epoxy resins Determination of overall volume shrinkage BS ISO 18280:2010ISO 18280:2010(E) 2 ISO 2010 All rights reservedISO 3675, Crude petroleum and liquid petroleum products Laboratory determination of density Hydrometer method ISO 4615:1979, Plastics Unsaturated polye
32、sters and epoxide resins Determination of total chlorine content ISO 4625-1, Binders for paints and varnishes Determination of softening point Part 1: Ring-and-ball method ISO 4630-1, Clear liquids Estimation of colour by the Gardner colour scale Part 1: Visual method ISO 4895, Plastics Liquid epoxy
33、 resins Determination of tendency to crystallize ISO 5661, Petroleum products Hydrocarbon liquids Determination of refractive index ISO 6271-1, Clear liquids Estimation of colour by the platinum-cobalt scale Part 1: Visual method ISO 7327, Plastics Hardeners and accelerators for epoxide resins Deter
34、mination of free acid in acid anhydride ISO 9702, Plastics Amine epoxide hardeners Determination of primary, secondary and tertiary amine group nitrogen content ISO 11357-3, Plastics Differential scanning calorimetry (DSC) Part 3: Determination of temperature and enthalpy of melting and crystallizat
35、ion ISO 12058-1, Plastics Determination of viscosity using a falling-ball viscometer Part 1: Inclined-tube method ISO 21048, Plastics Epoxy resins Determination of 1,2-glycol content ISO 21318, Plastics Epoxy resins Determination of electrical conductivity of aqueous resin extracts ISO 21627-1, Plas
36、tics Epoxy resins Determination of chlorine content Part 1. Inorganic chlorine ISO 21627-2, Plastics Epoxy resins Determination of chlorine content Part 2: Easily saponifiable chlorine ISO 21627-3, Plastics Epoxy resins Determination of chlorine content Part 3: Total chlorine 3 Description of test m
37、ethods 3.1 Physical properties 3.1.1 Determination of the melting range 3.1.1.1 Determination of the melting range using capillary methods The test shall be performed in accordance with ISO 3146:2000, method A. BS ISO 18280:2010ISO 18280:2010(E) ISO 2010 All rights reserved 3Principle of ISO 3146:20
38、00, method A A specimen is heated in a capillary tube at a controlled rate, and monitored visually for change in shape. NOTE Epoxy resins are not single chemical substances, but polymolecular compounds. This is evident from their melting behaviour the process is not limited to one temperature but ex
39、tends over a range of temperatures. The limits of the melting range consist of a “sinter point” (also known as the “stick point”) and the “melted stage”. The challenge is to establish exact definitions of these “points” for interpretation by various operators. The repeatability of the method is good
40、, but reproducibility can be poor, hence the necessity for agreement on the definitions of these “points”. The melting range is the temperature interval between the sinter point and the melted stage. The sinter point (stick point) is the temperature at which the first physical property change is obs
41、erved in the powdered resin. The melted stage is the temperature at which the mass of the resin becomes totally fluid or (as opposed to the melting of partially crystalline substances) the temperature at which the sintered mass of the resin becomes translucent (not transparent) and/or when the resin
42、 starts to shrink and separate from the capillary tube wall. The moisture content of the resin powder has an effect on the determination of the melting range. Since the melting range is to be determined on products as received, it is not permissible to subject the resin to drying before testing. How
43、ever, for comparative tests, it might be desirable to take into account the moisture content. In such a case, it is possible to dry the resin powder to a constant mass, or at least for 48 h, using diphosphorus pentoxide or a similar dehydrating agent. Preparation of the samples Use a sample of resin
44、 in powder form. When the resin is in lump or flake form, crush it in a mortar and sift the pulverized resin through a 250 m sieve. Take the sample from the material that passes through the 250 m sieve. 3.1.1.2 Determination of the melting range using DSC The test shall be performed in accordance wi
45、th ISO 11357-3. 3.1.2 Determination of the softening point The test shall be performed in accordance with ISO 4625-1 (ring-and-ball method). Principle of ISO 4625-1 The softening point is defined as the temperature at which a disc of the sample held within a horizontal ring is forced downward a dist
46、ance of 25,4 mm under the weight of a steel ball as the sample is heated at 5 C/min in a distilled-water or glycerol bath. 3.1.3 Determination of density The test shall be performed in accordance with ISO 1675 (pyknometer method) or ISO 3675 (hydrometer method). Unless otherwise indicated, the deter
47、mination shall be carried out at 23 C. Results are expressed in grams per cubic centimetre to three decimal places. The pyknometer method may be used for all liquid resins; the hydrometer method is suitable for resins with a viscosity below 1 Pas. BS ISO 18280:2010ISO 18280:2010(E) 4 ISO 2010 All ri
48、ghts reserved3.1.4 Determination of refractive index The test shall be performed in accordance with ISO 5661. 3.1.5 Determination of viscosity Three procedures for the determination of viscosity are proposed: A reference method: determination using a viscometer with a definite speed gradient, for ex
49、ample a plate/cone viscometer (ISO 3219). Two verification methods: determination with a rotary viscometer (ISO 2555); determination with a falling-ball viscometer (ISO 12058-1). NOTE Since, in a number of cases, liquid epoxy resins or epoxy resin solutions are non-Newtonian fluids, the measured value might be dependent on the test method. When carrying out comparative tests, it is therefore necessary to ensure
