BS-EN-ISO-8618-1998 BS-2782-4-METHOD-451M-1998.pdf

BRITISH STANDARD BS EN ISO 8618:1998 BS 2782-4: Method 451M: 1998 Plastics Liquid phenolic resins Conventional determination of non-volatile matter The European Standard EN ISO 8618:1998 has the status of a British Standard ICS 83.080.10 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:19:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 8618:1998 This British Standard, having been prepared under the direction of the Sector Board for Materials and Chemicals, was published under the authority of the Standards Board and comes into effect on 15 August 1998 © BSI 05-1999 ISBN 0 580 30055 2 National foreword This British Standard is the English language version of EN ISO 8618:1998. It is identical with ISO 8618:1995. It supersedes BS EN ISO 8618:1995 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC standards normally include an annex which lists normative references to international publications with their corresponding European publications. The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN ISO title page, page 2, the ISO title page, page ii, pages 1 to 3 and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:19:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 8618:1998 © BSI 05-1999i Contents Page National forewordInside front cover Foreword2 Forewordii Text of ISO 86181 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:19:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii blank Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:19:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN ISO 8618 June 1998 ICS 83.080.10Supersedes EN ISO 8618:1995 Descriptors: See ISO document English version Plastics Liquid phenolic resins Conventional determination of non-volatile matter (ISO 8618:1995) Plastiques Résines phénoliques liquides Détermination de lextrait sec conventionnel (ISO 8618:1995) Kunststoffe Flüssige Phenolharze Konventionsverfahren zur Bestimmung der nichtflüchtigen Anteile (ISO 8618:1995) This European Standard was approved by CEN on 24 May 1998. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions 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 Central Secretariat or to any CEN member. This European Standard exists in three 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 Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comité Européen de Normalisation Europäisches Komitee für Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels © 1998 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 8618:1998 E Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:19:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 8618:1998 © BSI 05-1999 2 Foreword The text of the International Standard from Technical Committee ISO/TC 61 “Plastics” of the International Organization for Standardization (ISO) has been taken over as an European Standard by Technical Committee CEN/TC 249 “Plastics”, the secretariat of which is held by IBN. This European Standard replaces EN ISO 8618:1995. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by December 1998, and conflicting national standards shall be withdrawn at the latest by December 1998. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard ISO 8618:1995 has been approved by CEN as a European Standard without any modification. Contents Page Foreword2 1Scope1 2Definition1 3Apparatus1 4Procedure1 5Expression of results1 6Test report1 Annex A (normative) Special procedures for testing at 150 °C3 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:19:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:19:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 8618:1998 ii © BSI 05-1999 Foreword 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 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, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted 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. International Standard ISO 8618 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials. This second edition cancels and replaces the first edition (ISO 8618:1987) which has been revised to include an air circulation oven as an alternative to the static convection oven. Annex A forms an integral part of this International Standard. Descriptors: Plastics, resins, liquid resins, phenoplasts, tests, determination, non-volatile matter. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:19:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 8618:1998 © BSI 05-19991 1 Scope This International Standard specifies a method for the conventional determination of the non-volatile matter of liquid phenolic resins (resols, novolak solutions, etc.). It can be used for commercial products or for resins in their various stages of manufacture. NOTE 1For phenolic resins, the term “non-volatile matter” is based upon arbitrary test conditions (see 4.2, note 3). Results obtained by this method may not agree with the results obtained in industrial applications of these resins. 2 Definition For the purpose of this International Standard, the following definition applies. 2.1 non-volatile matter the percentage residue obtained when the volatile components of a specific mass of a liquid phenolic resin are evaporated under specified conditions of temperature and time 3 Apparatus 3.1 Small disposable dishes made of aluminium, nickel, stainless steel, tinplate or galvanized sheet metal, with a flat base, an inner diameter at the base of 75 mm and a height of approximately 25 mm. NOTE 2Dishes of different diameters may be used if the mass of the test portion m1, in grams, is calculated according to the following relation: where A is the area, in square millimetres, of the dish base. 3.2 Precision balance, accurate to 1 mg. 3.3 Static convection oven, with natural ventilation, with a perforated metal shelf placed at one-third of the height of the oven and capable of being maintained at the test temperature (see 4.2). or Air circulation oven, with horizontal ventilation, having an air circulation speed of 0,8 m/s to 1,2 m/s. The type of oven used shall be stated in the test report since the results of the test depend on the type used (static convection or air circulation). 3.4 Desiccator, containing dehydrated calcium chloride or other suitable drying agent. 4 Procedure 4.1 Degrease a small dish (3.1), dry it in the oven (3.3), maintained at 135 °C (or the selected test temperature, see 4.2), and store it in the desiccator (3.4) until used. Determine the mass (m0) of the clean dry dish to the nearest 1 mg. Transfer 3,0 g ± 0,5 g of completely homogenized resin into the dish and record the mass (m1), to the nearest 1 mg, of the test portion therein (see 3.1, note 2). 4.2 Place the dish at the centre of the shelf in the oven, heated to the preferred test temperature of 135 °C ± 1 °C. An alternative test temperature (see note 3) may be used and shall be recorded in the test report. Recommended alternative temperatures are 120 °C ± 1 °C and 150 °C ± 1 °C (see note 4 and Annex A). NOTE 3The test temperature must be such that the volatile components evaporate without decomposition of the resin. When selecting the temperature, possible reactions between the individual components and polycondensation should also be considered. NOTE 4When testing is performed at 150 °C, a slightly different procedure may be used (dissolving the test portion in a solvent). (See Annex A.) 4.3 After 1 h ± 5 min at the selected test temperature, remove the dish from the oven, allow it to cool for at least 1 h in the desiccator and determine the mass (m2), to the nearest 1 mg, of the dish plus the non-volatile matter of the test portion. 4.4 Carry out a duplicate determination simultaneously. As the temperature is not the same in all parts of the oven at all times, place the two dishes at the same height and next to one another. 5 Expression of results 5.1 Calculate the non-volatile matter NV, as a percentage by mass, using the equation where 5.2 Calculate the arithmetic mean (to one decimal place) of the two determinations. If the difference between the two determinations is more than 5 % in relative value, repeat the test. 6 Test report The test report shall include the following particulars: m1 A - - 3 4 412 - -0 000 68 g,mm2= m0is the mass, in grams, of the dish (see 4.1); m1is the mass, in grams, of the test portion (see 4.1); m2is the mass, in grams, of the dish plus the non-volatile matter of the test portion (see 4.3); Úis the test temperature, in degrees Celsius (see 4.2). Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:19:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 8618:1998 2 © BSI 05-1999 a) a reference to this International Standard; b) all details necessary for complete identification of the resin tested; c) the type of dish used; d) the test temperature; e) the type of oven used; f) if necessary, the solvent used (test at 150 °C; see Annex A); g) the results of the individual determinations and their arithmetic mean. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:19:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 8618:1998 © BSI 05-19993 Annex A (normative) Special procedures for testing at 150 °C WARNING If the oven used is not an explosion-proof one, the determination of non-volatile matter at 150 °C ± 1 °C using solvent must not exceed the use of two small dishes. Fire and/or explosion could result if the number of test portions in small dishes were to be increased beyond two. A.1 Solvents A.1.1 Distilled toluene A.1.2 Isopropanol A.1.3 Methyl ethyl ketone A.2 Procedure Predry a dish (3.1) in the oven (3.3), maintained at 150 °C, allow to cool to ambient temperature and store in the desiccator (3.4). Determine the mass (m0) of the clean dry dish to the nearest 1 mg. Transfer sufficient resin into the dish so that the expected non-volatile matter will be 0,5 g ± 0,05 g and record the mass (m1), to the nearest 1 mg, of the test portion in the dish. Dissolve the resin in 5 ml of distilled toluene (A.1.1) or isopropanol (A.1.2). If the resin does not dissolve in these solvents, use methyl ethyl ketone (A.1.3). NOTE 5Methyl ethyl ketone cannot be used with resols. The dissolution process can be speeded up by heating briefly in the oven (10 s to 15 s). When the resin has dissolved and is distributed evenly over the base of the dish, place the dish in the oven, maintained at 150 °C ± 1 °C, so that the dish is horizontal and heat it for 2 h. Remove the dish from the oven and allow it to cool at ambient temperature in the desiccator. Determine the mass (m2), to the nearest 1 mg, of the dish plus the non-volatile matter of the test portion. Continue as in 4.4. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:19:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 8618:1998 BS 2782-4: Method 451M: 1998 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions British Standards are updated by amendment or revision. Users of British Standards should make sure that they possess the latest amendments or editions. It is the constant aim of BSI to improve the quality of our products and services. We would be grateful if anyone finding an inaccuracy or ambiguity while using this British Standard would inform the Secretary of the technical committee responsible, the identity of which can be found on the inside front cover. Tel: 020 8996 9000. Fax: 020 8996 7400