BS-EN-ISO-9371-1995 BS-2782-7-METHODS-734A-TO-D.pdf

BRITISH STANDARD BS EN ISO 9371:1995 BS 2782-7: Methods 734A to D:1995 Plastics Phenolic resins in the liquid state or in solution Determination of viscosity The European Standard EN ISO 9371:1995 has the status of a British Standard Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:13:56 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 9371:1995 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 December 1995 © BSI 12-1999 The following BSI references relate to the work on this standard: Committee reference PRI/21 Draft announced in BSI News August 1994 ISBN 0 580 24497 0 Committees responsible for this British Standard The preparation of this British Standard was entrusted to Technical Committee PRI/21, Testing of plastics, upon which the following bodies were represented: The British Apparel and Textile Confederation British Plastics Federation Department of the Environment (Building Research Establishment) Department of Trade and Industry (National Physical Laboratory) Electrical and Electronic Insulation Association (BEAMA Ltd.) GAMBICA (BEAMA Ltd) Institute of Materials Ministry of Defence Packaging and Industrial Films Association PIRA International RAPRA Technology Ltd. Royal Society of Chemistry Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:13:56 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 9371:1995 © BSI 12-1999i Contents Page Committees responsibleInside front cover National forewordii Foreword2 1Scope3 2Normative references3 3General (valid for all four methods)3 4Reference methods3 5Comparative test methods6 6Test report (valid for all four methods)6 Annex A (normative) Calibrating Ubbelohde viscometers7 Annex B (normative) Determination of the viscosity using a Hoeppler dropping-ball viscometer7 Figure 1 Details of Ubbelohde viscometer4 Figure B.1 Dropping-ball viscometer8 Table 1 Dimensions, approximate C-constants and kinematic-viscosity ranges of the Ubbelohde viscometer5 Table 2 Correspondence between spindle no. and viscosity range for a rotary viscometer6 Table B.1 Balls for use in a dropping-ball viscometer having a measurement tube with an inside diameter of 15,94 mm9 Table B.2 Precision data10 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:13:56 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 9371:1995 ii © BSI 12-1999 National foreword This British Standard has been prepared by Technical Committee PRI/21 and is the English language version of EN ISO 9371:1995 Plastics Phenolic resins in the liquid state or in solution Determination of viscosity. It is identical with ISO 9371:1990 published by the International Organization for Standardization (ISO). This standard has been dual numbered and is contained in the BS 2782 series of tests as BS 2782-7:Methods 734A-D. 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. Cross-references Publication referred toCorresponding British Standard BS 2782 Methods of testing plastics Part 7 Rheological properties ISO 2555:1989Method 730C:1992 Determination of apparent viscosity of resins by the Brookfield Test method ISO 3219:1977Method 730B:1994 Determination of the viscosity of polymers in the liquid, emulsified or dispersed state, using a rotational viscometer working at a defined shear rate Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN ISO title page, pages 2 to 10 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. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:13:56 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN ISO 9371 July 1995 ICS 83.080.10 Descriptors: Phenolic resins, plastics, viscosity, viscosity measurement English version Plastics Phenolic resins in the liquid state or in solution Determination of viscosity (ISO 9371:1990) Plastiques Résines phénoliques liquides ou en suspension Détermination de la viscosité (ISO 9371:1990) Kunststoffe Phenolharze, flüssig oder Lösung Bestimmung der Viskosität (ISO 9371:1990) This European Standard was approved by CEN on 1995-01-12. 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, 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 © 1995 Copyright reserved to CEN members Ref. No. EN ISO 9371:1995 E Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:13:56 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 9371:1995 © BSI 12-1999 2 Foreword The text of the International Standard from ISO/TC 61, Plastics, of the International Organization for Standardization (ISO) has been taken over as a European Standard by the Technical Committee CEN/TC 249, Plastics. 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 January 1996, and conflicting national standards shall be withdrawn at the latest by January 1996. According to the CEN/CENELEC Internal Regulations, the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:13:56 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 9371:1995 © BSI 12-19993 1 Scope This International Standard specifies four methods for the determination of the viscosity of phenolic resins, either as a liquid or in solution. It describes the following two types of method: a) Reference methods: 1) Determination using a viscometer with a definite speed gradient 2) Determination using an Ubbelohde capillary viscometer b) Comparative test methods: 1) Determination using a rotary viscometer 2) Determination using a Hoeppler dropping-ball viscometer Other methods may be used as long as it is verified that the same test results are obtained. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 2555:1989, Plastics Resins in the liquid state or as emulsions or dispersions Determination of apparent viscosity by the Brookfield Test method. ISO 3105:1976, Glass capillary kinematic viscometers Specification and operating instructions. ISO 3219:1977, Plastics Polymers in the liquid, emulsified or dispersed state Determination of viscosity with a rotational viscometer working at defined shear rate. 3 General (valid for all four methods) Test temperature Unless specified otherwise, determinations shall be performed at 23 °C within the tolerance allowed in the method used. Dissolving solid resins The solvent used and the concentration chosen shall be agreed between the parties concerned. Expression of results Dynamic viscosities shall be expressed in millipascal seconds (mPa·s), kinematic viscosities in square millimetres per second (mm2/s). 4 Reference methods 4.1 Viscosity determination using a viscometer with definite speed gradient The specifications of ISO 3219 shall be followed, either to determine the viscosity at a definite speed gradient, or to perform a rheological study of the resin and, in particular, to obtain a curve of viscosity as a function of the speed gradient. 4.2 Determination using an Ubbelohde capillary viscometer 4.2.1 Scope This sub-clause specifies a method of test, for reference purposes, for the determination of the kinematic viscosity of liquid phenolic resins, or resins dissolved in an appropriate solvent at a given concentration chosen by agreement between the parties concerned. The method is suitable for determining kinematic viscosity over the range 2 mm2/s to 10 000 mm2/s. NOTE 1Kinematic viscosity is a property of newtonian fluids. As resins and resin solutions are non-newtonian, the determination of the viscosity by this method will give an apparent viscosity which will depend on the specific conditions used. 4.2.2 Normative reference ISO 653:1980, Long solid-stem thermometers for precision use. 4.2.3 Principle The determination involves measuring the time required by a fixed volume of liquid resin or resin solution, contained in the bulb of a glass viscometer, to flow under gravity through a calibrated capillary under a reproducible driving head of liquid at a closely controlled temperature. 4.2.4 Apparatus 4.2.4.1 Ubbelohde viscometer, with design details and construction as shown in Figure 1. Table 1 gives the approximate C-constants (see Annex A), the diameter of the capillaries and the corresponding viscosity ranges. Bulb C has a volume of 4 ml for a viscometer whose constant is between 0,01 mm2/s2 and 0,05 mm2/s2, 5 ml for a constant from 0,2 mm2/s2 to 1,0 mm2/s2 and 6 ml for a constant between 3,0 mm2/s2 to 10,0 mm2/s2. The viscometer shall be fitted with supports designed to hold the various tubes which make up the viscometer in a vertical position as required by the method. The filler marks (G and H) on bulb A indicate the minimum and maximum quantities providing the pressure necessary for correct functioning. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:13:56 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 9371:1995 4 © BSI 12-1999 Figure 1 Details of Ubbelohde viscometer Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:13:56 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 9371:1995 © BSI 12-19995 Table 1 Dimensions, approximate C-constants and kinematic-viscosity ranges of the Ubbelohde viscometer 4.2.4.2 Thermoregulated bath, of such a design that the viscometer can be immersed in it so that bulb C above the top of the capillary is at least 30 mm below the surface of the liquid in the bath, but the tube and thermometer are both visible. A rigid support shall be provided to maintain the tube vertically to within 1°. The bath shall be fitted with a heater and stirrer capable, between them, of maintaining the bath at a temperature of 23 °C ± 0,1 °C along the entire length of the viscometer and from one viscometer tube to another. 4.2.4.3 Filter funnel, with sintered-glass disc, medium porosity (average pore diameter between 40 4m and 50 4m). 4.2.4.4 Stopwatch, accurate to 0,1 s. 4.2.4.5 Long-stem thermometer, covering the range from 20 °C to 45 °C, graduated at intervals of not more than 0,1 °C, in accordance with ISO 653 (STL/0,1/20/45). 4.2.4.6 Means of applying sufficient vacuum, to the top of tube N to raise the resin or resin-solution level to the level in bulb C required by the test procedure (see 4.2.5.3). 4.2.5 Procedure 4.2.5.1 Viscometer calibration Calibrate the viscometer (4.2.4.1) before using it for the first time, then periodically (see Annex A). Constants are usually provided with viscometers, but it is advisable to check them. 4.2.5.2 Viscometer cleaning Initially, then periodically, clean the viscometer with a chromic acid cleaning solution. The cleaning solution shall be kept in the viscometer for at least 12 h at ambient temperature, although this time may be shortened if the temperature is higher. Then empty the viscometer and rinse it first with deionized distilled water followed by acetone, finally drying it with stream of dry, filtered air. Clean the viscometer thoroughly between measurements by rinsing with a suitable highly volatile solvent. Dry the viscometer by passing a slow stream of dry, filtered air through it for 2 min, or until all traces of solvent are eliminated. 4.2.5.3 Determination of viscosity Fill the viscometer (4.2.4.1) with resin or resin solution, tilting the instrument about 30° out of vertical, keeping bulb A (see Figure 1) below the capillary, and passing the liquid through the sintered-glass filter funnel (4.2.4.3). Introduce sufficient liquid into tube L to raise the level to the lower filler mark (H), but below the upper filler mark (G), when the viscometer is returned to the vertical. The U-tube (P) at the bottom of the viscometer should then be completely full. It shall not contain any air bubbles. Immerse the viscometer in the bath (4.2.4.2), using the support to ensure the viscometer is vertical. Maintain the bath temperature at 23 °C ± 0,1 °C. Allow the filled viscometer to remain in the bath long enough to reach 23 °C ± 0,1 °C. Place a finger over tube M and apply suction to the top of tube N to draw liquid up tube N until it reaches the centre of bulb D. Approximate C-constantInternal diameter of capillaryVolume of bulb C Utilisation range Kinematic viscosity mm2/s2mm (± 2 %)ml (± 5 %) mm2/sa 0,01 0,03 0,05 0,1 0,3 0,5 1,0 3,0 5,0 10,0 0,58 0,78 0,88 1,03 1,36 1,55 1,83 2,43 2,75 3,27 4 4 4 5 5 5 5 6 6 6 2 to 10 6 to 30 10 to 50 20 to100 60 to300 100 to500 200 to1 000 600 to3 000 1 000 to5 000 2 000 to 10 000 a 1 mm2/s = 1 cSt Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:13:56 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 9371:1995 6 © BSI 12-1999 Disconnect the suction from tube N, remove the finger from tube M and place it immediately on tube N until the liquid in and below tube M has drained clear from the bottom end of the capillary (R). Remove the finger from tube N and, using the sto