Unknown BS EN 13302 2010 ICS 75 140; 91 100 50 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BRITISH STANDARD Bitumen and bituminous binders — Determination of dynamic viscosi[.]
BRITISH STANDARD Bitumen and bituminous binders — Determination of dynamic viscosity of bituminous binder using a rotating spindle apparatus ICS 75.140; 91.100.50 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BS EN 13302:2010 BS 2000-505:2010 BS EN 13302:2010 National foreword This British Standard is the UK implementation of EN 13302:2010 It supersedes BS EN 13302:2003, BS EN 13702-2:2003 and BS EN 14896:2006 which are withdrawn The UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroleum Testing and Terminology A list of organizations represented on this committee can be obtained on request to its secretary Energy Institute, under the brand of IP, publishes and sells all Parts of BS 2000, and all BS EN petroleum test methods that would be Part of BS 2000, both in its annual publication “Standard methods for analysis and testing of petroleum and related products and British Standard 2000 Parts” and individually Further information is available from: Energy Institute, 61 New Cavendish Street, London W1G 7AR Tel: 020 7467 7100 Fax: 020 7255 1472 This publication does not purport to include all the necessary provisions of a contract Users are responsible for its correct application Compliance with a British Standard cannot confer immunity from legal obligations This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 April 2010 © BSI 2010 ISBN 978 580 62920 Amendments/corrigenda issued since publication Date Comments BS EN 13302:2010 EN 13302 EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM March 2010 ICS 75.140; 91.100.50 Supersedes EN 13302:2003, EN 13702-2:2003, EN 14896:2006 English Version Bitumen and bituminous binders - Determination of dynamic viscosity of bituminous binder using a rotating spindle apparatus Bitumes et liants bitumineux - Détermination de la viscosité dynamique des liants bituminuex l'aide d'un viscosimètre tournant Bitumen und bitumenhaltige Bindemittel - Bestimmung der dynamischen Viskosität von bitumenhaltigem Bindemittel mit einem Viskosimeter mit rotierender Spindel This European Standard was approved by CEN on 23 January 2010 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 CEN Management Centre 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 CEN Management Centre has the same status as the official versions CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels © 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members Ref No EN 13302:2010: E BS EN 13302:2010 EN 13302:2010 (E) Contents Page Foreword 1 Scope 2 Normative references 3 Terms and definitions 4 4 Principle 5 Apparatus .5 6 Sampling 7 7.1 7.2 7.3 7.4 Procedure .7 General Bituminous binders (unmodified and modified) 7 Bituminous emulsions 8 Cut-back and fluxed bituminous binders 10 8 Expression of results 11 9 9.1 9.2 Precision 11 Repeatability 11 Reproducibility 11 10 Test report 12 Bibliography 13 BS EN 13302:2010 EN 13302:2010 (E) Foreword This document (EN 13302:2010) has been prepared by Technical Committee CEN/TC 336 “Bituminous binders”, the secretariat of which is held by AFNOR 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 September 2010, and conflicting national standards shall be withdrawn at the latest by September 2010 Attention is drawn to the possibility that some of the elements of this 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 13302:2003, EN 13702-2:2003, EN 14896:2006 This document is a merged document based on EN 13302:2003, EN 13702-2:2003 and EN 14896:2006 The reason for merging the three standards is that: the three standards did describe basically the same test method performed on three different types of bituminous materials originally developed by three different working groups almost parallel in time; minor insignificant differences in the three test methods were highly impractical for quality control/quality assurance in the laboratories using the same equipment for two or three of the mentioned standards According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom BS EN 13302:2010 EN 13302:2010 (E) Scope This European Standard specifies a method for the determination of the dynamic viscosity of a variety of bituminous binders: modified and unmodified bituminous binders, bituminous emulsions, cut-back and fluxed bituminous binders, by means of a rotating spindle apparatus (a coaxial viscometer) Standard application temperatures are quoted, although the dynamic viscosity can be measured at other temperatures if required Similarly, viscosity is quoted at standard rates of shear, although additional measures can be taken at varying shear rates if required WARNING — The use of this standard may involve hazardous materials, operations and equipment This standard does not purport to address all of the safety problems associated with its use It is the responsibility of the user of this standard to establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use Normative references The following 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 EN 58, Bitumen and bituminous binders — Sampling bituminous binders EN 12594, Bitumen and bituminous binders — Preparation of test samples Terms and definitions For the purposes of this document, the following terms and definitions apply 3.1 shear stress force acting tangentially to a surface divided by the area of the surface -2 NOTE Shear stress is expressed in Newton per square metre (N ⋅ m ), kilogram per meter per square second -1 -2 (kg ⋅ m ⋅ s ) or Pascal (Pa) 3.2 shear rate velocity gradient in a flowing fluid perpendicular to the stress NOTE -1 Shear rate is expressed in units per second (s ) NOTE The shear rate calculation depends upon the viscometer geometry This should be mentioned by the viscometer manufacturer 3.3 dynamic viscosity ratio between the applied shear stress and the shear rate NOTE sub-unit Dynamic viscosity is expressed in Pascal second (Pa ⋅ s) Millipascal second (mPa ⋅ s) is a frequently used NOTE Dynamic viscosity is the measurement of the resistance to flow of a liquid BS EN 13302:2010 EN 13302:2010 (E) 3.4 Newtonian fluid fluid having a viscosity that is independent of the shear rate NOTE The ratio of the shear stress to the shear rate is the viscosity of the fluid If this ratio is not constant the liquid is non-Newtonian and many fluids exhibit both Newtonian and non-Newtonian behaviour, depending on the temperature and the shear rate 3.5 apparent viscosity term used to characterise the resistance to flow of a Newtonian or non-Newtonian fluid 3.6 form factor specific factor or factors to be applied for the individual equipment in order to obtain the actual viscosity from the readings, mainly due to the geometry of the apparatus Principle The torque applied to a spindle (e.g a cylinder) rotating in a special sample container containing the test sample, measures the relative resistance of the spindle to rotation and provides a measure of the dynamic viscosity of the sample It may be necessary to apply a form factor to yield the actual dynamic viscosity at the test temperature NOTE Some bituminous materials may exhibit non-Newtonian behaviour under the conditions of this method Since non-Newtonian viscosity values are not unique material properties, but reflect the behaviour of the fluid and the measurement system, it should be recognised that measurements made by this method may not always predict performance under the conditions of use Comparisons between non-Newtonian viscosities should be made only for measurements under similar conditions of shear stress and shear rate NOTE Unlike penetration grade bitumen, polymer modified bitumens (PMBs) not show a straight line on the Heukelom-Diagram This implies that in order to obtain information about the temperature susceptibility of PMBs, viscosity should be measured at different temperatures Apparatus Usual laboratory equipment, together with the following: 5.1 Rotating spindle viscometer, dynamic viscosity measurements with rotational viscometers on the bituminous products addressed by this standard may cover wide ranges of shear rates and viscosities: -1 -1 − Range of shear rate: s to 10 s − Range of dynamic viscosities: 10 Pa ⋅ s to 10 Pa ⋅ s -2 In order to cover all product types mentioned in the Scope (Clause 1), under the most usual test conditions, this standards requires rotational viscometer(s) with sample containers and rotating spindles allowing following minimum capabilities: -1 -1 − Range of shear rate: s to 200 s − Range of dynamic viscosities: 10 Pa ⋅ s to 10 Pa ⋅ s -2 NOTE In QA/QC, and in the case of rotating cylinders, the following two conditions give an indication of correct measuring geometry: − Ratio of the radius: R2/R1 ≥ 1,1 (reference to Figure 1); − Difference between the radius R1 – R2 = mm to mm BS EN 13302:2010 EN 13302:2010 (E) Range of temperature: 40 °C to 200 °C; for oxidised grades: 40 °C to 230 °C NOTE Typical test temperatures are 40 °C for bituminous emulsions, 60 °C to 90 °C for cut-backs and fluxed bitumens, 90 °C to 180 °C for unmodified or polymer modified bituminous binders For any given spindle and sample container combination, the operating instructions of the equipment shall allow the operator to select the adequate rotation speed so as to obtain a desired shear rate Key Sample container Spindle Thickness of sample being measured Sample under test R1 Inner radius (spindle) R2 Inner radius (sample container Figure — Rotational viscometer (principle) 5.2 Appropriate spindle(s), a spindle, or set of spindles, appropriate for the equipment, that will allow, for the materials to be tested and each specific test condition, dynamic viscosities to be measured with an accuracy close to ± % and at least equal to ± % If achievable accuracy is not known from the information given by the manufacturer of the equipment, the spindles should be selected so as to obtain dynamic viscosity readings greater or equal to 20 % of the spindle working range for the chosen test conditions For low viscosity materials (typically, for viscosities below 100 mPa ⋅ s), it may be difficult to fulfil these requirements with existing equipment Lower accuracy is then permitted but needs to be documented while indicating, in the test report, the actually achieved level of accuracy or, if not known, the position of the reading with regard to the working range of the used spindle (Clause 10) 5.3 Sample container, specific to the rotating spindle viscometer, that allows the equipment to be used in coaxial mode and therefore enable the control of shear rate BS EN 13302:2010 EN 13302:2010 (E) 5.4 Temperature control device, such as a water or oil jacket or any other appropriate device The chosen device shall be capable of controlling temperature of the test sample to ± 0,5 °C Sampling A sample from the material to be tested shall be taken in accordance with EN 58 and prepared in accordance with EN 12594 Procedure 7.1 General This paragraph is divided in several parts to cope with small deviations in procedure due to differences in the product types covered by this European Standard 7.2 7.2.1 Bituminous binders (unmodified and modified) Preparation of test sample The bulk binder sample shall be placed in an oven maintained at a temperature of about 80 °C above the expected ring and ball softening point temperature or at a maximum of 200 °C which ever is the lower (in case of oxidised bitumen the maximum temperature is 230 °C) Do not overfill or underfill the sample container, as the sample volume is critical to meet the system calibration conditions The container shall be covered with a loose lid to protect it against oxidation The test sample shall be fluid before transferring it to the sample container The total heating time should not exceed h 45 for samples of 100 ml to 499 ml and h 15 for samples of 500 ml to 999 ml Test samples shall be tested within h of the start of their preparation 7.2.2 Preheating Set the temperature control device to the desired test temperature Refer to the operating instructions for the calibration of the temperature control device if necessary Connect the selected spindle to the rotating spindle viscometer and lower it into an empty sample container placed into the temperature control device Wait until equilibrium temperature is obtained (about h) If, for practical reasons, the spindle cannot be preheated while being connected to the viscometer, it is admitted that it is connected at ambient temperature and lowered into the hot sample Temperature equilibration time has then to be extended accordingly Additional sample containers may be preheated at the same temperature in a separate oven for at least 45 Remove the sample container from the temperature control device or the oven and add the volume of sample specified for the spindle to be used Do not overfill or underfill the sample container, as the sample volume is critical to meet the system calibration conditions Avoid incorporation of air bubbles into the samples Place the loaded sample container into the temperature control device Lower the spindle into the sample to the depth specified by the manufacturer Ensure the equipment is level by use of a levelling device (e.g spirit level) Allow the system to equilibrate at the test temperature Allow the moveable part to rotate during the pre-heating time at a very low shear rate Maintain the temperature during the test at within ± 0,5 °C up to 100 °C and ± 1,0 °C above 100 °C BS EN 13302:2010 EN 13302:2010 (E) NOTE Heating duration is fitted to the product type This duration is approximately between 15 to 30 min, but may be extended to h if necessary (case of non-preheated spindle) 7.2.3 Measurement Set the spindle rotating at a speed such that the desired shear rate is achieved with a precision of ± 10 % Allow to stabilise for a period of (60 ± 5) s, and then take a reading Record the following: torque, viscosity (where necessary, apply the form factor (see Clause 3.6) to calculate dynamic viscosity from the reading of the instrument), shear rate, temperature The reading shall be within the limits set for complying with the requirements on accuracy defined under 5.2 If it is not, change one of the variables, i.e the shear rate or the rotating equipment, and repeat the measurement to obtain a new result, complying with the requirements of 5.2 The actually achieved accuracy shall be recorded in the report (Clause 10) Repeat the measurement NOTE A change of the measurement geometry implies the procedure to be repeated from 7.2.1 onwards Reuse of sample is allowed for successive measurements at different temperature levels, as long as the total time for the hot sample does not exceed h 7.2.4 Test conditions This document specifies a test applicable to a large diversity of products for which the usable temperatures and shear rates are not necessarily the same Typical test temperatures range from 90 °C to 180 °C Depending on the product (e.g in the case of polymer modified binders) and test temperature, the material may display non-Newtonian behaviour In such cases, it is recommended to determine dependency upon shear rate following a path going from low to high, then from high to low shear rates 7.2.5 Repeat the measurement on a second separate sample 7.2.6 Continue with Clause 7.3 Bituminous emulsions 7.3.1 Place and maintain the bulk emulsion sample at the required test temperature in an appropriate oven Before transferring the emulsion into the sample container, manually agitate the bulk emulsion sample to ensure homogeneity, without imparting excessive stress to the sample To maintain the integrity of the sample and reduce the chance of evaporation or skinning, ensure the sample is covered when not being agitated 7.3.2 Set the temperature control device to the required test temperature Refer to the operating instructions for the calibration of the temperature control device if necessary Place the sample container and the selected spindle into the temperature control device (or in the oven) and wait until equilibrium temperature is obtained BS EN 13302:2010 EN 13302:2010 (E) Additional sample containers and spindles may also be preheated to the same temperature in a separate oven NOTE A typical test temperature for bituminous emulsions is 40 °C, but the method may be used at other temperatures as well 7.3.3 Transfer an amount of sample as defined by the particular viscometer’s coaxial set-up instructions, and taking into account the spindle size, to enable determination of dynamic viscosity, into the sample container Cover the sample container with a suitable cover to reduce the level of evaporation and sample skinning 7.3.4 Place the sample container containing the sample into the test equipment, lower the spindle into the sample to the depth specified by the equipment manufacturer and allow to reach equilibrium for a length of time such that the emulsion temperature is held steady at the required test temperature ± 0,5 °C NOTE 7.3.5 To accelerate temperature homogenisation, the spindle may be rotated at low speed during this phase Ensure the equipment is level by use of a levelling device (e.g spirit level) 7.3.6 To break storage induced thixotropy effects, set the spindle rotating at a speed such that a shear rate -1 of (10 ± 2) s is achieved Leave for (60 ± 5) s 7.3.7 Set the spindle rotating at a speed such that a shear rate of (2,0 ± 0,2) s stabilise for a period of (30 ± 3) s, then take a reading -1 is achieved Allow to Record the following: torque, viscosity (where necessary, apply the form factor (see 3.6) to calculate dynamic viscosity from the reading of the instrument), shear rate, temperature The reading shall be within the limits set for complying with the requirements on accuracy defined under 5.2 If it is not, change one of the variables, i.e the shear rate or the rotating equipment, and repeat the measurement to obtain a new result, complying with the requirements of 5.2 The actually achieved accuracy shall be recorded in the report (Clause 10) For low viscosity emulsions (typically, for viscosities below 100 mPa ⋅ s), the available equipment and spindles may not allow to reach the desired accuracy In this case, viscosity may be measured at a higher shear rate The actual shear rate employed must be recorded in the report (Clause 10) NOTE The material may display some instability and therefore exhibit a changing viscosity with applied stress, so timing of the readings is very important Any observations of instability behaviour should be recorded 7.3.8 If the material displays non-Newtonian behaviour, viscosities at other shear rates can be recorded, to -1 characterise the behaviour In such cases, the initial reading will be taken at a shear rate of s as from 7.3.3 -1 onwards The higher shear rate (typically 50 s or higher) should then be employed The shear rate should -1 then be dropped to intermediate levels of shear and a final reading back at the initial shear rate of s repeated 7.3.9 Repeat the measurement on a second separate sample 7.3.10 Continue with Clause BS EN 13302:2010 EN 13302:2010 (E) 7.4 Cut-back and fluxed bituminous binders 7.4.1 The bulk binder sample shall be placed in an oven maintained at a temperature that should not exceed which ever is the lower of following temperatures: 80 °C above the estimated ring and ball softening point temperature, 140 °C for fluxed bituminous binders, 80 °C for cut-backs The container shall be filled to at least 50 % of its volume and shall be covered with a loose lid to protect it against evaporation and oxidation Total heating time should be kept to the minimum allowing pouring the sample into the sample container Test samples shall be tested within h after the start of their preparation 7.4.2 Manually agitate the bulk sample to ensure homogeneity, without imparting excessive stress to the sample 7.4.3 Set the temperature control device to the required test temperature Refer to the operating instructions for the calibration of the temperature control device if necessary Connect the selected spindle to the rotating spindle viscometer and lower it into an empty sample container placed into the temperature control device Wait until equilibrium temperature is obtained If, for practical reasons, the spindle cannot be preheated while being connected to the viscometer, it is admitted that it is connected at ambient temperature and lowered into the hot sample Temperature equilibration time has then to be extended accordingly Additional sample containers may be preheated at the same temperature in a separate oven NOTE A typical test temperature for cut-back and fluxed bituminous binders is 60 °C but the method may be used at other temperatures as well (e.g 90 °C) 7.4.4 Transfer an amount of sample as defined by the particular viscometer’s coaxial set-up instructions, and taking into account the spindle size, to enable determination of dynamic viscosity, into the sample container Cover the sample container with a suitable cover to reduce the level of evaporation 7.4.5 Place the sample container containing the sample into the test equipment, lower the spindle into the sample to the depth specified by the equipment manufacturer and allow to reach equilibrium for a length of time such that the sample temperature is held steady at the required test temperature ± 0,5 °C NOTE 7.4.6 To accelerate temperature homogenisation, the spindle may be rotated at low speed during this phase Ensure the equipment is level by use of a levelling device (e.g spirit level) 7.4.7 To break possible storage induced thixotropy effects, set the spindle rotating at a speed such that a -1 shear rate of (50 ± 5) s is achieved Leave for (60 ± 5) s -1 7.4.8 Set the spindle rotating at a speed such that the shear rate of s is achieved Allow to stabilise for a period of (30 ± 3) s, and then take a reading Record the following: torque, viscosity (where necessary, apply the form factor (see 3.6) to calculate dynamic viscosity from the reading of the instrument), shear rate, temperature 10 BS EN 13302:2010 EN 13302:2010 (E) The reading shall be within the limits set for complying with the requirements on accuracy defined under 5.2 If it is not, change one of the variables, i.e the shear rate or the rotating equipment and repeat the measurement to obtain a new result, complying with the requirements of 5.2 The actually achieved accuracy shall be recorded in the report (Clause 10) For low viscosity cut-back and fluxed bituminous binders (typically, for viscosities below 100 mPa ⋅ s), the available equipment and spindles may not allow to reach the desired accuracy In this case, viscosity may be measured at a higher shear rate The actual shear rate employed must be recorded in the report (Clause 10) 7.4.9 If the material displays non-Newtonian behaviour, viscosities at other shear rates can be recorded, to -1 characterise the behaviour In such cases, the initial reading will be taken at a shear rate of s as from 7.4.4 -1 onwards The higher shear rate (typically 50 s or higher) should then be employed The shear rate should -1 then be dropped to intermediate levels of shear and a final reading back at the initial shear rate of s repeated 7.4.10 Repeat the measurement on a second separate sample Expression of results Express the dynamic viscosity, in Pascal ⋅ second or milliPascal ⋅ second as the mean of two results, obtained on two separate samples If the individual results differ by less than 10 %, report the mean value of the two results If the individual results differ by more than 10 % of the mean value of the two results, the individual results and the mean value shall be reported n If appropriate for higher values, express the viscosity values in Pa ⋅ s, as follows: (1,00 x 10 ) Pa ⋅ s 9.1 Precision Repeatability The difference between two successive results, obtained by the same operator with the same apparatus under constant operating conditions on identical test material would, in the long run, in the normal and correct operation of the test method, differ by more than the value, r, in Table in only one case in twenty 9.2 Reproducibility The difference between two single and independent results obtained by different operators working in different laboratories on identical test material would, in the long run, in the normal and correct operation of the test method, differ by more than the value, R, in Table in only one case in twenty 11 BS EN 13302:2010 EN 13302:2010 (E) Table — Repeatability and Reproducibility Repeatability r Reproducibility R (unmodified and modified) 5%a 15 % a Bituminous emulsions b b Cut-back and fluxed bitumens b b Product type Bituminous binders a The precision data are proposed as a conservative estimate from a similar method (ASTM D-4402-06 [1]) until results of round robin tests are available b The precision data of this part of the method has not been determined yet When available, data of round robin test will enable to determine repeatability and reproducibility, which shall be included in this European Standard 10 Test report The test report shall contain at least the following information: a) type and complete identification of the sample under test; b) reference to this European Standard; c) identification of the apparatus (manufacturer, model number and type); d) temperature(s) of test and temperature for sample preparation; e) measurement geometry: inner and outer radius of the measurement system, spindle type, spindle used including application of any form factors; f) length of time to reading the viscosity (only important if non-Newtonian behaviour occurs); g) mean viscosity or viscosity of the single measurements, if difference between single results differ by more than 10 %; h) level of accuracy or, if not known, the position of the reading with regard to the working range of the spindle used for the applied test conditions; i) shear rate(s) utilised for the test; j) any deviation, by agreement or otherwise, from the procedure specified; k) date and identification of the test, including identification of the laboratory where the test has been performed 12 BS EN 13302:2010 EN 13302:2010 (E) Bibliography [1] ASTM D 4402-06, Standard test method for viscosity determination of asphalt at elevated temperatures using a rotational viscometer 13 BS 2000 Series Energy Institute Buying Parts of BS 2000 Orders for BS 2000 publications should be addressed to either: Energy Institute – Library and Information Service 61 New Cavendish Street London W1G 7AR Tel: +44 (0)20 7467 7100 Fax: +44 (0)20 7255 1472 www.energyinst.org.uk Order standards securely via: www.energyinstpubs.org.uk or: British Standards Institution – Customer Services 389 Chiswick High Road London W4 4AL Tel: +44 (0)20 8996 9001 Fax: +44 (0)20 8996 7001 www.bsigroup.com Order hard copy standards securely via: www.bsigroup.com/shop Copyright Copyright exists in all BS 2000 publications No part of this publication may be reproduced in any form without the prior 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