BS EN 12607-3:2014 BS 2000-460-3:2014 BSI Standards Publication Bitumen and bituminous binders — Determination of the resistance to hardening under influence of heat and air Part 3: RFT method BS EN 12607-3:2014 BRITISH STANDARD National foreword This British Standard is the UK implementation of EN 12607-3:2014 It supersedes BS EN 12607-3:2007 which is withdrawn The UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroleum Testing and Terminology A list of organizations represented on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 This publication does not purport to include all the necessary provisions of a contract Users are responsible for its correct application © The British Standards Institution 2014 Published by BSI Standards Limited 2014 ISBN 978 580 77115 ICS 75.140; 91.100.50 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 November 2014 BS 2000 Series Energy Institute, under the brand of IP, publishes and sells all Parts of BS 2000, and all BS EN and BS ISO petroleum test methods that would be part of BS 2000, both in its annual publication “IP Standard Test Methods for analysis and testing of petroleum and related products, and British Standard 2000 Parts” and individually Amendments/corrigenda issued since publication Date Text affected EN 12607-3 EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM November 2014 ICS 75.140; 91.100.50 Supersedes EN 12607-3:2007 English Version Bitumen and bituminous binders - Determination of the resistance to hardening under influence of heat and air - Part 3: RFT method Bitumes et liants bitumineux - Détermination de la résistance au durcissement sous l'effet de la chaleur et de l'air - Partie 3: Méthode RFT Bitumen und bitumenhaltige Bindemittel - Bestimmung der Beständigkeit gegen Verhärtung unter Einfluss von Wärme und Luft - Teil 3: RFT-Verfahren This European Standard was approved by CEN on 16 August 2014 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-CENELEC 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-CENELEC 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR 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 worldwide for CEN national Members Ref No EN 12607-3:2014 E BS EN 12607-3:2014 EN 12607-3:2014 (E) Contents Page Foreword Scope Normative references Principle 4 Apparatus .5 Sampling 6 Procedure .6 Calculation 8 Expression of results Precision 10 Test report Annex A (informative) Characteristics of thermometer 10 Bibliography 11 BS EN 12607-3:2014 EN 12607-3:2014 (E) Foreword This document (EN 12607-3:2014) 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 May 2015 and conflicting national standards shall be withdrawn at the latest by May 2015 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 12607-3:2007 This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association In comparison with EN 12607-3:2007, the following significant changes have been made: — changed/added wording of the Warning in the Scope; — EN 13302, Bitumen and bituminous binders - Determination of dynamic viscosity of bituminous binder using a rotating spindle apparatus has been added to Clause 2; — the reference to mercury thermometer has been deleted (see subclause 4.4) and Annex A is informative; — subclause 5.2: reference to RFT instead of RTFOT EN 12607 consists of the following parts under the general title “Bitumen and bituminous binders – Determination of the resistance to hardening under the influence of heat and air”: — Part 1: RTFOT method; — Part 2: TFOT method; — Part 3: RFT method 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom BS EN 12607-3:2014 EN 12607-3:2014 (E) Scope This part of EN 12607 specifies a method for measuring the combined effects of heat and air on a thin moving film of bitumen or bituminous binder, simulating the hardening which most bituminous binders undergo during mixing in an asphalt mixing plant The method is suitable for other bituminous binders than paving grade bitumen, but the reference temperature might give excessive hardening that does not resemble real conditions during mixing at the plant The method may not represent the hardening that occurs during mixing of warm mix binders The method is referred to as RFT, i.e Rotating Flask Test WARNING — Use of this European Standard can involve hazardous materials, operations and equipment This European Standard does not purport to address all of the safety problems associated with its use It is the responsibility of the user of this European standard to identify the hazards and assess the risks involved in performing this test method and to implement sufficient control measures to protect individual operators (and the environment) This includes appropriate safety and health practices and determination of the applicability of regulatory limitations prior to use If there is a likelihood of volatile components being present in a binder, this procedure should not be used It should not be used for cut-back bitumen or bituminous emulsions before these products have been stabilized, e.g in accordance with EN 13074-2 Normative references The 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 EN 58, Bitumen and bituminous binders - Sampling bituminous binders EN 1425, Bitumen and bituminous binders - Characterization of perceptible properties EN 1426, Bitumen and bituminous binders - Determination of needle penetration EN 1427, Bitumen and bituminous binders - Determination of the softening point - Ring and Ball method EN 12594, Bitumen and bituminous binders - Preparation of test samples EN 12596, Bitumen and bituminous binders - Determination of dynamic viscosity by vacuum capillary EN 13302, Bitumen and bituminous binders - Determination of dynamic viscosity of bituminous binder using a rotating spindle apparatus Principle A moving film of bituminous binder is heated in a rotating flask of a rotary evaporator at a specified temperature for a given period of time The effect of rotation is that material forming on the surface of the sample in the flask is constantly replaced, preventing the formation of a skin The effects of heat and air are determined based on the change in mass (expressed as a percentage) or as a change in the bituminous binders’ characteristics such as penetration according to EN 1426, softening point BS EN 12607-3:2014 EN 12607-3:2014 (E) ring and ball according to EN 1427 or dynamic viscosity according to EN 12596 or EN 13302, before and after hardening Apparatus Usual laboratory apparatus and glassware, together with the following: 4.1 Rotary evaporator, capable of maintaining a rotational speed of (20 ± 5) r/min, used in conjunction with a 000 ml round bottom flask with a 29/32 ground cone socket NOTE Cooler and receiver are not required 4.2 Flow control device, capable of maintaining an air flow rate of (500 ± 10) ml/min at ambient temperature NOTE To eliminate the effects of oxidation reactions, the air can be replaced with inert gases such as nitrogen 4.3 Flowmeter, capable of measuring the airflow at a rate of 500 ml/min with a maximum indication error of ± ml/min 4.4 Temperature measuring device A temperature measuring device (combining sensor and reading unit) shall: — have a range from at least 30 °C to 200 °C, — be readable to 0,1 °C or less, and — have an accuracy of 0,5 °C or better Sensors based on platinum resistance thermometers have been found suitable but other principles are also allowed The thermal response time of the sensor shall be comparable with the former used reference (see informative Annex A) The temperature measuring device shall be calibrated regularly A solid stem mercury thermometer (which used to be the former reference thermometer as described in Annex A) is also allowed if national regulations permit its use When measuring and controlling nominally constant temperatures as in this test method, the thermal response time can be rather high (e.g slow response to a change in temperature) Care shall be taken to consider this aspect since low thermal response times of the sensor can indicate greater cyclic variations than the bituminous material in practise experiences 4.5 Glass air inlet pipe, approximately 400 mm long and with an inside diameter of mm, mounted along the axis of rotation of the flask, as illustrated in Figure 4.6 Compressor, or compressed air cylinder, fitted with a reducing valve 4.7 Thermostatically controlled oil bath, regulated to (165 ± 1) °C 4.8 Oven, capable of achieving temperatures up to no less than 120 °C 4.9 Balance, accurate to ± 10 mg BS EN 12607-3:2014 EN 12607-3:2014 (E) Sampling 5.1 General Ensure that the laboratory sample is homogeneous and is not contaminated (see EN 1425) Take all necessary safety precautions and ensure that the test sample is representative of the laboratory sample from which it is taken (see EN 58) The laboratory sample shall be taken in accordance with EN 58 5.2 Test sample preparation Prepare the test sample in accordance with EN 12594 Remove a sufficient quantity of the laboratory sample to perform tests to establish the characteristics to be measured on the bituminous binder before and after the RFT hardening test If necessary, use a warmed knife and transfer it to a suitable container according to EN 12594 The sample shall be free of water Heat the sample in an oven, in its container with a loosely fitted cover to a fluid condition not exceeding 10 °C below the test temperature, for the minimum time necessary to ensure that the sample is completely fluid Homogenize the sample by stirring If special bituminous binders, modified binders or bituminous binders with high softening point are tested, it may be necessary to prepare the sample at a higher temperature In this case, heat the sample as described above and in accordance with EN 12594 For polymer modified bitumen, the temperature may not exceed 200 °C, irrespective of the softening point 5.3 Measurement The test sample shall weigh (100 ± 1) g If this quantity of sample is not sufficient for the determination of the properties that are to be subsequently measured (see Table 1), further samples shall be separately subjected to the same test procedure 5.4 Measurement of initial characteristics Determine the initial characteristics of the bituminous binder, e.g.: — P1, penetration at 25 °C according to EN 1426; — T1, softening point ring and ball according to EN 1427; — η1, dynamic viscosity at 60 °C according to EN 12596 or EN 13302 Procedure 6.1 Test with the determination of change in mass Weigh the clean and dry flask of the rotary evaporator (4.1) to the nearest mg and record the mass m0 This value will be needed to determine the mass of the sample before and after hardening Weigh (100 ± 1) g of the test sample into the flask of the rotary evaporator (4.1) Allow to cool in a desiccator to a temperature between 18 °C and 28 °C, and weigh the flask to the nearest mg and determine the mass mE of the sample Heat the oil bath (4.7) to the test temperature ± °C and mount the flask containing the sample in the bath with the axis of rotation of the flask lying at an angle of 45° to the perpendicular and the spherical body of the flask being completely immersed in the bath liquid (see Figure 1) Insert the air-inlet pipe (4.5) along the axis of rotation of the flask with a clearance of (40 ± 2) mm between the lower end of the pipe and the bottom of BS EN 12607-3:2014 EN 12607-3:2014 (E) the flask As there is a danger that the flask may detach from the rotary evaporator during the test, ensure that the flask is secured, either by an integral clamp on the rotary evaporator or by a separate joint clip of suitable material (e.g PTFE) NOTE The reference temperature of the test is 165 °C, however, it is possible to perform the test at other temperatures Heat the sample without supplying additional air while the flask rotates at (20 ± 5) r/min After (10 ± 1) min, switch on the air supply at a flow rate of (500 ± 10) ml/min Ensure that the air supply is between 18 °C and 28 °C when entering the air-inlet pipe and that throughout the test, the temperature of the bath liquid is maintained at the test temperature ± °C After (150 ± 1) min, measured from the time when the air was first admitted, switch off the rotation mechanism and air supply and remove the flask immediately from the bath liquid When the flask has cooled slightly, wipe off the oil adhering to its outer surface with a cloth saturated with a suitable volatile solvent Immediately place the flask in the oven (4.8), set at (110 ± 5) °C and keep it there for (30 ± 1) to permit the sample dispersed over the inner wall during rotation, to collect at the bottom of the flask and to allow remaining solvent to be released Cool the flask in the desiccator for (90 ± 5) to an ambient temperature between 18 °C and 28 °C and weigh the content of the flask to the nearest mg Calculate the mass, mA of the sample after hardening Carefully bring the flask to 80 °C to 90 °C above the expected ring and ball softening point (EN 1427), and pour the contents immediately from the flask into the various vessels and moulds required for the subsequent tests For polymer modified bitumen, the temperature may not exceed 200 °C, irrespective of the softening point If two or more samples of a bitumen are subjected to this procedure, pour each sample firstly into a collecting vessel maintained at an ambient temperature of between 18 °C and 28 °C When the last sample has been poured into this collecting vessel, gently heat the contents to the pouring temperature, i.e 80 °C to 90 °C above the expected ring and ball softening point (see EN 1427) and stir thoroughly For polymer modified bitumen, the temperature may not exceed 200 °C, irrespective to the softening point When thoroughly mixed, pour the contents immediately into the vessels and moulds required for subsequent tests Measure the characteristics of the hardened binder as described in 6.3 6.2 Test without the determination of change in mass Carry out the procedure described in 6.1, but without determining the mass of the sample After the sample has been submitted to the hardening test, bring the contents of the flask to the pouring temperature (see 6.1), and fill the vessels and moulds necessary for subsequent tests If two or more samples are required, carry out the procedure as described in 6.1 Measure the characteristics of the hardened binder as described in 6.3 6.3 Measurement of binder characteristics after hardening of the binder Measure the characteristics of the hardened binder within 72 h in accordance with the various methods of tests Avoid reheating the samples more than once P2 is the penetration at 25 °C, T2 is the softening point ring and ball and η2 is the dynamic viscosity at 60 °C, of the hardened binder BS EN 12607-3:2014 EN 12607-3:2014 (E) Calculation Calculate the percentage of change in mass of the sample for procedure 6.1 as follows: ∆m, change in mass = 100 × mA − mE mE (1) where mE is the mass of the sample, in grams, before the hardening; mA is the mass of the sample, in grams, after the hardening Calculate the changes in the physical characteristics after the hardening procedure as follows: P percentage of retained penetration at 25 °C = 100 × P1 (2) change in softening point ring and ball = T2 - T1 (in °C) (3) ratio of dynamic viscosities at 60 °C = η2 η1 (4) Expression of results Express a loss in mass as a negative percentage change and a gain in mass as a positive percentage change Two results of the percentage of change in mass are considered valid if they not differ by more than 0,05 % mass fraction absolute Express the percentage of change in mass value as the average of the two valid determinations, to the nearest 0,01 % mass fraction absolute Precision 9.1 Repeatability The difference between two test 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, exceed the values given 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, exceed the values given in Table in only one case in twenty BS EN 12607-3:2014 EN 12607-3:2014 (E) Table — Precision Characteristic Repeatability, r Reproducibility, R 0,15 0,20 % retained penetration at 25 °C (% absolute) 10 Increase in softening point ring and ball (°C) Values < 6,5 °C Values ≥ 6,5 °C 1,5 3,0 2,0 4,0 Ratio of dynamic viscosity at 60 °C (% of mean) 10 20 % change in mass (% absolute) (>0,3 % and < 0,80 %) These precision data are not automatically applicable at other conditions and for modified bitumens and industrial bitumens For modified bitumens, they should only be used for guidance until criteria data are available 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 part of EN 12607; c) results obtained (see Clause 8); d) test temperature; e) any deviation, by agreement or otherwise, from the procedure specified; f) date of the test Dimensions in millimetres Key oil bath level Figure — Flask assembly during rotation BS EN 12607-3:2014 EN 12607-3:2014 (E) Annex A (informative) Characteristics of thermometer Table A.1 — Characteristics of thermometer Characteristics Temperature range Units °C 30 to 200 Subdivision °C 0,5 Long lines at each °C Numbers at °C Maximum scale error °C 0,3 Scalemarks Immersion total Expansion chamber permits heating to °C 250 Total length mm 390 to 400 Stem outside diameter mm 6,0 to 8,0 Bulb length mm to 14 Bulb outside diameter mm 4,5 to 5,5 Bottom of bulb to line at °C 30 Distance mm 75 to 90 Length of scale mm 245 to 280 Scale location NOTE 10 The thermometer ASTM 16C has been found suitable BS EN 12607-3:2014 EN 12607-3:2014 (E) Bibliography [1] EN 13074-2, Bitumen and bituminous binders - Recovery of binder from bituminous emulsion or cutback or fluxed bituminous binders - Part 2: Stabilisation after recovery by evaporation 11 This page deliberately left blank This page deliberately left blank NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW British Standards Institution (BSI) BSI is the national body responsible for preparing British Standards and other standards-related 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