BS EN 12607-1:2014 BS 2000-460-1:2014 BSI Standards Publication Bitumen and bituminous binders — Determination of the resistance to hardening under influence of heat and air Part 1: RTFOT method BS EN 12607-1:2014 BRITISH STANDARD National foreword This British Standard is the UK implementation of EN 12607-1:2014 It supersedes BS EN 12607-1:2007 which is withdrawn The UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroleum Testing and Terminology A list of organizations represented on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 77120 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 12607-1 EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM November 2014 ICS 75.140; 91.100.50 Supersedes EN 12607-1:2007 English Version Bitumen and bituminous binders - Determination of the resistance to hardening under influence of heat and air - Part 1: RTFOT method Bitumes et liants bitumineux - Détermination de la résistance au durcissement sous l'effet de la chaleur et de l'air - Partie : Méthode RTFOT Bitumen und bitumenhaltige Bindemittel - Bestimmung der Beständigkeit gegen Verhärtung unter Einfluss von Wärme und Luft - Teil 1: RTFOT-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 12607-1:2014 E BS EN 12607-1:2014 EN 12607-1:2014 (E) Contents Page Foreword Scope Normative references Principle Apparatus .5 Sampling 10 Procedure 10 Calculation 11 Expression of results 12 Precision 12 10 Test report 13 Annex A (informative) Characteristics of thermometer 14 Bibliography 15 BS EN 12607-1:2014 EN 12607-1:2014 (E) Foreword This document (EN 12607-1:2014) 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 12607-1:2007 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 12607-1:2007, the following significant changes have been made: — changed/added wording of the Warning in the Scope; — the reference to mercury thermometer has been deleted (see subclause 4.3) and Annex A is informative; — the second note in subclause 6.2 has been added to clarify the duration of the conditioning; — the second to last paragraph in subclause 6.2 highlights that it is allowed for polymer modified bitumen to raise the temperature shortly to 180 °C to pour the sample out of the containers 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 12607-1:2014 EN 12607-1:2014 (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 described is not applicable to some modified binders or to those where the viscosity is too high to provide a moving film In some cases the sample may creep out of the glass container and flow on the heating elements of the oven during testing The method is suitable for other bituminous binders than paving grade bitumen, but the reference temperature might give excessive hardening that 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 RTFOT, i.e Rolling Thin Film Oven 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 cutback 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 12735-1, Copper and copper alloys ― Seamless, round copper tubes for air conditioning and refrigeration ― Part 1: Tubes for piping systems EN 13302, Bitumen and bituminous binders ― Determination of dynamic viscosity of bituminous binder using a rotating spindle apparatus BS EN 12607-1:2014 EN 12607-1:2014 (E) Principle A moving film of bituminous binder is heated in an oven to a specified temperature for a given period of time with a constant supply of air The effects of heat and air are determined based on the change in mass (expressed as a percentage) or on the change in the bituminous binder's characteristics such as penetration according to EN 1426, softening point according to EN 1427 or dynamic viscosity according to EN 12596 or EN 13302, before and after the period in the oven The reference temperature of this conditioning is 163 °C Apparatus Usual laboratory apparatus and glassware, together with the following: 4.1 Oven, rectangular, double-walled and electrically heated The inside dimensions excluding the air plenum shall be as follows: — height: (340 ± 15) mm; — width: (405 ± 15) mm; — depth: (445 ± 15) mm The front door shall contain a symmetrically located window of the following dimensions: — width: (320 ± 15) mm; — height: (215 ± 15) mm This window shall contain two sheets of heat resistant glass separated by an air space The window shall permit an unobstructed view of the interior of the oven The top of the upper heating element shall be (25 ± 9) mm below the oven floor The oven shall be ventilated by convection currents of air; the oven shall have air inlets and outlets for the evacuation of hot gases The air inlets toward the bottom of the oven shall be located so that the air is able to flow around the heating elements and their total open area shall be (1 500 ± 100) mm The outlets for the hot gases evacuation shall be located in the upper part of the oven and their total open area shall be (1 000 ± 100) mm The oven shall incorporate an air flow around the side walls and ceiling The air plenum (between the wall and the sheaths) shall be of uniform thickness (38 ± 3) mm (Figure a)) The inside of the oven shall be equipped with a vertical circular aluminium carriage with a diameter of (300 ± 10) mm (Figure a)) The horizontal axis of the circular carriage is located (160 ± 10) mm from the upper inside wall of the oven, excluding the air plenum The carriage shall be provided with suitable openings and spring clips for firmly holding eight glass containers in a horizontal position (Figure b)) The carriage shall be mechanically driven by a 20 mm diameter shaft and shall make 15 turns within (60 ± 1) s The front surface of the carriage shall be (110 ± 5) mm from the rear inside wall of the oven On the upper surface and at the midpoint of the width of the oven and (150 ± 5) mm from the front face of the carriage, a squirrel cage-type fan shall be mounted with an outside diameter of (135 ± 5) mm and a thickness of (75 ± 5) mm and turned at (1 725 ± 100) r/min by an externally mounted motor BS EN 12607-1:2014 EN 12607-1:2014 (E) The fan shall be set so that it turns in an opposite direction to its vanes The air flow characteristics shall be suction from the floor of the oven then flow along the walls in the sheaths fitted for this purpose and exhaust at the upper surface through the fan (Figure a) and Figure b)) The oven shall be equipped with a thermostat capable of maintaining a constant temperature to ± 0,5 °C The corresponding regulation probe shall be situated on the right side of the oven as described in Figure or symmetrically on the left side The temperature shall be recorded inside the oven with the reading point (25 ± 5) mm below a horizontal line through the axle of the carriage, (50 ± 5) mm from the inside wall and (115 ± 5) mm from the front face of the carriage The heating capacity shall be sufficient to bring the oven back to the test temperature within a 10 period after insertion of the containers The oven shall be equipped with an air jet positioned to blow heated air into each container at its lowest point of travel The air jet shall have an outlet orifice with a diameter of (1,0 ± 0,1) mm connected to a copper tubing (see EN 12735-1) with an external diameter of (8,0 ± 0,1) mm and a length of (7,60 ± 0,05) m This tube shall be coiled to lie flat on the bottom of the oven and lead to a source of oil-free, dried and dust-free air The orifice of the tubing shall be between mm and 10 mm from the opening in the glass container The air jet shall blow along the main axis of the glass container NOTE Activated silica gel treated with an indicator is a satisfactory desiccant for the air The performance of the equipment (particularly the motor rotation speed and the fan rotation speed) should be verified and action should be taken if it does not comply with the requirements stated in this method 4.2 Flow meter, capable of measuring the airflow at a rate of (4,0 ± 0,2) l/min at ambient temperature and pressure 4.3 Temperature measuring device A temperature measuring device (combining sensor and reading unit) shall — have a range from at least 150 °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 permits 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 practice experiences 4.4 Glass containers, (in which the sample of bituminous binder is subjected to the test), made of heatresistant glass conforming to the dimensions shown in Figure NOTE An outside opening (convex) is more suitable than the standard inside (concave) opening to facilitate the pouring of the hardened bituminous binder BS EN 12607-1:2014 EN 12607-1:2014 (E) A special container with a removable ground-glass stopper (which allows easier cleaning) can be used for non-referee purposes provided all the standardized dimensions are satisfied 4.5 Balance, accurate to ± mg Dimensions in millimetres a) Oven (front view) b) Squirrel cage-type fan (bottom view) Key upper vents air flow direction of rotation thermometer regulation probe sheaths Figure — Oven and squirrel cage-type fan BS EN 12607-1:2014 EN 12607-1:2014 (E) Dimensions in millimetres a) Front view b) Side view Key (3,0 ± 0,1) mm thick aluminium disc; diameter: (300 ± 10) mm spring clips glass container retainer oven sample glass container thermometer copper tubing; diameter: (8,0 ± 0,1) mm orifice; diameter: (1,0 ± 0,1) mm spacer length: (55 ± 1) mm; external diameter: (12 ± 1) mm, internal diameter: (6,5 ± 1,0) mm spacer length: (20 ± 1) mm; external diameter: (12 ± 1) mm, internal diameter: (6,5 ± 1,0) mm 10 M6 screws at 90 °; on a diameter of (280 ± 2) mm 11 holes, diameter: (66,7 ± 1,0) mm; every 45° on a diameter of (200 ± 5) mm Figure — Circular metal carriage BS EN 12607-1:2014 EN 12607-1:2014 (E) Dimensions in millimetres Key inside (concave) or outside (convex) opening wall thickness (2,4 ± 0,3) mm Figure — Glass container BS EN 12607-1:2014 EN 12607-1:2014 (E) Sampling 5.1 General Make sure 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 RTFOT 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 temperature not exceeding 10 °C below the test temperature for the minimum time necessary to ensure the sample is completely fluid Homogenize the sample by stirring If special bituminous binders, modified binders or bituminous binders with a high softening point are tested, it may be necessary to prepare the sample at a higher temperature In this case, heat the sample in accordance with EN 12594 For polymer modified bitumen, the temperature may not exceed 200 °C, irrespective of the softening point 5.3 Initial characteristics Determine the initial characteristics of the bituminous binder e.g.: — P1, penetration at 25 °C (EN 1426); — T1, ring and ball softening point (EN 1427); — η1, dynamic viscosity at 60 °C (EN 12596) Procedure 6.1 Test conditions Make sure the oven (4.1) is level so that the horizontal axes of the glass containers (4.4) when in position in the carriage, are level Pre-heat the oven to the test temperature NOTE The reference temperature of the test is (163 ± 1) °C, however, it is possible to perform the test at other temperatures Check that the RTFOT oven can endure elevated temperatures before running the test NOTE Pre-heating the oven for h is generally sufficient 6.2 Determination and measurement Weigh separately at least two identifiable empty glass containers (labelled A and B for example) (4.4) to the nearest mg and tare the other containers NOTE It may be advantageous to document the mass of all the glass containers to determine the change in mass even if the procedure described fails for the containers A and B Pour (35,0 ± 0,5) g of the sample into each of the glass containers using the number of containers sufficient for executing all the planned characterization tests 10 BS EN 12607-1:2014 EN 12607-1:2014 (E) A To determine the percentage change in mass, take the two labelled containers (having empty masses m B and m 0) containing the bituminous binder (A and B), allow them to cool to ambient temperature for h in a A B desiccator, and weigh them separately to within mg to determine m and m When the oven has attained the set test temperature, arrange the containers holding the bituminous binder in the carriage so that the carriage is balanced Fill any unused spaces in the carriage with empty containers Close the door and rotate the carriage assembly at a rate of (15,0 ± 0,2) r/min Start the airflow at a set rate of (4,0 ± 0,2) l/min Maintain the samples in the oven and the air flowing for (75 ± 1) from the time the temperature reaches °C below the test temperature If the test temperature of (163 ± 1) °C is not reached within the first 15 min, discontinue the test At the end of the test period, remove the containers from the oven NOTE The aging time (75 ± min) starts from the time when the temperature of the oven is returned to (163 ± 1) °C The time required to reach the oven (163 ± 1) °C is not part of the duration of aging Allow the two containers (A and B) to cool for about h to ambient temperature in a desiccator Weigh to A B within mg to determine the relative masses, m and m Discard the residue from mass change determination, and not use it for other tests If additional runs are carried out, all residue can be combined unless mass change determination is specifically requested for these runs For the other containers, immediately pour all the hardened binder into the same collecting vessel before any cooling, and without reheating the containers Stir to homogenize the mixture but avoid incorporating air bubbles For polymer modified bitumen it is allowed – according to EN 12594 — shortly to elevate the temperature to 180 °C (maximum) to pour the sample out of the containers Any scraping tool or technique may be used, as long as an average of 90 % or more of the residue is removed from the sample containers It has been determined that circumferential scraping tends to be more effective than lengthwise scraping 6.3 Measurement Measure the characteristics of the hardened binder (EN 1426, EN 1427, EN 12596 or EN 13302) within 72 h in accordance with the various methods of the test and avoid reheating the sample more than once P2 is the penetration at 25 °C, T2 is the ring and ball softening point and η2 is the dynamic viscosity at 60 °C of the hardened binder If the desired suite of tests require successive conditionings to establish the necessary amount of material the time limit of 72 h can be passed The actual time from the first conditioning to the time of test shall be reported under Clause 10 e) Calculation Calculate the changes in the physical characteristics after the hardening procedure according to Formulae (1) to (3): P2 P1 (1) change in ring and ball softening point (in °C) = T2 − T1 (2) percentage of retained penetration at 25 °C ratio of dynamic viscosities at 60 °C = η2 η1 = 100 × (3) 11 BS EN 12607-1:2014 EN 12607-1:2014 (E) Calculate the percentage of the change in mass of the sample according to Formulae (4) and (5): percentage of change in mass (container A) percentage of change in mass (container B) m A − m A1 m A1 − m A m B − m B1 m B1 − m B = 100 × = 100 × (4) (5) Expression of results Express a loss in mass as a negative percentage change and a gain in mass as a positive percentage change The two results of percentage change in mass for containers A and B are considered valid if they not differ by more than 0,05 % mass fraction absolute Express the percentage of change in mass as the average of the two valid determinations to the nearest 0,01 % mass fraction absolute If the value of a physical property is measured on the sample after RTFOT, the change of the property can be expressed either as the absolute change in value in the units that the property is measured in (as for softening point Ring and Ball, EN 1427), or as a retained value in percent (as for needle penetration, EN 1426), or as a ratio of values (as for dynamic viscosity, EN 12596) Express a reduction in the value of a property as a negative value, or as a negative percentage change, and an increase in the value of a property as a positive value, or as a positive percentage change A reduction in value of a property when given as a ratio is expressed as a positive value less than unity An increase in the value of a property when given as a ratio is expressed as a positive value greater than unity 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 12 BS EN 12607-1:2014 EN 12607-1:2014 (E) Table — Precision Characteristic Repeatability, r Reproducibility, R Change in mass (% absolute) (>0,3 % and < 0,80 %) 0,15 0,20 10 values < 6,5 °C 1,5 2,0 values ≥ 6,5 °C 3,0 4,0 10 20 Retained at 25 °C penetration (% absolute) Increase in ring softening point Ratio of at 60 °C and ball (°C) dynamic viscosities (% of mean) NOTE These precision data were determined for a test temperature of 163 °C and are not automatically applicable at other conditions, for modified bitumen and for industrial bitumen For modified bitumen they should only be used for guidance, until data are available NOTE The precision of retained penetration is the precision of the calculated ratio (in %) of the penetration of the hardened binder over the penetration of the original, unhardened binder There is no precision statement for penetration on the hardened binder itself The determination of retained penetration is related to EN 12591 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) temperature at which the test was carried out; d) results obtained (see Clause 8); e) any deviation, by agreement or otherwise, from the procedure specified; f) date of the test 13 BS EN 12607-1:2014 EN 12607-1:2014 (E) Annex A (informative) Characteristics of thermometer Table A.1 — Characteristics of thermometer Characteristics Unit Temperature range °C 155 to 170 Subdivision °C 0,5 Long lines at each °C Numbers at each °C 155, 160, 162, 164, 165, 170 Maximum scale error °C 0,5 Scale marks Immersion total Expansion chamber permits heating to °C 200 Total length mm 150 to 160 Stem outside diameter mm 5,5 to 7,0 Bulb length mm 10 to 15 Bulb outside diameter mm 5,0 to stem diameter Bottom of bulb to line at °C 155 Distance mm 50 to 60 Length of scale mm 40 to 60 mm 30 Scale location Maximum distance chamber to the top NOTE 14 of contraction The thermometer ASTM 13C/IP47C has been found suitable BS EN 12607-1:2014 EN 12607-1:2014 (E) Bibliography [1] ASTM D2872-04, Standard Test Method for Effect of Heat and Air on a Moving Film of Asphalt (Rolling Thin-Film Oven Test) [2] EN 12591, Bitumen and bituminous binders — Specifications for paving grade bitumens [3] 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 15 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 publications, information and services BSI is incorporated by Royal Charter British Standards and other standardization products are published by BSI Standards Limited About us Revisions We bring together business, industry, government, consumers, innovators and others to shape their combined 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