BS EN 12697-39:2012 BSI Standards Publication Bituminous mixtures — Test methods for hot mix asphalt Part 39: Binder content by ignition BS EN 12697-39:2012 BRITISH STANDARD National foreword This British Standard is the UK implementation of EN 12697-39:2012 It supersedes BS EN 12697-39:2004 which is withdrawn The UK participation in its preparation was entrusted to Technical Committee B/510/1, Asphalt products A list of organizations represented on this committee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 2012 Published by BSI Standards Limited 2012 ISBN 978 580 76410 ICS 93.080.20 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 31 August 2012 Amendments issued since publication Date Text affected BS EN 12697-39:2012 EN 12697-39 EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM June 2012 ICS 93.080.20 Supersedes EN 12697-39:2004 English Version Bituminous mixtures - Test methods for hot mix asphalt - Part 39: Binder content by ignition Mélanges bitumineux - Méthodes d'essai pour mélange hydrocarboné chaud - Partie 39: Détermination de la teneur en liant par calcination Asphalt - Prüfverfahren für Heißasphalt - Teil 39: Bindemittelgehalt durch Thermoanalyse This European Standard was approved by CEN on 28 April 2012 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, 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 Management Centre: Avenue Marnix 17, B-1000 Brussels © 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members Ref No EN 12697-39:2012: E BS EN 12697-39:2012 EN 12697-39:2012 (E) Contents Page Foreword Scope Normative references Terms and definitions 7 Principle 5.1 Apparatus .8 Furnace Preparatory treatment of laboratory samples of bituminous mixtures 10 7.1 7.2 7.3 Procedure 10 General 10 Test procedure for furnace with internal balance (Method A) 11 Procedure for furnace without internal balance (Method B) 12 8.1 8.2 Calculation 12 Method A 12 Method B 13 Test report 14 10 Precision data 14 Annex A.1 A.2 A.3 A.4 A (normative) Calculation of calibration value 15 General 15 Calibration based on laboratory-prepared bituminous mixtures 15 Calibration based on parallel analysis with extraction methods 16 Calibration based on dry analysis of constituent aggregate 16 Annex B (informative) Aggregate grading 19 Bibliography 20 BS EN 12697-39:2012 EN 12697-39:2012 (E) Foreword This document (EN 12697-39:2012) has been prepared by Technical Committee CEN/TC 227 “Road materials”, the secretariat of which is held by DIN 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 2012, and conflicting national standards shall be withdrawn at the latest by December 2012 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 12697-39:2004 The significant technical changes made to EN 12697-39:2004 include the following: a) The need for calibration of a mixture is clarified in the scope; b) The definitions for precision concepts are removed; c) Minor clarifications in the principle; d) The nesting of baskets is clarified in the equipment; e) The tolerance on the temperature of the oven is widened; f) The maximum weight requirements of the external balance are corrected; g) The note that the calibration value based on dry analysis of constituent aggregate can only be regarded as an estimate is deleted; h) The catch pan to be placed in the furnace with the sample baskets is added; i) Note added that the mass of the sample baskets and catch pan need not be measured if the binder content is to be calculated using the mass loss directly; j) In Annex A, the total binder load is limited to 150 g; k) Precision added to Annex B This European Standard is one of a series of standards for Bituminous mixtures as listed below: EN 12697-1, Bituminous mixtures — Test methods for hot mix asphalt — Part 1: Soluble binder content EN 12697-2, Bituminous mixtures — Test methods for hot mix asphalt — Part 2: Determination of particle size distribution EN 12697-3, Bituminous mixtures — Test methods for hot mix asphalt — Part 3: Bitumen recovery: Rotary evaporator EN 12697-4, Bituminous mixtures — Test methods for hot mix asphalt — Part 4: Bitumen recovery: Fractionating column EN 12697-5, Bituminous mixtures — Test methods for hot mix asphalt — Part 5: Determination of the maximum density BS EN 12697-39:2012 EN 12697-39:2012 (E) EN 12697-6, Bituminous mixtures — Test methods for hot mix asphalt — Part 6: Determination of bulk density of bituminous specimens EN 12697-7, Bituminous mixtures — Test methods for hot mix asphalt — Part 7: Determination of bulk density of bituminous specimens by gamma rays EN 12697-8, Bituminous mixtures — Test methods for hot mix asphalt — Part 8: Determination of void characteristics of bituminous specimens EN 12697-10, Bituminous mixtures — Test methods for hot mix asphalt — Part 10: Compactability EN 12697-11, Bituminous mixtures — Test methods for hot mix asphalt — Part 11: Determination of the affinity between aggregate and bitumen EN 12697-12, Bituminous mixtures — Test methods for hot mix asphalt — Part 12: Determination of the water sensitivity of bituminous specimens EN 12697-13, Bituminous mixtures — Test methods for hot mix asphalt — Part 13: Temperature measurement EN 12697-14, Bituminous mixtures — Test methods for hot mix asphalt — Part 14: Water content EN 12697-15, Bituminous mixtures — Test methods for hot mix asphalt — Part 15: Determination of the segregation sensitivity EN 12697-16, Bituminous mixtures — Test methods for hot mix asphalt — Part 16: Abrasion by studded tyres EN 12697-17, Bituminous mixtures — Test methods for hot mix asphalt — Part 17: Particle loss of porous asphalt specimen EN 12697-18, Bituminous mixtures — Test methods for hot mix asphalt — Part 18: Binder drainage EN 12697-19, Bituminous mixtures — Test methods for hot mix asphalt — Part 19: Permeability of specimen EN 12697-20, Bituminous mixtures — Test methods for hot mix asphalt — Part 20: Indentation using cube or cylindrical specimens (CY) EN 12697-21, Bituminous mixtures — Test methods for hot mix asphalt — Part 21: Indentation using plate specimens EN 12697-22, Bituminous mixtures — Test methods for hot mix asphalt — Part 22: Wheel tracking EN 12697-23, Bituminous mixtures — Test methods for hot mix asphalt — Part 23: Determination of the indirect tensile strength of bituminous specimens EN 12697-24, Bituminous mixtures — Test methods for hot mix asphalt — Part 24: Resistance to fatigue EN 12697-25, Bituminous mixtures — Test methods for hot mix asphalt — Part 25: Cyclic compression test EN 12697-26, Bituminous mixtures — Test methods for hot mix asphalt — Part 26: Stiffness EN 12697-27, Bituminous mixtures — Test methods for hot mix asphalt — Part 27: Sampling EN 12697-28, Bituminous mixtures — Test methods for hot mix asphalt — Part 28: Preparation of samples for determining binder content, water content and grading EN 12697-29, Bituminous mixtures — Test methods for hot mix asphalt — Part 29: Determination of the dimensions of a bituminous specimen BS EN 12697-39:2012 EN 12697-39:2012 (E) EN 12697-30, Bituminous mixtures — Test methods for hot mix asphalt — Part 30: Specimen preparation by impact compactor EN 12697-31, Bituminous mixtures — Test methods for hot mix asphalt — Part 31: Specimen preparation by gyratory compactor EN 12697-32, Bituminous mixtures — Test methods for hot mix asphalt — Part 32: Laboratory compaction of bituminous mixtures by vibratory compactor EN 12697-33, Bituminous mixtures — Test methods for hot mix asphalt — Part 33: Specimen prepared by roller compactor EN 12697-34, Bituminous mixtures — Test methods for hot mix asphalt — Part 34: Marshall test EN 12697-35, Bituminous mixtures — Test methods for hot mix asphalt — Part 35: Laboratory mixing EN 12697-36, Bituminous mixtures — Test methods for hot mix asphalt — Part 36: Determination of the thickness of a bituminous pavement EN 12697-37, Bituminous mixtures — Test methods for hot mix asphalt — Part 37: Hot sand test for the adhesivity of binder on precoated chippings for HRA EN 12697-38, Bituminous mixtures — Test methods for hot mix asphalt — Part 38: Common equipment and calibration EN 12697-39, Bituminous mixtures — Test methods for hot mix asphalt — Part 39: Binder content by ignition EN 12697-40, Bituminous mixtures — Test methods for hot mix asphalt — Part 40: In-situ drainability EN 12697-41, Bituminous mixtures — Test methods for hot mix asphalt — Part 41: Resistance to de-icing fluids EN 12697-42, Bituminous mixtures — Test methods for hot mix asphalt — Part 42: Amount of coarse foreign matter in reclaimed asphalt EN 12697-43, Bituminous mixtures — Test methods for hot mix asphalt — Part 43: Resistance to fuel EN 12697-44, Bituminous mixtures — Test methods for hot mix asphalt — Part 44: Crack propagation by semi-circular bending test EN 12697-45, Bituminous mixtures — Test methods for hot mix asphalt — Part 45: Saturation ageing tensile stiffness (SATS) conditioning test EN 12697-46, Bituminous mixtures — Test methods for hot mix asphalt — Part 46: Low temperature cracking and properties by uniaxial tension tests EN 12697-47, Bituminous mixtures — Test methods for hot mix asphalt — Part 47: Determination of the ash content of natural asphalts prEN 12697-48, Bituminous mixtures — Test methods for hot mix asphalt — Part 48: Interlayer bonding1) prEN 12697-49, Bituminous mixtures — Test methods for hot mix asphalt — Part 49: Determination of friction after polishing1) BS EN 12697-39:2012 EN 12697-39:2012 (E) prEN 12697-50, Bituminous mixtures — Test methods for hot mix asphalt — Part 50: Scuffing resistance of surface course1) WARNING — The temperature of the oven and the different accessories is extremely high during the ignition method Special care shall be taken when handling the equipment and the samples baskets etc should be placed, shielded and marked in a way that helps ensure any unpremeditated contact is avoided 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, Turkey and the United Kingdom 1) In preparation BS EN 12697-39:2012 EN 12697-39:2012 (E) Scope This document describes a test method for the determination of the binder content of samples of bituminous mixtures by ignition As such, it is an alternative to the more traditional method of extracting the binder using solvents The method can be used for evaluation of mixture composition because the remaining aggregate can be used for determining aggregate gradation and density, provided excessive breakdown of the aggregate particles does not occur at the temperature reached The results can be used for process control or checks on the compliance of mixtures However, the need for calibration of a mixture, either on the complete mixture or on each of its component materials separately, before an analysis can be carried out makes this method easier to use with regularly used mixtures rather than with an extensive range of different mixtures from different aggregate sources The test method is equally suitable for the analysis of mixtures containing unmodified or modified binders because the method has to be calibrated for each mixture being checked when calibration on mixtures is used In case of doubt/dispute, the determination of the calibration value based on laboratory-prepared bituminous mixtures (see A.1 and A.2) is the reference method 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 12597, Bitumen and bituminous binders — Terminology EN 12697-1, Bituminous mixtures — Test methods for hot mix asphalt — Part 1: Soluble binder content EN 12697-14, Bituminous mixtures — Test methods for hot mix asphalt — Part 14: Water content EN 12697-27, Bituminous mixtures — Test methods for hot mix asphalt — Part 27: Sampling EN 12697-28, Bituminous mixtures — Test methods for hot mix asphalt — Part 28: Preparation of samples for determining binder content, water content and grading Terms and definitions For the purposes of this document, the following terms and definitions apply 3.1 binder covers both bitumen and bituminous binder as described in EN 12597 3.2 corrected binder content calculated binder content after correction by the calibration value in order to compensate for components in the asphalt material itself that, due to the high temperatures during ignition, could give rise to misinterpretations 3.3 calibration value mean difference between the actual and measured binder contents for a particular bituminous mixture, in per cent, as measured from three samples Note to entry: The calibration value is a specific, material-dependent value that normally results from a loss of mass during the ignition from constituents in the mixture other than the binder The principle of the binder content by ignition is based upon a pre-determination of the corrections for the constituents used in the mixture, primarily the aggregate Note to entry: Mineral aggregates will show varying losses of mass during the test depending on their origin (petrographic composition) Examples of components that give rise to high corrections are limestone, hydrated lime and cellulose fibres BS EN 12697-39:2012 EN 12697-39:2012 (E) Note to entry: Methods for determining the calibration values are given in Annex A (normative) 3.4 target temperature temperature to which the furnace would raise the sample in the test without the rise in temperature due to the exothermic reaction of burning the binder Note to entry: The target temperature (usually 540 °C) is determined during the calibration 3.5 test completion time time from when the temperature in the furnace returns to the target temperature, after the initial rise above that temperature, to when the test is completed with the sample having nominally reached constant mass Note to entry: If a furnace with an internal balance is used, the completion time is when the loss of mass between individual readings taken at intervals for three consecutive minutes is less than a constant mass limit If a furnace without an internal balance is used, the completion time is when the change in the mass of the sample after further ignition for 15 is less than a constant mass limit Principle The test method determines the binder content of bituminous mixtures by ignition of the mixture in a furnace The corrected binder content is obtained by a calculation that includes a calibration term Calibration terms are determined for particular asphalt mixtures or aggregates Two test methods are described: Method A utilises a furnace with an internal balance; Method B permits the use of a furnace and external balance Redetermination (re-calibration or re-calculation depending on the calibration method chosen from Annex A) shall be undertaken for each significant change in the mixture, including changes in the constituent materials or their proportions NOTE The ignition process should have a controlled rise in temperature in order to avoid excessive heating of the mineral aggregate which can break down the aggregate particles depending on the petrographic composition NOTE The calculation of the calibration value based on parallel analysis with extraction methods (A.1 and A.3) is appropriate for mixtures for which the intended proportions of the constituent materials are not known 5.1 Apparatus Furnace 5.1.1 Furnace, capable of burning all the binder with the features detailed in 5.1.2 to 5.1.6 for Method A and 5.1.2 to 5.1.4 for Method B NOTE The temperature required to burn all the binder will depend on the technology used and is determined as part of the calibration procedure (see Annex A) NOTE service The furnace should not have to operate at its maximum capacity in order to allow flexibility and to ensure long 5.1.2 Sample chamber, having an internal capacity capable of taking the sample without touching the sides and with the maximum dimensions not greater than twice the minimum dimensions NOTE Larger chamber sizes may expedite testing by allowing larger sample basket(s) (and thus the material to be tested can be placed in thinner layers) 5.1.3 Automatic lock, that shall not allow the door to be opened until the completion of the test procedure, and a warning system to indicate the end of the pre-programmed temperature cycle BS EN 12697-39:2012 EN 12697-39:2012 (E) 5.1.4 System for reducing furnace emissions, by which the furnace shall be vented into a hood or to the outside and which, when properly set up, shall permit no noticeable odours escaping into the laboratory The furnace shall have a fan with the capability to pull sufficient air through the furnace to expedite the test and to reduce the escape of smoke into the laboratory NOTE The method for reducing furnace emissions can comprise a filter and a post combustion chamber that is designed to eliminate the toxic residues produced by burning the binder NOTE If mechanical ventilation is used, the air flow should be adjusted so as not to affect the operation of the equipment (e.g a forced air extraction system may result in a loss of fines and the generation of fumes from the furnace) 5.1.5 Internal balance, capable of detecting mass variations of ± 0,1 g in the sample within the baskets The balance shall be thermally isolated from the furnace chamber 5.1.6 Data collection system and a warning system, which shall be capable of being set to a value such that the loss in mass between individual readings taken at intervals for three consecutive minutes at end of the pre-programmed temperature cycle is not higher than the values stated in Table 5.2 Metal baskets, manufactured from perforated sheet of tempered stainless steel or other suitable material that permits adequate air flow through the sample and retains the majority of the sample throughout the test The dimensions shall be specified by the furnace manufacturer to provide the maximum surface area for the sample while still providing sufficient room to safely load and unload the sample The baskets shall be capable of being nested 5.3 Catch pan, made of stainless steel with dimensions sized to accommodate the metal baskets specified in 5.2 5.4 Oven, with convection or forced draft, capable of maintaining a temperature of (110 ± 5) °C in the vicinity of the samples 5.5 External balance, capable of weighing the mass of trays plus the catch pan and the test sample according to Table to ± 0,1 g 5.6 Safety equipment, including safety glasses or face shield, high temperature gloves, and long sleeved jacket 5.7 Heat-resistant surface, capable of withstanding 650 °C and able to act as a heat sink that can speed the cooling of the sample baskets, and protective cage, capable of completely surrounding the sample baskets and preventing accidental physical contact with them NOTE An appropriate sign warning of the danger of ‘Very Hot Surfaces’ should be attached to the protective cage 5.8 Pan, larger than the sample basket(s), for transferring samples after ignition 5.9 Spatulas 5.10 Bowls 5.11 Wire brushes BS EN 12697-39:2012 EN 12697-39:2012 (E) Preparatory treatment of laboratory samples of bituminous mixtures 6.1 Sampling shall be performed in accordance with EN 12697-28 to achieve a sample size as given in Table The mass of the sample in the baskets during the test shall be the same as the mass used for the calibration to ± 100 g Table — Size of sample Nominal maximum aggregate size Mass of sample Maximum constant mass limit mm g g 000 to 400 0,15 5,6 or 6,3 or or 10 000 to 600 0,15 11,2 or 12,5 or 14 or 16 000 to 700 0,20 20 or 22,4 000 to 400 0,25 31,5 000 to 000 0,30 40 or 45 000 to 000 0,40 NOTE When the mass of the test specimen exceeds the capacity of the equipment used, the test specimen may be divided into suitable increments, tested, and the results combined by weighted average for calculation of the corrected binder content NOTE Large samples of fine mixtures tend to result in incomplete ignition of the binder 6.2 The sample shall be dried to constant mass in an oven at (110 ± 5) °C unless it is known that the sample does not contain water Alternatively, the water content shall be determined in accordance with EN 12697-14 for later correction NOTE is made 7.1 If a damp sample is tested, the water content will be driven off and could be counted as binder if no correction Procedure General 7.1.1 Obtain the calibration value in accordance with Annex A for the specific mixture to be analysed either directly or from records The calibration procedure (or re-calculation for calibration based on dry analysis of constituent aggregate) shall be carried out with a mixture before undertaking any acceptance testing, and repeated at regular intervals It shall also be carried out each time there is a significant change in the mixture design A significant change is classified as being: a change of source for any component material (particularly recycled asphalt pavement); and/or a change in the proportion of the component materials (other than the binder or recycled asphalt pavement) by 10 % or more of their original proportion; and/or a change in the proportion of any recycled asphalt pavement by % or more of the original proportion; and/or a change of target binder content by 0,5 % or more NOTE The calculation of the calibration value based on parallel analysis with extraction methods (A.1 and A.3) is appropriate for mixtures for which the intended proportions of the constituent materials are not known NOTE 10 The analysis method by ignition may be affected by the type of aggregate in the mixture BS EN 12697-39:2012 EN 12697-39:2012 (E) NOTE Mineral aggregate (and organic fibres) will show varying losses of mass during the test depending on their origin (petrographic composition) Examples of components that give rise to high corrections are limestone, hydrated lime and cellulose fibres The calibration value for these components can be measured by determination on a bitumen/filler mortar (A.4) 7.1.2 The test shall be carried out using the same equipment used in the calibration, including furnace and sample baskets 7.1.3 Pre-heat the ignition furnace Record the furnace temperature at the start of the test 7.1.4 Continue the procedure in accordance with either 7.2 (Method A) for furnaces with an internal balance or 7.3 (Method B) for furnaces without an internal balance NOTE When required, the aggregate grading can be determined in accordance with Annex B after the binder content has been obtained 7.2 Test procedure for furnace with internal balance (Method A) 7.2.1 Weigh the sample at a temperature of (110 ± 5) °C on the external balance and record the sample mass Ws,w, in grams, to the nearest 0,1 g 7.2.2 Place the available sample baskets in the catch pan in turn and without any appreciable loss of temperature Distribute the relevant proportion of the sample as evenly as possibly over each sample basket before placing the next Take care to keep the material away from the edges of the sample baskets Use a spatula or trowel to level the sample NOTE To ensure consistent results, the temperature of the test portion after determining Ws,w should not be allowed to cool from 110 °C for more than before loading into the furnace 7.2.3 Weigh to 0,1 g and record the mass of the sample, sample basket(s) and catch pan Wt+s, in grams, on the external balance 7.2.4 Place the sample baskets and catch pan in the furnace ensuring that they are not in contact with either the furnace wall or any temperature probe or other protrusion inside the furnace Run the appropriate ignition programme after the oven has been pre-heated according to the manufacturer’s instructions 7.2.5 Allow the test to continue until the balance indicator displays show that the sample mass has stabilised and so that the range of consecutive weighings, taken at intervals, is within the constant mass limit in Table Remove the sample baskets, placing them on the heat-resistant surface, immediately covering with the heat guard and allow to cool to approximately room temperature to permit safe handling NOTE wall Failure of the furnace scale to stabilise may indicate that the sample baskets are in contact with the furnace NOTE The cooling time for samples removed from the furnace is dependent primarily on sample size and dispersion in the baskets The time taken to cool to approximately room temperature is unlikely to be less than 30 7.2.6 Record the loss of mass Wloss, in grams, from the internal balance Then weigh and record the mass of the sample, sample baskets and catch pan Wt+a, in grams, to 0,1 g on the external balance NOTE Wt+a need not be measured if B is to be calculated using Wloss directly, but B should be calculated using Ws and Wa whenever used for reference purposes because the internal balance measures the mass loss at elevated temperature 11 BS EN 12697-39:2012 EN 12697-39:2012 (E) 7.3 Procedure for furnace without internal balance (Method B) 7.3.1 Weigh to 0,1 g and record the mass of the sample basket(s) and catch pan Wt, in grams, at room temperature Place the sample basket(s) in the catch pan and evenly distribute the specimen in the basket(s) Weigh to 0,1 g and record the mass of the sample, sample basket(s) and catch pan Wt+s, in grams 7.3.2 Heat the sample in the furnace at the test temperature ± °C for the time determined during the calibration ± 7.3.3 Remove the sample from the furnace and allow it to cool to below 35 °C Weigh to 0,1 g and record the mass of the sample, sample basket(s) and catch pan Wt+a, in grams 7.3.4 Return the sample back into the furnace After the furnace reaches the set point temperature, heat the sample for a further 15 Repeat 7.3.3 to determine the mass of the sample after the extended ignition period 7.3.5 Repeat 7.3.4 until the change in the mass of the sample after 15 of further ignition is less than the constant mass limit in Table Calculation 8.1 Method A 8.1.1 The total mass of bituminous mixture prior to ignition Ws,w, in grams, is determined in 7.2.1 8.1.2 If the sample was not initially dried to constant mass, calculate the dried total mass of bituminous mixture prior to ignition Ws, in grams, using the following formula: 100 Ws = Ws,w × 100 + M (1) where Ws is the dried total mass of the bituminous mixture prior to ignition, in grams (g); Ws,w is the total mass of bituminous mixture prior to ignition, in grams (g); M is the moisture content determined in accordance with EN 12697-14, in percent (%) If the sample was initially dried to constant mass, the dried total mass of bituminous mixture prior to ignition Ws, in grams, is identical to the total mass of bituminous mixture prior to ignition Ws,w, in grams 8.1.3 Calculate the total mass of aggregate remaining after ignition Wa, in grams, using the following formula: Wa = Wt + a − Wt where 12 Wa is the total mass of aggregate remaining after ignition, in grams (g); Wt+a is the mass of bituminous mixture, sample basket(s) and catch pan after ignition, in grams (g); Wt is the mass of the sample basket(s) and catch pan, in grams (g) (2) BS EN 12697-39:2012 EN 12697-39:2012 (E) 8.1.4 Calculate the corrected binder content of the sample by mass of the bituminous mixture sample B, in percent, using the following formula: B= (Ws − Wa ) W × 100 − CF = loss × 100 − CF Ws Ws (3) where B is the corrected binder content of the bituminous mixture sample, in percent (%); Ws is the dried total mass of the bituminous mixture prior to ignition, in grams (g); Wa is the total mass of aggregate remaining after ignition, in grams (g); CF is the calibration value, in percent (%); Wloss is the loss of mass from the internal balance, in grams (g) NOTE Calculating B using Wloss can be carried out more quickly, but B should be calculated using Ws and Wa for reference purposes because the internal balance measures the mass loss at elevated temperature 8.2 Method B 8.2.1 Calculate the total mass of bituminous mixture prior to ignition Ws,w, in grams, using the following formula: Ws,w = Wt + s − Wt (4) where Ws,w is the total mass of bituminous mixture prior to ignition, in grams (g); Wt+s is the mass of bituminous mixture, sample basket(s) and catch pan prior to ignition, in grams (g); Wt is the mass of the sample basket(s) and catch pan, in grams (g) 8.2.2 8.1.2 Calculate the dried total mass of bituminous mixture prior to ignition Ws, in grams, in accordance with 8.2.3 Calculate the total mass of aggregate remaining after ignition Wa, in grams, using the following formula: Wa = Wt + a − Wt (5) where Wa is the total mass of aggregate remaining after ignition, in grams (g); Wt+a is the mass of bituminous mixture, sample basket(s) and catch pan after ignition, in grams (g); Wt is the mass of the sample basket(s) and catch pan, in grams (g) 8.2.4 Calculate the corrected binder content of the sample by mass of the bituminous mixture sample B, in percent, in accordance with 8.1.4 13 BS EN 12697-39:2012 EN 12697-39:2012 (E) Test report The test report shall include the following information: a) identification number, type of mixture and composition; b) date and time of testing and name of operator; c) reference to this document; d) calibration value and the method used for determining the calibration value; e) maximum temperature during testing; f) binder content (rounded to nearest 0,1 % by mass); g) aggregate grading and aggregate density, when required; h) any observation which may have an influence on the evaluation 10 Precision data 10.1 Two precision experiments in accordance with ISO 5725 (all parts) with ignition analysis using Method A have been carried out The round-robin studies for surfacing mixtures carried out in the UK and Denmark are given in Tables and 3, respectively The precision has not yet been determined for Method B Table — Precision for determination of bitumen content Binder content of mixture, m, % by mass 4,0 5,0 6,0 7,0 Repeatability, r, % by mass 0,36 0,36 0,37 0,37 Reproducibility, R, % by mass 0,60 0,71 0,82 0,93 NOTE The precision statements in Table are based on four mixture types, two replicates (plus a third using solvent analysis) and 12 laboratories participating with one result from one laboratory being deleted as outlying observations Three of the mixtures were tested from mixed material prior to compaction and one using cores taken from a compacted mat Table — Precision for determination of bitumen content Short description Repeatability, r % by mass Reproducibility, R % by mass Bituminous bound base course GAB type 16 0,30 0,33 Dense graded wearing course AB 8t 0,17 0,19 Binder course ABB 16 PmB 0,25 0,33 10.2 Based on the average values from Tables and 3, the repeatability, r, can be taken as 0,31 % by mass and the reproducibility, R, can be taken as 0,56 % by mass NOTE The acceptable range of two test results is equivalent to half the tolerance that can be permitted in the specification on the binder contents for some mixtures 14 BS EN 12697-39:2012 EN 12697-39:2012 (E) Annex A (normative) Calculation of calibration value A.1 General A.1.1 The calibration value can be determined through three alternative methods, in accordance with A.2, A.3 or A.4 NOTE Some furnaces might have an automatic mixture calibration feature The use of such furnaces is not precluded provided that equivalent results can be demonstrated by a recognised statistical method of validation A.1.2 If the calibration value is greater than 0,70 % or if the grading of the residual aggregate does not conform to the grading of the mixture or aggregate as prepared, repeat the calibration at lower target temperatures The temperature shall be reduced in steps of 20 °C to 480 °C or until the calibration value is determined as being not greater than 0,70 % and the grading of the residual aggregate conforms to the grading of the mixture or aggregate as prepared The target temperature for any subsequent testing shall be 480 °C, and the highest temperature at which the calibration value was not greater than 0,70 % and the grading of the residual aggregate conformed to the grading of the mixture or aggregate as prepared The calibration value shall be the calibration value at the target temperature NOTE Certain aggregate types, such as basalt and gritstone, may result in an unusually high calibration value (> 0,70 %) which can give erroneous grading results unless lower ignition temperatures are used NOTE If the asphalt contains aggregates such as large size limestone aggregates, it may not be possible to obtain the original grading line totally In such cases, a calibration at 540 °C (if the calibration value is not greater than 0,70 %) may be preferable than risking incomplete binder ignition (i.e a small deviation in the coarse end of the grading analysis rather than an incorrect binder content determination) Nevertheless, the grading analysis will be practically unaffected by the ignition process in most cases NOTE If using an infrared oven, it is not possible to reduce the ignition temperature In such cases, higher calibration values up to 0,85 % may be accepted A.2 Calibration based on laboratory-prepared bituminous mixtures A.2.1 If the mixing plant has not been used immediately prior for a similar mixture, prepare a sample and discard a mixture at the target binder content in order to ensure an accurate binder content in the subsequent mixtures NOTE result The discarded sample is to ensure that the equipment is suitably covered in binder and does not affect the A.2.2 Prepare three sample mixtures under laboratory conditions at the target aggregate grading and at the target binder content to the mass requirements of Table A.2.3 Place the freshly mixed specimens in the sample baskets If allowed to cool, place the samples in an oven at (110 ± 5) °C to soften the mixture prior to placing in the sample baskets A.2.4 Test the specimens in accordance with either of the tests outlined in Clause When using Method B in accordance with 7.3, record the temperature every 30 s and the time from the start of the test to when the temperature returns to the target temperature Continue to record the time until the test is completed, including the added times associated with 7.3.3 and 7.3.5, and determine the test completion time as the time from when the temperature returns to the target temperature until the test is completed 15 BS EN 12697-39:2012 EN 12697-39:2012 (E) NOTE The temperature will rise above the target temperature due to the exothermic reaction of burning the binder and will return to the target temperature when all the flammable materials have been burnt A.2.5 Perform a grading analysis on the residual aggregate in accordance with Annex B A.2.6 Calculate the measured mass loss Csi, in percent, for each sample using the following formula: Csi = (Ws − Wa ) × 100 Ws (A.1) where Csi is the measured mass loss, in percent (%); Wa is the total mass of aggregate remaining after ignition, in grams (g); Ws is the total mass of the bituminous mixture sample prior to ignition, in grams (g) A.2.7 Calculate the calibration value CF, in percent, for the mixture as the average of the three results using the following formula: CF = (CS1 + CS2 + CS3 ) − Bmix (A.2) where CF is the calibration value, in percent (%); CSi is the measured mass loss for the i sample, in percent (%); Bmix is the target binder content added to the mixture, in percent (%) A.3 Calibration based on parallel analysis with extraction methods A.3.1 Obtain not less than three samples of the bituminous mixture Split each sample into two portions in accordance with EN 12697-27 A.3.2 Analyse the binder content of one portion from each sample using solvent analysis in accordance with one of the acceptable extraction methods of EN 12697-1 A.3.3 Calibrate the mixture in accordance with A.2.2 to A.2.7 but using the value of binder content found from the solvent analysis as Bmix NOTE If the correction is determined by parallel analysis without reference-mixtures with known binder content, the accuracy of the calibration will be reduced Calibration by this procedure consists of the difference between the results of the two methods and will, therefore, be influenced by the combined variance of the two methods A.4 Calibration based on dry analysis of constituent aggregate NOTE If the same aggregates are used in many different asphalt products at the same asphalt plant, it may be advantageous to determine the calibration value separately for each of the constituent materials included in the relevant mixture compositions and subsequently calculate the combined calibration value NOTE For bituminous mixtures containing hydrated lime or cellulose fibres, it will not be possible to determine the true calibration value by A.4 Instead, the calibration value for filler components can be estimated by using A.2 A known amount of pre-dried filler is mixed with a known amount of bitumen to a stiff mortar The total binder load should not 16 BS EN 12697-39:2012 EN 12697-39:2012 (E) exceed 150 g because of the possibility of excessive exothermic heat generation The mortar is tested in the furnace The calibration value, C FF, is calculated using the following formula: CFF = C s − BFM (A.3) where CFF is the calibration value, in percent (%); Cs is the measured mass loss for the filler mortar, in percent (%); BFM is the binder content in the filler mortar, in percent (%) A.4.1 Prepare three calibration specimens of the aggregate and reclaimed asphalt (if applicable) only The mass of each specimen shall conform to Table A.4.2 Preheat a specimen in an oven at (110 ± 5) °C for 25 Thoroughly mix the specimen with a spatula and then introduce it into the sample basket(s) A.4.3 Test the specimens in accordance with Clause 7, leaving the specimen in the furnace for either the minimum time given in Table A.1 or until the range of consecutive weighings, taken at intervals, is within the constant mass limit in Table A.1, whichever occurs first NOTE The target temperature for the calibration (but not for subsequent testing of mixtures with that calibration) can be increased by 40 °C to compensate for the lack of an exothermic reaction Table A.1 — Time in furnace for aggregate2) (only samples) Sample size Minimum time Maximum constant mass limit g g 000 to 999 40 0,4 000 to 999 60 0,7 000 to 000 75 0,8 A.4.4 Perform a grading analysis on the residual aggregate in accordance with Annex B A.4.5 Calculate the measured mass loss Csi, in percent, for each sample in accordance with A.2.6 A.4.6 If no reclaimed asphalt is used, calculate the aggregate calibration value CFA, in percent, for the aggregate grading as the average of the three results using the following formula: CFA = (C s1 + C s2 + C s3 ) (A.4) where 2) CFA is the aggregate calibration value, in percent (%); Csi is the measured mass loss for the i sample, in percent (%) Table also appropriate to reclaimed asphalt, if applicable 17 BS EN 12697-39:2012 EN 12697-39:2012 (E) A.4.7 If reclaimed asphalt is used, calculate the aggregate calibration value CFA, in percent, for the aggregate grading as the average of the three results using the following formula: CFA = (Cs1 + Cs2 + Cs3 ) P − Bra × 100 (A.5) where CFA is the aggregate calibration value, in percent (%); Csi is the measured mass loss for the i sample, in percent (%); Bra is the estimated binder content of the reclaimed asphalt, in percent (%); Pra is the proportion of reclaimed asphalt, in percent (%) A.4.8 For a particular mixture using the aggregate grading for which the aggregate calibration value has been derived, calculate the calibration value, CF, in percent, using the following formula: B CF = CFA × 1 − A 100 (A.6) where CF is the calibration value, in percent (%); CFA is the aggregate calibration value, in percent (%); BA is the nominal binder content of the asphalt mixture to be tested, in percent (%) NOTE iteration If the nominal binder content is not known, the measured binder content will need to be used, requiring A.4.9 If calibration values are required from combinations of different aggregates, repeat A.4.1 to A.4.8 for each of the component aggregates For each particular mixture using a combination of the aggregates, calculate the calibration value, CF, in percent, using the following formula: CF = ∑ ( pi × CFA,i ) × 1 − 100 BA 100 (A.7) where CF is the calibration value, in percent (%); pi is the proportion of aggregate type i in the asphalt mixture to be tested, in percent, where CFA,i is the aggregate calibration value determined for aggregate type i, in percent (%); BA is the nominal binder content of the asphalt mixture to be tested, in percent (%) NOTE value 18 ∑( pi ) = 100; For practical reasons, the asphalt mixtures at a plant may be divided into groups using the same calibration BS EN 12697-39:2012 EN 12697-39:2012 (E) Annex B (informative) Aggregate grading B.1 The specimen is allowed to cool to room temperature in the sample baskets B.2 The contents of the baskets are emptied into a flat pan A small wire sieve brush is used to ensure that any residual fines are removed from the baskets B.3 The remaining sample, consisting of mineral aggregate, should, when required, be used for determination of aggregate grading in accordance with EN 12697-2 and/or aggregate density in accordance with EN 1097-6 NOTE Deterioration of particles can occur for some types of aggregate NOTE Wet sieving is preferable to dry sieving because the filler particles tend to become stuck to the surface of the mineral aggregate procedure by the ignition process and can only be removed with the washing process of the wet sieving method B.4 The precision is indicated by the differences found in gradings from studies undertaken in France (see Table B.1) Table B.1 — Permissible differences in grading: France Francea Sieve Permissible differences 10 mm ±5% mm ±3% mm ±2% 0,080 mm ± 0,8 % a Contrôle des enrobés sans solvants (CESS) Une méthode propre et fiable, Eric Godard, RGRA n° 806, Mai 2002 19 BS EN 12697-39:2012 EN 12697-39:2012 (E) Bibliography [1] EN 1097-6, Tests for mechanical and physical properties of aggregates — Part 6: Determination of particle density and water absorption [2] EN 12697-2, Bituminous mixtures — Test methods for hot mix asphalt — Part 2: Determination of particle size distribution [3] ISO 5725 (all parts), Accuracy (trueness and precision) of measurement methods and results 20 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 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