BS EN 12697-41:2013 BSI Standards Publication Bituminous mixtures — Test methods for hot mix asphalt Part 41: Resistance to de-icing fluids BS EN 12697-41:2013 BRITISH STANDARD National foreword This British Standard is the UK implementation of EN 12697-41:2013 It supersedes BS EN 12697-41:2005 which is withdrawn The UK participation in its preparation was entrusted to Technical Committee B/510/1, Asphalt products A list of organizations represented on this committee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 2014 Published by BSI Standards Limited 2014 ISBN 978 580 82145 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 28 February 2014 Amendments issued since publication Date Text affected BS EN 12697-41:2013 EN 12697-41 EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM December 2013 ICS 93.080.20 Supersedes EN 12697-41:2005 English Version Bituminous mixtures - Test methods for hot mix asphalt - Part 41: Resistance to de-icing fluids Mélanges bitumineux - Méthodes d'essai pour mélange hydrocarboné chaud - Partie 41: Rộsistance aux fluides de dộverglaỗage Asphalt - Prüfverfahren für Heißasphalt - Teil 41: Widerstand gegen chemische Auftaumittel This European Standard was approved by CEN on 26 October 2013 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 © 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members Ref No EN 12697-41:2013: E BS EN 12697-41:2013 EN 12697-41:2013 (E) Contents Page Foreword Scope Normative references Term and definition Principle Apparatus .7 Solvent and other materials Preparation of test specimens .8 Procedure .9 Calculation and expression of results 10 Report 10 11 Precision 11 Bibliography 12 BS EN 12697-41:2013 EN 12697-41:2013 (E) Foreword This document (EN 12697-41:2013) 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 June 2014, and conflicting national standards shall be withdrawn at the latest by June 2014 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 12697-41:2005 This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association This document is one of a series of standards 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 — 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: Compactibility — 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 BS EN 12697-41:2013 EN 12697-41:2013 (E) — 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 — 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 BS EN 12697-41:2013 EN 12697-41:2013 (E) — 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 pre-coated 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 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 Bonding (Torque bond test — TBT, Shear bond test — SBT, Tensile Adhesion Test — TAT) — prEN 12697-49, Bituminous mixtures — Test methods for hot mix asphalt — Part 49: Determination of friction after polishing — prCEN/TS 12697-50, Bituminous mixtures — Test methods for hot mix asphalt — Part 50: Resistance to scuffing 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 12697-41:2013 EN 12697-41:2013 (E) Scope This European Standard specifies a test method to determine the resistance of bituminous materials to deicing fluids such as solutions of acetate and formate The procedure determines the surface tensile strength of a specimen of asphalt which has been stored in de-icing fluid This European Standard is primarily used as a test on asphalt to be laid on airfields, but it can be used for asphalt to be laid on roads or other paved areas 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 12697-6, Bituminous mixtures — Test methods for hot mix asphalt — Part 6: Determination of bulk density of bituminous specimens EN 12697-27, Bituminous mixtures — Test methods for hot mix asphalt — Part 27: Sampling 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 12697-35, Bituminous mixtures — Test methods for hot mix asphalt — Part 35: Laboratory mixing Term and definition For the purposes of this document, the following terms and definitions apply 3.1 surface tensile strength tensile stress at maximum force when testing the surface tensile strength according to this test method Principle Testing is performed on a sawn cylindrical specimen of asphalt on which a well-defined test surface has been drilled out in the bituminous mixture to a depth of about mm Four specimens are stored and four are not stored in a de-icing fluid A steel plate is bonded to the test surface of each specimen in turn During testing, the plate is pulled off with a tensile force increasing at a rate of 200 N/s, the force being applied perpendicular to the test specimen surface The tensile force at failure load and the mode of failure are recorded The results are compared with those for specimens which have not been stored in de-icing fluid BS EN 12697-41:2013 EN 12697-41:2013 (E) Apparatus 5.1 Vessel with a tight-fitting lid for storing specimens in the de-icing fluid 5.2 Vacuum desiccator 5.3 Vacuum pump for evacuation of the desiccator The pump shall be capable of achieving a pressure of 6,7 kPa within 10 and maintaining this pressure within ± 0,3 kPa throughout the vacuum treatment 5.4 Coring rig (optional) 5.5 Steel plates with a diameter of 50 mm and a tolerance of 0,5 mm The steel plate shall be attached by suitable means (e.g screwed) to the tensile test machine Minimum thickness of steel plate shall be 10 mm from bottom of steel plate to bottom of screw hole 5.6 Base and holder for fixing the specimen prior to testing (see Figure 1) Figure — Example of base, test specimen and tensile test machine 5.7 Tensile test machine, with force increasing rate control and automatic load recording fitted with suitable clamps and base to ensure that the tensile force can be applied without momentum perpendicular to the test specimen 5.8 Circular saw capable of cutting asphalt with finish that has no imperfections discernible by touch 5.9 Equipment for drilling out a test surface BS EN 12697-41:2013 EN 12697-41:2013 (E) 5.10 Conditioning device capable of maintaining a constant temperature of (23 ± 1) °C 5.11 Heating cabinet capable of maintaining a constant temperature of (40 ± 2) °C Solvent and other materials 6.1 Epoxy adhesive 6.2 Desiccator grease 6.3 De-icing fluid, the concentration of which shall correspond to the highest concentration intended for use on site Preparation of test specimens 7.1 Prepare a laboratory sample of asphalt mixture in accordance with EN 12697-35 or at an asphalt mixing plant 7.2 Compact a sample of a height of (60 ± 10) mm by roller compactor in accordance with EN 12697-33 and core out not less than four cylinders from the slab with a diameter of (100 ± 5) mm in accordance with EN 12697-27 Alternatively, one of the following methods of compaction can be used: — compact not less than four cylinders with a diameter of (100 ± 5) mm and a height of (60 ± 10) mm by impact compactor in accordance with EN 12697-30, by gyratory compactor in accordance with EN 12697-31 or by vibratory compactor in accordance with EN 12697-32; or — core not less than four cylinders with a diameter of (100 ± 5) mm from a compacted pavement of a thickness of at least 60 mm and trim the top and/or bottom to produce a height of (60 ± 10) mm in accordance with EN 12697-27 The compaction procedure shall be reported 7.3 Allow the cylinders to reach room temperature Mark them with a unique identification number Store the cylinders with an end face on a flat surface at a temperature of (23 ± 2) °C for (16 ± 4) h Determine the bulk density for each cylinder according to EN 12697-6 Divide the cylinders into two groups (a wet and a dry group) in which the mean bulk densities of the two groups shall not differ by more than 0,030 Mg/m 7.4 Saw the cylinders in half in a plane perpendicular to its axis Carefully drill in the centre of each specimen a test surface with a diameter of (50 ± 2) mm and a depth of (5 ± 1,5) mm 7.5 Allow the specimens to dry with an end face on a flat surface at an ambient temperature of (23 ± 2) °C between days and 42 days from the time of their manufacture NOTE The storage time influences the mechanical properties of the specimen Different storage times may be applied, but such deviation should be reported 7.6 Prepare the test surfaces of all specimens from both groups by gluing a test plate to the test surface of each of the specimens by carefully applying a thin layer of epoxy adhesive Allow the specimens to cure at a temperature of (23 ± 2) °C for (20 ± 1) h BS EN 12697-41:2013 EN 12697-41:2013 (E) Procedure 8.1 Storage 8.1.1 Store the specimens from the dry group at a temperature of (23 ± 2) °C 8.1.2 Place the specimens from the wet group in the desiccator with the test plate facing upwards 8.1.3 Pour de-icing fluid at a temperature of (23 ± 2) °C into the desiccator to a level 20 mm to 30 mm above the top of the specimen surface Evacuate to an absolute pressure of (6,7 ± 0,3) kPa within (10 ± 1) Keep the absolute pressure at (6,7 ± 0,3) kPa for h ± 10 NOTE The evacuation rate and pressure can be adjusted with a valve or rubber hose with clamp 8.1.4 Turn off the pump and carefully admit air into the desiccator until atmospheric pressure is reached Take the specimens out of the desiccator 8.1.5 Continue to store the specimens in a vessel with a tight-fitting lid at a temperature of (40 ± 2) °C for a further 70 d ± h The specimens shall be placed with the test plate upwards immersed in de-icing fluid to a level 20 mm to 30 mm above the top of the specimen surface 8.1.6 After storage, condition the specimens to the test temperature (23 ± 1) °C in the de-icing fluid for (20 ± 1) h 8.2 Test 8.2.1 Take the specimen out of the de-icing fluid and dry the steel plate with paper Directly fix the specimen in the tensile test machine and the test plate attached to the machine Apply an increase in tensile force of (200 ± 10) N/s to the test surface until failure occurs The force shall be applied perpendicular ± 5° to the test surface The test is carried out at (23 ± 1) °C NOTE The method to check that the load is applied perpendicular within the required tolerance will depend on the equipment used However, one possible method is to check that any shear force is not greater than tan(5°) = 0,087 times the vertical force 8.2.2 Record the tensile force, Fmax in newtons to one decimal place together with the type of failure (superficial, deep within the asphalt specimen or de-bonding from the glue) 8.2.3 Repeat 8.2.1 and 8.2.2 for the remaining specimens in both the wet and dry groups Calculation and expression of results 9.1 Calculate the surface tensile stress, in newtons per square millimetre to one decimal place, according to the formula: σ= Fm ax A (1) where σ is the tensile stress, in newtons per square millimetre (N/mm ); Fmax is the maximum tensile force recorded, in newtons (N); A is the area of the test surface, in square millimetres (mm ) BS EN 12697-41:2013 EN 12697-41:2013 (E) 9.2 Calculate the arithmetic mean tensile stresses from the four test specimens in the dry group, σdry, and from the four test specimens in the wet group, σwet 9.3 If the difference between the mean tensile stress and any individual tensile stress exceeds 20 % of the mean tensile stress for either the wet or the dry groups, repeat Clause 7, and 9.1 for two further specimens in each group Calculate the arithmetic mean of all the values for each group Reject any individual tensile stress value if it differs from the mean tensile stress for the group by more than 20 % of the mean tensile stress NOTE 9.4 Additional specimens can be prepared initially in anticipation of some divergence of results If any additional sample is rejected, recalculate the means for each group and repeat 9.3 9.5 If either mean is calculated from less than four measurements, repeat Clause to 9.4 for further specimens until the mean of both the dry and wet groups are the average of not less than four determinations NOTE Additional specimens can be prepared initially in anticipation of some divergence of results 9.6 Calculate the retained strength after storage in de-icing fluid, β, in percent with no decimal places according to the formula: β = σ wet × 100 σ dry (2) where β is the retained strength after storage in de-icing fluid in percent (%); σwet is the arithmetic mean wet tensile stress, in newtons per square millimetre (N/mm ); σdry is the arithmetic mean dry tensile stress, in newtons per square millimetre (N/mm ); 2 10 Report The test report shall include the following information as appropriate: a) type of asphalt, including the binder designation; b) method of compaction of the samples; c) type of de-icing fluid (e.g potassium acetate) and product name; d) concentration, density and pH-value of the de-icing fluid; e) surface tensile stress, σMax, in newtons per square millimetre, and type of failure for each specimen; f) mean tensile stress for both the wet, σwet, and dry, σdry, groups in newtons per square millimetre; g) number of samples tested and the number of individual results excluded from the calculation of the mean for both the wet and dry groups; h) retained strength after storage, β, in per cent; i) age of test specimen at test and storage conditions under which it was kept; j) number and date of this document 10 BS EN 12697-41:2013 EN 12697-41:2013 (E) 11 Precision In a round robin study, carried at the Division of Highway Engineering of the Royal Institute of Technology in Stockholm, Sweden, on a dense asphalt concrete (AC 16 with a 160/220 pen bitumen) using four different kinds of de-icing fluids, precision data of the test are determined In the round robin test, wherein nine laboratories participated, the following repeatability and reproducibility data were determined: — Repeatability sr = 130 N; r = 360 N; — Reproducibility sR = 220 N; R = 620 N For more information about this round robin test, see [1] 11 BS EN 12697-41:2013 EN 12697-41:2013 (E) Bibliography [1] 12 EKBLAD J., EDWARDS Y Precision of method for determining resistance of bituminous mixtures to deicing fluids Materials and Structures (2008) 41:1551–1562 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, 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