Bituminous mixtures - Test methods for hot mix asphalt - Part 1: Soluble binder content

This document describes test methods for the determination of the soluble binder content of samples of bituminous mixtures.
The test methods described are suitable for quality control purposes during the production of plant mix and for checking compliance with a product specification.
For the analysis of mixtures containing modified binders, the guidance of Annex D should be followed.

Asphalt - Prüfverfahren für Heißasphalt - Teil 1: Löslicher Bindemittelgehalt

Dieses Dokument beschreibt Prüfverfahren zur Bestimmung des löslichen Bindemittelgehaltes in Proben aus Asphalt. Die beschriebenen Prüfverfahren sind zur Qualitätskontrolle während der Herstellung des Mischgutes sowie zur Überprüfung der Übereinstimmung mit einer Produktspezifikation geeignet. Zur Untersuchung von Mischgut, das modifizierte Bindemittel enthält, sollten die Hinweise in Anhang D
beachtet werden.

Mélanges bitumineux - Méthode d'essai pour mélange hydrocarboné à chaud - Partie 1: Teneur en liant soluble

Le présent document décrit des méthodes d’essai pour déterminer la teneur en liant soluble d’échantillons de matériaux enrobés. Les méthodes d’essai décrites sont applicables pour la maîtrise de la qualité de production en usine et pour les vérifications de conformité aux spécifications des produits. Pour l'analyse des mélanges contenant des liants modifiés, il convient de suivre les lignes directrices données en Annexe D.

Bitumenske zmesi - Preskusne metode za vroče asfaltne zmesi - 1. del: Topni delež veziva

Ta dokument opisuje preskusne metode za določitev topnega deleža veziva v vzorcih bitumenskih zmesi. Opisane preskusne metode so ustrezne za namene kontrole kakovosti med proizvodnjo v asfaltnem obratu in za preverjanje skladnosti s specifikacijo izdelka. Pri analizi zmesi, ki vsebujejo modificirana veziva, naj bi se upoštevala navodila iz dodatka D.

General Information

Status
Withdrawn
Publication Date
05-Jun-2012
Withdrawal Date
10-Mar-2020
Current Stage
9960 - Withdrawal effective - Withdrawal
Due Date
06-Jun-2012

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Asphalt - Prüfverfahren für Heißasphalt - Teil 1: Löslicher BindemittelgehaltMélanges bitumineux - Méthode d'essai pour mélange hydrocarboné à chaud - Partie 1: Teneur en liant solubleBituminous mixtures - Test methods for hot mix asphalt - Part 1: Soluble binder content93.080.20Materiali za gradnjo cestRoad construction materialsICS:Ta slovenski standard je istoveten z:EN 12697-1:2012SIST EN 12697-1:2012en,fr,de01-september-2012SIST EN 12697-1:2012SLOVENSKI

STANDARDSIST EN 12697-1:20061DGRPHãþD
SIST EN 12697-1:2012
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 12697-1
June 2012 ICS 93.080.20 Supersedes EN 12697-1:2005English Version

Bituminous mixtures - Test methods for hot mix asphalt - Part 1: Soluble binder content

Mélanges bitumineux - Méthode d'essai pour mélange hydrocarboné à chaud - Partie 1: Teneur en liant soluble

Asphalt - Prüfverfahren für Heißasphalt - Teil 1: Löslicher Bindemittelgehalt 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 12697-1:2012: ESIST EN 12697-1:2012

EN 12697-1:2012 (E) 2 Contents PageForeword ..............................................................................................................................................................4Introduction .........................................................................................................................................................81 Scope ......................................................................................................................................................92 Normative references ............................................................................................................................93 Terms and definitions ...........................................................................................................................94 Preparatory treatment of laboratory samples of bituminous mixtures......................................... 105 Determination of binder content ....................................................................................................... 105.1 General principles of test ................................................................................................................... 105.2 Binder extraction ................................................................................................................................ 115.2.1 Solvent ................................................................................................................................................. 115.2.2 Apparatus ............................................................................................................................................ 115.2.3 Procedure ............................................................................................................................................ 115.3 Separation of mineral matter ............................................................................................................. 125.3.1 Apparatus ............................................................................................................................................ 125.3.2 Procedure ............................................................................................................................................ 125.4 Binder quantity .................................................................................................................................... 125.4.1 Apparatus ............................................................................................................................................ 125.4.2 Procedure ............................................................................................................................................ 125.5 Calculation and expression of results .............................................................................................. 125.5.1 General ................................................................................................................................................. 125.5.2 Binder determined by difference ....................................................................................................... 135.5.3 Binder by total recovery ..................................................................................................................... 135.5.4 Binder by recovery from portion (volume calculation) ................................................................... 135.5.5 Binder by recovery from portion (mass calculation) ...................................................................... 146 Drying to constant mass .................................................................................................................... 146.1 General ................................................................................................................................................. 146.2 Apparatus ............................................................................................................................................ 146.3 Procedure ............................................................................................................................................ 157 Reporting of results ............................................................................................................................ 157.1 Results ................................................................................................................................................. 157.2 Test report ........................................................................................................................................... 158 Precision data ..................................................................................................................................... 158.1 Precision — Experiment 1 ................................................................................................................. 168.2 Precision — Experiment 2 ................................................................................................................. 168.3 Precision — Experiment 3 ................................................................................................................. 178.4 Precision — Experiment 4 ................................................................................................................. 17Annex A (informative)

Guidance on the determination of binder content ................................................. 18A.1 Evaluation of the results .................................................................................................................... 18A.2 Effect of water content ....................................................................................................................... 18A.3 Choice of test equipment and the sequence of operations ........................................................... 19A.4 Determination of total binder content............................................................................................... 19Annex B (normative)

Use of equipment for the determination of binder content ..................................... 20B.1 Binder extraction ................................................................................................................................ 20B.1.1 Hot extractor (paper filter) method ................................................................................................... 20B.1.2 Hot extractor (wire mesh filter) method............................................................................................ 23B.1.3 Soxhlet extractor method .................................................................................................................. 24SIST EN 12697-1:2012

EN 12697-1:2012 (E) 3 PageB.1.4 Bottle rotation machine method........................................................................................................27B.1.5 Centrifuge extractor method .............................................................................................................. 29B.1.6 Cold mix dissolution of bitumen by agitation .................................................................................. 32B.2 Separation of mineral matter .............................................................................................................. 32B.2.1 Continuous flow centrifuge ................................................................................................................ 32B.2.2 Pressure filter ...................................................................................................................................... 34B.2.3 Bucket type centrifuge — Type 1 ....................................................................................................... 35B.2.4 Bucket type centrifuge — Type 2 ....................................................................................................... 36B.3 Soluble binder content ........................................................................................................................ 37B.3.1 Method by recovery from a portion using a volume calculation .................................................... 37B.3.2 Method by recovery from a portion using a mass calculation ....................................................... 39Annex C (normative)

Determination of residual mineral matter in the binder extract by incineration .......................................................................................................................................... 40C.1 General ................................................................................................................................................. 40C.2 Method 1 ............................................................................................................................................... 40C.2.1 Apparatus ............................................................................................................................................. 40C.2.2 Reagent................................................................................................................................................. 40C.2.3 Procedure ............................................................................................................................................. 40C.3 Method 2 ............................................................................................................................................... 41C.3.1 Apparatus ............................................................................................................................................. 41C.3.2 Procedure ............................................................................................................................................. 41Annex D (informative)

Guidance on determination of soluble binder content of mixtures with polymer-modified binders .................................................................................................................. 43D.1 General ................................................................................................................................................. 43D.2 Preparatory treatment of laboratory samples of bituminous mixtures ......................................... 43D.3 Determination of binder content ........................................................................................................ 43D.3.1 General principles of test ................................................................................................................... 43D.3.2 Binder extraction ................................................................................................................................. 43D.3.3 Separation of mineral matter .............................................................................................................. 45D.3.4 Binder quantity .................................................................................................................................... 46D.3.5 Calculation and expression of results .............................................................................................. 46D.4 Drying to constant mass ..................................................................................................................... 46D.5 Reporting of results ............................................................................................................................ 46D.6 Precision data ...................................................................................................................................... 46Bibliography ...................................................................................................................................................... 47

SIST EN 12697-1:2012

EN 12697-1:2012 (E) 4 Foreword This document (EN 12697-1:2012) has been prepared by Technical Committee CEN/TC TC “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 12697-1:2005. Compared with EN 12697-1:2005, the following changes have been made: a) Removal of warning that the precision may be comprised with polymer-modified binders even when following Annex D;

b) For the separation of mineral, a note is added that the residue depends on the solvent and the equipment used; c) The desiccator is made optional with the method of achieving a moisture-free atmosphere not fixed; d) The definition of constant mass is changed; e) Alternative procedures for determination of binder are extended; f) Volume units are corrected from mm³ to 10³ mm³ as appropriate; g) In Annex B, note is added to ensure the binder is well dissolved; h) In Annex B, density of perchloroethylene is changed from (1,6 ± 0,05) g/cm³ at 24 °C to (1,6 ± 0,05) Mg/m³ at 20 ºC; i) In Annex B, weighing of multiple sieves that are fitted to the feed funnel is allowed; j) In Annex B, repeating the procedure with a second cup in the centrifuge is undertaken with half the flow rate; k) In Annex B, note is added that the second run is unnecessary for some centrifuges with larger capacities; l) In Annex C, M2 is clarified as being the mass of fine mineral matter; m) In Annex C, the procedures for collecting the recovered binder are clarified; n) In Annex D, a note is added that a good solubility of the polymer-modified binder does not always guarantee a good extraction of the PmB in the bituminous mixture; o) In Annex D, the discussion on different solvents is refined; p) In Annex D, the flow rate is adjusted rather than just checked to avoid overflowing; SIST EN 12697-1:2012

EN 12697-1:2012 (E) 5 q) In Annex D, the exceptions on the apparatus and procedure for the centrifuge extractor method are removed and notes added; r) In Annex D, note is added to continuous flow centrifuge; s) In Annex D, precision statement is changed. 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 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 SIST EN 12697-1:2012

EN 12697-1:2012 (E) 6 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 prEN 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 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 SIST EN 12697-1:2012

EN 12697-1:2012 (E) 7 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 polishing prEN 12697-50, Bituminous mixtures — Test methods for hot mix asphalt — Part 50: Scuffing resistance of surface course1)

The applicability of this European Standard is described in the product standards for bituminous mixtures. WARNING — The method described in this European Standard may require the use of dichloromethane (methylene chloride), 1,1,1-trichloroethane, benzene, trichloroethylene, xylene, toluene, perchloroethylene (tetracloroethylene) or other solvents capable of dissolving bitumen. These solvents are hazardous to health and are subject to occupational exposure limits as detailed in relevant legislation and regulations. Exposure levels are related to both handling procedures and ventilation provision and it is emphasised that adequate training should be given to staff employed in the usage of these substances. 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. SIST EN 12697-1:2012

EN 12697-1:2012 (E) 8 Introduction This European Standard describes a unified approach to the examination of bituminous mixtures that allows some divergence in the detail of procedures followed by individual laboratories. In Clause 5 of this European Standard, a description is given of the basic operations that together form the test method for the proper determination of the binder content of bituminous mixtures. Guidance on the test method is given in Annex A and Figure A.1, while the use of alternative items of equipment that are equally suitable for carrying out particular parts of the test method are described in Annex B. Although the apparatus specified for the separation of mineral filler from the binder solution obtained after extraction is of a suitably efficient level not to affect the precision of the test described in Clause 8, a method for determining the amount of residual mineral matter in the extract is given in Annex C for use in those particular cases where some doubt may exist. Methods and equipment other than those described in Annex B and Annex C, including automated equipment, are permissible provided that they have been demonstrated to provide the same results as one of the methods in Annex B or Annex C within the limits of the precision given in this document. Guidance on determination of soluble binder content of mixtures with polymer-modified binders is given in Annex D. SIST EN 12697-1:2012

EN 12697-1:2012 (E) 9 1 Scope This document describes test methods for the determination of the soluble binder content of samples of bituminous mixtures. The test methods described are suitable for quality control purposes during the production of plant mix and for checking compliance with a product specification. For the analysis of mixtures containing modified binders, the guidance of Annex D should be followed. 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 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 12697-14, Bituminous mixtures — Test methods for hot mix asphalt — Part 14: Water content EN 12697-28:2000, Bituminous mixtures — Test methods for hot mix asphalt — Part 28: Preparation of samples for determining binder content, water content and grading EN 933-1, Tests for geometrical properties of aggregates — Part 1: Determination of particle size distribution — Sieving method ISO 3310-1, Test sieves — Technical requirements and testing — Part 1: Test sieves of metal wire cloth ISO 3310-2, Test sieves — Technical requirements and testing — Part 2: Test sieves of perforated metal plate 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 soluble binder content percentage by mass of extractable binder in an anhydrous sample, determined by extracting the binder from the sample Note 1 to entry: Extraction may be followed by binder recovery. 3.2 insoluble binder content percentage by mass of binder that adheres to the aggregate particles after extraction 3.3 precision closeness of agreement between independent test results obtained under stipulated conditions Note 1 to entry: Precision depends only on the distribution of random errors and does not relate to the true value or the specified value. SIST EN 12697-1:2012

EN 12697-1:2012 (E) 10 Note 2 to entry: The measure of precision is usually expressed in terms of imprecision and computed as a standard deviation of the test results. Less precision is indicated by a larger standard deviation. Note 3 to entry: “Independent test results” means results obtained in a manner not influenced by any previous result on the same or similar test sample. Quantitative measures of precision depend critically on the stipulated conditions. Repeatability and reproducibility conditions are particular sets of extreme conditions. 3.4 repeatability precision under repeatability conditions 3.5 repeatability conditions conditions in which independent test results are obtained with the same method on identical test items in the same laboratory by the same operator using the same equipment within short intervals of time 3.6 repeatability limit maximum absolute difference between two test results obtained under repeatability conditions that may be expected

with a probability of 95 % Note 1 to entry: The symbol used for repeatability limit is r. 3.7 reproducibility precision under reproducibility conditions 3.8 reproducibility conditions conditions in which test results are obtained with the same method on identical test items in different laboratories with different operators using different equipment 3.9 reproducibility limit maximum absolute difference between two test results obtained under re…bility conditions that may be expected

with a probability of 95 % Note 1 to entry: The symbol used for reproducibility limit is R. 3.10 single test result value obtained by applying the standard test method once, fully, on a single specimen

Note 1 to entry: The single test result may also be the mean of two or more observations or the result of a calculation from a set of observations as specified by the standard test method. 4 Preparatory treatment of laboratory samples of bituminous mixtures Prepare laboratory samples in accordance with EN 12697-28 to obtain suitable test portions. 5 Determination of binder content 5.1 General principles of test

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