Bituminous mixtures - Test methods - Part 3: Bitumen recovery: Rotary evaporator

This document describes a test method for the recovery of soluble bitumen from bituminous mixtures used in road, airfield or similar pavements in a form suitable for further testing. The test can be undertaken on either loose or compacted asphalt materials. The procedure is suitable for the recovery of paving grade bitumens, for which materials this European Standard is the reference method. The fractionating column procedure (see EN 12697-4) is the reference method for mixtures containing volatile matter such as cut-back bitumen.
For recovery of polymer modified bitumens, the rotary evaporator procedure is recommended.

Asphalt - Prüfverfahren - Teil 3: Rückgewinnung des Bindemittels: Rotationsverdampfer

Dieses Dokument beschreibt ein Prüfverfahren, mit dem aus Asphalt, der zum Bau von Straßen, Flugplätzen und ähnlichen Verkehrsflächen ver¬wendet wurde, lösliches Bindemittel in einer Form zurückgewonnen wird, die für weitere Prüfungen geeignet ist. Die Prüfung kann entweder an losem oder an verdichtetem Asphalt durchgeführt werden. Dieses Verfahren eignet sich nur zur Rückgewinnung von Straßenbaubitumen, für die das in dieser Europäischen Norm angegebene Verfahren das Referenzverfahren ist. Das Verfahren mit der Fraktionierkolonne (siehe EN 12697 4) ist das Referenzverfahren für Mischgüter, die flüchtige Bestandteile enthalten, wie z. B. verschnittenes Bitumen.
ANMERKUNG   Für die Rückgewinnung polymermodifizierten Bitumens wird der Rotationsverdampfer empfohlen.

Mélanges Bitumineux - Méthodes d'essai - Partie 3: Extraction des bitumes à l'évaporateur rotatif

Le présent document décrit une méthode d'essai permettant de récupérer du bitume soluble de mélanges bitumineux utilisés sur les routes, les terrains d'aviation ou chaussées similaires sous une forme se prêtant à des essais complémentaires. L'essai peut être réalisé sur des matériaux enrobés foisonnés ou compactés. La procédure convient uniquement à la récupération de bitumes routiers de grades usuels, pour lesquels cette Norme européenne est une méthode de référence. La méthode à la colonne à distiller (voir EN 12697-4) est la méthode de référence pour les mélanges qui contiennent des produits volatils tels que des fluxants.
Pour la récupération des bitumes modifiés par des polymères, la méthode à l’évaporateur rotatif est recommandée.

Bitumenske zmesi - Preskusne metode - 3. del: Ugotavljanje deleža veziva: rotacijski uparjalnik

Ta dokument opisuje preskusno metodo za ugotavljanje deleža topnega bitumna v bitumenskih zmeseh za ceste, vozišča letališč ali podobna vozišča v obliki, ki je primerna za nadaljnje preskušanje. Preskus se lahko opravi na razrahljanih ali zgoščenih asfaltnih materialih. Postopek je primeren za ugotavljanje deleža cestnogradbenih bitumnov, pri čemer je ta evropski standard referenčna metoda za njihov material. Kolonska frakcionirana destilacija (glej EN 12697-4) je referenčna metoda za zmesi, ki vsebujejo hlapne snovi, kot je rezani bitumen.
Za ugotavljanje deleža bitumnov, modificiranih s polimeri, se priporoča postopek z rotacijskim uparjalnikom.

General Information

Status
Published
Publication Date
10-Jan-2019
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
04-Jan-2019
Due Date
11-Mar-2019
Completion Date
11-Jan-2019

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Bitumenske zmesi - Preskusne metode - 3. del: Ugotavljanje deleža veziva: rotacijski uparjalnikAsphalt - Prüfverfahren - Teil 3: Rückgewinnung des Bindemittels: RotationsverdampferMélanges Bitumineux - Méthodes d'essai - Partie 3: Extraction des bitumes à l'évaporateur rotatifBituminous mixtures - Test methods - Part 3: Bitumen recovery: Rotary evaporator93.080.20Materiali za gradnjo cestRoad construction materialsICS:Ta slovenski standard je istoveten z:EN 12697-3:2013+A1:2018SIST EN 12697-3:2013+A1:2019en,fr,de01-februar-2019SIST EN 12697-3:2013+A1:2019SLOVENSKI
STANDARDSIST EN 12697-3:20131DGRPHãþD



SIST EN 12697-3:2013+A1:2019



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 12697-3:2013+A1
December
t r s z ICS
{ uä r z rä t r Supersedes EN
s t x { yæ uã t r s uEnglish Version
Bituminous mixtures æ Test methods æ Part
uã Bitumen recoveryã Rotary evaporator Mélanges Bitumineux æ Méthodes d 5essai æ Partie
uã Extraction des bitumes à l 5évaporateur rotatif
Asphalt æ Prüfverfahren æ Teil
uã Rückgewinnung des Bindemittelsã Rotationsverdampfer This European Standard was approved by CEN on
t z March
t r s u and includes Amendment
s approved by CEN on
{ November
t r s zä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Rue de la Science 23,
B-1040 Brussels
9
t r s z CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s t x { yæ uã t r s u ªA sã t r s z ESIST EN 12697-3:2013+A1:2019



EN 12697-3:2013+A1:2018 (E) 2 Contents Page Foreword . 3 1 Scope . 5 2 Normative references . 5 3 Terms and definitions . 5 4 Principle . 5 5 Apparatus . 6 5.1 Apparatus for the extraction of the soluble bitumen . 6 5.2 Apparatus for the clarification of the bitumen solution . 6 5.3 Distillation apparatus . 7 6 Solvent and other materials . 7 7 Procedure. 8 7.1 Extraction of the bitumen and removal of insoluble matter . 8 7.2 Assembling the apparatus . 8 7.3 Distillation procedure . 9 8 Preparation of the bitumen for testing . 11 9 Test report . 11 10 Precision . 11 Bibliography . 13
SIST EN 12697-3:2013+A1:2019



EN 12697-3:2013+A1:2018 (E) 3 Foreword This document (EN 12697-3:2013+A1:2018) has been prepared by Technical Committee CEN/TC 227 “Road materials”, the secretariat of which is held by BSI. 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 2019, and conflicting national standards shall be withdrawn at the latest by June 2019. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. This document includes Amendment 1 approved by CEN on 9 November 2018. The start and finish of text introduced or altered by amendment is indicated in the text by tags ! ". This document supersedes !EN 12697-3:2013". !The significant changes made in EN 12697-3:2013+A1:2018 compared to EN 12697-3:2013 are: — [Title] The series title no longer makes the method exclusively for hot mix asphalt; — [Foreword] The list of standards in the Foreword was deleted and the list of significant changes was adapted; — [5.1] NOTE: Paragraph deleted, stating that the hardening is usually approximately equivalent to the softening resulting from any solvent residue; — [5.3.6] The temperature range 100 °C to 200 °C for thermometer is replaced by range of temperatures specified in Table 1 according to the solvent used; — [7.1.2] Clarification that the 0,063 mm sieve is used for removal of any insoluble material; — [7.3] The whole sub-clause has been replaced, with the following significant changes: — the order of the procedure in the previous version (7.3.8 to 7.3.25) has been altered for clarity and is now described in 7.3.8 to 7.3.18; — NOTES introduced in 7.3.9 and 7.3.11 with advise to not exceed 120 °C for T2 for bitumen’s, designated and specified by kinematic viscosity at 60 °C regardless of solvent used; — [Clause 9] Reference to (7.1.15) amended to (7.3.13) followed by the changes in 7.3. — editorial updates." !A list of all parts in the EN 12697 series can be found on the CEN website." WARNING — The method described in this European Standard may require the use of dichloromethane (methylene chloride), !1,1,1-Trichlorethane", benzene, trichlorethylene, xylene, toluene, tetrachloroethylene or other solvent capable of dissolving bitumen. These solvents are hazardous to health and are subject to occupational exposure limits as detailed in relevant legislation and regulations. SIST EN 12697-3:2013+A1:2019



EN 12697-3:2013+A1:2018 (E) 4 Exposure levels are related to both handling procedures and ventilation provision and it is important that adequate training be given to staff employed in the usage of these substances. According to the CEN-CENELEC Internal Regulations, the national standards organisations 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, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.
SIST EN 12697-3:2013+A1:2019



EN 12697-3:2013+A1:2018 (E) 5 1 Scope This document describes a test method for the recovery of soluble bitumen from bituminous mixtures used in road, airfield or similar pavements in a form suitable for further testing. The test can be undertaken on either loose or compacted asphalt materials. The procedure is suitable for the recovery of paving grade bitumens, for which materials this European Standard is the reference method. The fractionating column procedure (see EN 12697-4) is the reference method for mixtures containing volatile matter such as cut-back bitumen. For recovery of polymer modified bitumens, the rotary evaporator procedure is recommended. 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 12594, Bitumen and bituminous binders — Preparation of test samples EN 12697-1:2012, Bituminous mixtures — Test methods for hot mix asphalt — Part 1: Soluble binder content EN 12697-38, Bituminous mixtures — Test methods for hot mix asphalt — Part 38: Common equipment and calibration 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 12697-1:2012 and the following apply. 3.1 soluble binder content proportion of extractable binder in an anhydrous sample determined by extracting the binder from the sample Note 1 to entry: Extraction can be followed by binder recovery. Note 2 to entry: The soluble binder content is expressed in percent by mass. 3.2 insoluble binder content proportion of binder that adheres to the aggregate after extraction Note 1 to entry: The insoluble binder content is expressed in percent by mass. 4 Principle The bitumen is separated from the sample by dissolving in dichloromethane (or other suitable solvent). After removal of undissolved solids from the bitumen solution, the bitumen is recovered from it by vacuum distillation using a rotary evaporator. The bitumen is in solution for less than 24 h. SIST EN 12697-3:2013+A1:2019



EN 12697-3:2013+A1:2018 (E) 6 5 Apparatus 5.1 Apparatus for the extraction of the soluble bitumen A suitable container with stopper in which the sample and solvent can be agitated together, an asphalt analyser or other apparatus for the extraction of soluble bitumen defined in EN 12697-1. !NOTE The use of the hot extraction methods in EN 12697-1 may harden the binder and hence affect the results from subsequent tests." 5.2 Apparatus for the clarification of the bitumen solution For clarification of the bitumen solution, a sample-tube centrifuge, a continuous centrifuge or a filtration system may be used. Centrifuges are suitable for separation of solids from any bitumen solutions and are the recommended apparatus for use with this method. The filtration apparatus may not be suitable for the separation of solids from all types of bituminous solutions but it has been included in this method because of the general availability of this equipment in asphalt testing laboratories. If difficulties are experienced using a pressure filter the centrifuge technique should be used. NOTE If an asphalt analyser is used for the extraction of soluble bitumen, the use of a centrifuge is not required. 5.2.1 Sample tube centrifuge, capable of developing an acceleration of at least 15 000 m/s2 in accordance with the formula: a = 1,097 × n2 × r × 105 (1) where a is the acceleration, expressed in metres per second squared (m/s2); n is the number of revolutions, expressed as revolution per minute (r/min); r is the radius to the bottom of the tubes (internal) when rotating, expressed in millimetres (mm). The centrifuge tubes shall be fitted with effective closures. The speed of rotation shall be verified regularly in accordance with EN 12697-38 to ensure that the centrifuge maintains its performance at all times. The centrifuge shall be maintained in accordance with this document. NOTE A typical centrifuge of this type, suitable for this method, carries four or six tubes of 200 ml or 500 ml capacity rotating at 3 000 r/min at a radius (as defined above) of 250 mm. 5.2.2 Continuous laboratory centrifuge, that takes a continuous feed of material, giving a continuous discharge of solution and capable of achieving an acceleration of 25 000 m/s2. 5.2.3 A pressure filter, of appropriate size. NOTE A pressure filter taking a paper of 270 mm diameter is suitable. 5.2.4 An air pump, for supplying oil-free air at about 200 kPa. 5.2.5 A supply of filter papers with a minimum retention size of 11 µm, to fit the pressure filter. SIST EN 12697-3:2013+A1:2019



EN 12697-3:2013+A1:2018 (E) 7 5.3 Distillation apparatus
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