Licensed copy: The University of Hong Kong, The University of Hong Kong, Version correct as of 30/10/2010 06:09, (c) BSI BS EN 13358:2010 BS 2000-525:2010 BSI Standards Publication Bitumen and bituminous binders — Determination of the distillation characteristics of cut-back and fluxed bituminous binders made with mineral fluxes NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW raising standards worldwide™ Licensed copy: The University of Hong Kong, The University of Hong Kong, Version correct as of 30/10/2010 06:09, (c) BSI BS EN 13358:2010 BRITISH STANDARD National foreword This British Standard is the UK implementation of EN 13358:2010 It supersedes BS EN 13358:2004 which is withdrawn The UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroleum Testing and Terminology A list of organizations represented on this committee can be obtained on request to its secretary Energy Institute, under the brand of IP, publishes and sells all Parts of BS 2000, and all BS EN petroleum test methods that would be Part of BS 2000, both in its annual publication “Standard methods for analysis and testing of petroleum and related products and British Standard 2000 Parts” and individually Further information is available from: Energy Institute, 61 New Cavendish Street, London W1G 7AR Tel: 020 7467 7100 Fax: 020 7255 1472 This publication does not purport to include all the necessary provisions of a contract Users are responsible for its correct application © BSI 2010 ISBN 978 580 69119 ICS 75.140; 91.100.50 Compliance with a British Standard cannot confer immunity from legal obligations This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 October 2010 Amendments issued since publication Date Text affected Licensed copy: The University of Hong Kong, The University of Hong Kong, Version correct as of 30/10/2010 06:09, (c) BSI BS EN 13358:2010 EN 13358 EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM June 2010 ICS 75.140; 91.100.50 Supersedes EN 13358:2004 English Version Bitumen and bituminous binders - Determination of the distillation characteristics of cut-back and fluxed bituminous binders made with mineral fluxes Bitumes et liants bitumineux - Détermination des caractéristiques de distillation des liants bitumineux fluidifiés et fluxés avec des fluxants d'origine minérale Bitumen und bitumenhaltige Bindemittel - Bestimmung des Destillationsverlaufes von mit Mineralölfluxmitteln verschnittenen oder gefluxten bitumenhaltigen Bindemitteln This European Standard was approved by CEN on 20 May 2010 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 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 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 and United Kingdom EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels © 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members Ref No EN 13358:2010: E Licensed copy: The University of Hong Kong, The University of Hong Kong, Version correct as of 30/10/2010 06:09, (c) BSI BS EN 13358:2010 EN 13358:2010 (E) Contents Page Foreword 1 Scope 2 Normative references 3 Terms and definitions 4 4 Principle 5 Apparatus 6 6.1 6.2 6.3 6.4 Procedure General Preparation of test samples 5 Preparation of apparatus Procedure 7 7.1 7.2 7.3 Calculations Bituminous residue after distillation 8 Total distillate Distillate fractions 8 8 Expression of results 9 9.1 9.2 Precision Repeatability 9 Reproducibility 10 Test report Annex A (normative) Specifications of thermometer 13 Licensed copy: The University of Hong Kong, The University of Hong Kong, Version correct as of 30/10/2010 06:09, (c) BSI BS EN 13358:2010 EN 13358:2010 (E) Foreword This document (EN 13358:2010) has been prepared by Technical Committee CEN/TC 336 “Bituminous binders”, the secretariat of which is held by AFNOR/BNPé 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 2010, and conflicting national standards shall be withdrawn at the latest by December 2010 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 13358:2004 This European Standard is based on ASTM D402-97 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 and the United Kingdom Licensed copy: The University of Hong Kong, The University of Hong Kong, Version correct as of 30/10/2010 06:09, (c) BSI BS EN 13358:2010 EN 13358:2010 (E) Scope This European Standard specifies a method for the determination of the distillation characteristics of cut-back and fluxed bituminous binders made with mineral fluxes WARNING — The use of this European Standard can involve hazardous materials, operations and equipment This European Standard does not purport to address all of the safety problems associated with its use It is the responsibility of the user of this European Standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use Normative references The following referenced documents are indispensable for the application of this document For dated references, only the edition cited applies For undated references, the latest edition of the referenced document (including any amendments) applies EN 58, Bitumen and bituminous binders — Sampling bituminous binders EN 12594, Bitumen and bituminous binders — Preparation of test samples Terms and definitions For the purposes of this document, the following terms and definitions apply 3.1 distillation process of evaporation and condensation of a liquid 3.2 mineral flux flux which may be of carbochemical or petrochemical origin or a mixture of both Principle Petroleum cut-back and fluxed bituminous binders are distilled at a controlled rate until the temperature of the liquid reaches 360 °C The volumes of distillate and residue obtained over specified temperature ranges are measured The residue from the distillation and also the distillate may be tested as required Apparatus Usual laboratory apparatus and glassware, together with the following 5.1 Distillation flask, 500 ml and with side-arm, of dimensions given in Figure 5.2 Condenser, standard, glass-jacketed, of nominal jacket length from 200 mm to 300 mm and overall tube length of (450 ± 10) mm (see Figure 3) 5.3 Adaptor, made with glass of approximately mm thickness, with reinforced top, having an angle of approximately 105° The inside diameter shall be (18 ± 2) mm at the wide end and not less than mm at the narrow end The lower surface of the adaptor shall be on a smooth descending curve from the wider end to the narrower The inside line of the outlet end shall be vertical, and the outlet shall be cut or ground (not fire-polished) at an angle of (45± 5)° NOTE In the equipment described in the above paragraphs and in Figure and Figure 3, cork stoppers are used, however, equipment with ground glassd joints may also be used Licensed copy: The University of Hong Kong, The University of Hong Kong, Version correct as of 30/10/2010 06:09, (c) BSI BS EN 13358:2010 EN 13358:2010 (E) 5.4 Shield and shield support 5.4.1 Shield, of steel, lined with mm of suitable thermal insulation material and fitted with transparent mica windows of the form and dimensions shown in Figure 2, which is used to protect the flask from air currents and to reduce radiation 5.4.2 Shield cover (top), consisting of two parts of fire resistant millboard of mm minimum thickness 5.5 Support for shield and flak, two sheets 150 mm × 150 mm of a mesh of approximately mm wire gauze on a tripod or ring 5.6 Heat source, adjustable Tirrill1) gas burner or equivalent 5.7 Chimney for protection of the gas burner flame, as given in Figure 5.8 Receiver, standard 100 ml graduated cylinder of dimensions as given in Figure 5.9 Thermometer, conforming to the requirements described in Annex A Other temperature measuring devices may be used instead of mercury stem thermometers However, the mercury stem thermometer is the reference device Therefore any alternative device employed shall be calibrated so as to provide the same readings as would be provided by the mercury stem thermometer, recognising and allowing for the fact of changed thermal response times compared with the mercury thermometer For this test method, in which increasing temperatures are read during the test procedure, documented corrections shall be determined in advance and applied to the observed readings 5.10 Residue container, of approximately 250 ml capacity A seamless metal container, with a slip-on cover of (75 ± 5) mm diameter and (55 ± 5) mm height, or similar, is suitable 5.11 Balance with a reading accuracy of at least 0,1 g Procedure 6.1 General The material under test shall be sampled in accordance with EN 58 6.2 Preparation of test samples 6.2.1 Samples shall be prepared in accordance with the provisions detailed in EN 12594, especially those regarding cut-back and fluxed bituminous binders In particular, stir the sample thoroughly, warming if necessary, to ensure homogeneity before removal of a representative portion for analysis 6.2.2 If sufficient water is present to cause foaming or bumping, dehydrate a sample of not less than 250 ml by heating in a distillation flask sufficiently large to prevent foaming over into the side-arm When foaming has ceased, stop the heating If any light oil has distilled over, separate and pour back into the flask when the contents have cooled down sufficiently to prevent loss of volatile oil Mix the contents of the flask thoroughly before removal for analysis 6.3 Preparation of apparatus 6.3.1 Calculate the mass of 200 ml of the sample from the density of the material at 15 °C Weigh this amount with an accuracy of ± 0,5 g into the 500 ml distillation flask (5.1) 1) Tirrill is an example of a suitable product available commercially This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of this product Licensed copy: The University of Hong Kong, The University of Hong Kong, Version correct as of 30/10/2010 06:09, (c) BSI BS EN 13358:2010 EN 13358:2010 (E) 6.3.2 Place the flask in the shield (5.4) supported by two sheets of gauze (5.5) on a tripod or ring Connect the condenser tube (5.2) to the side-arm of the flask with a cork stopper or equivalent, keeping the centre of its neck vertical Adjust the adapter (5.3) over the end of the condenser tube so that the distance from the neck of the distillation flask to the adapter outlet is (650 ± 50) mm 6.3.3 Insert the thermometer through a tight-fitting cork in the neck of the distillation flask so that the thermometer bulb rests on the bottom of the flask Raise the thermometer (6,5 ± 1,0) mm from the bottom of the flask using the scale divisions on the thermometer to estimate 6,5 mm above the top of the cork 6.3.4 Protect the burner by a suitable shield or chimney Place the receiver (5.8) so that the adapter extends into it by at least 25 mm but not to below the 100 ml mark Cover the neck of the receiver with a piece of suitably weighted blotting paper, or similar material, cut to fit the adapter snugly 6.3.5 Ensure that the flask, condenser, adapter and receiver are clean and dry Place the residue container and its cover in an area free from drafts 6.3.6 Pass cold water through the condenser jacket by reflux Use warm water if necessary to prevent the formation of solid condensate in the condenser tube 6.4 Procedure 6.4.1 If the barometric pressure, in Pascals2), at the time of the test is known, correct the temperature according to Table Do not correct for the emergent stem of the thermometer If the barometric pressure is not known, and the elevation of the laboratory is more than 150 m above sea level, correct the temperature according to Table NOTE 2) Only one correction is used each time Standard pressure is 013 hPa Licensed copy: The University of Hong Kong, The University of Hong Kong, Version correct as of 30/10/2010 06:09, (c) BSI BS EN 13358:2010 EN 13358:2010 (E) Table — Factors for calculating temperature corrections 160 Correctiona per 13,33 hPa difference in pressure (°C) 0,514 175 0,531 190 0,549 225 0,591 250 0,620 260 0,632 275 0,650 300 0,680 316 0,698 325 0,709 360 0,751 Nominal temperature (°C) a To be subtracted when the barometric pressure is below 013 hPa; to be added when the barometric pressure is above 013 hPa NOTE For the temperature correction, it is convenient to take into account that experimental temperatures can only be read at the nearest °C Table — Corrected fractionation temperature for various altitudes Fractionation temperature for various altitudes (°C) Elevation above sea level (m) -305 192 227 263 318 362 -152 191 226 261 317 361 190 225 260 316 360 152 189 224 259 315 359 305 189 224 258 314 358 457 188 223 258 313 357 610 187 222 257 312 356 762 186 221 256 312 355 914 186 220 255 311 354 1067 185 220 254 310 353 1219 184 219 254 309 352 1372 184 218 253 308 351 1524 183 218 252 307 350 1676 182 217 251 306 349 1829 182 216 250 305 349 1981 181 215 250 305 348 2134 180 214 249 304 347 2286 180 214 248 303 346 2438 179 213 248 302 345 Licensed copy: The University of Hong Kong, The University of Hong Kong, Version correct as of 30/10/2010 06:09, (c) BSI BS EN 13358:2010 EN 13358:2010 (E) 6.4.2 Apply heat such that the first drop of distillate falls from the end of the distillation flask side-arm within to 15 Conduct the distillation so as to maintain the following drop rates, at the adapter tip (all temperatures refer to corrected temperatures): up to 260 °C, 50 drops per minute to 70 drops per minute; from 260 °C to 316 °C, 20 drops per minute to 70 drops per minute; from 316 °C to 360 °C, complete the distillation within 10 6.4.3 Record the volumes of distillate to the nearest 0,5 ml in the receiver at the corrected temperatures If the volume of distillate recovered is critical, use receivers graduated in 0,1 ml divisions and immersed in a transparent bath maintained at (15 ± 2) °C 6.4.4 When the temperature reaches the corrected temperature of 360 °C, extinguish the flame and remove the flask and thermometer With the flask in a pouring position, remove the thermometer and then pour the contents into the residue container The total time from extinguishing the flame to pouring should be limited as far as possible, but shall not exceed 15 s When pouring, ensure that the side-arm is sufficiently horizontal to prevent condensate in the side-arm from falling back into the residue 6.4.5 Allow the condenser to drain into the receiver and record the total volume of distillate collected as total distillate to 360 °C 6.4.6 When the residue has cooled such that fuming has just ceased, stir the residue thoroughly and pour it into the receptacles for testing of properties such as penetration, viscosity or softening point Proceed as required by the appropriate standard test method from immediately following the pouring stage Calculations 7.1 Bituminous residue after distillation Calculate the residue, VR, as a volume percentage, using the following equation: VR = (200 − Dt )×100 200 (1) where Dt is the recovered volume to 360 °C, i.e the total distillate, in ml 7.2 Total distillate Calculate the total distillate D%, as a volume percentage, using the following equation: D% = Dt × 100 200 (2) 7.3 Distillate fractions 7.3.1 Calculate the volume percentage, with respect to the volume of the original sample, of each distillate fraction, Vp, as follows: Vp = Vf × 100 200 where Vf is the observed volume of the considered distillate fraction, in ml (3) Licensed copy: The University of Hong Kong, The University of Hong Kong, Version correct as of 30/10/2010 06:09, (c) BSI BS EN 13358:2010 EN 13358:2010 (E) 7.3.2 Calculate the volume percentage, with respect to the total distillate volume (D t) of each distillate fraction, Vpt , as follows: Vpt = Vf × 100 Dt (4) where Vf is the observed volume of the considered distillate fraction, in ml; Dt is the recovered volume to 360 °C, i.e the total distillate, in ml Expression of results Express the results calculated according to Clause in volume percentage rounded to the nearest 0,1 Precision 9.1 Repeatability The difference between two test results obtained by the same operator with the same apparatus under constant operating conditions on identical test material would, in the long run, in the normal and correct operation of the test method, exceed the value given in Table only in one case in twenty 9.2 Reproducibility The difference between two single and independent test results obtained by different operators working in different laboratories on identical test material would, in the long run, in the normal and correct operation of the test method, exceed the value given in Table only in one case in twenty Table — Precision Repeatability r volume percentage Reproducibility R volume percentage Up to 175 °C 3,5 Above 175 °C 2,0 Residue 2,0 Distillation fraction 10 Test report The test report shall contain at least the following information: a) type and complete identification of the sample under test; b) reference to this European Standard; c) the result of the test (see Clause 8), giving the precision of the distillate volume read in the receiver (0,5 ml or 0,1 ml as chosen by the operator); d) any deviation, by agreement or otherwise, from the procedure specified; e) date of the test Licensed copy: The University of Hong Kong, The University of Hong Kong, Version correct as of 30/10/2010 06:09, (c) BSI BS EN 13358:2010 EN 13358:2010 (E) Dimensions in millimetres Figure — Distillation flask Dimensions in millimetres Key Flange "Heat resistant" cover in two parts Two mica windows (45 ± 2) mm square at right angles to end slot "Heat resistant" lining 3,0 mm to 3,5 mm thick Figure — Shield 10 Licensed copy: The University of Hong Kong, The University of Hong Kong, Version correct as of 30/10/2010 06:09, (c) BSI BS EN 13358:2010 EN 13358:2010 (E) Dimensions in millimetres Key Mica window Two sheets wire gaze with mesh opening of approximately mm Chimney 11 Water jacketed condenser 200 mm to 300 mm 12 Adapter Cork stopper Shield Flask Burner Stand 10 Tight cork joint 13 Receiver 14 Blotting paper 15 Crow Receiver Thermometer Figure — Distillation apparatus 11 Licensed copy: The University of Hong Kong, The University of Hong Kong, Version correct as of 30/10/2010 06:09, (c) BSI BS EN 13358:2010 EN 13358:2010 (E) Dimensions in millimetres Figure — Crow receivers of capacities 25 ml, 50 ml and 100 ml 12 Licensed copy: The University of Hong Kong, The University of Hong Kong, Version correct as of 30/10/2010 06:09, (c) BSI BS EN 13358:2010 EN 13358:2010 (E) Annex A (normative) Specifications of thermometer Temperature range °C -2 to +400 Subdivision °C Long lines at each °C Numbers at each: °C 10 Maximum line width mm 0,15 Maximal scale error °C to 300 1,5 above 300 Scale marks Immersion Total Expansion chamber : permit heating to Required Total length mm 380 - 390 Stem outside diameter mm 6,0 - 8,0 Bulb length mm 10 to 15 Bulb outside diameter mm 5,0 and not greater than the stem Distance between bottom of bulb to line at °C mm 30 - 40 Length of scale range mm 290 - 330 Scale location NOTE The thermometer IP 6C / ASTM 8C has been found suitable 13 Licensed copy: The University of 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