Bsi bs en 12697 11 2012

NORME EUROPÉENNE English Version Bituminous mixtures - Test methods for hot mix asphalt - Part 11: Determination of the affinity between aggregate and bitumen Mélanges bitumineux - Mét

BSI Standards Publication

Bituminous mixtures — Test methods for hot mix asphalt

Part 11: Determination of the affinity between aggregate and bitumen

This British Standard is the UK implementation of EN 12697-11:2012

It supersedes BS EN 12697-11:2005 which is withdrawn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 2012 Published by BSI Standards Limited 2012

ISBN 978 0 580 75914 7 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 May 2012

Amendments issued since publication

Date Text affected

NORME EUROPÉENNE

English Version

Bituminous mixtures - Test methods for hot mix asphalt - Part 11: Determination of the affinity between aggregate and

bitumen

Mélanges bitumineux - Méthodes d'essai pour mélange

hydrocarboné à chaud - Partie 11: Détermination de

l'affinité granulat-bitume

Asphalt - Prüfverfahren für Heißasphalt - Teil 11: Bestimmung der Affinität von Gesteinskörnungen und

Bitumen

This European Standard was approved by CEN on 9 March 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

C O M I T É E U R O P É E N D E N O R M A L I S A T I O N

E U R O P Ä I S C H E S K O M I T E E FÜ R N O R M U N G

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 12697-11:2012: E

Contents

Foreword 3



1 Scope .7



2 Normative references .7



3 Terms and definitions 7



4 Principle .8



5 Rolling bottle method 8



5.1 Equipment .8



5.2 Preparation of test specimens 11



5.2.1 Aggregate 11



5.2.2 Bitumen 12



5.2.3 Mixing aggregate and bitumen 12



5.3 Conditioning 13



5.4 Procedure 13



5.5 Calculation and expression of results 15



5.6 Report 15



5.7 Precision 16



6 Static method 16



6.1 Equipment 16



6.2 Solvent and other materials 17



6.3 Preparation of test specimens 17



6.3.1 Aggregate 17



6.3.2 Bitumen 17



6.4 Procedure 17



6.5 Calculation and expression of results 18



6.6 Report 18



6.7 Precision 18



7 Boiling water stripping method 18



7.1 General 18



7.2 Equipment and materials 19



7.3 Sample preparation 20



7.3.1 Aggregate 20



7.3.2 Bitumen 21



7.3.3 Mixing aggregate and bitumen 21



7.4 Conditioning 21



7.5 Test procedure 21



7.5.1 Establishing the acid/base equivalence factor 21



7.5.2 Establishing the calibration curve 22



7.5.3 Stripping test 23



7.6 Calculation and expression of results 24



7.6.1 Determination of the calibration curve 24



7.6.2 Calculation of the degree of bitumen coverage 25



7.7 Test report 26



7.8 Precision 26



Annex A (informative) Guidance for estimation of the degree of bitumen coverage 27



Bibliography 28



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 12697-11:2005

List of main changes since this new edition:

• Most clauses, subclauses, etc in the existing standard renumbered and headlines for methods A (rolling bottle), B (static immersion) and C (Boiling water stripping method) deleted (which may be confusing to users of previous version of standard!);

• 5.1.12: Requirement to horizontally positioning of rolling machine added;

• 5.2.2.1: Reference to EN 58 added for sampling;

• 6.1.1: “Shallow trays” changed to “Flat bottomed container”;

• 6.3.1 and 6.3.2: Original text for preparation of aggregate and bitumen changed to reference to similar clauses in the rolling bottle method;

• 6.4.1: Now allowing use of 8-11,2 mm fraction alternatively, and definition of mixing temperature changed from 130 °C ± 5 °C to 15°C less than the mixing temperature defined in EN 12697-35;

• 6.6: In report, new list entry b) (sample identification number and date and time of testing, is added;

• 7.2.1: Requirements for test sieves changed to reference to 5.2.1 (previously specified sieves 7 and

14 mm deleted);

• 7.5.1.1., 7.5.1.2, 7.6.1.1, and 7.6.2.1: the symbol “r” previously used for acid/base equivalent factor is

changed to “feq” to avoid misunderstanding as “r” is also used for repeatability (change introduced with the latest comments);

• 7.3.3.4: Use of (8-11,2) mm aggregates added;

• Informative Annex A added

This European Standard 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 method for hot mix asphalt — Part 2: Determination of particle size distribution

— EN 12697-3, Bituminous mixtures — Test methods for hot mix asphalt — Part 3: Binder recovery: Rotary evaporator

— EN 12697-4, Bituminous mixtures — Test methods for hot mix asphalt — Part 4: Bitumen recovery:

— 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 aggregates 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

— 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 a 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

— FprEN 12697-45, Bituminous mixtures  Test methods for hot mix asphalt  Part 45: Saturation Ageing Tensile Stiffness (SATS) conditioning test

— FprEN 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 12697-49, Bituminous mixtures  Test methods for hot mix asphalt  Part 49: Determination of friction after polishing

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

In the rolling bottle method, the affinity is expressed by visual registration of the degree of bitumen coverage

on uncompacted bitumen-coated mineral aggregate particles after influence of mechanical stirring action in the presence of water

NOTE 1 The rolling bottle test is a simple but subjective test and suitable for routine testing It is not appropriate for aggregates that are highly abrasive

In the static test method, the affinity is expressed by visual registration of the degree of bitumen coverage on uncompacted bitumen-coated mineral aggregate particles after storage in water

NOTE 2 The static test is a simple, though subjective test that is generally less precise, but that can cope with high PSV-aggregates

In the boiling water stripping test method, the affinity is expressed by determining the degree of coverage on uncompacted bitumen-coated aggregate after immersion in boiling water under specified conditions

bitumen-NOTE 3 The boiling water stripping test is an objective test and has a high precision However, it is a more specialist test because it requires greater skill of the operatives and uses chemicals as reagent The latter point may also imply extra health and safety considerations

NOTE 4 The boiling water stripping test procedure can be used for any binder-aggregate combinations in which the mineral aggregate is calcareous, silico-calcareous or siliceous by nature

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 58, Bitumen and bituminous binders — Sampling bituminous binders

EN 1426, Bitumen and bituminous binders — Determination of needle penetration

EN 12697-2, Bituminous mixtures — Test method for hot mix asphalt — Part 2: Determination of particle size

distribution

EN 12697-35, Bituminous mixtures — Test methods for hot mix asphalt — Part 35: Laboratory mixing

3 Terms and definitions

For the purposes of this document, the following terms and definitions apply

3.2

affinity between aggregate and bitumen

degree of bitumen coverage visually determined on uncompacted bitumen coated mineral aggregate particles after influence of mechanical stirring action in the presence of water

3.3

completely coated

aggregate particle is completely coated by binder when there are no visible breaks, however small, in the film

of binder covering the particle

3.4

degree of bitumen coverage

average proportion of the surface area of the aggregate particles that are covered with bitumen, expressed as

a percentage (equal to 100 minus the percentage of stripping)

NOTE Other fractions may alternatively be used, but not smaller than the 2 mm to 4 mm fraction However, to avoid clusters, the above mentioned standard sizes should be used

For the method described in Clause 5, the bitumen coated aggregate is placed loosely distributed on a metal plate or silicone coated paper, stored at ambient temperature overnight, and then divided into three part samples for analysis Each part sample is transferred to a bottle filled with water The bottle is sealed and placed on a bottle-rolling device The bottles are rolled at ambient temperature and at a specified speed At specified time intervals the degree of bitumen coverage on the aggregate particles is visually estimated by two technicians independently (or alternatively by automated system)

For the method described in Clause 6, the bitumen coated aggregate is immersed in distilled water for 48 h and the number of particles that are no longer completely coated assessed

For the method described in Clause 7, the bitumen coated aggregate is subjected to stripping in boiling water under specified conditions, using a simple device in which no local overheating can occur By contact with a chemical reagent, the consumption of which is proportional to the uncoated surface of the aggregate, the degree of bitumen coverage is determined with reference to a calibration curve established by a well-defined procedure The reagent used is hydrochloric acid for calcareous aggregates and hydrofluoric acid for silico-calcareous or siliceous aggregates

5 Rolling bottle method

5.1 Equipment

5.1.1 Test sieves

Square openings conforming to EN 12697-2; 11,2 mm and 8 mm or 6,3 mm and 10 mm

NOTE Alternatively, square opening test sieves of 5,6 mm, 6 mm and 8 mm may be used

5.1.2 Ventilated oven, thermostatically controlled, adjustable from 100 °C to 180 °C, able to maintain the sample at (110 ± 5) °C for drying procedure and at the specified mixing temperature ± 5 °C (refer to 5.2.3.1)

5.1.3 Temperature measuring device

5.1.3.1 Temperature measuring device, capable of measuring the water temperature of 5 °C and 20 °C

with an accuracy of ± 1 °C

5.1.3.2 Temperature measuring device, capable of measuring the aggregate and bitumen temperature

at a range of 110 °C to 180 °C with an accuracy of ± 2 °C

NOTE The temperature measuring device may be a thermometer or an electronical measuring device

5.1.4 Balance

Capacity not less than 600 g, capable of determining an aggregate portion of 510 g with an accuracy of ± 2 g, and a balance capable of determining a binder test portion of 16 g to 18 g with an accuracy of ± 0,2 g (see 5.2.1.3 and 5.2.3.6)

NOTE A 'dual range' type balance may allow to weigh the aggregate and bowl with an accuracy of ± 2 g and after use of tare-function to determine the mass of binder added into the same mixing bowl with an accuracy of ± 0,2 g

5.1.5 Metal containers (tins)

Suitable size for bitumen heating and addition of adhesion agent

5.1.6 Mixing bowl

Glazed porcelain bowl or other bowl with smooth non-absorbent surface, suitable for mixing the specified test portion in accordance with 5.2

NOTE A porcelain bowl with diameter of 200 mm and internal height 50 mm may be considered suitable

5.1.7 Spatula, made of metal or other suitable, non-absorbent material for mixing of bitumen and aggregate

5.1.8 Silicone coated paper or a flat metal lid, for storage of coated aggregate particles as individual,

loose particles when cooling down after mixing

NOTE A flat metal lid with a rim height of 10 mm and diameter 300 mm may be considered suitable

5.1.9 Refrigerator, capable of maintaining a temperature of (5 ± 2) °C

5.1.10 Test bottles, made of borosilicate glass for high wear resistance

The volume capacity shall be approximately 500 ml The bottles shall have a diameter of (80 ± 10) mm and a height of (175 ± 10) mm The bottle shall have a shoulder height of (110 ± 10) mm (see Figures 1 and 2) The bottle neck shall have an opening diameter of (30 ± 5) mm, equipped with a water-tight fitting screw cap

5.1.11 Glass-rods, diameter of (6 ± 1) mm, equipped with (30 ± 10) mm long, fitting rubber tubes

The rubber tube shall be positioned on one end of the glass-rod so that the length of the rod is extended by approximately half of the tube length The length of the glass-rod shall be proportioned, so that the rod with rubber tube can be firmly fixed inside the test bottle between the bottom and the screw cap (see Figure 3)

NOTE The glass rod ensures mechanical stirring and reduces risk of coated aggregate forming lumps

5.1.12 Bottle rolling machine, capable of rolling not less than three test bottles at the same time

The rotation speed shall be adjustable, so that both a speed of 40 min-1 and 60 min-1 can be obtained with an accuracy of ± 10 % The machine shall be positioned such that the bottles rotate horizontally with a tolerance

of ± 5°

Figure 1 — Test bottle Figure 2 — Bottle rolling machine

5.1.13 Glass beakers

Volume not less than 200 ml

5.1.14 Test bowls, suitable for visual determination of degree of binder coating on the aggregate

The bowls shall be flat-bottomed and of sufficient diameter to allow for placing of a test portion of (150 ± 2) g aggregate in a single layer, and of sufficient height to allow the test portion of aggregate to be completely submerged in water

NOTE Flat-bottomed 'Petri-dishes' made of glass with approximate diameter 120 mm and height 15 mm may be considered suitable

5.1.15 Lamp to provide a suitable light source to facilitate visual determination of binder coating on

aggregate

5.1.16 Magnifying glass with low magnification, to facilitate determination of degree of binder coating on

aggregate (optional)

Dimensions in millimetres

Key

1 screw cap, bottle opening diameter (30 ± 5) mm

2 rubber tube

3 glass rod, diameter (6 ± 1) mm

4 glass test bottle

5 level A (shoulder)

Figure 3 — Test bottle with appropriate dimensions

5.2 Preparation of test specimens

5.2.1 Aggregate

5.2.1.1 Using test sieves from basic set plus set 1: Separate at least 600 g of aggregate passing the 11,2 mm test sieve and retained on the 8 mm sieve in accordance with EN 12697-2 to form a 8/11 mm fraction of the aggregate to be tested Wash the fraction on the 8 mm sieve

Using test sieves from basic set plus set 2: Separate at least 600 g of aggregate passing the 10 mm test sieve and retained on the 6,3 mm sieve in accordance with EN 12697-2 to form a 6/10 mm fraction of the aggregate

to be tested Wash the fraction on the 6,3 mm sieve

NOTE Alternatively, a smaller 5/8 mm fraction (passing the 8 mm sieve and retained on the 5,6 mm sieve, basic set +

set 1) may be used However, bitumen coated particles of the smaller 5/8 mm aggregate fraction have an increased risk of forming clusters during the rolling procedure, which may invalidate the test result Also, use of the smaller 5/8 mm fraction may complicate the visual determination of the degree of bitumen coverage on the aggregate surfaces Fractions smaller than 5/8 mm are not acceptable for the rolling bottle method Therefore, 8/11 mm or 6/10 mm aggregates are preferred

5.2.1.2 Place the aggregates in the ventilated oven set at (110 ± 5) °C and dry to a constant mass, i.e until three consecutive mass determinations with at least one minute intervals show a difference less than

1 %

NOTE It may be considered practical to let the aggregates dry overnight

5.2.1.3 Place a portion of (510 ± 2) g aggregates in a mixing bowl

5.2.2 Bitumen

5.2.2.1 Take a representative sample of the binder to be used in the plant mixtures in accordance with

EN 58 The sample shall include any modifiers and/or adhesion agents at the same proportion(s) as they are

to be used in the plant mixtures

5.2.2.2 Pour the sampled bitumen into suitable metal containers that are covered Ensure that the containers are filled

5.2.3 Mixing aggregate and bitumen

5.2.3.1 The mixing temperature shall be the reference temperature for mixtures as defined in

5.2.3.4 If a liquid adhesion agent is to be added to the bitumen, the adhesion agent shall be added to a bitumen sample of not less than 100 g heated to the mixing temperature Mix the binder and adhesion agent carefully with a spatula and proceed immediately with the aggregate/binder mixing process in accordance with 5.2.3.6

If the heat stability of the adhesion agent is to be evaluated, the mixing with aggregate should not be performed immediately after mixing binder and adhesion agent

5.2.3.5 If an adhesion improving filler is to be added to the mixture, the filler shall be added to the aggregate test portion and carefully mixed with a spatula before addition of bitumen

As the affinity is determined according to a procedure involving mechanical action, the test result may be influenced by mechanical wear, which may be different if the aggregate coating does not consist of pure binder If the effect of an adhesion improving filler (e.g cement or hydrated lime) is to be evaluated, the reference sample should also contain a filler, as binder coating on aggregate without filler is faster worn than binder coatings on aggregates mixed with filler (i.e the coating is a stiffer bitumen/filler mortar)

5.2.3.6 Using 8/11 mm aggregates, add a portion of (16,0 ± 0,2) g of bitumen into the mixing bowl with aggregates If 6/10 mm aggregates are used, add a portion of (17,0 ± 0,2) g bitumen into the mixing bowl with aggregates

NOTE The bitumen quantity specified corresponds to a bitumen content of 3,0 % (by weight of mix) for the 8/11 mm aggregate and is adjusted for 6/10 mm and 5/8 mm fractions to ensure that approximately the same binder film thickness

is obtained

The amount of bitumen to be added shall be corrected to the actual aggregate density by multiplying by the factor:

(1)

If 5/8 mm aggregates are used, add a portion of (18,0 ± 0,2) g bitumen into the mixing bowl with aggregates

5.2.3.7 Mix the aggregates and binder intensively by means of a spatula to obtain a uniform coating

Ensure that the surfaces of the aggregates are completely covered by bitumen Discard the mixed material if

total (100 %) bitumen coverage is not obtained Any thin, brownish translucent areas at edges of the

aggregates shall be considered fully coated

5.2.3.8 Spread the mixed material immediately onto the flat metal lid or silicone-coated paper Avoid any

lumps in the bitumen coated aggregates Ensure that the material is loosely spread as individual particles

5.2.3.9 Store the mixed material on the lid or silicone paper between 12 h and 64 h at ambient

temperature of (20 ± 5) °C Avoid direct exposure to sunlight and contamination with dust

5.3 Conditioning

5.3.1 Split the mixed material into three part samples each weighing (150 ± 2) g

5.3.2 Mark the test bottles and fill them to approximately 50 % of the volume with distilled or de-ionized

water having a temperature of (5 ± 2) °C

NOTE The low initial water temperature prevents the bitumen coated aggregate particles from forming lumps before

the rolling is started

5.3.3 Transfer, with moistened fingers in order to reduce adherence, a part sample of (150 ± 2) g to each

bottle, one particle at a time Fill the bottle with distilled or de-ionized water, having a temperature of

(5 ± 2) °C, to the shoulder level of the bottle (level A on Figure 3)

5.3.4 For each bottle, place the glass rod in the bottle as shown in Figure 3 and seal the bottle with the

screw cap Ensure that the glass rod with rubber tube is firmly fixed between the bottom of the bottle and the

screw cap

In order to avoid lump formation, perform procedures 5.3.3 and 5.3.4 and place the bottles on the rolling

machine as quickly as possible

NOTE This is especially important when using an adhesion improving agent

5.4 Procedure

5.4.1 For the test, adjust the bottle rolling machine to a rotation speed as stated below:

For pure bitumen with penetration above 100 1/10 mm at 25 °C determined in accordance with EN 1426, the

rotation speed of the bottles shall be 40 min-1± 10 % For harder, pure binders with penetration at 25 °C less

than or equal to 100 1/10 mm, and when using adhesion agents, adhesion improving fillers or modified binder,

the rotation speed shall be 60 min-1± 10 %

NOTE When adhesion improving additives are tested, the reference (without additive) shall also be tested with a

rotation speed of 60 min-1 ± 10 %

5.4.2 Place the bottles on the bottle rolling machine and start the rolling procedure

5.4.3 Perform the test at room temperature between 15 °C and 25 °C and avoid direct exposure to sunlight

)Mg/m (densityaggregate

650 (Mg/m3),

2

3

=

α

NOTE When the test is started, the water in the test bottles will have a temperature of (5 ± 2) °C according to 5.3.2 During the first part of the rolling procedure, the water temperature will increase until the room temperature as specified above is reached

5.4.4 Stop the bottle roller after 6 h ± 15 min of rolling time

5.4.5 Pour the water from the bottle into a beaker

5.4.6 Empty the aggregate particles from the bottle into a test bowl and fill with fresh, distilled or de-ionized

water to a level just above the top of the particle surfaces Place the test bowl on a white surface

NOTE The purpose of adding fresh water is to allow for optimal visual determination of binder coverage on the aggregate particles

5.4.7 Estimate by visual observation and record the average degree of bitumen coverage of the particles to

the nearest 5 % Use a lamp to facilitate the observation and estimation Any thin, brownish, translucent areas shall be considered fully coated Record if lumps of particles are observed

NOTE 1 A magnifying glass with low magnification may additionally be used to facilitate the estimation

NOTE 2 There may be a tendency to estimate the degree of bitumen coverage higher on dark aggregates than on bright aggregates For comparison, a similar quantity of uncoated aggregates, placed in a similar test bowl filled with water, may be used to facilitate the estimation

NOTE 3 To facilitate systematic visual estimations of the degree of bitumen coverage on particles, see Annex A for reference

NOTE 4 Automated systems can alternatively be used for determination of the degree of bitumen coverage, provided it has been documented that the same results are obtained for aggregates of similar darkness

5.4.8 Discard the water from the test bowl, return the aggregate particles to the bottle and refill with the

original water from the beaker Seal the bottle with the screw cap and continue the rolling procedure

5.4.9 Repeat steps 5.4.2 to 5.4.7, but this time stop the bottle after (18 h ± 15 min) of additional rolling time

(total of 24 h rolling time)

5.4.10 Optionally, observations may additionally be made after (48 ± 1) h and (72 ± 1) h total rolling time

If needed, the rolling procedure may temporarily be stopped during the prolonged test to allow the procedure

to follow normal working hours If the procedure is temporarily stopped, the water shall be poured from the bottle into a beaker, and the aggregate emptied out of the bottle and stored at a silicone coated paper or similar smooth surface at room temperature Avoid direct exposure to sunlight When the procedure is continued, the aggregate and the original water is poured into the bottle Seal the bottle with the screw cap and continue the rolling procedure

NOTE If testing is performed on aggregate/binder compositions with a high resistance to binder stripping, the test procedure may optionally be further extended to include readings after 96 h and 168 h

5.4.11 Each visual determination of binder coverage shall be carried out independently by two skilled

operators The same operators shall perform all the visual determinations throughout the test The operators may discuss the reading technique but shall not during the test procedure have access to the individual readings already noted by the other operator

NOTE The procedure involving two operators may not always be possible to follow in small laboratories In such cases, determinations carried out by a single operator is accepted, provided that it is clearly noted in the test report that only a single operator has performed the visual determinations

5.4.12 If lumps of particles are observed to an extent exceeding 10 % of the total number of particles, the

test result shall be discarded