BS EN 12607-2:2014

BS 2000-460-2:2014

BSI Standards Publication

Bitumen and bituminous

binders — Determination of
the resistance to hardening
under influence of heat and air
Part 2: TFOT method
BS EN 12607-2:2014 BRITISH STANDARD

National foreword
This British Standard is the UK implementation of EN 12607-2:2014.
It supersedes BS EN 12607-2:2007 which is withdrawn.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.
This publication does not purport to include all the necessary
provisions of a contract. Users are responsible for its correct
application.
© The British Standards Institution 2014.
Published by BSI Standards Limited 2014
ISBN 978 0 580 77117 0
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 30 November 2014.
BS 2000 Series
Energy Institute, under the brand of IP, publishes and sells all
Parts of BS 2000, and all BS EN and BS ISO petroleum test
methods that would be part of BS 2000, both in its annual
publication “IP Standard Test Methods for analysis and testing
of petroleum and related products, and British Standard 2000
Parts” and individually.

Amendments/corrigenda issued since publication

Date Text affected
EUROPEAN STANDARD EN 12607-2
NORME EUROPÉENNE
EUROPÄISCHE NORM November 2014

ICS 75.140; 91.100.50 Supersedes EN 12607-2:2007

English Version

Bitumen and bituminous binders - Determination of the

resistance to hardening under influence of heat and air - Part 2:
TFOT method

Bitumes et liants bitumineux - Détermination de la Bitumen und bitumenhaltige Bindemittel - Bestimmung der
résistance au durcissement sous l'effet de la chaleur et de Beständigkeit gegen Verhärtung unter Einfluss von Wärme
l'air - Partie 2: Méthode TFOT und Luft - Teil 2: TFOT-Verfahren

This European Standard was approved by CEN on 16 August 2014.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same
status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION

COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2014 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 12607-2:2014 E
worldwide for CEN national Members.
BS EN 12607-2:2014
EN 12607-2:2014 (E)

Contents Page

Foreword ..............................................................................................................................................................3
1 Scope ......................................................................................................................................................4
2 Normative references ............................................................................................................................4
3 Principle ..................................................................................................................................................4
4 Apparatus ...............................................................................................................................................5
5 Sampling .................................................................................................................................................6
6 Procedure ...............................................................................................................................................7
7 Calculation ..............................................................................................................................................7
8 Expression of results ............................................................................................................................8
9 Precision .................................................................................................................................................8
10 Test report ..............................................................................................................................................9
Annex A (informative) Characteristics of thermometers.............................................................................. 10
Bibliography ..................................................................................................................................................... 11

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 BS EN 12607-2:2014
EN 12607-2:2014 (E)

Foreword

This document (EN 12607-2:2014) has been prepared by Technical Committee CEN/TC 336 “Bituminous
binders”, the secretariat of which is held by AFNOR.

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 May 2015 and conflicting national standards shall be withdrawn at the
latest by May 2015.

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 12607-2:2007.

This document has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association.

In comparison with EN 12607-2:2007, the following significant changes have been made:

— changed/added wording of the Warning in the Scope;

— EN 12595, Bitumen and bituminous binders — Determination of kinematic viscosity has been added to
Clause 2;

— the reference to mercury thermometer has been deleted (see subclause 4.2) and Annex A is informative.

EN 12607 consists of the following parts under the general title “Bitumen and bituminous binders –
Determination of the resistance to hardening under the influence of heat and air”:

— Part 1: RTFOT method;

— Part 2: TFOT method;

— Part 3: RFT method.

The scope of this standard has been enlarged by adding oxidized bitumens and hard industrial bitumens that
are not used for paving applications. The reason is to facilitate that EN 13303, Bitumen and bituminous
binders – Determination of the loss of mass after heating of industrial bitumen can be replaced in product
standards by EN 12607-2 at the next revision of EN 13303.

It is to be noted that this – if so decided – will change the property from loss in mass into change in mass in
EN 13304, Bitumen and bituminous binders – Framework for specification of oxidized bitumens and in
EN 13305, Bitumen and bituminous binders – Framework for specification of hard industrial bitumens.

According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech
Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece,
Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.

3
BS EN 12607-2:2014
EN 12607-2:2014 (E)

1 Scope

This part of EN 12607 specifies a method for measuring the combined effects of heat and air on a film of
bitumen or bituminous binder, simulating the hardening which most bituminous binders undergo during mixing
in an asphalt mixing plant. The method is suitable for other bituminous binders than paving grade bitumen, but
the reference temperature might give excessive hardening that does not resemble real conditions during
mixing at the plant. The method may not represent the hardening that occurs during mixing of warm mix
binders.

Additionally, this part of EN 12607 specifies a method for the determination of the change in mass of oxidized
bitumens and hard industrial bitumens after heating. The method is used to detect volatile components.

The method is referred to as TFOT, i.e. Thin Film Oven Test.

WARNING — 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 identify the hazards and
assess the risks involved in performing this test method and to implement sufficient control measures
to protect individual operators (and the environment). This includes appropriate safety and health
practices and determination of the applicability of regulatory limitations prior to use.

If there is a likelihood of volatile components being present in a binder, this procedure should not be
used. It should not be used for cut-back bitumen or bituminous emulsions before these products have
been stabilized, e.g. in accordance with EN 13074-2.

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 1425, Bitumen and bituminous binders - Characterization of perceptible properties

EN 12594, Bitumen and bituminous binders - Preparation of test samples

EN 12595, Bitumen and bituminous binders - Determination of kinematic viscosity

3 Principle

A film of bituminous binder is heated in an oven at a specified temperature for a given period of time.

For bituminous binders for paving applications, the effects of heat and air are determined based on the
change in mass (expressed as a percentage) and on the change in the bituminous binder's properties such as
kinematic viscosity according to EN 12595, before and after the period in the oven.

For bituminous binders for industrial applications, the combined effects of heat and air and loss of volatiles are
determined based on the change in mass (expressed as a percentage). This will be the value from this
conditioning method that will be utilized in EN 13304 and EN 13305 as loss in mass (change in sign).

NOTE Penetration according to EN 1426 and softening point according to EN 1427 can be measured on harder
grades before and after oven treatment at 163 °C.

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 BS EN 12607-2:2014
EN 12607-2:2014 (E)

4 Apparatus

Usual laboratory apparatus and glassware, together with the following:

4.1 Oven, electrically heated and conforming to the performance requirements indicated in Table 1 for
operating temperatures up to 180 °C.

The oven shall be rectangular with a minimum interior height, width and depth of 330 mm.

The front door shall be hinged and tightly fitted, and have a clear opening of the same height and width as the
interior of the oven. The window on the door shall be at least 100 mm by 100 mm, with two sheets of glass
separated by an air space. The window shall permit an unobstructed view of the interior of the oven so that
the control thermometer, located as specified in 6.1 may be read without opening the door.

NOTE 1 The oven can alternatively be provided with an inner glass door through which the thermometer can be read
upon opening the outer door momentarily.

The oven shall be ventilated by convection currents of air; the oven shall have air inlets and outlets evacuating
hot gases meeting the requirements of Table 1.

NOTE 2 These inlets and outlets can be of different size and arrangement provided the requirements in Table 1 are
met.

Table 1 — Performance requirements for Thin Film Oven

Characteristics Requirements
Deviation from a specified test temperature throughout the testing chamber during a 24 h
period for the differential between ambient and test temperature, when more than 50 °C, 5
maximum, % of differential
Time constant, maximum, s 720
Rate of ventilation of testing chamber, air changes per h, minimum 10

NOTE 3 These performance requirements are extracted from ASTM E145, type IB (gravity convection ventilated oven).

The oven shall be provided with a metal circular shelf with a minimum diameter of 250 mm. The shelf shall
provide a flat surface to support the containers without blocking all air circulation through the shelf when the
containers are in place. The shelf shall be suspended by a vertical shaft and centred with respect to the
horizontal interior of the oven. The shelf shall be mechanically driven to rotate at the rate of (5,5 ± 1,0) r/min.
The shelf shall be vertically located as close to the centre of the oven as allowed by the requirements of 6.1
regarding thermometer placement.

Minimum size ovens allow the use of two containers. Larger ovens, having proportionally larger shelves to
accommodate a greater number of containers can be suitable. Under no circumstances should more than one
shelf, properly centred, be used in an oven.

4.2 Temperature measuring device.

A temperature measuring device (combining sensor and reading unit) shall

— have a range from at least 110 °C to 170 °C,

— be readable to 0,1 °C or less and,

— have an accuracy of 0,5 °C or better.

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EN 12607-2:2014 (E)

Sensors based on platinum resistance thermometers have been found suitable but other principles are also
allowed. The thermal response time of the sensor shall be comparable with the former used reference (see
informative Annex A). The temperature measuring device shall be calibrated regularly.

A solid stem mercury thermometer (which used to be the former reference thermometer as described in
Annex A) is also allowed if national regulations permit its use.

When measuring and controlling nominally constant temperatures as in this test method, the thermal response
time can be rather high (e.g. slow response to a change in temperature). Care shall be taken to consider this
aspect since low thermal response times of the sensor can indicate greater cyclic variations than the
bituminous material in practise.

4.3 Container, (in which the sample of bituminous binder is subjected to the test), cylindrical pan
(140 ± 1) mm in inside diameter and (9,5 ± 0,5) mm deep with a flat bottom, stainless steel or aluminium, with
a thickness of (0,6 ± 0,1) mm to (1,0 ± 0,1) mm.

NOTE 1 50 ml of sample in this container will give a film thickness of approximately 3,2 mm.

NOTE 2 Containers have a tendency to become warped or bent with use. Although a small amount of warping does
not significantly affect results, it is advisable to eliminate damaged pans.

4.4 Balance, accurate to ± 10 mg, readable to 1 mg.

5 Sampling

5.1 General

Make sure that the laboratory sample is homogeneous and is not contaminated according to EN 1425. Take
all necessary safety precautions and ensure that the test sample is representative of the laboratory sample
from which it is taken (see EN 58). The laboratory sample shall be taken in accordance with EN 58.

5.2 Test sample preparation

Prepare the test sample in accordance with EN 12594. Remove a sufficient quantity of the laboratory sample
to perform tests to establish the characteristics to be measured on the bituminous binder before and after the
RTFOT hardening test. If necessary, use a warmed knife and transfer it to a suitable container according to
EN 12594.

The sample shall be free of water. Heat the sample in an oven in its container with a loosely fitted cover to a
fluid condition not exceeding 10 °C below the test temperature for the minimum time necessary, to ensure that
the sample is completely fluid. Homogenize the sample by stirring. If special bituminous binders, modified
binders or bituminous binders with a high softening point are tested, it may be necessary to prepare the
sample at a higher temperature. In this case, heat the sample as described above and in accordance with
EN 12594. For polymer modified bitumens, the temperature may not exceed 200 °C, irrespective of the
softening point.

5.3 Initial characteristics

Determine the initial characteristics of the bituminous binder using an appropriate test method, according to
the grade in question, e.g. the kinematic viscosity at 60 °C (EN 12595), ν1.

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 BS EN 12607-2:2014
EN 12607-2:2014 (E)

6 Procedure

6.1 Test conditions

Ensure that the oven (4.1) is level so that the shelf rotates on a horizontal plane with a maximum tilt during
rotation of not more than 3° from the horizontal. Determine the temperature of the oven with the specified
thermometer (4.2) in a vertical position at a point equidistant from the centre and the outer edge of the shelf
and the bottom of the thermometer bulb approximately 6 mm above the top of the shelf.

For bituminous binders for paving applications, the reference temperature of the test is (120 ± 1) °C,
corresponding to the mixing temperature of soft paving grade bitumens.

NOTE However, it is possible to perform the test at other temperatures, e.g. (163 ± 1) °C for harder paving bitumen
grades.

For bituminous binders for industrial applications, the reference temperature of the test is (163 ± 1) °C.

6.2 Determination

Weigh separately containers (4.3) to the nearest 1 mg (m0).

Pour (50,0 ± 0,5) g of the sample into each of two or more of the containers. Allow the samples to cool to
room temperature for approximately 30 min, and weigh them separately to the nearest 1 mg (m1).

With the oven at the test temperature ± 1 °C, rapidly place the containers with the sample on the circular shelf,
close the oven, and commence rotating the shelf. Maintain the sample in the oven for 5 h from the time the
test temperature reaches 1 °C below the test temperature. Ensure that the total time that a sample is in the
oven is not more than 5 h 15 min. At the end of the heating period, remove the samples from the oven.

Cool to room temperature for approximately 30 min, weigh to the nearest 1 mg (m2), and calculate the change
in mass of the bituminous binder in each container.

Do not test different samples in the same oven at the same time.

When a complete test cannot be completed on the same day, weigh the residues and store them overnight
before reheating.

After weighing the samples, place them back on the shelf in the oven at the test temperature. Close the oven
and rotate the shelf for 15 min. Remove the samples and transfer the material from each pan into a 250 ml
container preheated to the test temperature. Stir the combined residues thoroughly, heating the container if
necessary.

6.3 Measurement of properties

Measure the properties chosen in 5.3 (e.g. the kinematic viscosity of the residue at 60 °C (EN 12595), ν2)
within 72 h. Avoid reheating the sample more than once.

NOTE Excessively reheating the sample can influence the test results obtained.

7 Calculation

Calculate the change in physical properties or characteristics after the hardening procedure as follows:

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BS EN 12607-2:2014
EN 12607-2:2014 (E)

ν2
Δν, ratio of kinematic viscosities at 60 °C = (1)
ν1

Δm, percentage of change in mass = 100 ×

(m2 − m1 ) (2)
(m1 − m0 )
where

ν1 is the kinematic viscosity of the sample before hardening, in millimetres squared per second;

ν2 is the kinematic viscosity of the residue, in millimetres squared per second;

m0 is the mass of the empty container, in grams;

m1 is the mass of the container with the sample before the test, in grams;

m2 is the mass of the container with the sample after the test, in grams.

8 Expression of results

Express a loss in mass as a negative percentage change and a gain in mass as a positive percentage
change.

The results of the percentage change in mass for two containers are considered valid if the difference of the
two measurements is equal to or less than 0,05 % mass fraction absolute.

Express the percentage change in mass as the average of a minimum 2 valid determinations to the nearest
0,01 %.

If the value of a physical property is measured on the sample after TFOT, e.g. kinematic viscosity, express the
ratio of viscosities to the nearest 0,1. Report the values of initial properties and residue properties.

9 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 values given in Table 2 in only one case in twenty.

9.2 Reproducibility

The difference between two single and independent 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 values given in Table 2 in only one case in twenty.

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 BS EN 12607-2:2014
EN 12607-2:2014 (E)

Table 2 — Precision

Characteristics Repeatability, r Reproducibility, R

a
Change in mass TFOT 120 °C
≤ 0,1 % mass fraction absolute 0,02 % mass fraction 0,14 % mass fraction
> 0,1 % mass fraction absolute 8,0 % of mean 38 % of mean
Ratio of dynamic viscosity at 60 °C
TFOT 120 °C a
Ratio < 1,5 6 % of mean 16 % of mean
These precision data are not automatically applicable to modified bitumen and
industrial bitumen. For modified bitumen they should only be used for guidance
until criteria data are available.
a
These figures are based on an analysis of data from sixteen laboratories on three
samples of soft paving grade bitumens with a viscosity ratio < 1,5.

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 part of EN 12607;

c) test temperature;

d) results obtained (see Clause 8);

e) any deviation, by agreement or otherwise, from the procedure specified;

f) date of the test.

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BS EN 12607-2:2014
EN 12607-2:2014 (E)

Annex A
(informative)

Characteristics of thermometers

Table A.1 — Characteristics of thermometers

Characteristics Units Test temperatures

120 °C 163 °C
Temperature range °C 114 to 130 155 to 170
Scale marks
Subdivision °C 0,5 0,5
Long lines at each °C 1 1
Numbers at °C 115, 120, 125, 130 155, 160, 165, 170
Maximum scale error °C 0,5 0,5
Immersion total total
Expansion chamber permits heating to °C 200 200
Total length mm 150 to 160 150 to 160
Stem outside diameter mm 5,5 to 7,0 5,5 to 7,0
Bulb length mm 10 to 15 10 to 15
Bulb outside diameter mm 5,0 to stem diameter 5,0 to stem diameter
Scale location
Bottom of bulb to line at °C 114 155
Distance mm 50 to 60 50 to 60
Length of scale mm 40 to 60 40 to 60
Maximum distance of contraction mm 30 30
chamber to the top
NOTE The thermometer ASTM 13C/IP47C has been found suitable for the test temperature at 163 °C.

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 BS EN 12607-2:2014
EN 12607-2:2014 (E)

Bibliography

[1] EN 1426, Bitumen and bituminous binders - Determination of needle penetration

[2] EN 1427, Bitumen and bituminous binders - Determination of the softening point - Ring and Ball
method

[3] EN 13074-2, Bitumen and bituminous binders - Recovery of binder from bituminous emulsion or cut-
back or fluxed bituminous binders - Part 2: Stabilisation after recovery by evaporation

[4] EN 13304, Bitumen and bituminous binders - Framework for specification of oxidised bitumens

[5] EN 13305, Bitumen and bituminous binders - Framework for specification of hard industrial bitumens

[6] ASTM E145-94 (2001), Standard Specifications for Gravity Convection and Forced-Ventilation Oven

[7] ASTM D1754-97 (2002), Standard Test Method for Effect of Heat and Air on Asphaltic Materials (Thin-
Film Oven Test)

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