Road Materials and Pavement Design

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The mechanisms of hydrated lime modification of

asphalt mixtures: a state-of-the-art review

Didier Lesueur, Joëlle Petit & Hans-Josef Ritter

To cite this article: Didier Lesueur, Joëlle Petit & Hans-Josef Ritter (2013) The mechanisms
of hydrated lime modification of asphalt mixtures: a state-of-the-art review, Road Materials and
Pavement Design, 14:1, 1-16, DOI: 10.1080/14680629.2012.743669

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Road Materials and Pavement Design, 2013
Vol. 14, No. 1, 1–16, http://dx.doi.org/10.1080/14680629.2012.743669

The mechanisms of hydrated lime modification of asphalt mixtures: a

state-of-the-art review
Didier Lesueura *, Joëlle Petitb and Hans-Josef Ritterc
a Lhoist R&D, 1400 Nivelles – Belgium; b Carmeuse, 5300 Seilles – Belgium; c Bundesverband der Deutschen
Kalkindustrie e.V., 50968 Köln – Germany

Although already known for a long time, hydrated lime (HL) attracted a strong interest as
an asphalt additive during the 1970s in the USA, when moisture damage and frost became
some of the most pressing pavement failure modes of the time. Given its extensive use in
the past 40 years, HL is known to be more than a moisture damage additive: it is an “active
filler” that also reduces the chemical ageing of the bitumen and stiffens the mastic more than
a normal mineral filler above room temperature. These properties impact durability, and HL
is now seen as an additive that increases asphalt mixture durability. This article is a literature
review on the fundamentals of the effect of HL on asphalt mixtures. The reasons for it being
so effective lie in the strong interactions between both the aggregate and the bitumen and a
combination of four mechanisms, two on the aggregate and two on the bitumen. HL modifies
the surface properties of the aggregate, allowing for the development of surface composition
and roughness more favourable to bitumen adhesion. Then, HL can treat the existing clayey
particles adhering to the aggregate surface, inhibiting their detrimental effect on the mixture.
Also, HL reacts chemically with the acids of the bitumen, which in turn slows down the age
hardening kinetics and neutralises the effect of the “bad” adhesion promoters originally present
inside the bitumen, enhancing the moisture resistance of the mixture. Finally, the high porosity
of HL explains its stiffening effect above room temperature.
Keywords: hydrated lime; bitumen; asphalt mixture; ageing; adhesion; mastic

1. Introduction
Hydrated lime (HL) has been known as an additive for asphalt mixtures from the very beginning
(Kennedy, 1984; Lesueur, 2010; Love, 1890). It attracted a strong interest during the 1970s in
the USA, partly as a consequence of a general decrease in bitumen quality due to the petroleum
crisis of 1973, when moisture damage and frost became some of the most pressing pavement
failure modes of the time. HL was observed to be the most effective additive (Hicks, 1991) and,
as a consequence, it is now specified in many states and it is estimated that 10% of the asphalt
mixtures produced in the USA now hold HL (Hicks & Scholz, 2003).
Given its extensive use in the past 40 years in the USA, HL has been seen to be more than a
moisture damage additive (Lesueur, 2010; Little & Epps, 2001; Little & Petersen, 2005; Sebaaly,
Little, & Epps, 2006; Sebaaly, 2007). Given its multifunctional effects, it is now seen as an
“active filler”. HL is known to reduce the chemical ageing of the bitumen (Lesueur, 2010; Little
& Epps, 2001; Little & Petersen, 2005; Sebaaly et al., 2006). Furthermore, it stiffens the mastic
more than a normal mineral filler (Lesueur, 2010; Little & Epps, 2001; Little & Petersen, 2005;
Sebaaly et al., 2006), an effect that is only observed above room temperature (Lesueur, 2010). As

*Corresponding author. Email: didier.lesueur@lhoist.com

© 2013 The Author(s). Published by Taylor & Francis.

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have been asserted.
2 D. Lesueur et al.

a consequence, no negative effect on the thermal cracking resistance is reported in the literature
(Lesueur, 2010; Little & Epps, 2001; Little & Petersen, 2005; Sebaaly et al., 2006).
Given that all the above-mentioned mixture properties impact the durability of asphalt mixtures,
the use of HL has a strong effect on the durability of asphalt mixtures. As detailed elsewhere
(Lesueur, Petit, & Ritter 2012), the field experience from North American state agencies estimates
that HL at the usual rate of 1%–1.5% in a mixture (based on dry aggregate) increases the durability
of asphalt mixtures by 2–10 years, that is, by 20%–50% (Hicks & Scholz, 2003).
The European experience is not yet as developed as the US experience, but the beneficial
effects of HL on the durability of asphalt mixtures have also been largely reported (Lesueur,
2010). As an example, the French Northern motorway company Sanef currently specifies HL
in the wearing courses of its network, because it observed that an HL-modified asphalt mixture
has a 20%–25% longer durability (Raynaud, 2009). Similar observations led the Netherlands to
specify HL in porous asphalt (CROW, 2007; Voskuilen & Verhoef, 2003), a type of mix that now
covers 70% of the highways in the country. As a result, HL is increasingly being used in asphalt
mixtures in most European countries, in particular, in Austria, France, the Netherlands, the UK and
Switzerland.
This article reviews the reasons for HL being so effective in asphalt mixtures and sheds some
light on what is meant by the concept of “active filler”. In order to do so, we focus on the
interactions between HL and the major components, that is, aggregate and bitumen. As a result,
the mechanisms of HL modification can be explained by a combination of four effects: two on
the aggregate and two on the bitumen.

2. HL as an additive for asphalt mixtures

This section presents HL and its relevant properties as far as asphalt modification is concerned.

2.1. HL properties
HL is mainly composed of calcium hydroxide Ca(OH)2 . It is obtained by hydrating quick-
lime (essentially calcium oxide, CaO) using specific equipments. Quicklime is manufactured
by burning limestone of very high purity (made of calcium carbonate, CaCO3 ) at temperatures
around 900◦ C in dedicated kilns (Boynton, 1980). The same cycle can be performed on dolomite
(CaCO3 .MgCO3 ) in order to obtain dolomitic lime (CaO.MgO) and then hydrated dolomitic lime
(Ca(OH)2 .Mg(OH)2 ).
In Europe, HL and quicklime are specified within the European standard EN 459-1 for con-
struction and civil engineering applications. In the USA, specifications for HL in asphalt concrete
are found in ASTM C 1097 and AASHTO M 303.
The principal qualities of the various grades of hydrated products found in Europe are sum-
marised in Table 1. The grades are for calcium lime (CL) and the number identifies the purity
in terms of the mass content of CaO + MgO. The letter “S” stands for ‘slaked’ and identifies
hydrated products in powder form.
As far as asphalt mixture modification is concerned, high-purity calcic HL is the product that is
mostly used. This corresponds to CL 90 S in EN 459-1 or ASTM C 1097 or Type I in AASHTO M
303 (Table 1). Still, hydrated dolomitic lime is also mentioned sometimes (Type II in AASHTO
M 303 – Table 1), and it was shown to behave in a similar manner (Stroup-Gardiner & Newcomb,
1990). Quicklime, on the contrary, was shown to be detrimental when used as a substitute for
HL (Stroup-Gardiner & Epps, 1987). Still, some very specific applications use either quicklime
or HL with a porous aggregate (porous basalt, slag, etc.) in order to prevent the so-called soup
phenomenon observed when the water from the aggregate emulsifies the bitumen during mixture
 Road Materials and Pavement Design 3

Table 1. The main characteristics of the various grades of calcic HL according to

EN 459-1, ASTM C 1097 and AASHTO M 303.

CaO + MgO Available or active lime MgO

wt.% wt.% wt.%
EN 459-1 CL90 S ≥90 ≥80 ≤5
CL80 S ≥80 ≥65 ≤5
CL70 S ≥70 ≥55 ≤5
ASTM C 1097 ≥90
AASHT0 M 303 Type I >90 ≤4
Type II ≥96 4–36

transportation (Sainton, Puiatti, & Walter, 1999). But in this case, the remaining water inside
the pores of the aggregate hydrates the quicklime and, in the end, HL is present in the mixtures.
Therefore, we focus here on standard HL.
HL generally comes in the form of a dry white powder with a particle density close to 2.2 Mg/m3
(Boynton, 1980). Because of a high level of particle porosity (of order 50%), its apparent density
typically ranges from 0.3 to 0.8 Mg/m3 as measured by EN 459-2 or ASTM C 110.

2.2. HL as a filler
Because of its mineral origin and powder form, HL is generally compared with mineral fillers in
the asphalt industry. As a matter of fact, the European standards for hot-mix asphalt (series EN
13108-1 to 13108-7) clearly say: “filler includes materials as cement and hydrated lime” (note
1 in paragraph 4.3.4). In this sense, HL can be evaluated using the specifications on aggregates
for asphalt mixtures as detailed in EN 13043. More precisely, the relevant part of this standard
for HL is the one dealing with fillers. The case of a mixed filler (mixture of filler and HL) is
also described in the standard. The standard mainly considers the properties of the filler related
to its stiffening effect on the bitumen. In particular, the voids of the dry compacted filler (Rigden
air voids – EN 1097-4 or Dry Compaction Test in NAPA IS-127) and delta ring and ball (EN
13179-1, no US equivalent) are measured.
Although some of the filler tests used in Europe are sometimes also mentioned in the USA,
there is no real need for the formulator to use them for HL because there are dedicated standards
describing the appropriate properties of HL for asphalt mixtures (ASTM C 1097/AASHTO M
303).
The voids of the dry compacted filler consist in measuring the density of a compacted specimen
of the studied filler and dividing it by the particle density of the filler. Mineral fillers generally
have Rigden voids ranging from 28% to 45% (Grabowski, Wilanowicz, & Sobol, 2009; Lesueur
et al., 2003; Schneider, Schellenberg, Ritter, & Schiffner, 2002; Vansteenkiste & Vanelstraete,
2008), with 30%–34% being the usual range for many fillers such as most limestone fillers. HL
has a higher Rigden value, generally between 60% and 70%, with 65% being a common value
(Lesueur, 2010). Clearly, this property differentiates HL from other mineral fillers. Note that the
low bulk density of HL also captures the high porosity of the product. As far as mixed fillers are
concerned, Rigden air voids increase when the HL content increases, with typical values being
in the 45%–50% range for 25 wt.% HL in the mixed filler (Grabowski et al., 2009; Vansteenkiste
& Vanelstraete, 2008).
The delta ring and ball test consists in measuring the increase in softening temperature of
70/100 bitumen after the addition of 37.5 vol.% of the studied filler. Mineral fillers typically have
the delta ring and balls between 8◦ C and 25◦ C, with 15◦ C being a common value (Grabowski
4 D. Lesueur et al.

Ring & Ball softening temperature (°C) 90

80

70

Hydrated Lime
60 Limestone
Graywacke

50

40

30
0 10 20 30 40 50 60 70 80
Filler content (wt.%)

Figure 1. The ring and ball softening temperature of a 200-penetration-grade bitumen as a function of
filler weight content for HL, limestone filler and graywacke filler.
Source: Cramer et al. (2001).

et al., 2009; Vansteenkiste & Vanelstraete, 2008). As detailed in several studies (Grabowski et al.,
2009; Lesueur, 2010), the test cannot be performed on pure HL. As a matter of fact, the stiffening
power of HL is so pronounced that the 37.5 vol.% blend is not fluid enough to prepare the test
specimen.
Still, an amount of HL lower than the one specified in the European standard allows quantifying
the stiffening effect (Cramer, Herz, & Radenberg, 2001), as shown in Figure 1. For example, Ger-
man studies generally use a stability index consisting in finding the filler/bitumen ratio that raises
the ring and ball value of a 200-penetration bitumen by 20◦ C (Cramer et al., 2001; Schellenberg
& Eulitz, 1999). Values for HL are typically in the 0.7–1.0 range, meaning that HL contents of
40–50 wt.% (23–31 vol.%) raise the ring and ball value by 20◦ C. Mineral fillers usually have
values in the 1.5–2.5 range (Cramer et al., 2001; Schellenberg & Eulitz, 1999). As a consequence,
when HL is used in the form of a mixed filler, 15 wt.% HL and 30 wt.% HL are seen to increase
the delta ring and ball by, respectively, 2–10◦ C and 8–20◦ C (Grabowski et al., 2009).
Note that the volume fraction (i.e. 37.5 vol.%) used in the standard test for the delta ring and
ball is not representative of the typical HL content in an asphalt mixture. As a matter of fact,

Table 2. The comparison of the typical properties of HL with those of mineral fillers.

Property Method Unit Hydrated lime Mineral filler

Particle density EN 1097-7 / AASHTO T84 Mg/m3 2.2 2.6–2.9

Voids in dry compacted filler EN 1097-4 – NAPA IS-127 % 60–70 28–45
Delta ring and ball EN 13179-1 ◦C n.m. 8–25
Bitumen number EN 13179-2 - 70–120 40–50
Mass in kerosene EN 1097-3 Mg/m3 0.3 0.5–0.9
Blaine specific surface EN 196-6 – ASTM C 204 cm2 /g >10,000 7000
Specific surface area BET (N2 adsorption) cm2 /g 150,000–200,000 14,000–95,000
Methylene blue value EN 933-9 g/kg <1 0–20
Notes: Data from Lesueur (2010) are given for the said European standard. When existing, the US equivalent method
is given for information, but the data range might slightly change when using the US standards due to minor differences
in the test methods (n.m.: not measurable – see the text for details).
 Road Materials and Pavement Design 5

typical HL content in an asphalt mixture is 1–1.5 wt.% based on dry aggregate. For a typical
binder content of 5 wt.% (based on dry aggregate), this amounts to 20–30 wt.% or 10–15 vol.%
HL in the bitumen.
Other properties used to specify mineral fillers for asphalt are also listed in Table 2. It sum-
marises the typical values for some properties of HL in comparison with those of mineral fillers
obtained from the crushing and classification of mineral aggregates. Table 2 is only intended to
give reasonable estimates for the listed properties, which will, of course, vary depending on the
origin of the materials. Note that fillers from other sources such as fly ash can have properties that
are very different from those of mineral fillers and must therefore not be confused with mineral
fillers.

3. HL in asphalt mixtures
As has been stated already in the introduction, the renewed interest for HL that occurred in the
USA in the 1970s was focused upon its beneficial effect on moisture damage and frost resis-
tance. However, it turned out that HL improved other properties of asphalt mixtures as well. In
the end, HL is now seen as a multifunctional additive that improves the durability of asphalt
mixes (Lesueur, 2010). Unfortunately, measuring the durability of asphalt mixtures in the labo-
ratory is not possible, because of the many distresses and failure modes that asphalt mixtures can
experience.
Still, test methods are available in order to evaluate the resistance of pavement materials to the
action of detrimental agents such as water, freeze–thaw cycles, temperature and Ultra-Violet light
exposure (ageing) and/or traffic. More precisely, HL is seen to improve (Lesueur, 2010; Little &
Epps, 2001; Little & Petersen, 2005; Sebaaly et al., 2006; Sebaaly, 2007)

• the resistance to moisture damage and frost,

• the resistance to chemical ageing and
• the mechanical properties, in particular, modulus, strength, rutting resistance, fatigue and
thermal cracking.

It is not the purpose of this article to review the laboratory evidence concerning these effects.
Interested readers can refer to the relevant literature where the effects of HL on asphalt mixtures
are clearly demonstrated with a diversity of materials (aggregate, bitumen and mixture formulas)
covering the five continents. A thorough literature review is available on the European Lime
Association website with a reference list classified by functionalities (www.eula.eu – Lesueur,
2010). Our concern here is to explain why HL is so effective in asphalt mixtures. In order to do
so, we first consider the effects of HL on the aggregate and then consider the effects of HL on the
bitumen.

3.1. Effect of HL on the aggregate

HL modifies the aggregate surface. Most of the US methods of adding HL consist in putting
it directly onto the wet aggregate, sometimes with marination (Hicks & Scholz, 2003). This
demonstrates that the surface modification of the aggregate is one key aspect of HL modification.

3.1.1. Surface modification of the aggregate

It is well known in asphalt science that siliceous aggregates have worst adhesive properties
towards bitumen when compared with limestone aggregates (Bagampadde, Isacsson, & Kiggundu,
6 D. Lesueur et al.

Figure 2. The effect of hydrated lime on the aggregate surface as proposed by Ishai and Craus.
Source: Ishai and Craus (1977).

2004; Curtis, Ensley, & Epps, 1993; Grönniger, Wistuba, & Renken, 2010; Hicks, 1991). The
reasons for this are that both anionic and cationic surfactants naturally present in the bitumen
strongly bond with calcium ions when only cationic surfactants strongly bond with silica atoms
(Curtis, 1993). As a consequence, anionic surfactants are easily displaced by water on siliceous
aggregates.
Therefore, one of the effects of HL is to allow for the precipitation of calcium ions onto the
aggregate surface, making it more favourable to bitumen. This effect has been recognised already
in a study by the Techion-Israel Institute of Technology in 1977 (Ishai & Craus, 1977). Once HL
has been added to the mastic (Figure 2(a)), calcium ions can accumulate at the aggregate sur-
face and then bond with the acids from the bitumen, forming water-insoluble salts (Figure 2(b)).
As a consequence, a surface treatment of the aggregate with almost no remaining HL parti-
cles already improves the bitumen–aggregate adhesion (Blazek, Sebor, Maxa, Ajib, & Paniagua,
2000).
In addition, calcium carbonate can precipitate in the presence of water (at the manufacturing
stage or in situ upon rain exposure) and therefore create a higher surface roughness, which is
known to favour bitumen adhesion as well (Ramond & Lesueur, 2004).
The overall interactions with the aggregate can be quite strong to the point that part of the HL
is not recovered after bitumen extraction. In the case of a basalt filler, about 40% of the HL was
not recovered when more than 90% was recovered with a limestone filler (Schiffner, 2003).
Still, the surface modification of the aggregate is not the only mechanism at stake. In fact, it
would be almost inexistent with a limestone aggregate. However, HL is known to improve the
adhesion of the limestone aggregates as well (Huang, Robertson, Branthaver, & Petersen, 2005;
Mohammad, Saadeh, Kabir, & Othman, 2008). So, other mechanisms must operate and especially
those acting on the bitumen as described below.
 Road Materials and Pavement Design 7

3.1.2. Clay flocculation

In the case of clayey aggregates, HL is known to be highly effective in improving the resistance
to moisture damage. This is the reason for HL being used in states such as California, Colorado,
Nevada and Utah, which all have aggregates contaminated by large amounts of clays (Aschen-
brener, 1995). More specifically, clays are generally present in the form of small inclusions inside
the rock and are liberated upon crushing. In this case, the role of HL is similar to that observed
in soil treatment (Little, 1995): lime flocculates the clay particles, preventing them from build-
ing a water-displaceable barrier between the bitumen and the aggregate. A German study with
controlled clay contamination confirmed that HL efficiently counteracts the effect of clay (Eulitz,
Schellenberg, Ritter, & Schmidt, 1998; Schellenberg & Eulitz, 1999).

3.2. Effect of HL on the bitumen

3.2.1. Chemical interaction with the bitumen
Bitumen ageing is a complex phenomenon and remains an active research area (Petersen & Glaser,
2011). The fact that HL slows down bitumen ageing was first highlighted in Utah at the beginning
of the 1970s. Bitumen extracted from a recovered field specimen of asphalt mixtures containing
HL was observed to have a significantly lower viscosity than the reference (Chachas, Liddle,
Peterson, & Wiley, 1971). Now, many studies confirm this finding and it is widely documented
that HL-modified bitumens show a decreased ageing susceptibility, as materialised by a slower
increase in viscosity (or any other mechanical property) versus ageing time (Lesueur, 2010; Little
& Petersen, 2005; Sebaaly et al., 2006). In all cases, asphaltene content increased at a slower pace
with HL-modified bitumens than with non-modified bitumens (Hopman, Vanelstraete, Verhasselt,
& Walter, 1999; Petersen, Plancher, & Harnsberger, 1987; Plancher, Green, & Petersen, 1976;
Verhasselt & Puiatti, 2004; Wisneski, Chaffin, Davison, Bullin, & Glover, 1996).
In parallel, the rate of carbonyl formation, which correlates well with viscosity increase (Martin,
Davison, Glover, & Bullin, 1990), slows down in HL-modified bitumens (Plancher et al., 1976;
Verhasselt & Puiatti, 2004; Wisneski et al., 1996). However, this effect was only found at ageing
temperatures of 88◦ C and above (respectively, 98.9–163◦ C, 88–99◦ C and 90–163◦ C), but was not
found at a lower temperature (60◦ C – Johansson, Branthaver, & Robertson 1995). The formation
of sulphides, sulphoxides and ketones seems not to be significantly modified by HL (Johansson
et al., 1995; Petersen et al., 1987).
HL-treated bitumens, that is, materials that have been in contact with HL that is later removed,
still show this reduced ageing effect (Petersen et al., 1987; Plancher et al., 1976).
Note that all the above effects are only seen with HL and not with a limestone filler (Huang,
Petersen, Robertson, & Branthaver, 2002; Petersen et al., 1987).
The origin of this surprising behaviour was at the heart of the pioneering work by Plancher
and co-workers (1976) at Western Research Institute (WRI). They took four bitumens that var-
ied widely in chemical composition. They prepared 1:1:600 weight solutions of bitumen, HL
and benzene, which were left to react for 24 h. After centrifugation and solvent extraction, they
recovered lime-treated bitumens, which were carefully analysed by infrared spectroscopy. About
4–6 wt.% of each bitumen was strongly adsorbed onto the HL particles (Plancher et al., 1976).
More recently, Hopman with the Netherlands Pavement Consulting has shown that HL is more
effective than a limestone filler with respect to the bitumen–filler interactions: on average, bitu-
men adsorption from several solvents (n-heptane, tetrahydrofuran – THF, toluene and methyl
chloride) on an active limestone filler containing 25 wt.% HL was 1.4 and 2.1 times higher than
that from those on a regular limestone filler for, respectively, Middle East and Venezuelan bitu-
mens (Hopman, 1998; Hopman et al., 1999). When comparing high-performance gel permeation
chromatography (HP-GPC) curves in toluene of the bitumens treated either with a limestone
8 D. Lesueur et al.

Figure 3. HP-GPC curves in toluene for two bitumens from Venezuela or Middle East after contact with
either a limestone filler or the same filler with 25 wt.% HL (active filler).
Source: Hopman et al. (1999).

Table 3. The concentration of functional groups in four AC-10 bitumens of different chemical
compositions before and after treatment with HL (data from Plancher et al., 1976).

Carboxylic Dicarboxylic
Ketones acids anhydrides 2-Quinolones Sulphoxides
Bitumen mol/l mol/l mol/l mol/l mol/l
B-2959 Untreated 0.015 trace 0.001 0.003 0.015
Lime treated 0.039 bld bld bld 0.013
B-3036 Untreated 0.021 trace 0.001 0.001 0.022
Lime treated 0.039 bld bld bld 0.019
B-3051 Untreated 0.017 0.014 0.003 0.009 0.010
Lime treated 0.039 bld 0.001 0.004 0.008
B-3602 Untreated 0.045 0.060∗ bld 0.011 0.015
Lime treated 0.100 0.014∗ 0.007 0.006 0.015
Note: bld: below level of detection; ∗ : present as carboxylate salts.

filler or with an active filler (Figure 3), it appears that short retention time moieties disappear
after the contact of the bitumen with HL. The interpretation is that HL has adsorbed some of the
heavy molecules of the bitumen. Note that the effect was less pronounced in THF than in toluene
(Hopman, 1998, 1999).
Information concerning the bitumen species adsorbed onto the HL surface can also be found in
the literature. As reproduced in Table 3, the lime-treated materials in the study by Plancher et al.
(1976) at WRI in Laramie showed lower concentrations of carboxylic acids, dicarboxylic anhy-
drides and 2-quinolones, which are typically concentrated in the heaviest components of bitumen
called the asphaltenes (see Lesueur, 2009 for a review of bitumen structure and chemistry). The
ketones were, however, more numerous. Sulphoxides did not change significantly.
Clearly, HL reacts with the acids, anhydrides and 2-quinolones of the bitumen. The same
conclusion was drawn in a more recent study by the same group (Petersen et al., 1987). One fifty
grams of bitumens from different origins were left to react under agitation for 6 h at 150◦ C with
 Road Materials and Pavement Design 9

Figure 4. Ageing index at 60◦ C (viscosity after ageing divided by the viscosity before ageing) for various
sources of bitumen modified with different weight proportions of HL (Hi-Ca) and hydrated dolomitic lime
(Dol). Ageing was performed in the TFAAT corresponding to 3 days at 113◦ C under air exchange.
Source: Replotted from Petersen et al. (1987).

Table 4. The concentration of functional groups in a Boscan bitumen before and after TFAAT ageing
in the presence of various amounts of HL or hydrated dolomitic lime (data from Petersen et al., 1987).

Carboxylic Dicarboxylic
Ketones acids anhydrides 2-Quinolones Sulphoxides
Lime treatment mol/l mol/l mol/l mol/l mol/l
None Unaged 0.00 0.015 0.000 0.017 0.02
Aged 0.28 0.015 0.007 0.017 0.35
10 wt.% high calcium Unaged 0.03 0.005 0.000 0.016 0.03
Aged 0.24 0.004 0.005 0.016 0.32
20 wt.% high calcium Unaged 0.03 0.003 0.000 0.014 0.03
Aged 0.22 <0.002 0.006 0.017 0.34
30 wt.% high calcium Unaged 0.03 <0.002 0.000 0.013 0.03
Aged 0.21 <0.002 0.006 0.014 0.32
20 wt.% Dolomitic Unaged 0.03 0.005 0.000 0.013 0.03
Aged 0.22 0.005 0.006 0.014 0.34

various amounts of HL or hydrated dolomitic lime. The limes could then be solvent-extracted.
The extent of ageing was quantified by the increase in viscosity at 60◦ C through an ageing
index (viscosity after ageing divided by that before – Figure 4). Infrared spectroscopy was used
to characterise the materials with and without lime treatment and before or after Thin Film
Accelerated Aging Test (TFAAT) ageing. As reproduced in Table 4, the presence of HL reduces
the amount of ketones, anhydrides and most of all carboxylic acids that form upon ageing.
Clearly, the acid–base reactions between HL and the acids naturally present in the bitumen are
fully supported by the published data (Little & Petersen, 2005). In addition, other data support
the importance of acid–base reactions in the anti-ageing effect:

• Johansson, Branthaver, and Robertson (1996) with the Swedish Royal Institute of
Technology (KTH) observed that the anti-ageing effect was not present with Mg(OH)2 ,
a weaker base than Ca(OH)2 .
10 D. Lesueur et al.

• Wisneski et al. (1996) at Texas A&M University observed that quicklime had an anti-ageing
effect that was the same as that HL did.

Still, acid–base neutralisations are not sufficient to explain the whole chemical interactions at
stake. WRI researchers proposed that HL acts as an inhibitor for the oxidation catalysts naturally
present in the bitumen (Petersen et al., 1987; Plancher et al., 1976). This was in part validated
by Johansson et al. (1996) (KTH), who showed that the catalytic effect of vanadium compounds
on bitumen ageing was decreased in the presence of HL, although they could not highlight any
specific vanadium–HL interactions.
In all cases, the intensity of HL–bitumen interactions depends on bitumen chemistry and
therefore on bitumen crude source (Huang et al., 2002; Lesueur & Little, 1999; Petersen et al.,
1987; Plancher et al., 1976; Verhasselt & Puiatti, 2004). As a result, these interactions have two
consequences:

• First, the polar molecules neutralised by the HL remain strongly adsorbed onto the HL
particles (Little & Petersen, 2005; Petersen et al., 1987; Plancher et al., 1976). This prevents
them from further reacting as a consequence of bitumen chemical ageing. Since they are
especially prone to ageing, their removal generates an overall slower ageing kinetics.
• Second, the polar molecules that are neutralised by the HL particles are also prevented
from diffusing to the bitumen–aggregate interface. As a consequence, only the remain-
ing non-acidic surfactants of the bitumen can move to the bitumen–aggregate interface
(Bagampadde et al., 2004; Stuart, 1990). These other surfactants are typically amine based
(Durrieu, 1977) and are not easily displaced by water, unlike anionic surfactants (Curtis
et al., 1993; Stuart, 1990). This effect is confirmed by the observation that putting the HL
directly inside the bitumen improves the moisture resistance of the corresponding asphalt
mixtures (Huang et al., 2005).

As a conclusion, the chemical interactions between HL and the acidic moieties of the bitumen
contribute to both the improved ageing resistance and the improved adhesion of HL-modified
mixes.

3.2.2. Physical interaction with the bitumen

As has been described earlier, HL has more voids in a dry compacted state (Rigden air voids) than
mineral fillers, with 65% being a typical value when compared with 30%–34% for mineral fillers
(see Section 2.2). The difference comes from the higher porosity of the HL particles (Figure 5):
for a mineral filler, the porosity essentially comes from the voids between the particles. For HL,
the porosity inside the particles sums up to the porosity between the particles, hence leading to a
much higher value.
It is well known in suspension rheology that the increase in the viscosity of a liquid upon
the addition of solid particles is mainly governed by the volume fraction of the solid particles
(Coussot, 2005; see also Lesueur, 2009, for a review of suspension rheology in the context of
bituminous materials): the higher the volume fraction of the solid particles, the higher the viscosity.
More precisely, the viscosity increases more rapidly when approaching the point where all the
particles are blocked by the contacts with each other, that is, the maximum packing fraction
of the solid particles. This explains, therefore, why the dry porosity of the filler is related to
its stiffening behaviour in bitumen. As a consequence, Rigden air voids correlate well with the
stiffening power as measured by the delta ring and ball test, as illustrated in Figure 6 using
data from two studies, one by the Belgian Road Research Center (BRRC – Vansteenkiste &
 Road Materials and Pavement Design 11

Figure 5. The difference in the dry porosity of HL (right) and that of a mineral filler (left). The dry porosity
of HL is higher than that of the mineral filler because the porosity inside the particles, which is negligible in
the mineral filler, sums up to the porosity between the particles.

40
stiffening effect (delta R&B - °C)

35
y = 1.2375x - 32.385
R2 = 0.95
30

25
BRRC study
Univ. Poznan study
20

15

10
30 35 40 45 50 55 60
dry porosity of the filler (Rigden air voids - %)
Figure 6. The correlation of the stiffening effect of several fillers with their dry porosity (Rigden air voids).
Data are from Vansteenkiste and Vanelstraete (2008) (BRRC), and Grabowski et al. (2009) (University
Poznan).

Vanelstraete, 2008) and the other by the Poznan University of Technology (Grabowski et al.,
2009).
Therefore, the stiffening effect of HL at a high temperature can be explained, at least partially,
by the higher porosity as captured by the high Rigden air void values.
Note that the build-up of the stiffening effect of HL is not immediate. It was observed that
several hours at 138◦ C were needed for one bitumen (known as AAM in the Strategic Highway
Research Program SHRP library) to develop a strong stiffening effect when modified with HL,
whereas it was almost instantaneous at the same temperature for another bitumen (known as
AAD in the SHRP library) (Figure 7 – Lesueur & Little, 1999). The kinetics of this process might
explain, at least partially, why the stiffening of HL is not observed always when asphalt mixtures
are tested.
Therefore, it can be concluded that the physical effect of HL essentially lies in its porosity,
which generates a higher stiffening effect than that of normal mineral fillers, as captured by the
Rigden air void test. However, the contribution to the stiffening effect coming from a possible
adsorbed layer of bitumen components onto the HL particles remains to be quantified.
12 D. Lesueur et al.

4
viscosity ratio

AAD + 20wt.% HL
AAM + 20wt.% HL

1
0 20 40 60 80 100 120 140
time (min)
Figure 7. The kinetics of viscosity build-up at 138◦ C for two bitumens modified with 20% HL. The
viscosity stabilises quickly for AAD when it keeps increasing after 120 min for AAM. The neat bitumen did
not show any significant viscosity change in the mean time.
Source: Plotted from data in Lesueur & Little (1999).

Finally, the high stiffening effect observed with HL at a high temperature disappears below
room temperature. This was first observed for three different bitumens in a joint study between
Esha (Groningen, the Netherlands) and the French Central Laboratory of Roads and Bridges
(Laboratoire Central des Ponts et Chaussées – Figure 8 – Wortelboer, Hoppen, Ramond, & Pastor,
1996). Later studies confirmed the fact that the stiffening effect of HL is temperature dependent,
with a behaviour similar to that of a mineral filler below room temperature but more effective above
it (Hopman et al., 1999; Khattak & Kyatham, 2008; Lesueur & Little, 1999; Pilat, Radziszewski,
& Kalabiska, 2000; Sebaaly et al., 2006). This was further evidenced in low-temperature studies,
showing that HL is similar to other mineral fillers in terms of stiffening effect at a low temperature
(Johansson & Isacsson, 1998; Lackner, Spiegl, Blab, & Eberhardsteiner, 2005).
No interpretation has been proposed so far, and it could be a consequence of the mechani-
cal contrast between the bitumen–swollen HL particles and the bituminous matrix. At a high
temperature, the internal pores of the HL particles are filled with bitumen, and this filled parti-
cles are seen as hard spheres in the bitumen matrix, therefore increasing the volume fraction as
explained earlier. The relevant volume fraction controlling the stiffening effect is therefore that
of the bitumen-filled hydrated lime particles (BFHLPs). Below room temperature, the BFHLPs
start to become deformable, and the mechanical contrast diminishes between the matrix and the
inclusions. Therefore, the system tends to behave as a function of the true volume fraction of the
solid instead of that of the BFHLPs.

4. Conclusions
Over the past 40 years, HL has become a key additive for asphalt mixtures, with a strong presence
in the USA and a growing use in Europe (Lesueur, 2010). It is now seen as a multifunctional
additive that increases the durability of asphalt mixes through its improvement of (Lesueur, 2010;
Little & Epps, 2001; Little & Petersen 2005; Sebaaly 2007; Sebaaly et al., 2006)

• the resistance to moisture damage and frost;

• the resistance to chemical ageing; and
 Road Materials and Pavement Design 13

1E+12

1E+11
70/100 + active filler
1E+10 70/100 + limestone
70/100
1E+09
1/J" (Pa)

1E+08

1E+07

1E+06

1E+05

1E+04

1E+03
–40 –20 0 20 40 60 80
Temperature (°C)
Figure 8. The comparison of the temperature dependence of the stiffening effect of HL and that of the
stiffening effect of a limestone filler: inverse of the imaginary compliance (1/J") at 10 rad/s versus temperature
for a 70/100 bitumen and the same bitumen with 50 wt.% of a limestone filler or an active filler (limestone
filler containing 40% HL).
Source: Wortelboer et al. (1996).

• the mechanical properties, in particular, modulus, strength, rutting resistance, fatigue and
thermal cracking.

The way HL is beneficial to asphalt mixtures can be explained by different mechanisms:

• aggregate modification, which includes surface precipitation of calcium ions and clay
flocculation; and
• bitumen modification, which includes an acid–base neutralisation of the acidic moieties of
the bitumen by the (basic) HL and a physical effect due to its high porosity.

The modification of the surface properties of the aggregate, thanks to the presence of calcium
ions, explains an improved bitumen–aggregate adhesion. Still, the chemical interactions with the
bitumen, due to the basic character of HL, also result in the improvement of the adhesive properties.
The neutralisation of the “bad” adhesion promoters originally present inside the bitumen, through
the formation of water-insoluble calcium salts, explains this effect.
Then, this neutralisation also results in the slowing down of the age hardening kinetics, because
these compounds would otherwise be very likely to oxidise further.
Finally, the physical effect on the bitumen, arising from the high porosity of HL, explains a
stronger stiffening effect on bitumen than that exhibited by mineral fillers above room temperature.
For all these reasons, the interactions between HL and the other components of asphalt mix-
tures are quite intense, explaining the improvement in properties as diverse as moisture damage
resistance, ageing resistance and mechanical properties.
Still, some theoretical aspects remain to be better understood, in particular, the temperature
dependence of the stiffening effect of HL on the bitumen and a detailed description of the
modification of the aggregate surface after HL treatment.
14 D. Lesueur et al.

Regarding the first topic, a proper theoretical framework might explain why some fillers develop
temperature-dependent stiffening effects. If the case of HL is presented at length in this paper, ultra-
fine particles can also be seen to exhibit a similar behaviour (Delaporte, Di Benedetto, Chaverot,
& Gauthier, 2009) and a common explanation might be found.
As far as the second topic is concerned, appropriate analytical methods may confirm in situ
the existence of the adsorbed layer and the details of the modification of aggregate surface,
thanks to HL addition. Although nuclear magnetic resonance spectroscopy, matrix-assisted laser
desorption/ionisation and atomic force microscopy might be ideal candidates, it is not yet clear
whether the right technology is available.

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