A preliminary investigation into the physical and chemical properties

of biomass ashes used as aggregate llers for bituminous mixtures

Roberto Melotti
a,
, Ezio Santagata
a
, Marco Bassani
a
, Milena Salvo
b
, Stefano Rizzo
b
a
Department of Environment, Land and Infrastructure Engineering, Politecnico di Torino, 24 corso Duca degli Abruzzi, 10129 Turin, Italy
b
Department of Applied Science and Technology, Politecnico di Torino, 24 corso Duca degli Abruzzi, 10129 Turin, Italy
a r t i c l e i n f o
Article history:
Received 8 September 2012
Accepted 17 May 2013
Available online 19 June 2013
Keywords:
Biomass ash
Waste management
Filler
Bituminous mixtures
Leachability
a b s t r a c t
Fly and bottom ashes are the main by-products arising from the combustion of solid biomass. Since the
production of energy from this source is increasing, the processing and disposal of the resulting ashes has
become an environmental and economic issue. Such ashes are of interest as a construction material
because they are composed of very ne particles similar to llers normally employed in bituminous
and cementitious mixtures. This research investigates the potential use of ash from biomass as ller in
bituminous mixtures. The morphological, physical and chemical characteristics of 21 different ashes
and two traditional llers (calcium carbonate and recovered plant ller) were evaluated and discussed.
Leaching tests, performed in order to quantify the release of pollutants, revealed that ve ashes do not
comply with the Italian environmental re-use limits. Experimental results show a wide range of values
for almost all the investigated properties and a low correlation with biomass type in terms of origin
and chemical composition. Furthermore, sieving and milling processes were found to improve the prop-
erties of the raw material in terms of grading and sample porosity. The effectiveness of these treatments
and the low content of organic matter and harmful nes suggest that most of the biomass ashes inves-
tigated may be regarded as potential replacements for natural ller in bituminous mixtures.
2013 Elsevier Ltd. All rights reserved.
1. Introduction
European Directive 2009/28/CE denes biomass as the biode-
gradable fraction of products, waste and residues from biological
origin from agriculture (including vegetal and animal substances),
forestry and related industries including sheries and aquaculture,
as well as the biodegradable fraction of industrial and municipal
waste. It is essentially any organic matter which contains stored
solar energy and can, therefore, be used as an energy source. In this
context, fossil fuels are not considered to be biomass.
The production of energy deriving from biomass combustion
and consequent generation of its by-products is increasing world-
wide: in Italy, in 2009, the gross domestic consumption from solid
biomass combustion was 4.1 Mtoe, with this gure being a 5% and
a 75% increase on the consumption gures for 2008 and 2000
respectively (ENEA, 2009).
Fly and bottom ashes represent the main residues of a combus-
tion process: they are composed of mineral materials (in their oxi-
dised form) absorbed by the biomass during its lifecycle or
incorporated during harvesting and of a small quantity (up to
20%) of unburned organic matter. The amount of ashes produced
depends on combustion chamber conditions and biomass type,
with values that vary between 2% (i.e. woodchips) and 20% (i.e. rice
husk). Bottom ashes, which settle under the grate of the combus-
tion chamber, are the coarsest and heaviest constituent part of
the combustion by-products, while y ashes, which remain sus-
pended in the ue gases, are the nest part. Fly ashes represent
up to 40% of the total ashes produced and are usually removed
through electrostatic precipitators and fabric-lter baghouses.
The recycling of biomass ashes as construction materials meets
the recommendations of the European Directive on waste 2008/98/
CE and has signicant environmental benets related to the de-
crease in the quantity of natural aggregates extracted from quar-
ries and to the reduction of waste carried to landlls. In Italy,
since the European Waste Catalogue (European Commission Deci-
sion 2000/532/CE) classies waste from biomass combustion as a
non-hazardous material, a simplied procedure (Regulation DM
05/02/98), requesting a communication of intent rather than a sub-
mission for formal authorisation for recycling these types of ashes,
is sufcient. According to this regulation, biomass ashes can only
be recycled in concrete, cement and brick production, in embank-
ment construction and environmental re-use, but not in other
applications such as the production of bituminous mixtures. In this
case, the usual authorisation procedure is required. In Italy, as a
result of legal constraints, the majority of these ashes are taken
0956-053X/$ - see front matter 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.wasman.2013.05.015

Corresponding author. Tel.: +39 011 090 5622; fax: +39 011 090 5614.
E-mail addresses: roberto.melotti@polito.it (R. Melotti), ezio.santagata@polito.it
(E. Santagata), marco.bassani@polito.it (M. Bassani), milena.salvo@polito.it
(M. Salvo), stefano.rizzo@polito.it (S. Rizzo).
Waste Management 33 (2013) 19061917
Contents lists available at SciVerse ScienceDirect
Waste Management
j our nal homepage: www. el sevi er. com/ l ocat e/ wasman
to landlls, involving considerable transportation, processing and
disposal costs. Their re-use in bituminous materials could make a
signicant contribution to a reduction in ash disposal costs when
one considers that 34.9 million tons of bituminous mixtures were
produced in Italy in 2009 (EAPA, 2009).
Bituminous mixtures are basically composed of aggregates of
different sizes, ller and bitumen. Fillers are mineral grains most
of which pass at 63 lm sieve (EN 13043), and represent 510% of
the aggregates by weight in the whole mixture. Filler can have a
natural origin when derived from the crushing of rocks, or can be
manufactured in industry as in the case of lime, cement, ash and
slag. Although its main function is lling the voids in the aggregate
skeleton to create a denser mixture, several studies have demon-
strated that ller has other important roles. Depending on its par-
ticle size and structure, it stiffens and/or extends the binder
(Kandhal and Parker, 1998; Grabowski and Wilanowicz, 2008),
consequently affecting the occurrence of rutting and fatigue phe-
nomena. Furthermore, ller also modies the ageing processes
(Gubler et al., 1999; Recasens et al., 2005) and its nest part may
act as an anti-stripping agent preventing moisture damage (Kand-
hal and Parker, 1998).
Although its importance is well recognised, most recent regula-
tions on ller for bituminous mixtures (EN 13043, ASTM D242,
AASHTO M17) establish limits for only a few characteristics such
as grading, water content, plasticity index and organic content. In
addition, the Superpave volumetric mix design system (Cominisky
et al., 1994) denes a limit for the quantity of ller in the mixture
(corresponding to a ller/binder ratio in the range 0.61.2 by
weight). The above mentioned characteristics are necessary pri-
marily for quality control, but are not sufcient to obtain informa-
tion correlated with the expected performance of bituminous
mixtures. This is even more evident for manufactured llers, like
biomass ashes, which often exhibit unique behaviours.
The study described in this paper is part of RICCO, a 3-year re-
search project nanced by the Italian Ministry of Agricultural, Food
and Forestry Policies which aims to investigate the possible re-use
of biomass ash as ller in bituminous mixtures. In particular, the
goal of the rst part of the project is to characterise several ashes
from biomass combustion by integrating the tests included in the
technical standards on ller for bituminous mixtures EN 13043,
with those tests that ongoing research has identied as reliable
performance indicators. Furthermore, since it is important to sub-
stantiate the hazardous nature of ashes, their environmental im-
pact can be assessed by the European regulation EN 12457-2 on
the evaluation of leaching potential.
2. Background
Several studies have been carried out in recent years to assess
the possible re-use of biomass ash and its recycling as a substitute
for aggregates in concrete mixtures (Martin Morales et al., 2011), in
cement production (Ajiwe et al., 2000), and also as a fertilizer (In-
sam and Knapp, 2011). In road applications, due to its cementing
and pozzolanic properties, most of the researches focused on the
recycling of biomass ash in soil stabilization (Basha et al., 2005;
Nordmark et al., 2011). The recycling of biomass ashes as ller in
bituminous mixtures has been studied in The Netherlands: an
extensive study led by the Energy Research Centre of The Nether-
lands (Pels et al., 2006) showed that y ashes from the gasication
of solid biomass are a valuable alternative to natural llers. Sarabr
and Haasnoot (2012) investigated the physical and chemical char-
acteristics of several y ashes derived from the combustion of dif-
ferent solid biomasses. Their experimental results indicated that
most of the ashes do not meet the requirement for passing 125
and/or 63 lm, concluding that, due to their gradation, biomass
y ashes can compete more with Municipal Solid Waste
Incinerator y ash and sewage sludge ash than coal y ash when
recycled as ller in bituminous mixtures. Unfortunately, the phys-
icalmechanical properties of ashbitumen mastics, slurries or
mixtures were not investigated. Moreover, the investigation by
Sarabr and Haasnoot (2012) does not take into account the fact
that characteristics like gradation, water solubility and soundness
are insufcient for an assessment of the use of biomass ashes as l-
ler in bituminous mixtures, as clearly indicated in the present
paper.
The majority of the studies concerning the possible re-use of
ashes as ller in bituminous mixtures investigate the behaviour
of y and bottom ash derived from coal combustion. A great quan-
tity of ash (2030% of the original matter) is produced from this
combustible which still represents the most widespread energy
source in many countries. In the European Union (EU 15) 61 mil-
lion tons of coal combustion products were produced in 2006
(European Coal Combustion Products Association, 2006), while in
the US 125 million tons were produced in 2009 (American Coal
Ash Association, 2009). Kavussi and Hicks (1997) evaluated the
properties of bituminous mixtures containing four different llers
(limestone, quartz, coal y ash, kaolin): they found that mastics
containing y ash were more susceptible to brittle failure because
of their high porosity, caused by the presence of very small air bub-
bles formed during the burning process. Sharma et al. (2010) dem-
onstrated that coal y ash having high calcium content exhibits
anti-stripping properties. In order to avoid excessive stiffening of
bituminous mixtures, they suggested a maximum value of 60%
for the ratio between bulk volume of compacted ller and total l-
lerbitumen volume. This study also showed that high values for
clay content in the ash, as revealed by the Methylene Blue (MB)
test, were correlated to low tensile strength ratio and retained sta-
bility values, proving that this test can also provide a good estimate
of moisture susceptibility.
In recent years the National Cooperative Highway Research Pro-
gram Project 9-45 (NCHRP, 2010) was developed in order to ad-
dress the theme of ller role in bituminous mixtures. The study
considered 32 different llers for which the effect on bituminous
mixture performance was thoroughly investigated. Out of the total
set of analysed llers, three were y ashes collected from coal com-
bustion plants. The research identied fractional voids, size distri-
bution, content of calcium compound and active clay content as
the most relevant properties for the characterisation of llers.
Compared to mineral llers routinely used for paving applications,
the properties of y ash encompassed a wider range of values. As a
consequence, the prediction model developed to estimate mastic
properties from ller characteristics was applicable only to natural
llers. The study concluded that manufactured llers have a un-
ique inuence on mastics and mixtures, with this effect requiring
a more detailed investigation.
Although coal ash is the one most studied, many investigations
deal with the possible re-use of other ashes in bituminous mix-
tures. Xue et al. (2009) investigated the effects of Municipal Solid
Waste Incinerator (MSWI) ash on Stone Mix Asphalt (SMA). The
use of 16% of MSWI ash meets the requirements of Marshall and
Superpave mix design procedures. However, the ash lowers the
water damage resistance of the mixtures due to its low CaO con-
tent causing poor adhesiveness between asphalt and ash. Hassan
et al. (2007) studied the effect of replacing 03 mm natural aggre-
gates with up to 40% of MSWI ash in bituminous mixtures: the
Marshall mix design showed that optimum asphalt content in-
creased signicantly as more ash was introduced into the mix, ow-
ing to the high absorption properties of the ash.
One solution to the problem of this increasing absorption of
binder is represented by vitrication. Bassani et al. (2009) studied
a bituminous mixture in which up to 32.5% of 02 mm natural
R. Melotti et al. / Waste Management 33 (2013) 19061917 1907
sand was replaced with vitried MSWI ash: they concluded that,
due to the glassy surface of ash, a smaller percentage of bitumen
can be used to reach given target values for mechanical and volu-
metric properties.
3. Materials and test methods
3.1. Materials
The ashes used in this study were collected from 12 different
power plants, eleven in Italy and one in Sweden. Two different
combustion technologies are adopted in the plants: moving grate
and uidized bed. The ashes are the by-products of several differ-
ent combustibles including woodchips, shells, rice husk, refuse de-
rived fuel, straw, bark and sludge. In one plant (Strongoli) the y
ashes are stored in silos and are not mixed with the bottom ashes,
while in the other eleven plants the two types of ashes are mixed
and stored in the same containers. As a result, in the investigation
bottom ash (BA), y ash (FA) and a mix of bottom and y ash (FBA)
have been studied (Table 1).
The ashes, 21 in total, were collected in two different periods
(April and December 2010) in order to evaluate the variability of
their properties over a production period of about 7 months. Those
ashes having most of their particles coarser than 125 lm were pro-
cessed for 1 h in a laboratory mill with a tungsten sphere: as a re-
sult, the total number of ashes to be tested increased to 27. Table 1
reports the complete list of ashes considered in this investigation;
the rst digit of the identication code refers to the sampling per-
iod (1 for April 2010, 2 for December 2010); the central part of the
code identies the power plant, while the last letter indicates the
type of laboratory processing (milled or not). In order to compare
the characteristics of the ashes to reference llers, a calcium
carbonate ller (CaCO
3
) and a recovered ller collected from an
bituminous mixture plant (code FR) were also included in the
study. In the last column of Table 1 the European Waste Catalogue
code for each sample is provided.
A standard 70/100 penetration unmodied bitumen was used
for the laboratory production of llerbitumen mastics since it
has characteristics which are typical for the bitumens commonly
used in Italy. In addition, the rheological properties required in
the Superpave mix design (Cominisky et al., 1994) are reported
in Table 2, indicating that the selected bitumen has a Performance
Grade equal to 58-16 (Strategic Highway Research Program A-370,
1994).
3.2. Test methods
The test plan was established in order to assess the physical and
chemical characteristics of the ashes according to the international
standard on ller for bituminous mixtures EN 13043. Grading
(investigated by sieve analysis), water content (EN 1097-5), harm-
ful nes (EN 933-9), particle density (EN 1097-7), voids of dry com-
pacted ller (EN 1097-4), variation in Ring and Ball temperature
(EN 13179-1) and water solubility (EN 1744-1) were evaluated.
Ring and Ball tests were performed only on the rst stock of
ashes (April 2010) since the majority of the mastics created with
a ller/bitumen volume ratio equal to 0.6 (EN 13179-1) were not
soft and sufciently homogeneous to be tested. EN 13043 pre-
scribes limits only for the percentage of material passing at
2000 lm (P2000), 125 lm (P125), 63 lm (P63) sieves and water
content (Table 3), while for the other characteristics only a classi-
cation into different categories is provided.
The literature review indicated that an evaluation of the above-
mentioned ller properties is useful for quality control, but is not
Table 1
Fillers considered in the laboratory investigation.
Identication code Power plant location Combustion technology Combustible Ash type European waste catalogue code
1-TO1-N Chieri (IT) Moving grate Woodchips FBA
b
100103
2-TO1-N Chieri (IT) Moving grate Woodchips FBA 100103
1-AO1-M Morgex (IT) Moving grate Woodchips FBA 100103
2-AO1-N Morgex (IT) Moving grate Woodchips FBA 100103
1-AO2-N Pollein (IT) Moving grate Woodchips FBA 100103
2-AO2-N Pollein (IT) Moving grate Woodchips FBA 100103
1-AO3-N Pr S. Didier (IT) Moving grate Woodchips FBA 100103
2-AO3-N Pr S. Didier (IT) Moving grate Woodchips FBA 100103
1-AO3-M Pr S. Didier (IT) Moving grate Woodchips FBA 100103
2-AO3-M Pr S. Didier (IT) Moving grate Woodchips FBA 100103
1-TO2-N Torino (IT) Moving grate Woodchips FBA 100103
2-TO2-N Torino (IT) Moving grate Woodchips FBA 100103
1-TO2-M Torino (IT) Moving grate Woodchips FBA 100103
1-SO-N Sondrio (IT) Moving grate Woodchips FBA 100103
2-SO-N Sondrio (IT) Moving grate Woodchips FBA 100103
1-KR1-N Strongoli (IT) Fluidized bed Woodchips and shells FA
c
100103
2-KR1-N Strongoli (IT) Fluidized bed Woodchips and shells FA 100103
2-KR1-M Strongoli (IT) Fluidized bed Woodchips and shells FA 100103
1-KR2-N Strongoli (IT) Fluidized bed Woodchips and shells BA
d
100101
2-KR2-N Strongoli (IT) Fluidized bed Woodchips and shells BA 100101
1-KR2-M Strongoli (IT) Fluidized bed Woodchips and shells BA 100101
2-KR2-M Strongoli (IT) Fluidized bed Woodchips and shells BA 100101
1-PV-M Pavia (IT) / Rice husk, wood, RDF
a
FBA 190114
1-SW-M Lidkping (SE) Moving grate Straw FBA /
1-VC-M Vercelli (IT) Moving grate Rice husk FBA /
2-TH-N La Thuile (IT) Moving grate Woodchips FBA 100103
2-VZ-N Verzuolo (IT) Fluidized bed Barks and sludge FBA 190114
CaCO
3
Trino vercellese (IT) / / Natural ller /
FR Torino (IT) / / Plant ller /
a
RDF: refuse derived fuel
b
FBA: y and bottom ash
c
FA: y ash
d
BA: bottom ash
1908 R. Melotti et al. / Waste Management 33 (2013) 19061917
sufcient for an accurate prediction of the performance of bitumi-
nous mastics and mixtures (NCHRP Project 9-45, 2010; Faheem
et al., 2010; Wang et al., 2011). For this reason additional tests
were conducted in order to obtain a more comprehensive charac-
terisation of the ashes.
Following the guidelines of NCHRP Project 9-45 (2010), the
chemical composition and the organic content of the ashes were
evaluated, by means of X-ray uorescence and LOI tests (AASHTO
T 267-86) respectively. In order to extend the grading analysis per-
formed with 2000, 125 and 63 lm sieves, that part of the material
with a particle size ner than 125 lm was investigated by a sedi-
mentation process using a hydrometer (ASTM D422-63). The ne-
ness modulus (FM), calculated by dividing the sum of the
percentages of material coarser than 75, 50, 30, 20, 10, 5, 3, and
1 lm by 100, was used to synthetically express the results.
With the aim of evaluating whether the ashes are hygroscopic,
each specimen was conditioned for 24 h at 20 C and 75% relative
humidity and then dried for a further 24 h at 40 C. The difference
in weight between the two stages represents the water adsorbed
during the conditioning period. Furthermore, since previous stud-
ies showed that biomass ashes have an irregular shape (Sforza
and Moriconi, 2005), the particle shape was evaluated through
Scanning Electron Microscopy (SEM).
Finally, since ashes may be classied as hazardous or non-haz-
ardous waste in the European Waste Catalogue (Table 1), their
Table 2
Rheological properties of the unmodied bitumen.
Ageing condition Temperature (C) Rheological characteristic
Unaged T = 135 h = 188 mPa s
T = 58.1 G

/sind = 1000 Pa
RTFO T = 64.1 G

/sind = 2200 Pa
PAV T = 18.9 G

sind = 5000 kPa

T = 18.8 S = 300 MPa
T = 7.6 m-Value = 0.300
Table 3
EN 13043 requirements on ller.
Specication EN 13043
Grading P2000 = 100% P125 > 85% P63 > 70%
Water content <1%
Limit on P2000
Limit on P125
Limit on P63
0
10
20
30
40
50
60
70
80
90
100
0.01 0.1 1 10
P
a
s
s
i
n
g

(
%
)
Sieve size [mm]
1-TO1-N
1-AO1-M
1-AO2-N
1-AO3-N
1-AO3-M
1-TO2-N
1-TO2-M
1-SO-N
1-KR1-N
1-KR2-N
1-KR2-M
1-PV-M
1-SW-M
1-VC-M
FR
Fig. 1. Experimental results of sieve analysis on the rst stock of ashes in their original state.
Limit on P2000
Limit on P125
Limit on P63
0
10
20
30
40
50
60
70
80
90
100
0.01 0.1 1 10
P
a
s
s
i
n
g

(
%
)
Sieve size [mm]
2-TO1-N
2-AO1-N
2-AO2-N
2-AO3-N
2-AO3-M
2-TO2-N
2-SO-N
2-KR1-N
2-KR1-M
2-KR2-N
2-KR2-M
2-TH-N
2-VZ-N
FR
Fig. 2. Experimental results of sieve analysis on the second stock of ashes in their original state.
R. Melotti et al. / Waste Management 33 (2013) 19061917 1909
environmental impact was assessed by means of leaching tests (EN
12457-2) and consequent chemical and pH analyses. Results were
compared with the Italian limits for environmental re-use (D.M.
05/04/2006 n. 186) and landll disposal in dumps for non-hazard-
ous materials (D.M. 27/09/2010). Due to the high costs associated
with leaching tests and SEM analysis, these tests were conducted
only on the rst stock of ashes (April 2010).
4. Results and data analysis
4.1. Geometrical and physical characteristics
4.1.1. Size distribution
The small dimension of ller particles is a requisite for lling
the aggregate matrix of bituminous mixtures and for creating a
strong chemical interaction with the binder. The experimental re-
sults of sieve analysis on ashes in their original state (Figs. 1 and 2)
show that all the ashes, with the exception of 1-SO-N, fail to re-
spect the EN 13043 limits on grading. The results also indicate that
the performed milling process is not sufcient to obtain the grada-
tion required by EN13043.
Sieving the raw material seems the most appropriate solution
to the problem of meeting the EN 13043 requirement. The results
reported in Fig. 3 prove that it is not sufcient to eliminate the par-
ticles coarser than 125 lm, since most of the ashes do not respect
the limits on passing at 63 lm. As a result, in order to satisfy this
last requirement, each ash has to be processed with a specic sieve
which ensures that at least 70% of the particles are ner than
63 lm.
In Table 4, the percentage of material passing at 75 (P75) and
20 lm (P20), and the neness modulus (FM) on the material ner
than 125 lm are provided. With the exception of 2-TO1-N, all the
ashes have neness modulus values greater than the reference ll-
ers, showing that a limited amount of very ne particles is present
in the ashes. This observation is coherent with the percentage of
material ner than 20 lm, which is lower than 30% for 20 ashes
out of 25. 2-KR1-N and 2-KR2-N had insufcient quantities of
material ner than 125 lm to be tested, hence in Table 4 the re-
sults are indicated with the label N/A (not available).
4.1.2. Rigden voids (EN 1097-4)
Rigden voids (RV) represent the porosity measured on a com-
pacted sample of ller, estimated on those particles ner than
125 lm. RV provide information on the ller absorption potential
of binder and they are, therefore, an indicator of the stiffening
power that ller has on bitumen (Faheem et al., 2010). Hence,
llers with high RV values are not desirable in bituminous mix-
tures because they can stiffen the mixture to an excessive degree.
The experimental results show that almost all the RV values of the
considered ashes are greater than those for reference llers (Fig. 4).
Although there is no acceptance limit on RV values in the EN
13043, ASTM D242 and AASHTO M17 international standard of
llers in bituminous mixtures, the traditional range of use lies
between 25% and 50%. The American Coal Ash Association (2003)
suggests a maximum value of 50%, while the 139/92 Italian
National Research Council standard requires that the RV fall into
the range 3045%. Fig. 4 indicates that, although the RV for most
0
10
20
30
40
50
60
70
80
90
100
P
a
s
s
i
n
g

(
%
)
P63
EN 13043 limit on P63
Fig. 3. Experimental results of sieve analysis on ash particles ner than 125 lm.
Table 4
Results of the sedimentation process on ash particles ner than 125 lm.
P75 P20 FM
Measurement unit % % /
1-TO1-N 83.9 25.2 5.77
2-TO1-N 93.6 52.0 5.13
1-AO1-M 71.0 19.6 6.23
2-AO1-N 82.7 45.2 5.43
1-AO2-N 86.1 55.7 5.20
2-AO2-N 80.2 27.6 5.77
1-AO3-N 77.0 26.3 5.91
2-AO3-N 72.8 14.7 6.02
1-AO3-M 62.2 0.0 7.01
2-AO3-M 84.7 12.4 5.99
1-TO2-N 75.6 15.4 6.04
2-TO2-N 64.3 0.0 6.61
1-TO2-M 70.5 7.7 6.49
1-SO-N 87.9 26.5 5.61
2-SO-N 74.1 21.0 6.00
1-KR1-N 64.3 15.9 6.40
2-KR1-N N/A N/A N/A
2-KR1-M 89.2 25.7 5.57
1-KR2-N 6.8 0.0 7.93
2-KR2-N N/A N/A N/A
1-KR2-M 54.3 9.4 6.91
2-KR2-M 75.2 21.8 6.16
1-PV-M 75.3 0.0 6.57
1-SW-M 77.5 28.4 5.88
1-VC-M 56.2 6.1 6.77
2-TH-N 78.7 37.4 5.69
2-VZ-N 76.7 52.5 5.39
CaCO
3
96.6 56.8 4.34
FR 89.1 40.6 5.22
1910 R. Melotti et al. / Waste Management 33 (2013) 19061917
of the ashes are higher than 50%, the milling process performed is
extremely effective in reducing biomass ashes porosity.
4.1.3. Particle shape
The particle shape of the ashes was investigated by means of
Scanning Electron Microscopy (SEM) observations. Unlike coal
combustion ashes, which are generally spherical in shape, all the
analysed samples contain particles with an irregular shape (Figs.
57) which may impact negatively on both the uidity and work-
ability of bituminous mixtures. This conrms the results from pre-
vious studies which demonstrated that biomass ashes have
irregular shapes (Sforza and Moriconi, 2005). The difference in
shape can be attributed to the higher temperature in coal combus-
tion chambers (greater than 1200 C) which allows the lightest
part of the material to melt and then solidify into spheres. This
melting process does not occur during biomass combustion since
the temperature is often less than 900 C.
4.1.4. Water content (EN 1097-5) and hygroscopy
Since ash is a residue of a combustion process, water content
should be low. The results displayed in Fig. 8 indicate that, in this
investigation, the exceptions are represented by 2-KR1-N and
65
66
60
58
57
50
61
51
52
57 59
33
44
55
48
61
70
44
35
36
43
71
73
41
36
47
61
0
10
20
30
40
50
60
70
80
90
R
i
g
d
e
n

v
o
i
d
s

(
%
)
Not milled ash
Milled ash
Traditional range of use
Italian National Research Council 139/92 limits
Fig. 4. Experimental results for Rigden voids on ash particles ner than 125 lm.
Fig. 5. 1-AO1-N biomass ash.
Fig. 6. 1-SO-N biomass ash.
Fig. 7. 1-KR2-N biomass ash.
R. Melotti et al. / Waste Management 33 (2013) 19061917 1911
2-KR1-M. They revealed high water content values due to the plant
process, in which a water treatment is used with the aim of
reducing the quantity of dust released into the environment.
1-SO-N, 1-KR1-N, 1-SW-M, 1-VC-M and 1-PV-M also exceed the
EN 13043 limit (water content lower than 1%). In all these cases
the presence of water could be caused by exposure to a humid
environment during storage and transportation or by the slightly
hygroscopic surface of the ashes (Fig. 8).
4.1.5. Ring and ball variation (EN 13179-1)
The Ring and Ball test consists of evaluating the softening tem-
perature onset of a circular specimen of bitumen under constant
load application and a positive temperature gradient. When
the test is performed both on the neat bitumen and on the ller
bitumen mastic, the difference between these two temperatures
(DR&B) indicates the stiffening power of the ller. The mastic sam-
ples were prepared with a llerbitumen volume ratio equal to 0.6
and by employing only that part of the ller ner than 125 lm. The
calculated softening temperature of the neat bitumen is equal to
44.9 C. From Table 5 it can be seen that the ashes increase the
bitumen softening point to different degrees with values falling
in a range between those for the reference ller. Furthermore,
the majority of the ashes created mastics that were not homoge-
neous, thus impossible to pour and test. This is the reason why
the test was performed only on the rst stock of ashes (April 2010).
4.1.6. Particle density (EN 1097-7)
The results reported in Table 6 show a wide range of particle
density values from 2.18 to 3.13 g/cm
3
. This is primarily caused by
the different densities of y and bottom ashes which are both pres-
ent in different percentages in each sample (except KR1 and KR2)
and secondly by the variable chemical composition of the ashes.
4.2. Chemical characteristics
4.2.1. Methylene blue test (EN 933-9)
The objective of this test is to investigate the presence of clay in
llers. Clay minerals are crystalline hydrated alumino-silicates
which, due to their charged surface and ability to exchange cations,
adsorb methylene blue (a cationic dye) from an aqueous solution.
0
2
4
6
8
10
12
14
16
18
20
22
24
26
28
30
32
34
W
a
t
e
r

c
o
n
t
e
n
t

(
%
)
EN 1097-5 test
Hygrometry test
EN 13043 water content limit
Fig. 8. Experimental results of water content.
Table 5
Experimental results of Ring and Ball test performed on ller/bitumen mastics.
Mastics Ring & Ball D R&B
Measurement unit C C
1-TO1-N Not homogeneous
1-AO1-M 64.5 19.5
1-AO2-N 71.9 27.0
1-AO3-N Not homogeneous
1-AO3-M 63.0 18.1
1-TO2-N Not homogeneous
1-TO2-M 64.3 19.4
1-SO-N Not homogeneous
1-KR1-N Not homogeneous
1-KR2-N N/A N/A
1-KR2-M 59.4 14.5
1-PV-M 70.7 25.8
1-SW-M Not homogeneous
1-VC-M Not homogeneous
CaCO
3
59.5 14.5
FR 75.3 30.3
Table 6
Experimental results of particle density, methylene blue and water solubility.
Particle density MB Water solubility
Measurement unit g/cm
3
g
BLUE
/kg
ASH
%
1-TO1-N 2.94 0.7 0.4
2-TO1-N 2.91 2.0 0.8
1-AO1-M 2.86 0.7 0.7
2-AO1-N 2.72 0.7 1.0
1-AO2-N 3.13 5.3 8.8
2-AO2-N 2.59 4.0 3.5
1-AO3-N 3.08 0.7 2.2
2-AO3-N 2.86 0.7 1.8
1-AO3-M 3.02 1.3 N/A
2-AO3-M 2.90 0.7 2.1
1-TO2-N 3.09 0.7 0.5
2-TO2-N 2.77 0.7 2.6
1-TO2-M 2.95 0.7 1.4
1-SO-N 2.82 2.3 6.6
2-SO-N 2.68 2.0 2.8
1-KR1-N 2.65 0.7 4.0
2-KR1-N 2.60 N/A 1.1
2-KR1-M 2.62 1.3 6.9
1-KR2-N 2.65 N/A 0.0
2-KR2-N N/A N/A N/A
1-KR2-M 2.64 3.0 0.1
2-KR2-M 2.68 1.3 0.0
1-PV-M 2.60 N/A 1.6
1-SW-M 2.51 6.0 10.3
1-VC-M 2.18 5.3 1.4
2-TH-N 2.65 1.3 1.2
2-VZ-N 2.49 1.3 1.2
CaCO
3
2.73 3.0 0.9
FR 2.82 2.3 0.1
1912 R. Melotti et al. / Waste Management 33 (2013) 19061917
Thus, the quantity of methylene blue adsorbed during the test in-
creases in proportion to the quantity of clay present. Clay is harm-
ful for bituminous mixtures, because of its plastic properties and
water retention. The results presented in Table 6 show that all
the ashes have low MB values, hence limited quantities of clay.
4.2.2. Water solubility (EN 1744-1)
Fillers for bituminous mixtures are required to have low solu-
bility in water values to avoid any change in their lling and stiff-
ening effects. The results reported in Table 6 represent the
percentage loss in mass after 24 h of stirring in water. Although
most of the analysed ashes have low water solubility, four of them
show values higher than 6% while only one (1-SW-M) exceeds the
acceptance limit of 10% (Sarabr and Haasnoot, 2012). These losses
in mass may be caused by some organic particles present in the
ashes that bond with the water molecules. The authors decided
not to investigate this phenomenon further as water solubility is
a parameter which is rarely required by international standards
and agencies and whose importance is not clear.
4.2.3. Loss on ignition test (AASHTO T 267-86)
The organic content of the ashes can be evaluated by means of
the Loss On Ignition (LOI) test. The LOI value is determined by the
weight loss in a dry sample of material ner than 2 mm measured
after heating it for 6 h at 455 C. In general, a low LOI value is desir-
able, since it indicates low organic content in the ller. The results
reported in Fig. 9 show that, with the exception of 1-SW-M, all the
ashes have LOI values lower than 12% which corresponds to the
limit specied in AASHTO M17-07.
4.2.4. Chemical composition
X-ray uorescence yielded the chemical composition of the
ashes expressed in terms of the percentage in weight of their oxi-
des. The compositions of the principal components of the rst and
second stock of ashes are shown in Figs. 10 and 11 respectively. It
can be observed that calcium oxide (CaO) is the principal compo-
nent in 13 out of 21 ashes, while silicon dioxide (SiO
2
) is the main
component in 7 out of 21 ashes. The only exception is 1-SW, which
is principally composed of potassium oxide.
4.2.5. Leaching test and pH value (EN 12457-2)
Leaching tests were performed in order to evaluate the release
of pollutants from the biomass ashes. A solution of ashes with par-
ticles ner than 400 lm and distilled water with a liquid to solid
ratio of 10 l/kg was prepared and thereafter continuously stirred
for 24 h. Subsequently, the solution was ltered by means of a
1.0
4.5
0.1 0.1
1.9
2.8
4.7
0.2
4.7
0.2
0.4
0.2
0.4
3.8
0.8
2.2
5.8 5.8
0.1 0.1 0.1 0.1
2.2
12.4
6.0
2.2
0.1 0.2
0.6
0
1
2
3
4
5
6
7
8
9
10
11
12
13
14
L
o
s
s

o
n

i
g
n
i
t
i
o
n

(
%
)Experimental results
AASHTO M17-07 limit
Fig. 9. Experimental results of loss on ignition tests on ash particles ner than 2 mm.
0
10
20
30
40
50
60
70
80
90
100
M
a
s
s

f
r
a
c
t
i
o
n

(
%
)
CaO
K2O
SiO2
SO3
Cl
Fig. 10. Chemical composition of stock 1 (April 2010).
R. Melotti et al. / Waste Management 33 (2013) 19061917 1913
0.45 lm pore size lter and chemical analyses were conducted.
From the results reported in Table 7 it can be seen that the concen-
tration of some of the detected elements exceeds the Italian accep-
tance limits, both for environmental re-use (DM 05/04/2006 n.
186) and landll disposal in dumps for non-hazardous materials
(DM 27/09/2010). This is especially evident for chrome and sul-
phate. Furthermore, from the chemical composition (Fig. 10) it
can be seen that those ashes having the highest SO
3
content
(1-AO2, 1-SO, 1-KR1 and 1-SW) have sulphate leaching values
which exceed the Italian limits for environmental re-use.
The results of pH tests carried out on the eluate of the leaching
test reveal that all the solutions are basic with values in a range
from 11.19 (ash 1-KR2) to 12.99 (ash 1-TO2). It is interesting to
note that most of the ashes have pH values exceeding the Italian
environmental re-use limits, which require values to lie in a range
between 5.5 and 12.
However, in this study leaching tests were performed on the
material in its original state, which does not take into account
the coating effect of bitumen. In fact, within a bituminous mixture,
the binder incorporates the ller and reduces the release of pollu-
tants and pH values, as several studies have demonstrated (Hassan
et al., 2007; Xue et al., 2009). For this reason, when bituminous
mixtures are studied in the nal stage of project RICCO, leaching
tests on mixtures containing the same biomass ashes will be
performed.
5. Discussion
In this section the results are discussed in order to evaluate
the inuence of biomass type and sampling period on ash
characteristics. In addition, the correlation between different ash
properties is investigated.
It was not possible to identify a clear connection between the
type of biomass and ash characteristics: in fact, even when the
combustible is the same (i.e. woodchips), most of the properties
Table 7
Results of leaching tests (values exceeding the environmental re-use limit in light grey, values exceeding the landll disposal limit in dark grey).
0
10
20
30
40
50
60
M
a
s
s

f
r
a
c
t
i
o
n

(
%
)
CaO
K2O
SiO2
SO3
Al2O3
Fig. 11. Chemical composition of stock 2 (December 2010).
1914 R. Melotti et al. / Waste Management 33 (2013) 19061917
exhibit a signicant variability. This is illustrated in Table 8 where
the values for coefcients of variation (CV) are listed both for the
entire set of llers and for woodchip ashes only. When the analysis
is restricted to ashes of the same origin only minor changes in the
CV values are observed.
In order to assess the correlation between all measured proper-
ties, a matrix was constructed as shown in Table 9.
The correlation (0.78) found between DR&B and RV demon-
strates that, as the compacted samples of ashes become more por-
ous, their stiffening power increases (Fig. 12). This is also
conrmed by the fact that in the cases of the ashes with the highest
RV values, the resulting mastic samples were too viscous and dry
to be poured, thereby proving the need to limit the RV value for
acceptance purposes. It should also be noticed that DR&B seems
to be affected by P63 (Table 9), as shown by the high correlation
coefcient (0.90): in fact, llers having approximately the same
RV values have greater stiffening power when they contain a high
quantity of P63 (e.g. FR).
In general, llers with high calcium compounds are more desir-
able, as a result of their stronger interaction with bitumen (Faheem
et al., 2008). Nevertheless, Table 9 shows poor correlation (0.14)
between CaO content and DR&B, meaning that, for these specic
llerbitumen combinations, other characteristics inuence the
stiffening power of the ashes (RV and P63).
The correlation (0.81) between pH and CaO content and the
negative correlation (0.71) between pH and SiO
2
content demon-
strate that pH values depend on the chemical composition of the
ashes. Therefore, pH values could be used as a viable alternative
to the estimate of CaO and SiO
2
content, hence avoiding the use
of expensive techniques such as X-ray uorescence.
In order to investigate the variability of the properties through-
out the year, most of the ashes were collected in two different peri-
ods (April and December 2010). In Table 10 such variability is
Table 9
Correlation matrix of test results (absolute values higher than 0.7 in bold).
P2000 P125 P63 FM RV Water content Particle density D R&B MB LOI pH Water solub. CaO SiO
2
P2000 1.00 0.63 0.50 0.05 0.22 0.56 0.16 0.52 0.23 0.01 0.50 0.12 0.01 0.02
P125 / 1.00 0.95 0.51 0.29 0.24 0.28 0.90 0.09 0.19 0.44 0.27 0.38 0.41
P63 / / 1.00 0.59 0.36 0.21 0.37 0.90 0.06 0.15 0.45 0.23 0.50 0.48
FM / / / 1.00 0.50 0.14 0.20 0.73 0.07 0.15 0.49 0.37 0.45 0.58
RV / / / / 1.00 0.30 0.27 0.78 0.44 0.59 0.11 0.33 0.06 0.08
Water content / / / / / 1.00 0.24 0.52 0.05 0.37 0.30 0.17 0.13 0.08
Particle density / / / / / / 1.00 0.23 0.42 0.29 0.88 0.01 0.64 0.65
D R&B / / / / / / / 1.00 0.57 0.23 0.23 0.73 0.14 0.41
MB / / / / / / / / 1.00 0.61 0.56 0.59 0.51 0.30
LOI / / / / / / / / / 1.00 0.21 0.62 0.33 0.08
pH / / / / / / / / / / 1.00 0.11 0.81 0.71
Water solubility / / / / / / / / / / / 1.00 0.13 0.29
CaO / / / / / / / / / / / / 1.00 0.82
SiO
2
/ / / / / / / / / / / / 1.00
0
5
10
15
20
25
30
35
30 35 40 45 50 55 60 65 70 75 80
Rigden voids (%)
Ashes tested
Reference fillers tested
Ashes impossible to test
R
i
n
g

&

B
a
l
l

[

C
]
Fig. 12. Correlation between Rigden voids and D Ring & Ball.
Table 8
Coefcients of variation (%) of test results.
All ashes Woodchip ashes
Stock 1 Stock 2 Stock 1 Stock 2
P2000 6.1 16.7 0.6 15.1
P125 40.7 57.9 30.0 50.0
P63 56.7 70.7 45.5 64.1
FM 10.9 7.2 9.2 7.6
RV 21.7 19.7 16.3 17.4
Water content 135.2 223.1 112.7 47.0
Particle density 9.7 4.9 3.8 4.4
DR&B 23.1 / 19.3 /
MB 93.1 67.6 106.5 77.9
LOI 118.2 127.6 93.0 118.5
pH 5.7 / 1.4 /
Water solubility 118.0 87.0 114.4 48.2
CaO 62.7 31.8 28.4 16.2
SiO
2
84.3 54.1 89.1 17.1
R. Melotti et al. / Waste Management 33 (2013) 19061917 1915
expressed in terms of the maximum relative variation (MRV), cal-
culated as the percentage ratio between absolute variation and
average value (also known as two sigma percent difference,
d2s%). Despite the fact that in each case the type of biomass re-
mains unchanged, most of the properties exhibit high MRV values:
this mainly depends on the seasonal availability of biomass, which
cannot be controlled during production (for example different
types of wood are used throughout the year for woodchips).
Furthermore, combustion chamber efciency and biomass
moisture content, which also change over time, affect ash charac-
teristics. The suppliers of biomass ashes which employ woodchips
only in moving grate plants reported that the target water content
for the creation of very ne ashes was 40%. Higher water content
values result in coarser ashes as a consequence of agglomeration
of the smallest particles. Similarly, water content values lower than
40% produce higher temperatures in the combustion chamber
leading to vitrication phenomena of the residues, hence the gen-
eration of ashes with coarser dimensions.
Finally, analysis of the mean values of the maximum relative
variations shows that TO1-N is the most consistent ash (average
MRV equal to 36.5%), while, when considering investigated charac-
teristics, P2000, FM, RV and particle density are those with the
lowest average MRV values (less than 15%). Although consistency
over time of ash properties is a key factor when determining their
potential re-use as a secondary raw material, the study of bitumi-
nous mastics and mixtures composition in future stages of project
RICCO will indicate to what extent this high variability is reected
in the variability of mastics and mixtures.
6. Conclusions
Due to the increasing production of energy from biomass com-
bustion in recent years, management of the resulting biomass y
and bottom ashes has become an issue of great concern. According
to the most recent European directives, these by-products are con-
sidered non-hazardous wastes and their recycling in the eld of ci-
vil construction is strongly encouraged. Since road construction
requires a great quantity of aggregates, the use of recycled biomass
ashes in place of traditional mineral ller in bituminous mixtures
seems to be a good solution to the problem of limiting, by as much
as possible, the quantity of the former to be disposed of.
Past research dealt with the potential use of biomass ashes as
ller in cement and bituminous mixtures. However, such investi-
gations did not give the necessary information regarding an effec-
tive use of biomass ash, which could be obtained simply by an
extensive characterisation.
In this study the characteristics of 27 different ashes derived
from the combustion of solid biomass were investigated, adhering
to the most recent international standards on ller characterisation
and waste recycling. Two traditional llers were also tested for
comparison purposes. The following general conclusions can be
drawn:
According to the EN 13043 specication, only ash 1-SO-N satis-
es size distribution limits for mineral ller in bituminous mix-
tures, signifying that it is necessary to sieve or mill the ashes in
order to obtain an adequate grading. When considering full
scale applications, bottom and y ashes should, following the
combustion process, be stored in separate containers, subject-
ing bottom ashes to a milling process and, possibly, y ashes
to a sieving process. In the case where bottom and y ashes
are stored together, a milling process is necessary in order to
reduce the dimensions of particles.
Some ashes do not respect the water content limit specied in
EN 13043. However, in these cases excess moisture was caused
by specic plant treatments, the hygroscopic surface of the
ashes or by exposure to a humid environment during storage
and transportation. Consequently, where appropriate handling
procedures are observed at an industrial level, excessive water
content is not expected to be a problem as regards the future
use of biomass ashes as llers in bituminous mixtures.
Rigden voids tests showed that compacted samples of biomass
ashes are characterised by very high porosity, with only ve
ashes having RV values lower than those measured for reference
llers. This nding is extremely signicant since ashes having
high RV values may stiffen the bitumen excessively, as proven
by ring and ball tests. Therefore, for the production of bitumi-
nous mixtures it is envisioned that limits be established both
for RV values and the llerbitumen ratio. Identication of the
limits will be the subject of future phases of the research project.
The low values for both the methylene blue and loss on ignition
tests show that the content of clay and organic matter, harmful
for bituminous mixtures, are limited in biomass ashes.
The results of leaching tests (EN 12457-2) indicate that the
release of pollutants and the pH value of the eluate of most of
the ashes exceed the Italian limits for environmental re-use.
This is particularly evident for chrome and sulphate. However,
several studies have shown that in bituminous mixtures the
coating effect of binder reduces the release of pollutants and
the pH value. As a consequence, this topic will be investigated
by the authors in the near future when the research deals with
the evaluation of bituminous mixture performances.
The properties of the ashes collected from the same power
plants in two different periods of the year exhibit high variabil-
ity. Since the type of biomass does not change, this variability is
mainly due to different seasonal supplies (of biomass) that vary
in terms of composition. This appears to be one of the main neg-
ative aspects of the use of biomass ashes that has been partly
referred to in previous research (Vansteenkiste and Vanelstrae-
te, 2008). Future phases of the research project will indicate to
what extent this high variability is reected in the variability of
the characteristics of bituminous mastics and mixtures.
The present preliminary study suggests that biomass ashes, if
subjected to a sieving process, may be considered as a valid alter-
Table 10
Maximum relative variations (sampling in April and December 2010) (%).
P2000 P125 P63 FM RV Water content Particle density MB LOI Water solub. CaO SiO
2
Mean
TO1-N 0.1 8.5 3.7 11.7 2.3 16.0 0.8 100.0 126.9 36.1 33.1 99.0 36.5
AO2-N 8.0 63.8 78.9 10.4 2.5 25.9 19.0 28.6 38.0 86.8 23.4 95.8 40.1
AO3-N 42.8 112.1 116.3 1.8 13.7 62.1 7.5 0.0 183.8 20.2 12.0 52.0 52.0
AO3-M 1.2 38.9 47.6 15.7 13.9 63.8 4.0 66.7 183.8 / 12.0 52.0 45.4
TO2-N 0.0 38.6 68.3 9.0 19.4 9.0 11.2 0.0 66.9 131.8 22.5 120.5 41.4
SO-N 0.1 79.1 101.0 6.7 18.3 129.4 4.9 15.4 130.6 82.0 63.4 42.1 56.1
KR1-N 51.3 108.4 106.4 / 28.2 168.9 1.9 / 89.0 112.0 43.2 1.2 71.1
KR2-N 15.8 86.4 140.8 / / 62.3 / / 43.2 / 4.9 9.4 51.8
KR2-M 0.0 28.4 34.5 11.5 2.2 41.7 1.2 76.9 43.2 191.6 4.9 9.4 37.1
Mean 13.2 62.7 77.5 9.6 12.6 64.3 6.3 41.1 100.6 94.4 24.4 53.5
1916 R. Melotti et al. / Waste Management 33 (2013) 19061917
native to natural ller in bituminous mixtures. However, some re-
sults appeared to give cause for concern due to the exceeding of
the acceptance limits established for traditional llers.
Nevertheless, future developments are needed to ascertain
which characteristics of the ashes directly affect mixture perfor-
mance: thus, the subsequent phases of the research project shall
focus on the rheological characterisation of bituminous mastics
and mixtures containing biomass ashes.
Acknowledgements
The research Project was nanced by the Italian Ministry of
Agricultural, Food and Forestry Policies (Ministero delle Politiche
Agricole Alimentari e Forestali Riutilizzo ceneri provenienti da
combustione di biomassa RICCO DM 28384/7815/09 del 02/12/
2009).
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