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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
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Waste Management
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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
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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