Waste Management 24 (2004) 589–596

www.elsevier.com/locate/wasman

Metallic aluminum in MSWI fly ash: quantification and influence

on the properties of cement-based products
J.E. Aubert *, B. Husson, A. Vaquier
Laboratoire Mat
eriaux et Durabilit
e des Constructions, INSA-UPS, 135 avenue de Rangueil, 31077 Toulouse Cedex 4, France

Accepted 26 January 2004

Abstract

This article focuses on the effects of metallic aluminum contained in municipal solid waste incineration (MSWI) fly ashes on
cement-based materials in which they are added. The ash under study was treated by an industrial physicochemical process of
neutralization. The paper also presents a method to quantify the metallic aluminum content of ash: it consists in measuring the
amount of hydrogen gas produced by the oxidation reaction of metallic aluminum. This method is simple and fast. Results show
that studied ash contains an appreciable amount of metallic aluminum. Investigations were carried out to study the incorporation of
the ash in concrete: in this case, the presence of metallic aluminum is worrying because it could be responsible for disorders in
concrete. In fact, swellings are observed on cement pastes and mortars containing ash during the first 24 h of hydration. A test based
on hydrostatic weighing permits to quantify the swelling of fresh cement paste and to study the evolution of this swelling. Causes of
swelling are analyzed. Results show that ettringite formation occurs after the end of the expansion reaction. So it can be concluded
that metallic aluminum is the sole responsible for the observed swelling. Consequences of swelling are also analyzed by measuring
compressive strength of ash-containing mortars: this swelling leads to cracks in the mortars and significant decrease of their
compressive strength.

2004 Elsevier Ltd. All rights reserved.

1. Introduction to recover the sodium which is used in technical soda

Currently, in France, municipal solid waste incinera-
tion (MSWI) produces 400,000 annual tons of gas
cleaning residues such as fly ashes and air pollution
control (APC) residues. Such residues are landfilled after
stabilization and solidification. With a view of reducing
the quantities to be landfilled, the SOLVAY Company, in
collaboration with the Universit
e Libre de Bruxelles, has
been working on development of a new physicochemical
treatment for these ashes, the REVASOL process.
This process was composed of three successive steps
(Derie and Depaus, 1999):
• Water dissolution of ash: during this washing, pH is
kept below 10.5 to prevent the dissolution of heavy
metals. In fact, the washing solution containing solu-
ble salts (especially chlorides (KCl and NaCl), the
alkaline sulfates being in an insoluble form) is treated
*
Corresponding author. Tel.: +33-56155-7757; fax: +33-36155-9949.
E-mail address: aubert@insa-tlse.fr (J.E. Aubert).
plants.
• Phosphation with phosphoric acid to stabilize heavy
metals.
• Calcination to eliminate organic compounds (espe-
cially dioxins), at a temperature higher than 600 C.
This step also enables the crystalline structure of
the final product to be stabilized.
The results of a micro-characterization approach
demonstrate that the process is able to stabilize heavy
metals contained in MSWI fly ash (Piantone et al.,
2003).
Investigations were carried out to study the incor-
poration of the ashes treated by this process in concrete:
they have shown that this incorporation is technically
feasible and that the environmental impact of the ash-
containing concrete is acceptable (Aubert, 2002). How-
ever, like all waste coming from municipal solid waste
incineration, the ashes treated by the process contain
metallic aluminum (Al0 ) that can lead to disorders when
these wastes are introduced into cement-based materials.

0956-053X/$ - see front matter
2004 Elsevier Ltd. All rights reserved.
doi:10.1016/j.wasman.2004.01.005
590 J.E. Aubert et al. / Waste Management 24 (2004) 589–596
These problems have been observed by many authors in
MSWI bottom ash (P
era et al., 1997; Qu
en
ee et al.,
2000; Goacolou, 2001; Pecqueur et al., 2001) and in
MSWI fly ash (Escadeillas et al., 1995; Morel-Bray-
mand, 1999; Guerrero et al., 2000; Chan et al., 2000;
Fernandez et al., 2000).
This article focuses on the study of metallic aluminum
contained in the fly ashes after treatment. First, a
method for measuring metallic aluminum content is
presented. There is no fast and easy method for deter-
mining metallic aluminum content in heterogeneous
material. Such analytical techniques as Atomic Ab-
sorption Spectroscopy, Atomic Emission Spectroscopy
and X-ray Fluorescence give the total quantity of alu-
minum in a sample in its different chemical forms and
oxidation states (metal, oxides, etc.). X-ray diffraction
(XRD) is able to detect metallic aluminum but it was
not suited to our case for several reasons:
• Determination of minor species is difficult and the
accuracy of measurements is low.
• A secondary peak of anhydrite and the main peak of
aluminum overlapped in studied ash.
The electron microprobe can distinguish between the
various forms taken by aluminum but total quantitative
analyses are almost impossible. A method used by min-
eralogists allows metallic aluminum to be recognized
(Fischesser, 1955): it is based on the reaction between
aluminum and cobalt nitrate but it cannot be used in
presence of zinc, which was the case for studied ash.
Moreover, the proportion of metallic aluminum cannot
be quantified with this method. Crignon et al. (1999) used
differential scanning calorimetry (DSC) to quantify me-
tallic aluminum in mortars but this method requires a
specific apparatus and is less simple than that presented in
this article. In fact, the technique presented in this study
100
80
Passing (%)
60
40
20
0
0.001
consists of determining metallic aluminum content by
measuring the amount of hydrogen gas produced by the
oxidation reaction of metallic aluminum. A similar
method was used by Coutaz (1996) in an attempt to de-
termine the metallic aluminum content of MSWI bottom
ashes but his experiment failed because the kinetics of
aluminum dissolution was too slow. The bottom ashes
had not been ground and the size of the particles (0–4 mm)
can explain this problem. To accelerate the reactions, the
ash under study was ground to <125 lm before the test.
On the other hand, swelling is observed in cement-
based materials containing ash during the first 24 h of
hydration. This swelling ca not be caused by Mg and Ca
hydroxide hydration because ash contains neither MgO
nor CaO. Two different causes can explain this swelling:
• Dihydrogen emission due to the reaction of metallic
aluminum contained in the ash with the alkalis of ce-
ment paste.
• Ettringite formation due to the significant sulfate
content of the ash.
Current extensometry techniques for cement-based
materials cannot be applied to fresh mixtures so that a
different technique based on hydrostatic weighing of
fresh paste was used. This technique will be precisely
described in Section 4. Moreover, the evolution of et-
tringite formation in cement pastes is analyzed by XRD
to identify the true origin (metallic aluminum or sul-
fates) of swelling.
Finally, the influence of the swelling on the com-
pressive strength of mortars is analyzed.
2. Ash characterization
The fly ash studied in this article is coming from a
single French incinerator. It has been treated in a pilot
0.01 0.1 1 10
particle size (mm)
Fig. 1. Size distribution of ash.
 J.E. Aubert et al. / Waste Management 24 (2004) 589–596 591

unit of 25 kg/h capacity. The calcination was carried out 3. Determination of metallic aluminum content
in a rotary kiln at a temperature of 750 C. Ash is a fine,
brown sand, the size distribution of which is given in The technique used is based on a principle similar to
Fig. 1. The 80 lm oversize fraction was analyzed by that applied to calcite quantification, with CO2 volume
sieving, while the finer fraction was analyzed by a par- measurement during acidic dissolution.
ticle size laser analyzer. At high pH, metallic aluminum is dissolved, with
The elemental composition of ash is presented in emission of dihydrogen according to the following re-
Table 1. The major elements were measured by action:
Inductively coupled plasma–atomic emission spec- 2Al þ 2OH
þ 2H2 O ! 2AlO

2 þ 3H2 ð1Þ
trometry (ICP-AES) and the minor ones by Induc-
tively coupled plasma–mass spectrometry (ICP-MS). OH
ions are provided by a sodium hydroxide solution
The water content (drying at 100 C) and the loss on and the volume of dihydrogen is measured at different
ignition (calcination at 1000 C) were also measured. time intervals. During the test, temperature and atmo-
The elemental composition highlights the high amount spheric pressure are measured. Also, using the assump-
of heavy metals (especially zinc and lead) and sulfate tion of perfect gases, the measured volume is calculated
(SO3 ¼ 11.6%). Moreover, the process involves an in- at normal conditions of temperature and pressure
crease of the phosphorous content (phosphatization (T0 ¼ 273 K, P0 ¼ 101:3 kPa).
step) and the disappearance of chlorides (washing The material is placed in a cell with a tube filled with
step). 50 ml of a 1 M sodium hydroxide solution. This cell is
The mineralogical phases were identified by a powder then hermetically closed and the volume of gas released
X-ray diffractometer equipped with a monochromator is measured by keeping the pressure in the cell equal to
using a Ka (k ¼ 1:789 A)  cobalt anticathode. The min- the atmospheric pressure. The experiment is started by
erals in order of decreasing content were: minerals of pouring the sodium hydroxide on to the powder.
gehlenite group (Ca2 Al2 SiO7 ), calcium phosphates in- The first stage in the measurement of the aluminum
cluding apatite (Ca5 (PO4 )5 (OH,F,Cl)) and whitlockite content in ash sample was the determination of a cali-
(b-Ca3 (PO4 )2 ), anhydrite (CaSO4 ), quartz (SiO2 ), tita- bration curve. Pure metallic aluminum ground to <125
nium oxides including titanite (CaTiSiO5 ) and perov- lm was used. The volume released was measured at
skite (CaTiO3 ), and hematite (Fe2 O3 ). These minerals several times: 10 , 20 , 30 , 50 , 100 and then every half-hour.
are accompanied by an amorphous phase (calcium alu- Fig. 2 presents examples of results but many others have
mino silicate). been made to allow the determination of the calibration
curve. These results taken as examples show the evolu-
tion of measured gas volume versus time, which per-
mitted to determine the completion of reaction. In fact,
Table 1 the curves can be divided in three parts.
Elemental composition of ash First, an instantaneous volume expansion ðvi Þ oc-
Major elements content (%) Minor elements content (mg/kg) curred for all the experiments even when there was no
CaO 25.2 Zn 24,046 metallic aluminum in the cell (mAl ¼ 0 g). This phe-
SiO2 20.7 Pb 8816 nomenon started as soon as the tube containing the
P2 O5 13.6 Sn 2883 solution was turned upside down in the cell and was
SO3 11.6 Cr 2078 independent of the solution used. Experiments with
Al2 O3 10.0 Ni 1889
demineralized water showed the same expansion: it
MgO 2.7 Cu 1714
Fe2 O3 2.7 Ba 1521 corresponded to an instantaneous evaporation of the
TiO2 1.7 Sb 1457 solution due to the abrupt increase of the liquid/gas
Na2 O 1.4 Cd 586 frontier.
K2 O 1.4 Sr 399 Second, a significant gas volume increase appeared
MnO 0.2 W 227
when testing metallic aluminum. This increase, during
Water content 0.2 Zr 149
Ignition loss 6.5 As 120 approximately 1 h, was proportional to the amount of
Co 79 metallic aluminum. It corresponded to the released gas
Mo 49 volume due to the oxidation of metallic aluminum. To
Rb 34 be sure that all the aluminum was attacked for each test,
Bi 30
the reference time was set to 150 min.
V 30
Ce 30 Finally, the volume continued to increase propor-
Ga 21 tionally to the time elapsed. This gas volume increase,
La 15 noted vðtÞ on Fig. 2, could be explained by the evapo-
Nd 11 ration of the solution contained in the cell. Like the
Nb 11
instantaneous volume expansion ðvi Þ, this increase was
592 J.E. Aubert et al. / Waste Management 24 (2004) 589–596

120
t=150min
mAl=0.067g
100

Measured gas volume,Vm (ml)

80

60

mAl=0.021g
40

vc mAl=0g
20
v(t)
0
vi
0 50 100 150 200 250 300
Time (min)

Fig. 2. Emission of gas as a function of time.

independent of the Al content and occurred even when We can notice that correlation between theoretical
there was no metallic aluminum in the cell (mAl ¼ 0 g). curve and experimental data is rather good.
To quantify metallic aluminum content, only the gas To determine metallic aluminum content, the ash
volume produced by the oxidation of aluminum have to sample ground to <125 lm was dissolved under the
be considered. So, corrected gas volumes vc were cal- same conditions as the pure aluminum.
culated by subtracting ðvi þ vðtÞÞ (determined on many The volume released after 150 min was measured and
tests without aluminum (mAl ¼ 0 g)) from the measured the mass of aluminum was computed using corrected
value vm . These corrected values are reported on Fig. 3. values, vc . The results obtained for three ash samples are
These values could be compared to the theoretical re- presented in Table 2. The aluminum content of the ash
leased gas volume obtained according to Eq. (2). In fact, ranged between 0:20
0:07 ¼ 0:13% and 0:28 þ 0:07 ¼
the relationship between the volume of hydrogen gas 0:35%.
released and the amount of metallic aluminum in the The method proved to be reliable, easy to use and
sample is relatively quick (150 min for one test). The method
3 mAl made it possible to determine the mass of metallic alu-
v H2 ¼ v0 ; ð2Þ minum with a good absolute accuracy, D, of 0.007 g
2 MAl
(Fig. 3). The relative accuracy is poor (approximately
where v0 is the molar volume, equal to 22.4 l/mol and equal to 30%) but it is due to the low content of metallic
MAl is the molar mass of aluminum, equal to 27 g/mol. aluminum in ash and not to the precision of the test.

110
Calculated curve (relation(3))
Experimental points zone
90
Corrected gas volume, Vc (ml)

- +

70

50

30

10

0.000 0.010 0.020 0.030 0.040 0.050 0.060 0.070 0.080

-10
Mass of aluminum (g)

Fig. 3. Corrected hydrogen gas volume evolved at t ¼ 150 min.

 J.E. Aubert et al. / Waste Management 24 (2004) 589–596 593

Table 2 4.2. Swelling measurement

Metallic aluminum content of ash
Mass of ash Corrected hydrogen
(g) gas volume (ml)
9.983 25
10.034 25
9.999 35
4. Swelling on cement pastes
4.1. Mixtures description
Ash had been introduced in cement pastes to replace
part of the cement. The cement used was an ordinary
portland cement (OPC) containing more than 95% of
clinker (CPA-CEM I 52.5R). Two compositions were
studied: a reference cement paste (100% OPC) and an
ash-containing paste (75% OPC and 25% ash). The
amounts of water were added in order to obtain a
normal consistency and the pastes were mixed according
to the standardized European EN 196-3 test method
(1994). The ratios Water/Binder (binder being consid-
ered as the sum of cement and ash) are, respectively,
equal to 0.29 and 0.31 for the reference paste and the
ash-containing paste.
For the XRD studies, pastes were cured in polyeth-
ylene tubes at 20 C. At several hydration times, a piece
of paste was manually sawn, without water, with a
hacksaw to prevent increase of temperature. Then the
sample was crushed, dried with acetone (at a tempera-
ture equal to 50 C during few minutes) and manually
ground to <40 lm.
Metallic Al content The test consisted of measuring by hydrostatic
weighing the variation of volume of an elastic, imper-
(g) (%)
meable membrane containing the cement paste under
0.020 ± 0.007 0.20 ± 0.07
0.020 ± 0.007 0.20 ± 0.07 study. The sample, immersed in a water bath, is hung on
0.028 ± 0.007 0.28 ± 0.07 a balance connected to a computer, which records the
weight values every minute with a precision of 1 mg (the
mass of the membrane containing paste is approxi-
mately equal to 200 g). The temperature in the water
bath is controlled and equal to 20 C.
The volume variations of the reference cement paste
and ash-containing paste are presented in Fig. 4.
Swelling was measured under two configurations, one
(referred to as ‘‘closed’’) where the membrane contain-
ing the paste was closed and the gas evolved was con-
fined, while the other (referred to as ‘‘open’’) where a
small opening was left so that the gas released could
leave the membrane. In this case, the volume increase of
the solid paste only was measured.
For the reference paste, a slight shrinkage was ob-
served over the first 12 h. But for the ash-containing
paste, the volume increase was very significant.
For the ‘‘closed’’ test, a gaseous cap formed in the top
of the membrane caused by the emission of hydrogen.
The reactions stopped after 10 h.
For the ‘‘open’’ test, the volume increase was smaller
than before and the expansion stopped after only 2 h.
The ‘‘open’’ test could only characterize the paste ex-
pansion, which depended on how easily the gas left the
paste. The measurement was influenced by many pa-
rameters, such as the characteristics of the porous media
and the rheological properties. So the interest of this test
lies in the comparison of similar materials (e.g. cement
pastes having the same consistency).

25
t=10 hours
closed
20
Expansion of the membran (%)

15

open
10

0
0.00 2.00 4.00 6.00 8.00 10.00 12.00
0% fly ash
-5
Time (h)

Fig. 4. Variation of swelling of the cement pastes.

594 J.E. Aubert et al. / Waste Management 24 (2004) 589–596

4.3. Study of ettringite formation by XRD
Ettringite formation, which could be a cause of
swelling, was studied on cement pastes through XRD.
To compare the different mixtures, the Klug and
AlexanderÕs (1974) relation was used
Km xm
I¼ ; ð3Þ
qm lT
where I is the peak intensity for the mineral m, xm is the
concentration (in mass) of the mineral in the sample, lT
is the total mass absorption coefficient of the sample, qm
is the density of the mineral (g/cm2 ) and Km is a coeffi-
cient that depends on the nature of the mineral (pa-
rameters of crystal phase) and on the working
conditions (geometry and operation of apparatus).
Considering the same mineral m in two mixtures 0
and 1, the mixture 0 being taken as the reference mix-
ture, relation (3) becomes
Km0 xm0
I0 ¼ ;
qm0 lT0
Km1 xm1
I1 ¼ :
qm1 lT1
For the same equipment and under the same working
conditions, it is possible to consider that Km0 ¼ Km1 . By
combining the two equations, one obtains
xm1 lT1 I1
¼ :
xm0 lT0 I0
Intensities I0 and I1 were directly measured on the dia-
grams. Coefficients lT0 and lT1 were computed by
multiplying the content of each element present in the
mixtures by the X-ray absorption coefficient of the ele-
ment. Content of element was determined from the
composition of the mixtures and the elemental compo-
sitions of the constituents (cement and ash). It was then
possible to follow the variation of the relative concen-
tration of a mineral compared to a reference. The ap-
proach also allowed mixtures with different chemical
compositions to be compared.
Fig. 5 shows the variation of the relative concentra-
tion of ettringite. The d spacing selected for the mea-
surement was 9.72 A  but results with peak at d ¼ 5:61 A

were similar. The concentration of ettringite in the ref-
erence paste after nine months of hydration was taken as
the reference x0 .
The total concentration of ettringite in ash-contain-
ing paste was much higher than this in reference paste.
But this increase in ettringite concentration, due to the
high sulfate content of ash, happened after 24 h. Until
approximately 10 h of hydration, the concentration of
ettringite in ash-containing paste was lower than this in
reference paste.
4.4. Discussion
Significant swelling is observed when ash is intro-
duced in cement paste. Swelling measurement have
permitted to conclude that this phenomenon happens
during the first hours of hydration and stopped rather
quickly (at the end of 10 h). There are two possible ex-
planations for this volume increase: emission of hydro-
gen caused by the presence of aluminum and expansion
due to the formation of ettringite. The study of ettringite
formation by XRD have shown that the concentration
of ettringite in the ash-containing paste was lower than
this in the reference paste in the first 10 h of hydration.
So the formation of ettringite cannot explain the early
expansion of the paste (cement + fly ash). We conclude
that swelling is only caused by the emission of hydrogen
gas due to the presence of metallic aluminum.

2.5

2.0
t =10 hours 25% fly ash

1.5
x/xo

0% fly ash
1.0

0.5

0.0
0.01 0.10 1.00 10.00 100.00 1000.00
Time (d)

Fig. 5. Variation of the relative concentrations of ettringite in the cement pastes.

 J.E. Aubert et al. / Waste Management 24 (2004) 589–596
80
70
Compressive strength (MPa)
60
50
40
30
20
10
0
0 28
Fig. 6. Compressive strength of the mortars versus time.
5. Consequences of swelling: mechanical strength of
mortars
Swelling caused by emission of hydrogen provokes
significant disruptions in cement-based materials con-
taining ash. To evaluate the effect of these disruptions,
compressive strengths of mortars were studied.
5.1. Mixtures description
Two compositions of mortars were studied: a refer-
ence mortar (100% OPC) and an ash-containing mortar
(75% OPC and 25% ash). Sand/binder and water/binder
ratios were 3 and 0.5, respectively, for all compositions.
To keep a constant workability, a plasticizer was added
to ash-containing mortars (plasticizer/binder ratio was
equal to 0.004). The samples were prepared according to
the standardized European EN 196-1 test method
(1995).
The mortars were cured at 20 C in water saturated
with calcium hydroxide. The 4 · 4 · 16 cm test samples
were initially broken in two pieces that were then tested
for compressive strength according to the standardized
European EN 196-1 test method (1995).
5.2. Results and discussion
The compressive strengths of the mortars are re-
ported in Fig. 6.
The compressive strength of the ash-containing
mortars was much lower than that displayed by the
control mixture. One reason for this is the dilution effect
on cement due to the ash addition. The effects of this
dilution can be computed by the BolomeyÕs relation
under its simplest form (Bolomey, 1935)
595
R0
R th
R 25
56 84 112 140 168
Time (d)
 
C
Rc ¼ fc k
0:5 ; ð4Þ
W
where Rc is the compressive strength of the mortars
(MPa), fc is the characteristic resistance of the cement
(MPa), k is a coefficient that depends on the aggregates,
C and W are the cement and water content, respectively.
As the cement was the same for the two mixtures, the
coefficients fc and k were constants. So, we can calculate
the theoretical curve (Rth in Fig. 6) corresponding to the
reduction in the C=W ratio of the mixture.
The experimental curve R25 is lower that Rth . Study of
the effect of ash on cement hydration has shown that ash
has a favorable effect (Aubert, 2002). Phosphates are
insoluble and do not play any role in the reactions. On
the other hand, gehlenite and calcium sulfates react to
form ettringite which consequence is a gain of strength
(because the formation of ettringite does not involve a
supplementary increase of volume). So, the loss of
compressive strength observed on mortars can only be
explained by the fact that the swelling of ash-containing
mixtures has led to supplementary air voids and cracks
(Fig. 7).
Fig. 7. Effects of swelling on the mortar.
596 J.E. Aubert et al. / Waste Management 24 (2004) 589–596
6. Conclusions
This article deals with the significant problem of
metallic aluminum in the wastes of MSWI and in par-
ticular in fly ashes. A method has been proposed to
determine the metallic aluminum content because it is
easy to use, fast and of good accuracy: it consists of
measuring the amount of hydrogen gas produced by the
oxidation reaction of metallic aluminum. Results show
that studied ash contains an un-negligible amount of
metallic aluminum, which leads to swelling in cement
pastes and mortars containing ash. In the other part,
studies of the hydration reaction on paste show that the
high sulfate content in the ash does not play any role in
this phenomenon because the increase in ettringite for-
mation in ash-containing paste occurs after the end of
the expansion reactions. So, we can conclude that only
aluminum generates the swelling, the consequence of
which is cracking of cement based materials. In mortars,
cracking lowers compressive strength and the results
obtained with ash are lower than those computed for an
inert addition. However, the use of this ash in building
materials is not to be excluded.
On the one hand, technical solutions exist to prevent
swelling: a module addition in the process enables me-
tallic aluminum to be eliminated. Ash being such treated
does not provoke swelling and have favorable effect on
compressive strength of mortar (Aubert, 2002).
On the other hand, the harmful influence of swelling
can be negligible or inexistent on highly porous mate-
rials. This is the case for low-strength concrete (Aubert,
2002), embankments and road works, for instance. In
these uses, the gas formed can easily leave the materials
and the effects of swelling are slighter than those oc-
curring in compact materials.
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