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Characterization of Municipal Solid Waste Incineration Residues From

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DOI: 10.1080/10473289.1997.10464059

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 Journal of the Air & Waste Management Association

ISSN: 1096-2247 (Print) 2162-2906 (Online) Journal homepage: http://www.tandfonline.com/loi/uawm20

Characterization of Municipal Solid Waste

Incineration Residues From Facilities with
Different Air Pollution Control Systems

N. Alba , S. Gassó , T. Lacorte & J.M. Baldasano

To cite this article: N. Alba , S. Gassó , T. Lacorte & J.M. Baldasano (1997) Characterization
of Municipal Solid Waste Incineration Residues From Facilities with Different Air Pollution
Control Systems, Journal of the Air & Waste Management Association, 47:11, 1170-1179, DOI:
10.1080/10473289.1997.10464059

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Alba, Gassó, Lacorte,
TECHNICAL PAPER and Baldasano
Characterization of Municipal Solid Waste Incineration
Residues from Facilities with Different Air Pollution
Control Systems
N. Alba, S. Gassó, T. Lacorte and J.M. Baldasano
Institute of Environmental Technology and Modelling (ITEMA), Universitat Politècnica de Catalunya (UPC),
Catalonia, Spain
ABSTRACT
Municipal Solid Waste incinerator residues produced
in two types of facilities were exhaustively character-
ized: granulometry, mineralogy, chemical composition,
leaching behavior, and elemental distribution as a
function of particle size. Air Pollution Control (APC)
residues coming from a semi-dry scrubber have shown
higher solubility than fly ashes originating in an Elec-
trostatic Precipitator (ESP), as well as higher contents
in volatile metals (Cd, Hg). Different metal speciation
and distribution as a function of particle size have been
found in fly ashes (ESP residues) and APC residues. In
APC residues, heavy metals (with the exception of Hg)
show a parabolic distribution with maxima in the
smallest and largest particles, following the same pro-
file as soluble salts. Metal distribution for APC resi-
dues exhibits that metals generally are not associated
with silicate aluminate matrix. Results show the effect
of adding lime to APC residues in metal speciation and
distribution.
IMPLICATIONS
Improvements in flue gas cleaning by modern incin-
erators produce APC residues with higher metal solu-
bility than fly ash. Because of their high concentrations
of Pb, Cl-, and SO42- in leachates, and according to ECC/
Draft Directive of/C212/02, APC residues and fly ashes
should be treated prior to landfill. As the urge to re-
cycle and reuse these types of waste materials in-
creases, a more rigorous approach is needed to cope
with a wide range of technical, physical, chemical, and
economical aspects. This paper tries to determine the
chemical and physical characterization of residues com-
ing from two different types of municipal solid waste
incinerator facilities. Characterization is further com-
pleted by analyzing solubilities, and major and heavy
metals distribution among different granulometric
ranges. Long-term leaching tests are required to study
leaching phenomena in depth, as well as modelling
them under controlled conditions.
1170 Journal of the Air & Waste Management Association
ISSN 1047-3289 J. Air & Waste Manage. Assoc. 47:1170-1179
Copyright 1997 Air & Waste Management Association
INTRODUCTION
Municipal Solid Waste Incineration (MSWI) is an inte-
grated waste management system. MSWI offers a reduc-
tion in both the mass and volume of waste subjected to
final disposal, as well as the possibility of energy recov-
ery; waste mass is reduced approximately 70%, and vol-
ume by about 90%, and it provides energy that can be
recovered to produce electricity or steam.1
Current regulations governing the operation of MSWI
try to reduce adverse human health effects and control
environmental impacts. A consequence of MSWI is the
generation of residues such as bottom ashes, fly ashes (par-
ticulate matter carried over from the furnace and removed
from the flue gas without injection of sorbents), and Air
Pollution Control (APC) residues (combined materials
collected in electrostatic precipitators or fabric filter de-
vices, including fly ash, injected sorbents and flue gas
condensate). These residues present a potential toxicity
because of their heavy metal and salt content, and there-
fore require proper management.
Safe management of these residues, which, by
some regulations, could be classified as hazardous, is
still a problem. MSWI residues are mainly landfilled,
but because of its chemical and leachability proper-
ties, ash can pose potential environmental impacts if
it is not handled appropriately.
As an alternative to land disposal, there is increasing
interest in incorporating MSWI residues in products rang-
ing from roadbase (cementitious stabilized)2 to masonry
bricks3-5 to ceramic products.6 Determining safe manage-
ment alternatives for these type of residues requires ex-
tensive characterization. Many studies have shown the
presence of such toxic metals as Cd, Pb, Cr, Zn, Hg, and
soluble salts, and have studied the leaching behavior of
these types of wastes.1,7-10 Several works11,12 have surveyed
heavy metal distribution in APC residue as a function of
particle size, showing that the most volatile elements,
except Hg, tend to concentrate on the smallest particles.
These results are in agreement with the assumption that
Volume 47 November 1997
 Alba, Gassó, Lacorte, and Baldasano

trace metals are volatilized during combustion and then Table 1. Operating plant parameters of the waste incinerators facilities sampled.
re-condensed on particle surface. Because the smallest
particles have the largest specific area, the recondensation Operating Parameters MSWIa MSWIb
phenomenon is more common. Two distinct trends re-
Startup Date 1975 1994
garding metal distribution as a function of particle size
Plant Capacity (t/day) 1080 480
have been found in APC residues:11 a parabolic distribu-
Furnace design 3 parallel furnacesa 2 parallel furnacesb
tion having maxima in central fractions for less volatile
Trash Accepted Mass Burn facility 50% Mass Burn 50 % RDF
metals (Cr, Cu), and a sigmoidal distribution that favors MSW feed Method overhead crane feeding overhead crane
high concentrations of more volatile metals (Cd, Pb, Zn) vibratory hoppers
in the smallest fractions. Furnace Temperature (°C) 850c Over 850
The purpose of this paper is to present results on the Residence Time (s) Not controlled minimum 2
determination of the chemical and physical characteriza- Steam produced 400 °C 40 Atm 380 °C 61 Atm
tion of residues coming from two different types of MSWI Backup Fuel Not available Methane
facilities, which represent the evolution that air pollution Energy Recovery yes yes
control systems have undergone during the last several Temperature before APC (°C) 270 200
years. The characterization is further completed by frac- APC devices ESP Semi-dry+ESP
Ash handling + Combined:bottom+ Separated (Bottom Ash
tionating fly ashes (from an electrostatic precipitator) and
management fly ash and APC residues)
APC residue (from a semi-dry scrubber) by particle size.
Heavy metals distribution among the different a
Composed of 3 grates (drying, burning, and final zone to guarantee total combustion).
granulometric ranges have also been analyzed. b
With rotary grates.
c
During sampling, the hourly mean temperature was sometimes below 850 °C.
MATERIALS AND METHODS
MSWI Description and Sampling Procedure a collection time of 8 hours (separation line of ferrous
The MSWI samples chosen to perform this work are lo- metal only works 8 hours per day).
cated in Catalonia (Spain) and were selected because their MSWIb was sampled once in September 1995. Ap-
air pollution control devices represent the evolution such proximately 100 kg were collected from several points of
devices have undergone in the last twenty years. a stockpile of bottom ashes produced over one day. For
Facility A (MSWIa), which began operation in 1975, APC residues, a representative sample (about 50 kg) from
is a mass burn incinerator with a nominal capacity of 1,080 one day’s operation was collected from the storage tank
tons per day. It consists of three parallel furnaces, boilers, when it was emptied out.
and electrostatic precipitators (ESPs). Bottom ashes and All sampling was done according to UNE 83-42113 on
fly ashes (ESP residues) are combined in a water quench sampling, conservation, and transport of coal fly ashes,
system and iron recovery is performed. Combined resi- and according to The Standard Guide for General Plan-
due is handled and stored prior to landfill disposal. ning of waste sampling (ASTM 4867-87). 14 Before the
Facility B (MSWIb), which began operation in 1994, analysis of every residue, a subsample of approximately 1
is a refuse-derived fuel incinerator (nearly 50% of trash kg was obtained by the quartering procedure.
comes from refuse in composting and recycling mate-
rials) with two parallel furnaces having a total nomi-
nal capacity of 480 tons per day. The flue gases are Analytical Methods: Bulk Samples
cooled through heat exchangers with a boiler, then sent X-Ray Fluorescence (PW-1400 Philips) was used to ana-
to a semi-dry scrubber. Particulate recovery is through lyze major elements preparing lithium tetraborate pearls
the use of an electrostatic precipitator. Evacuation, with samples previously calcined for 3 hours at 900 °C
handling, and management of bottom ashes and APC with a 1/20 dilution. Results are expressed in terms of
residues is carried out separately. weight percent of oxide (using the highest reasonable
Table 1 shows the summary of operating conditions oxidation state for each element) because both ashes and
of both plants that can affect MSWI residue characteris- pearls are formed under oxidizing conditions.
tics. The two facilities consist of energy recovery systems. Free CaO has been analyzed according to UNE 80-
MSWIa was sampled once in March 1995. Samples of 243,15 which refers to CaO dissolved in hot ethilenglicol
approximately 2.5 kilograms were taken from the ESP resi- and titrated with 0.1 N HCl using blue bromotimol.
due stream (before being combined with bottom ashes) Analysis of minor and trace metals (except Hg) was
every hour over a collection time of 24 hours. For the performed by two different procedures, which differed
combined ashes, three samples (after ferrous metals re- according to digestion method used. The objective was
covery) of approximately 5 kg were taken every hour over to compare results obtained by a total digestion attack

Volume 47 November 1997 Journal of the Air & Waste Management Association 1171
Alba, Gassó, Lacorte, and Baldasano
Figure 1. Particle size distribution in fly ash (MSWIa) and APC residue
(MSWIb).
(destroying silicate matrix) with results obtained by an
extractable digestion procedure, emphasizing differences
that can arise depending on digestion protocol performed,
which often is not well specified in legal or even scien-
tific papers.
To analyze total heavy metals (Zn, Pb, As, Cd, Ni,
and Cu), approximately 1g (per triplicate) of each
sample was digested using an HNO3/HF/HClO 4 mix-
ture in a teflon flask. Difficulties achieving complete
digestion have been reported in several studies.16 For this
study, three additions of 10 ml HF were necessary to com-
plete dissolution, and several additions of 0.2 ml H 2O2
to complete charcoal particles oxidation. The diges-
tion procedure to mineralize total Cr included a mix-
ture of HNO 3/HF/H2SO4. Quantification of the metals
was done using a Thermo Jarell-Ash inductive-coupled
argon plasma-atomic emission Spectrometer (ICP-AES).
ICP-AES accuracy has been confirmed in a previous
work 12 using certified reference materials 3171 and
3172.
On the other hand, extractable minor and trace heavy
metals were conducted by an ISO/CD11466 Digestion
Procedure,17 using aqua regia to digest samples that previ-
ously were grounded and sieved (< 150 mm).
1172 Journal of the Air & Waste Management Association
Figure 2. Total dissolved solids vs. granulometric ranges.
The volatility of Hg obliges it to follow a different
extraction protocol for its total determination; using
HCl/HNO3 in a closed tube with a teflon screw-on cap.
Hg quantification was done using cold vapor/atomic
absorption.
The crystalline phases of combined ashes and fly
ashes of MSWIa, and the bottom ashes and APC residues
of MSWIb, were identified by a Siemens D-500 powder
X-Ray Diffractometer equipped with a graphite monochro-
mator. A copper Tube Kα (1,54 Å ) was employed as an X-
ray source. The accelerating voltage was 45 kV, and the
current at 35 mA. Scans were conducted from 4 to 60 ° at
a rate of 1°2θ/min. Mineral identifications were based
on an automatic search of the Joint Committee on Pow-
der Diffraction Standards18 (JCPDS) data file.
To meet European regulatory requirements con-
cerning landfill disposal, the environmental impact
o f t h e se wa st e m a t e r i a l s wa s a ss e sse d u s i ng a
DIN-38414-S4 leaching test. 19 This test is included
in the Proposal for a Directive on the landfill of
waste [COM (93) 275 final-syn 335] 20 to classify
wastes for landfilling. The test uses demineralized
water with a liquid to solid mass ratio of 10 to 1
and a particle size less than 10 mm. The mixture is
shaken in a closed vessel for 24 hours, and the
leachate is filtered and subsequently analyzed. Trace
metals were analyzed by the ICP-AES standard addi-
tion calibration method, sulphates by gravimetry
(UNE 83-432), 21 and chlorides by Mohr titration
(4500 B Method APHA, AWWA, WPCF). 22
Analytical Methods: Particle Size Distribution
Particle size distribution of fly ashes (MSWIa) and APC
residues (MSWIb) was determined by a Laser dispersion
particle size analyzer (Microtrac SRA 150), which allows the
measurement of particles between 0.7 µm and 700 µm (see
Figure 1 and Figure 2). Because three modal distributions
were obtained, samples were fractionated by granulometric
Volume 47 November 1997
 Alba, Gassó, Lacorte, and Baldasano

ranges, passing Table 2. Major elements (XRF) of MSW incineration residues sampled compared with those found in bibliography (Wiles, 1994).
through 100 µm, 400
µm, and 630 µm ASTM MSWIa (% dry residue) MSWIb (% dry residue) Wiles (1994) (% dry residue)
a
normalized sieves. Combined Fly Ash Bottom Ashes APC residues Bottom Ashes Fly Ashes APC residuesb

In the four fractions

Al2O3 9.6±0.1 12.74±0.03 17.0±0.1 7.075±0.005 4.16-13.80 9.26-17.01 2.27-15.69
obtained (<100 µm, 100-
P2O5 1.74±0.01 2.69±0 2.02±0.01 1.57± 0.02 0.32-1.47 0.01-0.06 0.39-1.05
400 µm, 400-630µm,
K2O 1.16±0.01 4.275±0.005 1.57±0.01 4.355±0.005 0.09-1.92 1.44-5.28 0.71-4.8
>630 µm) the following CaO 15.94±0.05 24.30±0.02 14.8±0.2 27.7± 0.1 5.18-16.80 10.36-18.20 15.40-49.00
determinations were CaOc 1.52±0.03 3.7±0.1
performed: Total Dis- SiO 45.21±0.09 18.76±0.04 39.2±0.4 15.00±0.01 19.47-66.34 20.33-44.90 7.70-25.68
2
solved Solids (TDS) was TiO 0.74±0.02 1.525±0.015 0.77±0.04 1.03±0.02 0.43-1.59 1.14-2.34 0.12-0.95
2
used as an operationally- MnO 0.075±0.005 0.12±0 0.085±0.005 0.06±0.00 0.01-0.31 0.10-0.25 0.03-0.12
defined extraction, the Fe2O3 5.43±0.01 1.57±0.01 10.4±0.4 1.44±0.03 0.59-21.45 1.72-6.29 0.37-10.15
constituents in the MgO 2.615±0.005 2.61±0.01 1.91±0.02 1.91±0.01 0.07-4.32 1.83-3.15 0.85-2.32
soluble fraction were Na O 5.11±0.07 5.78±0.01 3.46±0.05 4.12±0.01 0.39-5.67 2.03-7.70 1.03-3.92
2
d
characterized, and the SO3 2.9±0.1 6.4±0.1 1.81±0.08 8.18±0.03 --- --- ---

residues were charac- a

Bottom ashes + fly ashes.
terized with an opera- b
Dry/semi-dry APC residues.
tionally-defined loss c
Free CaO, dissolved in Ethilenglicol and titrated with 0.1 N HCl using blue bromotimol as an indicator, according to UNE 80-243.
on ignition (LOI). In dGravimetric Analysis precipitating as BaSO (UNE 83-432).
4
addition, major ele-
ments were analyzed by XRF, and minor and trace ele-
ments were analyzed by performing a total acid digestion
coupled by ICP-AES.
Determination of TDS was carried out using three
sequential demineralized water rinses at a liquid to
solid ratio of 100 to 1 using a 1-day extraction period
for each rinse. TDS percentage was calculated as the
average of two replicates, after calculating the sum of
the three sequential rinses for each fraction and re-
ported as percent solubles per dry residue. Ionic chro-
matography was performed to analyze Cl-, NO2-, NO 3-,
PO43-, and SO42- in the soluble fraction; only Cl- and
2-
SO4 were found at a detectable level. ICP-AES was used
to quantify heavy metal concentrations in the soluble
fraction.
LOI was used to determine the amount of mass
that could be driven at moderate temperatures. This
wo u l d i ncl ude o rg a ni c co nst i t u ent s, wa t ers o f
hydratation, and highly volatile metals. It was deter-
mined by averaging the mass difference of two repli-
cates for each fraction, when dried samples were placed
in an ashing oven and heated to 700-800 °C over 1
hour (UNE 83-433).23 Results of LOI from different fa-
cilities are not directly comparable. Because the tempera-
ture of the flue gases exiting the heat recovery units are
much lower than the 700-800 °C temperature used in
this test, any flue gas reaction products that condense
out or sorb onto the ashes from APC systems are
re-volatilized during muffling. In addition, a portion of
volatile material (LOI) in the residues from lime-based
APC systems is attributed to loss of water of hydratation
at 700-850 °C from the excess of lime added.24
RESULTS AND DISCUSSION
Bulk Chemical Analysis
The major elements composing the four MSWI residues
sampled are summarized in Table 2. As shown in the table,
fly ashes (MSWIa) have a total SiO2, Al2O3, and Fe2O3 con-
tent of 33.07%, a CaO content of 24.3%, an SO3 content
of 6.4%, and a free CaO content of 1.52%. APC residues
(MSWIb) have a total SiO2, Al2O3, and Fe2O3 content of
23.51%, a CaO content of 27.7%, an SO3 content of 8.18%,
and a free CaO content of 3.7%. For its chemical composi-
tion, both residues would not meet specifications estab-
lished to use coal fly ashes as a filler in concrete (UNE 80-302
specifications25 establish that SiO2 + Al2O3 + Fe2O3 3 2/3).
According to ASTM C618-92a, coal fly ashes classification,
these residues could be classified as Type C (sulfocalcium
fly ashes).26 The MSWIa facility showed a high CaO con-
tent, comparing with data reported in the same type of
facilities. This can possibly be attributed to feeded waste.
The high CaO content has also been confirmed by the
analysis as being a function of particle size (see Table 3).
Using XRD and analysis of Free CaO content, it is shown
that MSWIa has a higher content of Ca in a silicated-
aluminated matrix (2 CaO. SiO2 and 3CaO. Al2O3 ), al-
though not necessarily related to a scrubber injection pro-
cess. Results confirm that Ca present in both residues are
not exactly the same species, but further chemical specia-
tion studies are needed.
Table 2 also summarizes the major element composi-
tion (% dry residue) of these types of wastes found in a
review paper.27 Comparing these values with those obtained
in this study, one can appreciate that most of them are
between ranges found in the literature. The main differ-

Volume 47 November 1997 Journal of the Air & Waste Management Association 1173
Alba, Gassó, Lacorte, and Baldasano

Table 3. Chemical analysis from fly ashes (MSWIa) and APC residues (MSWIb) as function of particle size.

Fly ashes (MSWIa) APC residues (MSWIb)

< 100 (mm) 100-400 (mm) 400-630 (mm) > 630 (mm) < 100 (mm) 100-400 (mm) 400-630 (mm) > 630 (mm)

a) soluble fraction

pH 10.2 11.2 11.8 11.5 12.7 12.3 10.8 12.3

Cond. (mS/cm) 4.67 3.45 3.24 2.97 10.39 5.62 3.66 6.80
Cu (mg/l) 7.9±0.6 11±1 5.6±0.9 5.9±0.4 24±1 11.6±0.8 1.4±0.3 5.4±0.7
Zn (mg/l) 50±3 76±5 150±9 100±4 1484±18 1614±70 34±5 2076±91
Pb (mg/l) <DL <DL <DL <DL 2537±207 488±14 <DL 861±18
Cr (mg/l) 164±10 275±9 214±11 135±4 79±2 95 ± 4 27±6 72±5
Cl- (mg/l) 868±5 790±4 692±4 677±4 2014±12 1158 ± 7 1119±7 1118±6
SO42- (mg/l) 755±6 410±3 192±2 263±2 485±4 411 ± 3 76±1 1179±10

b) major elements (% dry residue)

Al2O3 11.48±0.04 13.03±0.06 14.99±0.04 14.5±0.5 4.13±0.08 10.40±0.02 12.505±0.005 7.245±0.005

P2O5 2.95±0.02 2.70±0.01 2.215±0.005 2.02±0.06 1.31±0.01 2.00±0.01 1.565±0.005 1.335±0.005
K2O 5.21±0.01 4.525±0.005 4.19±0 3.9±0.1 4.72±0.01 3.42±0.01 3.415±0.005 7.11±0.02
CaO 24.9±0.1 24.34±0.01 22.31±0.06 19.4±0.6 30.32±0.09 23.34±0.03 22.58±0.03 22.02±0.03
SiO2 16.5±0.2 19.73±0.03 22.96±0.02 21.5±0.7 8.9± 0.1 24.85±0.07 21.64±0.02 12.37±0.06
TiO2 1.56±0.03 1.48±0.01 1.50±0.01 1.38±0.01 0.79±0.01 1.48±0.01 1.205±0.005 0.99±0.01
MnO 0.195±0.005 0.1±0 0.06±0 0.065±0.005 0.06±0.01 0.08±0 0.07±0 0.06±0
Fe2O3 1.84±0.02 1.655±0.005 1.48±0 1.38±0.02 0.981±0.009 2.26±0.01 1.975±0.005 1.44±0.02
MgO 2.85±0.01 2.645±0.005 2.58±0 2.56±0.08 1.70±0.02 2.31±0 1.98±0.02 1.74±0.02
Na2O 5.84±0.04 5.66±0 5.48±0.05 5.5±0.1 4.36±0.02 3.59±0.02 3.275±0.005 6.10±0.02
Total(%) 73.3±0.5 75.8±0.1 77.7±0.2 72±2 57.3±0.3 73.7±0.2 70.21±0.1 60.4±0.1

c) minor and trace metals concentration (mg/kg)

Cr 952±31 744±31 574±7 379±32 314.2±0.1 372±2 310±12 1058±443

Zn 12781±269 11140±73 9057±436 7724±115 14896±236 10008 8360±33 12740±190
Pb 5281±72 6069±22 5537±195 5214±37 3343±86 2767±118 3802±138 5206±161
Ni 339±12 167±13 138±25 110±6 41±2 70 55±11 28±2

ences are that bottom ashes (MSWIb) have higher Al2O3
and P2O5, APC residues (MSWIb) have higher P2O5 and
Na2O concentrations, and fly ashes (MSWIa) have higher
CaO and P2O5, and lower SiO2 and Fe2O3.
Distribution of metals in MSWI depends on the va-
por pressure of metal compounds and the temperature of
the different residual streams produced.28 This typical be-
havior is followed by results shown in Table 4 (section b).
Fly ashes (MSWIa) and APC residues (MSWIb) are more
concentrated in Pb, Zn, and Cd, when compared with
bottom ash and combined ash, respectively. In both fa-
cilities, Cu is preferentially found in bottom ashes or
combined ash. In most cases (except Cu), metal con-
centration in combined ashes are between fly and bot-
tom ash concentrations. Recent studies of heavy metal
contents in similar types of residues report concentra-
tions of the same order of magnitude of those obtained
in this work.10,24,27,29
APC residues compared with fly ashes are enriched
in volatile elements such as Cd and Hg. This can be par-
tially due to the efficiency improvement of APC systems.
The distribution of metals among different types of ashes
is also influenced by the operating conditions of the in-
cinerator. For example, poor incinerator operating condi-
tions, such as those found in MSWIa (temperature under
850 °C), typically result in reduced vaporization of rela-
tively volatile metals and potentially increased carryover
of particulates, including uncombusted carbonaceous
material. These operating conditions result in increased
volumes of captured fly ashes that contain decreased con-
centrations of metals.24
Table 4 (section a) gives the total minor and trace
element content of four types of residue samples analyzed
by performing a total acid digestion. Table 4 (section b)
shows minor and trace metals extracted by an extractable
digestion procedure with aqua regia (ISO/CD11466). 17

1174 Journal of the Air & Waste Management Association Volume 47 November 1997
 Alba, Gassó, Lacorte, and Baldasano

Table 4. Minor and trace element concentrations in MSWI residues. fly ashes (MSWIa) in which no sorbents
are injected. In fly ashes from MSWIa,
ELEMENT MSWIa (mg/kg dry residue) MSWIb (mg/kg dry residue) typical minerals from portland cement
Combined Ashes Fly Ashes Bottom Ashes APC residues are found (2CaO.SiO2 and 3CaO.Al2O3),
which can account for the hydraulic ac-
a) analysis performed by a total acid digestion
tivity observed in these residues. It is
important to note that the presence of
Cr 227 ± 12 365 ± 18 210 ± 8 276 ± 13
Zn 4043 ± 557 9382 ± 208 2067 ± 9 11392 ± 187
high sulphate concentrations can cause
Pb 2542 ± 39 5461 ± 236 1693 ± 22 3117 ± 83 ettringite formation as an hydratation
Ni 92.54 ± 0.04 117 ± 2 53 ± 3 51.50 ± 0.08 product of cement.32
Cu 2188 1322 ± 90 822 ± 4 465 ± 19
As < 50* < 50 < 50 < 50 Leaching Test
Cd 21.5 ± 0.1 92 ± 2 < 12.5 132 ± 3 The chemical composition of leachates
Hg 0.34 ± 0.05 0.29 ± 0.03 < 0.035 2.89 ± 0.09 obtained through the DIN 38414-S4 stan-
dard test are presented in Table 6. Because
b) analysis performed by an extractable digestion of the high soluble compound content
of such residues, two sequential extrac-
Cr 114 ± 3 242 ± 3 70 ± 3 114 ± 1
tions were performed.19
Zn 3685 ± 17 8036 ± 120 1796 ± 45 10450 ± 38
Fly ashes (MSWIa) and APC residue
Pb 2370 ± 60 5312 ± 67 1471 ± 21 2930 ± 11
Ni 114 ± 4 123 ± 5 61.3 ± 0.9 48 ± 1
(MSWIb) leachates have high alkalinity
Cu 883 ± 15 1141 ± 18 808 ± 17 454 ± 3 (pH 12-13). Recent studies have shown pH
As < 33 < 33 < 33 < 33 of the same order in water-soluble extracts
Cd 17.6 ± 0.2 125 ± 2 < 8.5 128.5 ± 0.9 of the same type of residues, and high con-
ductivity (30,000 to 50,000 µS/cm), as a
result of the large amounts of soluble salts
The importance of describing the digestion protocol 33
(e.g., chlorides). Under these standardized conditions
performed is clear. It should be noted that chromium
compounds are usually associated with unreactive sili- Table 5. Crystalline phases observed using XRD.
cate matrices (spinel mineral lattices) and are poten-
tially unavailable for leaching, whereas for Zn, Pb, Ni, Crystalline phases MSWIa MSWIb
and Cd, both digestions give more similar results. Some Combined Ash Fly Ash Bottom Ash APC residue
works stated that, with a sequential chemical extrac-
tion procedure, more than 75% Cd in APC residues is Halite (NaCl) X X X X
Sylvite (KCl) X X
immediately available for mild leaching conditions and
Anhydrite (CaSO4) X X X
that a large proportion of Pb and Zn is available for
Calcite (CaCO3) X X X X
leaching under acidic conditions.24
Portlandite(Ca(OH)2) X
Quartz (SiO2) X X X X
Crystalline phases Gehlenite(Ca2Al2SiO7) X X X
The main crystalline phases observed by XRD are pre- Tricalcium aluminate(Ca3Al2O6)* X
sented in Table 5. The amorphous phase was also abun- Bassanite (CaSO40.5H2O) X X
dant in four samples. The main crystalline phases observed Ingersonite (Ca2SiO4)* X
are in good agreement with those previously reported.16,30 Iron (Fe) X
Halite (NaCl) and Sylvite (KCl) are the predominant min- Anorthite (CaAl2Si2O8) X
eral phases in fly ashes (MSWIa) and APC residues Illite X
(MSWIb). Expected heavy metal rich mineral phases (such Muscovite X
Calcium Chloride Hydroxide (CaClOH) X
as PbCl2 or K2ZnCl2) have not been identified. Different
Gismondine (CaAl2Si2O8.4H2O) X
authors suggest separation methods (magnetic and den-
Albite (NaAlSi3O8) X
sity separation) to concentrate over 2% on heavy metal
Microcline (KAlSi3O8) X
crystalline phases.9,16,31 The excess calcium added in the
Magnetite (Fe3O4) X
semi-dry scrubber in MSWIb is not found as lime in APC Hematite (Fe2O3) X
residues. Relatively soluble calcium sources in these resi-
dues are anhydrite, calcite, bassanite, and calcium chlo- *
Both minerals are typical of dehydrated portland cement chemistry (not found in APC
ride hydroxide. On the contrary, portlandite is found in residue).

Volume 47 November 1997 Journal of the Air & Waste Management Association 1175
Alba, Gassó, Lacorte, and Baldasano

Table 6. Composition of leachates obtained with DIN 38414-S4.

MSWIa MSWIb
Combined Ashes Fly Ashes Bottom Ashes APC Residues
1st Ext 2nd Ext 1st Ext 2nd Ext 1st Ext 2nd Ext 1st Ext 2nd Ext

TOC (mg C/l) 13.56±0.04 2.9±0.1 1.52±0.08 1.13±0.04 79.5±0.2 14.4±0.1 4.1±0.1 1.4±0.1
pH 11.4 11.1 12.3 11.5 11.3 10.2 12.7 12.9
Cond.(mS/cm) 3113 797 31580 4350 1723 799 48500 12900
Zn (mg/l) < 0.025 < 0.025 1.55±0.02 0.421±0.003 0.035±0.003 < 0.025 4.73±0.06 2.6±0.1
Pb (mg/l) < 0.05 < 0.05 9.9±0.1 < 0.05 < 0.05 < 0.05 48.0±0.3 9.6±0.4
Cr (mg/l) < 0.025 <0.025 < 0.025 0.82±0.02 < 0.025 < 0.025 0.103±0.006 0.082±0.008
Cu (mg/l) 0.28±0.03 0.059±0.001 < 0.025 < 0.025 0.86±0.03 0.187±0.009 < 0.025 < 0.025
Ni (mg/l) < 0.025 < 0.025 < 0.025 < 0.025 < 0.025 < 0.025 < 0.025 < 0.025
Cd (mg/l) < 0.025 < 0.025 < 0.025 < 0.025 < 0.025 < 0.025 < 0.025 < 0.025
Hg (mg/l) < 0.010 < 0.010 < 0.010 < 0.010 < 0.010 < 0.010 < 0.010 < 0.010
As (mg/l) < 0.1 < 0.1 < 0.1 < 0.1 < 0.1 < 0.1 < 0.1 < 0.1
Cl- (mg/l) 723±9 113±5 8460±50 740±15 248 85.08 15571±13 1046±25
SO42-(mg/l) 299±1 136±3 3110±20 1210±10 167 152 1410±20 1374±10

< =below detection limit

only Zn, Pb, and Cr are solubilized. The other trace ele- On the other hand, bottom ash (MSWIb) leachates re-
ments—Cu, Ni, Cd, Hg, and As—are under the detec- sults imply that they should be considered as inert resi-
tion limit. Combined ashes (MSWIa) and bottom ashes dues. It is clear from the results obtained that mixing bot-
(MSWIb) are both slightly less alkaline, and show lower tom and fly ashes is not advisable, as has been reported
conductivity values. Cu is found at detectable levels in previous studies.24
in both residues and Zn only in bottom ashes from
MSWIb. Characterization as a Function of Particle Size
In APC residues (MSWIb), it is important to note the Particle size distributions are shown in Figures 1a and 1b.
presence of high Pb concentrations attributed to the am- Fly ashes (MSWIa) and APC residues (MSWIb) follow a
photeric behavior of this metal. It is also noticeable, in trimodal size distribution, which influenced further
total agreement with previous studies,34 that metals con- granulometric separation in 4 fractions: < 100 µm, 100-400
tained in APC residues (mainly Zn and Pb) show a higher µm, 400-630 µm, and > 630 µm.
solubility under alkaline or mild conditions in compari- Due to its granulometric distributions, none of these
son with pure fly ash. This is attributed to the presence of residues would be accepted for use as filler in concrete
amphoteric species due to the addition of lime. by the Spanish standard (UNE 83.415),35 which only
The environmental impact of those residues has been accepts a maximum of 40% coal fly ashes retained on
assessed by the sum of results obtained in both sequen- a 45-µm sieve (fly ashes from MSWIa present 68% re-
tial extractions performed. In fly ashes (MSWIa), the con- tained and APC residues from MSWIb 58% retained)
centration of chlorides, sulphates, Pb, and Cr in leachates and a 15% coal fly ashes retained on a 90-µm sieve (fly
is higher than limits established in the European regula- ashes from MSWIa 48% retained and 44% APC residues
tion concerning waste disposal (ECC/Draft Directive of
93/C212/02)20 (Limits considered: Cl- < 6000 mg/l, SO42- <
Table 7. Granulometric distribution and LOI results (%) for different size ranges.
1000 mg/l, Pb < 2 mg/l, Cr < 0.5 mg/l). These results im-
ply that these residues should be treated before landfilling.
Particle Size Granulometric distribution Loss on Ignition (LOI)
APC residue (MSWIb) leachates show higher chloride lev- (µm)
els than fly ashes (MSWIa), as stated before. Concentra- Fly Ash APC residues Fly Ash APC residues
tions of Pb, chlorides, and sulphates in APC residues are (MSWIa) (MSWIb) (MSWIa) (MSWIb)
higher than those accepted in the mentioned legislation,
which classify them as harmful wastes that need treat- < 100 54.79 57.77 5.4 ± 0.4 16.1 ± 0.2
ment before landfilling. In Combined Ash (MSWIa) 100-400 36.90 31.74 7,765 ± 0.005 12.72 ± 0.07
leachates, only sulphate concentrations show high levels 400-630 6.95 9.01 9.1 ± 0.2 17.1 ± 0.5
compared to the above EU Directive, which specified that > 630 1.36 1.48 14.2 ± 0.1 15 ± 1

these residues should be considered as harmful wastes.

1176 Journal of the Air & Waste Management Association Volume 47 November 1997
 Alba, Gassó, Lacorte, and Baldasano

from MSWIb). The addition of lime

in the MSWIb APC system causes
an alteration in granulometric
distribution, raising slightly the
percentage of particles lower than
100 µm.
Table 7 shows the percent-
age of particles, and the relation-
ship between particle size distri-
butions and LOI, for each sieved
fraction. For fly ashes (MSWIa),
the mass lost at 700-800 °C is
greater in the largest fractions
based on the organic content
and the ability of the charcoal
particles to absorb organics and
metals. These results are in good
agreement with results previ-
ously reported.11 The LOI of APC
residue (MSWIb) behavior is not
the same as reported earlier;11
higher values of LOI and less
soluble solids are found in the
middle size ranges (400-630 µm).
As can be seen from Table
7, the LOI of APC residues
(MSWIb) is higher than in fly
ashes (MSWIa). As previously
stated, this does not lead to the
conclusion that combustion ef-
ficiency in MSWIa is higher than
in MSWIb.
Figure 2 and Table 3a present
results from total dissolved sol-
ids and the concentration of ana-
lyzed species in the soluble frac-
tion as a function of particle size.
This figure shows that fly ashes
(MSWIa) and APC residues
(MSWIb) follow a different TDS
trend than previously reported.11 Figure 3. Comparison of total heavy metals concentration in fly ash (MSWIa) and APC residues (MSWIb),
In both residues, the more expressed in mg/kg dry residue and TDS-corrected mg/kg insoluble residue.
soluble fractions are the small-
est sizes followed by the largest ones. This parabolic trend sulphates follow a TDS parabolic trend. Only three
is significantly more accentuated in APC residues heavy metals have been detected in each size fraction:
(MSWIb). These results corroborate that using lime as a Cu and Cr (having a maximum in the 100-400 µm frac-
sorbent in APC systems generates a waste with altered tion), and Zn (with a maximum concentration in the
leaching properties and more soluble material. TDS re- 400-630 µm fraction).
sults from APC residues (MSWIb) are in agreement with Analysis of soluble fractions extracted (Table 3a) in APC
LOI values, showing that charcoal particles (insoluble sol- residues (MSWIb) shows a decrease of metals and soluble
ids) are concentrated in the 400-630 µm range. salts in the 400-630 µm range, which agrees with its less
As can be seen from Table 3a, chlorides in fly ashes solubility and higher LOI. Chlorides follow the same distri-
(MSWIa) are concentrated in the smallest range while bution as in MSWIa fly ashes, with higher concentrations

Volume 47 November 1997 Journal of the Air & Waste Management Association 1177
Alba, Gassó, Lacorte, and Baldasano
in the smallest fraction, explaining in part the higher solu-
bility of this fraction. The largest particles are significantly
enriched in sulphates, explaining the solubilities found
in them. Pb and Cu solubility follow chloride profiles,
whereas Zn follows sulphate distribution.
In Table 3b, major element results are presented for
both residues as a function of particle size. Major element
concentrations agree with TDS results. Fly ashes (from
MSWIa) follow an expected trend, with higher lime con-
centrations in the smallest fraction (more soluble), and
higher concentrations of insoluble aluminate-silicate
matrix in the largest particles (400-630 µm and > 630 µm).
APC residues (MSWIb) have higher Al2O3 and SiO2 con-
tents in central fractions (less soluble). The smallest size
fraction is clearly enriched with lime, which corresponds
to results previously reported.11
Heavy metal profiles of fly Ashes (MSWIa) and APC
residues (MSWIb) are shown in Table 3c. In APC residues,
metal concentration profiles were corrected based on the
amount of soluble solids. It was assumed that the soluble
portion of the APC residues (MSWIb) is attributed mainly
to the scrubber and the insoluble portion to fly ashes (see
Figure 3a to 3g).
Two major trends can be observed while examinating
both residues. In Fly Ashes (MSWIa), Cr, Zn, Ni, and Cu
concentrate on the smallest particles. These results
have been previously reported 11 and the explanation
is attributed to volatilization/condensation reaction.
Metals volatilize and condense back on the surface of
the ash particles when temperature is below the boil-
ing point of metal. Because the smallest particles have
the lower mass and largest surface area, they achieve
the temperature of the flue gas faster as it is cooled in
the energy recovery system.11 Hg has been found to be
associated with the largest particles. Pb and Cd present
higher and very similar concentrations in < 100 µm and
100-400 µm particles.
APC residues (MSWIb) present heavy metal pro-
files different from those mentioned above. Hg con-
centrates in the middle ranges, in agreement with
higher LOI results, assuming that it concentrates in
the poorest incinerated particles, which correlates with
the ability of the char particles to absorb metals and
the fact that powdered activated carbon is used to scrub
out Hg. Other heavy metals (except for Ni, mainly
found in the middle ranges) are concentrated in the
smallest or largest particles (the trend is more marked
while expressing results with TDS correction) follow-
ing a parabolic distribution, as TDS results. Cu, Cd, and Zn
present higher concentrations in the smallest particles; Cr
and Pb in the largest ones. No significant differences have
been found between profiles followed by volatile and non-
volatile metals (with the exception of Hg). These results
1178 Journal of the Air & Waste Management Association
show that heavy metals follow profiles associated with
lime and soluble salts (e.g., Cl-) and generally are not
associated with the silicate-aluminate matrix (enriched
in middle ranges). Results obtained show clearly the ef-
fect of lime addition in APC systems in metal speciation
and distribution.
CONCLUSIONS
In this study, residues from two types of incinerator
facilities—first generation (mass burn, electrostatic pre-
cipitator as air pollution control system) and second
generation (RDF, semi-dry APC control system)—have
been characterized.
It has been confirmed that combined (MSWIa) and
bottom (MSWIb) ashes have lower concentrations of Pb,
Zn, and Cd when compared to fly ashes (MSWIa) and
APC residues (MSWIb), respectively. In both facilities, Cu
is preferentially found in bottom and combined ashes.
Volatile metals such as Cd and Hg are more concentrated
in APC residues than in fly ashes. This can be due to the
increasing efficiency of APC systems and also can be in-
fluenced by poor incinerator operating conditions found
in MSWIa (temperature under 850 °C); thus, it can result
in relatively reduced vaporization of volatile metals and
potentially increased particulate material (uncombusted
carbonaceous material).
It has also been shown that digestion procedure has
to be well specified; otherwise it can lead to incompa-
rable results. When the standard leaching test
(DIN-38414-S4)18 is carried out, metal solubility in APC
residues is higher than in fly ashes, although total metal
content may be lower (i.e., Pb). These results can be at-
tributed to the presence of higher soluble fractions, such
as chlorides removed from flue gas. According to ECC/
Draft Directive of 93/C212/02,19 both fly ashes (MSWIa)
and APC residues (MSWIb) would be classified as poten-
tially toxic and would need to be treated before landfilling.
Regarding metal distribution as a function of particle
size, it is important to note the different behavior fol-
lowed by fly ashes and APC residues. Fly ashes follow
trends previously reported in literature, with higher metal
concentrations mainly found in the smallest, most soluble
particles. Hg in fly ashes concentrates in the largest par-
ticles, which present higher LOI values and are presum-
ably not incinerated effectively.
In APC residues (MSWIb), metals follow a parabolic distri-
bution with higher concentrations in the smallest and largest
particles. Analysis of soluble fractions leads to the identifica-
tion of a granulometric range (400-630µm) with low concen-
trations of metals and salts, which agrees with its less solubility
and higher LOI values, as well as a higher Hg content.
Results show that heavy metals follow profiles asso-
ciated with lime and soluble salts (except Hg) and they
Volume 47 November 1997

are not associated with the silicate-aluminate matrix. It is
reflected that the addition of a sorbent such as lime in
APC systems has a great effect on metal speciation, leach-
ing, and particle size distribution.
ACKNOWLEDGMENTS
The authors would like to thank the Spanish Ministerio de
Educación y Ciencia for a grant to support the work of Nuria
Alba. Also, the authors express their appreciation to Serveis
Científic-Tècnics of Universitat de Barcelona for its analyti-
cal assistance, as well as TERSA and Centre Integral de
Tractament de Residus del Maresme, that kindly provided
logistical support and access to sampling sites. The support
of the Junta de Residus of the Dpt. de Medi Ambient of the
Generalitat de Catalunya is also appreciated.
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Volume 47 November 1997
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About the Authors
Nuria Alba is a Ph. D. student of the Environmental Engi-
neering Program at the Institute of Environmental Technol-
ogy and Modelling (ITEMA) in the Universitat Politècnica de
Catalunya (UPC), Catalonia, Spain. Dr. Santiago Gassó is
presently Senior Research in the ITEMA and associate pro-
fessor in Engineering Projects in the High Technical School
of Industrial Engineers at UPC. Teresa Lacorte is senior
chemist in charge of ITEMA’s laboratory. Dr. José Mª
Baldasano is currently full professor in Environmental Sci-
ence and Technology in the High Technical School of Indus-
trial Engineers and Director of ITEMA at UPC. Correspon-
dence should be addressed to Dr José M. Baldasano, Institut
of Environmental Technology and Modelling (ITEMA), apdo.
correos 508, 08220 Terrassa (Barcelona), Spain.
Journal of the Air & Waste Management Association 1179