Marine Pollution Bulletin 57 (2008) 867872

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Marine Pollution Bulletin

journal homepage: www.elsevier.com/locate/marpolbul

Recycling of harbor sediment as lightweight aggregate

Yu-Ling Wei a,*, Jing-Chiang Yang a, Yong-Yang Lin a, Shih-Yu Chuang a, H. Paul Wang b,c
a
b
c

Department of Environmental Science and Engineering, Tunghai University, Taichung City 407 Taiwan
Department of Environmental Engineering, National Cheng-Kung University, Tainan City 701, Taiwan
Sustainable Environment Research Center, National Cheng-Kung University, Tainan City 701, Taiwan

a r t i c l e

i n f o

Keywords:
Sintering
Bloating process
Sediment recycling
Lightweight aggregate
Fe K-edge XANES

a b s t r a c t
Sediment sampled from Taichung Harbor was mixed with local reservoir sediment at different weight
ratios to prepare lightweight aggregate at 1050, 1100, and 1150 C. A pressure of 3000 or 5000 psi was
used to shape the powder mixtures into pellets before the heating processes. The results indicate that
the leaching levels of trace metals from the lightweight aggregate samples are considerably reduced to
levels less than Taiwan Environmental Protection Administration regulatory limits. Increasing nal process temperature tends to reduce the bulk density and crushing intensity of lightweight aggregate with a
concomitant increase in water sorption capability. Lightweight aggregate with the lowest bulk density,
0.49 g cm 3 for the 5000 psi sample, was obtained with the heating process to 1150 C. Based on the
X-ray absorption near edge structure results, FeSO4 decomposition with a concomitant release of SOx
(x = 2, 3) is suggested to play an important role for the bloating process in present study.
2008 Elsevier Ltd. All rights reserved.

1. Introduction
There has been extensive usage of lightweight aggregate (LWA)
materials in civil engineering, such as construction of tall building
to achieve the purpose of weight lessening, without losing the
function as thermal insulator and sonic barrier. The LWA materials
have also been applied to road and bridge construction for transportation. Other applications include soil engineering, gardening,
and ltering (Cheeseman et al., 2005). Natural resources used for
manufacturing LWA materials cover the ashes from incinerator
and coal power plant, volcanic ash, pumice, siliceous rock, shale,
and others (Cheeseman et al., 2005; Chiou et al., 2006; Hossain,
2004; Mladenovic et al., 2004). However, in most industrialized
and many developing countries, because the raw materials from
natural environment for the manufactures of LWA have been
depleting and because there is increasing public concerns on the
environmental impact arising from mining the natural raw materials, there is a worldwide tendency towards using waste as a substitute for the natural raw materials (Cheeseman et al., 2005). It has
been pointed out that waste materials containing shale, clay, slag,
sediment, and sewage sludge can be employed for the purpose of
manufacturing lightweight aggregate on condition that the chemical composition and particle size distribution are suitable for the
sintering and vesicant processes to take place in desired time order
when heated from room temperature to a typical high temperature, such as 11501200 C (Holm and Valsangkar, 1993). Riley
* Corresponding author. Tel.: +886 42 359 1368; fax: +886 42 359 6858.
E-mail address: yulin@thu.edu.tw (Y.-L. Wei).
0025-326X/$ - see front matter 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.marpolbul.2008.03.033

has suggested appropriate compositional ranges of raw material

to be suitable for manufacturing LWA. The suitable chemical composition of clay is: 4870% SiO2, 825% Al2O3, 312% FeO + Fe2O3,
112% CaO + MgO, and 0.57% K2O + Na2O. Fe2O3, CaO, Na2O, and
K2O are necessary ux (Riley, 1951; Chiou et al., 2006).
Some necessary conditions are required for the lightweight
aggregate formation of a specimen. First, glassy surface with enough viscosity must be formed through sintering reaction when
the specimen is heated to a pre-set high temperature. Second, after
the sintering reaction the specimen should be able to evolve enough amount of gas through vesicant process. The sintering reaction needs to occur no later than vesicant process to encapsulate
the evolved gas under glassy surface (Riley, 1951; Bhatty and Reid,
1989; Skrifvars et al., 1994).
Various bloating mechanisms associated with Fe compounds
have been previously proposed. Upon heating Fe2O3 decomposition to Fe3O4, FeO, and O2 is often employed to explain bloating
phenomenon, because Fe oxides are abundant in the earth crust.
O2 gas is responsible for bloating in this case. Despite the intensive
applications of LWA materials, the change of Fe speciation prior to
and after sintering and vesicant processes is case-dependent and
difcult to examine. Previous studies tend to not focus on examining the role played by Fe compounds due to the complexity of the
raw material matrix and due to the lack of proper instrumental
tools, thus most previously proposed bloating mechanisms associated with the change of Fe compounds are somewhat non-persuasive. However, with the growing usage of synchrotron-based X-ray
absorption spectroscopy (XAS) in environmental studies, it is possible to gain more insight into the role played by Fe compounds in

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Y.-L. Wei et al. / Marine Pollution Bulletin 57 (2008) 867872

the sintering and vesicant processes. Molecular environmental science with XAS technique has emerged to provide information
needed for a long-term solution of environmental remediation
and waste management (US DOE, 1995). An XAS spectrum, including X-ray absorption near edge structure (XANES) and extended Xray absorption ne structure (EXAFS), is capable of revealing speciation, distribution, form transformations, and mobility of target
metal (US DOE, 1995). The aim of this study is to study the feasibility of recycling sediment from Taichung Harbor of Taiwan as a raw
material for manufacturing LWA and to apply XAS technique to
investigate the change of Fe speciation prior to and after the sintering and vesicant processes.
2. Experimental methods
The experimental owchart is depicted in Fig. 1. Two sediments
were sampled: one from Taichung Harbor of Taiwan and the other
from a local reservoir. The reservoir sediment has been well studied and it is regarded as a satisfactory raw material for commercially manufacturing LWA. The reservoir sediment used in this
study is intended for comparison with the harbor sediment. Prior
to forming the pellet by the use of a pressure shaping method,
the sediment sampled from Taichung Harbor was thoroughly
end-to-end mixed with the local reservoir sediment at ve different weight ratios (100:0, 80:20, 60:40, 40:60, 20:80, and 0:100)
in a mixer which rotated at a speed of 30 rpm for 24 h. Preweighed amount of the sediment mixture was then loaded into a
stainless-steel holder, and pressurized into a disk-like dense pellet
by the use of a pressure shaping machine which is equipped with a
pressure gauge. Two different pressures, 3000 and 5000 psi, were
applied to the sediment mixtures to shape them into dense pellets.
The sizes of the dense pellets (8.00 g in weight) shaped with 3000
and 5000 psi are 4.1 and 3.6 cm3, respectively. To successfully prepare lightweight aggregate through sintering and vesicant pro-

Raw sediments

Dried at 105 C

Characterization
Ground to < 50mesh

of raw materials
with various

Mixed at different proportions

instruments

Shaped at 3000 and 5000 psi

cesses at 10501150 C, the dense pellets needed to experience a

de-volatile pretreatment process at much lower temperature than
10501150 C. The de-volatile (preheating) process at 500 C,
determined with a thermogravimetric analyzer, is intended to
drive out most organic components in order to avoid blasting the
pellet into small pieces, while being subjected to the subsequent
10501150 C heating process for 18 min. The sintering duration
was determined to be 18 min, because we found that such duration
could lead to satisfactory sintering thickness, approximately 1 mm.
Approximately, this time duration is also being used by a local
plant to generate light aggregate from the same reservoir sediment
employed in our study. For the de-volatile process, the dense pellets were gradually heated from room temperature to 500 C in
2 min and, subsequently, the temperature was held at 500 C for
another 2 min under atmospheric environment in a temperatureprogrammed electric furnace to drive out most organics. The devolatile pellets were then discharged and ready for the sintering
and vesicant processes. They were placed in alumina crucibles
and introduced into the furnace that has already reached a preset temperature (i.e., 1050, 1100, and 1150 C), and stayed inside
the furnace for 18 min.
After the 10501150 C process, the bulk density of LWA samples was measured based on Archimedes Principle (Cheeseman
et al., 2005). Note that the sizes of all LWA samples were measured
by immersing them into water by using a very slim metal wire to
suppress them downward. Because the difference in percent
weight loss after sintering is negligible (only approximately 1%),
the size of the LWA sample is inversely proportional to the bulk
density. The sizes of the LWA samples are in the 6.015.4 cm3
range. Water absorption capacity for the LWA samples was determined according to a method formulated by Taiwan government
(Taiwan CNS, 1993). The basic principle behind the water absorption capacity is to determine the amount of water absorbed by
LWA in 24 h (Taiwan CNS, 1993). The capability of the LWA samples against crushing was estimated with an auto-compressor device equipped with a microprocessor-control console. Pb toxicity
characteristic leaching procedure (TCLP) concentrations in all samples were determined with a ame atomic absorbance spectrometer (FAAS) based on the method formulated by US EPA (US EPA,
1992). The calibration curves have Pb concentration span 1.00
10.0 mg L 1 with the correlation coefcient >0.9995.
All Fe K-edge XAS spectra were recorded on the wiggler C (BL17C) beam-line at the National Synchrotron Radiation Research
Center (NSRRC) of Taiwan. During the XAS experimentation, the
facility had storage energy 1.5 GeV, an electric current 120
220 mA, and the energy spanning was 415 keV for the monochromator. The K-edge jump for Fe is 7112 eV. All XAS spectra from
reference compounds (Fe metal, Fe(OH)3, Fe2O3, Fe3O4, FeO, and
FeSO4) were recorded in transmittance mode at room temperature;
while the XAS spectra from lightweight aggregate samples and
sediment were all recorded in uorescence mode. Data reduction
was carried out using WinXAS software (Ressler, 1998).

Pretreated at 500 C for 2 minutes

3. Results and discussion

o

Thermally treated at 1050, 1100, and 1150 C

Characterization of the lightweight aggregate samples

(e.g., XRD, XAS, TCLP, weight loss,
bulk density, and absorption rate)

Fig. 1. Experimental owchart.

The main chemical compositions of these sediments are listed

in Table 1. Rigorous quality assurance and quality control approaches formulated by Taiwan Environmental Protection Administration (EPA) were referred to in performing the chemical
composition analyses in this study. These two sediments are generally similar in chemical compositions. Both sediments meet the
criterion in chemical compositions suggested for suitable raw
material for preparing LWA (Riley, 1951).
Presented in Table 2 are the Pb TCLP concentrations (mg L 1)
from all LWA samples. The environmental regulatory limit for Pb

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Y.-L. Wei et al. / Marine Pollution Bulletin 57 (2008) 867872

Table 1
Chemical compositions of harbor and reservoir sediments

1050 C

1100 C

1150 C

3000

0
20
40
60
80
100

1.19
0.84
0.65
0.55
0.51
0.28

0.37
0.35
0.36
0.29
0.22
0.26

0.24
0.20
0.23
0.10
0.22
0.18

0
20
40
60
80
100

0.12
0.13
ND
ND
ND
0.13

ND
ND
ND
ND
ND
ND

ND
ND
ND
ND
ND
ND

5000

ND: <0.092 mg L

40

20

20

0
100

0
100

80

80

60

60

Fractional Weight Percentage

Cumulative Weight Percentage

40

40

20

20

0
59
0
59
011
90
11
90
-2
00
0

Reservoir sediment fraction

(%)

40

7-

Shaping pressure
(psi)

60
Cumulative Weight Percentage

29

Table 2
Pb TCLP concentration from all lightweight aggregate samples

Fractional Weight Percentage

60

74
-1
49
14
929
7

Analyzed according to Taiwan CNS 11393 M3184 method (formulated in 1985).

Weight loss after heating at 900 C for 3 h. Since Taiwan regulatory TCLP limits
for Pb, Hg, As, Cd, Cu, and Cr are 100, 4, 100, 20, 300, and 100 mg kg 1, respectively;
thus only Pb was concerned for its leaching level from lightweight aggregate
samples.

80

-7
4

80

28.90%
7.57%
4.05%
1.02%
2.55%
0.32%
0.18%
212.8 mg kg 1
0.037 mg kg 1
6.46 mg kg 1
ND
ND
ND
5.72%

53

31.53%
7.67%
4.32%
2.52%
1.15%
0.51%
0.59%
84.6 mg kg 1
0.034 mg kg 1
6.69 mg kg 1
ND
ND
ND
4.17%

100

25

Sia
Al
Fe
K
Na
Ti
Ca
Pb
Hg
As
Cd
Cu
Cr
LOIb

100

<
2

Harbor sediment

Fractional Weight Percentage (%)

Reservoir sediment

Cumulative Weight Percentage (%)

Element

Particle Size (m)

Fig. 2. Particle size distribution of sediments sampled from a local reservoir (top
panel) and Taichung Harbor (bottom) in Taiwan.

10

3000 psi

1050 oC

1100 oC
1150 oC

Weight Loss (%)

ofcially enforced in Taiwan is 5.0 mg L 1 that can be translated to

100 mg kg 1 sample according to the TCLP procedure (US EPA,
1992). The Pb TCLP concentrations from all LWA samples meet
the regulatory limit. Other trace metals regulated by Taiwan EPA
in terms of TCLP concentration are Hg, As, Cd, Cu, and Cr. Table 1
shows that, for Hg, As, Cd, Cu, and Cr, the contents of each trace
metal in the raw sediments are lower than their regulatory limits
enforced by Taiwan EPA. Thus the TCLP test of these trace metals
from all LWA samples is not performed.
Fig. 2 shows that particle size distribution of harbor sediment is
slightly coarser than the reservoir sediment. The <2 lm fraction is
approximately 3738% for both sediments. However, the total reservoir sediment is ner in size. Finer particle size is responsible for
easier occurrence of sintering reaction to form glassy shell (surface) to encapsulate the gases evolved during the subsequently occurred bloating reaction. Fig. 3 presents the weight loss percentage
of the specimen after the 10501150 C sintering processes. The
weight loss for all samples is in the 68% range. This observation
is slightly greater than the LOI listed in Table 1, because the LOI
was determined at 900 C, that is lower than the temperatures
used for the sintering and bloating processes.
Fig. 4 depicts the bulk density of the LWA samples prepared
from sediment mixtures of different weight ratios and different
formation pressures. The LWA bulk density always decreases with
increasing nal temperature. Their bulk density is about 0.49
1.26 g cm 3. LWA with the lowest bulk density was obtained by

10
6

5000 psi
9

1050 oC
o
1100 C

1150 oC

6
0

20

40

60

80

100

Fraction of Reservoir Sediment (%)

Fig. 3. Weight loss of lightweight aggregates after sintering at 1050, 1100, and
1150 C.

Y.-L. Wei et al. / Marine Pollution Bulletin 57 (2008) 867872

1050 oC
1100 oC

3000 psi

1150 oC

Bulk Density (g cm-3)

0
1050 oC
1100 oC

5000 psi

1150 oC

0
0

20

40

60

80

100

Fraction of Reservoir Sediment (%)

Fig. 4. Bulk density of lightweight aggregates prepared with sintering at 1050,
1100, and 1150 C.

the processes at 1150 C: 0.49 and 0.69 g cm 3 for the 5000- and
3000 psi samples, respectively. It is noted that the generally
acceptable bulk density of LWA is <2.0 g cm 3 and LWA with different bulk density has various practical applications. This gure
shows that the LWA bulk density generally decreases with increasing fraction of reservoir sediment, because the average particle size
of the reservoir sediment is smaller than the harbor sediment; in
other words, the pellets containing more fraction of reservoir sediment are more closely packed. This would favor encapsulation of
the gases produced during the bloating process, leading to less bulk
density; however such trend is not observed for the results associated with 3000 psi and 1050 C (see the upmost curve in Fig. 4). To
explain this exceptional observation, we suggest that the benet of
ner particle size for easier sintering might have been offset by
both lower shaping pressure (3000 psi) and the richer Si + Al + Ca
content in the reservoir sediment (see Table 1). Note that SiO2,
Al2O3, and CaO all have relatively high melting point, consequently
greater content of these constituents would result in slower sintering reaction; thereby the gases generated by the bloating reaction
have more opportunity to slip out to the atmosphere through the
still-open interparticle space.
The effect of pellet shaping pressure on the LWA bulk density is
also indicated in Fig. 4. A general trend of decreasing bulk density
with increased shaping pressure is observed. This trend can be explained in a simple way by the fact that particles closer to each
other are easier to be brought together and sintered at elevated
temperature. Thus, the pellets shaped with greater shaping pressure would take less time to form the sintered layer (i.e., the shell)
which is glassy and considerably smooth. Once the shell is formed,
the gases generated during the subsequent vesicant process would
expand the shell dimension and the core region becomes porous
with the gases caught inside, resulting in less density of the light
aggregate.

Fig. 5 presents the water sorption capacity of the LWA samples

prepared at 10501150 C from the mixtures containing different
weight ratios of sediments and shaped with different pressures.
The generally acceptable water sorption capacity is 220% for practical civil engineering purpose, which is met by all LWA samples as
presented in Fig. 5. Fig. 5 indicates that as the fraction of reservoir
sediment increases, the LWA generally has less water absorption
capacity. The LWA samples produced from the reservoir sediment
have less water absorption capacity, as compared with that from
the harbor sediment, because the former sediment is ner in size,
and therefore easier to be sintered to form glassy surface. In addition, an increase in process temperature is observed to generally
lead to more water absorption capacity, presumably due to the following reason. Although the processing environment at higher
temperature would cause more active particle movement for easier
sintering reaction, it could also result in more vigorous gas production during the bloating process. The bloating process was so rigorous as to provide the vesicant gases with enough energy, and part
of the energized gases escaped to the atmosphere by tunneling
through the sintered shell with some tiny pores left behind on
the sintered surface. As to the pressure effect on the water absorption, LWA samples formed at 5000 psi, as compared to 3000 psi,
does not result in considerable change in water absorption
capacity.
Fig. 6 shows the crushing intensity of LWA samples prepared
with heating at 1050 and 1100 C. This gure indicates that higher
shaping pressure (5000 psi) leads to stronger crushing intensity;
this is due to the closer package of the particles, therefore better
sintering for the shell of the pellets. For the effect of temperature
on the crushing intensity, the general trend of the crushing intensity vs. temperature considerably corresponds to the trend of bulk
density vs. temperature presented in Fig. 4. Higher process temper-

16
14

3000 psi
1050 oC

12

1100 oC
1150 oC

10

Water Absorption Capacity (%)

870

8
6
4
16
14

5000 psi
1050 oC

12

1100 oC
1150 oC

10
8
6
4
0

20

40

60

80

100

Fraction of Reservir Sediment (%)

Fig. 5. Water absorption capacity of lightweight aggregates prepared with sintering
at 1050, 1100, and 1150 C.

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Y.-L. Wei et al. / Marine Pollution Bulletin 57 (2008) 867872

3500

2.0

105 oC raw sediment

1.5
3000 psi
1050 oC

3000

1.0
0.5

o
1100 C

0.0
2.0

Normalized Absorption (Arbitary Unit)

2500

Crushing Intensity (psi)

2000

1500

1000
5000 psi
3000

2500

2000

40

60

80

0.0
2.0

1050 oC-shell

1.5
1.0
0.5
0.0
2.0

1150 oC-core

1.5
1.0
0.5
1150 oC-shell

1.0

1000
20

0.5

1.5

1100 oC
0

1.0

0.0
2.0

1050 oC

1500

1050 oC-core

1.5

0.5

100

0.0

Amount of Reservoir Sediment (%)

7.12

7.16

7.18

7.12

7.14

7.16

7.18

Photon Engergy (keV)

Fig. 6. Crushing intensity of lightweight aggregates prepared with sintering at 1050

and 1100 C.

Fig. 7. XANES spectra (left) and their corresponding rst-derivative spectra (right)
from harbor sediment and lightweight aggregates prepared with sintering at 1050
and 1150 C. The vertical dotted lines running through each panels are intended for
easier comparison among various samples.

Normalized Absorption (Arbitary Unit)

ature (1100 C) results in less crushing intensity, which is suggested to be due to the rigorous bloating process at 1100 C, thereby providing the vesicant gases with enough energy to escape to
the atmosphere by tunneling through the sintered shell with some
tiny pores left behind on the glassy surface. In addition, because
the crushing intensities for all 1150 C LWA samples are less than
the minimum detection limit of the auto-compressor device,
166 psi, therefore being excluded from Fig. 6. Despite the considerably lower crushing intensity for the 1150 C LWA samples than all
samples manufactured at 1050 and 1100 C (i.e., 17273046 psi),
the 1150 C LWA samples, when properly incorporated into cement, may be able to effectively reduce the total density of the cement specimen while still retaining reasonable crushing strength
for the LWA-incorporated cement specimen because the strength
may be contributed by cement.
Fig. 7 presents the Fe K-edge XANES spectra from the LWA samples prepared from harbor sediment (not containing reservoir sediment). Each LWA sample was divided into two parts: shell and
core regions. The shell region corresponds to the glassy surface,
and the core region represents the bloating part. The main edge
peak (as indicated by the arrow in each panel) in the XANES spectra from all LWA samples, except the 1050 C-core, shifts toward
greater photon energy, indicating an increase in average oxidation
state of Fe. This is in contrast to the generally accepted mechanism
that during the vesicant process, the average oxidation state of Fe
decreases due to the transformation of Fe2O3 into Fe3O4, FeO, and
O2. Fig. 8 shows the results based on the simulation of XANES spectrum from raw harbor sediment using WinXAS program (Ressler,
1998). The Fe speciation in raw harbor sediment consists of
36.8% Fe2O3, 30.1% Fe3O4, 13.4% FeO, and 19.7% FeSO4. As indicated
in Fig. 7, the average oxidation state of Fe tends to increase after

7.14

2.0
harbor sediment
1.5

1.0

0.5

Fe2O3 36.8 %
FeO 13.4 %

Fe3O4 30.1 %
FeSO4 19.7 %

0.0
7.12

7.14

7.16

7.18

Photon Engergy (keV)

Fig. 8. Results from simulation of XANES spectrum for harbor sediment.

the sintering and bloating processes, we suggest that FeSO4 decomposition with a concomitant release of SOx might have played an
important role for the bloating process in present study. Noted that
this study also attempted to simulate other XANES spectra for
obtaining Fe speciation in LWA samples, however it is unsuccessful
due to the unavailability of a complete set of Fe reference

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Y.-L. Wei et al. / Marine Pollution Bulletin 57 (2008) 867872

compounds; in other words, part of Fe compounds might have

chemically reacted with other compositions of the harbor sediment to form very complex structures.
4. Conclusions
Sediment sampled from Taichung Harbor is suitable for preparing lightweight aggregate due to its proper chemical composition
and particle size distribution. Leaching levels of trace metals
including Pb, Hg, As, Cd, Cu, and Cr from all lightweight aggregate
samples are less than Taiwan EPA regulatory limits. All light weight
aggregate samples made from sediments with different mixing
proportions prepared through heating at 10501150 C for
18 min in this study can meet the <2.0 g cm 3 and 220% criteria
for LWA in terms of bulk density and water sorption capacity,
respectively. In addition, there is no criterion regarding the crushing strength for LWA, although this criterion has been set as
>176 kgf cm 3 (>2587.2 psi) by the American Society for Testing
and Materials for LWA-incorporated cement specimen. It seems
that the optimal sintering temperature for preparing LWA is
10501100 C, while the mixing proportion does not considerably
affect the properties of LWA.
The main edge peaks in the XANES spectra from most LWA samples shift toward greater photon energy, indicating an increase in
average oxidation state of Fe. This is in contrast to the generally accepted mechanism that during the vesicant process, the average oxidation state of Fe decreases due to the transformation of Fe2O3 into
Fe3O4, FeO, and O2. Based on the XANES results, FeSO4 decomposition with a concomitant release of SOx (x = 2, 3) is suggested to play
an important role for the bloating process in present study.

Acknowledgments
We thank Professor J.-F. Lee and the staffs of NSRRC of Taiwan
for their assistance in the XAS experiment. This study was sponsored by National Science Council of Taiwan through the contract
NSC 95-2221-E-029-010-MY2.
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