Marine Pollution Bulletin 63 (2011) 135140

Contents lists available at ScienceDirect

Marine Pollution Bulletin

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

Preparation of low water-sorption lightweight aggregates from harbor

sediment added with waste glass
Yu-Ling Wei a,, Chang-Yuan Lin a, Kuan-Wei Ko a, H. Paul Wang b,c
a

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

a r t i c l e

i n f o

Keywords:
Lightweight aggregate
Sintering
Sediment recycle
Bloating
Waste glass recycle

a b s t r a c t
A harbor sediment is successfully recycled at 1150 C as low water-absorption lightweight aggregate via
addition of waste glass powder. Sodium content in the waste glass is responsible for the formation of lowviscosity viscous phases during ring process to encapsulate the gases generated for bloating pellet samples. Water sorption capacity of the lightweight products can be considerably reduced from 5.6% to 1.5%
with the addition of waste glass powder. Low water-absorption property of lightweight products is benecial for preparing lightweight concrete because the water required for curing the cement would not be
seized by lightweight aggregate ller, thus preventing the failure of long-term concrete strength.
2011 Elsevier Ltd. All rights reserved.

1. Introduction
Taichung Harbor of Taiwan has been troubled with sludge
deposition problem in ship routes and harbor basin. The deposition
reduces the water depth. To effectively keep the harbor in usable
condition, regularly dredging the sludge is necessary although
the cost of nal disposal of the massy sludge is expensive. In Taiwan, the population density is high and the land available for
waste landll is very limited. Thus recycling the sludge as useful
resources is preferred. In a previous study, dredged sludge of the
harbor Taiwan was successfully manufactured into lightweight
aggregates (LWAs) after mixing with a reservoir sediment at different ratios and ring at 10501150 C (Wei et al., 2008).
LWAs have various applications. They can be used in room
partition to lessen the weight of building with great sonic and re
resistance and ease the shocking wave caused by earth quake.
LWAs can also be used in bridge construction, gardening, and soil
and environmental engineering (Cheeseman et al., 2005). In
producing LWAs, however, because of the gradual depletion of natural resources, such as shale, pumice, volcanic ash, siliceous rock,
and others (Chen et al., 2010; Mueller et al., 2008; Chiou et al.,
2006; Cheeseman et al., 2005; Hossain, 2004; Mladenovic et al.,
2004) and because of the increasing public requirement on green
environment, there is an increasing trend to use wastes as a substitute for the natural resources.
The water absorption capacity of the LWAs prepared in previous
study is relatively high (6.0%14.0%) (Wei et al., 2008). Thus, an at 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 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.marpolbul.2011.01.037

tempt is made in present study to improve the quality of LWAs

regarding water sorption capacity. LWAs have frequently been
used as a ller to prepare lightweight cement (LWC) for construction sector. It is highly desirable if the LWAs incorporated in LWC
do not absorb the water which is always added to cement for a
well-controlled pozzolanic reaction to form calcium silicate and
calcium aluminosilicate hydrates during cement hydration. The
cement hydration may take as long as four weeks to reach desired
long-termed strength and hardness. Conversely, if the incorporated
LWAs absorb considerable amount of water from cement, the
pozzolanic reaction activity inside the cement matrix will be inuenced and becomes difcult to control.
Traditionally, waste glass is recycled into secondary glass product and porcelain in Taiwan; however, these paths have lost their
competing capability against imported products due to relatively
high labor cost. Thus, new approaches in recycling waste glass
are desired. To enhance the sintering reaction occurring in various
high-temperature processes, addition of waste glass into raw
materials at different ratios has been investigated (Ducman and
Mirtic, 2009; Nemes and Jzsa, 2006; Corinaldesi et al., 2005; Ducman et al., 2002). Based on the principle that waste is a misplaced
resource, the present study recycles the harbor sludge, with/without addition of waste glass powder, as lightweight aggregates
(LWAs) via ring for considerably less process time, as compared
with what required for manufacturing bricks and porcelain.
2. Experimental methods
The harbor sediment was collected from Taichung Harbor
located in central Taiwan. This harbor has very serious sediment

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Y.-L. Wei et al. / Marine Pollution Bulletin 63 (2011) 135140

deposition problem resulting from the minerals brought in by

incoming sea wave, consequently the sediment has to be regularly
dredged; otherwise the ship routes would become too shallow to
function normally. After sampling, the sediment was dried at
105 C in an oven for 24 h and ground to pass a 50-mesh sieve. It
was end-to-end mixed for 6 h with waste glass powders at various
weight ratios (sediment/waste glass powder = 100:0, 100:10,
100:20, 100:30, 100:40, 100:50). The glass powders were supplied
by a local glass manufacturing plant that has been worrying about
their nal disposal. The mixture was again dried and ground to <50
mesh. A series of 50-gram mixtures were pressurized into disk pellets with 6-cm diameter. The disk pellets were cut into small rectangular pellets (approximately 2.5 cm  1.75 cm) which were then
red into LWAs at 1000, 1050, 1100, and 1150 C for 18 min after
being pre-treated to 500 C for 2 min with a heating rate of
100 C min 1. The pre-treatment, a de-volatilizing process, was
carried out to successfully generate LWAs without blasting the
rectangular pellets into small pieces when rapidly heated to
10001150 C. The experimental owchart is presented in Fig. 1.
The elemental compositions (referring Table 1), except Si, Cl ,
and SO24 , of the dried ground raw sediment and waste glass powders were determined with an inductively coupled plasma-atomic
emission spectrometer (ICP-AES, Optima 3000DV, Perkin Elmer,
USA) after a microwave (MDS-2000, CEM, USA)-assisted acidic
digestion step. Si content in both sediment and waste glass powders was determined based on the sample weight loss after their

Dry harbor sediment powder (<50 mesh)

Addition of waste glass powder at

different weight ratios
Addition of proper amount of water

End-to-end mixing at a rotational speed of

302 rpm for 6 hours

Drying and grinding to <50 mesh

Formation of 50-gram disc pellet (diameter 6

cm)

Slicing into small rectangular pellets

(approximately 2.5cm 1.75cm)
Sintering/bloating at 1000, 1050, 1100,
and 1150 oC for 18minutes

Characterizing the lightweight

aggregates (e.g. XRD, weight loss,
particle density, water absorption
rate, and surface morphology)

Fig. 1. Experimental owchart for preparing lightweight aggregates.

Table 1
Chemical compositions of harbor sediment and waste glass powder.
Composition

Sediment

Waste glass

SiO2
Al2O3
Fe2O3
K2O
Na2O
CaO
PbO
MgO
MnO2
ZnO
Cr2O3
Cl

62.5%
14.3%
5.79%
3.08%
2.03%
0.332%
93.7 mg kg
N.D
N.D
N.D.
263 mg kg
1.71%
0.69%

72.10%
0.53%
1.52%
1.15%
14.21%
5.68%
6101 mg kg 1
1.79%
100 mg kg 1
449 mg kg 1
392 mg kg 1
0.36%
N.D.

SO24
LOI

5.72%

2.15%

reactions with mixed acid consisting of concentrated HF and concentrated HClO4 (5.0 mL and 1.0 mL, respectively for 0.15-gram
dry sample) at 550 C to form H2SiF6 which is volatile and readily
vents away (Taiwan CNS, 1985). To determine the total contents
of SO24 and Cl in sediment, waste glass (Table 1), and LWAs,
0.100-gram sample in a mixed acid consisting of 10-mL concentrated HNO3 (66%), 3-mL concentrated HF (40%), and 1-mL H2O2
(30%) in a capped Teon vessel was digested at 180 C for 10 min
with microwave assistance, ltrated, and total contents of SO24 and Cl in the liquid phase was determined with an ion chromatograph (IC, DX-100, Dionex, USA). The concentration ranges of the
calibration curves for SO24 and Cl are 010.00 mg L 1 and
05.00 mg L 1, respectively. The square of the correlation coefcient for both curves is >0.999. The loss on ignition is dened
as the weight loss after heating in an electric furnace at 900 C
for 3 h under atmospheric air. The particle size distribution of both
sediment and waste glass powders were measured by the use of a
particle size analyzer (Coulter LS230, Beckman, USA). Thermal
behaviors of the sediment and waste glass powders were studied
with a thermogravimetric/differential thermal analyzer (TG/DTA,
Pryis Diamond, Perkin Elmer, USA) under air stream from room
temperature to 1220 C at a heating rate of 10 C min 1.
After the sintering/bloating process, water absorption capacity
and apparent particle density of the LWAs were determined.
Face-dry water absorption capacity of LWAs in 24 h was measured
following a method formulated by Taiwan government (Taiwan
CNS, 1993). The apparent particle density was measured based
on the Archimedes Principle (Cheeseman et al., 2005). To properly
measure the size for a LWA which had lower density than water,
the LWA was immersed into water by using a very slim metal wire
to suppress it downward. The morphologies of both green pellets
and LWAs were examined with scanning electron microscopy
(SEM, Quanta 400F, FEI, USA) and the crystalline phases present
in the matrix were determined with a X-ray diffraction spectrometer (XRD, D8 Advance, Bruker AXS, UK).
3. Results and discussion
The primary chemical compositions, expressed in oxide forms
except Cl , of the harbor sediment and waste glass powders are
listed in Table 1. The compositions of harbor sediment are similar
to clay which has proven to be an appropriate raw material for
preparing LWAs (Wei et al., 2008). The sediment contains 1.71%
chloride, limiting the LWAs reported in the present study to nonstructural usage, such as being incorporated into lightweight concrete (LWC) for room partition, gardening, and environmental
application. Using the LWAs in steel-reinforced concrete should
be avoided. Table 1 indicates that the waste glass contains

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Y.-L. Wei et al. / Marine Pollution Bulletin 63 (2011) 135140

14.21% Na2O that can reduce sintering temperature because of its

relatively low melting point. The ux content (dened as the
weight sum of Fe2O3, Na2O, K2O, CaO, and MgO) in the sediment
is 11.23%, while being 24.35% in the waste glass. This fact indicates
that addition of waste glass into the sediment can lead to more rapid sintering reaction. The sediment and waste glass contain 5.72%
and 2.15% LOI components, respectively which may be relevant to
the bloating phenomena for expanding the pellets at high temperatures. These LOI contents are too high to gradually expand the
pellets in present study, thus the green pellets were pre-treated
to de-volatize fractional LOI to prevent the pellets from being
blasted into small pieces during subsequent sintering/bloating process at 10001150 C.
To effectively encapsulate the gases for bloating the pellets, sintering reaction should take place in time to form continuous phase
before the gases escape from the pellets. To obtain a timely sintering reaction, particle size distribution has been considered as an
important physical factor. Finer particles can ll in the void space
among coarse particles, whereby neck growth rate among particles
during the high-temperature process can be rapid enough to form
continuous phase. As depicted in Fig. 2, the sediment is relatively
ner than the glass powder. More than 95% sediment powders
are <30.07 lm, and most glass powders are <121.8 lm. Although
the added waste glass powders are coarser than the sediment,
numerous ne sediment particles can ll in their void space.
Further, because the ux content in the glass is about twice that
in the sediment, glass powders tends to form continuous phase
because they readily melt and ow around sediment particle;
thereby rendering a greater sintering rate.
Fig. 3 shows the three-component diagram consisting of SiO2,
Al2O3, and ux components. It shows that to be suitable for preparing LWAs, the components of candidate material needs to fall in-

g/s=30/100
g/s=50/100
harbor
sediment

Al2O3
50 %

Flux
50 %
g/s=20/100

g/s=10/100

Fig. 3. Three-component diagram consisting of SiO2, Al2O3, and ux components.

side the region surrounded by the dotted circle (Riley, 1951). As

indicated in Fig. 3, all mixtures studied in the present study fall inside the circled region, and their ux component increases with
increasing ratio of glass to sediment.
Thermal behaviors of the sediment and glass, studied with TG/
DTA, are indicated in Fig. 4. The DTA curve of sediment (top panel
of Fig. 4) has an exothermic peak at 326.18 C with 1.6% weight loss
(see TGA). This exothermic peak has been attributed to the release
of CO resulting from incomplete oxidation of organic matters present in sewage sludge in a previous study (Xu et al., 2008). The TGA
curve indicates a major weight loss (3.8%) in the 400700 C range,
accompanied by endothermic changes which extend to 1220 C.
The endothermic changes results from crystalline phase transformation and/or formation and organics volatilization (Xu et al.,
2008). The DTA curve of the glass (bottom panel of Fig. 4) shows
two exothermic peaks: one at 427.4 C due to CO2 release from
organics oxidation (Xu et al., 2008), with a corresponding 2.2%
weight loss, and other in the 1147.81220 C range.

100

sediment

80

80
60

40

40

20

20

0
100

0
100

glass

80

80

60

60
(Number percentage)

40

(Cumulative number percentage)

96

0
94

-20

TGA

-40

92

-60

30

20

20

100

427.4 C

35

glass

DTA

99

25

TGA

20
40

98

20

DTA (V/mg)

60

sediment

40 DTA

Cumulative Weight Percentage (%)

(Cumulative number percentage)

100

326.18 C

60

(Number percentage)

Fractional Weight Percentage (%)

g/s=40/100

98

15

97

10

62
62
-1
21
.8
12
1.
823
4.
1
69
.

07
-6
9.

30
.

0.
0

8
.7
83
10

210
.7
3.
5

<3
.5

Particle Size Range (m)

Fig. 2. Particle size distribution of harbor sediment and waste glass powders.

TGA (%)

100

SiO2
100 %

96

1147.8 C

-5
200

400

600

800

1000

95
1200

Temperature ( oC)
Fig. 4. Thermal behaviors of harbor sediment and waste glass recorded with TGA/
DTA.

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Y.-L. Wei et al. / Marine Pollution Bulletin 63 (2011) 135140

Sintering/bloating reactions have caused some transformation

and formation of crystalline phases, as depicted by the XRD patterns in Fig. 5. Major crystalline phases found in the sediment
are silicon oxide (SiO2), corundum (a-Al2O3), and wusite (FeO).
Minor crystalline phases present are calcium oxide (CaO), halite
(NaCl), potassium oxide (K2O), sodium carbonate (Na2CO3), kyanite
(Al2SiO5), sillimanite (Al2SiO5), anorthite (CaAl2Si2O8), and enstatite (MgSiO3). After the sintering/bloating reaction at temperature
ranging from 1000 C to 1100 C, new crystalline phases (i.e., a-sodium silicate (Na2Si2O5) and calcium silicate (CaSiO3)) are formed
in the LWAs along with the disappearance of some crystalline
phases including calcium oxide, sodium carbonate, sillimanite,
and enstatite. Obviously, calcium oxide reacts with silicon oxide
to form calcium silicates. Sodium carbonate rst decomposes into
carbon dioxide and sodium oxide which subsequently reacts with
silicon oxide to form the new crystalline phase a-sodium silicate.
Because both calcium and sodium contents are ux component,
the can react with silicon oxide to form new crystalline phases.
This may explain why calcium oxide, halite, and sodium carbonate
are not found in the XRD patterns from 1000 C to 1100 C LWAs.
The other two ux components, wusite and potassium oxide crystalline phases, become either barely recognizable or absent in the
10001100 C diffraction patterns. In addition, the released carbon
dioxide contributes to the expansion of pellets. Additionally, Fig. 5
reveals that higher temperature generally leads to lower crystalline intensities, indicating that with more heat being provided to
the pellets, the crystalline size tends to gradually decrease.
After ring at 10001150 C, 4.67%6.51% sample weight was
lost from green pellets (see Table 2). For sintered sediment (g/
s = 0/100), the weight loss is 5.92%6.51% which is slightly greater
than the sediment LOI (5.72%, see Table 1) because the latter was

Fig. 5. XRD patterns from harbor sediment and lightweight aggregates prepared
from mixtures with a sediment-to-waste glass ratio of 50/100 at 10001100 C.

determined at a relatively lower temperature, 900 C. However,

the TGA-weight loss of the sediment (g/s = 0/100) is 7.2%7.8% in
the 10001100 C range (see Fig. 4), which is greater than both
sediment LOI and LWA weight loss. The difference is attributed
to different heating rate. The TGA experiment was performed at
a very slow heating rate (10 C min 1), while LWA preparation
and LOI test were associated with rapid heating as the samples
were directly exposed to the nal pre-set temperatures. Rapid
heating during LWA preparation would cause instant sintering to
generate viscous liquid phases to encapsulate high-pressure gases,
thereby forming LWAs. As to the effect of process temperature and
addition of glass on weight loss, the LWA weight loss generally increases with increasing temperature and decreasing glass content.
The generally acceptable particle density of LWAs is <2.0 kg m 3
and LWAs with different particle densities have various practical
applications. The effect of process temperature and glass addition
on LWA particle density is presented in Table 3. As the temperature
increases, the LWA particle density decreases due to two main reasons: formation of lower-viscosity viscous layer and generation of
more bloating gas. First, at higher temperature not only more viscous phase forms to encapsulate bloating gas, but also the viscosity
resistance against gas expansion is less than the viscosity present
at lower temperature. Second, more bloating gases will be released
at higher temperature, as supported by the TGA results. Pellet
expansion will continue with more pores formed as long as the
expanding force of the bloating gases is greater than the viscous
resistance force, and it will stop when these two forces are in balance. However, if the temperature is too high, the viscous layer
may be broken by the bloating gas. As to the effect of glass addition
on LWA particle density, Table 3 shows that more glass addition results in greater pellet expansion, too. The addition of glass would
result in two contradictory effects on LWA particle density. Upon
sintering/bloating, the glass generates less bloating gases than
the sediment because it contains less LOI than sediment. Yet it contains 14.21% sodium oxide, much greater than the 2.03% content in
sediment, which is known to melt at relatively low temperature
and can effectively generate more viscous phases with lower viscosity to encapsulate the bloating gases. Thus, the LWA pellets
which contain more glass would be more expanded. When heating
the mixture pellet with a g/s ratio of 50% at 1150 C, the viscosity of
the viscous phases was too low to effectively encapsulate the released gases; leading to a shrunk dense melted pellet that was
stuck on crucible surface. Thus no particle density was determined
for this product. For practical application, Table 3 shows that all
LWAs prepared at 1100 C and 1150 C meet the <2.0 kg m 3 criterion in particle density, while at 1050 C, an addition of =20% glass
is required to meet the criterion. If the process temperature is lowered to 1000 C, the least addition of glass is 50%.
The generally acceptable water absorption capacity based on
24-h soaking in water is <20%; LWAs with different water absorption capacity have various practical applications. All LWAs have a
water absorption capacity <20% (Table 4). However, to be incorporated in LWC, the water absorption capacity should be kept at a
minimum level. As to the effect of glass addition, Table 4 shows
that more glass addition results in less water absorption. Because
the waste glass contains 14.21% sodium oxide, it melts at a relatively lower temperature. Thus it can effectively generate more viscous phases with lower viscosity to smoothen the surface
roughness, leading to a less water absorption capacity. Table 4
shows that the LWAs made at 1150 C from the mixtures with
30% and 40% glass addition have an extremely low water absorption capacity, 2.5% and 1.5%, respectively. All LWAs prepared at
1100 C and 1150 C have a water absorption capacity <7.1%.
To study the effect of process temperature and glass addition on
the microstructure of LWAs, the morphologies of fractured cores of
the LWAs produced at 10001100 C were examined with SEM

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Y.-L. Wei et al. / Marine Pollution Bulletin 63 (2011) 135140

Table 2
Weight loss after ring the pellets consisting of various ratios of waste glass/sediment (g/s) at 10001150 C.
Temp. (C)

Weight loss (%)

g/s 0/100

g/s 10/100

g/s 20/100

g/s 30/100

g/s 40/100

g/s 50/100

1000
1050
1100
1150

5.92
6.16
5.98
6.51

5.55
5.39
5.64
5.72

5.46
5.13
5.41
5.27

5.15
5.18
4.85
5.53

4.80
4.96
5.25
5.39

4.76
5.09
4.67

Table 3
Effect of process temperature and waste glass/sediment ratio (g/s) on the particle density of LWAs.
Temp. (C)

1000
1050
1100
1150

Particle density (kg m

g/s 0/100

g/s 10/100

g/s 20/100

g/s 30/100

g/s 40/100

g/s 50/100

2.31
2.33
1.83
1.16

2.35
2.24
1.81
1.11

2.14
1.93
1.58
1.18

2.02
1.87
1.71
0.92

2.06
1.71
1.24
0.79

1.93
1.73
1.26

Table 4
Effect of process temperature and waste glass/sediment ratio (g/s) on the water absorption capacity of LWAs.
Temp. (C)

1000
1050
1100
1150

Water absorption (%)

g/s 0/100

g/s 10/100

g/s 20/100

g/s 30/100

g/s 40/100

g/s 50/100

17.5
13.2
7.1
5.6

16.9
11.3
5.5
5.1

16.5
10.5
4.9
3.7

17.3
8.3
4.1
2.5

11.7
4.8
3.8
1.5

11.8
4.4
2.7

(see Fig. 6). In general, the LWAs prepared under condition of lower
temperature and less glass addition are characterized by fewer and
ner pores in their fractured cores (see upper left panels of Fig. 6);
while the opposite condition leads to product containing larger
pores (see lower right panels). Firing the pellets containing glass
at 1100 C, the pores are so large that they even become interconnected due to the relatively low viscosity of the viscous phases
which could not withstand the bloating force from the high-pressure gases. As the heated pellets grow in size, the viscous phases

become thinner and their strength gets weaker. If this situation

continues to proceed, the thin weak viscous phases may eventually
break; thereby the pores being interconnected. In contrast, ring
the pellets at lower temperatures would produce LWAs with more
isolated spherical pores in the fractured cores, and the inter-pore
crystalline phases are thicker.
Furthermore, the leaching test of heavy metals from solid
building materials recycled from wastes (Taiwan EPA, 2010) was
performed on the LWAs with a total solid/liquid ratio of approxi-

Fig. 6. Morphologies of fractured cores of the lightweight aggregates produced at 10001100 C.

140

Y.-L. Wei et al. / Marine Pollution Bulletin 63 (2011) 135140

mately 1/100, and the leaching concentrations of Pb, Cr, Zn, and Mn
from all LWA samples are 60.096, 60.013, 60.015, 60.024 mg L 1,
respectively. Its noteworthy that Taiwan has not imposed any regulatory threshold on heavy metal leaching from construction
materials so far; how and what to be set as the regulatory threshold is a currently discussed issue among ofcials serving in various
Taiwan governmental ministries. For the practical application of
LWAs, because the LWAs contain 0.27%1.30% total chloride that
might be corrosive to steel and because the strength of the LWAs
reported in this manuscript can be as low as 22.6 kgf cm 2, the
LWAs reported in the present study are suggested to be limited
to non-structural usage in the absence of steel reinforcement, such
as being incorporated into lightweight concrete for room partition,
gardening, and environmental application.
4. Conclusions
Because of its relatively low melting point, waste glass additive
which is rich in sodium oxide and ux contents can effectively help
sinter to form continuous viscous phase to encapsulate gases for
preparing LWAs from harbor sediment.
Formed at higher temperature with more glass additive, the
LWAs are less dense due to a decrease in the viscosity of viscous
layer and to a generation of richer bloating gases. With waste glass
addition, the apparent particle density of LWAs prepared at
1150 C decreases from 1.16 kg m 3 to 0.79 kg m 3.
All LWAs have a water absorption capacity <20%. The LWAs
made from the mixtures with 30% and 40% glass additive at
1150 C have an extremely low water absorption capacity, 2.5%
and 1.5%, respectively. The low water absorption capacity is highly
desirable because if the LWAs are to be incorporated in LWC, they
will not absorb the water added to cement for a well-controlled
pozzolanic reaction to form calcium silicate and calcium aluminosilicate hydrates during cement hydration.
In general, the LWAs prepared under the condition of lower
temperature and less glass additive are characterized by ner
pores in their fractured cores; while the opposite condition leads
to LWA formation with larger pores.

Acknowledgment
We thank the National Science Council of Taiwan for the research fund through contract NSC 98-2221-E-029-003.
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