Waste Management xxx (2014) xxxxxx

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Waste Management
journal homepage: www.elsevier.com/locate/wasman

Solidication/stabilization of ash from medical waste incineration

into geopolymers
Konstantinos Tzanakos a,, Aliki Mimilidou a, Kalliopi Anastasiadou b, Antonis Stratakis c,
Evangelos Gidarakos a
a
Laboratory of Toxic and Hazardous Waste Management, Department of Environmental Engineering, Technical University of Crete, Chania P.C. 73100, Greece
b
Division Bridges and Structural Technology/Section Tunnel and Foundation Engineering, Tunnel Operation, Civil Security, Federal Highway Research Institute (BASt),
Bruederstrae 53, P.C. 51427 Bergisch Gladbach, Germany
c
Laboratory of Applied Mineralogy, Department of Mineral Resources Engineering, Technical University of Crete, Chania P.C. 73100, Greece

a r t i c l e i n f o a b s t r a c t

Article history: In the present work, bottom and y ash, generated from incinerated medical waste, was used as a raw
Available online xxxx material for the production of geopolymers. The stabilization (S/S) process studied in this paper has been
evaluated by means of the leaching and mechanical properties of the S/S solids obtained. Hospital waste
Keywords: ash, sodium hydroxide, sodium silicate solution and metakaolin were mixed. Geopolymers were cured at
Medical waste 50 C for 24 h. After a certain aging time of 7 and 28 days, the strength of the geopolymer specimens, the
Bottom ash leachability of heavy metals and the mineralogical phase of the produced geopolymers were studied. The
Fly ash
effects of the additions of y ash and calcium compounds were also investigated. The results showed that
Geopolymer
Heavy metal
hospital waste ash can be utilized as source material for the production of geopolymers. The addition of
Compressive strength y ash and calcium compounds considerably improves the strength of the geopolymer specimens (2
8 MPa). Finally, the solidied matrices indicated that geopolymerization process is able to reduce the
amount of the heavy metals found in the leachate of the hospital waste ash.
2014 Elsevier Ltd. All rights reserved.

1. Introduction (Malviya and Chaudhary, 2006). For stabilization, the objective is

Medical waste generation has increased considerably world-
wide in the last few decades (Rajor and Kunal, 2011). Among the
principal methods available for proper management of medical
waste, incineration and disposal of the resultant ash by landlling
is the priority method used (Xie et al., 2009). The main advantages
of incineration are the destruction of pathogens and the reduction
in the volume and weight of the waste. However, incineration pro-
duces residues that are enriched by toxic chemicals, such as heavy
metals (Jung et al., 2004). In some densely populated cities, the dis-
posal of the waste ash is becoming increasingly difcult, owing to
high cost, diminishing land availability, more stringent regulation,
and frequent public opposition to the sifting of new landlls
(Anamul et al., 2012). Due to this reasom, the need to manage
the produced ash in an environmentally friendly way has major
priority.
Stabilization/solidication is a pre-landll waste treatment pro-
cess, which has been used for different types of industrial wastes,
but is particularly suited to those containing heavy metals
Corresponding author. Tel.: +30 6980484623.
E-mail address: ktzanakos@gmail.com (K. Tzanakos).
to minimize the solubility and toxicity of contaminates while for
solidication, usually matrices like cement are used to encapsulate
the waste material in order to immobilize contaminates and
reduce leachability (Charles et al., 2010). Despite the fact that,
the stabilization/solidication of municipal solid waste incinera-
tion ash in geopolymers has been already studied by many authors
(Komnitsas et al., 2012; Lancellotti et al., 2010; Zheng et al., 2010;
Galiano et al., 2011), until today, only few have studied the stabil-
ization/solidication of medical waste incineration ash.
Anastasiadou et al. (2011) used medical waste ash in combination
with different amounts of Ordinary Portland Cement (OPC) as a
binder, in order to reduce the leachability of the heavy metals pres-
ent in this material and to increase its mechanical characteristics.
Sukandar et al. (2009) tried to stabilize the medical waste y ash
using chelating agent and phosphates. In this paper, geopolymer-
ization technology has been proposed to stabilize and solidify
medical waste ash. Although this paper focus on the advantages
of geopolymers towards heavy metal immobilization, because of
their physical properties these specimens can also be utilized in
the future as replacements for concrete in most instances.
During the past decade many researchers have started to deal
with the performance of one such stabilization agent. Geopolymer

http://dx.doi.org/10.1016/j.wasman.2014.03.021
0956-053X/ 2014 Elsevier Ltd. All rights reserved.

Please cite this article in press as: Tzanakos, K., et al. Solidication/stabilization of ash from medical waste incineration into geopolymers. Waste Manage-
ment (2014), http://dx.doi.org/10.1016/j.wasman.2014.03.021
2 K. Tzanakos et al. / Waste Management xxx (2014) xxxxxx
materials have attracted much more attention due to their excel-
lent mechanical properties, good chemical resistance, low shrink-
age, environmentally friendly nature and long-term durability
(Duxson et al., 2007). Their nal structure and physical properties
depend upon several parameters as water content, particle size,
thermal history, alkali metal content and degree of amorphicity
(Komnitsas, 2011). The properties and uses of geopolymers are
being explored in many scientic and industrial disciplines: mod-
ern inorganic chemistry, physical chemistry, colloid chemistry,
mineralogy, geology, and in all types of engineering process tech-
nologies (Davidovits, 2008). Potential products and applications
include among others concrete, building components and temper-
ature stable resins, encapsulation of toxic wastes, surface capping
and stabilization of tailing dams (Komnitsas et al., 2012). For the
production of the geopolymer matrices many kinds of raw materi-
als have been used, such as lignite bottom ash (Sata et al., 2012),
blast furnace slag (Zhang et al., 2007; Oh et al., 2010), red mud
and metakaolin mixture (Dimas et al., 2009), blends of circulating
uidized bed combustion y and bottom ash (Li et al., 2012) and
metakaolin (Rovnank, 2010). Due to the interesting ndings of
these studies, the possibility of using the residual ash of hospital
waste in combination with metakaolin as raw materials for the
production of geopolymers was investigated.
2. Experimental
2.1. Materials
Bottom and y ash were sampled from a Medical Waste Incin-
eration Facility (MWIF). Bottom ash was rst dried at 105 C and
then was ground in order to reduce its particle size class below
100 lm. The particle size of the y ash was already below
100 lm so there was no need for such pretreatment.
The chemical composition of the two kinds of ash (Table 1) and
the leachability of the heavy metals (Table 2) were measured with
the XRF and TCLP method respectively.
According to Table 1, the main elements of the bottom ash are
SiO2 (39.74%), CaO (27.77%) and Na2O (9.13%), while the major ele-
ment of the y ash is CaO (89.20%). The difference between the two
kinds of ash is remarkable, as the content of CaO in y ash is very
high due to its pre-treatment with hydrated lime. The concentra-
tion of all the heavy metals measured in bottom ash was within
permissible limits for the US EPA TCLP test (Method 1311). On
the other hand, concentrations of Zn and Pb were found to be high
in y ash, exceeding the limits of the TCLP method. According to
Rajor et al., 2012, feeding waste of medical waste incinerator is
susceptible to reactive chemicals such as chlorine compound that
may be originated from disinfectant and plastics, especially PVC.
The presence of large quantities of chlorine available, formation
of metal chlorides in the combustion zone appears generally to
increase. The results of this study are in agreement with previous
studies (Anastasiadou et al., 2011; Kougemitrou et al., 2011;
Javied et al., 2008).
Materials used for the production of the geopolymers in con-
stant quantities were sodium hydroxide solution of 10 M and
sodium silicate solution with a composition of 8.9 wt.% Na2O,
28.7 wt.% SiO2, 62.5 wt.% H2O, and metakaolin, produced by
calcination at 700 C for 4 h of kaolinite.
Table 1
Chemical composition of medical waste bottom and y ash.
Chemical composition SiO2 CaO Na2O
Bottom ash 39.74 27.77 9.13
Fly ash 6.00 89.2 2.50
Please cite this article in press as: Tzanakos, K., et al. Solidication/stabilization of ash from medical waste incineration into geopolymers. Waste Manage-
ment (2014), http://dx.doi.org/10.1016/j.wasman.2014.03.021
2.2. Mix proportions
Four series of experiments were carried out in this study. In the
rst series, only bottom ash was used as a raw material. In the sec-
ond series, a quantity of calcium carbonate was added in order to
study its effect on the geopolymer paste. In the third and fourth
series, y ash and bottom ash at proportions of 75:25 and 50:50
(FA:BA) were used, respectively. In all series three different propor-
tions of Medical Waste Ash (MWA): Metakaolin (MK) of 20:100,
30:100 and 50:100 were applied.
The production of the geopolymer matrices comprised the fol-
lowing steps: (a) preparation of the alkaline solution by dissolving
the quantity of sodium silicate and sodium hydroxide in distilled
water, (b) addition of the ash in the solution and stirring for
5 min (c) addition of the quantity of the MK and stirring until a
homogeneous and uid paste was formed. Then, the mixture was
poured into 50 mm 50 mm 50 mm cubic molds, which was
the samples dimension, and were cured in the oven at 50 C for
24 h to complete the geopolymerization reaction.
The values of the temperature (Chindaprasirt et al., 2007), of the
curing time (Palomo and Fuente, 2003) and of the concentration of
the sodium hydroxide solution (Rattanasak and Chindaprasirt,
2009; Chindaprasirt et al., 2009) were chosen based on the litera-
ture and after a large number of trials.
2.3. Methods of analysis
X-ray uorescence (XRF) method provides a qualitative identi-
cation and a quantitative analysis of the element. The samples
of bottom and y ash were initially grinded to a particle size class
<60 lm and then pressed to a pellet. An S2 Ranger EDS (Bruker
Ltd.) was then used for quantitative chemical analysis of both kinds
of medical waste ash. X-ray diffraction (XRD) was utilized to deter-
mine the mineralogical properties of the y and bottom ash sam-
ples and of the produced geopolymers. The XRD patterns were
recorded on a D8 Advance XRD (Bruker Ltd.) with a copper target
(k = 15.406 nm). A diffraction angle (2h) between 4 and 70 and
a scanning rate of 4/min was applied to analyze the crystal phases
of the y ash and bottom ash samples. Diffraction patterns were
manually analyzed using the Joint Committee on Powder Diffrac-
tion standards.
Characterization of the effectiveness of s/s treatment should be
based on determining the environmental impact of the treated
waste after it is disposed or reused (Batchelor, 2006). One method
to succeed this is to estimate the amount of contaminant that
might be released to the environment, using tests under specic
conditions.
The TCLP analysis (Method 1311) simulates landll conditions.
It determines which of the contaminants identied by the United
States Environmental Protection Agency are present in the leachate
and their concentrations (US EPA, 1992). Manually crushed mate-
rial (<1 cm) was leached using an extraction buffer of acetic acid
and sodium hydroxide (pH 4.93 0.05) at a liquid/solid ratio of
20:1. The extraction (at 25 2 C) was performed by shaking the
material for 18 h. Subsequently, the leachate samples were ltered
through a 0.8 lm borosilicate glass ber lter, and the resultant
TCLP extract (ltrate) was analyzed for heavy metals using Induc-
tively Coupled Plasma-Mass Spectrometer (ICPMS) Agilent Tech-
nologies, model 7500cx.
Al2O3 Fe2O3 MgO BaO TiO5 SO3 K2O Other
5.16 4.53 2.92 2.25 2.24 1.36 0.49 0.41
0.30 1.0 0.10
 K. Tzanakos et al. / Waste Management xxx (2014) xxxxxx
Table 2
TCLP leaching values for medical waste bottom and y ash samples.
Heavy metals Cr (mg/l) Ni (mg/l)
Bottom ash 0.3360 <DL
Fly ash 0.1865 <DL
TCLP limit 5 7
DL: Detection Limit
3. Results
3.1. X-ray diffraction analysis
Fig. 1 shows the XRD patterns of bottom and y ash samples as
well as selected geopolymer samples. The main crystalline phase of
the bottom ash was gehlenite, which is a composite mineral, while
other crystalline phases such as quartz, hematite, halite, stilbite
and calcite were also detected. Similar results have been presented
by Xu et al. (2010) and Li et al. (2012). The major mineral in the y
ash was calcite; halite, quartz, anhydrite were present in consider-
able amounts, and zeolite and thermonatrite in trace amounts.
Halite indicates the presence of clorides in the y ash. Chlorine is
a reactive chemical compound that may have originated from
medical disinfectants and decomposition of plastics (Valavanidis
et al., 2008). The results of the XRD analysis of y ash are in agree-
ment with the results of Kougemitrou et al. (2011), Anastasiadou
et al. (2011), Sata et al. (2012) and Guo et al. (2010).
The resulting geopolymers of the rst, second and third series
had almost amorphous phases and were similar to each other.
The main crystalline phase of these matrices was quartz. The sim-
ilarity between the XRD patterns indicate that the addition of cal-
cite carbonate in the second series and y ash in the third series
did not affect the crystalline phase of the geopolymers. Yip et al.
(2005, 2008) and Li and Liu (2007) agree with this conclusion.
On the other hand in the fourth series, where the quantity of the
y ash at the matrices increased considerably, the calcite became
the main crystalline phase. This was due to the fact that a percent-
age of the y ash added did not react during the geopolymer
process.
Fig. 1. X-ray diffractograms of the y and bottom ash and of the produced geopolymers binders.
Please cite this article in press as: Tzanakos, K., et al. Solidication/stabilization of ash from medical waste incineration into geopolymers. Waste Manage-
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3
Zn (mg/l) Cd (mg/l) Ba (mg/l) Pb (mg/l)
0.15400 <DL 2.5348 0.0096
11.8000 <DL 1.7965 6.0172
5 1 100 5
3.2. Compressive strength
Three specimens have been tested for each proportion of each
series and the average obtained compressive strength values are
presented in Fig. 2. The average values of all the geopolymers were
within 0.707.63 MPa.
The compressive strength of the geopolymers increased with
the use of calcium carbonate at the second series of the experiment
and with the addition of the y ash at the third and the fourth ser-
ies. This increase was due to the increase of calcium oxide and of
the ratio of SiO2/Al2O3 in the geopolymer matrices.
Many researchers have studied the effect of increasing calcium
oxide on the strength of the produced specimens, either with the
addition of calcium hydroxide and calcium carbonate (Alonso
and Palomo, 2001; Temuujin et al., 2009), or with the addition of
blast furnace slag rich in CaO (Yip et al., 2008; Li and Liu, 2007).
Calcination activates material by changing their crystalline struc-
ture into amorphous structure to store extra energy and increase
their activity, and increasing compressive strength (Khale and
Chaudhary, 2007). The results of the second series of the experi-
ment are in agreement with the results of Pinto (2004), who had
concluded that the compressive strength of the matrices increases
when the percentage of added source of calcium is up to 20% and
30% respectively. It is worth mentioning that in the second series
of the experiment the proportion of the added calcium carbonate
in the specimens ranged from 7% to 16%. Regarding the results
obtained from the third and fourth series of experiments, the com-
pressive strength of the produced geopolymers was greater than
the respective values of the rst series but smaller than the values
of the second series. The results of these series are in agreement
4 K. Tzanakos et al. / Waste Management xxx (2014) xxxxxx

Compressive strength values after 7 days

Compressive strength (MPa)

6
100% bottom ash
5
4 100% bottom ash (addition
3 of CaCO3)
2 75-25% bottom-fly ash
1
0 50-50% bottom-fly ash
0 10 20 30 40 50 60
Medical waste ash: Metakaolin

Compressive strength values after 28 days

Compressive strength (MPa)

10 100% bottom ash

8
100% bottom ash
6
(addition of CaCO3)
4
75-25% bottom-fly ash
2

0 50-50% bottom-fly ash

0 20 40 60
Medical waste ash: Metakaolin

Fig. 2. Summary of compressive strength values for all the produced geopolymers.

with the results of Yip et al. (2005) and Yip et al. (2008), who estab- 3.3. Leaching test for heavy metals
lished the favorable effect of the addition of slag high in calcium
oxide (43% CaO), at rates between 20% and 40% of the amount of The ability of the alkali-activated matrices to immobilize heavy
metakaolin, on the compressive strength of the matrices. metals after their addition during the mixture procedure has been
Moreover, many researchers have studied the effect of the ratio widely studied and it has been concluded that geopolymerization
of SiO2/Al2O3 on the compressive strength of the specimens (Silva can play an important role in waste management (Qian et al.,
et al., 2007; Fletcher et al., 2005; Duxson et al., 2005). A relatively 2003; Deja, 2002). However, few studies were conducted on the
small variation in initial molar concentrations of Na2O, SiO2 or production of geopolymer specimens with wastes which already
Al2O3 in a geopolymer system can dramatically change its long contained heavy metals. (Asavapisit and Chotklang, 2004).
term properties (Silva and Sagoe-Crenstil, 2008). According to In Table 3 the TCLP leaching values after 28 days of solidica-
Songpiriyakij et al. (2010), the increase in compressive strength tion are displayed for all the geopolymer matrices. In all the geo-
is due to the fact that as the mixture it is enriched by greater polymer specimens all the measured heavy metals were found at
amounts of silicon, the bonds between the SiOSi become stron- concentrations lower than the permitted limits for the US EPA TCLP
ger. In addition, by increasing the SiO2/Na2O ratio, complex poly- test. These results indicate that geopolymerization is able to reduce
meric structures were formed, which led to the increase of the at a high percentage the heavy metals found in the leachate of the
mechanical strength of the matrices. In the present work this ratio y ash.
ranged in all series from 1.5, when the proportion of MWA: MK
was 20%, to 2.5 when the corresponding proportion was 50%.
Table 3
But, according to Silva et al. (2007), Khale and Chaudhary (2007),
Summary of TCLP leaching values after 28 days for solidied geopolymer specimens.
increasing SiO2/Al2O3 molar ratios up to 3.43.8 is largely respon-
sible for the high-strength gains observed at later stages. This could Concentration of heavy metals (mg/l)
explain why the compressive strength values in the present work Heavy metals Cr Ni Zn Cd Ba pH
are lower compared with previous studies (Sathonsaowaphak TCLP limit (mg/l) 5 7 5 1 100
et al., 2009; Chindaprasirt et al., 2007; Somna et al., 2011). More- 100% bottom ash
over, Ferone et al., 2013 have demostrated the negative effect of 20% 0.0450 <DL 0.0120 <DL 0.3640 10.6
the presence of chlorides on the polycondensation kinetic. Chloride 30% 0.0560 <DL 0.0360 <DL 0.4260 10.4
50% 0.0722 <DL 0.0520 <DL 0.5760 10.0
could clearly retard the solidication of geopolymer gel (Lee and
van Deventer, 2002a) and lower the strength by causing structural 100% bottom ash (addition of CaCO3)
20% 0.0421 <DL 0.0162 <DL 0.2459 10.9
discontinuity within the gel (Lee and van Deventer, 2002b). So, 30% 0.7000 <DL 0.0194 <DL 0.3698 10.8
even though the produced geopolymers presented a satisfactory 50% 0.7304 <DL 0.0349 <DL 0.4896 10.6
compressive strength, an addition of washing pretreatment of 7525% bottom-y ash
the medical waste ash not only at the experimental procedure 20% 0.0321 <DL 1.2630 <DL 0.6235 11.2
but also at full scale application could improve the strength of 30% 0.0452 <DL 1.3569 <DL 0.7854 11.4
the matrices. Recently, researchers have started to examine the 50% 0.0632 <DL 1.5248 <DL 0.9856 11.6
effect of the water wash on geopolymerization (Zheng et al., 5050% bottom-y ash
2011; Ferone et al., 2013) and have concluded that this pretreat- 20% 0.0245 <DL 1.9856 <DL 0.5789 11.2
30% 0.0365 <DL 2.0145 <DL 0.5698 11.4
ment method substantially promote the early strength and result
50% 0.0695 <DL 2.1452 <DL 0.7854 11.4
in a higher ultimate strength of geopolymers.

Please cite this article in press as: Tzanakos, K., et al. Solidication/stabilization of ash from medical waste incineration into geopolymers. Waste Manage-
ment (2014), http://dx.doi.org/10.1016/j.wasman.2014.03.021
 K. Tzanakos et al. / Waste Management xxx (2014) xxxxxx
It is also important to note that as the percentage of medical
waste ash, that was used for the production of the geopolymers,
was increased, the concentrations of the heavy metals were smal-
ler than expected. All nal pH values of the TCLP leaching tests
were quiet similar and ranged between 10 and 11.6.
Finally, comparing the results of the four series of the experi-
ment, it was seen that the addition of calcium carbonate to the pro-
duced geopolymers (second series of experiment) did not affect the
leachability of the heavy metals, while the addition of y ash (third
and fourth series) caused the expected change in the concentration
of the nal stabilized specimens based on the concentration of
these metals in both kinds of ash.
4. Conclusions
This study demonstrates that geopolymers can be produced
with the use of only grounded medical waste bottom ash as a
raw material. Moreover, the addition of y ash and calcium car-
bonate caused a signicant increase in the compressive strength
of the geopolymer matrices. An increase at the compressive
strength of the geopolymers in all the series also was observed
with the percentage increase of the ash used for its production.
Regarding the results of the XRD method the addition of calcite
carbonate in the second series and y ash in the third series did not
affect the crystalline phase of the geopolymers. On the other hand
in the fourth series, where the quantity of the y ash at the speci-
mens increased considerably, the calcite became the main crystal-
line phase.
Furthermore, in all the geopolymer matrices all the measured
heavy metals were found at concentrations lower than the permit-
ted limits for the US EPA TCLP test. So, this study is another prove
that geopolymerization is able to reduce the leachability of the
heavy metals which already exist at the waste ash used for the pro-
duction of the geopolymers.
Finally, this study represents the rst attempt to use medical
waste ash as a raw material for the production of geopolymers. A
more systematic and long-term study of the physical characteris-
tics of the produced geopolymers, though, is suggested in the
future.
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Please cite this article in press as: Tzanakos, K., et al. Solidication/stabilization of ash from medical waste incineration into geopolymers. Waste Manage-
ment (2014), http://dx.doi.org/10.1016/j.wasman.2014.03.021