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Durability Against Wetting Drying Cycles of Water Treatment Sludge Fly Ash Geopolymer and Water Treatment Sludge Cement and Silty Clay Cement Systems
Durability Against Wetting Drying Cycles of Water Treatment Sludge Fly Ash Geopolymer and Water Treatment Sludge Cement and Silty Clay Cement Systems
Durability Against Wetting Drying Cycles of Water Treatment Sludge Fly Ash Geopolymer and Water Treatment Sludge Cement and Silty Clay Cement Systems
Abstract: The viability of using two waste materials, water treatment sludge (WTS) and fly ash (FA), for developing sustainable masonry
units has been previously investigated in terms of strength but the important aspect of durability against wetting–drying (w–d) cycles has yet
to be studied. A study on durability against w–d cycles, an important parameter for service life design of the sustainable masonry units, is
investigated in this paper. The liquid alkaline activator (L) was a mixture of sodium silicate (Na2 SiO3 ) and sodium hydroxide (NaOH), and a
high calcium fly ash (FA) was used as a precursor. The results of cyclic w–d test indicate that the WTS–FA geopolymer manufactured with an
optimum ingredient (L∶FA ¼ 1.6, Na2 SiO3 ∶NaOH ¼ 90∶10) and at an optimum heat condition of 85°C for 72 h can be used as durable
bearing masonry units; i.e., the compressive strength is greater than 12 MPa after 12 w–d cycles. For this optimum ingredient, the w–d
cycle strength, quðw−dÞ at heat temperatures between 65 and 95°C and durations between 24 and 120 h was found to be mainly dependent
upon the initial soaked (without w–d cycle) strength qu0 , and the normalized strength quðw−dÞ =qu0 versus number of w–d cycles relationship
expresses as a logarithm function. This relationship facilitates a mix design to attain the required strength at a target service life, which is
very useful for civil engineering practitioners and researchers alike. It is evident from this research that portland cement is not a suitable
cementing agent to manufacture WTS masonry units because alum in WTS retards the cement hydration, unlike a geopolymer binder, which
was proven to be suitable. Compared with a traditional clay–cement sample at the same initial soaked strength, the WTS–FA geopolymer
sample exhibits higher durability. This indicates that the WTS–FA geopolymer masonry units have a longer service life than clay–cement
masonry units, which is typically used in many countries. This research enables WTS traditionally destined for landfill to be used in a
sustainable manner as an aggregate in geopolymer masonry units, which is significant from engineering, economical, and environmental
perspectives. DOI: 10.1061/(ASCE)MT.1943-5533.0001351. © 2015 American Society of Civil Engineers.
Author keywords: Sludge; Fly ash; Geopolymer; Durability; Wet–dry cycles; Masonry units.
liquid alkaline activator. Fly ash (FA) derived from coal-fired elec-
tricity generation provides the greatest opportunity for commercial
utilization of this technology due to the plentiful worldwide raw
material supply (Van Jaarsveld et al. 1998; Mohapatra and Rao
2001). FA is extensively used as a precursor for geopolymers in
Australia (Rickard et al. 2011; Rickard et al. 2012) and Thailand Fig.1. Grain size distribution of WTS, silty clay, and FA
(Chindaprasirt et al. 2007; Sata et al. 2012).
Sukmak et al. (2013a, b, 2014) previously investigated the
strength and durability of a clay–FA geopolymer as bearing ma-
Table 1. Chemical Composition of WTS, Fly Ash, and Silty Clay
sonry units. The 7-day strength of the clay–FA geopolymer is
greater than 10 MPa, suitable as bearing masonry unit. The durabil- Chemical
ity against sulfate attack of clay–FA geoplymer is better than that composition (%) WTS Fly ash Silty clay
of clay–cement; i.e., there is no major change in the microstructure SiO2 67.33 47.51 26.15
and pH of the clay–FA geopolymer when exposed to sulfate Al2 O3 22.47 13.14 20.10
solutions. Fe2 O3 6.15 6.66 7.55
Even though Suksiripattanapong et al. (2015) have shown that CaO 0.68 30.24 32.89
the strength of WTS–FA geopolymer meets the requirement speci- MgO N.D. N.D. 0.47
fied by TIS, the durability of this material has not been examined. SO3 1.04 N.D. 4.92
This material generally encounters the change of weather during Na2 O N.D. 0.41 N.D.
K2O 1.26 1.63 3.17
wet (rainy) and dry (summer) seasons, which is particular relevant
LOI 0.78 0.42 3.44
for tropical countries such as Thailand, as well as parts of Australia.
The wetting and drying (w–d) cycles result in tension and surface Note: N.D. = Not detected.
cracks, which reduce the strength of material. The investigation of
the service life of the WTS–FA geopolymer via a w–d cycle test is
significant and is the focus of this research. SiO2 and Al2 O3 in crystal form. The specific gravity is 2.61
FA is used as a precursor and a mixture of NaOH and Na2 SiO3 is and the liquid limit is 69%. The WTS is classified as a nonplastic
used as a liquid alkaline activation in this research. The geopoly- material because the plastic limit could not be measured using
merization reaction is accelerated by appropriate heat temperature ASTM D 4318 (ASTM 2005). The compaction characteristics
and duration. The durability of the WTS–FA geopolymer is com- under modified Proctor energy [ASTM D 1557 (ASTM 2012b)]
pared with that of WTS–cement and silty clay–cement. The silty are optimum water content (OWC) of 34.3%, and maximum dry
clay is abundant and commonly used as aggregate to produce non- unit weight (γ dmax ) of 12.37 kN=m3 .
bearing masonry units in Thailand. Results of durability test on the
three materials (WTS–FA geopolymer, WTS–cement, and silty Silty Clay
clay–cement) will be compared to examine the role of aggregates Silty clay was collected from the Suranaree University of Technol-
and binders (cement and geopolymer) on the manufacture of ma- ogy campus in Nakhon Ratchasima province of Thailand at a depth
sonry units. This research will enable WTS traditionally destined of 3 m. Fig. 1 shows the grain size distribution of the silty clay,
for landfill to be used in a sustainable manner as an aggregate in indicating 2% sand, 43% silt, and 55% clay. D50 is 0.0009 mm
geopolymer masonry units, which is significant from engineering, and its specific gravity is 2.76. The liquid and plastic limits are
economical, and environmental perspectives. approximately 61 and 22%, respectively. Based on the unified soil
classification system (USCS), the clay is classified as highly plastic
(CH). The soil swelling potential was investigated by the free swell-
Materials and Methods ing test proposed by Prakash and Sridharan (2004), which predicts
the dominant clay mineralogy of soils satisfactorily (Horpibulsuk
et al. 2007). The free swell ratio, FSR, is defined as the ratio of
Materials
equilibrium sediment volume of 10 g of oven-dried soil passing
through a 425-μm sieve in distilled water (V d ) to that in carbon
Water Treatment Sludge (WTS) tetra chloride or kerosene (V k ). The clay is classified as low swell-
WTS was collected from the Bang Khen water treatment plant of ing with a free swell ratio (FSR) of 1.4. The chemical composition
the Metropolitan Waterworks Authority of Thailand. The WTS at using X-ray fluorescence (XRF) of the silty clay is shown in
this plant consists of 0.12% sand, 99.72% silt, and 0.16%. The Table 1.
average grain size, D50 , is 0.015 mm (15 microns). The grain size
distribution and mineral and chemical compositions were obtained Fly Ash (FA)
from laser particle and X-ray fluorescence (XRF) analysis as shown FA was obtained from the Mae Moh power plant of the electricity
in Fig. 1 and Table 1, respectively. WTS is composed mainly of generating authority of Thailand (EGAT) in the northern region of
Fig. 2. Scanning electron microscopy (SEM) images of (a) sludge; (b) silty clay; (c) fly ash
Thailand. The specific gravity of FA is 2.35. Table 1 summarizes of WTS–FA geopolymer was found at Na2 SiO3 ∶NaOH ratios
the chemical composition of FA using X-ray fluorescence (XRF). between 100:0 and 50:50 (Suksiripattanapong et al. 2015). The
Total amount of the major components (SiO2 , Al2 O3 and Fe2 O3 ) air-dried WTS and FA were mixed for 5 min in a mixer to ensure
are 67.58% while the CaO content is 30.24%; therefore, it is clas- uniformity of the mixture. The mixer was stopped and the mixture
sified as Class C according to ASTM C 618 (ASTM 2012a). Fig. 1 was activated by the liquid alkaline activator (L) and mixed for an
shows the grain size distribution curve of FA, which was tested by a additional 5 min. The mixture was then compacted under the modi-
laser particle size analysis. The average grain size of FA is 13.25 fied Proctor energy. Once the compaction curves were obtained,
microns, which is similar to that of WTS. It is shown that both the the WTS–FA–L mixture at various L–FA contents was statically
FA and WTS particles are larger than the silty clay ones. The mor- compressed in a cylindrical mold with a 50-mm diameter and a
phology of the WTS and the FA is shown in Fig. 2. The FA particles height of 100 mm. The compression was performed by a manual
are fine and spherical whereas the WTS and silty clay particles are hydraulic jack. The samples were dismantled, wrapped within vinyl
irregular in shape. sheet, and then cured at ambient room temperature, 65, 75, 85, and
95°C respectively for durations of 24, 48, 72, 96, and 120 h. After
Liquid Alkaline Activator (L)
heating (at 65, 75, 85, and 95°C), the samples were subsequently
The liquid alkaline activator (L) is a mixture of Na2 SiO3 , which
cured at room temperature (27–30°C) until the various preplanned
consists of 9% Na2 O and 30% SiO2 by weight, and NaOH with
curing times lapsed. Compressive strengths of WTS-FA geopoly-
a concentration of 10 molars. Both Na2 SiO3 and NaOH are chemi-
cal analytical reagents. mer samples were measured after 7 and 28 days of curing in accor-
dance with ASTM D 1633 (ASTM 2000). The durability of WTS–
FA geopolymer was measured after 28 days of curing in accordance
Sample Preparation with ASTM C599-03 (ASTM 2003).
Durability Test
The method of cyclic w–d test as per ASTM C599-03 (ASTM
2003) was adopted for sample preparations. The samples were sub-
merged in deionized water at room temperature for 5 h. They were
then dried in an oven at a temperature of 70°C for 48 h and air-dried
at room temperature for at least 3 h. This process is referred to as 1
Downloaded from ascelibrary.org by Indian Institute of Technology Hyderabad on 01/02/20. Copyright ASCE. For personal use only; all rights reserved.
w–d cycle. After attaining the target w–d cycles, the samples were
immersed in deionized water for 2 h at the constant temperature of
25–2°C. Unconfined compression (UC) tests were then undertaken
with a rate of vertical displacement of 1 mm=min. The 1, 3, 6, 9,
and 12 w–d cycles were considered in this study.
where the coefficient of correlation is 0.91. Using Eq. (1), the w–d
cycle strengths of samples at various heating conditions for a target
number of w–d cycles can be approximated once the corresponding
qu0 is known. The qu0 is simply determined directly from a labo-
ratory UC test. Eq. (1) is thus useful for civil engineering practi-
tioners and researchers since the durability test is time-consuming.
more suitable binder to stabilize WTS than portland cement. Buchwald, A., and Kaps, Ch. (2002). “Property controlling influences on
Alum in WTS retards the cement hydration and hence the the generation of geopolymeric binders based on clay.” Geopolymer
strength of WTS–cement is essentially the same even with 2002, Melbourne, Australia.
the increase in input of cement. When compared with two non- Chindaprasirt, C., Chareerat, T., and Sirivivatnanon, V. (2007). “Workabil-
bearing stabilized materials (silty clay–cement and WTS–FA ity and strength of coarse high calcium fly ash geopolymer.” Cem.
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geopolymer) at the same initial strength (before cyclic w-d test),
Davidovits, J. (1991). “Geopolymers.” J. Therm. Anal. Calorim., 37(8),
the durability of the WTS-FA geopolymer is better than that of 1633–1656.
the silty clay–cement. The strength of the silty clay–cement Davidovits, J., Buzzi, L., Rocher, R., Gimeno, D., Marini, C., and Tocco, S.
sharply decreases with c and becomes lower than the TIS (1999). “Geopolymeric cenment based on low cost geologic material
strength requirement when c > 9, while the strength of the results from the European Researh project GEOCIS-TEM.” Proc.,
WTS–FA geopolymer meets the TIS strength requirement even 2nd Int. Conf. Geopolymer, 83–96.
after 12 w–d cycles and it is essentially constant when c > 3. Disfani, M. M., Arulrajah, A., Bo, M. W., and Suthagaran, V. (2012).
• This research enables WTS traditionally destined for landfill “Environmental risks of using recycled crushed glass in road applica-
to be used in a sustainable manner as an aggregate in geopoly- tions.” J. Cleaner Prod., 20(1), 170–179.
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Authority of Thailand in the fiscal year 2013, the Thailand (2006)132:5(562), 562–576.
Research Fund under the TRF Senior Research Scholar program Horpibulsuk, S., Katkan, W., and Apichatvullop, A. (2008). “An approach
Grant No. RTA5680002, the Office of Higher Education Commis- for assessment of compaction curves of fine-grained soils at various
sion under NRU project of Thailand, and Suranaree University of energies using a one point test.” Soils Found., 48(1), 115–125.
Technology. Horpibulsuk, S., Katkan, W., and Naramitkornburee, A. (2009). “Modified
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