Stabilization of heavy oil fly ash (HFO) for construction ... · possibility of stabilizing HFO...

International Journal of Applied Engineering Research ISSN 0973-4562 Volume 12, Number 4 (2017) pp. 488-497

© Research India Publications. http://www.ripublication.com

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Stabilization of heavy oil fly ash (HFO) for construction and environmental

purposes

Mazen Alshaaera,b*, Mohammed Shqaira, Hesham G. Abdelwaheda,c, Khaled Abuhaseld, Montserrat Zamorano Toroe

a Plasma Technology and Material Science Unit (PTMSU), Physics Department, College of Science and Humanitarian Studies, Prince Sattam bin Abdulaziz University, Alkharj 11942, P.O 83, Saudi Arabia

bGeoBioTec — Geobiosciences, Geotechnologies and Geoengineering Research Center, Campus de Santiago, University of Aveiro, 3810-193 Aveiro, Portugal

c Theoretical Research group, Physics Department, Faculty of Science, Mansoura University, 35516 Mansoura, Egypt. d Mechanical Engineering Department, College of Engineering, University of Bisha, Bisha 61361, Kingdom of Saudi Arabia,

Saudi Arabia. e Department of Civil Engineering, Granada University, 18071 Granada, Spain

*ORCID: 0000-0001-5657-5418

Abstract

This work aims to investigate the stabilization of heavy oil fly

ash (HFO) using a geopolymerization technique. The

stabilization technique entails adding HFO as the filler

material to a geopolymer matrix derived from metakaolin.

Weight ratio of 20% — compared with the powder precursor

(metakaolin) — were added to the metakaolin-based

geopolymer. XRD analysis showed that the HFO-based

geopolymer comprised two amorphous phases: gel and HFO

particles. The HFO-based geopolymer cement exhibited a

flexural strength of 7.5MPa, and compressive strength of

31MPa and 28MPa, respectively under dry and immersed

conditions. The geopolymer produced featured relatively low

density, 1.34 g/cm3, and reasonable water absorption, 18%

(w/w), compared with other cement-based materials. A

leaching test showed that the HFO toxic metals, such as Ni,

Cr, Cu, and Pb, are effectively immobilized in the geopolymer

matrix and exhibit concentrations significantly lower than

those of HFO powder. The general evaluation of the

geopolymer cement produced from metakaolin and HFO

particles indicates its potential for a number of applications,

including “green” construction materials.

Keywords: Geopolymers, Metakaolin, Construction, Heavy

oil fly ash, microstructure

INTRODUCTION

Fuel oil fly ash (HFO) is a powdered residue generated in

large amount by plants that use oil as the source of fuel, as

power and water desalination plants. For example, in Saudi

Arabia, annually more than 40 million metric tons of oil are

consumed both for operation of sea water desalination and

thermal power plants [1]; and in Egypt, more than 4000 metric

tons of HFO are generated by electric power plants [2].

The chemical composition of HFO has been investigated by

several researchers [1-4], resulting on important differences

comparing to coal fly ash; it is mainly composed of C, around

95%, a very high percentage compared to coal fly ash with

values between 20 and 50 [Al-Malack et al., 2013]. These

results has also shown the presence of S and heavy metals,

particularly V, Fe and Ni [1,2], in addition to Pb, Al, Ca, Mg,

Si, and N, transition metals (Mn, and Co) and alkaline-earth

metals (Ba, Ca, and Mg) may also be added for the

suppression of soot or for corrosion control [1,2-12].

In some countries, for example Arabia Saudi, legislative

measures and monitoring are taken to protect the environment

from this contamination so the produced HFO is collected

using electrostatic precipitators (ESPs) installed in the major

facilities and, frecuently, disposed into landfills [11].

However in the case of another countries, for example Egypt,

none of the power plants, situated in a densely populated

region is fitted with ESPs and no legislative measures and

monitoring are taken to prevent the surrounding groundwater

and soil contamination [11]. In addition, most of the generated

ashes are not used for anything but landfill, so the disposal of

HFO is a major environmental challenge for thermal power

plants; it produces a dispersion of heavy metals in the

surrounding groundwater and soil that may cause a serious

contamination of water and soil with heavy metal.

Several studies have highlighted the toxic effects of the metal

constituents of HFO such as V, Ni, Zn and Pb [13-16] due to

the soluble metals in the extracts of the samples, carcinogenic

and other health hazards associated with their emission [13].

Particularly airborne particulate matter (PM) is more harmful

because they can inter the lung; smaller particles have been

associated with adverse health effects such as respiratory

disease and cardiovascular diseases. It is suggested that metal

ions encountered in the surface of HFO particles (like V and

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Ni) may be the main reason of the induction of allergic

responses in the respiratory system through suppressing

receptor 4, innate immunity receptors, degradation [17,18].

Therefore, HFO production should receive a considerable

attention to avoid the contamination of the environment and

minimize their negative effects on the human health.

Against this background, a study on the use of HFO as a

cement replacement material in low grade concrete

applications was recently performed [19]. Being a carbon-rich

material, with a high specific area and low density, HFO has a

significant influence on cement-based mixtures, contributing

to an extended setting time, and increasing water demand and

high levels of Portlandite. A suitable flowable fill concrete

was synthesized when limiting the cement replacement to

30% [19]; concrete masonry units with adequate strength were

produced with replacement levels of 20%. HFO has also been

used in epoxy pipe formulations for total or partial

replacement of a commercial light stabilizer, TN® N24,

without influencing the thermal or mechanical properties of

the pipes. The optimum amount of HFO was identified as 4

wt% in a previous study [20]; this replacement had no

observable impact on the thermal or mechanical properties of

the composites.

Another application for HFO is the production of activated

carbons through the pyrolysis of a mixture of HFO and road-

paving asphalt dissolved in kerosene at 650oC in an N2

atmosphere [21]. Asphalt acts as a binder to hold the HFO

particles together, and the HFO supports this carbon structure.

The activated carbon produced from HFO can also be used to

remove non-carbonaceous impurities. The results from this

study show a maximum adsorption capacity of 0.3001 mg/g

for NH4OH functionalized activated carbon with an 86.43%

regeneration efficiency [21].

Finally, stabilization is a process that involves the mixing of a

waste or filler with a binder material to reduce the

contaminant leachability and to convert the hazardous waste

into an environmentally acceptable waste form for land

disposal or construction applications [22]. Stabilizing wastes

using geopolymers is a solution that has been investigated

over a number of years [23-31]. One study [27] for stabilizing

HFO using untreated kaolinite-based geopolymers showed

that end products exhibit a high reduction in compressive

strength, varying from 30% to 85%, from adding HFO to this

type of geopolymers.

The present paper is a preliminary study to investigate the

possibility of stabilizing HFO from power plant using a

metakaolin-based geopolymer as the binder material. The

products have been evaluated for immobilization of HFO a

number of toxic heavy metals in the geopolymer matrix, and

for construction purposes.

MATERIALS AND METHODS

Sampling

A sample of HFO was collected from a Jordanian electric

power plant. The HFO sample was dried in an oven at 105 oC

for one day and finally it was sieved, taking the particle size

fraction less than 300 µm for study.

Production of geopolymer and HFO-based geopolymer

cements

Two series of geopolymer cements samples have been

prepared. Firstly a reference specimen (SK) was prepared with

metakaolin, and without HFO. Secondly a HFO-based

geopolymer cement (GA) was prepared by adding HFO as a

filler, without reducing the original weight ratio of precursor

(metakaolin); in this case the mass percentages of HFO used

was 20% of the metakaolin.

The geopolymer binder materials were prepared using HFO,

kaolinite and alkali solutions based on sodium silicate

(Na2SiO3) and sodium hydroxide (NaOH). Kaolinite from a

natural deposit located in the Ar Riyad-Al Kharj area,

specifically at Khushaym Radi [32]; it was heated at 750 oC

for 4 h in a laboratory furnace to obtain the respective

metakaolinite. Na2SiO3 and NaOH solutions were used as

alkaline activators for the dissolution of aluminosilicate

phases. The sodium silicate solution (Merck, Germany)

contained 27% SiO2 and 8% Na2O. The hydroxide solution, at

a concentration of 6.0 M, was prepared using sodium

hydroxide (NaOH) flakes of 98% purity (Merck) and distilled

water.

The following ratios were used in the alkaline activation

process:

SiO2 (in sodium silicate solution)/Al2O3 (in

metakaolinite) molar ratio of 1.

Na2O (in sodium silicate and NaOH solutions)/Al2O3

(in metakaolinite) molar ratio of 1.

The H2O/Na2O molar ratio was 13.

The geopolymer production method involves mechanical

mixing, for 1 min, of an aqueous solution composed of

Na2SiO3, NaOH and H2O, Figure 1. Afterward, the metakaolin

was mixed with the sodium hydroxide and sodium silicate

solutions for 15 minutes. The final pulp was then poured into

three rectangular molds to carry out in triplicates mechanical

and physical characterization (160mm×15mm×30mm each);

specimens were cured in a ventilated oven (Binder-ED115,

Germany) at 40ºC for one day and, after curing, they were

removed from the molds and cooled at room temperature [25].

In addition, three discs (2cm×2cm×1cm) were prepared from

each mixture, to carry out microstructural and mineralogical

analyses.



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Figure 1. Schematic diagram of the experimental procedure

Testing methods

X-ray Diffraction Studies

X-ray Diffraction (XRD) was carried out on HFO sample and

on powdered samples of kaolin geopolymer (SK) and heave

oil fly ash cement (GA) to analyse microstructural of HFO. It

was applied to identify major crystalline of HFO and

potentially newly formed phases after geopolymerization

process. A Shimadzu diffractometer-6000 (Japan) with a Co

tube and a scanning range from 5o to 80o 2θ at a scan rate of

2°/min was used. Qualitative analysis was carried out using

the crystalline phases, identified by detecting and analyzing

the positions of the peaks using the software package supplied

with the instrument.

Scanning Electron Microscopy and Energy-dispersive X-ray

spectroscopy (SEM/EDX)

The Scanning Electron Microscope combined with Energy-

dispersive S-ray spectrometry (SEM–EDX) was used to

study elemental analysis, chemical characterization and

morphology of HFO particles and stabilized HFO particles,

after geopolymerization process.

It was conducted with an Inspect F50 scanning electron

microscope (SEM) (The Netherlands). Samples were mounted

in epoxy resin and the surfaces were ground flat by 600 grit

abrasive paper. The samples were then polished to achieve a

smooth surface. The polished samples were placed into a

vacuum and etched into argon gas for 20 minutes. The

microstructures of the samples were examined with SEM and

photographs were taken to be analyzed. Finally, the energy



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dispersive spectroscopy (EDX) was used to determine the

elemental composition of manually chosen areas in the HFO

before and after stabilization process.

Physical characterization of HFO

Bulk density and total porosity of HFO have been determined

using helium pycnometry (Helium AccuPyc 1330,

Micromeritics, USA). Helium–air pycnometry is a

nondestructive, quick and reliable tool that measures the

volume of solid objects of irregular or regular shape whether

powdered or in one piece; therefore, helium–air pycnometry is

a well-suited technique to be used for HFO analysis [1]. The

pycnometer determines skeletal volumes by observing the

reduction of gas capacity in the sample chamber caused by the

presence of the given sample. Helium, as well as other

suitable gases, penetrates the smallest pores and surface

irregularities common in CCB samples, allowing the volunme

obtained to be used for the computation of the ultimate

theoretical density of the solid comprising the sample.

Leaching test

To study the effectiveness of geopolymerization on

immobilization of HFO heavy metals in the geopolymer

matrix, the leaching test results from the HFO-geopolymer

cement were compared with the leaching test results from the

HFO powder. The toxicity of the chemical elements are

classified according to the International Union of Pure and

Applied Chemistry (IUPAC).

For fly ash leaching analysis, 1g of fly ash (HFO) was heated

at 95oC for two hours with 10ml of 70% HNO3 and 3ml of

60% HClO4, according to German standard (DIN 38414). The

solution was cooled down and diluted with 10ml HCl 1:1

(density 1.18gml-1). The diluted solution was then filtered and

diluted with distilled water up to 50ml [32].

For the leaching test of the 50 g of powdered GA sample with

grain size <100 µm were placed in 500 ml deionized water.

After agitating the sample at room temperature for 24 hours, it

was filtered and analyzed by means of Inductively Coupled

Plasma–Optical Emission Spectrometry (ICP-OES) (GBC-

Quantima sequential, Australia). The leaching tests were done

at a constant pH solution of 7.

Geopolymer cements characterization

Physical characteristics of fabricated specimens have been

studied by bulk density and water absorption of fabricated

specimens; these tests were developed according to Standard

Methods ASTM C97 / C97M – 15 Standard Test Methods for

Absorption and Bulk Specific Gravity of Dimension Stone.

Flexural strength and compression strength were used to

mechanical characterization of the fabricated specimens for

each series. These tests were performed according to ASTM

C78 / C78M – 16 (Standard Test Method for Flexural

Strength of Concrete, Using Simple Beam with Third-Point

Loading) and ASTM C116-90 (Test Method for Compressive

Strength of Concrete Using Portions of Beams Broken in

Flexure), respectively. Both tests have been developed at

room temperature and with a universal testing machine. The

bending specimen's dimensions were: height=15 mm,

width=30 mm and length=160 mm; the distance between the

supports was 120 mm and the speed of the machine head

during testing was 0.1 mm/minute. Compression tests were

performed on the failed bending specimens, placed on their

side with a loading area=40×15 mm2 and height=30 mm. The

speed of the machine head during testing was 2 mm/minute.

RESULTS AND DISCUSSION

Microstructural characteristics

Metakaolin and HFO particles were transformed into solid

and hard matrix through the geopolymerization process. The

XRD patterns (Figure 2) of the resulting materials —SK, and

GA, cements— show high humps between 15o to 35o. The

hump with a few peaks indicates that the main phases of the

resultant products are largely amorphous [33-37]. The XRD

peaks correspond to the mineral anatase (TiO2), which already

existed in the precursor (kaolin) as previously reported [29].

In general, no significant change in the mineral composition is

observed with adding HFO (GA cement). This is indication

that HFO could be used as functional filler, with limited

contribution in setting reactions.

Figure 2, Qualitative XRD patterns of the cements

The heavy oil fly ash studied is made up mostly of porous

particles with a bulk density of 0.34g/cm3, and total porosity

of 82% as reported by the helium pycnometer measurements,

and this is in good agreement with previous studies [1]. The

SEM micrograph of HFO seen in Figure 3A shows that the

surface of the HFO particle is not smooth; it is characterized

by the presence of hollow voids several microns in diameter.

These hollow voids were formed by the eruption of gas during



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combustion. In consequence these particles would be weak

and easily disintegrate in liquids, and therefore release toxic

heavy metals such as Pb, Ni, Cr, and Cu. The SEM analysis

has been also applied to HFO stabilized particle in GA sample

(Figure 3B, point 1); it shows that HFO particles are fully

surrounded and bonded by geopolymer gel (point

2).;The higher magnification SEM images of the stabilized

HFO particle better display the macropores as reported in

Figure 3C showing that these pores are filled with geopolymer

gel filling during the reactions (Figure 3C, point 3). In

consequence we could conclude this geopolymer matrix could

stabilize the HFO particles, preventing their disintegration and

therefore the release of toxic heavy metals [25].

Figure 3. SEM image of A) HFO particle, B) typical HFO stabilized particle (GA), and C) Higher magnification SEM image of

the HFO particle

Figure 4. SEM image of geopolymer gel, and partially reacted metakaolin



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Metakaolinite, as a precursor in this study, was attacked by

the alkaline solution during geopolymerization as seen in

Figure 4. Microstructural observations through SEM analyses

reveal phase heterogeneities; geopolymer gel (point 1), and

partially reacted metakaolin (point 2). The chemical

analyses by EDX involved scanning three different areas of

the HFO particles and the geopolymer gel (GA and SK), as

displayed in Figure 5. The HFO particle comprises 72%

carbon, in addition to Na, Si, Al, and S. The low percentages

of Si (2%) and Al (3%) oxides of the HFO contents point to

the limited contribution of these particles to the composition

of the geopolymer gel. Thus, they are stable even after the

hardening of the material, as shown in Figure 3B.

Figure 5. EDX analysis of different phases; HFO particle, and geopolymer gel of GA and SK

The chemical EDX analysis, reflected in Table 1, gives the

complete set of compositional data expressed as mean molar

percentage of the HFO, GA, and SK. The geopolymer gels of

GA and SK cements are composed of the same elements.

Carbon and sulfur, constituents of HFO, are not involved in

the geopolymerization process and the resultant geopolymer

gel. The Si/Al and Al/Na molar ratios of the precursors are 1.

The Si/Al molar ratio changed to 1.3 in the reference

geopolymer cement (SK). This indicates that the Al oxide

decreased in the resultant gel, due to the partial reaction of

metakaolin (source of Al in the geopolymerization reactions).

When compared with reference geopolymer (SK), a slight

decrease in Na oxide is observed in the geopolymer gel of

GA. This reduction in the molar percentage of Na in GA

could be the result of adsorption of this element by the porous

HFO particles. However, the molar percentages of Al, Na, and

Si of the geopolymer gel in SK and GA cements are still

within an acceptable range, in view of previous studies [36,

38]. We may therefore conclude that the HFO particles

preserve their physical structure after geopolymerization, with

no significant involvement in the chemical composition of the

resultant geopolymer gel.



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Table 1. EDX analysis of different phases

Elements HFO particle GA SK

C 72.0 0.0 0.0

O 18.8 63.1 60.5

Na 1.8 11.1 13.6

Al 2.2 11.3 11.3

Si 3.0 14.6 14.7

S 2.2 0.0 0.0

Molar ratio HFO GA SK

Si/Al 1.3 1.3 1.3

Al/Na 1.2 1.0 0.8

Si/Na 1.6 1.3 1.1

Geopolymer cements properties

It may well be that HFO particles have no significant

chemical effect on the geopolymer cement as stated in the

previous section; however they could bear an influence on the

physical and mechanical properties because of their low

density and high porosity [1]. In consequence both properties

have been analyzed below.

Physical properties

On the one hand, the bulk density and water absorption of the

geopolymer cements are given in Figure 6. The bulk density

of the geopolymer without HFO (SK) is 1.41 g/cm3 -

comparable with other reports [34-39]. Adding low density

HFO particles with weight ratio of 20% as compared with the

metakaolin used would decrease the bulk density to 1.34

g/cm3. This limited decrease in bulk density could result from

geopolymer gel filling HFO macropores during the reactions.

On the other hand, the water absorption decreased by adding

20% of HFO particles (GA), from 21% to 18%, as seen in

Figure 6.

Results of bulk density and water absorption indicate that the

pore system of the HFO was blocked or filled by geopolymer

gel after geopolymerization, as we have concluded before.

Figure 6. Bulk density and water absorption of the produced

geopolymer cements

Mechanical properties

Figure 7 displays the maximum compressive strengths of

HFO-based geopolymer (GA), 31MPa and 28MPa,

respectively under dry and immersed conditions. These values

are approximately 9 and 29% lower than SK geopolymer. In

the case of immersed sample compressive strength of GA is

lower than 30 MPa, the value established by EH-08.

Figure 7. Mechanical properties of the produced geopolymer

cements

In the case of the flexural strength for dry conditions, HFO-

based geopolymer has resulted 7.5MPa (Figure 7), 39% lower

than SK geopolymer. These results have shown that using

calcinated natural kaolinitic soil as the precursor material and

HFO as a filler in the starting mixture affects the

microstructure and strength of the produced geopolymers to a

certain degree. Although the mechanical properties of HFO-

based geopolymers have been lower than SK geopolymers,

values are comparable with those of ordinary concrete with

values around [40]. Hence, the HFO-based geopolymers

studied here satisfy the criteria for use in housing and general

construction applications.



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Leaching behavior

A preliminary study was carried out to analyze the HFO

leachate from heavy metals, and the effectiveness of

immobilization of these heavy metals in the geopolymer

matrix. Table 2 shows the concentration of different metals

leached from the HFO powder and the HFO-based

geopolymer matrix (GA) after immersion in a solution of

pH=7 for one day. The toxicity of the chemical elements are

classified according to the International Union of Pure and

Applied Chemistry (IUPAC) [38].

The HFO powder exhibits high leachability for Na, Zn, Al,

Ni, Fe, Pb, Mn, Cu and trace elements Ca, Mg and Co in

neutral conditions. The first toxic element is Ni, which causes

allergy for many years; often it will remain for the rest of life

[41]; Co inhalation can lead to ‘hard metal disease’,

respiratory sensitization, pneumonia, wheezing, and asthma

[42]; Exposure to Pb can be toxic to humans and wildlife [43];

Excessive Cu absorption can occur through the skin, by

inhalation or by ingestion [44]. Finally, The toxic action of

Cr is confined to the hexavalent compound (Cr VI), which is

a highly toxic carcinogen and may cause death to humans and

animals if ingested in large doses [45].

Table 2. Concentration (ppm) of leached metals from HFO

powder and GA after immersion in pH = 7 for 1 day

Elemen

t

Toxicity ( IUPAC)

[38]

HFO

(ppm)

GA

(ppm)

Na X 21.6 179.2

Ca X 0.6 1.6

Zn X 164.0 0.0

Mg X 0.1 0.6

Fe X 3.3 0.1

Mn X 1.0 0.0

Al X 189.0 39.2

Ni Toxic 32.0 0.0

Co Toxic 0.1 0.0

Pb Toxic 1.6 0.0

Cu Toxic 1.2 0.0

Cr Toxic 4.1 0.0

Interestingly, Ni, Cr, Cu, Mn, Zn and Pb do not show

considerable leaching in GA despite their presence in the HFO

powder. For the GA specimens, however, these heavy metals

are effectively immobilized and exhibit concentrations

significantly lower than those of HFO powder. The GA matrix

exhibits high leaching of Na, and Al. The sources of these two

elements are the residual precursors of the geopolymer:

sodium silicate solution (Na), and metakaolin (Al). As evident

in Table 2, adding HFO to the geopolymers significantly

reduced leaching of the toxic heavy metals. Stabilization of

HFO heavy metals can occur chemically through

incorporation into the geopolymeric structure as a charge

balancing cation and/or physically through encapsulation

within the geopolymer gel [25, 38]. In this process, chemical

stabilization dominates the physical encapsulation because the

structural breakdown of the geopolymer gel does not lead to

substantial release of the heavy metals.

CONCLUSIONS

In this study, HFO particles were stabilized using a

geopolymerization technique. One important finding resides

in the possibility of using HFO for mass production of

geopolymer cement with high mechanical performance and

acceptable physical properties, a sound alternative to Portland

cement.

Metakaolin and HFO particles were transformed into solid

and hard matrix through the geopolymerization process. The

resultant phases are largely amorphous. The HFO is serving in

the resultant cement as functional filler, with limited

contribution in setting reactions. The HFO particles preserve

their physical structure after geopolymerization, with no

significant involvement in the chemical composition of the

resultant geopolymer gel. The geopolymer matrix stabilizes

the HFO particles, preventing their disintegration and

therefore the release of toxic heavy metals. The HFO pores

are filled with geopolymer gel filling during the reactions.

HFO particles bear an influence on the physical and

mechanical properties because of their low density and high

porosity. The mechanical properties of HFO-based

geopolymers are comparable with those of ordinary concrete.

Hence, the HFO-based geopolymers studied here satisfy the

criteria for use in housing and general construction

applications.

This study shows that HFO powder exhibits high leachability

for Na, Zn, Al, Ni, Fe, Pb, Mn, Cu and trace elements Ca, Mg

and Co in neutral conditions. Interestingly, Ni, Cr, Cu, Cd,

Mn, Zn and Pb do not show considerable leaching after

stabilizing in the geopolymer matrix. Stabilization of HFO

heavy metals can occur chemically through incorporation into

the geopolymeric structure as a charge balancing cation and/or

physically through encapsulation within the geopolymer gel.

Our research group has developed a preliminary study to use a

metakaolin-based geopolymer matrix that could provide a

satisfactory binder for the immobilization of a number of toxic

heavy metals, given its low permeability, resistance to acid

and chloride attack, and durability [28-29]. It is worth

mentioning that the leachability of contaminants from

stabilized metal geopolymer wastes is lower than that from

hardened Portland cement stabilized wastes [30,31].

http://corrosion-doctors.org/Pollution/chromiumtoxicity.htm

http://corrosion-doctors.org/Pollution/chromiumtoxicity.htm



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ACKNOWLEDGMENTS

The authors gratefully acknowledge financial support of the

project “Stabilization of heavy oil fly ash (HFO) for environmental and construction purposes” funded by the

Deanship of Scientific Research at Prince Sattam Bin

Abdulaziz University, within the Specialized Research Grant

program and under contract number 2014-01-2092 .

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