Mitigating Zinc Leachate from End-of-Life Tire Rubber in

Stabilized Clayey Soils

Thien Q. Tran, S.M.ASCE 1; Shiyu Li 2; Bin Ji 3; Xiang Zhao 4; Wencai Zhang 5;
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and Alexander S. Brand 6

Abstract: End-of-life tire (ELT) rubber has been widely researched to replace aggregates in construction materials such as asphalt concrete and
cementitious composites. Although most studies paid attention to its effect on engineering properties and the durability of the materials, very
few considered chemical reactions with pore solution and the potential for environmental leachate, especially rubberized stabilized soil, which
was proposed recently to increase the use of ELT rubber in civil engineering. This study proposes the use of rubberized stabilized soil (RSS) in
which clayey soils (e.g., kaolin and bentonite) were stabilized by portland cement (PC) and end-of-life tire (ELT) rubber particles. The authors
previously developed a methodology to extract zinc from the ELT rubber; therefore, this study explores the potential for RSS to immobilize the
leachate from the ELT rubber before and after this treatment. Three main topics are addressed in this study: (1) the capability of clay to capture
leached zinc under ambient and alkaline aqueous conditions; (2) engineering properties of RSS [i.e., unconfined compressive (UCS), flow] with
0%, 10%, 30%, and 50% ELT rubber added by clay volume; and (3) pore solution and leachability tests of RSS. A leaching experiment was
employed for Topic 1, UCS and flow tests were conducted for Topic 2, and pore solution extraction and leaching tests were performed for Topic
3. The results showed that the clayey soils and ELT rubber are synergistic in terms of engineering properties and the capturability of zinc and
total organic carbon (TOC). Although the ELT rubber and PC strengthen the clay structure, the clay absorbs leached zinc and TOC from the ELT
rubber particles. Adding untreated ELT rubber into PC-stabilized clays significantly increased the RSS strength; however, this improvement was
less significant for the treated ELT rubber. Ultimately, the results proved that the environmental and mechanical performance of RSS makes it a
viable construction material. DOI: 10.1061/JGGEFK.GTENG-12302. © 2024 American Society of Civil Engineers.
Author keywords: End-of-life tire (ELT) rubber; Rubberized stabilized soil (RSS); Total organic carbon (TOC); Zinc leachate; Clay
stabilization.

Introduction preserve natural resources (Bai et al. 2017; Koop and van Leeuwen
2017). End-of-life tire (ELT) is one waste issue that presents nu-
Waste recycling, particularly in urban areas, is of critical concern merous challenges to recycle (Abbas-Abadi et al. 2022). An esti-
to ensure quality of life, maintain or improve the ecosystem, and mated 3 billion ELTs are discarded worldwide every year (Rodgers
2021). In the US, 4.46 million tons of ELT were generated in 2019,
1
Ph.D. Student, The Charles Edward Via, Jr. Dept. of Civil and Envir- the majority of which was used as fuel and recycled into ground
onmental Engineering, Virginia Polytechnic Institute and State Univ., rubber and for other uses; however, an estimated 14.3% was land
Blacksburg, VA 24061. ORCID: https://orcid.org/0000-0002-0320-4418.
disposed, such as in landfills (US Tire Manufacturers Association
Email: [email protected]
2
Ph.D. Student, Dept. of Mining and Minerals Engineering, Virginia
2020). The US has an estimated stockpile of 56 million ELTs (US
Polytechnic Institute and State Univ., Blacksburg, VA 24061. Email: Tire Manufacturers Association 2020). Meanwhile, China gener-
[email protected] ates the highest amount of ELTs, at more than 15 million tons
3 of ELTs in 2019 (China Rubber Industry Association 2019). There-
Postdoctoral Researcher, Dept. of Mining and Minerals Engineering,
Virginia Polytechnic Institute and State Univ., Blacksburg, VA 24061. fore, sustainable practices and management of ELTs are of concern
Email: [email protected] (Araujo-Morera et al. 2021).
4
Undergraduate Researcher, The Charles Edward Via, Jr. Dept. of Civil Tire rubber is a complex formulation of various polymers
and Environmental Engineering, Virginia Polytechnic Institute and State (e.g., polyisoprene, polybutadiene, styrene-butadiene) and carbon
Univ., Blacksburg, VA 24061. ORCID: https://orcid.org/0009-0007
black with small amounts of zinc oxide, extender oil, stearic acid,
-9118-3293. Email: [email protected]
5
Associate Professor, Dept. of Mining and Minerals Engineering, and others (Rodgers 2021). Storage of ELTs can pose a fire hazard
Virginia Polytechnic Institute and State Univ., Blacksburg, VA 24061. (Poole 1998) since these materials are flammable and can pose a
Email: [email protected] risk to soil, groundwater, and air pollution (Gualtieri et al. 2005;
6
Assistant Professor, The Charles Edward Via, Jr. Dept. of Civil and En- Halsband et al. 2020). Of particular concern is zinc, which is added
vironmental Engineering, Virginia Polytechnic Institute and State Univ., as a vulcanizing agent and comprises 1% to 2% of the tire rubber by
Blacksburg, VA 24061; Affiliate Faculty, Dept. of Materials Science and mass (Rodgers 2021) since it can be leached into the living envi-
Engineering, Virginia Polytechnic Institute and State Univ., Blacksburg, ronment during landfilling (Buck et al. 2021; Councell et al. 2004;
VA 24061 (corresponding author). ORCID: https://orcid.org/0000-0001 Liu et al. 2018; Rhodes et al. 2012; Smolders and Degryse 2002). A
-6699-2020. Email: [email protected]
Note. This manuscript was submitted on September 15, 2023; approved
study by Smolders and Degryse (2002) found that during a one-
on June 11, 2024; published online on August 27, 2024. Discussion period year weathering period, 10% to 40% of the zinc in 100 μm ELT
open until January 27, 2025; separate discussions must be submitted for particles was leached. If the average amount of zinc in tire rubber is
individual papers. This paper is part of the Journal of Geotechnical 1.5% wt., then an estimated 287,000 tons of zinc could be leached
and Geoenvironmental Engineering, © ASCE, ISSN 1090-0241. into the environment based on the current yearly production of

© ASCE 04024107-1 J. Geotech. Geoenviron. Eng.

J. Geotech. Geoenviron. Eng., 2024, 150(11): 04024107

 ELTs in the US and China alone. Zinc not only damages the stom-
ach lining in living organisms but also exhibits toxicity toward a
wide range of organisms, including plants, invertebrates, and fish
(Li et al. 2023; Tran et al. 2022b). This can result in severe harm to
ecosystems and have long-lasting effects on the environment
(Liu et al. 2018). Various studies also reported the effects of zinc
toxicity on human health, such as in the form of prostate cancer
(Coradduzza et al. 2024; Karunasinghe 2022), respiratory disease
(Gu and Ruei-Lung Lin 2010), and immune systems (Stiles et al.
2024).
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Ground ELT rubber is used in civil engineering applications,

including portland cement concrete (Kara De Maeijer et al. 2021;
Lavagna et al. 2020; Shu and Huang 2014; Tran et al. 2022b),
asphalt concrete (Ma et al. 2022; Picado-Santos et al. 2020;
Shu and Huang 2014; Song et al. 2018; Wang et al. 2018),
cement-stabilized base materials (Liu et al. 2023), and soil stabi-
lization (Al-Bared et al. 2018). However, the potential for zinc to
Fig. 1. Particle size distribution curves of PC, kaolin, bentonite, and
be leached from the ELT rubber in these applications has been ELT rubber particles.
little researched. Some researchers found that higher concentra-
tions of zinc are leached from rubber-modified asphalt concrete
(Sampson et al. 2014; Vashisth et al. 1998), although using
ELT rubber in asphalt concrete reduces the rate of zinc leached
(Liu et al. 2018). Zinc was found to leach into soil stabilized significant improvement in strength. Beyond the engineering proper-
by ground ELT rubber (Smolders and Degryse 2002), although ties, the stabilized soil is expected to absorb the zinc leached from
some researchers proposed this methodology to improve the soil the ELT rubber through the CEC of the clay. This study is novel
quality in zinc-deficient soils (Taheri et al. 2011). Cement hydra- because it considers the fate of the zinc in conjunction with the
tion appears to immobilize any zinc remaining after using tire- engineering properties of RSS, which was not considered previ-
derived fuel in a cement kiln during the clinkering process ously in the literature.
(Trezza and Scian 2009).
When considering the fate of zinc leached from ELT rubber, no
studies evaluated the ability of a clayey soil to capture the leached Experimental Program
zinc in a rubberized stabilized soil (RSS) even though it is widely
known that clay can itself mitigate the leaching of heavy metals Materials
from industrial by-products (Bedford 2014; Deng et al. 2022;
Huang et al. 2022; Qi et al. 2023; Yang et al. 2017). A few studies In this study, two typical clays were used—kaolin and bentonite—
showed that ELT rubber can be used to engineer soil properties with specific gravities of 2.63 and 2.62, respectively. The specific
(Al-Bared et al. 2018; Yoon et al. 2006) and that portland cement gravity of PC was 3.15. Kaolin and bentonite have liquid limit (LL)
(PC) stabilization can be further used to modify soil properties values of 57% and 513%, respectively. The kaolin and bentonite
(Saberian and Rahgozar 2016; Yadav and Tiwari 2017). Clay soils CEC values were determined following ASTM C837 (Kennedy
are of particular interest in this capacity, given that certain clays can 1965) and were 15.75 meq=100 g and 71.75 meq=100 g, respec-
capture heavy metals through cation exchange (Ahmed et al. 2021; tively. The median particle sizes (D50 ) for kaolin, bentonite, and
Esmaeili et al. 2019; Farrah et al. 1980; Lothenbach et al. 1998). Type I/II PC were 3.8 μm, 1.4 μm, and 6.7 μm, respectively, and
Heavy metal cations, such as Zn2þ , are captured by negatively the particle size distributions are shown in Fig. 1.
charged clay in the soil via electrostatic forces through which neg- The ELT rubber was received from the manufacturer at a re-
ative soil particles attract the positive cations (Matthews 2014). duced particle size and was reported to consist of natural rubber,
This cation exchange capacity (CEC) strongly depends on clay butadiene rubber, and styrene-butadiene rubber. In this study, the
content, particle size, and type of clay in the soil, organic matter ELT rubber particles were used in the “as-received” form, herewith
content, salinity, and soil pH (Bellir et al. 2013; Kennedy 1965; referred to as untreated ELT rubber, and in the processed form from
Vangronsveld et al. 1995; Zhang et al. 2011). which the zinc was extracted, herewith referred to as treated ELT
This study proposes an approach to stabilize soft clayey soil us- rubber. The hydrometallurgical treatment process was based on a
ing ELT rubber and PC. ELT rubber and PC also act to immobilize previous methodology (Li et al. 2023), where 1.0 M HCl was used
any leached zinc from the ELT rubber. Specifically, ELT rubber to leach and subsequently recover the zinc from the ELT rubber.
before and after treatment is compared. The treatment follows a The treatment batch had a solid concentration of 200 g L−1 . The
hydrometallurgical process to preleach the zinc from the rubber treatment process was carried out at a leaching temperature of 90°C
to recover it as zinc oxide for other industries (Li et al. 2023; and was agitated for 5 h using a Polytetrafluorethylene (PTFE)-
Tran et al. 2024). This treatment process was developed in an effort coated magnetic stirrer at 600 rpm, resulting in a leaching recovery
to control the environmental impact of leached zinc from ELT rub- of zinc of approximately 95%. The specific gravity of untreated and
ber. The main purposes of this study are to evaluate whether clays treated ELT rubber was 1.20 and 1.18, respectively. The particle
can immobilize (1) zinc leached from untreated ELT rubber; and size distribution of the ELT rubber is shown in Fig. 1; the D50 for
(2) any remaining leachable zinc from the treated ELT rubber. untreated and treated ELT rubber was 0.34 mm and 0.45 mm,
Furthermore, PC is used to chemically stabilize the soil in addition respectively. The ELT rubber particles expanded slightly after
to the ELT rubber. Specifically, along with chemical reactions treatment.
between the PC and clay, the addition of ELT rubber is believed A Bruker D8 X-ray diffractometer (Bruker, Billerica, Massachu-
to mechanically change the stabilized soil structure, resulting in a setts) with Cu Kα radiation was employed for mineralogical

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J. Geotech. Geoenviron. Eng., 2024, 150(11): 04024107

 Table 1. Chemical composition of kaolin, bentonite, and PC the pH and zinc concentration of the leaching solution were
Chemical composition (%) Kaolin Bentonite PC determined using a pH meter and inductively coupled plasma mass
spectrometry (ICP-MS), respectively. The soaking proportion of
CaO 0.3 1.1 56.7
clay-rubber mixtures with different chemical solutions is presented
SiO2 43.0 50.2 30.1
Al2 O3 20.3 12.9 8.4 in Table 2.
MgO 0.6 1.6 2.1
Fe2 O3 1.3 3.8 2.9
TiO2 1.3 0.1 0.2 Engineering Property Tests
K2 O 0.3 0.3 0.5 Untreated and treated ELT rubber was mixed with clay and PC. For
Na2 O — 1.3 —
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the kaolin clay experiments, the ELT rubber content was 0%, 10%,
P2 O 5 — 0.1 —
30%, and 50% by clay volume. For the bentonite clay experiments,
Loss of ignition (LOI) 33.0 28.4 0.0
the ELT rubber content was 0% and 50% by clay volume. RSS with
kaolin used a water content of 2.0 LL of kaolin, whereas RSS with
bentonite used a water content of 0.5 LL of bentonite. PC was
added at 20% by solid mass. After mixing, the flowability of each
analysis of the clays. The kaolin clay was found to consist of only fresh RSS mixture was immediately determined according to ASTM
kaolinite, whereas the bentonite clay was composed of montmoril- D6103 (ASTM 2017) to evaluate the flowability improvement in
lonite and quartz (Tran et al. 2022a). ELT rubber in stabilized soil for the purpose of controlled low-
The major metals in the untreated ELT rubber were Mg, Al, Ca, strength material (CLSM) use or soil stabilization using a deep-
Fe, and Zn, as determined after digestion of the rubber in strong mixing method. Cylindrical specimens with lengths of 100 mm
acid, at concentrations of 567 mg kg−1 , 219 mg kg−1 , 627 mg kg−1 , and diameters of 50 mm were prepared via the dynamic compaction
131 mg kg−1 , and 10,389 mg kg−1 , respectively (Li et al. 2023). method (Kitazume et al. 2015) and cured in a curing chamber con-
The chemical composition of the kaolin, bentonite, and PC was ditioned at 23°C  2°C and 95%  2% of relative humidity until
determined by X-ray fluorescence analysis and presented in the testing time. The unconfined compressive strength (UCS)
Table 1. after 3 days, 7 days, and 28 days were determined in accordance
with ASTM D2166 (ASTM 2000). The mixture proportions and
Zinc Capture Test performed experiments for different mixtures are presented in
To test the hypothesis that clay can absorb leached zinc, a soaking Table 3.
test was employed in this study. The test was performed by soaking
clay and ELT rubber with a liquid-to-ELT solid ratio of 40 Isothermal Calorimetry
(L=S ¼ 40) at 23°C. For the control sample, 5 g of ELT rubber
powder was soaked in 200 g of deionized water in a closed Isothermal calorimetry (IC) was conducted using a Calmetrix I-Cal
250 mL glass bottle. Five grams of kaolin or bentonite were added Flex (Calmetrix, Boston) to observe the thermal power (W=g ce-
into other mixtures for the clay treatment. Different aqueous solu- ment) and total heat (J=g cement) of various RSS mixtures.
tions, including deionized water, 0.05 M NaOH, 0.18 M CaðOHÞ2 , Although IC is commonly used to understand cement hydration
and 0.45 M CaðOHÞ2 , were employed for this test to simulate dif- kinetics (Behravan et al. 2023; Liao et al. 2024; Torfin et al.
ferent leaching conditions when the clay mixture interacts with 2023; Wadsö et al. 2016), it was recently applied to study reactions
hydrating PC or exposed to different environmental conditions. in stabilized soils (Tran et al. 2022a). After the RSS mixtures were
In addition, the CEC of clay is affected by pH value; increasing thoroughly mixed in 15 mL plastic vials, the vials were transferred
pH in the soil increases CEC. Hence, the purpose of using alkaline to the isothermal chamber, which was set to 23°C. The heat of hy-
solutions in the leaching test is to observe whether increasing the dration was quantified for up to 3 days of curing time. To inves-
pH in the leaching solution can aid the immobilization of any re- tigate the heat development in the RSS matrix and how it was
maining leached zinc. After 1 day, 7 days, and 28 days of soaking, different from the one without ELT rubber added, mixtures coded

Table 2. Soaking proportion of clay-rubber mixtures

Solid (g) Liquid/chemical solution Measured pH
Kaolin Bentonite Untreated ELT Water 0.18 M or 0.05 M NaOH
Mix code (g) (g) rubber (g) (g) 0.45 M CaðOHÞ2 (mL) (mL) 1d 7d 28 d
1R_40W — — 5.0 200 — — 9.4 7.2 7.2
1K_40W 5.0 — — 200 — — 8.9 8.2 8.0
1B_40W — 5.0 — 200 — — 10.2 9.9 9.9
1K_1R_40W 5.0 — 5.0 200 — — 8.6 8.0 8.0
1K_1R_40W_0.2CaO 5.0 — 5.0 — 200 — 13.0 12.6 12.4
1K_1R_40W_0.5CaO 5.0 — 5.0 — 200 — 13.0 12.6 12.6
1K_1R_40W_NaOH 5.0 — 5.0 — — 200 13.0 12.5 12.5
1B_1R_40W — 5.0 5.0 200 — — 10.2 9.6 9.3
1B_1R_40W_0.2CaO — 5.0 5.0 — 200 — 13.0 12.6 12.3
1B_1R_40W_0.5CaO — 5.0 5.0 — 200 — 13.0 12.6 12.5
1B_1R_40W_NaOH — 5.0 5.0 — — 200 12.9 12.4 12.2
Note: R: ELT rubber; K: kaolin; B: bentonite; CaO: lime; W: water; and NaOH: sodium hydroxide. The number standing in front of each material name is its
ratio compared to the clay mass. For example, 1R_40W designates the mixture with 1 unit of ELT rubber soaked in 40 units of water.

© ASCE 04024107-3 J. Geotech. Geoenviron. Eng.

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 Table 3. Proportion of RSS and performed experiments
ELT rubber Performed experiments
content Cement ELT
(% clay C=S Clay (PC) rubber Water Leaching
Note Mix code volume) ratio (kg=m3 ) (kg=m3 ) (kg=m3 ) (kg=m3 ) UCS Flow IC SEM PSE test
Stabilized kaolin Ref-K 0 0.2 627.4 147.9 0 715.23 x x x x x x
Stabilized kaolin with URK-10 10 0.2 610.0 158.2 27.78 695.42 x x X — — —
untreated ELT rubber URK-30 30 0.2 578.0 177.1 78.95 658.9 x x x — — —
URK-50 50 0.2 549.2 194.2 125.0 626.1 x x x x x x
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Stabilized kaolin with TRK-10 10 0.2 610.0 158.0 27.36 695.5 x x x — — —

treated ELT rubber TRK-30 30 0.2 578.1 176.55 77.8 659.1 x x x — — —
TRK-50 50 0.2 549.4 193.3 123.2 626.3 x x x x x x
Stabilized bentonite Ref-B 0 0.2 331.1 78.34 0 849.2 x x — x — x
Stabilized bentonite with URB-50 50 0.2 307.8 109.3 70.4 789.6 x x x — x
untreated/treated ELT rubber TRB-50 50 0.2 307.9 108.7 69.29 789.75 x x — x — x
Untreated and treated ELT (U)ELT-C 50 — — 194.2 125.0 626.1 — — — — — x
rubber-cement mixture (T)ELT-C 50 — — 193.3 123.2 626.3 — — — — — x
without clay
Note: K = kaolin; B = bentonite; C=S = cement-to-solid ratio in volume; PC = cement UCS = unconfined compressive strength; IC = isothermal calorimetry;
PSE = pore solution extraction; and SEM = scanning electron microscopy.

Control-K, URK-10, URK-30, URK-50, TRK-10, TRK-30, and Results and Discussion
TRK-50 were subjected to the IC test.
Zinc Capture Test
Microstructure Study Fig. 2 depicts the zinc concentration of various leachates at differ-
Scanning electron microscopy (SEM) was employed to study the ent soaking times. As shown, the leachates of mixtures of kaolin
microstructure of the ELT rubber particles. A JEOL IT-500HR with water (1K_40) and bentonite with water (1K_40) did not ex-
SEM (JEOL, Tokyo) with a Schottky field emission electron source pose any significant zinc concentration after 28 days of the soaking
was used. Samples were sputter-coated with a ∼12-nm thick process. Meanwhile, the zinc that leached out from the ELT rubber
platinum/palladium layer. For these analyses, samples were into the deionized water (mixture 1R_40W) was dramatically high
vacuum-dried to remove moisture prior to the tests following since its concentration increased more than 270 times from 27.1 ppb
the method in a study by Kim et al. (2019). (1 day) to 7387 ppb (28 days). This clearly indicates that ELT rub-
ber possesses a potential for zinc to leach into the surrounding envi-
ronment. When kaolin or bentonite was introduced to the mixtures,
Pore Solution Extraction (PSE) and Environmental
Leaching Tests
PSE was used to understand the chemical composition in the pore
solution of mixture Ref-K, URK-50, and TRK-50. The PSE de-
vice in this study was based on the Barneyback and Diamond sys-
tem (Barneyback and Diamond 1981). The applied pressure to
extract the pore solution at curing ages of 7 and 28 days from
the cylindrical samples (50 mm in diameter and 100 mm in length)
was increased from 0 MPa to 22.5 MPa until 5 mL to 10 mL of
pore fluid was collected. The collected pore solution was then fil-
tered and immediately acidified with 12.1 M HCl at 2% by vol-
ume of solution to prevent precipitation. Finally, the extracted
solution was analyzed using a Thermo Electron iCAP-RQ ICP-
MS (Thermo Electron, Waltham, Massachusetts) and a Shimadzu
TOC-VCSN (Shimadzu, Kyoto, Japan) to quantify the zinc and
TOC concentrations, respectively, during the hydration process of
the RSS. These two analyses were also employed for the leachate
of the crushed UCS samples soaked in deionized water at L=S ratio
of 8 (at 7 days, 28 days, and 150 days) to check whether the proposed
material satisfies the environmental requirements. Of each sample,
200 mL was soaked in 1,600 mL deionized water in a 2-L bucket
with a sealed lid. Along with the three aforementioned mixture, two
more mixtures were prepared by eliminating the clay content in mix-
Fig. 2. Zinc concentration of various leachates at different soaking
tures URK-50 and TRK-50 for the leaching test to investigate the
times.
effects of clay in zinc and TOC immobilization in the leachate.

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 the 28-day zinc concentration of all the leachates significantly de-
creased by 95% (i.e., from 7,387 ppb to less than 300 ppb). Increas-
ing the pH with 0.18 M CaðOHÞ2 , 0.45 M CaðOHÞ2 , and 1 M
NaOH accelerated the zinc leaching rate at the early soaking times
(1 day) relative to water. The increased pH appeared to be effective
with bentonite to increase its cation absorbability; hence, it could
absorb more free zinc from leachate (i.e., zinc concentration de-
creased from 7,387 ppb to approximately 30 ppb). Meanwhile,
the increased pH did not have a remarkable effect on the zinc
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absorbability of kaolin because it could not absorb more free

zinc from leachate compared to the mixture soaked in distilled
water (1K_1R_40W). This might be explained that because the
CEC of kaolin is much smaller (approximately 5 times) than that
of bentonite, it might reach its maximum capacity to absorb
Fig. 4. Unconfined compressive strength of rubberized stabilized
more ions.
clays.
Another explanation for the reduction in zinc concentration in
Fig. 2 is that it precipitated out of solution. Above pH ∼ 10, Zn2þ
can precipitate out of solution as ZnO and/or ZnðOHÞ2 (Aimable
et al. 2010; Sinha et al. 2016). Similarly, Lothenbach et al. (1998)
found that zinc concentration in a clay-free system dropped dra- regardless of ELT rubber addition. It is worth noting that the clay
matically when pH was greater than 9. However, no white precip- was also able to immobilize any leached iron, and the pH modi-
itates were observed in these solutions, which would have been fication significantly enhanced the iron immobilization, which
indicative of ZnO and/or ZnðOHÞ2. It is possible that part of Zn2þ satisfied the requirement for iron content in drinking water
could be converted into hydroxides in alkaline conditions and pre- (<300 ppb) (ATSDR 2005). Other heavy metals, including lead,
cipitate on the surface of the clay (Zhang et al. 2011). In addition, chromium, cobalt, cadmium, and arsenic, were detected in
clay has multiple micropores such that zinc might diffuse and be extremely low (e.g., less than 30 ppb) to zero concentrations in
captured into the pore spaces of the clay structure. All three of these the leachates detected by ICP-MS.
hypotheses can occur simultaneously during this experiment. Since
all clay-rubber mixtures significantly reduced the zinc concentra- Unconfined Compressive Strength (UCS)
tion, the immobilization of zinc is most likely attributed to the CEC
of clays. Fig. 4 shows the UCS of conventional cement-stabilized soil
In addition to zinc, the only other heavy metal identified in (i.e., Ref-K and Ref-B), RSS with untreated ELT rubber
the leachate in appreciable quantity was iron, as presented in (i.e., URK-10, URK-13, and URK-50), and RSS with treated
the section “Experimental Program.” As shown in Fig. 3, mixtures ELT rubber (i.e., TRK-10, TRK-13, and TRK-50). The conventional
1B_40W (mixture of bentonite and water) and 1B_1R_40W (mix- mixtures exhibited low UCS values, as well as slow strength devel-
ture of bentonite, rubber, and water) appeared to have high iron opment during the curing time. However, when different amounts of
untreated ELT rubber were introduced, the strength of stabilized
concentration, which seemed to come from the nature of bentonite
clays remarkably improved. In general, a higher replacement per-
centage of treated ELT rubber yielded a greater strength. The 28-day
strength of rubberized stabilized kaolin with 50% untreated ELT
rubber (URK-50) was 1019 kPa, which roughly doubled the con-
ventional stabilized kaolin without any rubber added (523 kPa).
This improvement was nearly three times in the case of rubberized
stabilized bentonite (558 kPa compared to 179 kPa). However, the
treated ELT rubber was not as effective as the untreated ELT rub-
ber. The 28-day strength of RSS with 50% treated ELT rubber
(TRK-50) was decreased by 65% (from 1,019 kPa to 654 kPa)
compared to the untreated ELT rubber used case, which was just
25% higher than that of conventional stabilized kaolin. This hap-
pened similarly in the case of rubberized stabilized bentonite
(388 kPa versus 558 kPa).

Flowability
The flowability of different RSS mixtures is presented in Fig. 5.
Generally, untreated and treated ELT rubber enhanced the flowabil-
ity of rubberized stabilized kaolin up to 35%, increasing from
approximately 8 cm (Ref-K) to 11 cm (mixtures URK-10 and
TRK 30). The hydrophobic nature of the ELT rubber (e.g., Chen
et al. 2021; Di Mundo et al. 2018) could be one reason for the in-
creased flowability, as the rubber particles act to repel water. In
addition, since the cohesion of clay is high, the clay particles tend
Fig. 3. Total iron concentration of various leachates at different soak-
to agglomerate in the presence of water. The ELT rubber particles
ing times.
disrupt that cohesion and act to disperse the clay particles.

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 Meanwhile, the ELT rubber only slightly improved the flowability flowability of RSS when ELT rubber is added can be helpful in
of the stabilized bentonite, which is understandable since the se- the application of controlled low-strength materials.
lected water content of the rubberized stabilized bentonite mixture
was only 50% of its liquid limit value. The improvement in the
Isothermal Calorimetry (IC)
The thermal power generated from different RSS mixtures is
graphically presented in Fig. 6. During the hydration process, RSS
mixtures generally generated much higher thermal power (from 1.2
to 1.35 times) than that of the reference mixture (approximately
0.011 W=gcement ). This could be explained as follows: due to the
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hydrophobicity of the used ELT rubber, there is more “free” water

available in RSS skeleton, which provides more sufficient water for
the mineral diffusion for the hydration process of the mixtures.
Second, the leached zinc in the RSS matrix probably could homo-
geneously incorporate into the C–S–H to increase its growth rate
and provide a higher peak of hydration. This observation is in
good agreement with a previous study by Bazzoni et al. (2014),
who found changes in the nature of C–S–H as its layers became
thicker and its needle became clearly longer, and these changes
Fig. 5. Flowability of different RSS. were associated with the increase in degree of hydration and
increased heat of hydration. In addition, the mechanical and
physical engineering properties of ELT rubber are believed to
be more efficient than clay in helping strengthen the mixtures’
development.
Second, the data show that the peak of the thermal power curves
of the rubberized stabilized kaolin was mostly maintained with just
a few minute shifts. In addition, possible retardations in the hydra-
tion due to the contamination of the hydration media in the mix-
ture’s matrix via zinc, reported in some previous studies by Garg
and White (2017) and Ataie et al. (2015), were not yet found in this
case. The peak differences (hour), peak value (W=gcement ), and ac-
cumulated heat (J=gcement ) of various RSS are shown in Table 4.
Along with thermal power, Fig. 6 simultaneously reports the
total heat recorded from mixing to 24 h, and the detailed total heat
of each mixture over time up to 72 h of curing is shown in Table 5.
The data reveal that using ELT rubber in stabilized kaolin mixtures
Fig. 6. The thermal power generated from different RSS.
remarkably increased the total hydration heat. After 72 h, the in-
creases were up to 20% for 10% of untreated ELT rubber used and
up to 19% for both 10% and 30% of treated ELT rubber used.
Interestingly, the increases were less significant when using more
Table 4. Hydration thermal power of different RSSs
ELT rubber (up to 50%) in the mixtures. This tendency is not com-
Peak Peak Peak Peak value pletely in agreement with the UCS development shown in Fig. 3.
Mix code (h) delay (h) (W=gcement ) difference (%) Although other studies demonstrated that IC data can directly relate
Ref-K 10.8 N/A 1.12 × 10−2 N/A to strength development in cementitious composites (e.g., Tanesi
URK-10 10.9 0.1 1.41 × 10−2 25.9 and Ardani 2013), this study does appear to demonstrate similar
URK-30 10.7 −0.1 1.38 × 10−2 23.2 trends for RSS. However, the data indicate that the change in ther-
URK-50 10.7 −0.1 1.51 × 10−2 34.8 mal power peak and total heat during the hydration could be used to
TRK-10 10.8 0.0 1.35 × 10−2 20.5 predict the strength changing tendency of the stabilized soil mix-
TRK-30 10.7 −0.1 1.47 × 10−2 31.3
tures but cannot completely reflect the strength development
TRK-50 10.8 0.0 1.41 × 10−2 25.9
behavior of the mixtures.

Table 5. Hydration total heat generated from different RSSs

Total heat (J=gcement ) (percent difference between modified mixtures and PC)
Mix code 12 h 24 h 48 h 72 h
Ref-K 3.09 × 102 4.54 × 102 5.87 × 102 6.13 × 102
URK-10 3.81 × 102 (23.3) 5.58 × 102 (22.9) 7.03 × 102 (19.8) 7.38 × 102 (20.4)
URK-30 3.50 × 102 (13.3) 5.09 × 102 (12.1) 6.46 × 102 (10.1) 6.83 × 102 (11.4)
URK-50 3.65 × 102 (18.1) 5.37 × 102 (18.3) 6.81 × 102 (16.0) 7.25 × 102 (18.3)
TRK-10 3.76 × 102 (21.7) 5.45 × 102 (20.0) 6.92 × 102 (17.9) 7.30 × 102 (19.1)
TRK-30 3.82 × 102 (23.6) 5.52 × 102 (21.6) 6.93 × 102 (17.9) 7.30 × 102 (19.1)
TRK-50 3.50 × 102 (13.3) 5.18 × 102 (14.1) 6.59 × 102 (12.3) 7.01 × 102 (14.4)

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Fig. 7. SEM images of the (a and c) untreated ELT rubber particles; and (b and d) treated ELT rubber particles.

Microstructure with the findings from the zinc capture test in Fig. 2. In addition, the
results show that the zinc-recovery treatment could not completely
Secondary electron imaging with SEM was performed on the
ELT rubber particles. Figs. 7(a and c) show that the untreated remove all zinc in the ELT rubber particle, which agrees with the
ELT rubber particles possessed irregular and angular shapes with findings in a previous study (Li et al. 2023).
no visible microcracks. In contrast, significant cracks were ob-
served on the treated ELT rubber surface as a result of the treat-
ment process, as shown in Figs. 7(b and d). This change to the
particle morphology after treatment was reported previously and
is the reason for the increased specific surface area of the ELT
rubber (Li et al. 2023). In addition, the treated ELT rubber par-
ticle appeared to have many small scales on its surface due to the
formed cracks that are close to the particle edges, as is seen in
Fig. 7(d). These cracks and scales weaken the ELT rubber particle
and are likely the reason for the reduced mechanical performance
of the treated ELT rubber compared to the untreated ELT rubber
in Fig. 4.

Environmental Leaching Tests

Fig. 8 presents zinc concentration in the extracted pore solution of
RSS mixtures Ref-K, URK-50, and TRK-50. At early curing times
(7 days), the zinc concentration in the pore solution of all mixtures
was relatively high. However, there is an apparent immobilization
Fig. 8. Zinc concentration in the extracted pore solution of kaolin with
of the zinc at 28 days relative to 7 days, which is attributed to the
ELT rubber.
CEC of the clay in the RSS matrix. The result is in good agreement

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Fig. 11. TOC in the leachate of RSS mixtures.

Fig. 9. Zinc concentration in the leachate of RSS mixtures.

Fig. 10 illustrates the TOC content in the extracted pore solution
of RSS mixtures including Ref-K, URK-50, and TRK-50. Notably,
the amount of leached TOC in the pore solution was relatively high
Fig. 9 compares the zinc concentration in the leachate of RSS after 7 days of curing time and was significantly reduced after
mixtures and the ELT rubber-cement mixtures without kaolin [(U) 28 days (i.e., decreased to the level yielded by the reference
ELT-C and (T)ELT-C]. At 7 days of soaking, the mixtures (U)ELT-C mixture).
and (T)ELT-C exposed approximately 25 ppb to 40 ppb of zinc in Fig. 11 shows the TOC content in the leachate of the RSS mix-
the leachate, which were generally much higher than the RSS mix- tures, including Ref-K, URK-50, TRK-50, URB-50, and TRB-50.
tures (i.e., URK-50, TRK-50, URB-50, and TRB-50) that yielded The TOC content in the leachate of the RSS mixtures increased
negligible zinc concentrations. After 150 days, all leached zinc was over time. After 150 days of soaking, mixtures with kaolin could
evidently immobilized by clay in RSS mixtures, whereas small immobilize approximately 50% of the leached TOC when com-
amounts of zinc were still left in the leachate of the ELT rubber- pared to the amount of leached TOC from rubber-cement mixtures,
cement mixtures without clays, except for the case of mix TRK-50, keeping the TOC concentration in the leachate of rubberized sta-
which remained unexplainable. The CEC of hydration products bilized kaolin marginally under the zinc threshold for drinking
from cementitious materials, such as C–S–H, was reported to pos- water (25 mg=L) [Standard Methods For the Examination of Water
sess the ability to capture heavy metals (Bernard et al. 2021), which and Wastewater (APHA 2018)]. More noticeably, approximately
is also observed in this study through the zinc concentration reduc- 75% of leached TOC was immobilized for RSS mixtures with
tion in the leachate of rubber-cement mixtures, (U)ELT-C and (T) bentonite. These findings indicate that clays not only can absorb
ELT-C, between 7 and 28 days. Even though the zinc concentration zinc but also can immobilize the TOC leached from ELT rubber
recorded in the leachate of all mixtures satisfied the requirement particles.
for zinc content in drinking water (<5 ppm) (ATSDR 2005), it is
worth noting that the zinc immobilization of the RSS was enhanced
more effectively due to the presence of clay. Conclusions

In this study, the feasibility of using ELT rubber for soil stabiliza-
tion was investigated in terms of engineering and environmental
aspects. The effects of zinc-recovered treatment on ELT rubber
were also discussed. The main conclusions taken from this study
are as follows:
1. The results successfully proved the hypothesis that clays pos-
sess a strong ability for zinc immobilization.
2. Although the treatment process for zinc recovery from ELT rub-
ber could provide a more environmentally conscious material,
it adversely affected the engineering properties of the RSS.
3. ELT rubber enhanced the flowability of RSS mixtures, possibly
due to its hydrophobicity.
4. Although adding untreated ELT rubber into stabilized clay could
significantly enhance the strength of the mixture by up to ap-
proximately 95% (for kaolin mixture) and 300% (for bentonite
mixture), the zinc-recovery treatment process on ELT rubber
negatively affected the significance of the improvement in the
strength of the RSS mixtures.
5. The peak heat of hydration was exaggerated up to 1.35 times
Fig. 10. TOC in the pore solution of rubberized stabilized kaolin.
from the addition of ELT rubber in the stabilized clay mixture.

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J. Geotech. Geoenviron. Eng., 2024, 150(11): 04024107

 The change in the thermal power peak and total heat during hy- ASTM. 2000. Standard test method for unconfined compressive strength of
dration could be used to predict the strength changing tendency cohesive soil 1. ASTM C2166. West Conshohocken, PA: ASTM.
of the stabilized soil mixtures but cannot completely reflect the ASTM. 2017. Standard test method for flow consistency of controlled low
strength development behavior of the mixtures. strength material (CLSM). ASTM D 6103. West Conshohocken, PA:
ASTM.
6. Kaolin and bentonite could effectively immobilize the leached
Ataie, F. F., M. C. G. Juenger, S. C. Taylor-Lange, and K. A. Riding. 2015.
zinc and TOC contents in the RSS.
“Comparison of the retarding mechanisms of zinc oxide and sucrose on
7. Given an improvement in flowability and sufficient strength, the cement hydration and interactions with supplementary cementitious
RSS shows its feasibility for use as controlled low-strength materials.” Cem. Concr. Res. 72 (Jun): 128–136. https://doi.org/10.1016
material (CLSM) or for use in soil stabilization with regular /j.cemconres.2015.02.023.
mixing methods or through deep-mixing methods, which would
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ATSDR (Agency for Toxic Substances and Disease Registry). 2005.

significantly enhance the use of ELT rubber in civil engineering, Toxicological profile for zinc, public health statement. Washington,
especially geomaterials. DC: US Department of Health and Human Services.
8. This study provided a new possibility to use ELT rubber in geo- Bai, X., T. McPhearson, H. Cleugh, H. Nagendra, X. Tong, T. Zhu, and
materials in a sustainable way; however, durability (i.e., shrinkage Y.-G. Zhu. 2017. “Linking urbanization and the environment: Conceptual
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Data Availability Statement Bazzoni, A., M. Suhua, Q. Wang, X. Shen, M. Cantoni, and K. L.
Scrivener. 2014. “The effect of magnesium and zinc ions on the hydra-
All data, models, and code generated or used during the study tion kinetics of C3S.” J. Am. Ceram. Soc. 97 (11): 3684–3693. https://
appear in the published article. doi.org/10.1111/jace.13156.
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Acknowledgments
A. S. Brand. 2023. “Effect of pretreatment on reclaimed asphalt pave-
ment aggregates for minimizing the impact of leachate on cement
This study was supported by the Center for Tire Research
hydration.” Cem. Concr. Res. 173 (Nov): 107305. https://doi.org/10
(CenTiRe), Project SUST-2021-D14-4. The authors acknowledge .1016/j.cemconres.2023.107305.
Lehigh Technologies for providing the ELT rubber and Short Bellir, K., M. B. Lehocine, and A. H. Meniai. 2013. “Zinc removal from
Mountain Silica company for providing the kaolin and bentonite aqueous solutions by adsorption onto bentonite.” Desalin. Water Treat.
for this work. The authors thank Jeffrey Parks, Jody Smiley, 51 (25–27): 5035–5048. https://doi.org/10.1080/19443994.2013.808786.
Madeline E. Schreiber, and Aaron J. Prussin II for their assistance Bernard, E., Y. Yan, and B. Lothenbach. 2021. “Effective cation exchange
with ICP-MS and TOC analyses. This work used shared facilities at capacity of calcium silicate hydrates (C-S-H).” Cem. Concr. Res.
the Nanoscale Characterization and Fabrication Laboratory, which 143 (May): 106393. https://doi.org/10.1016/j.cemconres.2021.106393.
is funded and managed by Virginia Tech’s Institute for Critical Buck, T., A. Cooper Doherty, M. Ernst, M. Garland, M. Goings, K. Harris,
Technology and Applied Science. Additional support is provided and M. Safai-Amini. 2021. Rationale document for motor vehicle tires
by the Virginia Tech National Center for Earth and Environmental containing zinc. Sacramento, CA: California Dept. of Toxic Substances
Control.
Nanotechnology Infrastructure (NanoEarth), a member of the
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