Phosphorus, Sulfur, and Silicon and the Related Elements

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Synthesis and characterization of zeolite Linde

Type W and its metal oxide composite Ag-O-LTW
used for the decontamination of chemical warfare
agent simulant

Km Meenu, Neeraj Kumar, Kautily Rao Tiwari, Tara Yadav, Radha Tomar &
Arvind Kumar Gupta

To cite this article: Km Meenu, Neeraj Kumar, Kautily Rao Tiwari, Tara Yadav, Radha Tomar &
Arvind Kumar Gupta (2020): Synthesis and characterization of zeolite Linde Type W and its metal
oxide composite Ag-O-LTW used for the decontamination of chemical warfare agent simulant,
Phosphorus, Sulfur, and Silicon and the Related Elements, DOI: 10.1080/10426507.2020.1762193

To link to this article: https://doi.org/10.1080/10426507.2020.1762193

Published online: 13 May 2020.

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PHOSPHORUS, SULFUR, AND SILICON AND THE RELATED ELEMENTS
https://doi.org/10.1080/10426507.2020.1762193

Synthesis and characterization of zeolite Linde Type W and its metal oxide
composite Ag-O-LTW used for the decontamination of chemical warfare
agent simulant
Km Meenua , Neeraj Kumara, Kautily Rao Tiwaria, Tara Yadavb, Radha Tomara, and Arvind Kumar Guptab
a
School of Studies in Chemistry, Jiwaji University, Gwalior, MP, India; bDefence Research and Development Establishment (DRDE), Gwalior,
MP, India

ABSTRACT ARTICLE HISTORY

In this study, we have evaluated the performance of novel adsorbent zeolite Linde Type W and Received 13 January 2020
modified LTW with AgO metal oxide composite for the decontamination of chemical warfare Accepted 25 April 2020
agent simulant 2-chloroethylphenylsulphide (CEPS). Zeolites are nanoporous aluminosilicate miner-
KEYWORDS
als composed of silicon, aluminum and oxygen framework with cations and water molecules
Chemical warfare agent
within the pores. The synthesized zeolite LTW and its composites Ag-O-LTW was characterized by simulant; zeolite LTW;
XRD, FTIR, SEM-EDS and BET analytical techniques. The decontamination study of CWA simulant, decontamination
CEPS was monitored by using GC-FID technique. The nanocrystalline zeolite LTW and Ag-O-LTW
composites were found powerful adsorbents and showed great decontamination potential toward
CWA simulant CEPS. The Ag-O-LTW showed better results (
98 % decontamination in 7 hours)
than LTW zeolite.

GRAPHICAL ABSTRACT

Introduction
Zeolites are aluminosilicate minerals, which have inorganic
microporous frameworks that possess a large variety of well-
defined internal structures such as uniform cages, cavities,
or channels.[1] They have a small particle size (0.2-0.6 nm)
used to remove organic matter, trace metal ions and pollu-
tants from water due to their adsorption and ion exchange
capacity. Zeolite LTW with well-defined size and morph-
ology can be employed in various applications. Zeolites con-
sist of crystalline structure built from [AlO4]5– and
[Si(O4)]4– bonded together in such a way that all four oxy-
gen atom are located at the corner of each tetrahedral
unit.[2–8] They have good adsorption property for decontam-
ination of toxic metal and chemical warfare agents and their
stimulants. Zeolite LTW (MER Type) framework structure is
given below in Figure 1.
Decontamination of chemical warfare agents (CWA’s) is
much more important not only for battlefield applications
but also for cleanup as well. CWA simulants have similar
chemical structure and properties as CWA’s but are much
less toxic. Klabunde and his coworkers observed that nano-
crystalline metal oxides are promising destructive adsorbent
for CWA’s and its simulants.[9–16] The decontamination of
chemical warfare agents and their simulants were studied
using nanoporous materials, such as zeolites, metal oxides of
zeolites and clay. A sorption study of trace metal ions from
wastewater on clintonite for the measurement of NaY and
AgY zeolite adsorption potential and a chemical study
against VX and its stimulants O,S-diethyl phenyl phospho-
nothiolate (DEPPT) were reported.[17a,b] Chemical warfare
agents are commonly known as blister agents or vesicant
and nerve agents. The blister agents such as sulfur mustard
gas (HD, HT), lewisite (L), nitrogen mustard gas (NH-1,
NH-2, NH-3) are strongly responsible for blistering action
which damage eyes, respiratory tract and mucous mem-
brane.[18] Nerve agents such as Tabun (GA), Sarin (GB),
Soman (GD) and VX disrupt neurological function within
biological system through inhibition of organophosphorus
cholinesterase.[19,20] Sulfur mustard, bis(chloroethyl) sulfide,
is one of the most known chemical warfare blister agent
with the molecular formula of (ClCH2CH2)2S, commonly

CONTACT Km Meenu singhmeenu458@gmail.com School of Studies in Chemistry, Jiwaji University, Gwalior, MP, India.
ß 2020 Taylor & Francis Group, LLC
2 K. MEENU ET AL.
Figure 1. Structure of zeolite-LTW (MER Type) framework.
abbreviated as HD, H for munition grade and D for dis-
tilled. Less-toxic analogs (simulants) of HD are 2-chloroethyl
ethyl sulfide (CEES) and chloroethyl phenyl sulfide (CEPS),
with similar physicochemical properties. The decontamin-
ation of the above mentioned toxic agents and their simu-
lants is a main challenge for chemists. If exposed to these
compounds commonly brings blister to the skin and mucous
membrane, so they are called blister agents and vesicants.[21]
One of the most important fields for multiple defense appli-
cations are nuclear, biological, chemical (NBC) warfare,
destructive adsorption, and decomposition of acid gases and
polar organics, including CWAs and their mimics.[22–24] The
CWA simulants DMMP (less volatile) and CEES (highly
volatile) are the toxic compounds which have to be removed
from the environment.
In our investigation, we focused on the decontamination
of these chemical warfare agents simulants. In the present
study, zeolite-LTW and metal oxide composite of LTW were
synthesized by hydrothermal method and ion exchange with
metals such as Ag by impregnation method. These synthe-
sized nanocomposite materials show greater physical adsorp-
tion of CEPS in less time span. Hence, it was found that
zeolite material LTW and its composite are the best adsorb-
ent toward CEPS.
Experimental
Materials
Potassium hydroxide (KOH) Pellets (Fisher Scientific), alu-
mina basic (Al2O3, HIMEDIA), colloidal Silica (30 wt % sus-
pension in H2O, Aldrich), magnesium nitrate (MgNO3 
6 H2O, Chemical drug House (P) L.T.D. New Delhi), silver
nitrate pure (AgNO3) Merck-Mumbai, potassium perman-
ganate (KMnO4) Merck-Mumbai were used for pre-
sent study.
Synthesis of zeolite Linde Type W
The zeolite Linde Type W was synthesized by hydrothermal
method in a stainless autoclave in a two-step process. In the
first step, in 20 mL distilled water were added 12.4 g KOH
and 5.0 g basic alumina and heated to gentle boiling with
stirring until a clear solution was obtained. The solution was
cooled to room temperature and the loss of water during
heating was corrected by addition of water. In the second
step, to 24.2 g colloidal silica in 18.5 mL of water the reac-
tion mixture was added with stirring until a homogeneous
reaction mixture was obtained. The reaction mixture was
placed in a 300 mL stainless steel autoclave and kept at
150  C for 48 hours. The reaction mixture was filtered and
washed several times until pH 10 was reached and subse-
quently kept at 110  C overnight. The yield of the synthe-
sized zeolite Linde Type W was 12.7 g (84.7 %).
Modified zeolite Linde Type W with AgO metal
oxide composite
The synthesized zeolite Linde Type W (LTW) was modified
with silver oxide: to 1.5 g zeolite LTW in 10 mL of distilled
water were added 1.70 g of AgNO3 and the reaction mixture
was stirred for 5 hours at room temperature. KMnO4
(0.395 g) dissolved in 12.5 mL of distilled water was slowly
added and reaction mixture was further stirred for three
hours. The reaction mixture was filtered and the product
was dried at 100  C in vacuo. Subsequently it was calcinated
at 500  C for 4 hours.
Characterization
The synthesized zeolite Linde Type W was characterized by
XRD, FTIR, N2 BET surface area, SEM and EDX, and GC-
FID techniques.
XRD analysis
The powder X-ray diffraction pattern of zeolite-LTW and its
doped zeolite composite sample were recorded using
MiniFlex600 X-ray powder diffractometer over the 2h range
of 2-90 with a goniometer scanning speed of 10 2h/min
and a step size of 0.02 . The X-ray diffraction pattern of the
synthesized zeolite-LTW and its composite Ag-O-LTW are
shown in Figure 2. The XRD pattern reveals that zeolite-
LTW is crystalline in nature. The diffraction signal of the 2-
theta value observed at 25.80, 35.28, 43.50, 52.71, 57.59 and
68.34 clearly indicate the formation of zeolite-LTW. The
XRD pattern of zeolite-LTW with metal Ag is in semicrys-
talline state due to some point defects in the crystal-
line lattice.
FTIR analysis
The FT-IR spectra of zeolite-LTW and Ag-O-LTW nano-
composite were measured as KBr pellets with a Perkin
Elmer FTIR Spectrum 100 instrument and are shown in

Figure 2. XRD diffraction pattern of Linde Type W and Ag-O-LTW.
Figure 3. Combined FTIR spectra of zeolite Linde Type W and Ag-O-LTW.
–1
Figure 3. The absorption bands at around 579 to 804 cm
are characteristic and are attributed to SiO4 and Al-O-Al
motives. A wide absorption band of the OH group for the
silanol (Si-OH) is observed at 3440 cm–1. The absorption
band due to bending vibration of the H-OH group was
observed at around 1645 cm–1. This band was present in sin-
tered samples and is typical for the deformation H-OH
vibration of adsorbed H2O.[25] The bands observed at
around 1030 cm–1 and 702 cm–1 are due to asymmetric and
PHOSPHORUS, SULFUR, AND SILICON AND THE RELATED ELEMENTS 3
symmetric stretching of Si-O-Si and Al-O-Al structural
motives in the zeolite framework.[26,27]
Scanning electron microscopy
Surface morphology of zeolite-LTW and Ag-O-LTW was
investigated with a JEOL JSM 6010 LA, SEM-EDAX
(Scanning Electron Microscopy-Energy Dispersive X-ray
Spectroscopy) instrument. The zeolite-LTW particles appear
to be barbell shape with a particle size of 1 lm (LTW) and
of 5–10 lm (Ag-O-LTW). As can be seen in Figure 4 the
surface micrographs of Ag-O-LTW metal oxide composites
and LTW show different morphology indicating that the
morphology observed at the same magnification totally
changes after modification of synthesized LTW with metal
oxides. The SEM micrographs of zeolite LTW showed clear
barbell shape structure with a particle size in the micrometer
range.
Electron dispersion spectroscopy analyses
The EDS analyses were obtained for samples grid coated
with thin gold foil in order to avoid charge influence. Silver
(Ag), aluminum (Al), silicon (Si), oxygen (O) and potassium
(K) were confirmed as the only elementary components in
zeolite-LTW with silver oxide composite. No impurity or
unidentified peaks were observed in the EDS spectrum. It
reveals a pure material with the composition of LTW and
Ag-O-LTW composite. The weight percentage (%) and atom
percentage (%) are given with graph in tabular form in
Figure 5.
4 K. MEENU ET AL.

Figure 4. Combined SEM of zeolite Linde Type W and Ag-O-LTW.

Figure 5. Combined EDS analysis of zeolite LTW and Ag-O-LTW.

N2 adsorption/desorption BET surface area analyses pore volume of LTW and Ag-O-LTW is 0.03 cm3/g and
0.37 cm3/g, respectively (Figure 7). BET theory is used to
Surface area adsorption/desorption isotherm measurement
explain the physical gas/liquid adsorption of molecules on a
was performed with Autosorb 2020 by nitrogen adsorption
solid surface. In BET analysis a nitrogen uptake at very low
at liquid N2 temperature applying multipoint N2-BET
relative pressure (P/P0 ¼ 0.02) was observed indicating the
method. The synthesized zeolite LTW and the modified zeo-
filling of the micro-pores, followed by a desorbtion. The N2
lite LTW (Ag-O-LTW) were measured using N2 adsorption/
adsorption-desorption isotherm shows the adsorption cap-
desorption BET and show the isotherm in Figure 6. The
acity of the material (how much toxic chemicals it will

adsorb). The BET surface area of zeolite LTW and Ag-O-
LTW was found to be 15.75 m2/g and 118.38 m2/g, respect-
ively. The surface area of Ag-O-L is higher probably due to
larger particle size of Ag. The surface area of zeolite LTW is
lower than that of modified zeolite Ag-O-LTW metal oxide
composite. It clearly demonstrates that surface area has
increased after modification. Adsorption data for the relative
pressure (P/P0) range 0.004156 cm3/g to 0.03 cm3/g (LTW)
and 0.02 cm3/g to 0.37 cm3/g (Ag-O-LTW) were obtained
(Table 1).
Sample preparation for UV-Vis study
The samples were prepared as follows: in 20 mL Erlenmeyer
flask 5 lL CEPS were added to 5 mL hexane and the flask
Figure 6. Linear adsorption/desorption isotherm of zeolite-LTW and Ag-O-LTW.
Figure 7. Pore volume of zeolite LTW and Ag-O-LTW.
Table 1. BET surface area, single point adsorption, adsorption average and BJH desorption average pore width of synthesized zeolites-LTW and Ag-O-LTW.
Single point adsorption total
Sample name BET surface area, m2/g pore volume of pores, cm3/g
LTW 15.75 0.030299
Ag-O-LTW 118.38 0.375994
PHOSPHORUS, SULFUR, AND SILICON AND THE RELATED ELEMENTS 5
was sealed to prevent the vaporization of the solvent. Each
of the prepared samples was vortexed for 1 min and consid-
ered as a standard sample. Then 0.30 g of synthesized zeo-
lite-LTW or metal oxide composite (Ag-O-LTW) were
added to the above solution and the sample was shaken on
water shaker for 7 hours. The prepared solution was investi-
gated by UV-Vis spectroscopy.
Decontamination study using UV-Vis study
The decontamination study of 2-chloroethylphenylsulphide
(CEPS) simulant by zeolite LTW and metal oxide composite
of LTW was performed by UV-Vis analysis and the results are
shown in Figure 8. The UV-Vis band of CEPS standard was
observed at 252 nm due to the p-p transition of the aromatic
ring. In the observed UV-Vis spectrum of CEPS this absorb-
ance decreased due to the adsorption of the compound by the
zeolite or its metal oxide composite. The metal oxide Ag-O-
LTW performed a higher decontamination of CEPS as com-
pared to LTW zeolite. In this study, we observed, that Ag-O-
LTW is a good adsorbent for CEPS simulant.
GC-FID analyses
The decontamination studies were performed using Trace
GC Ultra (Thermoscientific) instrument. The GC analytical
conditions were as follows: the GC column temperature ini-
tially was kept at 60  C for 2 min and was increased at a rate
of 25  C min1 to 200  C final temperature, which was kept
about 10 min. The carrier gas N2 was used as flow medium
with a rate of 1 mL min1.
Figure 8. UV-Vis analysis of zeolite LTW and Ag-O-LTW against the decontam-
ination of CEPS in hexane.
Adsorption average pore BJH desorption average pore
width (4V/A): Å width (4V/A): Å
76.9125 57.281
127.0443 87.557
6 K. MEENU ET AL.
Figure 9. Combined GC-FID graph of CEPS with zeolite LTW in acetonitrile (a) CEPS standard (b) LTW CEPS (c) Ag-O-LTW CEPS.
Table 2. GC-FID results for sulfur mustard simulant CEPS with zeolite-LTW, and Ag-O-LTW.
Sample name Retention time of peak toluene CEPS Peak area of toluene
CEPS 3.95 122,640
Standard 7.55
LTW 3.93 135,071
CEPS 7.58
Ag-O-LTW 3.95 160,892
CEPS 7.70
Sample preparation for decontamination analysis
In this study decontamination reactions of CWA blister
agent (sulfur mustard) simulant CEPS were carried out on
the surface of zeolite-LTW and the metal oxide composite
Ag-O-LTW. The sample was prepared as follows: In a
20 mL Erlenmeyer flask were placed 5 mL of hexane and
10 lL solution of a 5:1 (v/v) ratio of CEPS : H2O in 10 lL of
toluene as the internal standard and the flask was sealed to
prevent the vaporization of the solvent. The samples were
vortexed for 1 min to give the standard samples.
Subsequently 0.30 g of synthesized zeolite-LTW or the metal
oxide composite of zeolite-LTW (Ag-O-LTW) was added to
the above solution. To complete adsorption, the prepared
solutions were shaken using a magnetic stirrer for 7 hours at
room temperature in N2 atmosphere. Finally, the upper
solution from the prepared samples was centrifuged for
2 min and 10 lL of each sample were injected to GC-FID by
using a microsyringe. Interaction was observed between syn-
thesized zeolite-LTW or the metal oxide composite of Ag-
O-LTW with blister agent sulfur mustard simulant CEPS.
Peak area of CEPS The ratio of CEPS/toluene (%) of decontamination
62,128 0.506 0
16,513 0.122 75.88
1126 0.006 98.81
GC-FID results
The decontamination studies were performed on blister agent
simulant 2-chloroethylphenylsulphide (CEPS) using zeolite-
LTW or the metal oxide composite of Ag-O-LTW. The decon-
tamination was measured by GC-FID analysis as a rapid and
suitable analytical technique. The GC chromatograms are shown
in Figure 9 for the CEPS simulant. It becomes evident from the
GC chromatogram, that CEPS has a retention time at about
7.5 min and the standard toluene a retention tome of 3.95 min.
For the calculation of the destructed amount of 2-chloroethyl-
phenylsulphide (CEPS) the integrated area under curve (AUC)
of CEPS and toluene as the internal standard from a reaction
during 7 hours were evaluated. The ratio of integrated data (inte-
grated AUC of CEPS and toluene) was higher for CEPS standard
(a) and after 7 hours (b) for zeolite-LTW CEPS and (c) for Ag-
O-LTW it decreases. When increasing the reaction time with
LTW and Ag-O-LTW, AUC of CEPS intensity in comparison to
standard CEPS decreases. High amounts of the simulant mol-
ecule were neutralized. The AUC data (a) for CEPS standard (b)
for LTW CEPS and (c) for Ag-O-LTW CEPS and the

decontamination percentage (%) are given in Table 2. The exact
amount of CEPS adsorbed was calibrated by the ratio of the area
under curve of the obtained adsorption peak and the peak
obtained for the standard sample of CEPS.
Conclusion
In this investigation zeolite-LTW was synthesized according
to International Zeolite Association (IZA) and successfully
modified with metal oxide composite of silver oxide. This was
confirmed by different characterization techniques such as
XRD, FTIR, SEM-EDS, and BET analyses. The decontamin-
ation studies were performed using UV-Vis and GC-FID
chromatography. The nanocrystalline zeolite LTW and Ag-O-
LTW showed great potential for decontamination of CWA
simulant of CEPS. The decontamination of CEPS was found
to be high for Ag-O-LTW during 7 hours of about 98 %. It
was found that adsorption increases with increasing of surface
area. The desorption analyses were also carried out success-
fully and desorption pattern also revealed the adsorption cap-
acity of CWA agent simulant. Ag-O-LTW shows a great
decontamination ability for CEPS because the modified zeolite
LTW has a larger surface area as compared to that of LTW.
Acknowledgement
The authors gratefully acknowledge the encouragement and support of
Professor of Head (P.I.) Prof. Radha Tomar, and Dr. D. K. Dubey,
Director, DRDE (DRDO), Gwalior, to pursue this research work and
also for their valuable suggestions. We also thank Dr. T. C. Shami, for-
mer Scientist ‘G’ DMSRDE (DRDO), and IIT Kanpur, for facilitating
the characterizations of synthesized samples.
ORCID
Km Meenu http://orcid.org/0000-0002-4383-7084
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