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Hydrothermal Preparation of Nanocrystalline TiO2 Powders

Under Various Concentrations of the Solvent


for Photocatalytic Reduction of Pentavalent and Trivalent
Astri Aldelina , Diana Rakhmawaty Eddy , Atiek Rostika Noviyanti
Arsenic
Department of Chemistry, Faculty of Mathematics
and Natural Sciences,Universitas Padjadjaran
1,2

1,3

astrialdelina22@gmail.com,

diana.rahmawati@unpad.ac.id

ABSTRACT
Arsenic is one of WHOs 10 chemicals of major public health concern. The greatest threat to public health from arsenic
originates from contaminated groundwater. Two forms are common in groundwater: arsenite (AsO 33) and arsenate
(AsO43), referred to as arsenic(III) and arsenic(V). One of the most well-known method of arsenic remediation is
adsorption. Titanium dioxide (TiO2) can be used as an absorbent to remove arsenic. Sorption capacity of different
polymorph TiO2 depends on sorption site density, surface area, particle size, surface energy, crystallinity and
crystalline structure, all these parameters depends on particle preparation technique. Many different preparation
methods have been described in order to obtain high-performance TiO2 nanoparticles, including hydrothermal
methods. This method is commonly used to grow large good-quality crystals and highly homogeneous nanoparticle.
Various parameters had been studied in order to get the better product like temperature, experimental duration,
pressure (percentage fill), pH, molar ratio of the starting materials, and solvent type. The preparation of TiO 2
nanocrystal will be carried out using various concentration of acid and base solvents using hydrothermal method.
Synthesized materials will be characterized and calculated using x-ray diffraction, SEM (Scanning Electron Microscope)
and Brunauer-Emmett-Teller (BET) surface area theory respectively, whilst sorption data will be interpreted in terms of
the Freundlich and Langmuir equations. This research is expected to obtain the optimal concentration of the solvents
to produce high purity TiO2 crystals for photocatalytic purpose.

METHODOLOGY

Keywords: hydrothermal method, nanocrystalline TiO2, photocatalyst TiO2, arsenic sorption


EXPERIMENTAL
TiCl4(aq) (3 mL)

INSTRUMENTS

Aqua bidest (25 mL)

Ice-water bath (2oC)


Ti(OH)4(s)

H2SO4 (25 mL)

HCl (25 mL)

NaOH (25 mL)

NaOH (25 mL)

var.
concentration
(1M, 1.5M, 2M)

var.
var.
var.
concentration
concentration
concentration
(1M, 1.5M, 2M)
(1M, 1.5M, 2M)
(1M, 1.5M, 2M)
Stirred for 45 min
Stirred for 45 min
Stirred for 45 min
Stirred for 45 min
at 60oC
at 60oC
at 60oC
at 60oC
added NH3.H2O
added NH3.H2O
added NH3.H2O
added NH3.H2O
until the pH value
until the pH value
until the pH value
until the pH value
reached about 7
reached about 7
reached about 7
reached about 7

Precipitation

Precipitation

Precipitation

Precipitation

Teflon-lined Autoclave
Power supply

Glass container

moved to teflon-lined autoclave

As + catalyst
suspension

heated at 160oC for 24 h

Cooling water inlet

Residue

Cooling water
outlet
UV lamp
Quartz glass
tube
Sample collection port
Magnetic pellet
Magnetic
stirrer

Filtrat

washed with AgNO3

The schematic diagram of the photocatalytic


reactor

calcinated at 600 C for 2 h


o

TiO2 nanocrystals

characterized with XRD and SEM


investigated the photocatalytic activity
through As removal

visib
le
light

Result

O
2

As
(III)
As
(V)

RESEARCH GOAL
This research is expected to obtain the appropriate
concentration of the solvents used to produce high
performance nanocrystal TiO2 in photocatalytic reduction
of Arsenic.

TiO2 photocatalytic
Activity

REFERENCES
[1] Gupta, K. K., N. L. Singh, A. Pandey, S. K. Shukla, S. N. Upadayay, V. Mishra, P. Srivastava, N. P. Lalla & P. K. Mishra. 2013.
Effect of Anatase/Rutile TiO2 Phase Composition on Arsenic Adsorption. Varanasi, India. Journal of Dispersion Science and
Technology, 34:10431052, July 2013
[2] Li, W., & T. Zeng. 2011. Preparation of TiO2 Anatase Nanocrystals by TiCl4 Hydrolysis with Additive H2SO4. Massachusetts,
United States of America.
Journal of Plose One, Volume 6, Issue 6, June 2011