Detection limit of PL sensor

Report
DETECTION OF COPPER IN THE SYNTHETIC
WASTEWATER BY USING PYRAZOLIDINE
LUMINOL (PL)
Syarifah Hikmah Julindaa, Preeda Parkpiana and Srung Smanmoob
aSchool
of Environment, Resources and Development, Asian Institute of Technology, 58, Moo 9, km.42, Phaholyothin Highway,
Klong Luang, Pathumthani 12120 Thailand
bBioresources Research Unit, National Center for Genetic Engineering and Biotechnology (BIOTEC), 113 Thailand Science
Park, Phaholyothin Road, Klong 1, Klong Luang, Pathumthani 12120 Thailand
Presented
By
Syarifah Hikmah Julinda, S.Pi, M.Sc
1
Contents





2
Background of study
Research objective
Methodology
Results and discussions
Conclusions
Background
Environmental levels of Copper
Copper is an essential trace
elements but also an environmental
pollutant
Media
Levels/standard
Seawater
<1 µg/ l (Ellingsen et al., 2007)
Lake & river
1-10 µg/ l (Ellingsen et al., 2007)
Drinking water/tap water
< 1300 µg/ l (US EPA, 1993)
Industrial Effluent
< 2 mg/l (PCD, 2008)
25%
40%
35%
Industrial wastewater
Storm water and surface runoff
Domestic wastewater
Composition of copper releases to water bodies
(United States Department of Agriculture, 1998)
3
Measurement
Common methods for Cu (II) ion detection require the use of sophistication
and expensive instrumentation
Spectrophotometer
4
Sample Preparation
Method
Detection
Limit
Reference
Acidify with 1:1 HNO3 to
pH < 2
AAS
20 µg/litre
US EPA
(1986)
Filter and acidity sample
ICP
2-10 µg/litre
US EPA
(1986)
Filter and acidity sample
ICP-AES
6 µg/litre
ATSDR
(1990)
Sample solutions should
contain 0.5 % HNO3
GF-AAS
1 µg/litre
US EPA
(1986)
Acid digestion with
HNO3, reflux
ICP-MS
0.01 µg/litre
US EPA
(1994)
Chemosensor
Upon binding metals:
 A fluorescent chemosensor induces
fluorescent change
 A colorimetric chemosensor exhibits
color change. This is challenging
technique since the detection of Cu (II)
ion can be achieved by naked eye
Successful chemosensor for detection metals
Method
Detection
Limit
Reference
Rhodamine B hydroxylamine
as fluorescent chemosensor
Cu(II) ion
20 µg/litre
Chen et al
(2009)
Terpyridine as
colorimetric chemosensor
Hg(II) ion
2 µg/litre
Shunmugam
(2008)
A dual responsive colorimetric and fluorescent
Hg2+ ion from rhodamines based sensor in
aqueous media (Huang et al., 2008)
5
Pyrazolidine Luminol (PL)

PL is defined as a colorimetric chemosensor for Cu(II) ion detection. Upon
binding with Cu(II) ion, PL induces a color change followed by appearing
peak of absorbance around 425 nm. (Nasomphan et al., 2009)
Cu(II) ion
Pyrazolidine Luminol
6
Research objectives

Developing a PL sensor as a colorimetric chemosensor for the detection of
Cu (II) ion

Determination of detection limit and optimum conditions of PL sensor
7
Methodology
Phase I
Pre research
Materials and Reagents
Preparation
Synthesis of sensor and
1HNMR analysis
Phase II
Developing of
sensor
8
Selectivity of sensor
Naked eye
Detection limit of sensor
UV-vis
spectrophotometer
PL sensor solution
Optimum conditions of
PL sensor :
- Time response
- pH
UV-vis
spectrophotometer
Results and discussions
PL
Cu2+ Ag+
Na+ Mn2+ Zn2+ Co2+ Cd2+ Hg2+ Pb2+ Fe2+ Ba2+ Al2+ Ca2+ Ni2+
Absorbance of PL in the
presence of various metal
ions
0.35
0.3
Abs 425/350
0.25
0.2
0.15
0.1
0.05
0
Ni2+ Cd2+ Mn2+ Hg2+ Pb2+ Zn2+ Ba2+ Ca2+ Na2+ Ag+
Al2+ Co2+ Fe2+ Cu2+
Metal ions
Selectivity of PL sensor
9
Concentration of PL and metal ions were 10-3 M
Detection limit of PL sensor
10-3
0
10-2
10-1
Naked eye :
Detection limit
found at 3.75
x 10-4 M
0.7
0.6
Absorbance
0.5
0.4
UV spectro :
Detection limit
found at 0.6 x
10-4 M
0.3
0.2
0.1
0.0
0
2
4
6
8
Cu(II) ion concentration (mM)
10
10
12
Optimum conditions of PL sensor (Cont’)
Time influence of UV-vis titration
spectra of PL sensor (10-3 M)
upon addition Cu(II) ion 10-3 M
0.5
Absorbance
0.4
0.3
PL + Cu2+
PL + H2O
0.2
0.1
0.0
0
5
10
15
20
30
60
Time (min)
1.2
Absorbance
0.9
0.6
0.3
Effect of pH on UV-vis results of
absorbance PL sensor (10-3 M) at 425
nm upon addition Cu(II) ion 10-3 M
11
0
0
2
4
6
pH
8
10
12
Conclusions

There were changes in color of PL sensor upon addition of
Cu(II) ion, followed by appearing peak of absorbance at
425.92 nm (UV-Vis spectra)

Detection limit PL sensor 3.75 x 10-4 M of Cu(II) ion by naked
eye observation and 0.6 x 10-4 M by UV-vis
spectrophotometer

PL sensor give highly selectivity. In addition, PL sensor was
more preferable to Cu(II) ion rather than Cu(I) ion.
12
Terimakasih
TerimakasiH
THANK YOU
13

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