1
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 ThailandbBioresources Research Unit, National Center for Genetic Engineering and Biotechnology (BIOTEC), 113 Thailand Science Park, Phaholyothin Road, Klong 1, Klong Luang, Pathumthani 12120 Thailand
PresentedBy
Syarifah Hikmah Julinda, S.Pi, M.Sc
2
Contents
Background of study Research objective Methodology Results and discussions Conclusions
3
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)
Environmental levels of Copper
40%
35%
25%
Industrial wastewater
Storm water and surface runoff
Domestic wastewater
Composition of copper releases to water bodies (United States Department of Agriculture, 1998)
Background
Copper is an essential trace elements but also an environmental pollutant
4
Measurement
SpectrophotometerSpectrophotometer
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)
Common methods for Cu (II) ion detection require the use of sophistication and expensive instrumentation
5
A dual responsive colorimetric and fluorescent Hg2+ ion from rhodamines based sensor in aqueous media (Huang et al., 2008)
ChemosensorChemosensorUpon binding metals: A fluorescent chemosensor inducesfluorescent change A colorimetric chemosensor exhibitscolor change. This is challengingtechnique since the detection of Cu (II) ion can be achieved by naked eye
Method Detection Limit
Reference
Rhodamine B hydroxylamine as fluorescent chemosensor Cu(II) ion
20 µg/litre
Chen et al (2009)
Terpyridine ascolorimetric chemosensor Hg(II) ion
2 µg/litre
Shunmugam (2008)
Successful chemosensor for detection metals
6
Pyrazolidine Luminol (PL)
Cu(II) ionCu(II) ion
Pyrazolidine Luminol Pyrazolidine Luminol
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)
7
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
Research objectives
8
Methodology
Phase IIDeveloping of
sensor
Phase IPre research
Selectivity of sensor
Detection limit of sensor
Optimum conditions of PL sensor :- Time response - pH
Materials and Reagents Preparation
Materials and Reagents Preparation
Synthesis of sensor and 1HNMR analysis
PL sensor solution
Naked eye
UV-vis spectrophotometer
UV-vis spectrophotometer
9
PL Cu2+ Ag+ Na+ Mn2+ Zn2+ Co2+ Cd2+ Hg2+ Pb2+ Fe2+ Ba2+ Al2+ Ca2+ Ni2+
Concentration of PL and metal ions were 10-3 M Selectivity of PL sensor
0
0.05
0.1
0.15
0.2
0.25
0.3
0.35
Ni2+ Cd2+ Mn2+ Hg2+ Pb2+ Zn2+ Ba2+ Ca2+ Na2+ Ag+ Al2+ Co2+ Fe2+ Cu2+
Metal ions
Ab
s 42
5/35
0
Absorbance of PL in the presence of various metal ions
Results and discussions
10
Detection limit of PL sensor
0 10-3 10-2 10-1
Naked eye :Detection limit found at 3.75 x 10-4 M
UV spectro :Detection limit found at 0.6 x 10-4 M
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0 2 4 6 8 10 12
Cu(II) ion concentration (mM)
Ab
sorb
ance
11
Optimum conditions of PL sensor (Cont’)
0.0
0.1
0.2
0.3
0.4
0.5
0 5 10 15 20 30 60
Time (min)
Ab
so
rban
ce
PL + Cu2+
PL + H2O
0
0.3
0.6
0.9
1.2
0 2 4 6 8 10 12
pH
Ab
sorb
ance
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
Time influence of UV-vis titration spectra of PL sensor (10-3 M) upon addition Cu(II) ion 10-3 M
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.
13
TerimakasiHTHANK YOU
Terimakasih