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M. MARUTHUPANDI
RRN: 180913701001
Ph.D. Research Scholar
Department of Chemistry
SUPERVISOR
Dr. N. VASIMALAI
ASST. PROFESSOR
Department of Chemistry
Tentative title
1
2
Outline
Introduction
Experimental Details
Characterization
Applications
Summery
3
Outline
Introduction
Experimental Details
Characterization
Applications
Summery
 Toxic ions pollutants affect on the environment and also on human health
 Metallic mercury vapors and organic mercury derivatives affect
many different areas of the brain, heart, kidney and stomach 1
 Estimated by the U.S. Environmental Protection Agency (USEPA)
that the total mercury released into the environment reaches ∼7,500 tons per year 2
 WHO have recommended the level of Hg(II) must be 2 μg/L in drinking water 3
 Mercury is used in the electrolytic production of chlorine, in electrical appliances, in
dental amalgams and as a raw material for various mercury compounds
 Environmentally, mercury occurs through a variety of natural including oceanic and
volcanic emissions, gold mining, solid waste 2
4
 Sulfide can regulate blood pressure, heart, nervous system and
bacterial protection of Sulphur present proteins and amino acids
 Notably, S2- combine with protons to form HS- or H2S has caught
up in many serious health problems 4
 However, irregular levels of S2- in biological system cause severe problems such as
diabetes, respiratory paralysis, liver cirrhosis and Alzheimer’s disease 5
 Acid rain is caused by emissions of sulfur dioxide and nitrogen oxide, which react
with the water molecules in the atmosphere to produce acids.
 Environmentally, Sulfide occurs through a variety of spring, surface and wastewater
 Monitoring the dangerous level of Hg2+ and S2- in biological and water samples is
great importance in biological and environmental fields 6 5
6
 Metal nanoclusters consist of a small
number of atoms, at most in the tens
 Nanoclusters contains either of a single
or of multiple elements and size is less
than 2 nm 7
 Researches have been focused in the
field of gold and silver nanoclusters. But
fluorescent copper nanocluster is less
cost, high photo luminance, bio
compatible and easy synthesis
procedure 8
7
Objectives
Introduction
Experimental Details
Characterization
Applications
Summery
8
AA = Ascorbic Acid ; TG = 1-Thio-β-D-glucose; CuNCs = Copper Nanocluster
9
Outline
Introduction
Experimental
Characterization
Applications
Summery
(A) UV-vis spectra of (a) Cu (NO3)2, (b) AA, (c) Cu (NO3)2 + AA, (d) TG, (e) Cu (NO3)2 + AA + TG and (f) TG-CuNCs. (B)
Day light and (C) Under UV light Corresponding photographs of (a-f). 9
10
(A)
(B)
(C)
(a) UV-vis and (b) fluorescence spectra of TG-CuNCs (λex:350; λem:430 nm). Inset: Photograph of
TG-CuNCs under (a) day light and (b) UV light. 9
11
UV-vis spectra of (a) freshly prepared and (b) 2-months aged CuNCs. Inset: (a) and (b), Photograph of
corresponding CuNCs.
12
FT-IR spectra of (a) TG and (b) TG-CuNCs. 10, 11, 12, 13
113
HR-TEM images of TG-CuNCs with (A) 50 nm and (B) 20 nm magnifications. Inset: Particle size histogram.
The obtained TG-CuNCs are well dispersed spherical like shape and the range of particles diameter was
calculated to be 2.58 ± 0.03 nm by HR-TEM. 14, 15, 16, 17 11
114
1.0 1.5 2.0 2.5 3.0 3.5 4.0
0
10
20
30
40
Frequency
Particle size (nm)
(A) (B)
(A) HR-TEM of image of TG-CuNCs, (B) Selected area diffraction pattern of TG-CuNCs.
The obtained TG-CuNCs are crystal lattice was calculated to be 0.21 nm by HR-TEM. 18, 19
11
115
(A) (B)
Effect of Time: (A) CuNCs in the presence of 1.5 × 10-6 M Hg2+ [3 mins], (B) CuNCs in the presence of 1.5 × 10-6 M
S2- [5 mins] at different time Vs relative intensity.
116
Hg2+
S2-
(A) (B)
3
Outline
Introduction
Experimental Details
Characterization
Applications
Summery
117
Emission spectra of CuNCs in the presence of different concentration Hg2+ (a) 0, (b) 0.5, (c) 1.0, (d) 1.5, (e) 2.0, (f)
2.5, (g) 3.0, (h) 3.5, (i) 4.0, (j) 4.5 and (k) 5.0×10-6 M Hg2+. Inset: (i) straight line curve (ii) Photographs of UV light
(a) before and (k) after the addition 5.0×10-6 M of Hg2+. 118
LOD = 1.70 nM
Hg2+
119
Absorbance spectra of CuNCs in the presence of different concentration Hg2+ (a) 0, (b) 1.0, (c) 2.0, (d) 3.0, (e) 4.0,
(f) 5.0, (g) 6.0 and (h) 7.0×10-6 M Hg2+. Inset: Enlarge scale 20
120
Emission spectra of CuNCs in the presence of different concentration S2- (a) 0, (b) 0.5, (c) 1.0, (d) 1.5, (e) 2.0, (f)
2.5, (g) 3.0, (h) 3.5, (i) 4.0, (j) 4.5 and (k) 5.0, (l) 5.5×10-6 M S2-. Inset: (i) straight line curve (ii) Photographs of UV
light (a) before and (l) after the addition 5.5×10-6 M of S2-.
LOD = 1.02 nM
S2-
121
Absorbance spectra of CuNCs in the presence of different concentration S2- (a) 0, (b) 1.0, (c) 2.0, (d) 3.0, (e) 4.0,
(f) 5.0, (g) 6.0, (h) 7.0×10-6 M S2-. 21
22
Schematic representation for the possible mechanism of Hg2+ and S2-Sensor. 122
23
24
(i) 1.08×10-3M (720 fold) of
common interferences such as
Na+, K+, Cd2+, Zn2+, Pb2+, Fe2+,
Ni2+, Mn2+,
(ii) 9.00×10-4M (600 fold) of
common interferences such as
Fe3+, Mg2+, Co2+,
(iii) 1.84×10-3M (1229 fold) of
common interferences such as
Br-, F-, Cl-, I-, HPO4
-, AcO-, NO2
-,
SO4
2-, NO3
-, SCN-, CO3
-, SCN-
above mention common
potential interference did not
interact for the detection of 1.5
× 10-6M of Hg2+ and S2-.
21
123
24
Outline
Introduction
Experimental Details
Characterization
Applications
Summery
25
 We have successfully synthesized TG-CuNCs at room
temperature within 1 min
 The synthesized TG-CuNCs was well characterized by several
techniques
 Then, TG-CuNCs was used as probe for the detection of Mercury
and Sulfide corresponding LOD was found to be 1.70 and 1.02
nM
 600 to 1229-fold excess of common interferences did not
interfere for the detection of 1.5 µM Mercury and Sulfide ions
 Finally we have discuss possible mechanism of detection
Mercury and Sulfide ions
26
TG in the presence of different concentration of Mercury
and Sulfide monitoring UV-vis spectrophotometer
Future characterisation XRD and DLS spectroscopy
Then, Sensor system applying real sample analysis
Preparation of paper based kit
Smart phone based validation method
colloquium-2.pptx

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colloquium-2.pptx

  • 1. M. MARUTHUPANDI RRN: 180913701001 Ph.D. Research Scholar Department of Chemistry SUPERVISOR Dr. N. VASIMALAI ASST. PROFESSOR Department of Chemistry
  • 5.  Toxic ions pollutants affect on the environment and also on human health  Metallic mercury vapors and organic mercury derivatives affect many different areas of the brain, heart, kidney and stomach 1  Estimated by the U.S. Environmental Protection Agency (USEPA) that the total mercury released into the environment reaches ∼7,500 tons per year 2  WHO have recommended the level of Hg(II) must be 2 μg/L in drinking water 3  Mercury is used in the electrolytic production of chlorine, in electrical appliances, in dental amalgams and as a raw material for various mercury compounds  Environmentally, mercury occurs through a variety of natural including oceanic and volcanic emissions, gold mining, solid waste 2 4
  • 6.  Sulfide can regulate blood pressure, heart, nervous system and bacterial protection of Sulphur present proteins and amino acids  Notably, S2- combine with protons to form HS- or H2S has caught up in many serious health problems 4  However, irregular levels of S2- in biological system cause severe problems such as diabetes, respiratory paralysis, liver cirrhosis and Alzheimer’s disease 5  Acid rain is caused by emissions of sulfur dioxide and nitrogen oxide, which react with the water molecules in the atmosphere to produce acids.  Environmentally, Sulfide occurs through a variety of spring, surface and wastewater  Monitoring the dangerous level of Hg2+ and S2- in biological and water samples is great importance in biological and environmental fields 6 5
  • 7. 6  Metal nanoclusters consist of a small number of atoms, at most in the tens  Nanoclusters contains either of a single or of multiple elements and size is less than 2 nm 7  Researches have been focused in the field of gold and silver nanoclusters. But fluorescent copper nanocluster is less cost, high photo luminance, bio compatible and easy synthesis procedure 8
  • 9. 8 AA = Ascorbic Acid ; TG = 1-Thio-β-D-glucose; CuNCs = Copper Nanocluster
  • 11. (A) UV-vis spectra of (a) Cu (NO3)2, (b) AA, (c) Cu (NO3)2 + AA, (d) TG, (e) Cu (NO3)2 + AA + TG and (f) TG-CuNCs. (B) Day light and (C) Under UV light Corresponding photographs of (a-f). 9 10 (A) (B) (C)
  • 12. (a) UV-vis and (b) fluorescence spectra of TG-CuNCs (λex:350; λem:430 nm). Inset: Photograph of TG-CuNCs under (a) day light and (b) UV light. 9 11
  • 13. UV-vis spectra of (a) freshly prepared and (b) 2-months aged CuNCs. Inset: (a) and (b), Photograph of corresponding CuNCs. 12
  • 14. FT-IR spectra of (a) TG and (b) TG-CuNCs. 10, 11, 12, 13 113
  • 15. HR-TEM images of TG-CuNCs with (A) 50 nm and (B) 20 nm magnifications. Inset: Particle size histogram. The obtained TG-CuNCs are well dispersed spherical like shape and the range of particles diameter was calculated to be 2.58 ± 0.03 nm by HR-TEM. 14, 15, 16, 17 11 114 1.0 1.5 2.0 2.5 3.0 3.5 4.0 0 10 20 30 40 Frequency Particle size (nm) (A) (B)
  • 16. (A) HR-TEM of image of TG-CuNCs, (B) Selected area diffraction pattern of TG-CuNCs. The obtained TG-CuNCs are crystal lattice was calculated to be 0.21 nm by HR-TEM. 18, 19 11 115 (A) (B)
  • 17. Effect of Time: (A) CuNCs in the presence of 1.5 × 10-6 M Hg2+ [3 mins], (B) CuNCs in the presence of 1.5 × 10-6 M S2- [5 mins] at different time Vs relative intensity. 116 Hg2+ S2- (A) (B)
  • 19. Emission spectra of CuNCs in the presence of different concentration Hg2+ (a) 0, (b) 0.5, (c) 1.0, (d) 1.5, (e) 2.0, (f) 2.5, (g) 3.0, (h) 3.5, (i) 4.0, (j) 4.5 and (k) 5.0×10-6 M Hg2+. Inset: (i) straight line curve (ii) Photographs of UV light (a) before and (k) after the addition 5.0×10-6 M of Hg2+. 118 LOD = 1.70 nM Hg2+
  • 20. 119 Absorbance spectra of CuNCs in the presence of different concentration Hg2+ (a) 0, (b) 1.0, (c) 2.0, (d) 3.0, (e) 4.0, (f) 5.0, (g) 6.0 and (h) 7.0×10-6 M Hg2+. Inset: Enlarge scale 20
  • 21. 120 Emission spectra of CuNCs in the presence of different concentration S2- (a) 0, (b) 0.5, (c) 1.0, (d) 1.5, (e) 2.0, (f) 2.5, (g) 3.0, (h) 3.5, (i) 4.0, (j) 4.5 and (k) 5.0, (l) 5.5×10-6 M S2-. Inset: (i) straight line curve (ii) Photographs of UV light (a) before and (l) after the addition 5.5×10-6 M of S2-. LOD = 1.02 nM S2-
  • 22. 121 Absorbance spectra of CuNCs in the presence of different concentration S2- (a) 0, (b) 1.0, (c) 2.0, (d) 3.0, (e) 4.0, (f) 5.0, (g) 6.0, (h) 7.0×10-6 M S2-. 21
  • 23. 22 Schematic representation for the possible mechanism of Hg2+ and S2-Sensor. 122 23 24
  • 24. (i) 1.08×10-3M (720 fold) of common interferences such as Na+, K+, Cd2+, Zn2+, Pb2+, Fe2+, Ni2+, Mn2+, (ii) 9.00×10-4M (600 fold) of common interferences such as Fe3+, Mg2+, Co2+, (iii) 1.84×10-3M (1229 fold) of common interferences such as Br-, F-, Cl-, I-, HPO4 -, AcO-, NO2 -, SO4 2-, NO3 -, SCN-, CO3 -, SCN- above mention common potential interference did not interact for the detection of 1.5 × 10-6M of Hg2+ and S2-. 21 123
  • 26. 25  We have successfully synthesized TG-CuNCs at room temperature within 1 min  The synthesized TG-CuNCs was well characterized by several techniques  Then, TG-CuNCs was used as probe for the detection of Mercury and Sulfide corresponding LOD was found to be 1.70 and 1.02 nM  600 to 1229-fold excess of common interferences did not interfere for the detection of 1.5 µM Mercury and Sulfide ions  Finally we have discuss possible mechanism of detection Mercury and Sulfide ions
  • 27. 26 TG in the presence of different concentration of Mercury and Sulfide monitoring UV-vis spectrophotometer Future characterisation XRD and DLS spectroscopy Then, Sensor system applying real sample analysis Preparation of paper based kit Smart phone based validation method