Functionalized polythiophene-coated magnetic nanoparticles for solid-phase extraction of phthalates / Siti Nor Atika Baharin
Polythiophene, poly(3-hexylthiophene), poly(N-phenyl-1-(2-thienyl)methanimine) and poly(phenyl-(4-(6-thiophen-3-yl-hexyloxy)-benzylidine)amine) were successfully coated on the surface of Fe3O4 magnetic nanoparticles (MNP). Two of the functionalized monomers, N-phenyl-1-(2-thienyl)methanimine and...
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| Format: | Thesis |
| Published: |
2016
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| Online Access: | http://studentsrepo.um.edu.my/7058/ http://studentsrepo.um.edu.my/7058/4/atika.pdf |
| _version_ | 1848773314522120192 |
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| author | Siti Nor Atika , Baharin |
| author_facet | Siti Nor Atika , Baharin |
| author_sort | Siti Nor Atika , Baharin |
| building | UM Research Repository |
| collection | Online Access |
| description | Polythiophene, poly(3-hexylthiophene), poly(N-phenyl-1-(2-thienyl)methanimine)
and poly(phenyl-(4-(6-thiophen-3-yl-hexyloxy)-benzylidine)amine) were
successfully coated on the surface of Fe3O4 magnetic nanoparticles (MNP). Two of
the functionalized monomers, N-phenyl-1-(2-thienyl)methanimine and phenyl(4-(6-
thiophen-3-yl-hexyloxy)-benzylidine)amine were successfully synthesized.
Characterization by FT-IR, TGA, XRD, VSM and BET confirmed the coating has
taken place. Further characterization of MNP coated poly(phenyl-(4-(6-thiophen-3-
yl-hexyloxy)-benzylidine)amine) (P3TArH) was conducted using TEM and FESEM.
Among those nanocomposites, MNP coated P3TArH has shown higher
determination capabilities of phthalates. The adsorption behaviour of di(2-
ethylhexyl) phthalate (DEHP) onto the MNP coated P3TArH showed fast kinetics,
occurred heterogenously on the adsorption sites and exothermic. The activation
energy determined found was -40.6 kJ mol−1 K−1, indicated the process is
physisorption. The successful synthesised magnetic nanoparticles were further
optimized for magnetic solid-phase extraction (MSPE) of environmental samples.
Separation and determination of the extracted phthalates namely dimethyl phthalate
(DMP), diethyl phthalate (DEP), dipropyl phthalate (DPP), dibutyl phthalate (DBP),
butyl benzyl phthalate (BBP), dicyclohexyl phthalate (DCP), di(2-ethylhexyl)
phthalate (DEHP) and di-n-octyl phthalate (DNOP) were conducted by gas
chromatography-flame ionization detector (GC-FID). The best working conditions
were as follows; sample at pH 7, 30 min extraction time, ethyl acetate as elution
solvent, 500 μL elution solvent volumes, 10 min desorption time, 10 mg adsorbent
dosage, 20 mL sample loading volume and 15 g L-1 concentration of NaCl. Under the
optimized conditions, the analytical performances were determined with linear range of 0.1-50 μg L-1 and limit of detection at 0.054-0.468 μg L-1 for all the studied
analytes. The intra-day (n=7) and inter-day (n=3) relative standard deviations, RSD
(%) of three replicates each demonstrated in the range of 3.7-4.9 and 3.0-5.0
respectively. The steadiness and reusability studies suggested that the
MNP@P3TArH could be used up to five cycles. The proposed method was executed
to analysis of real water samples namely commercial bottled mineral waters and
fresh milk and recoveries in the range of 68-101 % and relative standard deviation
(RSD %) lower than 7.7 % were attained. |
| first_indexed | 2025-11-14T13:40:26Z |
| format | Thesis |
| id | um-7058 |
| institution | University Malaya |
| institution_category | Local University |
| last_indexed | 2025-11-14T13:40:26Z |
| publishDate | 2016 |
| recordtype | eprints |
| repository_type | Digital Repository |
| spelling | um-70582019-09-23T23:36:01Z Functionalized polythiophene-coated magnetic nanoparticles for solid-phase extraction of phthalates / Siti Nor Atika Baharin Siti Nor Atika , Baharin Q Science (General) Polythiophene, poly(3-hexylthiophene), poly(N-phenyl-1-(2-thienyl)methanimine) and poly(phenyl-(4-(6-thiophen-3-yl-hexyloxy)-benzylidine)amine) were successfully coated on the surface of Fe3O4 magnetic nanoparticles (MNP). Two of the functionalized monomers, N-phenyl-1-(2-thienyl)methanimine and phenyl(4-(6- thiophen-3-yl-hexyloxy)-benzylidine)amine were successfully synthesized. Characterization by FT-IR, TGA, XRD, VSM and BET confirmed the coating has taken place. Further characterization of MNP coated poly(phenyl-(4-(6-thiophen-3- yl-hexyloxy)-benzylidine)amine) (P3TArH) was conducted using TEM and FESEM. Among those nanocomposites, MNP coated P3TArH has shown higher determination capabilities of phthalates. The adsorption behaviour of di(2- ethylhexyl) phthalate (DEHP) onto the MNP coated P3TArH showed fast kinetics, occurred heterogenously on the adsorption sites and exothermic. The activation energy determined found was -40.6 kJ mol−1 K−1, indicated the process is physisorption. The successful synthesised magnetic nanoparticles were further optimized for magnetic solid-phase extraction (MSPE) of environmental samples. Separation and determination of the extracted phthalates namely dimethyl phthalate (DMP), diethyl phthalate (DEP), dipropyl phthalate (DPP), dibutyl phthalate (DBP), butyl benzyl phthalate (BBP), dicyclohexyl phthalate (DCP), di(2-ethylhexyl) phthalate (DEHP) and di-n-octyl phthalate (DNOP) were conducted by gas chromatography-flame ionization detector (GC-FID). The best working conditions were as follows; sample at pH 7, 30 min extraction time, ethyl acetate as elution solvent, 500 μL elution solvent volumes, 10 min desorption time, 10 mg adsorbent dosage, 20 mL sample loading volume and 15 g L-1 concentration of NaCl. Under the optimized conditions, the analytical performances were determined with linear range of 0.1-50 μg L-1 and limit of detection at 0.054-0.468 μg L-1 for all the studied analytes. The intra-day (n=7) and inter-day (n=3) relative standard deviations, RSD (%) of three replicates each demonstrated in the range of 3.7-4.9 and 3.0-5.0 respectively. The steadiness and reusability studies suggested that the MNP@P3TArH could be used up to five cycles. The proposed method was executed to analysis of real water samples namely commercial bottled mineral waters and fresh milk and recoveries in the range of 68-101 % and relative standard deviation (RSD %) lower than 7.7 % were attained. 2016-12 Thesis NonPeerReviewed application/pdf http://studentsrepo.um.edu.my/7058/4/atika.pdf Siti Nor Atika , Baharin (2016) Functionalized polythiophene-coated magnetic nanoparticles for solid-phase extraction of phthalates / Siti Nor Atika Baharin. PhD thesis, University of Malaya. http://studentsrepo.um.edu.my/7058/ |
| spellingShingle | Q Science (General) Siti Nor Atika , Baharin Functionalized polythiophene-coated magnetic nanoparticles for solid-phase extraction of phthalates / Siti Nor Atika Baharin |
| title | Functionalized polythiophene-coated magnetic nanoparticles for solid-phase extraction of phthalates / Siti Nor Atika Baharin |
| title_full | Functionalized polythiophene-coated magnetic nanoparticles for solid-phase extraction of phthalates / Siti Nor Atika Baharin |
| title_fullStr | Functionalized polythiophene-coated magnetic nanoparticles for solid-phase extraction of phthalates / Siti Nor Atika Baharin |
| title_full_unstemmed | Functionalized polythiophene-coated magnetic nanoparticles for solid-phase extraction of phthalates / Siti Nor Atika Baharin |
| title_short | Functionalized polythiophene-coated magnetic nanoparticles for solid-phase extraction of phthalates / Siti Nor Atika Baharin |
| title_sort | functionalized polythiophene-coated magnetic nanoparticles for solid-phase extraction of phthalates / siti nor atika baharin |
| topic | Q Science (General) |
| url | http://studentsrepo.um.edu.my/7058/ http://studentsrepo.um.edu.my/7058/4/atika.pdf |