SYNTHESIS AND CHARACTERIZATION PARTICLE COLUMN LIQUID CHROMATOGRAPHY BASED POLYMER@SILICA AND SILICA-ORGANIC AND ITS APPLICATIONS FOR SEPARATION
Liquid chromatography column particles are generally made of silica or polymer based materials. Various modifications are made to the material’s surface for the best separation performance. In this study, new silica-organik materials were synthesized from vinyltrimethoxysilane and divinylbenzen...
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| Format: | Theses |
| Language: | Indonesia |
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| Online Access: | https://digilib.itb.ac.id/gdl/view/86687 |
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| Institution: | Institut Teknologi Bandung |
| Language: | Indonesia |
| Summary: | Liquid chromatography column particles are generally made of silica or polymer
based materials. Various modifications are made to the material’s surface for the
best separation performance. In this study, new silica-organik materials were
synthesized from vinyltrimethoxysilane and divinylbenzene, whhich were
compared with polymer@silica particles synthesized from silica-phenyl-modified
methyl methacrylate and divinylbenzene. The polymer@silica particles obtained
optimum results at a composition of 18,80 x 10-3 mol MMA + 25,25 x 10-3 mol
DVB, after silica and phenyl modification obtained a homogeneous spheric particles
with a diameter of 3,03 µm. FTIR spectra had peaks of 722, 1081 and 2855 cm-1 for
Si-C, Si-O, dan C-H bonds, respectively. Optimum conditions for the 100 mm × 4,6
mm column were achieved at a mobile phase of methanol : water 60:40, flow rate
1,0 mL/min, and ? 274 nm, with Rs 3,86 and symmetrical factor 1,05. linearity was
good in the range of 10-100 ppm, R2 0,994 for paracetamol and R2 0,996 for
caffeine. Polymer@silica could separate paracetamol and caffeine, but could not
separate paracetamol precursors (oxime and acetophenone). Silica-organic materials
obtained optimum results at a composition of 23,51 x 10-3 mol VTMS + 28,05 x 10
3mol DVB, with homogeneous spheric particles of 2,3 µm diameter. FTIR spectra
had peaks of 1000, 1081 and 2855 cm-1 for Si-C, Si-O, and C-H bonds, respectively.
Optimum conditions for the 100 mm × 4,6 mm were achieved at a mobile phase of
acetonitrile : water 15:85, a flow rate of 1,0 mL/min, and ? 274 nm with Rs 3,96 and
symmetrical factor 1.10. Linearity was good in range of 10-100 ppm, R2 0,994 for
paracetamol and R2 0,996 for caffeine. This silica-organic particles can separate the
analysis of paracetamol, paracetamol precursor, and caffeine. |
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