![Silica particles (1) Polystyrene bound silica particles (4)
Previous
study [46]
Previous
Study[36]
Current
Study
Previous study
[46]
Previous
study [36]
Current
study
Pore size (Å) a
343 212 343 252 146 221
Pore volume (cm3
/g) b
1.06 0.83 1.06 0.84 0.53 0.80
Surface area (m2
/g) c
136 283 136 131 161 125
a. BJH adsorption average pore diameter.
b. Total pore volume at P/Po = 0.99.
c. BET specific surface area.
Result and Discussion
Table. 1 BET/BJH analysis data for bare silica and polystyrene bound silica
Table.2 Comparison of elemental analysis results
Element Initiator bound silica prepared
without DBTDC
Initiator bound silica prepared
with DBTDC
Polystyrene
bound silica
Carbon % 4.30 5.93 10.21
Hydrogen % 0.51 0.65 1.30
Sulfur % 1.78 2.41 2.12
Nitrogen % 0.79 1.03 0.85](https://image.slidesharecdn.com/presentation-1-240926015439-256da7b8/85/Presentation-on-the-project-management-t-9-320.jpg)
Presentation on the project management t
- 1. Faiz Ali Department of Chemistry University of Malakand, KP, Pakistan. Advanced Separation Sciences Department of Chemistry and Chemical Engineering, INHA university, South Korea. faizecs@yahoo.com Acrylamide incorporated polystyrene bound stationary phases on silica monolith particles and inside fused silica capillary for the anomeric separation of d-glucose and saccharide analysis. Faiz Ali and Won Jo Cheong*
- 2. 4-Chloromethylphenylisocynate + Ground silica monolith NH Cl C O Si O S N O NH C O Si O PEG(Mn10,000) + Urea + TMOS + 0.01N Acetic acid Heating at 40C˚(LC-ovan), at120C˚ (Autoclave in GC-ovan) then drying at 70C˚ NH C O Si O n S N O Chain growing area Abstract Calcination Grinding Styrene mediated RAFT-polymerization Sodium diethylditio- carbamate-initiator Dibuty tin dichloride- catalyst 1mm ID,30cm long column 60/40 ACN/water, 0.1%TFA Tremendously high separation efficiency Better selectivity
- 3. Introduction porous/nonporous inorganic, surface Initiator attachment to their active sites Hydrophobic polymer layers on the surface Organic-inrorganic hybrid materials acting as RPLC- stationary phase media Using various reaction protocols one of the method development for better chromatographic performance has been the improvement of column efficiency by reducing particle size of stationary phase Initially in 100µm range Up to sub-2µm range Recently and specially developed stationary phases core-shell particles very fine porous particles Monoliths particles Fast HPLC-analysis
- 4. This study resulted in polystyrene bound partially sub-2µm silica monolith particulate stationary phase excellent separation efficiency Better selectivity highest N values for a column packed with a stationary phase based on silica particles better chromatographic performance than that of previous study Ali, F.; Cheong, W. J.; ALOthman, Z.A.; ALMajid, A.M. J. Chromatogr. A. 2013, 1303, 9-17 Introduction Catalysis of the Isocyanate-Hydroxyl Reaction by Werner J. Blank, Z. A. He and Ed T. Hessell King Industries Inc. Norwalk, CT. 06852 USA Why use DBTDC-catalyst 1) Its solubility in the polymerization reaction mixture-solvent 2) To uniformly attach 4-CPI to silica surface to avoid lumps of polystyrene in the final phase Reference S.S. Kim, W.J. Cheong, Bull. Korean Chem. Soc. 30 (2009) 722–725. S1-Initiator system
- 5. Overall scheme PEG,Mn10,000+Urea+TMOS+0.01N Acetic acid Heating at 40C˚, at 120C˚ then drying at 70C˚ (Condensation ) Grinding Calcination at 550˚C Silica monolith particles 4-Chloromethylphenylisocynate + Sodium dietdithiocarbamate Uniformly distributed thin Polystyrene Bound Silica Particles Styrene, RAFT Solution under Ice cold conditions Experimental DBTDC-Catalyst Spacer Ligand Initiator Ligand
- 6. Course of Reactions Experimental Schematic pathways for the synthesis of silica modified with chlorine-terminated ligand (A), initiator attached silica (B), and polystyrene bound silica (C), and the initiator silica structures prepared with 4-Chloromethylphenylisocynate (S1) and 3-chloropropyltrimethoxysilane (S2) as in previous study. The arrows denote the bond where the polymer chain is grown.
- 7. Microscopic view of silica monolith particles (A) and polystyrene bound silica monolith particles (X), SEM images of silica particles (B and C, wide and close views, respectively) and polystyrene- attached particles (Y and Z) A B C X Y Z Result and Discussion Comparison of the Architectural views of the bare silica and polystyrene bound silica
- 8. Particle size distribution and pore size distribution of silica particles (●) and polystyrene bound silica (○). The expression “d(x)” indicates the particle diameter corresponding to the integrated area ratio of x when integrated in the range of 0-d(x) diameter Result and Discussion Particle size distribution and BJH pore size distribution of silica particles (●) and polystyrene bound silica (○).
- 9. Silica particles (1) Polystyrene bound silica particles (4) Previous study [46] Previous Study[36] Current Study Previous study [46] Previous study [36] Current study Pore size (Å) a 343 212 343 252 146 221 Pore volume (cm3 /g) b 1.06 0.83 1.06 0.84 0.53 0.80 Surface area (m2 /g) c 136 283 136 131 161 125 a. BJH adsorption average pore diameter. b. Total pore volume at P/Po = 0.99. c. BET specific surface area. Result and Discussion Table. 1 BET/BJH analysis data for bare silica and polystyrene bound silica Table.2 Comparison of elemental analysis results Element Initiator bound silica prepared without DBTDC Initiator bound silica prepared with DBTDC Polystyrene bound silica Carbon % 4.30 5.93 10.21 Hydrogen % 0.51 0.65 1.30 Sulfur % 1.78 2.41 2.12 Nitrogen % 0.79 1.03 0.85
- 10. 10 Result and Discussion Cross sectional FE-SEM images of the capillary column where thin and compact co-polymer layer can be seen. Wide view (left) and close view (right). An applied potential of 15 kV was used for electron beam, while the magnification was 10,000 and 30,000 and selected scale bar size was 5 µm and 1 µm for the left and right photos, respectively.
- 11. 11 Comparison between Cross sectional FE-SEM images of bare silica (left) and Co-polymer immobilized (right) silica capillary column Result and Discussion
- 18. Result and Discussion 10 20 30 40 50 60 4 6 8 10 12 14 16 18 20 HETP (um) Flow rate (uL/mint) Phenol Acetophenone 4-Mehtyl-2-Nitroaniline Benzene Toluene HETP band width plot
- 19. Conclusion catalytic isocyanate-hydroxyl reaction(DBTDC) 4-Chloromethyl- phenylisocynate Partial Sub-2µm particles with shape diversity Uniform Ligand attachment→ Sodium diethyldithiocarbamate RAFT- polymerization Uniform, thin polystyrene bound smooth silica particulate stationary phase Packed in a column of 1mm, ID and30Cm long 3. Excellent separation efficiency 4. N-Values are better than any commercially available HPLC stationary phase 1. Better selectivity 2. High enough permeability
- 20. Thank you Any Question Please? F. Ali et al and W.J. Cheong et al Advanced Separation Lab Department of Chemistry and Chemical Engineering INH University, South Korea Advanced Separation Sciences INHA University Incheon South Korea