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CH5011-COLLOIDS AND SURFACES
Jayadheer A (CH09B001)
Sai Prashanth Reddy D (CH09B015)
Nirup Kumar N (CH09B034)
KrishnaTeja R (CH09b050)
 To find the appropriate proportions of given
polymer and particle solutions that forms a
shake gel i.e., shears induced gelation.
 To verify the reversible gelation mechanism
 Interaction between PVP and the surface of silica
takes place mainly by means of hydrogen bonds.
 Research has shown that PVP occurs in two forms
on the silica surface, reversibly adsorbed and
irreversibly grafted onto the surface of silica.
 The irreversible adsorption can be attributed to
the formation of relatively strong –C=O….H-OSi
hydrogen bonds whereas the interactions
between Si and N.
Ref.Toki,TY Chow,T Ohnaka, H Samura, &T Saegusa, 1992)
 PVP (Polyvinylpyrrolidone k-30, average Mw
= 40,000)
 Silica particles (LUDOXTM-50 colloidal silica,
50 wt. % suspension in water)
 Weighing balance
 Vacuum Pipette
 Milli-Q water
 Magnetic Stirrer
 Culture Bottles
 Polyvinylpyrrolidone also commonly called
Polyvidone or Povidone,
 Monomer: N-vinylpyrrolidone.
 molecular weight of nearly 40,000
 K value of 30 (Fikentscher's formula)
(Ref. Ashland_Inc)
Where, c = concentration in g/100 ml;
c = viscosity of the solution;
0 = viscosity of the solvent;
k = value according to Fikentscher (K = 1000* k)
(Fikentscher's Formula)
 Spherical silica particles are suspended in an
aqueous phase.
 The colloidal suspension is stabilized by pH
adjustment and then concentrated, usually
by evaporation.
Brand Aldrich
Formula SiO2
Mol Wt. 60.08 g/mol
Density 1.4 g/ml @25 oC
Table: Data for LUDOXTM-50 colloidal silica, 50 wt. % suspension in water
(Ref. Aldrich)
 Polymer solution
 Colloidal Silica suspension
 Take different proportions of the solutions
using micro-pipette
 Mix them in a culture bottle
 Shake the bottle to observe the formation of
gel
 Repeat the experiment for various
concentrations
 Glassware should be properly cleaned and
sterilized in ovens or using nitrogen vents
 Store the micro pipette vertically to prevent
liquids from running inside the shaft of the
pipette.
 Minimize the exposure time for PVP while
weighing, as it can gain weight by absorbing
atmospheric water
 Should wear goggles and potentially lab aprons
Table 2: Colloidal Silica data from manufacturer
(Aldrich)and PVP data from (Ashland_Inc)
Material Density (g/ml)
@ 25oC
Silica 50% 1.4
PVP 02% 1.008
PVP 10% 1.02
PVP 30% 1.07
By Volume By Weight Inference
2 % PVP 50 %Silica 2 % PVP 50 %Silica
1 1 1.008 1.4 Very less viscous mixture
10 % PVP 50 %Silica 10 % PVP 50 %Silica
1 1 1.02 1.4 viscous liquid
1 3 1.02 4.2 more viscous
1 6 1.02 8.4 more viscous
30 % PVP 50 %Silica 30 % PVP 50 %Silica
2 1 2.14 1.4 very high viscous
4 3 4.28 4.2 Some gel is formed
1 1 1.07 1.4 Some gel is formed
1 3 1.07 4.2 Shake gel
1 7 1.07 9.8 Shake gel
From Stanford Univ.
 The structure of the gel formed can be
studied using IR spectroscopy, SEM, DLS and
other relevant techniques
 The rheological properties likeVisco-elasticity
of the gel can be studied with changing the
polymer and silica proportions.
 The gelation that occurred upon shaking the
solution rigorously has contribution of both
reversibly and irreversibly adsorbed polymer
particles.
 When left to settle, a part of polymer desorbs
and this can be attributed to reversible
gelation
 A number of experiments were conducted
using different concentrations, and
proportions of PVP with 50% colloidal silica.
 Experiments were also conducted using PVA as
polymer. Since, 20% PVA solution formed a very
viscous fluid, PVP was considered for further
experiments
 Using 30% PVP and 50% Silica in 1:1 volume
proportions, a near gel was formed.
 So, different proportions of these mixtures were
tried and a near shake gel is finally obtained.
 Increasing the proportion of silica particles led to
the formation of better shake gels.This also
supports the mechanism of reversible gelation.
 Belyakova, L.A., Anatoly M.Varvarin, DianaY. Lyashenko, & NadiyaV. Roik.
(2003). Study of interaction of poly(1-vinyl-2-pyrrolidone) with a surface.
Colloid Interface Sci., 264, 2–6.
 Spinde, K., Konstantinos Pachis, JoannaAntonakaki, & Silvia. (2011). Influence
of Polyamines and Related Macromolecules on Silicic Acid
Polycondensation: Relevance to “Soluble Silicon Pools”? Chemistry of
Materials, 4676–4687.
 Toki, M.,TY Chow,T Ohnaka, H Samura, &T Saegusa. (1992). Structure of
poly (vinylpyrrolidone)-silica hybrid. Polymer Bulletin, 36.
 Aldrich, S. (n.d.). LUDOX®TM-50 colloidal silica. Retrieved Nov 10, 2012, from
http://www.sigmaaldrich.com/catalog/product/aldrich/420778?lang=en&regio
n=IN
 Ashland_Inc. (n.d.). IspCorp. Retrieved Nov 10, 2012, from
http://online1.ispcorp.com/Brochures/Performance%20Chemicals/PVP.pdf
ThankYou 

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Shake gels

  • 1. CH5011-COLLOIDS AND SURFACES Jayadheer A (CH09B001) Sai Prashanth Reddy D (CH09B015) Nirup Kumar N (CH09B034) KrishnaTeja R (CH09b050)
  • 2.  To find the appropriate proportions of given polymer and particle solutions that forms a shake gel i.e., shears induced gelation.  To verify the reversible gelation mechanism
  • 3.  Interaction between PVP and the surface of silica takes place mainly by means of hydrogen bonds.  Research has shown that PVP occurs in two forms on the silica surface, reversibly adsorbed and irreversibly grafted onto the surface of silica.  The irreversible adsorption can be attributed to the formation of relatively strong –C=O….H-OSi hydrogen bonds whereas the interactions between Si and N.
  • 4. Ref.Toki,TY Chow,T Ohnaka, H Samura, &T Saegusa, 1992)
  • 5.  PVP (Polyvinylpyrrolidone k-30, average Mw = 40,000)  Silica particles (LUDOXTM-50 colloidal silica, 50 wt. % suspension in water)  Weighing balance  Vacuum Pipette  Milli-Q water  Magnetic Stirrer  Culture Bottles
  • 6.
  • 7.  Polyvinylpyrrolidone also commonly called Polyvidone or Povidone,  Monomer: N-vinylpyrrolidone.
  • 8.  molecular weight of nearly 40,000  K value of 30 (Fikentscher's formula) (Ref. Ashland_Inc) Where, c = concentration in g/100 ml; c = viscosity of the solution; 0 = viscosity of the solvent; k = value according to Fikentscher (K = 1000* k) (Fikentscher's Formula)
  • 9.  Spherical silica particles are suspended in an aqueous phase.  The colloidal suspension is stabilized by pH adjustment and then concentrated, usually by evaporation. Brand Aldrich Formula SiO2 Mol Wt. 60.08 g/mol Density 1.4 g/ml @25 oC Table: Data for LUDOXTM-50 colloidal silica, 50 wt. % suspension in water (Ref. Aldrich)
  • 10.  Polymer solution  Colloidal Silica suspension  Take different proportions of the solutions using micro-pipette  Mix them in a culture bottle  Shake the bottle to observe the formation of gel  Repeat the experiment for various concentrations
  • 11.  Glassware should be properly cleaned and sterilized in ovens or using nitrogen vents  Store the micro pipette vertically to prevent liquids from running inside the shaft of the pipette.  Minimize the exposure time for PVP while weighing, as it can gain weight by absorbing atmospheric water  Should wear goggles and potentially lab aprons
  • 12. Table 2: Colloidal Silica data from manufacturer (Aldrich)and PVP data from (Ashland_Inc) Material Density (g/ml) @ 25oC Silica 50% 1.4 PVP 02% 1.008 PVP 10% 1.02 PVP 30% 1.07
  • 13. By Volume By Weight Inference 2 % PVP 50 %Silica 2 % PVP 50 %Silica 1 1 1.008 1.4 Very less viscous mixture 10 % PVP 50 %Silica 10 % PVP 50 %Silica 1 1 1.02 1.4 viscous liquid 1 3 1.02 4.2 more viscous 1 6 1.02 8.4 more viscous 30 % PVP 50 %Silica 30 % PVP 50 %Silica 2 1 2.14 1.4 very high viscous 4 3 4.28 4.2 Some gel is formed 1 1 1.07 1.4 Some gel is formed 1 3 1.07 4.2 Shake gel 1 7 1.07 9.8 Shake gel
  • 15.
  • 16.
  • 17.  The structure of the gel formed can be studied using IR spectroscopy, SEM, DLS and other relevant techniques  The rheological properties likeVisco-elasticity of the gel can be studied with changing the polymer and silica proportions.
  • 18.  The gelation that occurred upon shaking the solution rigorously has contribution of both reversibly and irreversibly adsorbed polymer particles.  When left to settle, a part of polymer desorbs and this can be attributed to reversible gelation  A number of experiments were conducted using different concentrations, and proportions of PVP with 50% colloidal silica.
  • 19.  Experiments were also conducted using PVA as polymer. Since, 20% PVA solution formed a very viscous fluid, PVP was considered for further experiments  Using 30% PVP and 50% Silica in 1:1 volume proportions, a near gel was formed.  So, different proportions of these mixtures were tried and a near shake gel is finally obtained.  Increasing the proportion of silica particles led to the formation of better shake gels.This also supports the mechanism of reversible gelation.
  • 20.  Belyakova, L.A., Anatoly M.Varvarin, DianaY. Lyashenko, & NadiyaV. Roik. (2003). Study of interaction of poly(1-vinyl-2-pyrrolidone) with a surface. Colloid Interface Sci., 264, 2–6.  Spinde, K., Konstantinos Pachis, JoannaAntonakaki, & Silvia. (2011). Influence of Polyamines and Related Macromolecules on Silicic Acid Polycondensation: Relevance to “Soluble Silicon Pools”? Chemistry of Materials, 4676–4687.  Toki, M.,TY Chow,T Ohnaka, H Samura, &T Saegusa. (1992). Structure of poly (vinylpyrrolidone)-silica hybrid. Polymer Bulletin, 36.  Aldrich, S. (n.d.). LUDOX®TM-50 colloidal silica. Retrieved Nov 10, 2012, from http://www.sigmaaldrich.com/catalog/product/aldrich/420778?lang=en&regio n=IN  Ashland_Inc. (n.d.). IspCorp. Retrieved Nov 10, 2012, from http://online1.ispcorp.com/Brochures/Performance%20Chemicals/PVP.pdf

Notes de l'éditeur

  1. It is soluble in water and other polar solvents. Being a branched polymer, it is extensively used as a binder in many pharmaceutical, adhesive industries.