4(%3)3 - Ecole nationale supÃ©rieure de chimie de Montpellier

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The AFM instrumentation and its specifications remains the same as mentioned in the firstsection. The membranes with absorbed BSA protein molecules were detached from non-wovenfabric and then placed delicately onto small Silicon wafers for analysis. To avoid the samplecontamination and distortion, the drying was carried out in the same manner as described before.8.2.5 Concentration Calibration for Poly(styrene) & Silica NanoparticlesSince the membranes were susceptible to clogging due to possible high concentration ofnanoparticles hence optimum concentrations for both Polystyrene and Silica nanoparticles byobtaining the calibration curves using Photon Cross Correlation Spectroscopy (PCCS) (Nanophox®).In case of Polystyrene, a mother solution of Poly(styrene) latex beads (Sigma-Aldrich®, 10 wt%, 10148 M.W.) was prepared in ultrapure water (0.1146 g in 20 g water). A small part of thissolution taken in crown glass vial and analyzed using PCCS to obtain the particle size distributioncurve and the corresponding average intensity value (Kcps; Kilo Counts Per Second). The remainingsolution was then subsequently diluted with ultrapure water (MilliQ®) and analyzed using PCCS toobtain the average intensity values (Table – 8.2).S.No.Amount ofMotherSolution taken(g)Amount ofWater Added(g)Amount of Poly(styrene)(g)Concentration(g/ml) X 10 -8AverageKcps1 5.01* 5.0047 4.53916E-08 0.45325 17.952 5.06** 5.0025 1.81204E-07 1.80078 33.753 0.025 10.2454 7.16221E-07 6.97365 56.54 0.0509 10.18 1.45823E-06 14.2532 129.455 0.0999 9.9992 2.86202E-06 28.3394 259.26 0.2001 10.0511 5.73263E-06 55.9216 481.457 0.3011 10.039 8.62617E-06 83.4245 497.458 0.4021 10.0519 1.15197E-05 110.194 959.19 0.5007 10.0154 1.43445E-05 136.405 1299.7Tablee – 8.2: The absolute concentrations of poly(styrene) nanoparticles solutions with their corresponding Kcpsvalues as obtained from Photon Cross Correlation Spectroscopy to obtain concentration calibration curve. ** means5.06 g of solution was taken from solution no. 3, * denotes that 5.01 g of solution was taken from solution no. 2.In case of silica, the mother solution was prepared starting with 0.0012 g of silica dispersedinto 4.0036 g of ultrapure water. For a uniform homogeneous solution, the vial containing the147
solution was ultrasonicated for 15 minutes before being analyzed using PCCS. The ultrasonicationstep extends the time window in which PCCS measurements can be performed effectively beforethe silica nanoparticles settles at the bottom of the vial. The situation gets less pronounced as theconcentration decreases with further dilutions. However the ultrasonication step was performed foreach diluted solution (Table – 8.3).SP1SP2Concentration Average Concentration Average(g/ml) X 10 -5 Kcps (g/ml) x 10 -5 Kcps30 926,69 7 223.949.86 289,47 3.48 103.910.934 33,45 1.78 661.46 520.843 47.45Tablee – 8.3: The absolute concentrations of silica nanoparticles (SP1 & SP2) solutions with their correspondingKcps values as obtained from Photon Cross Correlation Spectroscopy to obtain the concentration calibration curve.8.2.6 Preparation of Feed Solutions of Nano-Objects for TranslocationThe Poly(ethylene glycol) (PEG) feed solution was prepared by weighing 0.25 g each ofdifferent PEGs ( 35 KDa, 100 KDa, 200 KDa and 400 KDa) ( Sigma-Aldrich®, 99.5 %) and dissolving inultrapure water to obtain a 1g.L -1 solution. This feed solution was first analyzed in terms of refractiveindex using refractive index detector (Water® 2440) of Gel Permeation Chromatography technique(Waters Corporation®).The Bovine Serum Albumin (BSA, Aldrich, >96%) solution was prepared at a concentration of1.5 mg.ml -1 in Phosphate buffered saline solution. The feed solution was analyzed by UV-VisSpectrometry at a wavelength 280 nm. The concentration could then be estimated from thefollowing calibration curve.An aqueous solution of Polystyrene particles (0.1146 g in 20 g of water) was further dilutedwith 200 ml of ultrapure water and the resulting solution was used as feed solution for Polystyrenetranslocation.For both series of silica particles, two 100 ml solutions were prepared containing 0.0024 g ofSP1 and SP2 silica particles respectively. Both the solutions were ultrasonicated for 1 hour.148
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THESISPRESENTED ATNATIONAL GRADUATE
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As the human civilization progress
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CHAPTER - 1 SELF-HEALING POLYMERIC
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8.1.5 Atomic Force Microscopy …
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Synthetic engineering materials in
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esponse to a specific external stim
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The first work based on this approa
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een prepared from urea-formaldehyde
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monomer systems. The addition of EN
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Figure - 1.10: Self-healing process
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was required to reach healing effic
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In addition to above works, some ot
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that have been identified to be tak
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part of the chapter, these material
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Figure - 1.17: Self-healing of the
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commercialized under tradenames; Nu
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joined together at temperature high
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Inspired by these findings, the fir
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temperature greater than 80 o C in
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Figure - 1.27: Sulfur chemistry bas
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A different kind of sulfur chemistr
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Figure - 1.29: Dynamic covalent che
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cracks. The recovered droplets afte
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23 White, S. R. et al. Autonomic he
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65 Taber, D. F. & Frankowski, K. J.
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107 Kushner, A. M., Vossler, J. D.,
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148 Park, J. S., Kim, H. S. & Hahn,
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The value of subscripts “n”,
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The formation of spherical micelles
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the micelle assembly showed the pre
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gain onto the electrodes by buildin
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The resistance R can be further exp
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empty-tower velocity U only depends
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This apparent morphological switchi
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In a further qualitative analysis,
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noteworthy and though its feasibili
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Furthermore within this range, lowe
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Figure - 2.22: Scanning Electron Mi
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While the resistance measurements g
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In conclusion, a self-healing membr
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23 Giacomelli, F. C., Riegel, I. C.
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micelles enabled the membrane to se
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The second class is represented by
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To avoid the probable clogging of t
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181614SP2 - iNumber of Particles121
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1000900800y = 3E+06xR² = 0,9911y =
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very high value of 1.5 g.l -1 . Thi
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Since the only change in the membra
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100Retention (%)8060400,100,20,40,6
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Figure - 3.18: Scanning Electron Mi
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(Figure - 3.20). A cursory look at
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When compared to poly(styrene) NPs,
Page 108 and 109: Figure - 3.24: Scanning Electron Mi
Page 110 and 111: REFERENCES1 Metzler, R. & Klafter,
Page 112 and 113: 46 Bemporad, D., Luttmann, C. & Ess
Page 114 and 115: In this chapter, preparation of 3D
Page 116 and 117: obtain complex macromolecular archi
Page 118 and 119: The polymerization was conducted at
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Page 122 and 123: mg/ml),the micelles’ hydrodynamic
Page 124 and 125: Figure - 4.15: The monolayer and mu
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Page 128 and 129: The presence of the dispersed micel
Page 130 and 131: Heating the multilayer micelle asse
Page 132 and 133: stable zipping of the micelles. Mul
Page 134 and 135: 24 Moad, G., Rizzardo, E. & Thang,
Page 136 and 137: The concept of nano-gel based self-
Page 138 and 139: Figure - 5.4: Size distribution of
Page 140 and 141: In a typical process, the two compo
Page 142 and 143: Figure - 5.10: 1HNMR spectra obtain
Page 144 and 145: The 1 HNMR spectrum obtained for th
Page 146 and 147: REFERENCES1 White, S. R. et al. Aut
Page 148 and 149: healing ability shown by the membra
Page 150 and 151: 7. PERSPECTIVESBeing the first such
Page 153 and 154: 8. MATERIALS & METHODSThis chapter
Page 155 and 156: 8.1.3 PEG Filtration MeasurementsTh
Page 157: addition of TEOS due to formation o
Page 161 and 162: Triethylamine (TEA) (Sigma-Aldrich
Page 163 and 164: To prepare the monolayer assembly o
Page 165 and 166: was added followed by addition of 0
Page 168 and 169: ELABORATION OF SELF-HEALING POLYMER
Page 170 and 171: ELABORATION DES MEMBRANES POLYMERES
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4(%3)3 - Ecole nationale supÃ©rieure de chimie de Montpellier

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