Material Characteristics
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1 Material Characteristics technology: domains interface body surface supermolecular structures hydro colloids chemistry: states crystalline amorphous gel / glass dissolved
2 Starch: granules formed by molecules Serge Perez, CNS Grenoble, F / Eric Bertoft, Abo Akademi Univ, Turku / SF CePoL/MC Central Polymer Lab / Molecular Characteristics
3 Aldoses aldo-triose, aldo-tetraoses, aldo-pentoses, aldo-hexoses Carbohydrates Ketoses keto-triose, keto-tetraoses, keto-pentoses, keto-hexoses cyclic form: hemi-acetals cyclic form: hemi-ketals polymerization: formation of (full)acetals / (full)ketals by glycosidic linkages
4 1 4 α-d-glcp- (1 4)-α-D -Glcp α-d-glycopyranosyl- (1 4)-α-D -glucopyranose ( maltose ) Polysaccharides: Made by Nature glycosidic linkage α-d-glcp- (1 2)-β-D -Fruf α-d-glucopyranosyl- (1 2)-β-D -fructofuranosid ( sucrose )
5 basic α(1 4) linked glycosyl residue Polysaccharides: Made by Nature N C n n modified unimers C6-position uronic acid 3 C oxidation / substitution / C2-position glucosyl-2-n-acetyl C n 3 C C n oxidation / C2-position acetate oxidation / substitution / C4-position glycosyl-4-sulfate S n oxidation / C2-position glucosyl-2-amine P N 2 n n oxidation / C6-position glucosyl-6-phosphate
6 Symmetry / conformation of starch glucans αd(1 4)-glucans + α(1 6) Glcx branches 4)-αD-Glcp-(1 4)-αD-Glcp-(1 non-branched starch component nb-glucans / amylose-type lcb / scb glucans / amylopectin-type (long-chain-branched / short-chain-branched) helical conformation irregular / globular conformation P n CePoL/MC Central Polymer Lab / Molecular Characteristics oxidation / C6-position glucosyl-6-phosphate
7 Starch glucan populations a1t8 a1t7 a1t6 a1t5 a1t4 a1t3 a1t coherence lenghts [nm] homogeneous scb glucan cereal starch amaranth up to C in DMS a1t w1t8 w1t7 w1t6 w1t5 w1t4 w1t3 w1t radius [nm] scb + lcb heterogeneous glucan cereal starch wheat up to C in DMS w1t1
8 Managing eterogeneity by Fractionation LC affff/ AF4 S k kt md: V e lg(m) SEC PLC mc: CCD lcb, scb separation coefficient Entropy controlled separation ( S/k) due to differences in excluded volume (V e ) Size Exclusion Chromatography (SEC) Diffusion mobility controlled separation due to 1st approach: differences in excluded volume (V e ) asymmetric flow field flow fractionation (affff or AF4)
9 Distributions and Mean values by Separation and Detetection
10 asymmetric Field Flow Fractionation: AF4 objects are separated according to differences in their diffusion coefficient / difusive mobility
11 Diffusive Mobilty D T ydrodynamic adius h Stokes-Einstein: D T from retention times (t r ) of AF4 D = ( t 0 F cr 0 6V w 2 ) 1 t r h = kt 6πη D t 0 (void time), F cr (cross-flow), w (channel thickness), V 0 (void volume) and t r (retention time) T (temp), k (Boltzmann const), η (intrinsic visc)
12 Light Scattering Detection: Scattering vs. Spectroscopy probing soft matter by radiation (typically electromagnetic, but also neutrons). The electromagnetic radiation introduces dipole oscillations. Part of the energy will be absorbed when close to resonance spectroscopy Any acceleration of charges leads to emission of secondary radiation scattering field. Analysis of the scattered field provides information about local structure (due to interference) and mobility (time dependence of the signal) of the sample At short wavelengths (X-rays) we are far above most resonance frequencies (spectroscopy), all electrons are polarized and emit a secondary wave, i.e. the signal will depend on the electron density At much larger wavelengths (visible light) we are below most resonances, but we only polarize the valence electrons. The polarizablility is a function of the wavelength and is related to the refractive index.
13 Static and Dynamic Scattering
14 Scattering facts Zimm plot 4 π Θ q =. sin λ 2 q = K. c. M. P q K. c 1 1 =. + 2 A2. c Θ PΘ Mw x-axis: sin 2 (Θ/2) + k c q 2 + k c y-axis: K c / Θ intercept: 1 / M w slope (q 2 0): g slope (c 0): A 2
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