Analytical ultracentrifugation of polymers and nanoparticles / Walter Mächtle, Lars Börger.

Format:

Book

Author/Creator:

Mächtle, Walter.

Contributor:

Börger, L.

Class of 1939 Fund.

Series:

Springer laboratory

Language:

English

Subjects (All):

Ultracentrifugation.

Polymers--Analysis.

Polymers.

Nanoparticles--Analysis.

Nanoparticles.

Physical Description:

xiii, 237 pages : illustrations ; 25 cm.

Place of Publication:

Berlin ; New York : Springer, [2006]

Summary:

Analytical ultracentifugation (AUC) is a powerful method for the characterization of polymers, biopolymers, polyelectrolytes, nanoparticles, dispersions and other colloidal systems. The method is able to determine the molar mass, the particle size, the particle density and interaction parameters like virial coefficients and association constants. Because AUC is also a fractionation method, the determination of the molar mass distribution, the particle size distribution and the particle density distribution is possible. A special technique, the density gradient method, allows fractionating heterogeneous samples according to their chemical nature that means being able to detect chemical heterogeneity. The book is divided into seven chapters concerning the history and basic theory, instrumentation, sedimentation velocity runs, density gradient runs, sedimentation equilibrium runs, application examples and possible future developments. In particular, the detailed application chapter demonstrates the versatility and power of AUC by means of many interesting and industrial important examples. Thus the book concentrates on practical aspects rather than details of centrifugation theory. Both authors have decades of experience in an industrial AUC research laboratory of a world leading chemical company.

Contents:

1.1 Historic Examples of Ultracentrifugation 2

1.1.1 Investigations on Gold Colloids in 1924 3

1.1.2 Investigations on the Structure of DNA in 1957 5

1.2 Basic Theory of Ultracentrifugation 7

1.2.1 Svedberg's Simplified Theory 8

1.2.2 Derivation of Lamm's Equation 10

1.3 Basic Experiment Types of Ultracentrifugation 12

1.3.1 Sedimentation Velocity Experiment 12

1.3.2 Synthetic Boundary Experiment 13

1.3.3 Sedimentation Equilibrium 13

1.3.4 Density Gradient 14

1.3.5 Approach-to-Equilibrium (or Archibald) Method 15

2 Analytical Ultracentrifugation, Instrumentation 17

2.1 Ultracentrifuges 18

2.1.1 The Beckman-Coulter Optima XL-A/I 19

2.1.2 User-Made Centrifuges 21

2.2 Rotors 25

2.3 Measuring Cells 26

2.4 Detectors 29

2.4.1 Absorption Optics 31

2.4.2 Interference Optics 34

2.4.3 Schlieren Optics 37

2.4.4 Other Detectors 38

2.5 Multiplexer 43

2.6 Auxiliary Measurements 43

2.6.1 Measurement of the Solvent Density and the Partial Specific Volume 43

2.6.2 Measurement of the Refractive Index and the Specific Refractive Index Increment 45

3 Sedimentation Velocity 47

3.2 Basic Example of Sedimentation Velocity 47

3.2.1 Determination of s 50

3.2.2 Standard Conditions for s Estimation 51

3.2.3 Radial Dilution and Thickening 52

3.2.4 Concentration Dependence 53

3.3 Advanced Theory of Sedimentation Velocity Runs 54

3.3.1 Johnston-Ogston Effect 54

3.3.2 Self-Sharpening of Boundarie 55

3.3.3 Pressure Dependence 55

3.3.4 Speed Dependence 56

3.3.5 Charge Effects 57

3.3.6 Separation of Sedimentation and Diffusion 58

3.3.7 Test of Homogeneity 61

3.4 Sedimentation Velocity Runs of Macromolecules to Measure Average M and MMD 62

3.4.1 Evaluation of the Average Molar Mass M by Sedimentation Velocity Runs via Scaling Laws 62

3.4.2 Evaluation of Molar Mass Distributions (MMD) by Sedimentation Velocity Runs via Scaling Laws 64

3.5 Sedimentation Velocity Runs on Particles to Measure Average d[subscript p] and PSD 69

3.5.1 Particle Size Distribution via AUC Turbidity Detector and Mie Theory 70

3.5.2 Coupling Technique to Measure very Broad PSD 77

3.5.3 H[subscript 2]0-D[subscript 2]0 Density Variation Method to Measure Particle Densities via Sedimentation Velocity Runs 80

3.5.4 PSD Measurement of very Small Platinum Clusters Using UV Optics 84

3.6 Synthetic Boundary Experiments 86

3.6.1 Synthetic Boundary Crystallization Ultracentrifugation 93

4 Density Gradients 97

4.2 Static Density Gradients 101

4.2.1 Theory of Static Density Gradients 102

4.2.2 Gradient Materials 115

4.2.3 Experimental Procedure 117

4.3 Dynamic Density Gradients 120

4.4 Other Types of Density Gradients 125

4.4.1 Percoll Density Gradient 125

5 Sedimentation Equilibrium 131

5.2 Experimental Procedure 133

5.3 Data Analysis 138

5.3.1 Basic Equations for Molar Mass Averages - Classical Evaluation of AUC Equilibrium Runs 138

5.3.2 Basic Equations for Molar Mass Distributions - Nonlinear Regression Evaluation (Lechner Method) 141

5.3.3 Application of the Basic Equations - Classical and Nonlinear Regression Evaluation 144

5.3.4 M-STAR, a Special Data Analysis to obtain M[subscript w] 149

5.4.1 Absorption Optics Examples of a Polyelectrolyte and Calibration Polystyrene NBS 706 152

5.4.2 Association Equilibrium Example and AUC Buoyant Density Method to Determine [Characters not reproducible] 155

5.4.3 The New Fluorescence Detector of Laue Used for Green Fluorescent Protein 158

5.5 Further AUC Methods to Measure Molar Masses 159

6 Practical Examples of Combination of Methods 163

6.1 Combination of Different AUC Methods 163

6.1.1 Core/Shell Particles 163

6.1.2 Characterization of Microgels and Nanogels 170

6.1.3 Ion Exchange in Carboxylated Latices 179

6.2 Combination of AUC with Other Techniques 189

6.2.1 AUC and SFFF 190

6.2.2 AUC and EM 198

6.3 Literature Examples: AUC and Nanoparticles 212

7 Recent Developments and Future Outlook 215

7.1 New AUC Instrumentation and Detectors 216

7.2 New AUC Methods 222

7.3 New AUC Data Analysis 228.

Notes:

Includes bibliographical references and index.

Local Notes:

Acquired for the Penn Libraries with assistance from the Class of 1939 Fund.

ISBN:

3540234322

OCLC:

64571899

Publisher Number:

9783540234326