Determination of molecular weights and polydispersity of high polymers:
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1964
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adam_text | ACADEMY OF SCIENCES OF THE USSR
SR RAFIKOV,
S A PAVLOVA and I I TVERDOKHLEBOVA
Determination of
Molecular Weights and Polydispersity
of High Polymers
Israel Program for Scientific Translations
Jerusalem 1964
TABLEOFCONTENTS
EXPLANATORY LIST OF ABBREVIATIONS viii
INTRODUCTION 1
Chapter I THE CONCEPT OF THE MOLECULE AND MOLECULAR
WEIGHT OF HIGH-MOLECULAR COMPOUNDS 3
1 The Polydispersity of High-Molecular Compounds and Its
Influence on the Average Values of Molecular Weights 5
2 The Influence of Low-Molecular Admixtures on the Average
Values of Molecular Weight 11
3 Special Features of Solutions of Polymeric Substances 13
BIBLIOGRAPHY 18
Chapter II FRACTIONATION OF HIGH-MOLECULAR COMPOUNDS 19
t
1 Fractional Precipitation 26
(a) Fractional precipitation by evaporation of solvent 39
(b) Fractional precipitation by decreasing the tempera
ture of the solution 41
2 Fractional Dissolution 43
3 Chromatographic Fractionation 50
4 Fractionation by Distribution between Two Immiscible Solvents 56
5 Polymer Fractionation by Thermal Diffusion 58
6 Turbidimetric Titration 61
7 Treatment of Results 63
BIBLIOGRAPHY 80
Chapter III LIGHT SCATTERING 86
1 Introduction 86
(a) Light scattering by molecules which are small in
comparison with the 1 Lght wavelength 87
(b) Light scattering by particles of dimensions compa
rable to the wavelength of the light 90
(c) Determination of polydispersity from light
scattering data 96
2 Experimental Procedure and Instruments 99
(a) The preparation of the solutions 99
(b) Nephelometers 103
(c) Cells and thermostats 118
3 Corrections 121
(a) Correction for light absorption by the solution 121
(b) Correction for the fluorescence of the solution 122
(c) Correction for the refractive index 122
(d) Volume correction factor 123
BIBLIOGRAPHY 128
Chapter IV DIFFUSION METHOD 130
1 Calculation of the Diffusion Coeffi cient 133
(a) The method of maximum ordinate 133
(b) The method of moments 133
2 Experimental Methods 134
(a) Diffusion cells 134
* (b) Optical recording methods 136
BIBLIOGRAPHY 141
Chapter V ULTRA CENTRIFUGE SEDIMENTATION METHOD 142
1 Ultracentrifuges 144
(a) General information 144
(b) Rotor 147
(c) Cells 148
2 The Calculation of the Sedimentat ion Constant and of
Molecular Weight 150
(a) Measurement of sedimentation velocity 151
(b) The method of sedimentation equilibrium 154
(c) Non-equilibrium method 155
3 The Estimation of the Polydispersity 159
(a) Calculating the distribution curves 160
(b) The average values of th i molecular weight and
polydispersity 165
4 The Dependence of the Sedimentation Constant on the
Concentration 166
BIBLIOGRAPHY 167
Chapter VI OSMOMETRY 169
1 Introduction 169
2 Osmotic Method 170
3 The Influence of the Nature of the Solvent and of the
Concentration of the Polymer Solution on the Osmotic
Pressure (Second Virial Coefficient A2) 171
4 Osmometers 172
(a) Osmometers with a horizontal membrane 174
(b) Osmometers with vertical membranes 177
(c) Other osmometers 187
(d) Osmotic balance 196
5 General Information on Membranes 201
(a) Preparation and treatment of membranes 205
(b) The application of membranes to special purposes 211
(c) Membrane porosity and permeability 212
(d) Membrane swelling 218
(e) The optimum number of membranes, their diameter
and the volume of the cell 219
t
6 Errors in Osmometry 219
(a) Adsorption of material on the membrane 219
(b) Membrane asymmetry 220
(c) Sagging (balloon effect) 221
(d) Partial drying of membrane while the osmometer
is being filled 222
(e) Evaporation of solvent 222
(f)Osmometerswithlooseseals223
(g) Air bubbles in the osmometer 223
(h) Diffusion of the dissolved material through the
membrane 223
7 The Accuracy of the Osmometric Method 224
BIBLIOGRAPHY 225
Chapter VII EBULLIOSCOPIC, CRYOSCOPIC AND ISOPIESTIC METHODS 228
1 Introduction 228
2 Ebullioscopy 233
(a) Ebullioscopes 235
(b) Parts of the ebullioscopes 249
(c) Errors in ebullioscopy 251
3 Cryoscopy 255
(a) Cryoscopes 255
(b) Introducing the sample into the cryoscope 262
4 Anomalous Effects in Cryoscopy and Ebullioscopy 263
5 Isopiestic Method 263
(a) Micro- and macromethods of molecular weight
determination 263
(b) Other methods 270
BIBLIOGRAPHY 271
CHapter VIII MOLECULAR WEIGHT DETERMINATION BY END
GROUP ASSAY 273
1 Determination of Carboxyl Groups 278
2 Determination of Amino Groups or the Combined
Determination of Amino and Carboxyl Groups 284
3 Determination of Hydroxyl Groups 288
4 Determination of Aldehyde Groups 296
5 Extermination of Other Terminal Groups 297
BIBLIOGRAPHY 300
Chapter IX VISCOMETRY 302
1 Viscosity of Polymer Solutions 302
(a) Dependence of viscosity on the molecular weight
of the polymer 302
(b) Viscometric evaluation of polydispersity 310
(c) Effect of rate of shear on solution viscosity 311
(d) Anomalies in the concentration dependence of
viscosity at high dilutions 317
2 General Information on Viscometers and Manostats 322
(a) Viscometers 322
(b) Manostats 330
3 General Information about Thermostats 332
BIBLIOGRAPHY 334
Chapter X METHODS OF WEIGHT DETERMINATION OF LINEAR
POLYMERS, BASED ON THE STUDY OF THEIR
VARIOUS PHYSICAL PROPERTIES 337
1 Molecular Weight Determination of Amorphous Linear
Polymers by Their Pour Point 337
2 Molecular Weight Determination from Relaxation Data 338
, 3 Determination of the Molecular Weight of a Polymer by
Its Viscosity 340
4 Determination of the Molecular Weight of High Polymers
by Means of Dynamic Mechanical Measurements 341
5 Determination of the Molecular Weight of Polymers by
Spectroscopic, Election-Microscope and Other Physical
Investigations 343
BIBLIOGRAPHY 344
APPENDIX The Constants K and a in the equation 345
BIBLIOGRAPHY 354
t
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spelling | Rafikov, Sagid R. Verfasser aut Determination of molecular weights and polydispersity of high polymers 1964 txt rdacontent n rdamedia nc rdacarrier HEBIS Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=018229071&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis |
spellingShingle | Rafikov, Sagid R. Determination of molecular weights and polydispersity of high polymers |
title | Determination of molecular weights and polydispersity of high polymers |
title_auth | Determination of molecular weights and polydispersity of high polymers |
title_exact_search | Determination of molecular weights and polydispersity of high polymers |
title_full | Determination of molecular weights and polydispersity of high polymers |
title_fullStr | Determination of molecular weights and polydispersity of high polymers |
title_full_unstemmed | Determination of molecular weights and polydispersity of high polymers |
title_short | Determination of molecular weights and polydispersity of high polymers |
title_sort | determination of molecular weights and polydispersity of high polymers |
url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=018229071&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
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