Handbook of Size Exclusion Chromatography and Related ...

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35. M Souaille, H Fischer. Kinetic conditions for living and controlled free radical polymerizations mediated by reversible combination of transient propagating and persistent radicals: the ideal mechanism. Macromolecules 33:7378–7394, 2000. 36. NA Listigovers, MK Georges, PG Odell, B Keoshkerian. Narrow-polydispersity diblock and triblock copolymers of alkyl acrylates by a “living” stable free radical polymerization. Macromolecules 29:8992–8993, 1996. 37. S Grimaldi, JP Finet, F Le Moigne, A Zehdaoui, P Tordo, B Benoit, M Fontanille, Y Gnanou. Acyclic-phosphonylated nitroxides: a new series of counter-radicals for “living”/controlled free radical polymerization. Macromolecules 33:1141–1147, 2000. 38. DH Salomon, E Rizzardo, P Cacioli. Polymerization process and polymers produced thereby U.S. Patent 4,581,429, 1985. 39. A Goto, T Fukuda. Kinetic study on nitroxide-mediated free radical polymerization of tert-butyl acrylate. Macromolecules 32(3):618–623, 1999. 40. F Chauvin, AM Alb, D Bertin, P Tordo, WF Reed. Kinetics and molecular weight evolution during controlled radical polymerization. Macromol Chem Phys 203:2029– 2041, 2002. 41. G Odian. Principles of polymerization. 3rd ed. New York: John Wiley & Sons, 1991. 42. H Çatalgil-Giz, A Giz, AM Alb, A Öncül Koç, WF Reed. Online monitoring of composition, sequence length, and molecular weight distributions during free radical copolymerization, and subsequent determination of reactivity ratios. Macromolecules 35:6557–6571, 2002. 43. FR Mayo, FM Levis. Copolymerization I. A basis for comparing the behavior of monomer in copolymerization; the copolymerization of styrene and methyl methacrylate. J Am Chem Soc 66:1594–1601, 1944. 44. S Duc, A Petit. Copolymerization of phenylacetylene and 1-hexyne using Ziegler– Natta and methathesis catalyst systems: copolymer compositions and reactivity ratios by 1 H NMR spectroscopy. Polymer 40:589–597, 1999. 45. W Buschuk, H Benoit. Light scattering studies of copolymers. 1. Effect of heterogeneity of chain composition on the molecular weight. Canadian J Chem 36:1616–1626, 1958. 46. WH Stockmayer, LD Moore, M Fixman, BN Epstein. Copolymers in solution. 1. Preliminary results for styrene-methyl methacrylate. J Polym Sci 16:517–530, 1955. 47. A Faldi, JBP Soares. Characterization of the combined molecular weight and composition distribution of industrial ethylene/a-olefin copolymers. Polymer 42:3057–3066, 2001. 48. Y Feng, JN Hay. The measurement of compositional heterogeneity in a propylene– ethylene block copolymer. Polymer 39:6723–6731, 1998. 49. WH Stockmayer. Distribution of chain lengths and compositions in copolymers. J Chemical Phys 13:199–207, 1945. 50. TE Patten, K Matyjaszewski. Copper(I) catalyzed atom transfer radical polymerization. Acc Chem Res 32:895–903, 1999. 51. F Candau, J Selb. Hydrophobically modified polyacrylamides prepared by micellar polymerization. Adv Colloid & Interface Sci 79:149–172, 1999. © 2004 by Marcel Dekker, Inc.
52. M Hulden. Hydrophobically modified urethane–ethoxylate associative thickeners: rheology of aqueous solutions and interactions with surfactants. Colloids and Surfaces A82:263–277, 1994. 53. E Larson. Method for producing polymers using micellar polymerization. U.S. Patent 6,127,494, 2000. 54. WF Reed. Time dependent light scattering from singly and multiply stranded linear polymers undergoing random and endwise scission. J Chem Phys 103(17): 7576–7584, 1995. 55. JL Ganter, WF Reed. Real time monitoring of enzymatic hydrolysis of galactomannans. Biopolymers 59:226–242, 2001. 56. S Ghosh, WF Reed. New light scattering signatures from polymers undergoing depolymerization with application to proteoglycan monomer degradation. Biopolymers 5:435–450, 1995. 57. Kinetics of aggregation and gelation. In: FF Family, DP Landau, eds. Amsterdam: Elsevier Science Publishers, 1984. 58. JW Cahn, JE Hilliard. Free energy of a non-uniform system. J Chem Phys 28:258–267, 1958. 59. F Brochard, PG De Gennes. Kinematics of polymer dissolution. Physicochem Hydrodynam 4:313–321, 1983. 60. MF Herman, SF Edwards. A reptation model for polymer dissolution. Macromolecules 23:3662–3667, 1990. 61. A Parker, F Vigouroux, WF Reed. The dissolution kinetics of polymer powders. Am Inst Chem Eng Journal 46:1290–1299, 2000. 62. NA Peppas, JC Wu, ED von Meerwall. Mathematical modeling and experimental characterization of polymer dissolution. Macromolecules 27:5626–5634, 1994. 63. S Ghosh, RM Peitzsch, WF Reed. Polyelectrolyte aggregates and other particles as the origin of the “extraordinary” diffusional phase. Biopolymers 32:1105–1122, 1992. 64. RG Smits, ME Kuil, M Mandel. Quasi-elastic light scattering study on solutions of linear flexible polyelectrolytes at low ionic strengths. Macromolecules 27: 5599–5608, 1994. 65. KS Schmitz. On the “filterable aggregates and other particles” interpretation of the extraordinary regime of polyelectrolytes. Biopolymers 33:953–959, 1993. 66. JP Wyatt. Light scattering and the absolute characterization of macromolecules. Analytica Chimica Acta 272:1–40, 1993. 67. R Strelitzki, WF Reed. Automated batch characterization of polymer solutions by static light scattering and viscometry. J Appl Polym Sci 73:2359–2368, 1999. 68. S Förster, M Schmidt. Polyelectrolytes in solution. Adv Polym Sci 120:53–133, 1995. 69. E Bayly, JL Brousseau, WF Reed. Continuous monitoring of the effect of changing solvent conditions on polyelectrolyte conformations and interactions. Int J Polymer Characterization and Analysis, in press. 70. GA Sorci, WF Reed. Electrostatically enhanced second and third virial coefficients, viscosity and interparticle correlations for linear polyelectrolytes. Submitted for publication. © 2004 by Marcel Dekker, Inc.
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MARCEL DEKKER Handbook of Size Excl
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CHROMATOGRAPHIC SCIENCE SERIES A Se
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60. Modern Chromatographic Analysis
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Preface to the Second Edition Gel p
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Preface to the First Edition Molecu
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Contents Preface to the Second Edit
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17. Size Exclusion Chromatography o
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James F. Curry Analytical Departmen
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Iwao Teraoka, Ph.D. Othmer Departme
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The graphical data display typicall
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polymer molecule can elute. The tot
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individual states) allowed to them.
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unsaturation while the IR detector
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Sampleconcentrationshouldbeminimize
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averagesdefinedintermsofthemolecula
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information regarding appropriate M
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Analytical. Two models, the KMX-6 a
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Figure 6 Overlay of time-sliced pea
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accurately for very large and very
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4 GENERAL REFERENCES The interested
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46. TA Chamberlin, HE Tuinstra. US
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materials are commercially availabl
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Table 1 Commercial Column Packing M
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necessarily comparable. For this re
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adjusted such that the pore size di
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narrowmolecular weight range, indiv
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Figure 8 Effect of particle size on
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Figure 9 SEC calibration using poly
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Table 4 Typical Eluent Systems for
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Figure 12 Analysis of poly-2-vinyl
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24. E Meehan, S O’Donohue. The ro
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into accepted laboratory techniques
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Table 1 Trace Metal Impurities in C
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mass and biological activity, for m
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Experimental efficiency vs. velocit
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Table 3 Properties of SEC Silica Ge
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operate at aflow rate that can easi
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Figure 3 Efficiency of amide-bonded
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mechanically stable packing materia
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Figure 5 Pore size distributions of
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Figure 6 Separation of polystyrenes
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60-120 A ˚ are large enough to be
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Table 6 Selected Silica-Based Colum
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Table 7 Separation Ranges for Polym
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the decline in permeability is perm
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sample components can be varied by
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Figure 10 Diol bonding reactions. I
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ecause of the higher relative molec
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valuesfork1,k2,anda,theunknownmolec
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water-soluble and detergent-soluble
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the importance of secondary retenti
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discussed in Table 8(33). Based on
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individual dispersion processes ins
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The detector time constant can dist
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5.3 Mobile Phase A mobile phase is
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less steep and still linear at high
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35. P Bristow, J Knox. Chromatograp
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112. K Gooding, K Lu, G Vanecek, F
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for branched polymers or copolymers
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Figure 1 “Bridge design” flow-r
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Figure 3 A light-scattering photome
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Figure 5 SEC universal calibration
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where hn is the hydrodynamic volume
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It should be noted that dn=dc also
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sensitivity for many samples compar
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that is, log[h] vs. logM,generated
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Figure 8 Effect of band broadening
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Table 1 Measurement of Molecular We
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Figure 10 Differential refractomete
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Figure 11 (A) Mark-Houwink plot of
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Table 3 Measurement of Molecular We
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size information is derived from un
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Table 5 Molecular Weight Distributi
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By measuring the scattered intensit
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8 APPENDIX: INSTRUMENT COMPANIES 8.
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53. G Marot, J Lesec. J Liq Chromat
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125. D Slootmaekers, JAPP Van Dijk,
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200. JG Bindels, GJJ Bessems, BM De
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possibly with hydrodynamic volume (
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An insurmountable limitation of SEC
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to sDR(V) when either nPS ¼nPB ¼c
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1,4-trans;and8%1,2-vynil.TheglobalC
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The goal is to find the MWD and CCD
Page 167 and 168:
As expected, pS is closer to the no
Page 169 and 170:
Figure 3 Example 3: MWD and BD of a
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9. BH Zimm, WH Stockmayer. The dime
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45. RO Bielsa, GR Meira. Linear cop
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solubility properties. They are use
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determination of the absolute molec
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Figure 4 Result of the PBT analysis
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Figure 8 Result of natural spider s
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7 Size Exclusion Chromatography of
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As pointed out earlier, rubber must
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Table 2 Various Solvents and Operat
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Figure 2 Typical GPC calibrations w
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© 2004 by Marcel Dekker, Inc. Figu
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Natural and Synthetic Rubbe177 vari
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Another example, shown in Fig. 5 (3
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APPENDIX: SEC CONDITIONS FOR RUBBER
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Appendix (Continued) Polymer Column
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Page 203 and 204:
Page 205 and 206:
5. J West, E Rodriguez. Rubber Chem
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Page 209 and 210:
associate. Girdler (67) and Speight
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Table 1 Fractions Obtained Using Co
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Figure 1 SEC analyses of an aged as
Page 215 and 216:
Apparently more polar compounds are
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40% was fractionated into four frac
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Figure 7 SEC analyses of an unaged
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Figure 9 Comparison of percentage L
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Figure 11 Comparison of SEC chromat
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Figure 12 Comparisons of SEC chroma
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percentage LMS at the other locatio
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the total area into up to 12 sectio
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attempted to develop an SEC method
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parameterisbasedontheinternalpressu
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5 MODIFIED ASPHALTS The addition of
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Oxidation of the rubber and asphalt
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Figure 20 SEC chromatogram for an a
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Figure 21 Comparisons of apparent m
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© 2004 by Marcel Dekker, Inc. S/
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PS/10 4 þ 10 3 þ 500 þ 100 THF/1
Page 247 and 248:
Nevertheless, SEC of asphalts is es
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56. NW Garrick, RR Biskur. Trans Re
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Asphalts 235 122. M-S Lin, JM Chaff
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Page 255 and 256:
Table 1 Applications of Acrylamide
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(AM/AA), and acrylamide/dimethyldia
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polymer, a large size filter of 5,
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Figure 1 Size exclusion chromatogra
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Table3 MWandMWDofaBroad-MWDPAMStand
Page 265 and 266:
Another commercially available MW d
Page 267 and 268:
Table 5 Weight-Average Molecular We
Page 269 and 270:
Figure 6 (a) Size exclusion chromat
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compared to anormal product. By com
Page 273 and 274:
StudyingtheKineticsofaChemicalReact
Page 275 and 276:
this information, the higher MW pea
Page 277 and 278:
Page 279 and 280:
Page 281 and 282:
46. CJ Kim, A Hamielec, A Bendek. J
Page 283 and 284:
Page 285 and 286:
A relatively new technique utilizin
Page 287 and 288:
where ais the exponent of the Mark-
Page 289 and 290:
Figure 2 TDS chromatograms for full
Page 291 and 292:
Figure 5 Comparison of molecular we
Page 293 and 294:
Table 3 Summary of TDS Molecular We
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thepartiallyhydrolyzedPVAwiththecol
Page 297 and 298:
Table 5 Summary of Conformation and
Page 299 and 300:
a¼0.627andlog(K) ¼23.249.Theseare
Page 301 and 302:
The limits of detection of the PVA
Page 303 and 304:
Figure 12 PVAc broad molecular weig
Page 305 and 306:
4 SUMMARY Advances in SEC character
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Page 309 and 310:
2.1 Molecular Weight Grades of PVP
Page 311 and 312:
exclusion chromatography with low-a
Page 313 and 314:
weightandmolecularweightdistributio
Page 315 and 316:
© 2004 by Marcel Dekker, Inc. Figu
Page 317 and 318:
Figure 4 PEOcalibrationofUltrahydro
Page 319 and 320:
Figure 6 Overlay of GPC chromatogra
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plus Ultrahydrogel 120 A ˚ ,Shodex
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Figure 10 SEC traces of PVP/AA copo
Page 325 and 326:
Figure 11 Molecular weight distribu
Page 327 and 328:
Page 329 and 330:
2 CHEMICAL, MACROMOLECULAR AND MORP
Page 331 and 332:
Table 2 The Relative Composition of
Page 333 and 334:
considered to be 3. After the DS ha
Page 335 and 336:
een extensively studied by methods
Page 337 and 338:
The silylation was performed in LiC
Page 339 and 340:
observed using column materials hav
Page 341 and 342:
Table 6 (Continued) Packing materia
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4.5 Other Cellulose Derivatives Bes
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Table 8 SEC Conditions for Characte
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dextrans swell too much in cadoxen
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stirring at room temperature for an
Page 351 and 352:
Figure 2 MMDofunbleached(HP)andblea
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Figure 4 MMDofbirchkraftpulpdegrade
Page 355 and 356:
adequate when evaluating the influe
Page 357 and 358:
differential refractive index (DRI)
Page 359 and 360:
30. HA Krässig. Effects of structu
Page 361 and 362:
67. E Sjöholm, K Gustafsson, A Col
Page 363 and 364:
104. B Fleury, J Dubois, C Léonard
Page 365 and 366:
136. D Miller, D Senior, R Sutcliff
Page 367 and 368:
166. SS Cutié, CG Smith. Determina
Page 369 and 370:
200. R Berggren, F Berthold, E Sjö
Page 371 and 372:
13 Molar Mass and Size Distribution
Page 373 and 374:
measurements, and vapor pressure os
Page 375 and 376:
The calibration of SEC columns by c
Page 377 and 378:
The division according to eluent ty
Page 379 and 380:
Apolymer produced by UV irradiation
Page 381 and 382:
Because DMAC/LiCl is also agood sol
Page 383 and 384:
compoundsandwasexplainedbyadsorptio
Page 385 and 386:
isolated lignins because they are e
Page 387 and 388:
The Separon HEMA and Separon HEMA B
Page 389 and 390:
Figure 4 GPC elution curves of the
Page 391 and 392:
liquor is highest throughout the co
Page 393 and 394:
topological anisotropy in the polym
Page 395 and 396:
29. M Ristolainen, R Alen, J Knuuti
Page 397 and 398:
eds. Proc Int Symp 1998. Canton, Pe
Page 399 and 400:
92. L Jurasek. Towards a three dime
Page 401 and 402:
Table 1 Selected Industries Connect
Page 403 and 404:
into C3-metabolites, which then may
Page 405 and 406:
Table 4 Key Enzymes in the Biosynth
Page 407 and 408:
Table 5 Cloned Mutants of Starch En
Page 409 and 410:
Figure 3 Modeled x-ray diffraction
Page 411 and 412:
In the native environment (plant ce
Page 413 and 414:
Figure 6 (a) Large starch granules
Page 415 and 416:
number of branching points); crossl
Page 417 and 418:
Both absolute approaches are extrao
Page 419 and 420:
Table 7 (Continued) Approach Experi
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structures, excluded volumes, and t
Page 423 and 424:
Figure 10 (a) SEC elution profile o
Page 425 and 426:
Figure 12 Wheat glucans: DRI elutio
Page 427 and 428:
Figure 13 Wheat glucans. Normalized
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Figure 16 Wheat glucan. Normalized
Page 431 and 432:
Figure 18 Wheat glucan.Elution prof
Page 433 and 434:
Figure 20 Wheat glucans. Absolute m
Page 435 and 436:
Figure 22 Wheat glucan. (a) Intrins
Page 437 and 438:
Figure 24 Wheat PA-glucan. Elution
Page 439 and 440:
an Ubbelohde-viscometer for concent
Page 441 and 442:
Rheological investigations of stabi
Page 443 and 444:
shifts to applied laser light, whic
Page 445 and 446:
Table 8 Characteristic Parameters f
Page 447 and 448:
Table 8 (Continued) and H2O. A part
Page 449 and 450:
10. SG Ball, MHBJ van de Wal, RGF V
Page 451 and 452:
52. W Praznik, R Beck. J Chromatogr
Page 453 and 454:
Page 455 and 456:
3 PROTEIN PARTITIONING IN SEC 3.1 G
Page 457 and 458:
Figure 1 Plot of Kav vs. log M for
Page 459 and 460:
yconsideringtheproteinsolutestobesp
Page 461 and 462:
globular proteins and selected flex
Page 463 and 464:
silanol groups (52-54); even capped
Page 465 and 466:
most proteins to be maximally stabl
Page 467 and 468:
Figure 4 Chromatograms of BSA and P
Page 469 and 470:
concentrated) steps of protein puri
Page 471 and 472:
Table 3 Characteristics of Dextran-
Page 473 and 474:
preparative SEC. The capabilities o
Page 475 and 476:
37. GR Noll, N Nagle, JO Baker, DJ
Page 477 and 478:
Page 479 and 480:
Figure 2 Separation of total E. col
Page 481 and 482:
Figure 3 Separation of HaeIII-cleav
Page 483 and 484:
The recovery of DNA fragments has b
Page 485 and 486:
Endotoxin should also be removed fr
Page 487 and 488:
Table 3 Best Columns for the Separa
Page 489 and 490:
Figure 10 Dependence of HETP on flo
Page 491 and 492:
Appendix (Continued ) Polymer Colum
Page 493 and 494:
REFERENCES 1. CT Wehr, SR Abbott. J
Page 495 and 496:
MALDI-MS has been applied to determ
Page 497 and 498:
Figure 1 Calibration curvesof SEC c
Page 499 and 500:
Figure 3 Chromatograms of epoxy res
Page 501 and 502:
wherenandn0 aretheRIsofthesample an
Page 503 and 504:
Figure 5 SEC chromatogram of n-alka
Page 505 and 506:
Figure 7 Refractive indexes of comm
Page 507 and 508:
Another detector recently applied i
Page 509 and 510:
Figure 11 Absolute MW calibration p
Page 511 and 512:
Figure 12 Chromatogram of Acrawax C
Page 513 and 514:
18 Two-Dimensional Liquid Chromatog
Page 515 and 516:
largerispressuredropandresultingexp
Page 517 and 518:
elations between molar masses and s
Page 519 and 520:
Figure 2 (Continued) chapter, one o
Page 521 and 522:
where Nis the column efficiency exp
Page 523 and 524:
composition/architecture/molar mass
Page 525 and 526:
solvent. Here again, solvent-solven
Page 527 and 528:
or repulsive interactions between m
Page 529 and 530:
macromolecules may strongly differ
Page 531 and 532:
temperature. The efficacy of an ads
Page 533 and 534:
however, aliphatic bonded groups ma
Page 535 and 536:
Figure 10 Schematic representation
Page 537 and 538:
packing materials for SEC of synthe
Page 539 and 540:
Quantitative relations between sila
Page 541 and 542:
Both strength and thermodynamic qua
Page 543 and 544:
where Cand Dare constants for apart
Page 545 and 546:
ThisisimportantwhenLCCCisappliedtoc
Page 547 and 548:
Page 549 and 550:
Page 551 and 552:
However, strong adsorption of macro
Page 553 and 554:
elution step may be sufficient for
Page 555 and 556:
Figure 16 Block scheme of a full ad
Page 557 and 558:
processing of 2D-HPLC data. Knowled
Page 559 and 560:
Figure 20 Set of full retention-elu
Page 561 and 562:
distributions of complex polymers a
Page 563 and 564:
constituents were not discriminated
Page 565 and 566:
(Sec. 7) and therefore they can be
Page 567 and 568:
2. Identify sample solvents. First
Page 569 and 570:
1 Segmental interaction energy para
Page 571 and 572:
58. BG Belenkii. Pure Appl Chem 51:
Page 573 and 574:
19 Methods and Columns for High-Spe
Page 575 and 576:
Table 1 Summary of Methods for Incr
Page 577 and 578:
not savealot of time and solvent, d
Page 579 and 580:
Figure 3 Conventional SEC chromatog
Page 581 and 582: chromatogram at 4mL/min, which is f
Page 583 and 584: Sincethereductionoftheinternaldiame
Page 585 and 586: Table 3 Summary of Column Performan
Page 587 and 588: Figure 11 Dependence of column perf
Page 589 and 590: . Two-dimensional chromatography ru
Page 591 and 592: The standard deviations for the mol
Page 593 and 594: Figure 15 Comparison of time requir
Page 595 and 596: Figure 17 Accuracy and precision of
Page 597 and 598: polymer analysis. Samples are “ru
Page 599 and 600: just ignoring the fractionation of
Page 601 and 602: 20 Automatic Continuous Mixing Tech
Page 603 and 604: out at low enough concentration tha
Page 605 and 606: educed viscosity, h r, to be comput
Page 607 and 608: © 2004 by Marcel Dekker, Inc. Figu
Page 609 and 610: Figure 2 Raw ACOMP signals from mul
Page 611 and 612: Figure 4 Mw vs. monomer conversion,
Page 613 and 614: decreases smoothly and monotonicall
Page 615 and 616: Figure 7 Effects of fluctuating rea
Page 617 and 618: Finally, the use of a light-scatter
Page 619 and 620: Figure 8 Linear and cubic increases
Page 621 and 622: where r(t) is now given by 2 6 r(t)
Page 623 and 624: Figure 11 Light scattering from sol
Page 625 and 626: 3.1 ASimple System: Equilibrium Cha
Page 627 and 628: Figure 13 (a) ACM applied to the ch
Page 629 and 630: Also of note in Fig. 13b is how hig
Page 631: 15. JM Starita, CL Rohn. Rheologica
Page 635 and 636: 21 Light Scattering and the Solutio
Page 637 and 638: therefore, is to remove any lingeri
Page 639 and 640: is often found in the literature wh
Page 641 and 642: Figure 2 Configuration of an SEC se
Page 643 and 644: 5 THE IMPORTANCE OF SOFTWARE Like a
Page 645 and 646: standard deviations of the measured
Page 647 and 648: These include the differential weig
Page 649 and 650: Figure 8 Data of Fig. 7corrected fo
Page 651 and 652: Figure 11 Data of Fig. 10 with spik
Page 653 and 654: Figure 13 Fitstodatacollectedatasli
Page 655 and 656: Table 1 Errors (in %) Characteristi
Page 657 and 658: homogeneous copolymer, that is, tak
Page 659 and 660: process may be used to identify the
Page 661 and 662: fractionated sample. They represent
Page 663 and 664: Figure 16 An example of poor SEC ch
Page 665 and 666: on) methods, whereby the average di
Page 667 and 668: 23. WH Stockmayer, LD Moore Jr, M F
Page 669 and 670: condition, as is explained in this
Page 671 and 672: Figure 2 Partition coefficients KL
Page 673 and 674: 4 COLUMNS FOR HOPC Detailsaregiveni
Page 675 and 676: and concomitant clogging of columns
Page 677 and 678: Figure 5 Concentration dependence o
Page 679 and 680: Table 1 Solution Volume, Polymer Ma
Page 681 and 682: in Fig. 4a. The middle fractions (8
Page 683 and 684:
Figure 10 SEC chromatograms for som
Page 685 and 686:
appropriate for the early fractions
Page 687 and 688:
23 Size Exclusion/ Hydrodynamic Chr
Page 689 and 690:
Figure 2 Calibration curve for the
Page 691 and 692:
Figure 5 Elutionbehaviorofpolystyre
Page 693 and 694:
Table 1 Comparison Between SEC and
Page 695 and 696:
egular SEC column in which the pore
Page 697:
Such an ideal separation can be obt
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