- Page 1 and 2: MARCEL DEKKER Handbook of Size Excl
- Page 3: CHROMATOGRAPHIC SCIENCE SERIES A Se
- Page 7 and 8: Preface to the Second Edition Gel p
- Page 9 and 10: Preface to the First Edition Molecu
- Page 11 and 12: Contents Preface to the Second Edit
- Page 13 and 14: 17. Size Exclusion Chromatography o
- Page 15 and 16: James F. Curry Analytical Departmen
- Page 17 and 18: Iwao Teraoka, Ph.D. Othmer Departme
- Page 19 and 20: The graphical data display typicall
- Page 21 and 22: polymer molecule can elute. The tot
- Page 23 and 24: individual states) allowed to them.
- Page 25 and 26: unsaturation while the IR detector
- Page 27 and 28: Sampleconcentrationshouldbeminimize
- Page 29 and 30: averagesdefinedintermsofthemolecula
- Page 31 and 32: information regarding appropriate M
- Page 33 and 34: Analytical. Two models, the KMX-6 a
- Page 35 and 36: Figure 6 Overlay of time-sliced pea
- Page 37 and 38: accurately for very large and very
- Page 39 and 40: 4 GENERAL REFERENCES The interested
- Page 41 and 42: 46. TA Chamberlin, HE Tuinstra. US
- Page 43 and 44: materials are commercially availabl
- Page 45 and 46: Table 1 Commercial Column Packing M
- Page 47 and 48: necessarily comparable. For this re
- Page 49 and 50: adjusted such that the pore size di
- Page 51 and 52: narrowmolecular weight range, indiv
- Page 53 and 54: Figure 8 Effect of particle size on
- Page 55 and 56:
Figure 9 SEC calibration using poly
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Table 4 Typical Eluent Systems for
- Page 59 and 60:
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
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As expected, pS is closer to the no
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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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Appendix (Continued) Polymer Column
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Appendix (Continued) Polymer Column
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5. J West, E Rodriguez. Rubber Chem
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8 Size Exclusion Chromatography of
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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
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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
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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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9 Size Exclusion Chromatography of
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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
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Another commercially available MW d
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Table 5 Weight-Average Molecular We
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Figure 6 (a) Size exclusion chromat
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compared to anormal product. By com
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StudyingtheKineticsofaChemicalReact
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this information, the higher MW pea
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Appendix (Continued) Polymer Column
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Appendix (Continued) Polymer Column
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46. CJ Kim, A Hamielec, A Bendek. J
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10 Size Exclusion Chromatography of
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A relatively new technique utilizin
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where ais the exponent of the Mark-
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Figure 2 TDS chromatograms for full
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Figure 5 Comparison of molecular we
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Table 3 Summary of TDS Molecular We
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thepartiallyhydrolyzedPVAwiththecol
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Table 5 Summary of Conformation and
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a¼0.627andlog(K) ¼23.249.Theseare
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The limits of detection of the PVA
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Figure 12 PVAc broad molecular weig
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4 SUMMARY Advances in SEC character
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11 Size Exclusion Chromatography of
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2.1 Molecular Weight Grades of PVP
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exclusion chromatography with low-a
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weightandmolecularweightdistributio
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© 2004 by Marcel Dekker, Inc. Figu
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Figure 4 PEOcalibrationofUltrahydro
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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
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Figure 11 Molecular weight distribu
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12 Size Exclusion Chromatography of
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2 CHEMICAL, MACROMOLECULAR AND MORP
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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
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The silylation was performed in LiC
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observed using column materials hav
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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
- Page 347 and 348:
dextrans swell too much in cadoxen
- Page 349 and 350:
stirring at room temperature for an
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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
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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
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The division according to eluent ty
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Apolymer produced by UV irradiation
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Because DMAC/LiCl is also agood sol
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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
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topological anisotropy in the polym
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29. M Ristolainen, R Alen, J Knuuti
- Page 397 and 398:
eds. Proc Int Symp 1998. Canton, Pe
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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
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Figure 6 (a) Large starch granules
- Page 415 and 416:
number of branching points); crossl
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Both absolute approaches are extrao
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Table 7 (Continued) Approach Experi
- Page 421 and 422:
structures, excluded volumes, and t
- Page 423 and 424:
Figure 10 (a) SEC elution profile o
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Figure 12 Wheat glucans: DRI elutio
- Page 427 and 428:
Figure 13 Wheat glucans. Normalized
- Page 429 and 430:
Figure 16 Wheat glucan. Normalized
- Page 431 and 432:
Figure 18 Wheat glucan.Elution prof
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Figure 20 Wheat glucans. Absolute m
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Figure 22 Wheat glucan. (a) Intrins
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Figure 24 Wheat PA-glucan. Elution
- Page 439 and 440:
an Ubbelohde-viscometer for concent
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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:
15 Size Exclusion Chromatography of
- 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:
16 Size Exclusion Chromatography of
- 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:
Figure 12 Schematic representation
- Page 549 and 550:
Figure 14 Schematic representation
- 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 and 632:
15. JM Starita, CL Rohn. Rheologica
- Page 633 and 634:
52. M Hulden. Hydrophobically modif
- 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