Exclusion Chromatography Methodology and Characterization of Polymers and Related Materials
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T h e o d o r e P r o v d e r , Editor Glidden Coatings and Resins Looks at recent advances in size exclusion chromatography and its application in t h e analysis a n d characterization of polymers and related materials. Details major efforts made in SEC in the mechanism, instrumentation, calibration, and data treatment; operational variables, column technology, and oligomer analysis; and analysis of copolymers, branching, and cross-linked networks. CONTENTS Particle Chromatography Modeling · Gel Permeation Chromatography (GPC) Modeling · Supercritical Fluid Chromatograph · Automated Data Analysis for GPC · SEC Using Narrow and Broad Molecular Weight Distribution • SEC of Polyethylenes · GPC: Correction for Imperfect Resolution · Molecular Weight Separation and SEC Column Dispersion · Fuzes Statistical Methods for Testing Identity of Polymer Molecular Weight Distribution · Polymer-Based High-Efficiency GPC Columns · GPC Separation of Small Molecules · HighPêrformance High-Speed GPC · Deuterium Oxide Use in Aqueous SEC · High-Performance GPC of Polyethylene terephthalate) · Degradation of Very High Molecular Weight Polymers in GPC · High-Efficiency GPC for Analysis of Oligomers and Small Molecules · Petroleum Crude and Distillates Analysis by GPC · SEC of Polyethylene · Characterization of Absolute Molecular Weight Distribution of Polymers · Linear and Branched Block Copolymers · Thermoset Resin Cross-link Architecture · Epoxy Resin Cure Kinetics · Sulfonated Polystyrenedivinylbenzene Networks · Commercial Cellulose Triacetate Based on a symposium sponsored by the Division of Organic Coatings and Plastics Chemistry of the American Chemical Society
ACS Symposium Series No. 245 390 pages (1984) Clothbound LC 83-27515 ISBN 0-8412-0826-3 US & Canada $65.95 Export $79.95 Order from: American Chemical Society Distribution Office Dept. 69 1155 Sixteenth St., N.W. Washington, DC 20036 or CALL TOLL FREE 800-424-6747 and use your VISA, MasterCard, or American Express credit card.
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Figure 8. Schematic diagram of multidetector LC approach Nondestructive detectors are indicated with asterisks
hydrogen atoms attached to carbons b e a r i n g t h e s t e r o i d - e s t e r linkage. I n sharp contrast, the L C - 1 9 F - N M R profiles (Figure 7) of t h e s e derivatized steroids indicate t h a t t h e 1 9 F chemical shifts a r e clearly s e p a r a t e d in t h i s d o main. Thus, monitoring other N M R nuclides provides " a n o t h e r d i m e n s i o n " in characterizing complex m i x t u r e s , which m a y overlap in either t h e c h r o m a t o g r a p h i c or t h e *H chemical shift d o m a i n s . Obviously, o t h e r examples can b e a n t i c i p a t e d w i t h future s t u d i e s in t h i s area.
Extension to Other HPLC Detectors As s t a t e d earlier, t h e N M R d e t e c t o r is a noninvasive d e t e c t o r ideally s u i t e d t o " m u l t i d i m e n s i o n a l " analysis a p p r o a c h e s , along w i t h o t h e r d e t e c t o r s . T h i s is schematically i n d i c a t e d in Figu r e 8 for various parallel d e t e c t o r s . I n some cases, d e t e c t o r s in series can also be used. A l t h o u g h t h i s a p p r o a c h h a s n o t b e e n systematically s t u d i e d , trivial e x a m p l e s of d e t e c t o r s in series w i t h t h e N M R d e t e c t o r h a v e already been u s e d (e.g., refractive index, ultraviolet). N M R will u n d o u b t e d l y play a n
756 A · ANALYTICAL CHEMISTRY, VOL. 56, NO. 6, MAY 1984
even m o r e i m p o r t a n t role as a d e t e c t o r for H P L C in future analytical studies.
References (1) Suryan, G. Proc. Indian Natl. Sci. Acad. Part A 1951,15, 53. (2) Singer, J. R. Science 1959,130,1652. (3) McCormick, W. S.; Birkenmeirer, W. P. Rev. Sci. Instrum. 1969,40, 346. (4) Morse, O. C ; Singer, J. R. Science 1970,770,440. (5) Kumar, J.; Kumar, V. Science 1972, 775,794. (6) Singer, J. R. Science 1972, J 75, 794. (7) Arnold, D. W.; Burichart, L. E. J. Appl. Phys. 1965,36, 870. (8) Grover, T.; Singer, J. R. J. Appl. Phys. 1971 42 938. (9) Haywàrd, R. J.; Packer, K. J.; Tomunson, D. J. Mol. Phys. 1972,23,1083. (10) Stejskal, E. O. J. Chem. Phys. 1965, 43, 3597. (11) Forsen, S.; Rupprecht, J. J. Chem. Phys. Ε 1969,2, 292. (12) Zhernovoi, A. I.; Latyshev, G. D. "NMR in a Flowing Liquid"; Consul tants Bureau: New York, N.Y., 1965. (13) Fyfe, C. Α.; Cocivera, M.; Damji, S.W.H.; Hostetter, Τ. Α.; Sproat, D.; O'Brien, J. J. Magn. Reson. 1976,23, 377. (14) Fyfe, C. Α.; Damji, S.W.H.; Koll, A. J. Am. Chem. Soc. 1979,101, 951. (15) Fyfe, C. Α.; Damji, S.W.H.; Koll, A. J. Am. Chem. Soc. 1979,101, 956. (continued on p. 758 A)
