H Size-Exclusion Chromatography

Mourey, T. H. and Coll, H., Size exclusion chromatography with two-angle laser light-scattering (SEC-TALLS) of high-molecular-weight and branched polymers, /. Appl. Polym. Sci., 56, 65, 1995. 

Cinchonidine displays a tertiary amine, an aromatic amine and a free hydroxyl functionality. Direct hydrosilylation with unprotected cinchonidine (derivatized with a double bond for hydrosilylation), led to a cross-linked product. Thus, hydrosilylation was performed on PHMS with the trimethylsilyl derivative 1 (Fig. 10), in the presence of (EtjS)jPtClj as catalyst (0.05%), for 6h at 80°C in toluene. The hydroxyl group was deprotected with methanol at 65°C during 120 h. Size Exclusion Chromatography showed that the polysiloxane backbone was not degraded. A maximal grafting percent of 15% could be obtained, relative to the SiH units. 

Mori, S. Barth, H. Size Exclusion Chromatography, Springer-Verlag Berlin, 1999. 

Sano, T. Iguchi, N. lida, K. Sakamoto, T. Baba, M. Kawaura, H. Size-exclusion chromatography using self-organized nanopores in anodic porous alumina. Appl Phys Lett 2003, 83, 4438-4440. 

Barth, H. G. (1987). 1 ACS Symposium Series 352, Detection and Data Analysis in Size Exclusion Chromatography (T. Provder, ed.), pp. 29-46. American Chemical Society, Washington, DC. 

Figure 3 Reversed-phase chromatography of products after alkaline hydrolysis of /3-poly(L-malate), Discrete polymer products are formed, which differ in length by several units of L-malate. The absorbance at 220-nm wavelength was measured, (a) /3-Poly(L-malate) before hydrolysis, (b) After 10-min incubation in 20 mM NaOH at 37°C. (c) After 15 h in 20 mM NaOH at 37°C. (d) After I h in 500 mM NaOH at 100°C. High pressure chromatography (HPLC) on Waters reversed-phase Ci8- i-Bondapak. The methanol gradient (in water-trifluoro acetic acid, pH 3.0) was programmed as follows 0-40 min 0.3-23%, 40-47 min 23-40%, 47-49 min 40%, 49-54 min 40-0%. (d) Inset size exclusion chromatography after 3-min alkaline hydrolysis at pH 10.2. BioSil SEC 250 column of 300 mm x 7.8 mm size, 0.2 M potassium phosphate buffer pH 7.0.

Sugar beet pulp was saponified and then hydrolysed with 0.1 N HCl at 80 °C for 72 h. Linear RG oligomers of DP 6 to 18, abbreviated RGO 6 to 18, were isolated by ion-exchange chromatography and size-exclusion chromatography by Renard et al. (1995). 

The partially hydrolysed material was fractionated by size exclusion chromatography on a Bio Gel PIO (Bio Rad) column (2,6 x 90 cm) and eluted with 50 mM ammonium hydrogen carbonate at 20 ml/h and fractions of 3.2 ml each were collected. Fractions 45-70 were pooled and subjected to HPAEC-PAD for further separation. 

Garcia-Rubio, L.H., MacGregor, J.F., Hamielec, A.E., "Copolymer Analysis Using GPC with Multiple Detectors , presented at the Symposium on Recent Developments in Size Exclusion Chromatography , 178th ACS National Meeting, Washington, D.C., September 9-14, 1979. 

Pfannkoch, E., Lu, K. C., Regnier, F. E., and Barth, H. G., Characterization of some commercial high-performance size-exclusion chromatography columns for water-soluble polymers, /. Chromatogr. Sci., 18, 430, 1980. 

Stegeman, G., Kraak, J. C., and Poppe, H., Hydrodynamic and size-exclusion chromatography of polymers on porous particles, ]. Chromatogr., 550, 721, 1991. 

Mourey, T. H., Miller, S. M., and Balke, S. T., Size exclusion chromatography calibration assessment utilizing coupled molecular weight detectors, /. Liq. Chromatogr., 13, 435, 1990. 

Jackson, C. and Yau, W. W., Computer simulation study of multidetector size-exclusion chromatography. Flory-Schulz molecular weight distribution, in Chromatographic Characterization of Polymers, Hyphenated and Multidimensional Techniques, Provder, T., Barth, H. G., and Urban, M. W., Eds., American Chemical Society, Washington, D.C., 1995, chap. 6. 

Mourey, T. H. and Bryan, T. G., Size-exclusion chromatography using mixed-bed columns with dimethylformamide at near-ambient conditions comparison of pStyragel HT Linear and PL Gel mixed-bed columns, /. Liquid Chromatogr., 14, 719, 1991. 

Frederiksson, H., Andersson, R., Koch, K., and Amon, P, Calibration of a size-exclusion chromatography system using fractions with defined amylopectin unit chains, /. Chromatogr. A, 768, 325, 1997. 

Figure 1. Size exclusion chromatography of Ru3(C0)i2 catalyzed polymerization of MeNH-[H2SiNMe]x-H as a function of time. Polystyrene standards used for calibration.

Barth, H.G. and Smith D.A. "High-Performance Size-Exclusion Chromatography of Guar Gum," J Chromatog. (1981) 206, 410-415. 

Bedani, F., Kok, W.Th., Janssen, H.-G. (2006). A theoretical basis for parameter selection and instrument design in comprehensive size-exclusion chromatography x liquid chromatography. J. Chromatogr. A 1133, 126-134. 

Chen, J., Radke, W., Pasch, H. (2002). Analysis of polyamides by size exclusion chromatography and laser light scattering. Macromol. Symp. 193, 107. 

Pasch, H. (2004). Characterization of Polymer Heterogeneity by 2DLC. In Striegel, A.M., editor.Multiple Detection in Size-Exclusion Chromatography. ACS Symposium Series 893, American Chemical Society Washington, D.C. 

Determined by size exclusion chromatography with polystyrene standard in 1,2,4-trichlorobenzene dBranching density per 1000 carbons determined by H NMR... 

Tetramethylammonium chloride (2 mg) and 5 (1. Og) were placed in a vial, sealed, and heated in an oil bath at 107°C for 65 h. H-NMR analysis of the colorless, viscous grease showed the ratio of signals at 4.6 and 3.90ppm as ca. 60/1. The small amount of cyclic dimer formed (GC anlaysis) was removed by Kugelrohr distillation (up to 100°C/0.05 mm). 19F-NMR featured the internal/ terminal CF2CH20 group ratio as ca. 83/1. Size-exclusion chromatography showed the major peak with Mn, =26,700 and Mw =52,800, consistent with condensation polymer 7. 

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