Size exclusion chromatography-viscometer calibration

Novolac molecular weights were measured in THF at 35°C by high pressure size exclusion chromatography using a Waters Model 510 pump (flow rate=1.0 ml/min), 401 differential viscometer detector and a set of Dupont PSM 60 silanized columns. A universal calibration curve was obtained with a kit of 10 narrow molecular weight distribution, linear polystyrene standards from Toya Soda Company. Data acquisition and analysis were performed on an AT T 6312 computer using ASYST Unical 3.02 software supplied with the Viscotek instrument. 

The size exclusion chromatography for this study was done in the routine manner execept for the inclusion of an online viscosity detector called a Differential Viscometer <3> (Viscotek Corp., Porter, Texas, USAl. This instrument together with an RI concentration detector permits the calculation of intrinsic viscosities across the chromatogram. An IBM PC data system with software is also provided (5). The software acquires data from both detectors, and performs calculations of intrinsic viscosity and molecular weight distributions using the Universal Calibration Method. 

Figure 2.2 Typical setup of size-exclusion chromatography equipped with triple detection for determination of the moiecuiar weight of polymers without the need for prerequisite calibration. DRi, differential refractive index detector DV, differentiai viscometer I, injector MALS, multi-angle light-scattering detector (depending on the model, the scattered light is measured at 3 or 18 different angles) P, pump. The central unit includes a computer and software.

The molecular weights of the samples were determined by size exclusion chromatography (SEC) using a PMMA calibration. A Waters GPCV 2000 with a temperature-controlled column/detector compartment that holds a three capillary viscometer and a differential refractometer was used. The temperature in the column/detector compartment was 95°C. 

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