Stephen Hutcheson

The measurement of mechanical properties of glycerol, m-toluidine, and sucrose benzoate under consideration of corrected rheometer compliance: An in-depth study and review

Determination of the mechanical response of materials can be fraught with error if rheometer compliance is not properly taken into account. The resulting inaccuracies in the determined mechanical properties of the materials of interest can result in mistakes in material modeling, design, and theory. In the present work, we build on our previous report [K. Schroter, S. A. Hutcheson, X. Shi, A. Mandanici, and G. B. McKenna, J. Chem. Phys. 125, 214507 (2006)] and investigate the effects of instrument compliance that result from use of a commercial rotary rheometer and its fixtures on the determination of the dynamic shear and stress relaxation responses of glycerol, m-toluidine, and sucrose benzoate near to the glass transition regime. We revisit the procedure for compliance corrections presented in earlier work and correct dynamic shear data for these materials. We also present a new correction procedure to obtain shear stress relaxation curves from data that was obtained using this instrument. In addition, we broaden our consideration of compliance effects to materials, such as polymer melts, that have lower moduli than the simple glass formers previously considered. We discuss the possible errors for the viscoelastic response of glass-forming liquids and polymer melts or rubber networks that have been reported in the literature. A major purpose of the present work is to alert the community to possible problems in modulus values and relaxation functions obtained for a large number of materials for which rotary rheometers were used in a range where material stiffness (modulus and geometry effects) was comparable to the rheometer stiffness. Finally, we include recommendations for both experimental protocol and instrument design to avoid, minimize, or correct for compliance effects.

Dynamic shear modulus of glycerol: Corrections due to instrument compliance

A recent article by Shi et al. [J. Chem. Phys.123, 174507 (2005)] reports results from mechanical measurements on three simple inorganic glass formers: glycerol, m-toluidine, and sucrose benzoate. The experiments carried out were stress relaxation, aging, and dynamic (all in shear) using a torsional rheometer, an advanced rheometric expansion system (TA Instruments). The original force rebalance transducer (2KFRT) supplied with the system was replaced with a custom-made load cell (Sensotec) that had a capacity of 20 000 g cm in torque and 5000 g in normal force. The replacement of the load cell was done due to the belief that the main source of compliance in this instrument was from the 2KFRT. With this assumption, the authors published their results for the three materials of interest and compared their results with the techniques of Schroter and Donth [J. Chem. Phys.113, 9101 (2000)] for the measurements on glycerol and reported important differences. These differences were disputed by one of the present authors (Schroter), and the present report shows that the results from Schroter and Donth are correct. We show that the reasons have to do with the instrument compliance being greater than originally thought by Shi et al. Here we examine the effects of platen diameter/geometry on the glycerol dynamic moduli, describe a means to correct dynamic data, present a revised comparison of the corrected data with that of Schroter and Donth, and provide a discussion of future work and conclusions.