Guidelines for checking performance and verifying accuracy of rotational rheometers: viscosity measurements in steady and oscillatory shear

Abstract

The paper addresses techniques for checking the performance of rotational rheometers with cone–plate, plate–plate, or concentric cylinder geometry. We focus on the determination of the viscosity as a function of the shear rate and of the magnitude of the complex viscosity as a function of the angular frequency. After summarizing the relevant definitions and test modes, we show examples of measurements in the linear viscoelastic range, and applications of the Cox–Merz relationship. Sources of reference fluids with defined viscosities are presented, and their use in tests for verification of accuracy is demonstrated. Relevant issues, predominantly for Newtonian reference liquids, are the exploration of measurement limits, related either to the shear rate range or to reliably accessible viscosity levels. Viscoelastic reference samples are also discussed. Prerequisites for sample preparation and loading are addressed. In particular, we present recommendations based on experience from various laboratories. Finally, we discuss the problem of temperature calibration, presenting techniques that allow the determination of the true sample temperature for a given set temperature of the rheometer. This paper summarizes contributions from various industrial and academic laboratories.