Viscoelasticity dynamic frequency sweep tests

Dynamic-shear measurements are of the complex viscosity rj ) as a function of the dynamic oscillation rate (o), at constant temperature. These tests are defined as isothermal dynamic frequency sweeps. Since the dynamic frequency sweeps are conducted at a given amplitude of motion, or strain, it is necessary to ensure that the sweeps are conducted in the region where the response is strain-independent, which is defined as the linear viscoelastic region. This region of strain independence is determined by an isothermal strain sweep, which measures the complex viscosity as a function of applied strain at a given frequency. This ensures that a strain at which the dynamic frequency sweep may be conducted in the linear viscoelastic region is selected. 

Dynamic temperature sweep tests, in the linear viscoelastic range, were conducted at 1 °C/min and 1 % strain, at 2 constant frequencies 6.28 and 10 rad/s (AASHTO-TP5). 

The sample is loaded onto the instrument and the time reference is noted by starting a timer or resetting a timer in the software. A dynamic test for viscoelastic structure is then used to monitor changes in the sample that could result from mechanical relaxation, drying, or thixotropy. A time sweep test is usually performed at a constant temperature. The test is also run at a constant frequency that is comparable to real-time observation (typically 1 Hz) or at a constant angular frequency (10 rad/sec or 1.6 Hz). 

The four variables in dynamic oscillatory tests are strain amplitude (or stress amplitude in the case of controlled stress dynamic rheometers), frequency, temperature and time (Gunasekaran and Ak, 2002). Dynamic oscillatory tests can thus take the form of a strain (or stress) amplitude sweep (frequency and temperature held constant), a frequency sweep (strain or stress amplitude and temperature held constant), a temperature sweep (strain or stress amplitude and frequency held constant), or a time sweep (strain or stress amplitude, temperature and frequency held constant). A strain or stress amplitude sweep is normally carried out first to determine the limit of linear viscoelastic behavior. In processing data from both static and dynamic tests it is always necessary to check that measurements were made in the linear region. This is done by calculating viscoelastic properties from the experimental data and determining whether or not they are independent of the magnitude of applied stresses and strains. 

Rheological measurements were performed in shear using a stress controlled rheometer (Carri-Med CSL 100) operating in cone-plate geometry. Each sample is submitted successively to a first frequency sweep in range 10 3-40 Hz under 3% strain, to a creep and recovery test, and finally to a second frequency sweep identical to the first one. The dynamical strain amplitude (3%) and the value of the creep stress (chosen so as to keep the maximum strain below 10%) were set in order to remain within the linear viscoelasticity domain. Creep and creep recovery were recorded during 20 h and 80 h, respectively, times which allowed the steady state to be reached in all cases. A fresh sample was used for each solvent/temperature combination. 

A torsion dynamic rheometer, Rheometric SCIENTIFIC RDA-II, was employed with a plate-plate fixture (i.e., 25 mm in diameter). Frequency sweep experiments were performed in the range 0.1 to 100 rad/s at 190°C in the linear viscoelastic range of the MDPE s. The tests were performed to obtained indirect evidences of the differences in molecular weights and molecular weight distribution of the samples. 

Fig. 3 Dynamic test frequency oscillation sweep. For viscoelastic fluid of 1 wt% poly (ethylene-oxide)(PEO) in 55 wt% glycerol water. Molecular weight of PEO is 2 X 10 g/mol...

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