The rheological measurements were made using an Anton Paar modular compact rheometer MCR 92 (Anton Paar, Graz, Austria), with a cone-plate measuring system and a gap of 48 μm. The apparent viscosity of the polyols was measured at 25 °C and the shear rate was 50 s−1 using standard flow curve measurement and shear rate sweep from 0.1 s−1 to 100 s−1.
Modular compact rheometer mcr 92
Manufactured by Anton Paar
Sourced in Austria
The Modular Compact Rheometer MCR 92 is a laboratory instrument designed for rheological measurements. It provides precise control and measurement of material properties such as viscosity, viscoelasticity, and flow behavior.
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5 protocols using modular compact rheometer mcr 92
1
Rheological Characterization of Polyols
2
Rheological Characterization of Materials
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Rheology tests were carried out using an Anton Paar Modular Compact Rheometer MCR 92 equipped with an Anton Paar Measuring Cone Plate CP50-1 (diameter 50 mm, angle 1°). Data were analyzed with RheoCompassTM software. In the amplitude sweep experiment, to determine the LVER, a range of deviation tolerance of ±5% was set.
3
Rheological Characterization of Hyaluronic Acid and Chitosan
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The rheological properties of HA, Ch, and the complex were studied using a Modular Compact Rheometer MCR 92 (Anton Paar GmbH, Graz, Austria), equipped with a 50-mm-diameter cone–plate geometry, with a cone angle of 1°. For all tests, the temperature and the gap between the plates were kept constant 20 °C and 0.98 mm, respectively.
Viscosity measurements were performed in rotation mode, they were investigated in the range of 0.1–100 s−1 and ten points per decade were acquired.
The sample viscoelastic behaviour was investigated in the oscillation mode, to determine the storage modulus G’(ω) and the loss modulus G”(ω). First, preliminary tests were conducted to determine the upper amplitude limit of the linear viscoelastic region (LVE), testing the samples over an extended strain field (0.01–100%). Second, after the LVE was determined (2% for HA and HA/Ch and 20% for Ch), the samples were tested by performing a frequency sweep test over the 0.628 rad/s–628 rad/s (i.e., 0.1–100 Hz) frequencies, at a constant strain. Data were elaborated with RheoCompass™ software.
For the analysis, the same solutions as for Zp were tested. Before the analysis, solutions were sonicated to reduce air bubbles.
Viscosity measurements were performed in rotation mode, they were investigated in the range of 0.1–100 s−1 and ten points per decade were acquired.
The sample viscoelastic behaviour was investigated in the oscillation mode, to determine the storage modulus G’(ω) and the loss modulus G”(ω). First, preliminary tests were conducted to determine the upper amplitude limit of the linear viscoelastic region (LVE), testing the samples over an extended strain field (0.01–100%). Second, after the LVE was determined (2% for HA and HA/Ch and 20% for Ch), the samples were tested by performing a frequency sweep test over the 0.628 rad/s–628 rad/s (i.e., 0.1–100 Hz) frequencies, at a constant strain. Data were elaborated with RheoCompass™ software.
For the analysis, the same solutions as for Zp were tested. Before the analysis, solutions were sonicated to reduce air bubbles.
4
Rheological Characterization of Sol-Gel Precursors
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The hydrolyzate apparent viscosity was determined using a rotary viscometer LV DV-II+Pro (Brookfield Engineering, Middleboro, MA, USA) using a CPE-52 spindle at 60 rpm and RT.
The oscillatory time sweeps of the complex viscosity were measured using an MCR 92 modular compact rheometer (Anton Paar GmbH, Graz, Austria) with a CP50-1 cone-and-plate spindle with 50 mm diameter and 1° cone angle at a constant 0.101 mm gap. Approximately 1 ml of ST precursor sol was collected 5 min after the addition of chelated TiPOT solution (solution 2) to the hydrolyzate solution (Si precursors, solution 1). The setup was previously heated to the desired temperature (50 or 85 °C) before the start of the test. The complex viscosity was monitored under constant 1% shear strain and 2 Hz frequency over 30 minutes. These parameters were chosen to maintain the sol–gel samples in the viscoelastic regime.29 Rotational tests were also performed to obtain the viscosity curves and compare different emulsions in terms of viscosity evolution along a shear rate ranging from 1 to 100 s−1. Flow tests were also performed using the same system along a shear rate ranging from 1 to 100 s−1. The flow curves analysis allowed a better understanding of different emulsions used as templates for the spherical particles.
The oscillatory time sweeps of the complex viscosity were measured using an MCR 92 modular compact rheometer (Anton Paar GmbH, Graz, Austria) with a CP50-1 cone-and-plate spindle with 50 mm diameter and 1° cone angle at a constant 0.101 mm gap. Approximately 1 ml of ST precursor sol was collected 5 min after the addition of chelated TiPOT solution (solution 2) to the hydrolyzate solution (Si precursors, solution 1). The setup was previously heated to the desired temperature (50 or 85 °C) before the start of the test. The complex viscosity was monitored under constant 1% shear strain and 2 Hz frequency over 30 minutes. These parameters were chosen to maintain the sol–gel samples in the viscoelastic regime.29 Rotational tests were also performed to obtain the viscosity curves and compare different emulsions in terms of viscosity evolution along a shear rate ranging from 1 to 100 s−1. Flow tests were also performed using the same system along a shear rate ranging from 1 to 100 s−1. The flow curves analysis allowed a better understanding of different emulsions used as templates for the spherical particles.
5
Rheological Characterization of FucoPol Solutions
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The rheological properties of FucoPol aqueous solutions (1.0 wt%) were studied using a MCR 92 modular compact rheometer (Anton Paar, Madrid, Spain), equipped with a PP50/S parallel plate geometry (diameter 50 mm). The temperature was kept constant at 25 °C using a P-PTD 200/AIR Peltier plate (Anton Paar, Madrid, Spain. The flow curves were determined using a steady-state flow ramp in a shear rate range of 0.01 to 1000 s−1. The flow curves obtained were fitted to the equation based on Cross model [30 (link)] described as follows:
where η is the apparent viscosity (Pa·s), η0 (Pa·s) is the viscosity at zero shear rate, τ (s) is the relaxation time, and m is a dimensionless constant, related to the exponent of power-law (n) by m = 1 − n [24 (link),27 (link)]. Frequency sweep tests were performed with frequency ranging from 0.01 to 100 rad/s with a constant strain of 0.5% that was well within the linear viscoelastic limit (LVE), which was evaluated through preliminary amplitude sweep tests. All tests were performed in triplicate.
where η is the apparent viscosity (Pa·s), η0 (Pa·s) is the viscosity at zero shear rate, τ (s) is the relaxation time, and m is a dimensionless constant, related to the exponent of power-law (n) by m = 1 − n [24 (link),27 (link)]. Frequency sweep tests were performed with frequency ranging from 0.01 to 100 rad/s with a constant strain of 0.5% that was well within the linear viscoelastic limit (LVE), which was evaluated through preliminary amplitude sweep tests. All tests were performed in triplicate.
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