Polymerization Technology Laboratory Course

Viscometers/Rheometry

Lab Report
HOANG LONG LUU MUHAMMAD FAROOQ

ABSTRACT Different Concentrations of Methyl Cellulose by weight percent were filled in the measuring cylinders of DIN 125 & DIN 145 at different parametric conditions in order to measure the flow properties like Viscosity & Shear stress. Different values of Viscosity and Shear Stress were obtain at different temperature and concentrations which were represented in graphical notations to establish a relationship between the Shear Stress & Viscosity , Shear Rate & Viscosity and Shear Stress & Shear Rate. Values of zero shear rate viscosities at 25 C, 37 C & 42 C were measured by using the extremely low shear rate values and were presented in a graph to get a clear picture of zero sear rate dependency on temperature. THEORY Viscosity Viscosity is the resistance to the flow of liquid. Its a material property and can be determined by using different techniques and methods. Mathematically Viscosity is the ratio between the shear stress and shear rate. Viscosity Shear Stress Shear Rate

We can describe the shear rate & shear stress by elaborating the following diagram. F Y

Diagram (1) A Fluid is been kept between the two plates. Upper plate is moveable and lower plate is fixed. As we move the upper plate the layers of fluid near to the upper plate move along with the plate. The velocity of the upper layers is more than the velocity of the layers, with the bottom plate as the bottom plate is fixed. We consider the velocity of the upper plate is V, whereas velocity of the lower or bottom plate is zero. All the layers in between the plate will move with different velocities. Which can be defined with velocity gradient dv/ dy. So we can say that stress is directly proportional to the change in velocity along y direction. Stress dv/dy F/A= dv/dy

Units of Viscosity Pascal Second Pa. Sec Kilo gram per meter second Kg/m. sec Newton second per meter square N. Sec/m Types of Fluids on the basis of flow behavior Fluids are of two types, Newtonians and Non Newtonians. The major difference between the two categories is their flow behavior. In Newtonians fluids like water stress is directly proportional to strain means the stress Vs Strain curve is linear. Change is shear rate does not impart any effect on the viscosity. Whereas most of the plastics are Non Newtonians and their flow characteristics change as we change the shear rate in other words the stress strain curve is non-linear.

Pseudoplastic Shear Thinning fluids in which viscosity of the fluid decreases with an increase in shear rate. But it has been seen that for a very small values of shear rate the viscosity of the fluid remains constant. This viscosity at zero shear rates or at steady state conditions in called zero viscosity. Dilatants These are also called Shear Thickening fluids, fluids which gain viscosity upon increase in shear rate. Bingham plastic These are viscoelastic materials in nature. They does not respond to low shear rate whereas does flow as visous fluid on high shear rates. Ostwaldde Waal Equation This is also known as power law. According to this law a relationship has been devised which is as follows. If the value of n is less than one then as per law the viscosity would decrease with increase shear rate.

Shear Rate K is the flow consistency index n is the flow behavior index

Viscosities of the different materials

Material Air Water Ethyl alcohol Mercury Ethylene glycol Olive oil 100% Glycerol Honey Corn syrup

Pascal Sec 105 103 1.2103 1.5103 20103 0.1 1.5 10 100

Experiment 1. A solution of methyl cellulose (3 wt% in water) is filled into the measuring system (DIN 125). The flow characteristic is measured at different temperatures (25 / 35 / 45 / 55 C) by variation of the shear rate. 2. Fill different concentrations of methyl cellulose (0, 1, 2, 5 wt% in water) into the measuring system (DIN 145) and measure the flow characteristic at a temperature of 25C by variation of the shear rate. Apparatus Rotary Rheometer with cylinder measuring system DIN 125 AND DIN 145 was used to determine the flow characteristics of methyl cellulose at different temperature and concentrations. Method The test material is poured in the hollow cylinder. A solid cylinder in then moved in with some force so it should go in the hollow cylinder completely. This assembly is now slide in the Rheometer and then inner cylinder is clamped with the Rheometer head. A threaded mechanism is used to hold the outer cylinder at the bottom. Electrical unit is used to control the motor speed which gives us the different values of torque. Two types of speeds are available 100 & N. We use N speed when the initial viscosities have remarkable difference. Rheometer is equipped with a thermometer.

RESULTS & DISCUSSION Analysis # 1 A solution of methyl cellulose (3 wt% in water) is filled into the measuring system (DIN 125). The flow characteristic is measured at different temperatures (25 / 37 / 42 C) by variation of the shear rate. Following are the empirical values obtained from the experiment.

For the above obtained values from the results different graphs have been plotted to understand the flow behavior of methyl cellulose 3% in water at different temperatures.

Viscosity Vs Shear Stress

10000

1000

Viscosity mPa.S
100

10

1 1000 "Viscosity @ 25 C

10000

100000 Viscosity @ 37 C

1000000 Viscosity @ 42 C

Shear Stress mPa

Discussion From the above graph between viscosity and shear stress it can be seen that viscosity decreases with an increase in shear stress. As one composition at three different temperatures was subjected to the change and we found that the solution of 3% at 25 C shows more drop in viscosity at the same shear stress as compare to the other samples at higher temperature.

Viscosity Vs Shear Rate

10000

1000

Viscosity mPa.S
100

10

1 1 10 Viscosity @ 25 C 100 Viscosity @ 37 C 1000 Viscosity @ 42 C 10000

Shear Rate 1/sec

Discussion From the above graph between viscosity and shear rate it can be seen that viscosity decreases with an increase in shear rate. Increase in shear rate is decreasing the viscosity of the solution .A general idea can be made that the lower the temperature of the solution more is the change in viscosity upon increase in shear rate.

Shear Stress Vs Shear Rate

500000 450000 400000 350000

Shear Stress mPa

300000 250000

200000
150000 100000 50000 0 0 200 400 @ 25 C" 600 @ 37 C" 800 @42 C " 1000 1200

Shear Rate 1/sec

Discussion From the above graph between shear rate and shear stress it can be seen that upon an increase in shear rate, shear stress increase. As one composition at three different temperatures was subjected to the change and we found that the solution of 3% at 25 C demonstrates more shear stress upon increased shear rate. The solution at 37 C also shows an increase in shear stress upon increasing shear rate but the value of shear stress in smaller than that of solution at 25 C. The same is the case with the solution at 42 C, higher the temperature, lower the shear stress gradient. Determination of zero shear rate viscosity In order to calculate the zero shear rate viscosities we have to calculate the values of shear viscosities at least shear rate. We assume that at minimum shear rate the difference between the zero viscosity and experimental value of viscosity is negligible. Calculations Value for the Viscosity factor is considered at shear rate at 1st step which is = 6.65 1/sec So, At 25 C At 37 C At 42 C 0 =T X f 0 = 23.5 x 171.6 = 4032.6 mPa.S 0 =T X f 0 =15.5 x 171.6 = 2659.8 mPa.S 0 =T X f 0 = 12.5 x 171.6 = 2145.0 mPa.S

Zero Viscoity Vs Temp.

4500 4000 3500

Viscosity mPa.S

3000 2500 2000 1500 1000 500 0 25 37 42

Temp.

Calculate the activation energy EA of the Arrhenius-Andrade correlation:

In the result of the Arrhenius Andrade equation, we have:

Then With 1= 4032.6 mPa.s, 2 = 2145 mPa.s, T1 = 298 K, T2 = 315 K and R = 8.314 J.mol-1.K-1 then we get the result.

Activation energy is E = 28.98 KJ.

Analysis # 2 Different concentrations of methyl cellulose (0, 1, 2, 5 wt% in water) were filled into the measuring system (DIN 145) and flow characteristic at a temperature of 25C by variation of the shear rate were measured. Following are the empirical values of the experiment.

For the above obtained values from the results different graphs have been plotted to understand the flow behavior of methyl cellulose in water at different concentrations and constant temperatures of 25 C.

Viscosity and Shear Stress at 250C in different concentrations

100000
10000 Viscosity [mPa.s] 1000 100 10 1 100 1000 10000 Shear Stress [mPa] 100000 1000000

1% 2% 3% 5% - N position

Discussion From the above graph we can estimate the flow behavior of a solution at different concentrations. Increase in shear stress is decreasing the viscosity in 2 wt%, 3 wt% and 5 wt% in water. All stated three concentrations follow the same identical behavior. Whereas solution with 1 wt% in water is having an opposite trend. It have been observed that the increase in shear stress is actually increasing the viscosity slightly which is due to the very dilute concentration of methyl cellulose in the particular solution. Viscosity and Shear rate at 250C in different concentrations
100000 10000 Viscosity [mPa.s] 1000 100 10 1 1 10 100 Shear rate [1/s] 1000 10000

1% 2% 3% 5% - N position

Discussion In the above plotted graph the generalized trend of different concentration solutions shows decrease in viscosity as the shear rate is increased. Same like above situation we do observe an increase in viscosity upon an increase in shear rate in a 1wt % in water solution. This behavior is due to the very low concentration of methyl cellulose.

Shear Rate and Shear Stress at 250C in different concentrations

1000000 Shear Stress [mPas] 800000 600000 400000 200000 0 -200000 0 200 400 600 800 1000 1200 Shear rate [1/s] 1% 2% 3% 5% - N position

Discussion Above plotted graph gives us a relationship between the shear stress and shear rate. It is evident from the above observation that as the higher the concentration, higher the shear stress will be experienced if we increase the shear rate. As we see in 1wt % in water solution has very little shear stress as shear rate was increased. In case of 5wt % in water solution has most shear stress value upon increasing the shear rate which gives us a generalized opinion that higher the concentration, higher the viscosity will be and if the viscosity is more that more shear stress will be shows by the material as we will increase the shear rate. Fit the data with Oswald de Waal equation: Oswald de Waal equation describes the flow behavior of shear thinning polymer solutions:

From the equation, we can get the relation between shear rate and shear stress in another form :

We can see that the logarithm value of shear stress and shear rate is linear with the slope of the line n. If the obtained shear stresses in the experiments have a linear relation with shear rate in the log/log chart then these results fit with the Oswald de Wall Equation.
Shear Stress and Shear Rate for 5% solution in 100 position
log log 4 3 2 1 0 2 3 4 5 6 log

Shear Stress and Shear Rate for 2% solution in 100 position

4 3 2 1 0 2 3 4 5 log

In the chart, the log/log values of shear stress and shear rate in the 100 position express a linear relation and that proves the data fit with the Oswald de Waal equation.