Instrumentation

Journal of Physics 35 No. 2 (1989) 274-281

Concentric Cylinder Viscometer Extremely Low Shear Stress.

R. T. Rodriguez, Raul Montiel C. and A. Romo U.
Department of Physics, University Autonomy Metropolitan - Iztapalapa, PO Box 55-534, 09340 Mexico, DF (Received August 2, 1988; accepted January 13, 1989) Summary. This paper describes the design and construction of a viscometer of ZimmCrothers type, which allows very accurate viscosity measurements at various values of shear stressesusing only an extremely small rotor. Abstract We describe the design and construction of a Zimm Crothers type viscosimeter which permits us to get very accurate neasurements of viscosity at several values of the extremely low shear stress, using only one rotor.

1. Introduction One of the oldest techniques and used in the characterization of materials in solution is plyometrics viscometry. This is based on the fact that the presence of large particles dissolved or suspended in a liquid produced a radical change in the flow property of the system. A very important advantage of this technique is that the amount is determined experimentally, either viscous or the torque flow time is

directly

proportional

to

viscosity.

It may happen, however, that the viscosity of the polymer solution is dependent on the flow conditions of the instrument used: in these cases it is said that the non-Newtonian viscosity. This type of behavior is found mainly in solutions of highly asymmetric molecules rigid or flexible molecules in solutions of very high molecular weight. The capillary viscometer has proven to be a versatile and inexpensive,

however, due to progress in the study of biological macromolecules, has been found that many of these molecules are degraded under the action of even small shear forces found in the viscometers capillaries. Furthermore, some biological and synthetic molecules have non-Newtonian behavior when subjected to shear stresses experienced in regular sized capillaries.

FIGURE 1. The diagram shows the position of the rotor in the stator. 2. Design and construction The viscometer of Zimm-Crothers type [1], is a concentric cylinder viscometer, which is made entirely of glass, this feature provides the facility to work with almost any solvent. The outer cylinder (called the stator) remains fixed, while the inner cylinder (called the rotor) is rotating (Fig.1). At the bottom of the stator was placed a tube for introducing the sample is from the bottom of the viscometer. This device also facilitate filling, very accurately adjusts the height of the rotor on the stator core to be reproducible in the viscosity measurements, in general, the relative viscosity measurements have an accuracy of no more than 0.2% . All the viscometer is introduced into a heating jacket (Fig. 2) which allows the device to operate at different temperatures. As temperature control was used brand Haake recirculating bath with platinum resistance control, which

In view of this, there is need for a viscosity comparable to convenience and availability of a capillary viscometer, but operating at high shear rates of several orders of magnitude lower than the capillary. The instrument described herein is cheap, puts the solution in contact with only glass, runs at different shear stresses and has been used in cutting forces from 0.003 to 0.0008 dynes/cm2, which are several orders of magnitude less than commonly, used capillary viscometers.

controls with 0.05C.

accuracy

of

The viscometer should be mounted rigidly to preserve the geometry of the system. For this is supported with a nylon ring which is mounted on a bracket that allows five movements: first, the position of the viscosity on the external magnetic field is carried out through three platforms that move in the x - y z; second, the orientation thereof with respect to the magnet takes place by three screws placed in the nylon ring which allow movement zenithal and azimuthal (, ) (Fig. 2). It is important to note that the alignment of the viscometer with respect to the external magnetic field is vital to prevent movement of precession of the rotor.

FIGURE 2. The figure shows a cross section of the concentric cylinder viscometer and the description of its components.

By determining the viscosity is directly proportional to the time of revolution of the rotor as shown in the following expression: =

where P is the period of revolution for the solution to the solvent P0 and Pm to the external magnetic field. In our case having us that Pm = 0.1 second, thus a negligible amount is about P which is on the order of 300 seconds and P0 is the order of 90 seconds. To determine this period of revolution is made a small mark on the aluminum which is observed using a cathetometer, which is fixed to the worktable. Was used additionally an electronic counting, which operates in the following manner: a disk mounted with regularly spaced perforations on the

synchronous motor, and through an optocoupler mounted on the base of the viscometer (Fig. 2), the frequency was measured angle of rotation of the disc which resulted to be of 16.4-Hz, the signal obtained by rotating the disc is sent to an electronic counter, the reading of this is proportional to the viscosity of the solution in the viscometer. In Fig 3 shows a photograph of the instrument, and in Figs. 4a and 4b show schematic diagrams of electronics involved in this device. It is very important to keep a careful cleaning of the rotor in operation, it should not be touched with fingers while the viscometer is placed in, as this will cause problems in flotation and centered.

supported solely by flotation, can be used only a single rotor with liquids whose densities vary in a range of less than five percent. Fig 5 shows a schematic diagram of the experimental equipment and Figs. 6 and 7 show graphs of the calibration curves of viscosity for toluene and carbon tetrachloride, respectively. In Tables I, II, III summarizes some of the physical characteristics of the instrument. There have been several attempts by other authors [2, 3], in order to automate this instrument by adding optical devices, which allow more precise measurements.

Figure 3. The photograph shows the viscometer mounted on its base. It should be noted that the density of the liquid is very important in the use of this viscometer, because the rotor is

3. Experimental results. As mentioned above, some of the systems suitable for use in this type viscometers are those in which the molecules are asymmetrical, or polymer molecules which have the form of rigid rods, this is because the analysis of viscometer these solutions must be made extremely low cutting speed. Because of this, we used this type viscometer on solutions of poly(butylisocyanate) in carbon

tetrachloride (CCl4 PBIC on. Molecules of poly-(butylisocyanate) for not too high molecular weights (less than 105) have the form rigid rod. Due to the asymmetrical shape of the molecules, they have a phase transition, which was predicted by Flory [4] of an isotropic state in which all the molecules have random orientations to a nematic state in which there is a direction privileged along which the polymer chains tend to align.

This phase transition modifies the viscosity of the solution, and is intended to detect this by viscometric measurements. However, the viscosity must
Perforated disc

output

FIGURE 4a. The photo detector output signal is a square type of 0-5V.

FIGURE 4b. Electronics viscometer.

concentric

cylinder

Have very low shear for the velocity field does not induce the phase transition. Two solutions were prepared in CCl4 PBIC. Was analyzed each of these solutions at different temperatures in the range of 18C to 42C. In Figure 8a shows a graph of experimental results obtained for the system in CCI4 PBIC. Clearly shows that there is a discontinuity in the viscosity when the temperature changes. This graph was made at a concentration of 8.6 x 10-4g / g. In Figure 8b shows the detail of the transition for the same system at a concentration of 9x10-4g/g. FIGURE 5. The figure shows the experimental setup used.

FIGURE

6. Calibration

curve

of

toluene.

FIGURE 7. Calibration curve for carbon tetrachloride.

FIGURE 8A. Log graph of viscosity vs. reciprocal temperature for the solution-CCI4 PBIC the concentration of 8.6x10-4g/g.

FIGURE 8. Log graph of viscosity vs. reciprocal temperature for the solution-CCI4 PBlC the -4g/g. concentration 9.0x10

TABLE 1. Physical data of the stator and rotor comprising the concentric cylinder viscometer.

TABLE 2. Details of the aluminum core of the rotor.

TABLE 3. Comparative data between the concentric cylinder viscometer and a capillary viscometer typical.

4. Conclusions The concentric cylinder viscometer presented here, despite being a little more difficult than using a capillary viscometer, practically does not disturb the system under study, the shear so small that they can be obtained with this instrument at all, in some cases , the only means which can measure the viscosity of solutions or suspensions of large particles.

5. References: 1. H. H. Zimm & C.M.Crothers, Proc. Nat. Acad. Sci. 48 (1962) 905. 2. W. H. J. Stork & H. Vroome, J. Phys. E: Sci lnst 5 (1972) 314. 3. H. J. Seherr, H. C. Vautine & L.P. Witnaver, J. Phys E: Sci Inst 3 (1970) 322. 4. P. J. Flory, Proc. Roy. Soc. London A234 (1956) 73.