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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 Zimm-
Crothers 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                              directly   proportional   to   viscosity.

One of the oldest techniques and used           It may happen, however, that the
in the characterization of materials in         viscosity of the polymer solution is
solution is plyometrics viscometry. This        dependent on the flow conditions of the
is based on the fact that the presence          instrument used: in these cases it is
of large particles dissolved or                 said     that     the     non-Newtonian
suspended in a liquid produced a                viscosity. This type of behavior is found
radical change in the flow property             mainly in solutions of highly asymmetric
of      the system.                             molecules rigid or flexible molecules in
                                                solutions of very high molecular
A very important advantage of this                     weight.
technique is that the amount is
determined experimentally, either               The capillary viscometer has proven to
viscous or the torque flow time is              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            FIGURE 1. The diagram shows the
viscometers capillaries. Furthermore,      position of the rotor in   the
some       biological   and synthetic             stator.
molecules       have      non-Newtonian
behavior when subjected to shear             2. Design and construction
stresses experienced in regular sized
capillaries.                                 The viscometer of Zimm-Crothers
                                             type [1], is a concentric cylinder
                                             viscometer, which is made entirely
In view of this, there is need for a         of glass, this feature provides the
viscosity comparable to convenience          facility to work with almost      any
and availability of a capillary                  solvent.
viscometer, but operating at high shear      The outer cylinder (called the stator)
rates of several orders of magnitude         remains fixed, while the inner
       lower than the capillary.             cylinder (called the rotor) is rotating
                                                 (Fig.1).
The instrument described herein is
cheap, puts the solution in contact with     At the bottom of the stator was
only glass, runs at different shear          placed a tube for introducing the
stresses and has been used in cutting        sample is from the bottom of the
forces from 0.003 to 0.0008 dynes/cm2,       viscometer. This       device     also
which are several orders of magnitude        facilitate filling, very accurately
less than commonly, used capillary           adjusts the height of the rotor on the
       viscometers.                          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
controls   with       accuracy     of
   ±0.05°C.

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 (θ, φ) (Fig.     FIGURE 2. The figure shows a
2). It is important to note that the    cross section of the concentric
alignment of the viscometer with        cylinder viscometer and the
respect to the external magnetic        description of its components.
field is vital to prevent movement of
precession of the          rotor.
                                        where P is the period of revolution
                                        for the solution to the solvent P0 and
By determining the viscosity is         Pm to the external magnetic field. In
directly proportional to the time of    our case having us that Pm = 0.1
revolution of the rotor as shown in     second, thus a negligible amount is
the following expression:               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          supported solely by flotation, can be
   optocoupler mounted on the base of         used
   the viscometer (Fig. 2), the
   frequency was measured angle of               only a single rotor with liquids
   rotation of the disc which resulted to        whose densities vary in a range of
   be of 16.4-Hz, the signal obtained            less than five percent. Fig 5 shows
   by rotating the disc is sent to an            a schematic diagram of the
   electronic counter, the reading of            experimental equipment and Figs. 6
   this is proportional to the viscosity of      and 7 show graphs of the calibration
   the solution in the viscometer. In Fig        curves of viscosity for toluene and
   3 shows a photograph of the                   carbon tetrachloride, respectively. In
   instrument, and in Figs. 4a and 4b            Tables I, II, III summarizes some of
   show schematic diagrams of                    the physical characteristics of the
   electronics involved in this device.             instrument.

   It is very important to keep a careful        There have been several attempts
   cleaning of the rotor in operation, it        by other authors [2, 3], in order to
   should not be touched with fingers            automate this instrument by adding
   while the viscometer is placed in, as         optical devices, which allow more
   this will cause problems in flotation         precise             measurements.
   and         centered.




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.                              tetrachloride (CCl4 PBIC on.
                                                        Molecules of poly-(butylisocyanate)
  As mentioned above, some of the                       for not too high molecular weights
  systems suitable for use in this type                 (less than 105) have the form rigid
  viscometers are those in which the                        rod.
  molecules are asymmetrical, or
  polymer molecules which have the                      Due to the asymmetrical shape of
  form of rigid rods, this is because                   the molecules, they have a phase
  the analysis of viscometer these                      transition, which was predicted by
  solutions must be made extremely                      Flory [4] of an isotropic state in
  low          cutting          speed.                  which all the molecules have
                                                        random orientations to a nematic
  Because of this, we used this type                    state in which there is a
  viscometer on solutions of poly-                      direction privileged along which the
  (butylisocyanate)    in    carbon                     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         concentric    cylinder
     viscometer.
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 18°C to    42°C.

   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
                                                    concentration          9.0x10-4g/g.




TABLE 1. Physical data of the stator and      TABLE 2. Details of the aluminum
rotor comprising the concentric cylinder      core of the     rotor.
 viscometer.




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.

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35 2 0274(1)

  • 1. 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 Zimm- Crothers 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 directly proportional to viscosity. One of the oldest techniques and used It may happen, however, that the in the characterization of materials in viscosity of the polymer solution is solution is plyometrics viscometry. This dependent on the flow conditions of the is based on the fact that the presence instrument used: in these cases it is of large particles dissolved or said that the non-Newtonian suspended in a liquid produced a viscosity. This type of behavior is found radical change in the flow property mainly in solutions of highly asymmetric of the system. molecules rigid or flexible molecules in solutions of very high molecular A very important advantage of this weight. technique is that the amount is determined experimentally, either The capillary viscometer has proven to viscous or the torque flow time is be a versatile and inexpensive,
  • 2. 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 FIGURE 1. The diagram shows the viscometers capillaries. Furthermore, position of the rotor in the some biological and synthetic stator. molecules have non-Newtonian behavior when subjected to shear 2. Design and construction stresses experienced in regular sized capillaries. The viscometer of Zimm-Crothers type [1], is a concentric cylinder viscometer, which is made entirely In view of this, there is need for a of glass, this feature provides the viscosity comparable to convenience facility to work with almost any and availability of a capillary solvent. viscometer, but operating at high shear The outer cylinder (called the stator) rates of several orders of magnitude remains fixed, while the inner lower than the capillary. cylinder (called the rotor) is rotating (Fig.1). The instrument described herein is cheap, puts the solution in contact with At the bottom of the stator was only glass, runs at different shear placed a tube for introducing the stresses and has been used in cutting sample is from the bottom of the forces from 0.003 to 0.0008 dynes/cm2, viscometer. This device also which are several orders of magnitude facilitate filling, very accurately less than commonly, used capillary adjusts the height of the rotor on the viscometers. 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
  • 3. controls with accuracy of ±0.05°C. 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 (θ, φ) (Fig. FIGURE 2. The figure shows a 2). It is important to note that the cross section of the concentric alignment of the viscometer with cylinder viscometer and the respect to the external magnetic description of its components. field is vital to prevent movement of precession of the rotor. where P is the period of revolution for the solution to the solvent P0 and By determining the viscosity is Pm to the external magnetic field. In directly proportional to the time of our case having us that Pm = 0.1 revolution of the rotor as shown in second, thus a negligible amount is the following expression: 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
  • 4. synchronous motor, and through an supported solely by flotation, can be optocoupler mounted on the base of used the viscometer (Fig. 2), the frequency was measured angle of only a single rotor with liquids rotation of the disc which resulted to whose densities vary in a range of be of 16.4-Hz, the signal obtained less than five percent. Fig 5 shows by rotating the disc is sent to an a schematic diagram of the electronic counter, the reading of experimental equipment and Figs. 6 this is proportional to the viscosity of and 7 show graphs of the calibration the solution in the viscometer. In Fig curves of viscosity for toluene and 3 shows a photograph of the carbon tetrachloride, respectively. In instrument, and in Figs. 4a and 4b Tables I, II, III summarizes some of show schematic diagrams of the physical characteristics of the electronics involved in this device. instrument. It is very important to keep a careful There have been several attempts cleaning of the rotor in operation, it by other authors [2, 3], in order to should not be touched with fingers automate this instrument by adding while the viscometer is placed in, as optical devices, which allow more this will cause problems in flotation precise measurements. and centered. 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
  • 5. 3. Experimental results. tetrachloride (CCl4 PBIC on. Molecules of poly-(butylisocyanate) As mentioned above, some of the for not too high molecular weights systems suitable for use in this type (less than 105) have the form rigid viscometers are those in which the rod. molecules are asymmetrical, or polymer molecules which have the Due to the asymmetrical shape of form of rigid rods, this is because the molecules, they have a phase the analysis of viscometer these transition, which was predicted by solutions must be made extremely Flory [4] of an isotropic state in low cutting speed. which all the molecules have random orientations to a nematic Because of this, we used this type state in which there is a viscometer on solutions of poly- direction privileged along which the (butylisocyanate) in carbon 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 concentric cylinder viscometer.
  • 6. 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 18°C to 42°C. 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.
  • 7. FIGURE 8. Log graph of viscosity vs. reciprocal temperature for the solution-CCI4 PBlC the concentration 9.0x10-4g/g. TABLE 1. Physical data of the stator and TABLE 2. Details of the aluminum rotor comprising the concentric cylinder core of the rotor. viscometer. 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.
  • 8. 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.