U.S. patent number 3,864,962 [Application Number 05/349,842] was granted by the patent office on 1975-02-11 for capillary viscosimeter.
This patent grant is currently assigned to Ciba-Geigy AG. Invention is credited to Markus Jungo, Jean-Claude Lambiel, John-Hermann Stark.
United States Patent |
3,864,962 |
Stark , et al. |
February 11, 1975 |
CAPILLARY VISCOSIMETER
Abstract
A capillary viscosimeter of the type in which liquid is supplied
in excess to an overflow vessel upstream of the capillary during a
viscosity measurement and is discharged downstream of the capillary
into a measuring vessel is described in which the liquid discharges
into the measuring vessel from an overflow vessel which is
geometrically similar to or identical with the upstream overflow
vessel.
Inventors: |
Stark; John-Hermann (Marly,
CH), Lambiel; Jean-Claude (Marly, CH),
Jungo; Markus (Tafers, CH) |
Assignee: |
Ciba-Geigy AG (Basel,
CH)
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Family
ID: |
4290701 |
Appl.
No.: |
05/349,842 |
Filed: |
April 10, 1973 |
Foreign Application Priority Data
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Apr 10, 1972 [CH] |
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5265/72 |
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Current U.S.
Class: |
73/54.07 |
Current CPC
Class: |
G01N
11/06 (20130101) |
Current International
Class: |
G01N
11/00 (20060101); G01N 11/06 (20060101); G01n
011/06 () |
Field of
Search: |
;73/55,54,56 |
References Cited
[Referenced By]
U.S. Patent Documents
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3071961 |
January 1963 |
Heigl et al. |
3559463 |
February 1971 |
Tovrog et al. |
3699804 |
October 1972 |
Gassmann et al. |
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Foreign Patent Documents
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285,215 |
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Oct 1970 |
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OE |
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68,392 |
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Aug 1969 |
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DL |
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Other References
Lessing, I. W., Automatisierte Kapillarviskosimeter nach Ubbelohde
und Ostwald. Chemie-Ing. Techn. 42(20) p. 1274-1278, 1970..
|
Primary Examiner: Myracle; Jerry W.
Assistant Examiner: Roskos; Joseph W.
Attorney, Agent or Firm: Wenderoth, Lind & Ponack
Claims
What is claimed is:
1. A capillary viscosimeter, comprising:
a capillary through which liquid is arranged to flow during a
viscosity measurement;
an overflow vessel connected upstream of said capillary and adapted
to be supplied with an excess of said liquid during said viscosity
measurement;
a discharge overflow vessel connected downstream of said capillary
and arranged to discharge liquid which has passed through said
capillary by overflow;
a measuring vessel positioned to receive the overflow from said
discharge overflow vessel;
means within said measuring vessel for defining and sensing a lower
and a higher liquid level within said measuring vessel; and
time measuring means connected to said level defining and sensing
means for measuring the time interval required for the liquid level
in said measuring vessel to rise from said lower to said higher
level.
2. A capillary viscosimeter according to claim 1, wherein said
capillary forms part of a U-shaped tube, one end of which is
connected to the first mentioned overflow vessel, and the other end
of which is connected to said discharge overflow vessel.
3. A capillary viscosimeter according to claim 2, wherein said
discharge overflow vessel is directly connected to the downstream
side of said capillary.
4. The capillary viscosimeter as defined in claim 2, wherein said
U-shaped tube comprises two straight legs and a flexible tube
connecting the lower ends of said two straight legs, said two
straight legs being arranged to be adjustable in height relative to
each other.
5. A capillary viscosimeter as claimed in claim 1, wherein said
discharge overflow vessel is geometrically similar to said first
mentioned overflow vessel.
6. A capillary viscosimeter as claimed in claim 1, wherein
saiddischarge overflow vessel is geometrically identical to said
first mentioned overflow vessel.
7. A capillary viscosimeter according to claim 6, wherein both said
first mentioned overflow vessel and said discharge overflow vessel
consists of a funnel.
8. A capillary viscosimeter according to claim 6, wherein said
capillary forms part of a U-shaped tube, one end of which is
connected to the first mentioned overflow vessel, and the other end
of which is connected to said discharge overflow vessel.
9. A capillary viscosimeter according to claim 8, wherein said
discharge overflow vessel is directly connected to the downstream
side of said capillary.
10. The capillary viscosimeter as defined in claim 1, wherein each
of said liquid level defining and sensing means comprise an
electrode having one end communicating with the inside of said
measuring vessel and cooperating with a common electrode disposed
below said lower liquid level defining and sensing electrode, each
of said two electrodes forming with said common electrode and the
liquid therebetween a switch-on and a switch-off means,
respectively, for said time measuring means.
11. The capillary viscosimeter as defined in claim 10, wherein a
control and reset unit is associated to said time measuring means
and wherein said control and reset unit is controlled by a signal
derived from said switch-off means to reset said time measuring
means, to discharge said measuring vessel and to initiate a further
viscosity measurement.
12. A capillary viscosimeter, comprising:
a capillary through which liquid is arranged to flow during a
viscosity measurement;
an overflow vessel connected upstream of said capillary;
means for supplying excess of said liquid to said overflow vessel
whereby liquid overflows therefrom during a viscosity
measurement;
a discharge overflow vessel connected downstream of said capillary
and arranged to discharge liquid which has passed through said
capillary by overflow;
a measuring vessel positioned to receive the overflow from said
discharge overflow vessel;
means defining a lower and a higher liquid level in said measuring
vessel; and
time measuring means for measuring the time interval for the liquid
level in said measuring vessel to rise from said lower to said
higher level.
13. A capillary viscosimeter according to claim 12, wherein said
capillary forms part of a U-shaped tube, one end of which is
connected to the first mentioned overflow vessel, and the other end
of which is connected to said discharge overflow vessel.
14. A capillary viscosimeter according to claim 13, wherein said
discharge overflow vessel is directly connected to the downstream
side of said capillary.
15. The capillary viscosimeter as defined in claim 13, wherein said
discharge overflow vessel is connected directly to the downstream
end of said capillary.
16. The capillary viscosimeter as defined in claim 13, wherein said
U-shaped tube comprises two straight legs and a flexible tube
connecting the lower ends of said two straight legs, said two
straight legs being arranged to be adjustable in height relative to
each other.
17. The capillary viscosimeter as defined in claim 12 wherein said
discharge overflow vessel is geometrically similar to said first
mentioned overflow vessel.
Description
FIELD OF THE INVENTION
The present invention relates to a capillary viscosimeter of the
type in which an overflow vessel is connected upstream of the
capillary and is adapted to be supplied with excess liquid during a
viscosity measurement, and in which a measuring vessel is provided
for collecting liquid which has passed through the capillary.
BACKGROUND TO THE INVENTION
A capillary viscosimeter of this general kind is disclosed in
German Patent Specification No. 713,990. Such viscosimeters differ
from other capillary viscosimeters (for example Ubbelohde
viscosimeters and variations thereof such as that described by
Cannon in U.S. Pat. No. 2,805,570) by virtue of the fact that it is
not necessary for the liquid to flow twice through the measuring
capillary in performing a complete measuring cycle.
The known capillary viscosimeter of German Patent No. Specification
No. 713,990 comprises a vertical strand in which, as seen from top
to bottom, a storage vessel for the liquid to be measured is
followed by a drip capillary which in turn extends into a spherical
overflow vessel which is disposed upstream of the measuring
capillary proper. An overflow duct extends laterally from the
overflow vessel and the measuring capillary extends from the lowest
point of the overflow vessel. The lower end of the measuring
capillary directly opens into a zone of increased cross-section
which forms the upper end of a graduated measuring vessel. The said
upper end of the aforementioned measuring vessel is connected
through a rising pipeline to a manifold duct into which the
overflow duct from the overflow vessel also extends, the lower end
of the aforementioned manifold duct extending into a collecting
vessel.
The hydrostatic pressure which acts on the liquid column in the
measuring capillary of this arrangement is practically constant
because the difference of head between the (constant) level in the
overflow vessel and the meniscus which forms at the lower end of
the measuring capillary is constant. However, the hydrostatic
pressure is not the only force which acts on the liquid column and
is therefore not the only factor which influences the rate of flow
of the liquid through the measuring capillary per unit time. A
further force acts as a result of the surface tension of the liquid
itself particularly at the meniscus formed at the lower end of the
measuring capillary so that an additional correction is necessary
when working with the capillary viscosimeter of German Patent
Specification No. 713,990.
It is an object of the present invention to provide a capillary
viscosimeter in which the hydrostatic pressure across the capillary
may be maintained constant whilst avoiding surface tension effects
at the lower end of the capillary due to the formation of a
meniscus.
It is another object of this invention to provide a simple accurate
and reliable capillary viscosimeter.
These and other objects of the invention will become apparent from
the following detailed description when taken together with the
accompanying drawings.
SUMMARY OF THE INVENTION
The objects of this invention are obtained by a capillary
viscosimeter, comprising:
a capillary through which liquid is arranged to flow during a
viscosity measurement;
an overflow vessel connected upstream of said capillary and adapted
to be supplied with an excess of said liquid during a viscosity
measurement;
a discharge overflow vessel connected downstream of said capillary
and arranged to discharge liquid which has passed through said
capillary by overflow; and
a measuring vessel positioned to receive the overflow from said
discharge overflow vessel.
Preferably the two overflow vessels are geometrically similar or
better still geometrically identical. It is convenient if both
overflow vessels are funnel-shaped. In this case any forces acting
on the liquid column in the capillary and resulting from the
surface tension of the liquid will be cancelled.
The capillary is advantageously provided as part of a U-shaped
tube, the overflow vessels being connected to opposite ends
thereof. In this case, it is advantageous if the discharge overflow
vessel is connected directly downstream of the capillary. In other
words, this means that when seen in the flow direction, the
capillary is disposed in the rising branch of the U-shaped tube.
This enables any air bubbles that may be formed to rise freely into
the discharge overflow vessel without impairing the flow through
the capillary.
As will be readily understood, the time taken for a predetermined
volume of liquid to pass through the capillary provides a relative
indication of viscosity. Alternatively if the geometry of the
capillary is known, an absolute determination is possible.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic representation of a capillary viscosimeter
constructed in accordance with the present invention;
FIG. 2 shows schematically a variation of the capillary
viscosimeter adapted to periodically measure the viscosity of a
liquid which is obtained continuously or at regular intervals from
a storage vessel or a duct;
FIG. 3 schematically illustrates a modified capillary viscosimeter
adapted for periodic measurement of the viscosity of a measured
liquid specimen; and
FIG. 4 shows a further variation in schematic form.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring again to FIG. 1, there is shown diagrammatically an
embodiment of capillary viscosimeter comprising a U-shaped tube 1
which may be constructed of glass or some other material and is
disposed in a thermostatic bath which is not shown in the drawing.
A measuring capillary is shown at 2, and the upper end of that
branch of the U-shaped tube which contains the said measuring
capillary is provided with an overflow funnel 3 which opens into a
collecting vessel 5 here shown open-topped. The lower end of the
said collecting vessel is provided with a discharge connection 7.
The other branch of the U-shaped tube 1 is provided with a
similarly formed overflow funnel 4 which opens into a measuring
vessel 6, here shown open at the top. The lower end of the said
measuring vessel is provided with a discharge connection having a
closable tap 8. Contacts 9, 10, 11, shown in FIG. 1, are connected
via a line 12 of control conductors to an electric clock. The
contact 9 is arranged to function as a common terminal, the contact
10 to initiate timing and the contact 11 to cause the timing to
cease. In operation liquid is supplied to funnel 3 continuously and
in excess through the open top of vessel 5 so that it overflows
into the said vessel over the rim of funnel 3 and is discharged
through connection 7. The timing procedure may be repeated at will
by opening the tap 8, discharging the measuring vessel and then
closing the tap 8 again. Timing then occurs automatically.
FIG. 2 shows a variation of the capillary viscosimeter adapted to
periodically measure the viscosity of a liquid which is obtained
continuously or at regular intervals from a storage vessel or a
duct. In this embodiment the capillary is incorporated into the
shorter branch of the U-tube so that any bubbles occurring will
automatically escape through the capillary. The timing apparatus
and the discharge tap 8 are connected to control apparatus 14, 15
which is arranged to first open the discharge tap 8, then to close
the discharge tap, and periodically to initiate and complete the
timing operation in accordance with a preset cyclic timing
programme. A recorder 16 may be provided as shown for automatically
recording the measured times. The liquid whose viscosity is to be
measured is supplied to funnel 3 in excess from an inlet vessel
supplied in turn through a valve from the duct. The excess liquid
overflows from the rim of funnel 3 into vessel 5 as before and is
discharged through connection 7. The gas spaces in the closed top
vessels 5 and 6 are maintained at the same pressure.
The modified capillary viscosimeter schematically illustrated in
FIG. 3 is adapted for periodic measurement of the viscosity of a
measured liquid specimen which is returned into the storage vessel
after measurement is completed. To this end, the viscosimeter is
provided with two separate inlet vessels 34, 33 which may be
connected by ducts 38 and 39 to a remotely controlled valve 18 and
thence through a duct 37 to the vessel 5. In operation, a measured
liquid volume is first filled into one of the two vessels 33 or 34,
the valve 18 remaining closed for the time being. The said valve is
then opened and liquid begins to flow through the duct 37 into the
overflow funnel 3. The liquid flow through the duct 37 should
exceed the amount which is discharged through the capillary 2 so
that the funnel 3 is completely filled and overflows along its edge
into the vessel 5. The viscosimeter becomes filled with liquid to
the edge of the funnel 4 and liquid will then also overflow from
this funnel into the measuring vessel 6. The filling process is
completed when the entire supplied liquid volume has been
discharged from the vessel 33 or 34.
Each of the vessels 33, 34 is connected by a respective duct 27, 28
to a vacuum chamber 29. Each duct 27, 28 includes a respective
control valve 21, 22 and a pressure regulating valve 24, 23.
Further regulating valves 25 and 26 provide for regulation of the
pressure in ducts 28 and 27 relative to atmospheric. After the
filling process is complete valves 21 and 22 are opened under
control of the unit 15 to which they are connected by respective
lines such as 41 while valve 18 is automatically closed under
control of unit 15 via a line 40. A valve 20 is opened by control
of unit 15 via a line 42 to connect the interior of vessel 5 to
atmosphere via a pressure regulating valve 45. The liquid disposed
in the measuring vessel 6 is drawn back through a duct 35 into the
vessel 34 as a result of the negative pressure in the vessels 33
and 34 and the liquid which is disposed in the vessel 5 is drawn
through a duct 36 into the vessel 33. To this end, the valves 23,
24, 25, 26 and 45 are adjusted so that the correct pressure
conditions required for this operation are obtained in the vessels
33, 34 and 5. Due to the negative pressure which prevails in the
vessel 5 the liquid disposed in the right-hand branch of the
viscosimeter is simultaneously drawn back towards the capillary 2
so that any air bubbles which may be present in the instrument
escape through the overflow funnel 3. The back-drawing operation is
automatically complete as soon as the liquid level in the vessel 34
reaches a contact 32 provided for this purpose therein.
The instrument is then ready for measurement. The measurement is
started by first opening the valves 20, 21 and 22 to atmosphere.
The valve 18 is then opened and liquid begins to flow from the two
vessels 33 and 34 through the duct 37 into the funnel 3. The
measuring vessel 6 begins to fill after the overflow funnel 4 is
filled. Timing starts automatically as before when the contact 10
is reached and is completed when contact 11 is reached after which
the instrument is ready for a fresh cycle.
The valve 18 should be constructed so as to open its entire
cross-section when the valve is in the open state. This prevents
any rheological changes resulting from increased shear action on
the liquid as it flows through a restriction, since such changes
could falsify subsequent measurement. A magnetically operated tube
squeezing valve or a cock whose opening in the open state
corresponds to the full cross-section of the supply duct 37 are
suitable to this end.
The operation of the cycle, closing and opening of the various
valves and resetting of the timer to zero after a cycle has elapsed
are controlled by the control unit 15 while the time sequence of
the individual measuring cycles is controlled by a timer 116.
The valves 20, 21 and 22 may be three-way valves, and instead of
connecting them to atmosphere during the timing procedure, they may
be connected to a further chamber, not shown in the illustration,
but having a controlled pressure higher or lower than atmospheric.
The force acting on the liquid and conveying it through the
measuring capillary may thus be altered at will and measurements
may be performed at different rates of shear which may be freely
selected. This may also be achieved in another way by connecting
the two branches of the viscosimeter with a flexible tube by means
of which the difference of head between the upper edges of the two
overflow funnels 3 and 4 may be altered as desired.
FIG. 4 shows a further variation, in which a sample of the liquid
whose viscosity is being measured may be returned by means of the
pump 46 into inlet vessel 34. The system is completely enclosed so
as to avoid any loss of liquid due to evaporation. The pump
operates continuously and the measuring process is subdivided into
two operating cycles by periodic resetting of the valve 8 which
here controls discharge both from vessel 6 and from vessel 5.
Cycle 1 (measuring cycle)
The vessel 34 is filled with liquid to a specific level; the liquid
level in the vessel 5 is slightly below the edge of the inlet
funnel 3. The valve 8 is open in the direction towards the vessel 5
but closed in the direction towards the vessel 6. The liquid
disposed in the vessel 5 is pumped back into the vessel 34 from
which it flows downwardly into the inlet funnel 3 in excess. From
funnel 3 the liquid flows through the U-tube 1 and the capillary 2
to the overflow funnel 4 so that the measuring vessel 6 is
gradually filled and the contacts 10 and 11 for controlling timing
are successively actuated as before. In the meantime the vessel 5
is emptied by the pump because the amount of liquid which overflows
from the funnel 3 into vessel 5 is less than the delivery capacity
of the pump. After timing is completed a control device 14 opens
the valve 8 towards the vessel 6 and closes it in the direction
towards the vessel 5.
Cycle 2 (return)
The action of the pump returns the liquid from the measuring vessel
6 into the inlet vessel 34. Liquid continues to be discharged from
the vessel 34 to the inlet funnel 3. Since the valve 8 to the duct
7 is closed the vessel 5 is filled by the liquid which overflows
from the funnel 3. The measuring vessel 6 must continue to be
emptied for as long as the liquid level in vessel 5 is still below
the edge of the funnel 3. The time measuring device 13 is reset to
zero by a control device 16. The control device 14 is arranged to
switch the valve 8 into the other operating position and the
measuring cycle is then restarted.
The two vessels 5 and 6 remain connected by a duct 47 during both
operating cycles so that there is a constant pressure compensation
between both vessels.
* * * * *