CA1219146A - Viscometer - Google Patents
ViscometerInfo
- Publication number
- CA1219146A CA1219146A CA000456144A CA456144A CA1219146A CA 1219146 A CA1219146 A CA 1219146A CA 000456144 A CA000456144 A CA 000456144A CA 456144 A CA456144 A CA 456144A CA 1219146 A CA1219146 A CA 1219146A
- Authority
- CA
- Canada
- Prior art keywords
- arm
- bight
- viscometer
- capillary
- stopper
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/02—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material
- G01N11/04—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture
- G01N11/06—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture by timing the outflow of a known quantity
Abstract
Abstract of the Disclosure A viscometer for measuring the viscosity of volatile liquids or liquids that are easily contaminated in the air, is disclosed. The viscometer is of the capillary type and includes a U-shaped tube with a capillary adjacent the bight in one arm and a collector adjacent the bight in the other arm. In addition, the arm containing the capillary has two bulbs in series above the capillary and a stopcock adjacent the upper end. The other arm is equipped with a reservoir for a liquid sample to be tested, a branch passage adjacent the top and a plug valve for closing off the arm below the branch passage. The two arms are joined by a bypass above the reservoir and the bulbs. A stopcock is included in the bypass.
Description
~2~ 46 The present inven-tion relates to viscometers and more particularly to viscometers for measuring the viscosity of vola tile liquid or liquids that are easily contaminated in the air.
Methods of measuring viscosities of volatile and hygro-scopic liquids are not properly described in the litera-ture. Ba]l type viscometers do not provide the required accuracy, and are not suitable for such systems. Capillary viscometers, based on the Ostwald type have been used for measurement on such mixtures, bu-t the data is unreliable and of questionable validity. The major limitiations of existing capillary type viscome-ters when dea]ing with volatile and readily contaminated liquids are:
a) The apparatus is an open sys-tem, leading to the con-tamination of the test sample.
b) A considerable 1oss of solvent and solute is possible, particularly where these are volatile.
c) It is difficult to introduce highly volatile solute and gases.
The present invention proposes an apparatus designed for kinematic viscosity measurements of liquid systems involving very hygroscopic solvents and volatile so]utes such as a gas.
According to the present invention there is provided a viscometer comprising a substantially U~shaped tube having a bight and a first and second arm, a capillary in the first arm adjacent the bight, a stopper for each arm remote from the bight, a branch passage joining the first arm between the stopper and the capillary to the second arm between the stopper and the bight, and a valve in the branch passage.
The apparatus is a modification of the known Cannon-Fenske ..
4~
~2~
type capi]lary viscometer~ ~Iowever, the viscome-ter may be com-pletely closed against the atmosphere when in use so as to prevent contamination or the loss of volati]e components.
Preferably, -the apparatus includes a reservoir for liquid that is branched off the second arm between the stopper and the bight. A liquid can be in-troduced to the reservoir and then frozen while the viscometer is subjected -to a vacuum to remove contaminants from the viscometer. The reservoir is also useful for degassing the liquid by repeated freezing and thawing.
A collector may be employed in the second arm between the stopper and the bight. This is in the form of a bulb-type enlarge-ment in the arm.
In most preferred embodiments, the first arm includes two bulbs, one directly above the capillary and the other spaced slightly above the first bulb. Two marks may -then be provided on the first tube on opposite sides of the first bulb. In use of the viscometer, the time for flow be-tween the two marks is taken as in measure of the viscositiy.
To facilitate the introduction of liquids, the second arm is preferably provided with a branch passage and a stopper in the form of a plug valve for closing the second arm below the branch passage.
The accompanying drawiny illustrates an exemplary embodi-ment of the present invention.
Referring to the drawing, there is illustrated a viscometer 10, the main component of which is a glass tube 12 formed into a generally U-shape with a first arm 14, a second arm 16 and a bight 18 joining the two arms. The first arm 14 has a capillary section 20 leading from the bight ~8. The capillary leads into a bulb 22 which, in turn, leads to a second bulb 2~ throu~h a neck 26 in the ~914~
tube. Adjacent its upper end, 1-he first arm 14 is equipped with a stopcock 28.
The second arm 16 has an enlarged collector 30 adjacent the bight and a pear-shaped reservoir 32 branching off the arm 16 above the collector. At its upper end, -the second arm 16 has a branch passage 34 ending in a ground glass joint 36. A rotary stopper 38 in the form of a plug valve is fi-tted to the end of the arm 16. When the stopper 38 is closed, its pluq 40 engages a seat 42 in the arm 16 to close off the arm 16 below the branch passage 34. The two arms 12 and 14 are bridged by a branch passage 44 leading from a position on the first arm 14 between the stopcock 28 and the second bulb 24 to a position on the second arm 16 between the valve sea-t 42 and the reservoir 32. The branch passage 44 is equipped with a stopcock 46.
To use the described viscometer, a gas tight syringe is connected to the outlet of the stopcock 28 by a short piece of silicon rubber tubing~ The stopcocks 28 and 46 are slightly greased and the clean, dry viscometer assembly is weighed.
With the stopcocks 28 and 46 and the stopper 38 open, the instrument is placed in an argon glove box. The required volume of high purity liquid test sample is introduced into the pear shaped reservoir 32 through the branch passage 34 of the second arm 16. The stopcocks 28 and 46 and the rotary stopper 38 are closed and -the unit is removed from the glove box. A vacuum line is then connected to the ground glass joint 36 and the liquid is frozen, for example by submerging the reservoir in liquid nitrogen. Opening the rotary stopper 38 allows the vacuum to draw off any gases in the viscometer. If desired, the solvent .
9~
may be degassed by closing the rotary stopper 38, thawing and s~bsequen'~ly free~irlcl the sample and reopenin(f the rotary s-topper 38 to draw off ~ny gases. The procedure may be repeated a numher of tlmes if necessary.
After any necessary de~assing has been completed, the rotary stopper 38 is closed and the viscometer is removed fron-l-the vacuum line. The sample in the reservoir 32 is melted and poured from the reservoir 32 into the collector 30 and the hight 18 of the tube tube 12~ The viscometer is then set in a thermo-staticly con-trolled bath with the capillary -tube 20 in a vertical orientation. The vertical orientation is not critical, but it is ideal. The orientation should, in any event, remain the same for all test runs with the viscometer.
Once the viscometer has attained temperature equilibrium, the stopcock 28 is opened and the syringe is used to draw the liquid sample from the collector 32 up the arm 14 past a mark 48 on the neck 26 between the bulbs 22 and 24. The stopcock 46 is then opened and the vapour drawn into the syringe is slowly pushed back into the viscometer with the syringe. The stopcock 28 is then closed and the time for flow between the mark 48 and a mark 50 on the tube immediately below the bulb 22 is taken as a measure of viscosity. The procedure can be repeated for con-sistency. If a volatile component, such as a gas, is to be added to the liquid sample, the viscometer is weighed in order to determine the initial weight of liquid. The liquid in the visco-meter is transferred into the reservoir 32 by slowly tilting the viscometer. The liquid is then frozen. The stopcocks S~ and S~
remain closed and the rotary stopper 38 is opened to admit the solute gas. The rotary stopper 38 is then closed. The amount of gas transferred can be determined from the weight of the assembly.
9~4~
The viscosity of the solution can then he determined as described above. The procedure can be continued for further incremental additions of solute gas.
Methods of measuring viscosities of volatile and hygro-scopic liquids are not properly described in the litera-ture. Ba]l type viscometers do not provide the required accuracy, and are not suitable for such systems. Capillary viscometers, based on the Ostwald type have been used for measurement on such mixtures, bu-t the data is unreliable and of questionable validity. The major limitiations of existing capillary type viscome-ters when dea]ing with volatile and readily contaminated liquids are:
a) The apparatus is an open sys-tem, leading to the con-tamination of the test sample.
b) A considerable 1oss of solvent and solute is possible, particularly where these are volatile.
c) It is difficult to introduce highly volatile solute and gases.
The present invention proposes an apparatus designed for kinematic viscosity measurements of liquid systems involving very hygroscopic solvents and volatile so]utes such as a gas.
According to the present invention there is provided a viscometer comprising a substantially U~shaped tube having a bight and a first and second arm, a capillary in the first arm adjacent the bight, a stopper for each arm remote from the bight, a branch passage joining the first arm between the stopper and the capillary to the second arm between the stopper and the bight, and a valve in the branch passage.
The apparatus is a modification of the known Cannon-Fenske ..
4~
~2~
type capi]lary viscometer~ ~Iowever, the viscome-ter may be com-pletely closed against the atmosphere when in use so as to prevent contamination or the loss of volati]e components.
Preferably, -the apparatus includes a reservoir for liquid that is branched off the second arm between the stopper and the bight. A liquid can be in-troduced to the reservoir and then frozen while the viscometer is subjected -to a vacuum to remove contaminants from the viscometer. The reservoir is also useful for degassing the liquid by repeated freezing and thawing.
A collector may be employed in the second arm between the stopper and the bight. This is in the form of a bulb-type enlarge-ment in the arm.
In most preferred embodiments, the first arm includes two bulbs, one directly above the capillary and the other spaced slightly above the first bulb. Two marks may -then be provided on the first tube on opposite sides of the first bulb. In use of the viscometer, the time for flow be-tween the two marks is taken as in measure of the viscositiy.
To facilitate the introduction of liquids, the second arm is preferably provided with a branch passage and a stopper in the form of a plug valve for closing the second arm below the branch passage.
The accompanying drawiny illustrates an exemplary embodi-ment of the present invention.
Referring to the drawing, there is illustrated a viscometer 10, the main component of which is a glass tube 12 formed into a generally U-shape with a first arm 14, a second arm 16 and a bight 18 joining the two arms. The first arm 14 has a capillary section 20 leading from the bight ~8. The capillary leads into a bulb 22 which, in turn, leads to a second bulb 2~ throu~h a neck 26 in the ~914~
tube. Adjacent its upper end, 1-he first arm 14 is equipped with a stopcock 28.
The second arm 16 has an enlarged collector 30 adjacent the bight and a pear-shaped reservoir 32 branching off the arm 16 above the collector. At its upper end, -the second arm 16 has a branch passage 34 ending in a ground glass joint 36. A rotary stopper 38 in the form of a plug valve is fi-tted to the end of the arm 16. When the stopper 38 is closed, its pluq 40 engages a seat 42 in the arm 16 to close off the arm 16 below the branch passage 34. The two arms 12 and 14 are bridged by a branch passage 44 leading from a position on the first arm 14 between the stopcock 28 and the second bulb 24 to a position on the second arm 16 between the valve sea-t 42 and the reservoir 32. The branch passage 44 is equipped with a stopcock 46.
To use the described viscometer, a gas tight syringe is connected to the outlet of the stopcock 28 by a short piece of silicon rubber tubing~ The stopcocks 28 and 46 are slightly greased and the clean, dry viscometer assembly is weighed.
With the stopcocks 28 and 46 and the stopper 38 open, the instrument is placed in an argon glove box. The required volume of high purity liquid test sample is introduced into the pear shaped reservoir 32 through the branch passage 34 of the second arm 16. The stopcocks 28 and 46 and the rotary stopper 38 are closed and -the unit is removed from the glove box. A vacuum line is then connected to the ground glass joint 36 and the liquid is frozen, for example by submerging the reservoir in liquid nitrogen. Opening the rotary stopper 38 allows the vacuum to draw off any gases in the viscometer. If desired, the solvent .
9~
may be degassed by closing the rotary stopper 38, thawing and s~bsequen'~ly free~irlcl the sample and reopenin(f the rotary s-topper 38 to draw off ~ny gases. The procedure may be repeated a numher of tlmes if necessary.
After any necessary de~assing has been completed, the rotary stopper 38 is closed and the viscometer is removed fron-l-the vacuum line. The sample in the reservoir 32 is melted and poured from the reservoir 32 into the collector 30 and the hight 18 of the tube tube 12~ The viscometer is then set in a thermo-staticly con-trolled bath with the capillary -tube 20 in a vertical orientation. The vertical orientation is not critical, but it is ideal. The orientation should, in any event, remain the same for all test runs with the viscometer.
Once the viscometer has attained temperature equilibrium, the stopcock 28 is opened and the syringe is used to draw the liquid sample from the collector 32 up the arm 14 past a mark 48 on the neck 26 between the bulbs 22 and 24. The stopcock 46 is then opened and the vapour drawn into the syringe is slowly pushed back into the viscometer with the syringe. The stopcock 28 is then closed and the time for flow between the mark 48 and a mark 50 on the tube immediately below the bulb 22 is taken as a measure of viscosity. The procedure can be repeated for con-sistency. If a volatile component, such as a gas, is to be added to the liquid sample, the viscometer is weighed in order to determine the initial weight of liquid. The liquid in the visco-meter is transferred into the reservoir 32 by slowly tilting the viscometer. The liquid is then frozen. The stopcocks S~ and S~
remain closed and the rotary stopper 38 is opened to admit the solute gas. The rotary stopper 38 is then closed. The amount of gas transferred can be determined from the weight of the assembly.
9~4~
The viscosity of the solution can then he determined as described above. The procedure can be continued for further incremental additions of solute gas.
Claims (7)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A viscometer comprising a substantially U-shaped tube having a bight and a first and second arms, a capillary in the first arm adjacent the bight, a stopper for each arm remote from the bight, a branch passage joining the first arm between the stopper and the capillary to the second arm between the stopper and the bight, and a valve in the branch passage.
2. A viscometer according to claim 1, including a reservoir for liquid branched off the second arm between the stopper and the bight.
3. A viscometer according to claim 2, including a collector in the second arm between the reservoir and the bight.
4. A viscometer according to claim 3, including a first bulb in the first arm above and adjacent the capillary.
5. A viscometer according to claim 4, including a second bulb in the first arm above the first bulb.
6. A viscometer according to claim 4, or 5, including two marks, on the first arm, adjacent and on opposite sides of the first bulb.
7. A viscometer according to claim 1, 3 or 5, including a branch passage leading from the second arm and wherein the stopper for the second arm comprises a plug valve for closing the second arm below the branch passage.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000456144A CA1219146A (en) | 1984-06-08 | 1984-06-08 | Viscometer |
| US06/737,844 US4583395A (en) | 1984-06-08 | 1985-05-24 | Viscometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000456144A CA1219146A (en) | 1984-06-08 | 1984-06-08 | Viscometer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1219146A true CA1219146A (en) | 1987-03-17 |
Family
ID=4128055
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000456144A Expired CA1219146A (en) | 1984-06-08 | 1984-06-08 | Viscometer |
Country Status (2)
| Country | Link |
|---|---|
| US (1) | US4583395A (en) |
| CA (1) | CA1219146A (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6182503B1 (en) * | 1999-07-01 | 2001-02-06 | Rheometric Scientific, Inc. | On-line rheological measurement for process control |
| US7832257B2 (en) * | 2007-10-05 | 2010-11-16 | Halliburton Energy Services Inc. | Determining fluid rheological properties |
| US8047059B2 (en) * | 2008-09-10 | 2011-11-01 | Cannon Instrument Company | Viscometer with integral sample retention reservoir |
| EP2249142A1 (en) * | 2009-05-06 | 2010-11-10 | Poulten Selfe & Lee Ltd. | A viscometer and a method for operating the same |
| WO2015166443A2 (en) * | 2014-04-30 | 2015-11-05 | Man Singh | An instrument and method for quantitative determination of physicochemical properties of chemical substances |
| CN107036936A (en) * | 2016-10-27 | 2017-08-11 | 北京润道油液监测技术有限公司 | Test system and its method of testing for testing oil sample kinematic viscosity |
Family Cites Families (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2048305A (en) * | 1932-03-24 | 1936-07-21 | Ubbelohde Leo | Viscosimeter |
| US2095282A (en) * | 1935-03-15 | 1937-10-12 | Standard Oil Co | Capillary viscometer |
| US2091896A (en) * | 1936-07-17 | 1937-08-31 | Ubbelohde Leo | Arrangement for testing the viscosity of liquid materials |
| US2343061A (en) * | 1943-10-29 | 1944-02-29 | Irany Ernest Paul | Capillary viscometer |
| US2805570A (en) * | 1954-04-30 | 1957-09-10 | Michael R Cannon | Viscometer |
| DE1032576B (en) * | 1955-08-13 | 1958-06-19 | Jenaer Glaswerk Schott & Gen | Viscometers, especially capillary viscometers |
| US3277694A (en) * | 1965-08-20 | 1966-10-11 | Cannon Instr Company | Viscometer |
| US3559463A (en) * | 1969-06-02 | 1971-02-02 | Phoenix Chemical Lab Inc | Viscometers |
| CH519168A (en) * | 1970-01-22 | 1972-02-15 | Ciba Geigy Ag | Capillary viscometer |
| CS172998B2 (en) * | 1974-07-16 | 1977-01-28 | ||
| DE2442943A1 (en) * | 1974-09-07 | 1975-04-17 | Seaplan Elekt Gmbh & Co Kg | Viscosity meter using vertical tubes - includes washing, drying and filling arrangement for a capillary viscosity meter |
| NL7602153A (en) * | 1975-03-07 | 1976-09-09 | Hoechst Ag | MODIFIED UBBELOHDE VISCOSITY METER. |
| FR2373050A1 (en) * | 1976-12-06 | 1978-06-30 | Electronique Nucleaire Soc | Viscometer which need not be inverted to empty - comprises reservoir with filling tube and viscometer pipette, incorporating emptying tube connected to vacuum |
| DE2950010A1 (en) * | 1979-12-12 | 1981-06-19 | Bayer Ag, 5090 Leverkusen | Viscosimeter allowing automatic operation - has pressure equalisation tube leading to measuring chamber formed by upper extension of capillary |
| DE3014705C2 (en) * | 1980-04-17 | 1983-06-01 | Bayer Ag, 5090 Leverkusen | Viscometer |
-
1984
- 1984-06-08 CA CA000456144A patent/CA1219146A/en not_active Expired
-
1985
- 1985-05-24 US US06/737,844 patent/US4583395A/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| US4583395A (en) | 1986-04-22 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| MKEX | Expiry |