WO1997009602A1 - Rubber testing - Google Patents
Rubber testing Download PDFInfo
- Publication number
- WO1997009602A1 WO1997009602A1 PCT/GB1996/002201 GB9602201W WO9709602A1 WO 1997009602 A1 WO1997009602 A1 WO 1997009602A1 GB 9602201 W GB9602201 W GB 9602201W WO 9709602 A1 WO9709602 A1 WO 9709602A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- sample
- rubber
- annular space
- measurements
- members
- Prior art date
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
- G01N11/10—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
- G01N11/14—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by using rotary bodies, e.g. vane
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/44—Resins; rubber; leather
Definitions
- This invention relates to methods of testing rubber and apparatus for carrying out such methods.
- a method of testing rubber wherein a sample of the rubber is entered to fill an annular space defined between coaxial cylindrical surfaces of two relatively- rotatable members, and measurements of the viscous torque of the sample and the force it exerts axially of the annular space during relative rotation of the two members is derived to provide a measure of quality of the sample.
- a multiplicity of measurements of the viscous torque and the axial force may be derived during a period of relative rotation of the two members ⁇ o as to provide time-related characteristic ⁇ dependent re ⁇ pectively upon the vi ⁇ cosity and the elasticity of recovery of the sample. Determination of acceptability or otherwise of the sample may then be made in dependence upon the degree of conformity of the characteristics to predetermined criteria.
- the measurements may be made for each of a series of samples taken at successive stages of manufacture of a rubber product.
- the samples may be taken from the raw rubber, from the product of compounding in a primary masticator-mixer, and from the product of extrusion, calendering or injection-moulding of the compounded rubber.
- the method of testing is desirably carried out at a temperature and for a duration comparable with the temperature and duration of the next proce ⁇ ing stage to which the rubber from which the ⁇ ample was taken, is to be submitted.
- the temperature in primary compounding is generally in the range 130 to 150 degrees Celsius for natural rubber, 140 to 170 degrees Cel ⁇ ius for general- purpose synthetic rubber ⁇ , and 100 to 120 degree ⁇ Celsius for butyl rubbers, and may exceed 200 degrees Celsius for high temperature rubbers.
- the ⁇ peed of relative rotation of the two member ⁇ i ⁇ desirably such as to give rise to a rate of shear within the sample comparable with that to which the rubber is to be submitted in the next processing stage.
- the speed of relative rotation of the two member ⁇ may in thi ⁇ respect be within the range 50 to 1,000 revolutions per minute, or more especially within the range 100 to 500 revolutions per minute.
- apparatu ⁇ for te ⁇ ting a ⁇ ample of rubber compri ⁇ es two relatively-rotatable members having coaxial cylindrical ⁇ urface ⁇ to define an annular ⁇ pace between the two members for receiving the sample, means for rotating the two members relative to one another, mean ⁇ to derive a mea ⁇ urement dependent upon the viscous torque of the sample, and means to derive a mea ⁇ urement dependent upon the force exerted axially of the annular ⁇ pace during relative rotation of the two members.
- the apparatus may include means for heating the sample within the annular space, and the axial length of the annular space may be substantially larger than its radial width to minimise end effects.
- the apparatu ⁇ may include means for blocking one end of the annular space during relative rotation of the two members, and in these circumstance ⁇ the mean ⁇ for deriving a measurement dependent upon axial force may be responsive to the force exerted axially by the sample, at the other end of the space.
- a loading chamber for receiving the sample of rubber may be coupled to the annular space via a plurality of passages that open axially into said one end of the space.
- Ram means may then be provided for forcing the sample from the loading chamber into the annular space via the ⁇ e passages.
- Figure 1 is a ⁇ ectional ⁇ ide elevation of part of the rubber-testing apparatus according to the invention
- Figure ⁇ 2 and 3 are enlarged views of the region designated A in Figure 1 during different stages of the rubber-testing method of the invention.
- Figures 4 and 5 are illustrative of characteristics plotted from mea ⁇ urements taken during operation of the rubber-testing apparatus of Figure 1.
- the rubber-testing apparatus involves an annular ⁇ pace 1 for receiving the sample of rubber to be tested.
- the ⁇ pace 1 i ⁇ defined between coaxial cylindrical surfaces 2 and 3 respectively of a rotor 4 and stator 5.
- the rotor 4 is mounted on a shaft 6 for rotation relative to the stator 5 by a motor (not shown) , and the sample is entered into the space 1 from a loading chamber 7.
- Thi ⁇ enables the top of the space 1 to be completely closed off when it is full.
- the measurements represented by this signal are plotted again ⁇ t time during rotation of the rotor 4, as also are measurements represented by an electric signal from a torque ⁇ ensor 15 on the ⁇ haft 6.
- the re ⁇ ultant time-related characteristics provide an indication of the quality of the sample.
- the cylindrical surfaces 2 and 3 of the rotor 4 and stator 5 are ribbed parallel to the rotational axis of the shaft 6 ⁇ o that the rotational torque measured by the torque sensor 15 is dependent upon the viscosity V of the sample rubber.
- the load cell 14, responds to the force which acts parallel to the shaft 6 in consequence of the ⁇ hear brought about in the ⁇ ample by the rotation; thi ⁇ force is dependent upon the elasticity of recovery E of the sample rubber.
- Figures 4 and 5 illustrate, respectively, visco ⁇ ity V and elasticity E characteristics 16 and 17 which have been plotted in accordance with the ⁇ ignal ⁇ derived from the torque sensor 15 and the load cell 14 during testing of a rubber sample.
- the sample may be of raw rubber (natural or synthetic) taken from a bale of rubber for the purpose of assessing its quality and therefore acceptability or otherwise for processing.
- the viscosity and elasticity characteristics are plotted for the sample over a period of some minutes with the temperature of the sample regulated by means of a heater 18 in thermal contact with the stator 5.
- the heater 18 is regulated to maintain the sample at substantially the same temperature a ⁇ that of the compounded rubber leaving the ma ⁇ ticator-mixer in the primary proce ⁇ sing of the rubber.
- the duration for which the testing apparatus is operated and measurements are taken, is ⁇ ub ⁇ tantially the same as that for which the compounding process is carried out in the masticator- mixer, and the speed of rotation of the ⁇ haft 6 is chosen to replicate the highest rate of shear to which the rubber is submitted in the process (for example, 100 s' 1 ) .
- Testing of samples of various supplies of raw rubber is carried out to derive for each an appropriate pair of V and E characteristics.
- the different rubbers are proces ⁇ ed to identify which ,i ⁇ the mo ⁇ t ⁇ ati ⁇ factory for the application concerned, and from thi ⁇ the corre ⁇ ponding pair of V and E characteri ⁇ tic ⁇ provides a criterion or standard for acceptance or otherwise of raw rubber for processing.
- a ⁇ ample of each new batch of raw rubber i ⁇ te ⁇ ted and it ⁇ pair of V and E characteristic ⁇ compared with the standard pair. If within certain limits there is a match, then the new batch can be accepted for processing with a greater degree of certainty for the maintenance of con ⁇ i ⁇ tency of resultant product than otherwise would be the case.
- the tolerance limits applicable are cho ⁇ en in dependence upon the degree of consistency required and may be plotted on the characteri ⁇ tic ⁇ a ⁇ by pairs of lines 19 and 20 shown in Figures 4 and 5, to define the range of acceptability.
- V and E characteri ⁇ tic ⁇ are in general applicable a ⁇ appropriate criteria of quality only in regard to the particular manufacturing line and condition ⁇ for which they were derived.
- similar V and E characteristics do indicate rubbers of similar quality or proce ⁇ ability on the ⁇ ame machine ⁇ or machine ⁇ of ⁇ imilar operation (for example ⁇ hear rate) under similar conditions (for example temperature and duration) .
- Raw-rubber supplies can therefore be characterised by their V and E characteri ⁇ tic ⁇ for a particular te ⁇ t, and accepted for manufacture if tho ⁇ e characteri ⁇ tic ⁇ are within the appropriate tolerance ranges of the standard characteri ⁇ tics for that manufacturing proces ⁇ .
- the method of the invention i ⁇ of e ⁇ pecial importance in relation to the te ⁇ ting of raw rubber before proce ⁇ sing ⁇ tarts, it may be applied to the rubber during proce ⁇ sing. It may be applied to the compounded rubber prior to its submission to the next stage of processing, for example, extrusion, calendering or injection-moulding. More especially, the sample may be taken from the output of the mastication-mixing ⁇ tage and in this ca ⁇ e the duration of te ⁇ ting, the ⁇ peed of rotation of the shaft 6, and operation of the heater 18 will be related to the duration, shear condition ⁇ (for example, 1,000 s '1 ) and temperature applicable in the next processing stage.
- shear condition ⁇ for example, 1,000 s '1
- the rubber product of this next ⁇ tage may also be tested in a comparable way in accordance with the conditions applicable to the following stage, so that as processing proceeds, V and E characteristics for each successive stage are plotted and compared with standard V and E characteri ⁇ tic ⁇ of acceptability derived for that re ⁇ pective stage of the proces ⁇ .
- Acce ⁇ s to the space 1 can be gained by lifting the chamber 7, and with it the plate 11, clear of the rotor 4 and stator 5, on rods 21. This enables the ⁇ pace 1 to be cleared after te ⁇ ting, but al ⁇ o enables the ⁇ pace 1 to be loaded directly with a ⁇ trip ⁇ ample of the rubber bent round to fill the ⁇ pace 1, or with an annular ⁇ tamping of the ⁇ ample rubber, if desired.
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE69620769T DE69620769D1 (en) | 1995-09-06 | 1996-09-06 | TESTING RUBBER |
JP9510988A JPH11512185A (en) | 1995-09-06 | 1996-09-06 | Rubber test |
US09/043,018 US6000279A (en) | 1995-09-06 | 1996-09-06 | Rubber testing |
EP96929437A EP0848812B1 (en) | 1995-09-06 | 1996-09-06 | Rubber testing |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GBGB9518176.4A GB9518176D0 (en) | 1995-09-06 | 1995-09-06 | Rubber testing |
GB9518176.4 | 1995-09-06 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1997009602A1 true WO1997009602A1 (en) | 1997-03-13 |
Family
ID=10780276
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/GB1996/002201 WO1997009602A1 (en) | 1995-09-06 | 1996-09-06 | Rubber testing |
Country Status (6)
Country | Link |
---|---|
US (1) | US6000279A (en) |
EP (1) | EP0848812B1 (en) |
JP (1) | JPH11512185A (en) |
DE (1) | DE69620769D1 (en) |
GB (2) | GB9518176D0 (en) |
WO (1) | WO1997009602A1 (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6164818A (en) * | 1999-01-21 | 2000-12-26 | Alpha Technologies | Method and apparatus for measuring viscous heating of viscoelastic materials |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1365677A (en) * | 1971-12-08 | 1974-09-04 | Secretary Trade Ind Brit | Instrument for measuring the characteristics of a sample |
US4275600A (en) * | 1978-05-09 | 1981-06-30 | Avon Rubber Company Limited | Testing rubber |
US4601195A (en) * | 1985-04-11 | 1986-07-22 | Rheometrics, Inc. | Apparatus and method for measuring viscoelastic properties of materials |
US4760734A (en) * | 1986-02-07 | 1988-08-02 | Bryce Maxwell | Apparatus for measuring the rheological properties of materials |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR873976A (en) * | 1940-07-16 | 1942-07-24 | Messerschmitt Boelkow Blohm | Device for indicating that a combustion engine is ready to operate at full load |
NL95389C (en) * | 1954-03-05 | |||
US3479858A (en) * | 1966-03-08 | 1969-11-25 | Japan Synthetic Rubber Co Ltd | Apparatus for measuring viscoelasticity |
US4092849A (en) * | 1977-05-27 | 1978-06-06 | Bryce Maxwell | Method and apparatus for measuring melt elasticity of polymers |
US4352287A (en) * | 1980-06-23 | 1982-10-05 | Dresser Industries, Inc. | Rotational viscometer |
FR2535052A1 (en) * | 1982-10-25 | 1984-04-27 | Agronomique Inst Nat Rech | METHOD AND APPARATUS FOR MEASURING THE RHEOLOGICAL PROPERTIES OF SEMI-SOLID BODIES BY HARMONIC SHEAR IN ROTATION |
GB8319195D0 (en) * | 1983-07-15 | 1983-08-17 | Spri Ltd | Pheometer |
SU1254864A1 (en) * | 1984-01-05 | 1987-03-30 | Институт нефтехимического синтеза им.А.В.Топчиева | Method for studying rheological characteristics of pulverulent and polymeric systems |
DE3490625T1 (en) * | 1984-01-05 | 1985-11-28 | Institut neftechimičeskogo sinteza imeni A.V. Topčieva Akademii Nauk SSSR, Moskau/Moskva | Method for determining rheological parameters of polymeric and disperse systems and device for its implementation |
US5163317A (en) * | 1990-03-26 | 1992-11-17 | Bridgestone Corporation | Apparatus for measuring stress of viscoelastic material |
-
1995
- 1995-09-06 GB GBGB9518176.4A patent/GB9518176D0/en active Pending
-
1996
- 1996-09-06 DE DE69620769T patent/DE69620769D1/en not_active Expired - Lifetime
- 1996-09-06 WO PCT/GB1996/002201 patent/WO1997009602A1/en active IP Right Grant
- 1996-09-06 JP JP9510988A patent/JPH11512185A/en active Pending
- 1996-09-06 EP EP96929437A patent/EP0848812B1/en not_active Expired - Lifetime
- 1996-09-06 GB GB9618654A patent/GB2304907B/en not_active Expired - Fee Related
- 1996-09-06 US US09/043,018 patent/US6000279A/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1365677A (en) * | 1971-12-08 | 1974-09-04 | Secretary Trade Ind Brit | Instrument for measuring the characteristics of a sample |
US4275600A (en) * | 1978-05-09 | 1981-06-30 | Avon Rubber Company Limited | Testing rubber |
US4601195A (en) * | 1985-04-11 | 1986-07-22 | Rheometrics, Inc. | Apparatus and method for measuring viscoelastic properties of materials |
US4760734A (en) * | 1986-02-07 | 1988-08-02 | Bryce Maxwell | Apparatus for measuring the rheological properties of materials |
Also Published As
Publication number | Publication date |
---|---|
GB2304907A (en) | 1997-03-26 |
GB9518176D0 (en) | 1995-11-08 |
EP0848812A1 (en) | 1998-06-24 |
GB2304907B (en) | 1999-05-05 |
EP0848812B1 (en) | 2002-04-17 |
JPH11512185A (en) | 1999-10-19 |
DE69620769D1 (en) | 2002-05-23 |
US6000279A (en) | 1999-12-14 |
GB9618654D0 (en) | 1996-10-16 |
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