The present invention relates to rheological properties of chewing gum and gum base. More specifically, this invention relates to nonlinear rheology of chewing gum and gum base.
An important property of chewing gum and gum base is texture. Tests for measuring texture or correlating to texture may be divided into objective tests that are performed by instruments and sensory tests that are performed by people.
In early stages of the research and development of new chewing gum or gum base formulations, it may be too expensive or not feasible to do sensory testing with human subjects. Especially if the formulation includes new cutting edge ingredients that have not been food approved, there is a need to have an objective test that does not require humans to chew or consume the gum. Also for new ingredients, it may be very expensive to produce product in even small quantities so there is a need to be able to test new chewing gum or gum base formulations with as little material as possible. Also sensory tests can be expensive and may take a long time to set up and perform since it may require getting safety and toxicology studies beforehand as well as costs to run a sensory panel, pay panelists, and get analysis compiled. Therefore there is a need for an objective test that would be cheaper and be faster than performing sensory testing. Another need is to have comprehensive objective tests in the early stages so that subjective opinions are not the only screening methods for potential commercially viable chewing gum. Objective testing may allow for a bigger breadth of samples to be tested in the early stages of product development.
Objective tests for chewing gum and gum base include rheological, optical, chemical, and acoustical testing. Rheological testing of chewing gum including gum base in the linear viscoelastic region is known. A small amplitude oscillatory shear (SAOS) test may be performed to determine linear viscoelastic properties of materials including G′ (elastic or storage modulus), G″ (viscous or loss modulus), and tan delta (tangent of the phase angle—the ratio of viscous modulus to elastic modulus).
One problem with SAOS rheological testing in the linear viscoelastic region is that for materials like chewing gum and gum base that go through nonlinear large, complex, and unsteady deformations during chewing, processing, manufacturing, or even bubble forming, linear rheology does not sufficiently describe the deformations occurring in those situations.
There is a need for nonlinear rheology of chewing gum and gum base to determine commercial viability.
A method of selecting a commercially viable chewing gum including testing a chewing gum using nonlinear rheology, compiling rheological data from the nonlinear rheology, and then comparing the rheological data obtained to rheological data ranges of commercially acceptable chewing gum. The nonlinear rheology can include large amplitude oscillatory shear (LAOS) test, start-up of steady uniaxial extension test, and lubricated or unlubricated uniaxial compression test.
a is a graph illustrating rheological data from an unlubricated uniaxial compression test at constant squeezing velocity and constant temperature.
b is a graph illustrating rheological data from a relaxation test at constant temperature after the unlubricated uniaxial compression test of
Chewing gum provides an excellent everyday example of viscoelastic behavior. It flows when being chewed or pulled slowly between the fingers, internal stresses persist after the deformation has ceased, and recoil occurs when it is suddenly relieved of an externally imposed stress. It also breaks when being blown into bubbles or pulled rapidly. Hence, understanding the rheological properties of chewing gums is important for application and processing purposes. The act of chewing involves nonlinear large, complex, and unsteady deformations from the closing phase, gliding phase, to the opening phase. The closing phase can be correlated to biaxial extension or uniaxial compression. The gliding phase can be correlated to large amplitude oscillatory shear test (LAOS) and the opening phase can be correlated to start up flows in uniaxial extension.
The present invention provides a method of selecting a commercially viable chewing gum using nonlinear rheology. The nonlinear rheology may include large amplitude oscillatory shear (LAOS), start-up of steady uniaxial extension, or relaxation after uniaxial compression (lubricated or unlubricated).
Selecting a commercially viable chewing gum includes testing a chewing gum using nonlinear rheology, compiling the rheological data from the nonlinear rheology, and then comparing the rheological data from the nonlinear rheology to rheological ranges of commercially acceptable chewing gum. Further, selecting a commercially viable chewing gum may include determining whether the rheological data from the nonlinear rheology falls within the rheological data ranges of commercial chewing gum.
Commercially acceptable chewing gum and gum base include chewing gums and gum bases that are already commercially available and have consumer accepted properties like texture and bubble formation. Commercial acceptable also means that the chewing gums and gum bases are manufacturable and processable for retail sale.
Whereas commercially viable may mean that the chewing gum and gum base has potential to be commercially acceptable and are within the realm of possibility that it may one day be commercially acceptable. Additionally, commercially viable may mean that the rheological properties of the chewing gum or gum base may not fall within the range of commercially acceptable products but lies close to the range. Closeness to the commercially acceptable rheological data range may mean that the new data taken be an order of magnitude or two orders of magnitude within the range.
Nonlinear rheology may include any methods or techniques to measure the nonlinear rheological properties of materials that flow.
In the nonlinear rheology described herein, may include controlling stress/force, strain, or strain rate, temperature or a combination of any of these parameters. Controlling these parameters may include keeping one of the parameters constant. For example, the strain may be kept constant during one of the tests described below. Control may also include changing one of the parameters in a step function. For example, the strain rate can be changed from zero to a constant rate or changed from a constant strain rate down to zero (to study the relaxation response of a material). Additionally, control may also include changing one of the parameters in an oscillatory function. In LAOS tests, the strain amplitude or the shear frequency may be varied in an oscillatory function.
Chewing gum samples are prepared for testing according to the method described below.
Sample Preparation for Start-Up of Steady Uniaxial Extension, LAOS, and Uniaxial Compression (Lubricated or Unlubricated) and Relaxation:
Approximately two to eight grams of chewing gum or gum base are chewed for at least 15 to 20 minutes. Alternatively, water soluble components may be extracted by placing a thin strip of chewing gum under running water overnight followed by kneading the gum by hand under running water for an additional two minutes. Yet another method is to knead the gum under running water for at least 20 minutes. Afterwards, samples of chewing gum or gum base are kept constantly in de-ionized water for at least 1 hour and no more than 12 hours to maintain hydration during measurements.
Testing Procedures for Start-Up of Steady Uniaxial Extension:
A ceramic tile is dabbed with tap water from a moist cloth to prevent sticking. The sample is placed on the ceramic tile fixed with a 0.7 mm spacer. Another ceramic tile, dabbed with tap water in the same manner, is placed on top of the cud and gentle pressure is applied until the second tile contacts the spacer. The sample is compressed for 30 to 60 seconds to maintain the thickness of 0.7 mm at room temperature. If necessary to prevent spring-back, the temperature of the tile and cud may be increased slightly by placing them in an oven. Such heating time and temperature should be limited to the minimum necessary to prevent spring-back. After compression, a 21 mm by 5 mm rectangular test specimen is cut from the flattened cud. Any remaining sample on the tile can be retained for further testing by covering the tile and flattened cud with a moist cloth to prevent drying. Samples are re-measured for more precise dimensions before loading onto the EVF fixture for the ARES.
Alternatively, a mold with rectangular holes with a press may be used at room temperature to form samples for start-up of steady uniaxial extension tests while keeping hydration. The pressed gum cud can be greater than or equal to 21 mm and the width and the thickness may vary in the range of 5-10 mm and 0.5-1 mm.
The rectangular sample is then loaded onto the uniaxial extensional viscosity fixture (EVF) on an TA Instruments ARES or ARES-G2 rotational rheometer. The sample is loaded by threading it carefully between the pins of the EVF fixture using wafer tweezers. The pins are then gently pressed into the sample specimen using the wafer tweezers using care not to press so far that the sample fails at the pin instead of in the deformation region (region between the rotating drums) during extension. Any portion of the cud not in the deformation region is lightly pressed onto the base of the drums to increase sample adhesion and thus prevent slipping during extension. After loading, the sample is equilibrated to 37° C. (mouth temperature) for 5 minutes before beginning the test (or other temperatures). Uniaxial extension measurements will be carried out up to sample failure (which typically occurs at Hencky strain ranging from 3 to 10).
Uniaxial extensional strain hardening parameter is measured by plotting uniaxial extensional viscosity on a log plot versus a log plot of time. A representative log plot of uniaxial extensional viscosity (Pa*s) versus log plot of time at 37° C. is shown in
A sample of a commercial chewing gum, US Trident White® Chewing Gum manufactured by Cadbury, was purchased from a retail market.
A sample of a commercial chewing gum, US Trident Soft Chewing Gum manufactured by Cadbury, was purchased from a retail market.
A sample of a commercial chewing gum, US Trident® Bubble Gum manufactured by Cadbury, was purchased from a retail market.
A sample of a commercial chewing gum, US Hubba Bubba® Outrageous Original manufactured by Wm. Wrigley Jr. Company, Chicago, Ill. USA was purchased from a retail market.
A sample of a commercial chewing gum, US Hubba Bubba® Tape Outrageous Original manufactured by Wm. Wrigley Jr. Company, Chicago, Ill. USA was purchased from a retail market.
As can be seen in
Testing Procedures for LAOS:
TA Instruments ARES-G2 Rheometer may be used with a cone and plate configuration, specifically, an 8 mm cone with a recirculating fluid bath. The sample that has been hydrated in de-ionized water is then stamped out of the bulk chewed gum with a metal stamper. Then the outside of the sample is dried with a paper towel. The sample is then loaded onto the lower rheometer plate and compressed to a trim gap and trimmed with a scapel. For chewing gum, the trim gap is 0.07 mm. For bubble gum, the trim gap is 0.075 mm. The sample is then compressed to the cone geometry gap and then allowed to equilibrate for 5 minutes and heated by the recirculating fluid bath to 37° C. (mouth temperature) or other temperatures. The transient LAOS test includes 5 delay cycles and 5 sampling cycles with strain sweep from 0.01-1000% at 3 points per decade and 256 data points collected per cycle using frequencies 0.1, 1 and 10 rad/s.
An example of data output from LAOS testing at 37° C. is shown in
Testing Procedures for Uniaxial Compression (Lubricated or Unlubricated):
TA Instruments ARES-G2 Rheometer may be used with parallel plates with a convection oven or parallel plates with the bottom plate being heated. Bulk chewed gum is pressed through a Teflon mold with 8 mm diameter and 6 mm height. Excess gum is trimmed from the mold and the sample is pressed out of mold and remolded to a cylinder shape. The sample is then loaded between lubricated parallel plates (with silicon oil) or unlubricated and compressed to initial test gap L0=6 mm. The sample is allowed to equilibrate for 5 min at 37° C. in the convection oven or other temperatures. The sample is then compressed at a constant Hencky strain rate.
Testing Procedure for Uniaxial Compression and Relaxation:
TA Instruments ARES-G2 Rheometer may be used with parallel plates. Both plates may be made of steel or a plate that is made of cement and another made of steel. Bulk chewed gum is prepared and loaded between the parallel plates. The plates may be lubricated or unlubricated. The sample is then allowed to equilibrate for 5 min at 37° C. or other temperatures via a convention over or other heating means. The sample is then compressed to a final gap value at a constant speed. Next, the sample is then held at the final gap value and relaxed for a period of time.
a is an example of data output for an unlubricated uniaxial compression test conducted at 37° C. at a constant uniaxial compression speed of 0.1 mm/s to a final gap of 4 mm for US Eclipse® Peppermint Chewing Gum, US Extra® Peppermint Chewing Gum, and US Freedent® all manufactured by Wm. Wrigley Jr. Company, Ill. USA, which was purchased from a retail market. The top parallel plate is made of cement and the lower plate is made of steel. The samples have a diameter of 10 mm.
b is an example of data output for a relaxation test following the unlubricated uniaxial compression test conducted from
Rheological data ranges of commercially acceptable chewing gums may be different depending on the nonlinear rheology used. For start-up of steady uniaxial extension tests, the stress plateau value at Hencky strain less than 1, the Hencky strain at the break of a sample, and the maximum stress/plateau stress are important parameters. Commercially acceptable chewing gums may typically have a stress plateau value (at strain less than 1) between 3,000 to 300,000 Pa, and preferably from 6,000 to 30,000 Pa. Another rheological parameter for commercially acceptable chewing gums is the Hencky strain at the break point. The Hencky strain at break for commercially acceptable chewing gums is from 1 to 12 and preferably from 3.5 to 9.6. The value of the maximum stress divided by the plateau stress is another important parameter. Commercially acceptable chewing gums have a maximum stress/plateau stress between 1 to 100, and preferably between 30 to 100. In
For uniaxial compression tests followed by a relaxation test, the maximum uniaxial compression force at a final gap value and the normal force after 20 second of relaxation are important rheological parameters. First, the maximum uniaxial compression force at a constant speed of 0.1 mm/s to a final gap of 0.4 mm, and plate diameter of 10 mm, is between 5 to 20 N for commercially acceptable chewing gums. The normal force after 20 seconds of relaxation for commercially acceptable chewing gums is between 0 to 2 N, and preferably between 0.1 to 1.5 N.
Reformulation or optimization may include changing a gum base in the chewing gum. Changing a gum base may include changing the physical structure of a polymer in the gum base by crosslinking the polymer, increasing or decreasing the molecular weight of the polymer, branching the polymer, making the polymer more linear, or by changing the chemical structure of the polymer by changing the constituent monomers. Additionally, reformulating or optimizing the chewing gum may include adding a different gum base, increasing or decreasing by weight of a softener, filler, emulsifier, and/or a plasticizer in the chewing gum or even changing those ingredients to another softener, filler, emulsifier, or plasticizer.
The fundamental components or ingredients of a chewing gum typically are a water-insoluble gum base portion and a generally water-soluble bulk portion. The primary component of the gum base is an elastomeric polymer which provides the characteristic chewy texture of the product. The gum base will typically include other ingredients which modify the chewing properties or aid in processing the product. These include plasticizers, softeners, fillers, emulsifiers, plastic resins, as well as colorants and antioxidants. The generally water soluble portion of the chewing gum typically includes a bulking agent together with minor amounts of secondary components such as flavors, high-intensity sweeteners, colorants, water-soluble softeners, gum emulsifiers, acidulants and sensates. Typically, the water-soluble bulk portion, sensates, and flavors dissipate during chewing and the gum base is retained in the mouth throughout the chew. Even though they are often water insoluble, flavors and sensates are at least partially released with the water soluble bulking agent during chewing and are considered part of the water soluble portion.
A water-insoluble gum base typically constitutes approximately 5 to about 95 percent, by weight, of a chewing gum of this invention; more commonly, the gum base comprises 10 to about 50 percent of a chewing gum of this invention; and in some preferred embodiments, 20 to about 35 percent, by weight, of such a chewing gum.
In addition to the water-insoluble gum base portion, a typical chewing gum composition includes a water-soluble bulk portion (or bulking agent) and one or more flavoring agents. The water-soluble portion can include high intensity sweeteners, binders, flavoring agents (which may be water insoluble), water-soluble softeners, gum emulsifiers, colorants, acidulants, fillers, antioxidants, and other components that provide desired attributes.
The present invention may be used with a variety of processes for manufacturing chewing gum including batch mixing, continuous mixing, sheeting, extrusion, coating, and tableted gum processes.
Chewing gum is generally manufactured by sequentially adding the various chewing gum ingredients to commercially available mixers known in the art. After the ingredients have been thoroughly mixed, the chewing gum mass is discharged from the mixer and shaped into the desired form, such as by rolling into sheets and cutting into sticks, tabs or pellets or by extruding and cutting into chunks. The product may also be filled (for example with a liquid syrup or a powder) and/or coated for example with a hard sugar or polyol coating using known methods.
After forming, and optionally filling and/or coating, the product will typically be packaged in appropriate packaging materials. The purpose of the packaging is to keep the product clean, protect it from environmental elements such as oxygen, moisture and light and to facilitate branding and retail marketing of the product.
The present patent application is a 371 of international application Ser. No. PCT/US11/46819 filed Aug. 5, 2011, which claims benefit from Ser. Nos. 61/371,073 filed Aug. 5, 2010; 61/373,431 filed Aug. 13, 2010; 61/373,454 filed Aug. 13, 2010; and 61/407,220 filed Oct. 27, 2010. All of the applications listed above are incorporated by reference as if entirely restated herein.
Filing Document | Filing Date | Country | Kind | 371c Date |
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PCT/US2011/046819 | 8/5/2011 | WO | 00 | 9/20/2013 |
Number | Date | Country | |
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61371073 | Aug 2010 | US | |
61373454 | Aug 2010 | US | |
61373431 | Aug 2010 | US | |
61407220 | Oct 2010 | US |