Patent ID: 12216038

Similar reference characters denote corresponding features consistently throughout the attached drawings.

DETAILED DESCRIPTION

InFIGS.1A and1B, a first embodiment of the physical stability analysis container1is shown, including a flexible sheet2which may be made of an elastic, transparent material. In particular non-limiting examples, flexible sheet2may be formed of borosilicate glass, plastic (polymers), or perfluoroalkoxy (PFA). Container1further includes a sample enclosure3having an upper rim3aand lower rim3b. In the non-limiting embodiment shown, sample enclosure3is formed by a single cylindrical sidewall made up of flexible sheet2which is fed from a source roll4. Source roll4includes an upper rim4aand a lower rim4b. Both sample enclosure3and source roll4extend vertically from a base5and are in contact with base5along their respective lower rims3b,4b.

Sample enclosure3is sealed by a square shaped gasket that is adjusted to a C-shaped stainless-steel plate6that is fixed vertically on the outside of the vial cavity to form a guide slot6afor the flexible sheet2to pass through. The end of flexible sheet2will be fixed on one of the inner surfaces6bof the gasket after passing through the slot6a.

As shown inFIG.1B, the sample enclosure3is uniform in cross section with respect to an axis A extending perpendicular from base5. Although the sample enclosure is shown in the shape of a cylinder having a circular cross section, other shapes are conceivable for the cross section of sample enclosure3including elliptical, curvilinear, or a combination of curvilinear (i.e. curved lines) and polygonal (i.e. straight lines).

As shown inFIG.1AandFIG.1B, sample enclosure3is configured to be adjustable in diameter and cross-sectional area. Numerical markings7aand lines7bindicate adjustments in diameter which may be made to sample enclosure3. The cross-sectional area of the sample enclosure3is configured to be increased by rotating the source roll4in a first direction, such as counter-clockwise, to feed more of the flexible sheet material into the sample enclosure. The cross-sectional area is decreased by rotating the source roll4in a second direction opposite to the first direction, such as clockwise, to retract the flexible sheet2from the sample enclosure3. Rotation of the source roll4can be accomplished by any suitable means such as a shaft and gear arrangement (not shown), or by manually gripping and rotating the source roll4.

To prevent leakage from the sample enclosure3, a sealing material such as clay may be used at the bottom of the outer surface3b. Alternatively, a gasket material can be added to the bottom of the flexible sheet2. Also, the bottom surface of flexible sheet2can be coated with metallic nanoparticles, after which a magnet can be placed below base5to secure its required final form. In any case, a user will have the capability to modify the cross-sectional area of the sample enclosure3, based on their requirements and targeted sample suspension by adding or retracting the flexible sheet2.

In a second embodiment, shown inFIGS.2A-Da physical stability analysis container100includes three nested cylindrical sidewalls101a,101b,101cextending from a base103of the outermost sidewall101a. Outermost sidewall101ais fixedly attached to a base103while the nested inner sidewalls101b,101care open ended and removable. The innermost sidewall101cdefines a sample enclosure into which is placed a particle suspension or other sample to be tested. As shown inFIG.2C, sidewalls101a-care of uniform cross section with respect to an axis A extending perpendicularly from base103. Although the sidewalls101a-care shown as nested cylinders of circular cross section, other shapes are conceivable for the cross section of the sidewalls including elliptical, curvilinear, or a combination of curvilinear (i.e. curved lines) and polygonal (i.e. straight lines).

To adjust the cross-sectional area of the sample enclosure, innermost sidewall101cis configured to be removed thereby causing the particle suspension or sample to settle within the next available sidewall101bwhich then defines the new sample enclosure of adjusted cross-sectional area. The procedure may be repeated by removing sidewall101bto allow the particle suspension or sample to settle within sidewall101a.

It should be noted thatFIG.2AandFIG.2Bdepict container100in an expanded state for illustration purposes and that during normal usage the sidewalls101a-care in a compact nested state as shown inFIG.2D. As seen inFIG.2D, sidewalls101a-ccontain different respective diameters D1, D2, D3but are of uniform height H1.

Similarly to the previous embodiment, container100may be sealed by a material such as clay on the bottom surfaces of sidewalls101a-c. Alternatively, the bottom of sidewalls101a-cmay have a ring shaped gasket material placed thereon or be coated with metallic nanoparticles, after which a magnet can be placed below base103to secure sidewalls101a-c. Furthermore, the bottom rims of cylindrical sidewalls101a-cmay be partially or fully covered by magnets102a-c. Magnets102a-cmay serve to secure sidewalls101a-cin place.

FIGS.3A-Dshow a third embodiment of a container200used for physical stability testing. Similarly to the previous embodiment, container200contains nested cylindrical sidewalls201a-cof substantially uniform cross-section with respect to an axis extending from base203. Container200has only a minor variation in cross-section resulting from the shown mating arrangement of pins203and cavities202. However, it should be understood, that by the term ‘substantially uniform’ as used in the present disclosure with regards to cross-sectional shape and size, this term is defined herein as a singular cross sectional shape and size existing along the length of the sidewalls, without tapering or conical variations in cross section but only minor variations due to any mating arrangements between the sidewalls such as protruding pegs, threads, magnets, or other mating arrangements used on the base, sides, or upper rims of the nested sidewalls. An example of shapes that would not be ‘substantially uniform’ in cross section as defined herein would include cones, pyramids, or other tapered shapes. Examples of shapes that are ‘substantially uniform’ in cross section would include cylinders, semi-cylinders, cubes, or other shapes having uniform cross sectional dimensions along their length with only minor variations permitted due to any mating arrangements or small protrusions, grooves, etc. such as those already described.

As a non-limiting example of a minor variation in cross section, while still conforming to the definition of ‘substantially uniform’ in cross-section as defined herein, reference is made to pins203and cavities202used for joining sidewalls201a-cof container200. Pins203are shown on the outer surface of sidewalls201a-cand fit within corresponding cavities202of a mating sidewall. Cavities202may be in any suitable shape, but in particular may be L-shaped as shown inFIG.3B, with a vertical portion202aand horizontal portion202b.

Similar sealing solutions may be provided on bottom surfaces of sidewalls201a-cas previously described, including clay material, ring-shaped gaskets corresponding to the sidewall cross section, or a magnetic nanoparticle coating. Furthermore, as in previous embodiments, other shapes may be used rather than cylindrical sidewalls such as curvilinear shapes, polygonal shapes, or shapes using a combination of straight and curved surfaces or lines, provided that the enclosed sidewalls defined by the shape are of uniform or substantially uniform cross section along the length of the sidewall, with the only minor variations in cross section due to, for example. mating interfaces between the sidewalls.

FIGS.4A-Cshow a fourth embodiment of a physical stability analysis container300including cylindrical sidewalls301a-cextending from a base303which is fixedly attached to outermost sidewall301a. As in the previous two embodiments, only the outermost cylindrical sidewall is fixedly attached to the base303, while the nested inner sidewalls are unattached and removable. The sidewalls are substantially uniform in cross section wile containing a threaded mating arrangement shown by threads302.

Turning toFIG.5A, physical stability analysis container1is shown in a particle dispersion stability test, namely a light transmission and absorption test. Testing the amount of light transmitted and absorbed by a sample is a useful indicator with regards to the stability and dispersion of particles within the sample, as well as the composition of particles within a sample.

The elements of the light transmission and absorption test include a laser source8, filter9, lens10, and charge coupled device (CCD)13. Laser source8provides a focused beam of light11, shown as a first section11abetween laser source8and container1, and a second section11bthat has passed through container1and enters CCD13. CCD13may be any suitable image sensor used to analyze characteristics such as particle size, distribution and concentration. In particular CCD13may be a CCD camera or a UV spectrophotometer. Lens10serves to focus light11onto the sample within container1as well as towards CCD13, which captures and measures the intensity of the transmitted or absorbed light, which can be analyzed to infer particle size, concentration, and the degree of stability or aggregation in a sample.

FIG.5Bshows an embodiment of container100used in a light transmission and absorbance test. In order to use container100for a light transmission and absorbance test, it would be necessary to conduct a reference measurement using the base fluid absent of suspended particles in the same configuration to be used when container100contains a particle suspension sample. Taking such a reference measurement accounts for changes in refractive index of the multiple sidewalls used in container100.

FIG.6Ashows an embodiment of container1used in a dynamic light scattering test. The components of the dynamic light scattering test include laser light source8a, focusing lenses10a,10b, photon detector14and digital signal processor (DSP)16. Photon detector14serves to detect scattered light11passing through lenses10a,10band container1that result from the Brownian motion of particles in a sample. Brownian motion refers to the random and continuous movement of particles suspended in a fluid as a result of their collisions with surrounding molecules. As particles undergo Brownian motion in a solution, they create fluctuations in the scattered light. DSP16serves to process electrical signals passed along wiring15by photon detector14. DSP16analyzes the intensity fluctuations in the scattered light over time and performs calculations to extract information about the size distribution and dynamics of the particles in the suspension sample.

FIG.6Bshows an embodiment of container100used in a dynamic light scattering test. Similarly to the light transmission and absorbance test conducted with container100, it would be necessary for the dynamic light scattering test ofFIG.6Bto conduct a reference measurement using the base fluid absent of suspended particles. By conducting a reference measurement, changes in refractive index of the multiple sidewalls used in container100may be accounted for in the dynamic light scattering test.

FIGS.7A and7Bshow examples of a sedimentation photographical capturing test using containers1and100, respectively. The sedimentation photographic capturing test involves visually capturing images or photographs of particles settling or sedimenting in a liquid. Photographs or images of the sedimentation process are captured at regular intervals using a camera17or other imaging equipment. The frequency of image capture depends on the expected settling rate of the particles and the duration of the test. The captured images are then analyzed to observe and measure the settling behavior of the particles. Key parameters that may be assessed include the settling rate, the formation of sediment layers, the extent of aggregation or flocculation, and the overall stability of the system.

Although specific reference has been made to sedimentation photographical capturing, light transmittance and absorbance testing as well as dynamic light scattering, the containers described herein may be used in any test where changes in size of the container may influence the outcome of the test. Examples of other tests may include zeta potential analysis, 3-ω approach, scanning electron microscopy analysis, transmitted electron microscopy characterization, spectral analysis, centrifugation, and particle size analysis.

By using the containers of adjustable size as set forth and described herein, physical stability analysis testing may be performed on a prepared particle suspension sample without the need for replacing the container with a new container of different size, but rather by simply making a physical adjustment of the container to thereby increase or decrease the size of the sample enclosure. In doing so, test procedures may be repeatedly performed using the same container at multiple sizes to observe the role of container size on the outcome of the test.

It is to be understood that the containers for physical stability analysis and methods of use thereof are not limited to the specific embodiments described above, but encompass any and all embodiments within the scope of the generic language of the following claims enabled by the embodiments described herein, or otherwise shown in the drawings or described above in terms sufficient to enable one of ordinary skill in the art to make and use the claimed subject matter.