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Title:
CANNABIS REFINER
Document Type and Number:
WIPO Patent Application WO/2021/162710
Kind Code:
A1
Abstract:
A method and device for refining cannabis are provided. The device includes a container and a heater operative to heat the contents of the chamber. The device further comprises a surface having a temperature lower than the container temperature. The method includes loading cannabis in a container and applying an elevated temperature to the container while providing a surface having a temperature lower than the container temperature.

Inventors:
LEMKIN MARK (US)
Application Number:
PCT/US2020/018469
Publication Date:
August 19, 2021
Filing Date:
February 16, 2020
Export Citation:
Click for automatic bibliography generation   Help
Assignee:
LEMKIN MARK ALAN (US)
International Classes:
B01L7/00; A61K31/00; G01N1/44; G01N33/15; H05B1/00
Foreign References:
US20180243710A12018-08-30
US20150223515A12015-08-13
US20140054307A12014-02-27
US20190204283A12019-07-04
US4279824A1981-07-21
US4913865A1990-04-03
Download PDF:
Claims:
CLAIMS im:

1. A device for refining cannabis comprising: a container comprising a first surface; a heater coupled to the container; a second surface; and, a path for air, water, or carbon dioxide to leave and enter the container; wherein the heater causes the container to rise to a first temperature; and, wherein the second surface is maintained at a second temperature lower than the first temperature.

2. The device of claim 1 wherein the second surface comprises a lid.

3. The device of claim 1 wherein the path to leave or enter the container comprises one selected from the following list: a groove; a hole; a surface finish; or, a manufacturing imperfection.

4. The device of claim 2 wherein the maintaining of the second surface temperature comprises one selected from the following list: passive thermal dissipation to the ambient; or, forced convection by a fan.

5. The device of claim 2 wherein the lid temperature is regulated towards a constant temperature.

6. The device of claim 2 further including a material having a thermal conductivity lower than the container coupled to at least one selected from the list of: the container; or, the lid.

7. The device of claim 1 further including a casing; wherein the casing surrounds at least a portion of the container.

8. The device of claim 6 wherein the material having a thermal conductivity lower than the container comprises at least one material selected from the following list: a plastic, cork, wood, silicone, fiber.

9. The device of claim 2 wherein the lid further comprises a non-stick coating.

10. The device of claim 1 further including a timer coupled to the heater.

11. The device of claim 1 further including a detector responsive to at least one of the following: deposited material; or, a rate of deposition of material.

12. The device of claim 1 wherein a refinable material selected from the following list is deposited on the second surface: cannabidiolic Acid; cannabigerolic acid; cannabichromenic acid; tetrahydrocannabinolic acid; cannabidiol; cannabigerol; cannabichromene; tetrahydrocannabinol; myrcene; limonene; linalool; caryophyllene; pinene; alpha-bisabolol; eucalyptol; trans-nerolidol; humulene; delta 3 carene; camphene; borneol; terpineol; valencene; or, geraniol.

13. The device of claim 2 wherein a cannabinoid, a cannabinoid acid, or a terpene is volatilized within the container and deposited on the lid.

14. A device for refining cannabis comprising: a container; a heater coupled to the container; a lid; and, a region of lowered thermal conductivity coupled between the lid and container; wherein the heater causes the container to rise to a first temperature; and, wherein the lid is maintained at a second temperature lower than the first temperature.

15. The device of claim 14 wherein the region of lowered thermal conductivity comprises a material coupled between the lid and the container selected from the following list: a plastic; a silicone; fiber; cork; wood; a material having a thermal conductivity lower than the thermal conductivity of the container; or, a material having a thermal conductivity lower than the thermal conductivity of the lid.

16. The device of claim 14 further including a cannabinoid, a cannabinoid acid, or a terpene volatilized within the container and deposited on the lid.

17. A method for refining cannabis comprising: loading a quantity of cannabis into a container; applying an elevated temperature to the container; providing a surface having a lower temperature than the container; and, providing a path for air, water, or carbon dioxide to leave and enter the container; wherein the surface having a lower temperature than the container is exposed to gasses or vapors released by the cannabis.

18. The method of claim 17 wherein the step of providing a surface having a lower temperature than the container comprises at least one selected from the following list: passively dissipating heat to the ambient environment; or, actively dissipating heat to the ambient environment using forced convection.

19. The method of claim 17 further including a step of detecting at least one of the following: deposited material; or, a rate of deposition of material.

20. The method of claim 17 wherein a cannabinoid, a cannabinoid acid, or a terpene is volatilized within the container and deposited on the surface having a lower temperature than the container.

Description:
CANNABIS REFINER

TECHNICAL FIELD

[0001] This disclosure generally relates to refining of plant materials, and more particularly to the refinement of plant materials containing a cannabinoid or terpene.

DESCRIPTION OF RELATED ART

[0002] Cannabis and hemp flowers (e.g. Cannabis sativa, Cannabis sativa forma indica), as well as other plant parts, collectively hereby termed cannabis, contain various chemical components having medicinal, recreational, or otherwise desirable properties. These chemical components are often preferred in their isolated form, free from the other portions of the plant material. Various methods are presently available to purify the desired materials from plant material including solvent extraction with a solvent such as ethanol, iso-propanol, or liquified butane; carbon dioxide extraction techniques including liquid- or supercritical- carbon dioxide extraction; and, vacuum distillation.

SUMMARY

[0001] Refinement of cannabis using two surfaces having different temperatures placed in proximity to each other provides for the refinement of cannabis without costly vacuum or high-pressure systems and without needing solvents.

In accordance with an embodiment described herein, a device for refining cannabis includes a container comprising a first surface and a heater coupled to the container. The heater causes the container to rise to a first temperature. A second surface is maintained at a temperature lower than the temperature of the first surface.

In some embodiments the second surface comprises a lid.

In some embodiments, a path is included for air, water, or carbon dioxide to leave or enter the container.

The lid temperature may be maintained through passive thermal dissipation to the ambient; or, via forced convection through use of a fan. Furthermore, the lid temperature may be regulated towards a constant temperature or the lid temperature may be unregulated.

In some embodiments a material having a thermal conductivity lower than the container is coupled to the container or the lid. In some embodiments the material includes one or more of a plastic, cork, wood, silicone, or fiber.

In some embodiments a casing surrounding a portion of the container is included.

In some embodiments a covering is included over the lid.

To prevent sticking of refined materials to the lid, in some embodiments the lid includes a non-stick coating.

In some embodiments a timer is coupled to the heater to control the duration of heating by de-energizing the heater after a period of time has elapsed.

In some embodiments a detector is included, the detector being responsive to at least one of the following: deposited material; or, a rate of deposition of material. The detector output is processed to provide an indication of amount of refined material, or whether refinement is completed to beyond a threshold of completion. The detector output may be further coupled to the heater to de-energize the heater after refinement has completed to beyond a threshold.

Refinable materials include cannabidiolic acid; cannabigerolic acid; cannabichromenic acid; tetrahydrocannabinolic acid; cannabidiol; cannabigerol; cannabichromene; tetrahydrocannabinol; myrcene; limonene; linalool; caryophyllene; pinene; alpha-bisabolol; eucalyptol; trans-nerolidol; humulene; delta 3 carene; camphene; borneol; terpineol; valencene; geraniol; a cannabinoid; a cannabinoid acid; or, a terpene.

In accordance with an embodiment described herein, a method for refining cannabis includes loading a quantity of cannabis into a container; applying an elevated temperature to the container; and, providing a surface having a lower temperature than the container, wherein the surface having a lower temperature than the container is exposed to gasses or vapors released by the cannabis.

In some embodiments the step of providing a surface having a lower temperature than the container includes passively dissipating heat to the ambient environment; or, actively dissipating heat to the ambient environment using forced convection. An additional step of detecting deposited material or, a rate of deposition of material on a lid may be included.

In some embodiments the step of exposing the lower-temperature surface to gasses or vapors released by the cannabis includes gasses or vapors comprising a cannabinoid, a cannabinoid acid, or a terpene.

BRIEF DESCRIPTION OF DRAWINGS

[0003] The figures listed below illustrate exemplary embodiments, and are not intended to coverall possible embodiments, including embodiments with additional or fewer components, steps, or connections. The embodiments, techniques, components, connections, and other teachings described in the figures are exemplary and were chosen to provide a clear explanation without unnecessary obfuscation.

[0004] FIG. 1 illustrates a schematic diagram of a first embodiment of a refiner.

[0005] FIG. 2 illustrates a schematic diagram of a second embodiment of a refiner with a casing.

[0006] FIG. 3 illustrates a schematic diagram of a third embodiment of a refiner with a protective covering.

[0007] FIG. 4 illustrates a schematic diagram of a fourth embodiment of a refiner comprising forced convection.

[0008] FIG. 5 illustrates a schematic diagram of a fifth embodiment of a refiner comprising passive heat removal.

[0009] FIG. 6 illustrates a schematic diagram of a sixth embodiment of a refiner comprising an alternate mechanical connection.

[0010] FIG. 7 illustrates a schematic diagram of a seventh embodiment of a refiner comprising an area of increased thermal resistance.

[0011] FIG. 8a illustrates a schematic diagram of a circuit suitable for capacitor detection. [0012] FIG. 8b illustrates a schematic diagram of a sensing capacitor.

DETAILED DESCRIPTION

[0013] A refinable material is hereby defined as any cannabinoid, cannabinoid acid, terpene or other compound that may be volatilized (i.e. made into a vapor or gas) by applying heat to attain a temperature in a range between 80C and 300C. In some embodiments, volatilization comprises reaching a partial pressure of greater than 1 Pa. In some embodiments, volatilization comprises reaching a partial pressure of greater than 1 kPa. Illustrative examples of refinable materials include: CBDA (Cannabidiolic Acid), CBGA (Cannabigerolic Acid), CBCA (cannabichromenic acid), THCA (Tetrahydrocannabinolic acid), CBD (Cannabidiol), CBG (Cannabigerol), CBC (cannabichromene), THC (Tetrahydrocannabinol), Myrcene, Limonene, Linalool, Caryophyllene, Pinene, Alpha- bisabolol, Eucalyptol, Trans-nerolidol, Humulene, Delta 3 Carene, Camphene, Borneol, Terpineol, Valencene, and Geraniol.

[0014] Figure 1 shows a cross-sectional schematic view of a generally-cylindrical container 100 coupled to a heater 102. Container 100 is made of a metal, such as aluminum, copper, or steel. In various embodiments container 100 is shaped in a rectangular, cuboid, hexagonal or any other appropriate shape or geometry. In some embodiments a thermal sensor (e.g. a thermocouple or a thermistor) coupled to the container is used in conjunction with a controller (e.g. a microcontroller or a circuit) to maintain the temperature of the container at a desired temperature by adjusting the power supplied to heater 102 in response to information from the thermal sensor. In some embodiments a positive-temperature-coefficient (PTC) heater is used, thereby providing automatic regulation of the temperature without a separate thermal sensor. Plant material comprising refinable material is placed into container 100, and in contact with the interior surface of container 100. Removable lid 106, which also comprises metal, is then placed over the chamber opening thereby forming a closed space 104, or chamber. Region 108, on which removable lid 106 rests is made of a material having a lower thermal-conductivity than container 100, such as plastic (e.g. PEEK, PPS, PPSU, etc.). High performance plastics such as PEEK, PPS, or PPSU have a high service temperature allowing container 100 to be operated at a higher temperature than were a low service-temperature plastic (e.g. PET, PLA) to be used. In some embodiments, material other than a plastic is used to form region 108; for example, compressed fiber material of a type similar to that used for gaskets, cork, wood, or silicone.

[0015] To start the refining process, heater 102 is energized causing the temperature of container 100 to increase. As the temperature increases air in chamber 104 starts to expand and escape through a path to ambient between the removable lid 106 and region 108, and / or between container 100 region 108. The temperature of lid 106 also starts to rise due to thermal conduction through region 108 as well as contact with the chamber gasses. In some embodiments a small groove is cut in the lid, chamber, or region 108, the groove extending between the chamber volume 104 and the exterior facing portion of the lid or region 108; the groove provides a path for gas to leave or enter the chamber. In some embodiments surface roughness, surface texture, or other manufacturing imperfections (e.g. imperfections of the type specified by Ra) in the lid, container, or region 108 provide a sufficient path for gas or vapor to leave the chamber (e.g. when the container is being heated or remains at temperature) or enter the chamber (e.g. when the container is cooled after refinement completes). Providing a path to ambient allows chamber oxygen to be purged as the chamber is heated, as well as maintains a low pressure differential as the container is cooled; were the ambient gasses unable to enter the chamber during cooling the chamber pressure would drop as it was cooled and make it difficult if not impossible to manually remove the lid. Extremely flat surfaces can impede gas or vapor transport between the chamber and ambient. In some embodiments a path to ambient provides sufficient flow to prevent more than 10kPa pressure differential to exist between the chamber and ambient for a period of longer than 1 minute. In some embodiments a hole is formed in either the lid or the chamber to provide a path to ambient.

[0016] As the temperature of the plant material rises to 100C the water in the plant material completely vaporizes. If the surface temperature of inner-surface region 110 of removable lid 106, facing into the chamber, is less than 100C then water may condense on this inner- surface of the lid. If the temperature of removable lid 106 facing into the chamber is greater than 100C then this water vapor will escape the chamber through either the interface between lid 106 and region 108, container 100 and region 108, or via a groove which may be cut into either or all of container 100, lid 106, or region 108. Starting at a temperature near 100C, cannabinoid-acids such as CBDA or THCA start to appreciably decarboxylate into their neutral form (e.g. CBD or THC) releasing carbon dioxide in the process; the carbon dioxide also mixes with the gasses in the chamber and escapes. Water vapor and carbon dioxide from decarboxylation of cannabinoid acids help purge the chamber of oxygen. In some embodiments additional water, beyond what naturally is present in the plant material, is added before heat is applied to provide additional purging of oxygen. Purging of oxygen minimizes oxidation of desired refinable material at higher temperatures.

[0017] As the temperature within the chamber rises the vapor pressure of refinable materials become appreciable (e.g. greater than 1 Pa, or in some embodiments greater than 1kPa), from refinable material leaving the plant matter and turning into a vapor or gas. However, if the lid remains at a sufficiently low temperature, which is dependent upon at least the particular terpene, cannabinoid, or compound of interest, vaporized or gaseous molecules will impinge upon and stick to inner-surface 110 due to the lower temperature; this is as opposed to the carbon dioxide or heated air which are released to the atmosphere since the lid is far above the temperature at which air or carbon dioxide liquify. Keeping the lid at a sufficiently low temperature causes the vapor pressure of the terpenes or cannabinoids immediately at the inner lid surface 110 to become lower than the vapor pressure in the chamber at large thereby causing deposition of the terpene or cannabinoid on the inner surface 110, and inducing a diffusion process from portions of the chamber with a higher vapor pressure to this region of lowered vapor pressure. In some embodiments the lid remains at a temperature between 80C to 150C. The vapor pressure of the refinable material within the chamber will increase as the plant material and chamber temperature increase thereby increasing the rate of deposition on the interior portion of the lid were the lid held at constant temperature.

[0018] Because different refinable materials have different vapor pressure versus temperature curves, preferential deposition of one or more terpenes or cannabinoids may be attained by selecting a chamber temperature and duration. For example, suppose that at a particular temperature THC were to have a vapor pressure of p1 and CBD were to have a vapor pressure of p2 where p2 < p1 ; then, the THC would more rapidly move from the plant material to the lid since the chamber vapor pressure is higher. However, eventually the CBD would also transfer from the plant material to the lid. By removing the heat before the CBD has had a chance to more fully transfer to the lid the refined material will have a higher THC concentration than the starting material. If desired, the refined material which is richer in THC may be removed from the lid by, e.g. scraping with a straight-edge, and the plant material re-processed at a higher temperature or for a longer time; this material is now richer in CBD in comparison to THC than the original starting material because the THC was preferentially removed before the CBD was more fully refined.

[0019] The rate at which refinement occurs will depend on the temperature of the lid, the temperature of the chamber and plant material, the particular terpene or cannabinoid vapor pressure versus temperature curve(s), and the distance from the lid to the plant material. Optimal values of various design parameters may be determined through a design of experiments (e.g. running experiments at different temperatures and measuring the deposition rate of refinable material on the lid); or calculations based upon chemistry and thermodynamics, which are well known to those skilled in the art, in conjunction with vapor pressure versus temperature data of one or more refinable materials.

[0020] In some embodiments the lid is maintained at a higher temperature to preferentially select a cannabinoid or terpene with a lower vapor pressure at temperature. In this embodiment the undesired vaporized cannabinoid or terpene does not condense on the lid, held at a higher temperature, but is expelled through the path to ambient. [0021] Figure 2 shows an embodiment having a container 200 coupled to casing 212. Casing 212 prevents personal injury caused by contact with the container when at an elevated temperature as well as reduces heat transfer from the container to ambient. Container 200 is screwed to region of lower thermal-conductivity 208 with metal screws 214 countersunk below the surface of region 208 to prevent physical contact of the screws to the lid. Region 208 in this embodiment is part of casing 212 and is fabricated as a single piece of plastic through a process such as injection molding or 3D-printing. Casing 212 is made from a plastic having a high service temperature such as PPS, PEEK, PPSU, Nylon or other suitable plastic. In some embodiments casing 212 is made from wood. The region 220 between casing 212 and container 200 is filled with an insulating material such as fiberglass or vermiculite. In various embodiments the region between the container and the casing is left unfilled; or, comprises a vacuum. Casing bottom 224 is screwed to casing 212 via screws 226.

[0022] In some embodiments screws 214 are not countersunk to keep from physical contact with the lid 206, thereby aiding in heat transfer from the container to the lid.

[0023] In some embodiments a thermal fuse is thermally coupled to container 200 and electrically coupled to heater 202 (e.g. in series with heater 202) and provides protection against fire or overheating by removing power from heater 202 in the event of an overtemperature condition, thereby de-energizing heater 202.

[0024] With reference to Figure 3, in some embodiments a protective covering 330 made of plastic is placed over lid 306 to prevent injury from direct contact with the lid surface. In some embodiments protective covering 330 is made of wood. Protective covering 330 has holes 332 for allowing air circulation to cool lid 306 to the desired temperature. In some embodiments the lid inner-surface 336 is flat. In some embodiments the lid surface that faces the container includes a portion 338 that protrudes into the container when the lid is placed over the container thereby preventing lateral movement of the lid and reducing the amount of refinable material deposited on the portion of the region of lower thermal conductivity that faces the chamber.

[0025] With reference to Figure 4, in some embodiments a fan 440 is used to force air circulation thereby increasing the rate of heat removal. Fan 440 forces air to move through intake airholes 442 (formed in protective covering 430) past the surface of lid 406, and out the airholes 444. In some embodiments the direction of flow is reversed. In some embodiments baffling formed in either of the protective covering or the surface of the lid is included to provide increased heat transfer by the forced air. In various embodiments the fan runs at a constant speed independent of lid temperature; or, the fan is controlled to regulate the temperature of the lid to a constant temperature using a temperature sensor (e.g. a thermistor; a silicon temperature sensor comprising a diode, a junction, or a transistor; or, a thermocouple and a microprocessor; or, a thermostat).

[0026] In some embodiments a temperature sensor is coupled to the lid and a processor; the processor is further coupled to a fan. When energized by the processor, the fan cools the lid. The temperature sensor output is processed by the processor to estimate the temperature of the lid. The processor uses the processed temperature sensor output to energize the fan in a manner to bring the estimated lid temperature closer to a desired temperature using feedback-control techniques.

[0027] In some embodiments a thermostat coupled to the container is used to control heater operation.

[0028] Figure 5 shows a heat sink 550 similar to the type used to cool electrical components such as a microprocessor attached to lid 506. Heat sink 550 passively dissipates heat from lid 506 at a rate higher than the rate without heat sink 550, and is sized to provide a temperature sufficiently low at the inner surface of lid 510. In some embodiments lid 506 further comprises a protective covering over the heatsink wherein the protective covering includes holes allowing for air circulation and is similar to protective covering 330. In some embodiments a fan is used in conjunction with a heat sink to further increase cooling capacity.

[0029] In some embodiments the lid includes on the inner surface a non-stick surface similar to that used in nonstick cookware (e.g. PTFE, ceramic, or similar to as described in US Patent US7093340B2). A nonstick surface treatment helps aid the removal of the refined material, which can be sticky. In some embodiments the lid is cooled (e.g. in a refrigerator or freezer), thereby hardening the refined material and easing removal from the lid after refinement is completed. In some embodiments a membrane thermally coupled to the lid (e.g. Kapton film, paper, aluminum foil) is placed between the lid and the chamber so that the refined materials collect on the membrane, which is removed after refinement, thereby avoiding materials collecting directly on the lid.

[0030] In some embodiments the precise value of what range of lid temperatures are sufficiently low is determined through a design of experiments, experimentation, ortrial-and- error. In some embodiments high-performance liquid chromatography (HPLC) or gas- chromatography (GC) are used to identify the composition of the refined material deposited on the lid thereby allowing discrimination of refined material composition on a molecular basis.

[0031] In some embodiments the range of lid temperatures which are sufficiently low is determined by heating plant material comprising refinable material to a first temperature while maintaining the lid at a second temperature. After a fixed amount of time the lid is removed and the amount of refined material on the lid quantified. The process is repeated with new plant material with the lid maintained at a third temperature. After the same fixed amount of time the lid is removed and the amount of refined material on the lid quantified (e.g. weighed or measured volumetrically). This process is repeated for multiple lid temperatures and the results tabulated thereby allowing a temperature to be chosen that provides refined material at the rate desired; this temperature is a sufficiently low temperature. In some embodiments the decomposition-rate of refined materials, which increases with increasing temperature, is also considered in choosing a sufficiently-low lid temperature.

[0032] In some embodiments the desired chamber temperature is determined by heating plant material comprising refinable material to a first temperature while maintaining the lid at a second temperature. After a fixed amount of time the lid is removed and the amount of desired refined material on the lid quantified. The process is repeated with new plant material with the chamber maintained at a third temperature. After the same fixed amount of time the lid is removed and the amount of desired refined material on the lid quantified. This process is repeated for multiple chamber temperatures and the results tabulated thereby allowing a temperature to be chosen that provides refined material at the rate desired. In some embodiments the decomposition-rate of refined materials is considered in choosing a desired chamber temperature.

[0033] In some embodiments the lid directly contacts the metal of the container without a region having lower thermal conductivity.

[0034] In some embodiments the lid further incudes a heater distinct from the heater coupled to the container.

[0035] In some embodiments the lid is sealed to the container and gasses are prevented from escaping between the lid and the container during the refining process; sealing is accomplished using a seal (e.g. an o-ring, or gasket) and fasteners (e.g. screws, or clamps) to secure the lid to the container in the presence of pressure within the chamber.

[0036] In some embodiments the lid is separated from the heated container by a region of lowered thermal conductivity. Such a lowered region of conductivity allows the lid to maintain a different temperature than the chamber or container without a large amount of heat flux from the heater that would otherwise need to be dissipated from the lid.

[0037] In some embodiments the heater comprises a power resistor suitable for heating applications, such as a Riedon UAL-series aluminum-housed wirewound resistor, and is affixed to the container with a fastener (e.g. a screw, a rivet). In some embodiments, a thermally-conductive compound such as heatsink grease is applied to the container or the power resistor before affixing the resistor to the container to provide for a lower thermal resistance interface between the heater and the container.

[0038] In some embodiments high-conductivity regions of exposed metal within the region of lower conductivity are included; such regions of exposed metal provides a path of a portion of the container to more rapidly transfer heat from the container to the lid than were the regions of exposed metal not present.

[0039] In some embodiments the colder portion of the chamber (e.g. lid) is located lower in height than a hot portion thereby attenuating convection within the chamber.

[0040] In some embodiments the lid is kept above 100C to prevent condensation, thereby providing a dry surface for refined materials to collect upon.

[0041] With reference to Figure 6, in some embodiments the casing 612 extends continuously 608 above the top of the container providing a region of increased thermal resistance. The container is secured to the casing from the bottom: screw 660 is screwed into boss 662, formed in casing 612, through hole 664 in container 600. Thus, the screws do not protrude from the top surface allowing a region of lowered thermal conductivity to encircle the entire perimeter providing lower thermal conductivity than were the screws exposed towards the lid.

[0042] In some embodiments the region of lowered thermal conductivity includes regions of space for air pockets to form thereby reducing further the heat transfer from the container. As illustrated in Figure 7, fingers 770 of casing 712 are formed in a pattern such as a honeycomb pattern or in a grid pattern. Conductivity may be tuned by adjusting the number, height, width, or spacing of the fingers. In some embodiments, fingers project towards the container, versus being projected to towards the lid as shown in 770, with a flat surface at the casing top and the fingers projecting towards the container from this surface.

[0043] In some embodiments a region of lowered conductivity is coupled (e.g. fastened, screwed) to the lid as opposed to, or in conjunction with, a region of lowered conductivity coupled to the container.

[0044] In some embodiments the temperature of the lid is lower than the temperature of the container by a temperature between 25C and 75C. In some embodiments the temperature of the lid is lower than the temperature of the container by a temperature between 75C and 150C.

[0045] In some embodiments a timer is used to control the heater. The timer is started when the chamber temperature reaches a threshold. In some embodiments the timer is started when the heater is first energized without regard to a particular temperature threshold. After a predetermined period of time after the timer is started, the timer de-energizes the heater thereby halting the refining process.

[0046] In some embodiments, detection, estimation, or monitoring of deposited material at the lid inner surface using a detector is used to indicate when refinement has completed to a desired extent or to estimate an amount of material deposited on the lid. For example during refinement, using estimated deposition vs time data, refined material deposition over time may be fit to an exponential curve allowing the final amount of refined material to be estimated; the heater may be de-energized upon reaching a threshold, (e.g. 90%, 95%) of the estimated final value. In various embodiments mechanical, electrical, or optical techniques are used to detect deposited material.

[0047] In some embodiments, a mechanical sensor utilizes mass loading or resonant frequency shifting for detection, estimation, or monitoring of deposited material at the lid inner surface. In some embodiments a piezoelectric transducer, similar in construction to those used for low-cost speakers, is coupled to the inner lid surface. A thin layer of Kapton tape is placed over the piezoelectric transducer to prevent refined material from sticking to the transducer. As refined material deposits on the Kapton tape, the resonant frequency and frequency response of the piezoelectric transducer will change. An electrical circuit is used to estimate a frequency response characteristic (i.e. a gain and / or a phase at one or more frequencies) of the transducer by any of many well-known techniques including forcing a voltage across, and measuring a current through, the piezoelectric transducer at multiple frequencies; or, forcing a current through, and measuring a voltage across, the piezoelectric transducer at multiple frequencies. Conversion of frequency response to an amount of deposited material is accomplished by a design of experiments comprising applying a known amount of refined material and measuring a resonant frequency response. In some embodiments the frequency response characteristic is measured at the beginning of the refinement process to account for manufacturing variations or left-over refined material from a prior refinement cycle (e.g. to tare the sensor).

[0048] With reference to Figures 8a and 8b, in some embodiments, an electrical sensor utilizes a capacitance for detection, estimation, or monitoring of deposited material at the lid inner surface. In some embodiments a capacitive sensor includes a first electrode 800 and a second electrode 802 disposed upon, and electrically isolated from, the lid inner surface 810; the first and second electrodes are interdigitated with fingers separated by a distance. In alternate embodiments any other appropriate electrode configuration comprising two terminals is used, including when one of the electrodes is the lid itself. The first and second electrodes form a capacitor 824 the value of which will vary as material is deposited due to the differing dielectric constant between air and the refined material. Monitoring of the value of the capacitance or the change in capacitance is accomplished using a circuit with an amplifier 822 in combination with an excitation signal 828 applied to capacitor 824 at input node 830. The amplifier circuit includes a feedback element 820 which in this embodiment is a fixed capacitor such as a ceramic-chip capacitor with a parallel resistor to provide for dc biasing; in other embodiments a combination of capacitors and resistors is used according to well-known circuit techniques. Changes in capacitor 824 due to deposition of refined material are reflected by changes in circuit output 832 reflected in amplitude variations of waveform 834. In some embodiments the circuit output is further processed by an analog- to-digital converter coupled to a microcontroller or microprocessor. Refinement is deemed completed when the rate of change in capacitance decreases below a threshold. In some embodiments a processed estimate of capacitance is used to provide an estimate of the quantity of refined material under the lid based upon a relationship between capacitance and dielectric thickness established through either experiment or application of theory.

[0049] In some embodiments, an optical sensor utilizes index of refraction for detection, estimation, or monitoring of deposited material at the lid inner surface. In some embodiments an optical sensor comprises a photodiode to detect light (e.g. visible, infra-red, or ultraviolet), and a light-emitting diode (LED) to emit light in one or more wavelengths suitable for the photodiode. The photodiode is optically coupled to a first piece of clear material having an index of refraction higher than air, such as a clear plastic, silicone, or glass. The LED is similarly optically coupled to a second piece of clear material. The first piece of clear material and the second piece of clear material are separated by a gap. As refined material is deposited the gap is filled with refined material. Since the refined material has an index of refraction closer to that of the clear material than the air does the amount of optical energy coupled between the LED and the photodiode will increase as refined material is deposited. The output of the photodiode is processed to provide an estimate of the refined material.

[0050] The embodiments, techniques, components, connections, and other teachings described herein are examples and were chosen to provide a clear explanation without unnecessary obfuscation. The scope of coverage is not intended to be limited to the specific exemplary teachings set forth herein, but rather the scope of coverage is set forth by the claims listed below.

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