A PUBLICATION
Cannabis on Collision Course with Science
extractionmagazine.com ISSUE 17 Jan/Feb 2021
Extending the Power of Dense Gas It All Comes Beyond Extraction Out During Spoiler Alert - Dense Distillation Gas is Underused and Misunderstood
From Soil to Oil We Have the Technology but Why are We Using It? Crafting Cannabis Concentrates at Home Using Ethanol Extraction Hydrocarbon Extraction Fundamentals SUPERIOR POWER & PERFORMANCE
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Introducing Pollen Tech™! Born out of Greenlane Studio’s 15+ years of vaporization product expertise, Pollen Tech supplies the industry with high-quality and innovative vaporization solutions.
Our proprietary ceramic core technology delivers < 1% failure rate, impressive vapor production, and full flavor. Pollen Tech excels in creating customizable designs using high-quality, ethically-sourced materials. Contents From Gaseous Monster to Superhero 06 for Green Extraction and Purification
Extending the Power of 10 Dense Gas Beyond Extraction Publisher MACE Media Group Hydrocarbon Extraction Fundamentals CEO 14 Celeste Miranda Editor-in-Chief From Soil to Oil Jason S. Lupoi, Ph.D. 16 Authors Jason S. Lupoi, Ph.D. It All Comes Out John MacKay, Ph.D. 22 During Distillation Joe Kookoothe AC Braddock Crafting Cannabis Concentrates at Steven Bennett, Ph.D. Home Using Ethanol Extraction Troy Ivan 24 Harry Resin Joseph Encinosa Molecular Formulated Live Resin Designer 30 Marko Nedeljkovic Advertising Bradford Burgess High precision temperature control
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For more information visit : www.huber-usa.com/Unistat815 or call: 800.726.4877 6 EXTRACTION MAGAZINE From Gaseous Monster to Superhero for Green Extraction and Purification Repurposing carbon dioxide for wellness product manufacturing By Jason S. Lupoi, Ph.D.
Reduce. Reuse. Recycle — an environmental mantra. As sterilization [11], and botanical extraction and purification, garbage piles on land and in seas, augmented by COVID-19 which is the matter at hand. [1], our Earth continues to cry “Uncle.” Relentless packaging, improperly disposed of electronics, and the over extraction The Ideal Gas Law (PV=nRT; P for pressure, V for volume, of natural resources like fossil fuels offer glimpses into the n for amount of material, R for the ideal gas constant, and Earth’s banshee wail. At one point in my life, I was involved T for temperature) states that pressure and temperature in research on how plants could help lessen the use of fossil are proportional, meaning that as one goes up or down, the fuels, the burning of which creates greenhouse gases like other does in tandem. A substance’s critical point regards the carbon dioxide (CO2). [2] CO2 provided a suitable demon temperature and pressure combo that causes the substance and studies have demonstrated its contribution to rising, to behave as a liquid and a gas. These parameters can global temperatures. [3] I know, I know. Some people don’t be jockeyed to tune one’s extraction strategy based upon believe or even recognize the data but that’s negligible for specific analytes within the feed. this discussion. The point is that many efforts have sought to prevent relentless CO2 levels from polluting our world. Supercritical CO2 (sCO2, with a critical point of 31.1°C, 72.8 atm) is often used for decaffeinating coffees and teas, where
Due to its ostracization, CO2 comes very cheap. It can be it has been said to offer better selectivity for preferentially captured from industrial processes like burning fossil fuels removing caffeine while leaving essential flavor molecules for energy or transportation, cement production, or the forging of iron and steel. Or by giant machines that exemplify innovation meant to change the world. [4]
Once harnessed, it can be repurposed for applications like creating low-carbon liquid fuels or as a building block in chemical syntheses. [5] Another option for repurposing CO2 is to manipulate its temperature and pressure such that it becomes a supercritical fluid where it can be used to extract soils and marine sediments for hydrocarbon contaminant extraction and quantitation [6,7], alcohols from water [8], or organic contaminants like polycyclic aromatic hydrocarbons from plastic waste so the garbage can be recycled [9].
Repurposed CO2 can also be used as a substitute for more toxic chemicals used for dry cleaning [10], for medical device EXTRACTION MAGAZINE 7
behind. [12,13] sCO2 can also be used to remove fat from nuts and potato chips [14] and to extract antioxidants and omega fatty acids from algae [15,16] and crustacean by-products [17].
sCO2 and its subcritical complement have been frequently used to extract hops [18] and cannabis and essential oils contained within those and many other plants as diverse as patchouli [19], carrots [20], or medicinal mushrooms [21]. These extracts could be used on their own or in creating products like a tetrahydrocannabinol (THC)-rich vape cart, a rosemary essential oil for use in one’s cultivation due to the herb’s pesticidal properties from terpenes like eucalyptol, pinene, and camphor [22], or to create a terpene-infused beer like New Image Brewing did with their Pure Isolate India pale ale. (There’s even an sCO2 system on the can!)
Some cannabis product manufacturers have turned to sCO2 instead of hydrocarbon solvents to create concentrates like shatter and wax that do not come with worries of residual solvents, as the CO2 is depressurized back to a gas for subsequent recycling.
The ideal solvation of a substance occurs when the solubility parameter of the solute matches the solubility parameter of the solvent. Easy enough. While ethanol offers a solubility parameter close to many cannabinoids at ambient conditions, when the temperature is reduced, so is the solubility of undesirable constituents like waxes. [23] That’s a good thing and illustrates the foundation of winterization, but terpenes and cannabinoids are also less soluble as temperatures get colder. The overlap in solubility parameters between hydrocarbons and terpenes is substantial, but these solvents, as well as ethanol, require ethical disposal and remediation such that they are not taxing an already aching Earth. Dense CO2 provides suitable green alternatives. These principles apply to other plant ingredients, such as curcumin from turmeric, capsaicin from chiles, and beta-carotene from various other botanicals. [24]
Coming full circle, another green solution to obtain augmented stockpiles of beneficent, food-related phytonutrients regards using sCO2 on agricultural waste products that might be destined for use as feedstock for renewable energy applications. When specific crops have been suggested for fuel applications, the dichotomy of fuel versus food has proven divisive into two factions of thought. We might as well extract the most from any cultivated crop, whether oranges, onions, cannabis, or eucalyptus trees.
Molecules not required for bio-based fuels (which need cellulose) have purpose elsewhere. Hearing that farmers are 8 EXTRACTION MAGAZINE
growing hemp for cannabidiol (CBD) alone doesn’t exemplify and acetonitrile, both of which are health hazards that require the fundamental of maximizing the “fruits” of our labors. So, remediation. This could be to measure the tocopherol and running an sCO2 extraction on the biomass first can allow us ferulic acid found in the rice bran extract discussed or to to pull out remaining nutrients for wellness applications before measure the cannabinoid profile of a given chemovar. sending the cellulosic raffinate on its final journey to fuel. Examples of this include antioxidants from olive, grape, citrus SFC also provides a powerful method for product purification, waste, tomato, onion skins, and spent brewers’ yeast. [24] whether application is intended for separation of enantiomers (mirror-image molecules) or for remediating THC from Jerry King, Ph.D., offers a glimpse into this paradigm federally legal hemp products. [25] switch from fuel against food to fuel and food using rice as an example. [24] Brown and white rice can undergo sCO2 To end on a cosmic note, sCO2 has been implicated as a treatment to prolong shelf-life; rice bran can be defatted, potential life-sustaining solvent on other planets in the creating a powdered rice bran product; and the rice bran universe. [26] The life supported in these environments may can also be extracted, the product of which can be rich with be weird but sCO2 can catalyze reactions that do not happen tocopherol and ferulic acid. Glycerol can also be refined from in water exemplified by the fact that enzymes are more rice bran extract which can then be used in the formation of stable in sCO2 because of their augmented inflexibility (they polymers. Further treatment with other supercritical fluids can’t unravel). These environments also aren’t necessarily can produce biodiesel from the rice bran extract for energy or extraterrestrial like Venus because lurking below the ocean as a building block for creating surfactants. floor is a place flooded with sCO2.
But wait, there’s more, as the villainous CO2 can be used for So, there’s CO2 up above and sCO2 down below. We can supercritical fluid chromatography, or SFC. This technique demonstrate our evolution by better learning how to harness can be used for analytical or preparatory purposes. In the overabundance of something harmful for a greater analytical SFC, sCO2 provides the mobile phase to enable good while we continue to adopt advanced methods for its analyte separation, replacing organic solvents like methanol reduction. EXTRACTION MAGAZINE 9
References
[1] Sarkodie SA, Owusu PA. Impact of COVID-19 pandemic on Journal of Agricultural and Food Chemistry. 1996;44(2):574- waste management [published online ahead of print, 2020 Aug 578. [journal impact factor = 4.192; times cited = 10] 26]. Environ Dev Sustain. 2020;1-10. [journal impact factor = [15] Montanes F, Catchpole OJ, Tallon S, Mitchell K, Lagutin 1.930; times cited = 2] K. Semi-preparative supercritical chromatography scale plant [2] NASA. The causes of climate change. NASA website. polyunsaturated fatty acids purification. Journal of Supercritical accessed December 15, 2020. Fluids. 2013;79:46–54. [journal impact factor = 3.620; times cited = 16] [3] Lindsey, R. If carbon dioxide hits a new high every year, why isn’t every year hotter than the last? Climate.gov website. [16] Sanzo GD, Mehariya S, Martino M, et al. Supercritical published February 12, 2020; accessed December 15, 2020. carbon dioxide extraction of astaxanthin, lutein, and fatty acids from Haematococcus pluvialis microalgae. Mar Drugs. [4] www.carbonengineering.com 2018;16(9):334. [journal impact factor = 4.073; times cited = [5] Hepburn C, Adlen E, Beddington J, et al. The technological 38] and economic prospects for CO utilization and removal. 2 [17] Ahmadkelayeh S. Hawboldt K. Extraction of lipids Nature. 2019;575(7781):87-97. [journal impact factor = 42.778; and astaxanthin from crustacean by-products: A review times cited = 88] on supercritical CO2 extraction. Trends in Food Science & [6] US EPA. Method 3561: Supercritical fluid extraction of Technology. 2020;103:94-108. [journal impact factor = 11.077; polynuclear aromatic hydrocarbons. 1996. times cited = 0] [7] Librando V, Hutzinger O, Tringali G, Aresta M. Supercritical [18] Zekovic Z, Pfaf-Sovljanski I, Grujic O. Supercritical fluid fluid extraction of polycyclic aromatic hydrocarbons extraction of hops. J. Serb. Chem. Soc. 2007;72:81–87. from marine sediments and soil samples. Chemosphere. [journal impact factor = 1.097; times cited = 33] 2004;54(8):1189-1197. [journal impact factor = 5.778; times [19] Donelian A. et al. Comparison of extraction of patchouli cited = 63] (Pogostemon cablin) essential oil with supercritical CO2 and [8] Brignole E, Andersen P, Fredenslund, A. Supercritical by steam distillation. J. of Supercritical Fluids. 2009;48:15–20. fluid extraction of alcohols from water. Ind. Eng. Chem. Res. [journal impact factor = 3.620; times cited = 118] 1987;26(2):254–261. [journal impact factor = 3.573; times [20] Glisic, S. et al. Supercritical carbon dioxide extraction cited = 74] of carrot fruit essential oil: chemical composition and [9] Alassali A, Aboud N, Kuchta K, Jaeger P, Zeinolebadi antimicrobial activity. Food Chemistry. 2007;105:346-352.
A. Assessment of supercritical CO2 extraction as a method [journal impact factor = 6.306; times cited = 84] for plastic waste decontamination. Polymers (Basel). [21] Lupoi J. Extracting medicinal mushrooms, chapter 2: 2020;12(6):1347. [journal impact factor = 3.426; times cited = supercritical CO extraction. Extraction Magazine. published 0] 2 June 25, 2020; accessed December 16, 2020. [10] Pallado P. Dry-cleaning with liquid carbon dioxide. [22] Lupoi J. The Cannabis Terpene Experience. Mace Media Industrial Chemistry Library. 2001;9:641-649. [journal impact Group. 2020. factor = N/A; times cited = 2] [23] King J. The relationship between cannabis/hemp use in [11] Soares GC, Learmonth DA, Vallejo MC, et al. Supercritical foods and processing methodology. Current Opinion in Food CO technology: The next standard sterilization technique?. 2 Science. 2019;28:32-40. [journal impact factor = 4.577; times Mater Sci Eng C Mater Biol Appl. 2019;99:520-540. [journal cited = 10] impact factor = 5.880; times cited = 14] [24] King JW. Modern supercritical fluid technology for food [12] Marco I, Riemma S, Iannone R. Supercritical carbon applications. Annu Rev Food Sci Technol. 2014;5:215-238. dioxide decaffeination process: a life cycle assessment study. [journal impact factor = 9.840; times cited = 74] Chemical Engineering Transactions. 2017;57:1699-1704. [journal impact factor = 0.76; times cited = 5] [25] Lupoi J. Green cannabinoid isolation using supercritical fluid chromatography. Extraction Magazine. July-August 2020. [13] Zosel K. Process for recovering caffeine. US Patent No. 3806619. 1974. [26] Budisa N, Schulze-Makuch D. Supercritical carbon dioxide and its potential as a life-sustaining solvent in a planetary [14] Chiou R, Yu Z, Wu P, et al. Partial defatting of roasted environment. Life (Basel). 2014;4(3):331-340. [journal impact peanut meals and kernels by supercritical CO using 2 factor = 2.991; times cited = 42] semicontinous and intermittently depressurized processes. 10 EXTRACTION MAGAZINE Extending the Power of Dense Gas Beyond Extraction Spoiler Alert: Dense Gas is Underused and Misunderstood By John MacKay, Ph.D., Synergistic Technologies Associates
Extraction Magazine focuses on techniques and technologies these tools’ power, you need to acquire the accessories. considered for the concentration of compounds in cannabis The analogy holds for power tools that drill holes, reverse (including hemp because hemp is cannabis) and other direction, and cut wood, and takes me to the use of counter- botanicals. It has expanded the technological knowledge of current extraction, counter-current separation, the making all types of concentration (extraction and separation). With of nanoparticles and crystallization with the addition of a the expansion of the digital version, it is tempting to forget thermally controlled column, or a nozzle for rapid expansion that people once had to extract at a scale that served few for the formation of crystals. The base is the pump, heat people and many had to rely on word of mouth or the web to exchangers, pressure regulators, and switching valves. [1] learn about the extraction of cannabis. There was little motive to expand beyond extracting oil. Dense Gas & Pressure Dense gas (e.g., supercritical fluid) is used in very diverse The pioneers’ choices for extraction were based on what applications outside of cannabis or botanical extraction, was available to them in box stores, local hardware such as for the cleaning of microbes from chicken [2], bones stores, or purchased by mail. Without access to analytical before grafting [3], or parts used in aerospace, as well as tools (e.g., chromatography), the sources they relied on the extraction of various plants for their natural compounds. were based on the authors’ experiences to validate their Many of the early supercritical fluid extraction products had choices. Photographs and reports of injuries were (and are) a pressure limit of less than 2,000 psi (pounds per square sometimes front-page news. inch), and temperature control was maintained with a sump pump and a heating coil. There were no regulations on Most of the legacy extraction processes could not be scaled products certified by state-licensed certified professional to provide the amount and quality of extracted material engineers. needed for the medical level – certainly not the new hemp quantities needing to be processed. The ability to have These were the products appropriate at the time. But today, mobile and affordable at-line testing has changed the the products go to 10,000 psi. To open the envelope from low extraction process. pressure to high pressure is not just about the extraction of cannabinoids but rather the ability to remove what you want People were limited to focus on cannabis extraction with to extract. Many studies demonstrate the power of pressure. only low technology instruments. The initial systems had [4] no control or knowledge of flow rates and rudimentary temperature control versus the systems available today. If Dense Gas & Temperature you follow the progression of tools for mixing ingredients, The temperature needs to be regulated to perform a people first used their hands. This progressed to simple controlled extraction, including keeping a temperature below tools, hand whisks, and hand mixers. Then we had electric 0°C. To have this type of control, you need a broad range of mixers and food processors. To take full advantage of temperatures. EXTRACTION MAGAZINE 11 12 EXTRACTION MAGAZINE
20 minutes for each 10-liter run, and running them in series, you would not need to stop. A 50-liter vessel might take 4 hours to complete with the low pressure and the time to fill and empty the vessel. With a loading time of 10 minutes, the 10-liter vessel will do 80 liters of material in the same 4-hour period.
The Four S’s of Extraction Speed: From the time you begin to prepare the material until the time you have the ingredients you desire, what are the things that concern you the most? Cycle time of the entire concentration process Grinding, moisture, chemical state, setup of instruments, Standard Operating Processes (SOPs), collection and post-processing, and then set up for the next cycle (clean-in-place), etc.
Scale: Ability to start small (lab) and transition to pilot and expand the manufacturing Choosing between multiple units versus larger units with the same amount of output per day Complying with amounts of material that are allowed at a facility or facilities Complying with the chemical engineers looking for the parts of the process that are minor in the lab and possibly major in larger-scale processes Sample preparation, introduction, waste removal
Selectivity: Influencing the order of elution in the entire concentration process Dense Gas & Flow Rate Providing a minimal amount of overlap with other Pressure and temperature control the solubility and vapor compounds in the mixture pressure of extracted materials. The flow rate determines Polarity the mass transfer of material from the extractor to the Size separators. A real flow rate of 2,000 grams of carbon dioxide Class of compounds (CO ) per minute versus 200 grams of CO per minute is 2 2 Volatility theoretically a ten-fold increase in throughput. Mass transfer Solubility needs to be scaled to thermodynamics. $pend Size of Components in the System What are the investment criteria that will influence The scale of system components and the tubes that connect the business? them is critical. The vessels need to match the throughput When is the return on assets? of ingredients needed for manufacturing. Is a 10-liter vessel Based on the ENTIRE process as well as the withstanding 10,000 psi better than a 50-liter vessel rate at individual processes? 2,000 psi? If the flow rate is the same on both, the 10-liter Based on the future direction of the company? vessel will far outperform the 50-liter vessel. It might be only EXTRACTION MAGAZINE 13
Number of Extraction and Separator Vessels and Accessories separates the oil from the trichomes, making extraction faster Maximizing a continuous operation of a modern system and more complete. necessitates a minimum of two extraction vessels and three collection vessels. Extraction occurs in one vessel, while the Physical Science is Objective – The Economics Will Follow other is loaded for the next extraction. Anything less undermines An emotional attachment to any extraction process will the power of dense gas potential. Bringing the extraction vessel drive the individual to be tempted to make subjective to high pressure and then selectively reducing the pressure versus objective decisions. There is always someone who across multiple vessels provides an opportunity to segment approaches a seminar or attends an exhibition with a singular the compounds by their disparate solubilities in CO2 at different passion for ethanol, propane, butane, CO2, isopropanol, densities. It requires an understanding of the principles of phase acetone, hexane, etc. They say, “The only solvent to use diagrams and an understanding of solubility. is ______. If you are doing it any other way, you are wrong.” Their list is long on the benefits of their process and The addition of ethanol as a co-solvent is well documented. all others are full of limitations. But as regulatory standards encompass the technology for clean-in-place and the need to make more applications like Do you use the same process to clean your hands? Are you nanoparticles or counter-current extraction, this will become cleaning from grease or from potential exposure to a virus? even more essential. The types of nebulizers available for You use different choices depending on the material on your extraction and separators are important, just like accessories hand. This is the same for extraction of compounds in the for making bread, cookies, or whipped cream. cannabis plant.
Accessories for Pre- and Post-Processing Most of the next steps following extraction regard removal of unwanted components, such as waxes and lipids. References This is done by diluting the oil in a minimum amount of ethanol, freezing it for 24 to 48 hours, filtering it, and then [1] Baldino L, Scognamiglio M, Reverchon E. evaporating the ethanol to 5% and the remaining in an oven. Supercritical fluid technologies applied to the extraction Decarboxylating in an open oven or removing terpenes and of compounds of industrial interest from Cannabis sativa lipids before distillation are steps used in the early days. L. and to their pharmaceutical formulations: A review. The Journal of Supercritical Fluids. 2020;165:104960. Inline Accessories [journal impact factor = 3.744; times cited = 6] Extraction is based on the pressure and temperature of the [2] Gonzalez-Alonso V, Cappelletti M, Bertolini FM, CO2. For example, at a fixed pressure of 2,000 psi, increasing Lomolino G, Zambon A, Spilimbergo S. Microbial the temperature from 45°C to 55°C reduces density and inactivation of raw chicken meat by supercritical carbon the number of compounds extracted increases. This is also dioxide treatment alone and in combination with fresh true of cold brew versus hot brew coffee. The hotter the culinary herbs [published online ahead of print, 2019 temperature, the more compounds are extracted. The time is Sep 25]. Poult Sci. 2019;pez563. [journal impact factor overnight for cold brew and minutes for hot brew. = 2.659; times cited = 5]
A second example is removal of compounds during the [3] Bulat M.V., Pigaleva M.A., Novikov I.V., et al. The process. Many people use filters on their facets to clean method of cleaning and modification of the material their water. With the appropriate accessories, you can for bone xenografts in bi-phase media containing high pressure CO . Доклады Академии наук (Doklady do inline decolorization, remove metals, and concentrate 2 cannabinoids. This would be similar to regenerating a Akademii Nauk). 2019;485(5):588-593. [journal impact carbon filter with a solvent that would remove the captured factor = N/A; times cited = 0] pesticides and ions from the waters. [4] Moreno T, Montanes F, Tallon S, et al. Extraction of cannabinoids from hemp (Cannabis sativa L.) using high More recent products have taken advantage of hyphenated pressure solvents: An overview of different processing principles that have provided a new market. Using option. J. of Supercritical Fluids. 2020;161:104850. ultrasonic-, microwave-, or electrodynamic-assisted [journal impact factor = 3.744; times cited = 5] extraction combined with a non-polar media like CO2 14 EXTRACTION MAGAZINE
Hydrocarbon Figure 2b: Residue from bad gas Extraction Fundamentals By Joe Kookoothe, MPX Arizona
One of the beautiful things about hydrocarbon extraction is Figure 2a: Old tank the different ways it can be approached. There ultimately are no rules to performing them other than doing them safely 2. Using Clean Solvent and compliantly. Different cultivars, cultivation techniques, The second fundamental of hydrocarbon extracts is to use resin freshness, solvent blends, equipment, and extraction clean solvent. When solvent or hydrocarbon gas is delivered methods make the term “hydrocarbon extraction” quite to extraction labs, it’s not always sent in a brand-new tank vague. Not every extraction is performed for the same (Figure 2a). Therefore, it is crucial to check the quality of purpose. For example, some are performed with the intent the gas before using it. Any gas that has a foul odor should of making premium, craft-batch dabbing products, while not be used. To check gas quality, empty some gas into a others might simply intend to recoup whatever oil was left collection vessel, allow it to evaporate out, and observe any in the trim of flower sold to the market. Less fresh or trim residue (Figure 2b). If the gas is clear, non-odorized, and material is often extracted for a more cost-effective product residue free, it’s ready to use. for the consumer, while fresh-frozen resin might be used to make premium products of the highest quality. (Figure 1) 3. Solvent Temperature So, what are the fundamentals that seem to be consistent for The third fundamental aspect of all hydrocarbon extractions hydrocarbon extractions everywhere, regardless of all these is that solvent should be as cold as possible. And when I say variables? “cold,” I mean -45°C or below (if possible), which is beneath the boiling points of both butane and propane, the most 1. Quality Starting Material common solvents used. Sure, warmer solvent will provide a The first, and most fundamental thing to understand, is higher yield, but it also washes heavier compounds into the that no matter the extraction situation, poor quality starting oil, which dilutes the final product’s potency and essential material going into the extractor will not magically come out oil concentration. Often, lipids and cellular material from the as top quality. Extractors are simply removing the oil from biomass are co-extracted with warmer solvent (above -45°C) the starting material and hopefully not adding anything. Good quality starting material can, however, be ruined if some fundamental techniques are overlooked.
Figure 3: Two extractions of the same starting material. The jar to the left is lighter in color and was extracted using chilled solvent at -82°C Figure 1. Results from fresher starting material versus the darker jars on the right, which were extracted using room- (left) versus less fresh starting material (right) temperature solvent. EXTRACTION MAGAZINE 15
which can be seen visually. Figure 3 shows two extractions can handle. With too much pressure, a screen can tear (see of the same starting material. The jar to the left is lighter in Figure 4), letting all the plant matter into the collection pot color and was extracted using chilled solvent at -82°C versus with the oil! It is best to check with manufacturers for screen/ the darker jars on the right, which were extracted using gasket tolerances prior to use. room-temperature solvent. Figure 5: Depicts using a separate Cold solvent results in coagulation of plant lipids and cellular vacuum gauge material, causing them to harden and essentially be too independent of the oven’s gauge to large to fit through the filter screens at the bottom of the verify the oven’s material columns. This coagulation occurs because heavier gauge is properly compounds have reached their precipitation point, which calibrated is when substances solidify out of a solution. That’s what happens in the winterization of oils. When washing the solvent over the biomass, it’s important to pass it all entirely through before the solution warms up above the precipitation point of the undesirables. Otherwise those fats and such will redissolve and end up passing through filters into the collection tank.
More sophisticated closed-loop systems have large 5. Removing Residual Solvents refrigeration chillers or utilize evaporation cooling to keep The fifth and final fundamental of hydrocarbon extraction solvent constantly cold. These elaborate systems may also is to remove remnants of the hydrocarbon solvent. Freshly have a separate “de-wax” chamber specifically for in-line poured extract oil still contains hydrocarbon gases that winterization. Older or simpler setups may not have these must be removed via agitation or vacuum oven. To ensure fancy cooling systems, which is often why extractors turn to vacuum ovens reach the deepest vacuum possible, check dry ice to chill their solvent tanks manually. that all hoses, seals, and connections are tight. Also, using a separate vacuum gauge independent of the oven’s gauge is 4. Filtration helpful to verify the oven’s gauge is properly calibrated (see The fourth fundamental of hydrocarbon extraction is that the Figure 5). materials column needs to have some sort of filter to screen plant material out from the oil being extracted. The idea is Ultimately, no hydrocarbon extraction is complete until much the same as using coffee filters which are 20-micron a third-party testing lab confirms that residual solvents, filters. Smaller filters, such as 10 microns, can work as well, amongst other things, are at safe levels. The threshold but they will constrict flow more than larger ones. Smaller for residual hydrocarbons in safe-to-consume cannabis filters causing slower flow often tempt the extractor to use concentrates depends on state-to-state regulations. more pressure to pass the fluid through the screens faster, Fortunately, batch samples which fail testing for high residual but beware not to exceed the pressure that the filter screen hydrocarbons can be remediated further via continuing agitation or vacuuming. Some batches may require more time than others due to varying viscosities of the oils.
Figure 6: Finished hydrocarbon extract
Figure 4: Image of a torn filter screen 16 EXTRACTION MAGAZINE From Soil to Oil We Have the Technology But Why Are We Using It? By AC Braddock, Eden Labs
There are a plethora of extraction techniques and a medical system based in patent rights and profits over technologies to procure the intrinsic value from plants. The patients; and the political hobbling of a new industry based real question is: What do we want out of it and why? The how in real medical science that could alleviate many social ills if is truly secondary to the purpose of an extraction and causes only more emphasis had been placed on why instead of how us to miss the big picture regarding the design of products in the innovation process. that help solve societal problems. In the case of cannabis, it lies within regulation of our endocannabinoid system and a Let’s begin in 1805 when Freidrich Wilhelm Adam Serturner myriad of illnesses and disorders that this plant can remedy. extracted the first alkaloid from the opium poppy and named it morphine. [3] Fast forward to 1853, and the Think of it this way – you are training to run in a race. The type hypodermic needle was invented. The popularity of this of race matters in how you train. You don’t train for a marathon new plant derivative grew as it could be injected whereas by only doing sprints. The same is true with extraction – the other treatments like cannabis could not since it’s not end justifies and drives the means. You don’t do a full run with water soluble. What they did not realize for many years supercritical fluid extraction to make sauce. You sprint. You was morphine’s highly addictive, and all too often, fatal don’t use warm ethanol to get a terpene-rich, golden oil. You go properties. Despite that, cannabis was still widely used for a lower (temp) and slower. Each method and solvent has benefits vast number of inflictions until a few capitalists in the early and drawbacks, so the process isn’t as important as the reason 1900s created an incredibly effective propaganda campaign why the extraction is being performed, and the why is much to stigmatize and penalize the use of cannabis and hemp in larger than a single extracted product or method. all its forms and uses.
The natural world is full of highly beneficial plants whose In 1913, a wonderful thing happened because as the Ford curative powers have been demeaned and sometimes company was gearing up to mass produce the Model-T, purposely obliterated by Big Agriculture, greed, racism, they discovered a way to fuel automobiles with biomass and modern allopathic medicine. A prime example is of from hemp. However, this was extremely disturbing news course Cannabis, which was utilized for health by humans to the DuPont Company, who wanted to sell gasoline to fuel for thousands of years [1] until the 19th century when Ford’s cars. [4] They were also perturbed by the possible pharmaceutical companies that still exist today, and who had competition of hemp with their new petroleum-based dozens of products on the market, stopped manufacturing inventions: synthetic rubber, plastic, rayon, and oil-based cannabis products. Some notable examples are: Parke Davis industrial paint. Dupont had even invented a sulfur-based had 27 products, Upjohn had 30, Eli Lilly made 23, Abbot process to turn wood fiber into paper. Laboratories had 4 and is the only existing pharmaceutical company still associated with cannabis through its spin-off This was also disturbing news to Andrew Mellon, who was company AbbVie Pharmaceuticals who made the synthetic the Secretary of the Treasurer under President Herbert pill, Marinol. [2] What happened? Hoover and owned the 6th largest bank in the country, Mellon Bank, which was invested in DuPont’s paper-making process, A series of events fueled by careless innovation, greed, and and in 1916, the US Department of Agriculture processed racism that culminated in the subjugation of whole plant paper from hemp pulp and determined that it was superior to treatments with synthetics and isolated molecules and ended the wood version, and was far more durable, sustainable, and in an opiate crisis; the highest incarceration rate in the world; efficient to grow and produce. EXTRACTION MAGAZINE 17
At this juncture, William Randolph Hearst, who owned thousands of acres of timber to make pulp for the US newspaper industry, determined something had to be done. He didn’t want competition in his vertical business plan from tree to paper to selling paper, so he used his newspapers to promote a racist propaganda campaign to undermine the hemp and medical cannabis industries. This fear-based propaganda campaign claimed cannabis was a dangerous drug that caused murderous psychotic breaks, black men to take advantage of stoned white women, and a range of other utterly and devastatingly destructive nonsense whose immoral and unscientific assertions still negatively affect our culture and the formation and formulations of our burgeoning cannabis and hemp industries.
The nail in the coffin for a millennia of cannabis use came from the formation of the Federal Bureau of Narcotics in 1930 by The US Department of the Treasury. Andrew Mellon appointed his niece’s husband Harry J. Anslinger as its Chief, and Anslinger began his own propaganda campaign in Congress and with law enforcement across the country. After two short years, the agency proposed The Marijuana Tax Act of 1937 which severely penalized physicians from using Cannabis in their practices, so they stopped using it and substituted cannabis with opiates and morphine to treat pain and a wide range of ills. Why we innovate matters more than innovation. The adage “necessity is the mother of invention” obviously comes to mind.
Do you see how careless innovation based in “how” led to the demise of thousands of years of medical cannabis use? Why? Why separate the strongest molecule out of poppies to procure pure morphine? Why did we make plastics and fuel out of fossil fuels when we could have used hemp? Why are we remediating delta-9-tetrahydrocannabinol (THC)? Why are we extracting for cannabidiol (CBD) and not the whole plant? Why is an isolate of CBD better than a concentration of the whole plant? It has been shown that it’s not better for many patients [5,6], so why are we extracting it? Isolating it? Of course, we have the technology but why are we using it? CBD isn’t the end all be all of cannabinoids; it is simply, currently, politically palatable and THC is not. Why? Lies made up by greedy shortsighted men for short-term gain nearly 100 years ago. This position is not scientifically sustainable – not in the holistic treatment of human genetics with plant genetics. It’s not science, it’s politics. And as Nikola Tesla said, “Science is but a perversion of itself unless it has as its ultimate goal the betterment of humanity.”
Hash Cube We have, in fact, lost thousands of years of knowledge on the Photo credit: Randy Reed, Lehua Group USA™ simplest of equations – that we are, or should be, completely 18 EXTRACTION MAGAZINE
entwined with the things that naturally grow at our feet for our health and wellbeing. If you haven’t read Ishmael by Daniel Quinn and are in the cannabis or hemp industry, you should. [7] Also Stolen Harvest: The Hijacking of Our Global Food Supply by Dr. Vanda Shiva. [8] Why? Because extraction is a myopic image of the big picture. Instead of nonstop coverage of a “stolen election,” we should have had constant coverage of the pathetic condition of our soil and our bodies and how to boost our immune systems with the things we imbibe. Soil nutrients are being depleted from outdated farming techniques by Big Agriculture. We actually have to eat more to get the same nutritional value that used to be in our food supply. The farm-to-table movement aims to bring us back to local, sustainable farming that’s better for us, and the same is true for the cannabis brands that understand that soil to oil, the entire process is related to the extraction process.
A good extraction begins in the soil and in the genetics of plants and people. A good extraction is directly related to the “why” of the branded end product. A good extraction in the cannabis industry is the same as a good extraction in the natural products industry. Did you know they have been on the same hockey stick growth pattern since the early 1990s? Is this coincidence? Or is it a cultural return to valuing the Live Resin tremendous capacity of plants to preserve and promote Photo credit: Randy Reed, health? It’s obvious our health is undeniably dependent Lehua Group USA™ on a healthy planet and that the hippies (and healers for thousands of years) were right about pretty much everything from the real benefits of aromatherapy to hemp seeds and of course, cannabis, konopi, qannabbos, bhang, ganja, etc., whatever name you want to call it.
So, what matters these days in capturing the essences of the plant in mechanical separation? System designs
using butane, propane, and supercritical CO2 are largely unchanged in their basic performance. Any changes in the systems are minor in actual functionality but big on fine- tuning for specific products and an increase in capacity. At this point, the focus is on specialized extraction standard operating procedures (SOPs) for specific products and SOPs to avoid or enhance postprocessing, which is simply an added layer of extraction, especially if it’s to remediate particular cannabinoids based on supplying mitigated oils to a politicized market.
Skilled CO2 operators are generally doing short runs at low temperature and pressure to procure essentially pure Pure Terps terpenes or terp sauce, then turning up temperature and Photo credit: Randy Reed, Lehua Group USA™ pressure to pull out more resistant cannabinoids. Pressures EXTRACTION MAGAZINE 19
near 3,000 psi (207 bar) and temperature near 170°F (77°C) can yield rapid extractions that need minimal refinement for a whole plant product or to be further extracted for a mitigated product. As with hops (cannabis’s kissing cousin) and many other botanicals, it is widely agreed that, as the cannabis and
hemp markets mature, large scale supercritical CO2 will be the most cost-efficient method of extraction as the solvent is inexpensive and easy to store, remove from the oil, and dispose of, and the process has an extremely wide range of SOPs for an abundance of end products.
Cannabinoids are extremely easy to extract compared to molecules in other botanicals, and an ethanol extraction is exceptionally fast and a relatively inexpensive capital expenditure with control in end product by manipulating temperature and filtration, which is why the hemp industry has adopted this method early in its growth as an industry. Most large-scale ethanol extraction has moved to cryo (cold) temperature extraction. This type of extraction is most prevalent with getting CBD out of hemp. There are still major inefficiencies with this method, however, as chilling large vats of ethanol is time-consuming, expensive, hard on pumps, bearings, seals, etc., and can present workplace hazards. Alternative methods using ambient temperature
CO2 High Terps Full Spectrum ethanol and vastly improved filtration eliminate the expense Photo credit: Randy Reed, Lehua Group USA™ of large chillers and energy use and decrease run times. Terpenes can be retained using this methodology if the Terp Sauce, SCFE material is run at a low temperature (not cryo) with a slower Photo credit: Randy Reed, Lehua Group USA™ run time.
Improving ethanol extraction involves developing continuous feed extractions, whereby hemp and ethanol are flowing through a centrifuge on a continuous basis, and a stream of cannabinoid saturated ethanol is streaming out one port while spent hemp with low ethanol content is flowing out another. This continuous process is in the R&D stage. Current designs on the market are batch processes requiring constant filling and emptying of filter sacks which have varying degrees of durability.
Light hydrocarbon extraction has also moved towards cryo extraction and increased capacity, although there are only a few large-scale systems in use for hemp. Cannabinoids and their associated terpenes are uniquely suited for efficient extraction with multiple solvents in a cryo state. Most hydrocarbon extraction is done on an artisan level with high-grade cannabis to make boutique products like waxes, shatter, crumble, and terp sauce to supply a specific segment of the recreational industry. 20 EXTRACTION MAGAZINE
Photo credit: Randy Reed, Lehua Group USA™
What is somewhat new is the growing use of co-solvents in all the aforementioned solvents and systems. There is a tremendous range of possibilities in this area that affect References specialized SOPs, run times, operational expense, and post processing. [1] Lupoi J. Cannabis in Ancient Asia. Terpenes & Testing Magazine website. uploaded January 31, 2020; Companies acquiring these kinds of systems have become accessed December 30, 2020. far more savvy in doing their due diligence before making a [2] Borchardt D. Pfizer, Eli Lilly were the original medical purchase. As transactional extraction system manufacturers marijuana seller. Forbes Magazine website. uploaded flooded the market, horror stories of failed engineering and April 8, 2015; accessed December 30, 2020. a lack of industry understanding in regulation and market [3] History of Morphine. Talbott Recovery website. creation has led to atrocious customer service, class accessed December 30, 2020. action lawsuits, and the tragic demise of those businesses purchasing from subpar manufacturers who are essentially [4] Reichard Z. Exposed: the full story behind why machine shops and not biotech entrepreneurs. marijuana is illegal & classified as a Schedule 1 drug. Medical Jane website. uploaded January 23, 2013; How this industry takes its next steps in a friendlier political accessed December 30, 2020. climate will determine why we are extracting this plant. It will [5] Pamplona FA, da Silva LR, Coan AC. Potential clinical also establish how extraction technology evolves to support benefits of CBD-rich cannabis extracts over purified CBD the efficacy of end products and to lead our culture in the in treatment-resistant epilepsy: observational data meta- sustainability of an industry based in health and wellness. If analysis [published correction appears in Front Neurol. we, as an industry, lead from “why,” those submerged in the 2019 Jan 10;9:1050]. Front Neurol. 2018;9:759. [journal politics will come around to the empirical realization that we are impact factor = 2.889; times cited = 52] the change in healthcare, circular economics, and social reform. [6] Gallily R, Yekhtin Z, Hanus L. Overcoming the bell-shaped dose-response of cannabidiol by using cannabis extract enriched in cannabidiol. Pharmacology & Pharmacy. 2015;6(2):75-85. [journal impact factor = N/A; times cited = 39] [7] Quinn, D. Ishmael. Bantam. 1995. [8] Shiva, V. Stolen Harvest: The Hijacking of Our Global Food Supply. South End Press. 2000. When process expertise and support matter. PROVIDING TECHNOLOGY & EQUIPMENT WORLDWIDE FOR OVER 50 YEARS.
Engineered and manufactured in the USA, Pope’s critical processing equipment has been utilized world - wide by the pharmaceutical, biomedical, food and fine chemical industries. Our distillation, reaction, filtering and other equipment are available in lab testing, pilot plant and production scale. Pope’s unparalleled depth of experience in equipment design, application support, toll processing, piloting and testing help you achieve the best possible results.
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This system design has been utilized by pharmaceutical Distillation systems available from lab through multi-stage companies to optimize isolation. Simultaneously running production size, to greater than 100 kg/hr throughput. the crystallizing Reactor and Nutsche Filter Dryer provides Pictured: 10 kg/hr PLC operated 2-Stage turnkey system. efficiency along with the greatest purity, yield & product value in your cannabinoid applications.
DECARBOXYLATION • REACTION • EVAPORATION • DISTILLATION • ISOLATION
Cannabis site: www.popecannabisdistillation.com | 262-268-9300 @popescientificinc | Main site: www.popeinc.com | Manufactured in WI, USA 22 EXTRACTION MAGAZINE It All Comes Out During Distillation By Steven Bennett, Ph.D., Prescott Logic Technologies, Ltd.
Choosing the right extraction techniques to utilize in Since cannabinoids are quite large, they require some coaxing your cannabis processing facility will take some careful from the oil matrix with very high temperatures and an ultra- considerations. Do the current regulations permit your deep vacuum, whereas ethanol requires only a warm water desired approach? Will you require Class 1 Division 1 (C1D1) bath to effectively be separated. And, unlike the variability in enclosures for operation? How much solvent will you need on quality witnessed during extraction, distillation marks the first hand, and how often can you reuse it? Which final products step in product standardization – that is, the quality of the do you wish to distribute? Answers to these questions and starting oil, in terms of potency, determines the quantity of more will ultimately be weighed by each licensed producer to cannabis distillate produced and represents the cannabinoid select the best method(s) to satisfy their business plan. There fraction of the starting biomass. Simply stated, distillation are benefits and drawbacks of every extraction method, so allows an operator to “boil off” molecules of interest from developing a clear understanding of these is paramount for those of less interest (for more information on this topic, success.
Following extraction, material can either be packaged and sold directly to consumers, typically as “craft” concentrate products, or further refined to a higher level of purity. The techniques utilized after extraction, typically referred to as “post-processing,” are less varied than the art of extraction itself. The “classic” method involves the introduction of a polar solvent (typically ethanol) and cold temperatures to freeze out lipids and waxes, along with moisture that would interfere with subsequent processes and lend to a less-desirable end product. Winterization effectively precipitates these constituents out of the extracted oil, regardless of the selected extraction method, to best prepare the material for fractional distillation.
Distillation describes, simply, the separation of molecules by boiling point. The process describes the recollection of solvent in a rotary evaporator as well as the separation of cannabinoids from extracted crude oil during wiped film. The main difference between these two techniques is based on the molecular weight and relative volatility of the target molecule(s). EXTRACTION MAGAZINE 23
Reference [1] Bennett, S. “Life After Extraction: Standardization Begins with Distillation”, Extraction Magazine, May-June 2019.
please review “Life After Extraction: Standardization Begins 10x. So, the cost of a continuous system might be closer to with Distillation”). [1] Unlike extraction, there are relatively 200,000 USD (for the same evaporative surface area), but that few choices to make when it comes to selecting fractional can be quickly justified with such greatly reduced operating distillation equipment (aka short path, wiped film, thin film, costs. and molecular distillation). The first choice for an operator to make regards use of a benchtop unit or a vertical system. The main decision to make with wiped film distillation equipment, as with any processing equipment, is between Benchtop systems offer very attractive price points and can cost and quality. One exists at the expense of the other, “get you there” as far as proof of concept, but they are reputed and this cannot be emphasized enough: You get what you to have lower throughputs, high operator variability, long pay for. So, maybe you want to run a lean startup and that cleaning procedures, easily damaged parts, and higher risk of unit manufactured for ⅓ the price of the competition seems damaging product from heat (oxidation). This leads operators, appealing at first. But it’s only a short matter of time that the almost inevitably, to acquiring vertically-designed wiped film equipment fails, parts take weeks (or months) to arrive, and distillation systems, as the overall performance is far more support is non-existent. There is no shortcut to quality in reliable, which is of obvious importance when producing buying a car, nor in the components that are relied upon to standardized products, as with Good Manufacturing Practices, drive a successful company. or GMP, where assuring the end-user the same experience is paramount. At Prescott Logic, we understand the plight of the hemp and cannabis operator and do not simply repurpose equipment Once a vertical molecular still has been chosen, there from another industry. We put our focus into achieving is one fundamental selection to be made aside from the the deepest vacuum possible and offer numerous mindful manufacturer: continuous operation (automatic) versus batch- innovations to boost the performance of the equipment. We to-batch distillation (manual). This decision is based largely offer a patented stainless steel and borosilicate glass design on cost, as manual systems are typically below 100,000 USD that is available in a manual system (P1000 LITE) and can and are limited in throughput, since the operator is required be upgraded to the continuous version (P1000 Pro) when to stop and restart between passes. Continuous systems have the customer is ready. Similarly, our modular design allows specialized gear pumps hermetically sealed to the vacuum for conjoining several processes together as the company within the distillation system but open to the atmosphere so grows, allowing operators to preserve precious resources that crude oil can be fed in and out of the system 24 hours a when they are needed most. Moreover, our equipment can day, 7 days a week, without stopping runs. Typically, manual be rapidly cleaned and maintained. We build our distillation distillation systems are suitable for producers that need systems with the operator and the business in mind. Some 10kg per shift or less – anything more warrants the cost of a groups are happy to make sales; we are happy to watch your continuously operating system as the throughput is closer to business succeed. 24 EXTRACTION MAGAZINE
Crafting Cannabis Concentrates at Home Using Ethanol Extraction By Troy Ivan, ExtractCraft
Extraction is intimidating, if not scary, for people unfamiliar Lastly, it doesn’t perform well with hemp for cannabidiol (CBD) with it. Most mistakenly assume making high-quality extraction due to typically lower cannabinoid concentration and extractions at home safely is beyond their reach, so simple it’s greasier nature. So, while I do like rosin and it makes great infusion is typically the first step for those beginning to terpene-rich dabs, it may not be the best choice for a home experiment with cannabis “processing.” Infusion is attractive user looking for more flexibility and value-based extraction. because it’s simple and familiar, very much like cooking, and the end product looks like a normal and familiar oil. However, Then, there is ethanol extraction. Until recently, ethanol infusion is very limited in use and this oil is typically low in extraction wasn’t really an option for making high-quality potency. For a person to really expand their horizons and products at home. I would argue it’s the best choice. Ethanol experience true versatility, potency control, and an enormous extraction isn’t new to home processing but the ability to jump in the quality of their crafting, they must wade into the use it to make high-quality cannabis extractions is. Cannabis unfamiliar and unknown process of extraction. Luckily, there medicinal tincture making dates back hundreds of years, but in are options today that make it easier than most people expect. more recent history, products like a legendary, old school, and rather esoteric cannabis extract known as “cherry oil” were Which Extraction Method is Best for You? made in the 1960s and 1970s. The Isomerizer was also used in Choosing which extraction method is preferable comes down the 1970s, rice cookers in the 1990s, and, more recently, water to what a person is looking to make. The main forms of home distillers have been used to make low quality but effective extraction include using a rosin press to squeeze rosin from medicine. flowers or using solvents like butane and ethanol. While some will argue the opposite, I consider butane too dangerous to be Those processes were performed in an open atmosphere and performed at home and it won’t be part of the discussion here. at high temperatures, resulting in oxidization, decarboxylation, Rosin and ethanol are both well suited for the home user but I and destruction of any terpenes and flavonoids that may have believe one is a better choice if you can only choose one. been present. Previously, the only way to avoid the downfalls of open atmosphere and high temperatures was to use a rotary Rosin pressing is very safe and has become very popular. I evaporator (rotovap) for ethanol recovery, but rotovaps aren’t like rosin but there are limitations and downsides that limit its exactly affordable or easy for home use. New technology attractiveness. Rosin is primarily used with high-grade flower has stepped in and solved the equipment problem, adapted or dry-sift/bubble hash and the squishing isn’t as easy as it protocols, built communities, provided education and made looks. Lower-quality flower and trim don’t work well due to a the process as easy as pushing a button so that anyone can lower amount of extractable oil content. Then the final product, operate the equipment easily and safely. while smelling amazing, has a large wax and lipid component that chars bangers and is quite unhealthy for the lungs. Next, Ethanol extraction also has some disadvantages due to the the large amount of oil that remains in the pressed chips, nature of the solvent. Ethanol is polar and nonpolar to different pucks, and bags is evidence of how inefficient the process is. degrees. The problem with working with solvents that have EXTRACTION MAGAZINE 21 26 EXTRACTION MAGAZINE
of concentrates like sap, sugar, wax, pull-n-snap, shatter, and sauce that can be used to make vapables, edibles, topicals, potent infusions, and more.
In addition to cannabis, ethanol extraction is great for culinary, scenting (like for perfume, soaps, and candles), apothecary, and home remedies. Users can make extractions using espresso beans, lavender, mint, elderberry, citrus peel, cinnamon, and more with the same primary process. The world really opens up when you begin to consider all the wonderful scents and flavors that can combine with cannabis and hemp extractions. All of this is achievable by beginners with food-grade inputs.
The value advantage that comes with ethanol extraction is attractive. In addition to using cannabis and hemp flower, polar tendencies is that they are attracted to hydrophilic home extractors can also process trim and shake, turning components like chlorophyll, while hydrocarbons don’t have possible waste into gold. Good sugar leaf can process as well that problem. Fortunately, using cold temperatures can limit as flower, while old beat up trim isn’t perfect but can still be and eliminate chlorophyll extraction. Another disadvantage is used to make incredibly strong edibles and topicals. Nothing that, in this process, the terpene component may not be as goes to waste. strong as with hydrocarbon extraction and rosin. Using cold temperatures with ethanol extraction to avoid chlorophyll Lastly, just as I am a fan of rosin, it just so happens that sacrifices some terpene extraction, but it’s the cleanest ethanol extraction also likes rosin. Ethanol can be used to possible concentrate made compared to hydrocarbon solvents’ winterize rosin, removing the lipids and wax to substantially toxic nature and the higher lipid and wax content in rosin. The increase potency. It will lose some terpenes that the clean end product is incredibly smooth with a serious potency lipids and wax bind with but will be cleaner and stronger. boost, so the small terpene disadvantage is a large potency Remember the inefficiency I mentioned about rosin leaving advantage in disguise. lots of cannabinoid content behind in the chips, pucks, and bags? With a bit of ethanol and the new low temperature The new equipment designed by ExtractCraft specifically ethanol recovery devices, that waste can be recovered in for the home user is where cannabis or hemp gets much concentrate form. Diehards will flip out at the rosin no longer more interesting than it’s ever been before and provides being “solventless” but I would argue that food grade ethanol everyday people easy access to very cool advanced skills. The measured in parts per million (ppm) is harmless, especially equipment is self-regulating so it’s easy enough for anyone to compared to the obvious danger of big lipid and wax hits to use and, when it’s reclaiming all the ethanol under vacuum, it’s the lungs on a regular basis. exceedingly safe. Moreover, there’s great flexibility afforded to make full spectrum extractions with any cultivar the user Ethanol Extraction Process chooses. The equipment works at low temperatures under The base process for ethanol extraction is the same as any vacuum, so no appreciable decarboxylation occurs during the solvent extraction. Before beginning the extraction process, the process. If a decarbed end product is desired, either the flower desired end product must be decided because it will determine can be decarbed before extraction or in the resultant oil after how each of the processing steps is approached. To avoid extraction. disappointment, having a realistic expectation with regard to what the starting material is capable of is key. Then, just four With this approach, the user has a degree of control and easy steps: prepare material, combine ethanol with a botanical versatility that was considered unobtainable. The product to allow the oils from the plant to be fractionated, separate coming out of the equipment at the end of the process is botanical matter and filter tincture, and finally evaporate solvent classified as “oil.” This oil closely resembles the cannabinoid from the oil. It sounds much more complicated than it actually and terpene profile of the starting material [see reference 1 for is. Each step has unique considerations that will affect how the an example] that was used and is the foundation of most forms concentrate will turn out, so let’s look at each step individually. EXTRACTION MAGAZINE 27
Step 1. Prepare Material Ethanol extraction doesn’t work well with moisture so all material needs to be dry. Any material can be used: kief, flower, mids (middle-grade cannabis), larf (immature buds), shake, or trim. The golden rule is pretty much quality-in, quality-out, so the starting material is a good indicator of best possible outcome. Old, beaten up trim is great to make a potent, effective medicine but don’t expect to turn it into top-shelf fire.
Trim and Shake: These are very convenient to use because they are pretty much ready to be used as is. A good bag of shake has a ton of trichomes settling in the bottom of the bag which is like hidden treasure. One downside is that the plant material is usually torn up with lots of material damage so it’s easy for chlorophyll to be picked up by the ethanol and will result in what we call “green leak.” Another downside is that trim and shake are not usually stored well, so advanced oxidation and decarboxylation will result in darker end products. Just because they are dark doesn’t mean they aren’t great medicine; it just means you recovered great value from low quality starting material.
Kief: While kief is kief, what’s riding along with it requires consideration. Kief is simply a collection of trichomes holding the targeted oils, but in collecting the kief, very small ground up biomass particles may also be present. If there’s ground up plant material in the kief, it could easily result in green leak. The cleaner the kief, the better.
Flower: The beauty of working with flower is that, aside from any trimming, the botanical structures are mostly intact with the lowest risk of green leak. The challenge is getting it into a form where ethanol can freely access and flow over the individual structural components including the trichomes tucked inside the center of the flowers. To make the cleanest oil for vaping, you will want to be careful and break up the buds by hand causing the least amount of damage possible. On the other hand, if you are making edibles and topicals, buds can be broken up more aggressively or mechanically, but the more damage done, the more green leak there will be.
Fresh frozen and live resin made with hydrocarbon extraction is some of the most aromatic and terpy extractions around. Unfortunately, ethanol doesn’t do well with the moisture content of fresh material. However, freeze-drying fresh material for ethanol extractions makes top-shelf concentrates.
Rosin Byproducts: Pressed chips, pucks, and bags are rich in unclaimed cannabinoid heavy oil. Preparation is similar to 28 EXTRACTION MAGAZINE
flower — the more you break them up, the higher the risk of -40°F (-40°C) for maximum protection. The marginal benefit green leak is, but depending on the intended use, it may or of temperatures lower than -40°F (-40°C) begins to diminish may not matter. The oil hung up in bags can be very clean quickly, in my experience. The colder temperatures allow for while the pressed contents may lend themselves to green good agitation for the ethanol to diffuse most effectively. leak, so it can be beneficial to take apart and process the screen bags and their contents separately. This is a great Time of Exposure: This is the most flexible factor, as what’s way to recoup great value and make up for the inefficiency happening with the tincture as time passes can be observed. of pressing. If there’s a change you aren’t happy with it, the soak can be stopped. Old schoolers making RSO and FECO often talk Step 2. Combine Ethanol with Cannabis or Hemp about leaving the cannabis to soak for days, weeks, or even When ethanol is combined with cannabis or hemp, you are months. At room temperature with agitation, I would suggest mainly targeting the trichomes’ cannabinoid and terpene that ethanol is aggressive enough to collect everything content. Some people want a clean, golden extraction valuable in 5-10 minutes. In these conditions, all material and others want to go deep and pull out all plant-based forms will produce a deep green tincture and result in a compounds. Managing the balance of material, temperature, black extract, but material that’s more damaged will end up and time of exposure in the primary tincture extraction is how with more chlorophyll faster. the characteristics of the final product are determined. For golden extracts, we have to work with cold temperatures Material: The more intact the material is, the more to avoid any green pickup. The optimal time of exposure will aggressively time and temperature can be used. Agitation vary between different materials. If the soak time is uncertain, is also important, as it allows the ethanol to work its way a small sample can be tried first to find the best time/ around the material. If the material is more intact, agitation temperature combination; then move into working with larger will do nothing but improve yield, but if the material is very samples, saving some frustration. beaten up, it will increase green leak. In general, the normal freezer temperature time range is 5-30 Temperature: Ethanol is aggressive at room temperature, minutes; the shorter end of the range is for trim and is longer for grabbing everything it can uninhibitedly and it doesn’t need flower that’s in good shape. When working at much time to do so. Cold temperatures can be used to have -40°F (-40°C), the range is 20-60 minutes. At low temperatures, a winterizing effect reducing the pickup of lipids and wax. the rate of extraction slows, so 5- to 10-minute washes lead The temperature range can be from ambient down to -70°F to very low yields. In my experience, the yield is maximized (-57°C). In general, room temperature would be used for a near the 60-minute mark with dry ice but I have had success green/black Rick Simpson Oil (RSO) or Full Extract Cannabis stretching this out to 48 hours just for testing and still oil (FECO), freezer temperatures for decent lipid, wax, and maintained a beautiful color with no appreciable increase in green leak protection, and then temperatures of around yield.
Step 3. Separate Botanical Matter And Filter Tincture There are two separate operations here. First, separate the cannabis away from the ethanol tincture quickly to arrest the risk of green leak. A fine wire mesh strainer works very well for separating the plant material. The point is to use something that flows very fast but catches all the green material.
The second operation involves filtering small plant particles; there are a couple options. For making edibles and topicals, the very best filtration isn’t necessary – two coffee filters can do a pretty good job. It’ll just take quite a while for the tincture to work its way through because the filters will quickly clog with the small particles. To make the highest quality concentrate, EXTRACTION MAGAZINE 29
fine filtration is important. The easiest and quickest way to apprehensive about a small amount of ethanol remaining, but do this is by using a vacuum-assisted Buchner filtration set it’s useful to keep in mind that it’s food-grade ethanol made with filter papers of around three microns. The vacuum assist for human consumption; the vanilla extract in the cupboard is makes it fast and the fine filter papers make it crystal clear. 35% alcohol and no one worries about using it as is. This is my recommended standard operating procedure. For a vapable end product, some form of simple post- Step 4. Evaporate Solvent from Cannabis Oil processing should be used to purge the oil. The simplest This is the easiest part. Using the new equipment available, the approach is to spread the oil in a thin layer on a silicone mat filtered tincture can be loaded. The processing happens at a and allow it to air dry for a day or two. We’ve seen air-purging push of a button, working under vacuum at low temperatures get down to 2,000 ppm in just 1-2 days. To take the post- for 2-3 hours. When it’s finished, the ethanol from the tincture process purging further and faster, a vacuum oven can be will be reclaimed and separated for reuse, and the cannabis oil used, but most home users find air-drying sufficient to make will be ready for collection. nice quality pull-n-snap or wax. You can get fancy and whip the oil with a little heat and hit it with some vacuum to make How to Use the “Oil” crumble or let it set in an airtight closed container, and in a “Oil” is used to describe the first increase in form stability “loose” state (consistency of oil) to work on making some from an ethanol tincture. As the residual ethanol purges from sauce. Once you have the oil, you have the foundation for the oil, the concentrate will continue to increase in stability many concentrate forms and uses. over time. Many concentrate forms can be made using the oil. When the oil is collected from the ethanol recovery device, it’s probably between 3%-5% ethanol. This is pretty much ready to be used to add to carrier oils, making edibles, or adding to topical formulations. People sometimes get
Reference [1] Ichibancrafter, “Closed Wash Decarb (CWD): Activate Cannabinoids and Keep the Terpenes”, www. extractcrafter. com. Uploaded October 23, 2020; Accessed December 7, 2020. 30 EXTRACTION MAGAZINE
Molecular Formulated Live Resin Fresh Frozen Flowers vs Trim By Harry Resin & Joseph Encinosa, Accentian, Inc.
Live Resin Manufacturing from Cannabis Trim Currently, traditional live resin retails for $14 to $16 a gram A proprietary hardware hydrocarbon solution whereas we retail live resin for $10 to $12 a gram.
Today, two types of cannabis oil cartridges dominate the vape In addition to the cost savings, our proprietary extraction market. Brands use either a distillate base or a hydrocarbon system extracts more THC content than traditional methods extraction using butane and/or propane. Distillate is crude oil using fresh frozen material. This creates a higher THC content that has been further refined through a wiped film evaporator. product than traditional live resin (Tables 1-3; our product is Crude is traditionally manufactured from cannabis trim which related in Table 3). contains little, if any, taste or flavor. By nature, the distillation process further degrades the product. Therefore, distillate is Live Resin Pen typically combined with botanical or cannabis terpenes to re- The longstanding industry supposition is fresh frozen provides introduce the flavor profile. Recently, the cannabis industry has the customer a stronger, richer, fuller flavor product. Quality shifted to using distillate combined with HTE, or high terpene live resin is considered the closest experience to flower, just extraction, to create a “live resin-type” cartridge. in a dab or cartridge. Once the oil is processed, it is put into a device that forces the tetrahydrocannabinolic acid (THCA) Today, live resin is one of the most commonly found inputs to crystallize or “crash out”, leaving behind the terpene-rich in vape cartridges. Live resin is manufactured using fresh fraction. What’s left is HTE and a diamond layer of THCA frozen cannabis flower which is harvested, vacuum sealed, and crystalline. This terpene layer is what’s typically used for both immediately frozen on the cultivation. While expensive, this refined live resin and “live resin-type” pens. For the refined process helps limit terpene degradation because it remains cartridges, this layer is blended with distillate to change the frozen up to the hydrocarbon extraction process. This in- viscosity of the oil so that its cartridge is stable meaning that demand oil is extracted using hydrocarbons in a closed-loop THCA does not crystallize thereby prohibiting the cartridge system at sub-zero temperatures of -70°C or colder. This from working. resulting live resin is more of a full spectrum oil that has not been degraded by temperature like distillate. By using fresh For live resin pens, the HTE fraction is blended back into frozen flower as its starting input, live resin better represents the converted THCA crystals. This conversion process the original taste of the flower. decarboxylates the THCA into delta-9 THC so that the oil in the pen is stable and the right level of viscosity. Our data suggests At Accentian Inc, we have invented a proprietary hardware that these cartridges have an average of 4.85% terpenes and hydrocarbon extraction system that unlocks the same delta- 79% THC content (Table 1). 9-tetrahydrocannabinol (THC) molecules from trim that were previously only found in fresh frozen flower. Since the input Distillate Pen is fresh indoor trim, our live resin costs a fraction of the price Distillate-based cartridges makes up the bulk of vape sales in of live resin extracted from fresh frozen flower. In turn, our California. Distillate is refined through a process of distillation value-based proposition is passed on to our product offering. and usually involves first producing crude oil via ethanol EXTRACTION MAGAZINE 31 32 EXTRACTION MAGAZINE
Cultivar Terpenes % THC % Cultivar Terpenes % THC % L’orange 4.9 76.5 GMO 16.4 82 Strawberry Lemonade 3.5 81.6 Forbidden Fruit 19.3 80 Blueberry 6.3 76.6 Skunk Berry 6.1 94 Average % 4.9 78.2 Into the Pines 5.9 91 Table 1: Live Resin (Fresh Frozen) Average % 11.9 86.8 Table 3: Molecular Formulated Oil Cultivar Terpenes % THC%
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