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Challenges with Process Scale Up in Cannabis/Hemp Extraction

By Darwin Millard
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What makes scaling up your process so difficult?

There are many factors that can lead to the challenges people face when scaling up their processes. These challenges are not unique to the cannabis/hemp industry, but they are exacerbated by the consequences generated from decades of Reefer Madness. In my time operating in the cannabis/hemp space, 15+ years, I have seen established equipment vendors and sellers of laboratory supplies, like Sigma-Aldrich (now Millipore-Sigma), Fisher-Scientific, Cerilliant, Agilent, and others, go from reporting individuals inquiring about certified reference materials to setting up entire divisions of their companies to service the needs of the industry. Progress. But we are still a fledgling marketplace facing many challenges. Let’s look at a few specific to process scale up.

Darwin Millard will deliver a presentation on this topic during the Cannabis Extraction Virtual Conference on June 29. Click here to learn more.Equipment Availability: Lack of available equipment at larger and larger process scales can severely impact project timelines. Making not only equipment acquisition difficult, but also limiting the number of reputable equipment manufacturers you can work with.

Non-Linear Expansion: NEVER assume your process scales linearly. Perhaps one of the most avoidable mistakes during process scale up. You will quickly find that for many processes you cannot just put in a larger unit and expect a proportional increase in output. This is because as process equipment increases so to must utilities and other supporting infrastructure, but not only that, process vessel geometry, proportions, and design are contributing factors to process efficiency as your scale of operations increases.

Hazardous Material Quantities: Just as important to the process as the equipment are the solvents and reagents used. As your scale of operations increases so does your demand and production of hazardous materials; solvents including carbon dioxide (CO2), ethanol, and liquid petroleum gases (LPG) like Butane and Propane are obvious hazards, but so too are the refrigerants used in the chillers, fuels used to power generators, steam created to heat critical systems, and effluents and wastewater discharged from the process and supporting systems. Not every municipality wants thousands of gallons of flammable substances and hazardous waste being generated in their backyard…

Contractor/Vendor Misrepresentation: Finding out in the middle of you project that your contractor or equipment vendor has never set up a system at this scale before is never a good feeling. Unfortunately, contractor and vendor misrepresentation of qualifications is a common occurrence in the cannabis/hemp space.

If all this was not bad enough, all too often the consequences of improper planning and execution are not felt until your project is delayed or jeopardized due to misallocation of funds or undercapitalization. This is especially true when scaling up your production capacity. Now let’s look at some ways to avoid these mistakes.

The Rule of 10

Construction drawings for a piece of process equipment.

When scaling up your process, NEVER assume that a simple linear expansion of your process train will be sufficient. It is often the case that process scale up is non-linear. Using the Rule of 10 is one way of scaling up your process through a stepwise iterative approach. The Rule of 10 is best explained through an example: Say you are performing a bench-top extraction of a few grams and want to scale that up to a few thousand kilograms. Before jumping all the way to your final process scale, start by taking a smaller jump and only increase your bench-top process by a factor of 10 at a time. So, if you were happy and confident with your results at the tens of grams scale, perform the same process at the hundreds of grams scale, then the thousands of grams scale, tens of kilograms scale, and so forth until you have validated your process at the scale of operations you want to achieve. By using the Rule of 10 you can be assured that your process will achieve the same yields/results at larger and larger scales of operation.

Scaling up your process through an iterative approach allows you to identify process issues that otherwise would not have been identified. These can include (but by no means should be considered an exhaustive list) improper heat transfer as process vessels increase in size, the inability to maintain process parameters due to inadequately sized utilities and/or supporting infrastructure, and lower yields than expected even though previous iterations were successful. However, this type of approach can be expensive, especially when considering custom process equipment, and not every processor in the cannabis/hemp space is going to be in the position to use tools like the Rule of 10 and instead must rely on claims made by the equipment vendor or manufacture when scaling up their process.

The Cannabis/Hemp Specific Process Equipment Trap

How many times have you heard this one before: “We have a piece of process equipment tailor-made to perform X,Y,Z task.”? If you have been around as long as I have in the cannabis/hemp space, probably quite a few times. A huge red flag when considering equipment for your expansion project!

Unless the equipment manufacturer is directly working with cannabis/hemp raw materials, or with partners who process these items, during product development, there is no way they could have verified the equipment will work for its purported use.

GMP compliant phytocannabinoid processing facility underconstruction.

A good example of this are ethanol evaporation systems. Most manufacturers of evaporators do not work with the volumes of ethanol they claim their systems can recover. So how did they come up with the evaporation rate? Short answer – Thermodynamics, Heat Transfer, and Fluid Mechanics. They modeled it. This much surface area, plus this much heat/energy, with this much pressure (or lack thereof), using this type of fluid, moving through this type of material, at this rate of speed, gets you a 1000-gal/hr evaporator or some other theoretical value. But what is the real rate once an ethanol and cannabis/hemp solution is running through the system?

For a straight ethanol system, the theoretical models and experimental models are pretty similar – namely because humans like alcohol – extensive real-world data for ethanol systems exist for reference in designing ethanol evaporators (more accurately described as distillation systems, i.e. stills). The same cannot be said for ethanol and cannabis/hemp extract systems. While it is true that many botanical and ethanol systems have been modeled, both theoretically and experimentally, due to prohibition, data for cannabis/hemp and ethanol systems are lacking and the data that do exist are primarily limited to bench-top and laboratory scale scenarios.

So, will that 1000-gal/hr evaporator hit 1000-gal/hr once it is running under load? That’s the real question and why utilizing equipment with established performance qualifications is critical to a successful process scale up when having to rely on the claims of a vendor or equipment manufacturer. Except this is yet another “catch 22”, since the installation, operational, and performance qualification process is an expensive endeavor only a few equipment manufacturers servicing the cannabis/hemp market have done. I am not saying there aren’t any reputable equipment vendors out there; there are, but always ask for data validating their claims and perform a vendor qualification before you drop seven figures on a piece of process equipment on the word of a salesperson.

Important Takeaways

Improper design and insufficient data regarding process efficiencies on larger and larger scales of manufacturing can lead to costly mistakes which can prevent projects from ever getting off the ground.

Each aspect of the manufacturing process must be considered individually when scaling your process train because each element will contribute to the system’s output, either in a limiting or expansive capacity.

I go further into this topic in my presentation: Challenges with Process Scale Up in the Cannabis/Hemp Industry, later this month during Cannabis Industry Journal’s Extraction Virtual Conference on June 29th, 2021. Here I will provide real-world examples of the consequences of improper process scale up and the significance of equipment specifications, certifications, and inspections, and the importance of vendor qualifications and the true cost of improper design specifications. I hope to see you all there.

Until then. Live long and process.

extraction equipment

THC Remediation of Hemp Extracts

By Darwin Millard
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extraction equipment

Remediation of delta-9 tetrahydrocannabinol (d9-THC) has become a hot button issue in the United States ever since the Drug Enforcement Agency (DEA) released their changes to the definitions of marijuana, marijuana extract, and tetrahydrocannabinols exempting extracts and tetrahydrocannabinols of a cannabis plant containing 0.3% or less d9-THC on a dry weight basis from the Controlled Substances Act. That is because, as a direct consequence, all extracts and tetrahydrocannabinols of a cannabis plant containing more than 0.3% d9-THC became explicitly under the purview of the DEA, including work-in-progress “hemp extracts” that because of the extraction process are above the 0.3% d9-THC limit immediately upon creation.

The legal ramifications of these changes to the definitions on the “hemp extracts” marketplace will not be addressed. Instead, this article focuses on the amount of d9-THC that is available in the plant material prior to extraction and tracks a “hemp extract” from the point it falls out of compliance to the point it becomes compliant again and stresses the importance of accurate track-n-trace protocols at the processing facility. The model developed to support this article was intended to be academic and was designed to follow the d9-THC portion of a “hemp extract” through the lifecycle of a typical CO2-based extract from initial extraction to THC remediation. A loss to the equipment of 2% was used for each step.

Initial Extraction

For this exercise, a common processing scenario of 1000 kg of plant material at 10% cannabidiol (CBD) and 0.3% d9-THC by weight was modeled. This amount, depending on scale of operations, can be a facility’s total capacity for the day or the capacity for a single run. 1000 kg of plant material at 0.3% d9-THC has 3 kg of d9-THC that could be extracted, purified, and diverted into the marketplace. CO2 has a nominal extraction efficiency of 95%, meaning some cannabinoids are left behind in the plant material. The same can be said about the recovery of the extract from the equipment. Traces of extract will remain in the equipment and this little bit of material, if unaccounted for, can potentially open an operator up to legal consequences. Data for the initial extraction is shown in Image 1.

Image 1: Summary Data Table for Typical CO2-based Extraction of Phytocannabinoids

As soon as the initial extract is produced it is out of compliance with the 0.3% d9-THC limit to be classified as a “hemp extract”, and of the 3 kg of d9-THC available, the extract contains approx. 2.8 kg, because some of the d9-THC remains in the plant material and some is lost to the equipment.

Dewaxing via Winterization and Solvent Removal

Dewaxing a typical CO2 extract via winterization is a common process step. For this exercise, a wax content of 30% by weight was used. A process efficiency of 98% was attributed to the wax removal process and it was assumed that 100% of the loss can be accounted for in the residue recovered from the equipment rather than in the removed waxes. Data for the winterization and solvent recovery are shown in Image 2 and 3.

Image 2: Summary Data Table for Typical Winterization of a CO2 Extract
Image 3: Summary Data Table for Solvent Removal from a CO2 Extract

Two things occur during winterization and solvent removal, non-target constituents are removed from the extract and there is compounded loss from multiple pieces of process equipment. These steps increase the concentration of the d9-THC portion of the extract and produce two streams of noncompliant waste.

Decarboxylation & Devolatilization

Most cannabinoids in the plant material are in their acid form. For this exercise, 90% of the cannabinoids were considered to be acid forms. Decarboxylation is known to produce a mass difference of 87.7%, i.e. the neutral forms are 12.3% lighter than the acid forms. Heat was modeled as the primary driver and a process efficiency of 95% was used for the conversion rate during decarboxylation. To simplify the model, the remaining 5% acidic cannabinoids are presumed destroyed rather than degraded into other compounds because the portion of the cannabinoids which get destroyed versus degrade into other compounds varies from process to process.

Devolatilization is the process of removing low-molecular weight constituents from an extract to stabilize it prior to distillation. Since the molecular constituents of cannabis resin extracts vary from variety to variety and process to process, the extracts were assumed to consist of 10% volatile compounds. The model combines the decarboxylation and devolatilization steps to account for complete decarboxylation of the available acidic cannabinoids and ignores their weight contribution to the volatiles collected during devolatilization. Destroyed cannabinoids result in an amount of loss that can only be accounted for through a complete mass balance analysis. Data for decarboxylation and devolatilization are shown in Image 4.

Image 4: Summary Data Table for Decarboxylation and Devolatilization of a CO2 Extract

As the extract moves along the process train, the d9-THC concentration continues to increase. Decarboxylation further complicates traceability because there is both a known mass difference associated with the process and an unknown mass difference that must be calculated and justified.

Distillation

A two-pass distillation was modeled. On each pass a portion of the extract was removed to increase the cannabinoid concentration in the recovered material. Average data for distilled “hemp extracts” was used to ensure the model did not over- or underestimate the concentration of the cannabinoids in the distillate. The variables used to meet these data constraints were derived experimentally to match the model to the scenario described and are not indicative of an actual distillation. Data for distillation is shown in Image 5.

Image 5: Summary Data Table for Distillation of a Decarboxylated and Devolatilized Extract

After distillation, the d9-THC concentration is shown to have increased by 874% from the original concentration in the plant material. Roughly 2.2 kg of the available 3 kg of d9-THC remains in the extract, but 0.8 kg of d9-THC has either ended up in a waste stream or walking out the door.

Chromatography – THC Remediation Step 1

Chromatography was modeled to remove the d9-THC from the extract. Because there are several systems with variable efficiency rates at being able to selectively isolate the d9-THC peak from the eluent stream, the model used a 5% cut-off on the front-end and tail-end of the peak, i.e. 5% of the material before the d9-THC peak and 5% of the material after the d9-THC peak is assumed to be collected along with the d9-THC. Data for chromatography is shown in Image 6.

Image 6: Summary Data Table for d9-THC Removal using Chromatography

After chromatography, a minimum of three products are produced, compliant “hemp extract”, d9-THC extract, and noncompliant residue remaining in the equipment. The d9-THC extract modeled contains 2.1 kg of the available 3 kg in the plant material, and is 35% d9-THC by weight, an increase of 1335% from the distillation step and 11664% from the plant material.

CBN Creation – THC Remediation Step 2

For this exercise, the d9-THC extract was converted into cannabinol (CBN) using heat rather than cyclized into d8-THC, but a similar model could be used to account for this scenario. The conversion rate of the cannabinoids into CBN through heat degradation alone is low. Therefore, the model assumes half of the available cannabinoids in the d9-THC extract are converted to CBN. The entirety of the remaining portion of the cannabinoids are assumed to convert to some form of degradant rather than a portion getting destroyed. Data for THC destruction is shown in Image 7.

Image 7: Summary Data Table for THC Destruction through Degradation into CBN

Only after the CBN cyclization step has completed does the product that was the d9-THC extract become compliant and classifiable as a “hemp extract.”

Image 8: Summary Data Table for Reconciliation of the d9-THC Portion of the Hemp Extract

Throughout the process, from initial extraction to the final d9-THC remediation step, loss occurs. Of the 3 kg of d9-THC available in the plant material only 2.1 kg was recovered and converted to CBN. 0.9 kg was either lost to the equipment, destroyed in the process, attributable to the mass difference associated with decarboxylation, or was never extracted from the plant material in the first place. All of these potential areas of product loss should be identified, and their diversion risk fully assessed. Not every waste stream poses a risk of diversion, but some do; having a plan in place to handle waste the DEA considers a controlled substance is essential. Without a track-n-trace program following the d9-THC and identifying the potential risk of diversion would be impossible. The point of this is not to instill fear, instead the intention is to shed light on a very real issue “hemp extract” producers and state regulators need to understand to protect themselves and their marketplace from the DEA.

The Craft of Extraction: Like Beer Making, It’s All About Control

By Jeremy Diehl
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Any brewmaster from the more than 7,000 U.S. craft breweries will tell you one of two things: That their art is a science, or that their science is an art. The answer might depend upon the brewer’s individual approach, but a combination of experience, process, precise measurement and intuition is exactly what’s required to create great beer. In a very similar way, the cannabis industry has its own version of the brewmaster: Extraction technicians.

A cannabis extraction technician deploys knowledge from multiple science disciplines to apply industrial solvents, heat and pressure to plant matter through a variety of methods with the aim to chemically extract pure compounds. Extraction techs use their passion for the cannabis and hemp plants, combined with chemistry, physics, phytobiology and chemical engineering to help create a result that’s not quite art, but not quite completely science. By manipulating plant materials, pressure, heat and other variables, the extraction technician crafts the building block for what will become an edible, tincture or extract.

Similarly, brewmasters use their knowledge of multiple science disciplines like chemistry and microbiology, as well as different brewing processes and a variety of ingredients to develop creative recipes that result in consistent, interesting beers. The brewmaster’s work is both science and art, as well. And they also manipulate plant materials, pressure, heat and other variables to achieve their desired results.

Author Jeremy Diehl collects cannabis extract from equipment for testing

“I would certainly consider brewing to be an art and a science, but it takes a very disciplined approach to create consistent, yet ever evolving beers for today’s craft market,” says Marshall Ligare, PhD. Research Scientist at John I. Haas, a leading supplier of hops, hop products and brewing innovations. “We work to ensure brewers can create something different with every new beer, as well as something that helps create an experience as well as a feeling.”

In both brewing and extraction, the art comes in the subjective experience of the craftsman and his or her ability to curate the infinite possibilities inherent in each process. However, both are a science in their requirement of establishing production methodologies that guarantee a consistent, reliable product experience every time to win customer loyalty (and regulatory compliance). In the same way hops determine recipes for beer flavors, the cannabis plant determines extraction recipes, especially considering the role that terpenoids play in the quality, flavor and effects of the end product.

The development of new and appealing cannabis products is beginning to mimic the vast variety of craft beers now found all over the world. In the same way beer connoisseurs seek out the perfect stout, lager or IPA, discriminating cannabis consumers now search for that gem of a single-origin, specialty-strain vaporizer oil or irresistible dab extract.

“I see an exciting new day for quality-focused, craft extraction that tells a story, not only of where the cannabis plant might have been grown and how, but also the care that was taken in the processing of that strain into smokable or edible oil,” says John Lynch, Founder of TradeCraft. “Imagine the impact in the marketplace when product-makers figure out how to do seasonal one-offs where engaged connoisseurs are willing to pay a premium for the art behind limited releases.”

In the same way hops determine recipes for beer flavors, the cannabis plant determines extraction recipes

In either process, you’re essentially creating art with science. Each process works with different strains. Each is concerned with chemical and flavor profiles. Each has its own challenges. In both worlds, quality depends upon consistency. You’re creating art, but you need to replicate that art over and over – which can only occur with strict control of the process. Brewmasters seek control of things like yeast quantity and health, oxygen input, wort nutritional status and temperature, among other things. In their pursuit, extraction technicians seek to control temperature, pressure and flow rate–as well as all the ways these variables interact with each other. What enables this control in both efforts is the equipment used to achieve results.

“A modern brewhouse is very much like a scientific laboratory,” Ligare says. “Brewers treat their setup with the same care and attention a scientist gives to their lab equipment, and are equally concerned with precision, cleanliness and the purity of the result. With each new beer, they want to develop a process that can be controlled and replicated.”

The key to creating a precise process is to use instrument-grade extraction machinery that performs to specifications – and allows you to repeat the process again and again. The value of using high-quality instrumentation to manage and monitor either the brewing or extraction process cannot be overstated. Although it seems counterintuitive, this is where the “craft” comes into play for both brewing and cannabis extraction. Precise instrumentation is what allows the brewer or extraction “artist” to manipulate and monitor the conditions required to meet recipe standards. Along with the quality of the ingredients (hops, cannabis, hemp, etc.), the quality of the equipment utilized to create the product is one critical element impacting the end result. “Imagine the impact in the marketplace when product-makers figure out how to do seasonal one-offs where engaged connoisseurs are willing to pay a premium for the art behind limited releases.”

In cannabis extraction, a second crucial decision is determining which solvent is the best solution for the recipe you’re using and the end result you’re hoping to achieve. This decision is a part of the “craft” of extraction, and determined according to a combination of criteria. There’s no question that each solvent has a business case it serves best, and there is ongoing debate about which approach is best. But overwhelmingly, the solvent that best serves the most business needs is CO2 due to its inherent versatility and ability to have its density tuned to target specific compounds.

“Control is what makes or breaks any craft product,” says Karen Devereux, Vice President of Northeast Kingdom Hemp. “We’re based in Vermont and love how Vermont is known for its quality craft beer, cheese and maple syrup. We wanted to bring that craft approach to hemp extraction, and everyone knows that any craft endeavor is focused on the details and getting them right again and again. You can’t do that without controlling every aspect of the process.”

Greater control of the process can also open up worlds of discovery. The inherent “tunability” of CO₂ enables the extraction technician to target specific compounds, enhancing the potential for experimentation and even whimsy. This can lead to entirely new products much in the way a brewer can control his process to create new, interesting beers.

American portrait photographer Richard Avedon famously declared that art is “about control,” describing the artistic process as “the encounter between control and the uncontrollable.” The same can be said for beer making and cannabis extraction. The more precisely you can control variables, the more options you’ll have for yourself and your customers. The more choices you’ll have with regard to different recipes and products. And the more loyalty you’ll ultimately generate among fans of your products.

Advancements in Extraction & the Growth of the Concentrate Category

By Dr. Dominick Monaco
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Due to quick progressions in legalization, today’s cannabis industry bears little resemblance to the industry of five years ago. As the cannabis space gains mainstream acceptance, it resembles more “traditional” industries closely. In turn, how we consume cannabis has changed dramatically within this novel legal framework.

A brief visit to a cannabis dispensary quickly illuminates just how much the industry has changed in the past few years.

Within the dynamic of modern cannabis, perhaps no vertical has seen the same advancements as cannabis extracts. It’s precisely the growth of the concentrate category that has given rise to the many branded products that define the legal market.

To give a clear picture of how advancements in extraction have stimulated the concentrate category’s growth, we put together this brief exploration.

Standards & Technology

extraction equipmentBefore legalization, the production of cannabis extracts was a shady affair done in clandestine and often dangerous ways. Especially concerning BHO (Butane Hash Oil), home-based laboratories have long since been notorious fire hazards. Even more, with a total lack of regulation, black-market extracts are infamous for containing harmful impurities.

In the few short years that cannabis has been legal in Nevada, Washington and other states, extract producers have adopted standards and technology from more professional arenas. By borrowing from the food and pharmaceutical industries, concentrate companies have achieved excellence undreamed of a decade ago.

Good Manufacturing Practices

One of the essential elements in the extracts vertical advancements is the adoption of good manufacturing practices. According to the World Health Organization website, “Good Manufacturing Practice (GMP) is that part of quality assurance which ensures that products are consistently produced and controlled to the quality standards appropriate to their intended use.”

When adult-use cannabis was legalized in markets such as Colorado, cannabis companies were able to come out of the shadows and discuss GMPs with legit businesses. In doing so, they implemented professional controls on extract manufacturing in accordance with “quality standards” of state regulatory agencies.

Supercritical CO2 Extraction

As cannabis businesses adopted GMP from other industries, extract producers also embraced more sophisticated technology. Of these, supercritical CO2 has pushed the cannabis concentrates vertical into the future.

IVXX processingAccording to the equipment manufacturer Apeks Supercritical, “CO2 is considered to be a safer method of extraction because the solvent is non-volatile. The extract is purer because no trace of the solvent is left behind. It is also versatile and helps protect sensitive terpenes, by allowing cold separation.” By deriving methods from food production, supercritical equipment manufacturers have given cannabis companies a viable option for the commercial production of extracts.

Supercritical technology has helped push the concentrates vertical forward by providing a clean and efficient way to produce cannabis extracts. Nonetheless, supercritical CO2 equipment is highly sophisticated and carries a hefty price tag. Producers can expect to pay well over $100,000 for commercial supercritical CO2 extraction setup.

Products

Just as standards and technology have evolved in the cannabis extracts vertical, we have also seen products rapidly mature. Notably, the legal environment has allowed manufacturers to exchange ideas and methods for the first time. In turn, this dialogue has led to the development of new products, like isolates and live resin.

Isolates

Just as the name implies, isolates are concentrates made from a singular, pure cannabinoid. In today’s market, CBD isolates have grown increasingly popular because people can consume pure CBD without ingesting other cannabinoids or plant materials, including the legal 0.3% THC found in hemp.

Isolates are made by further purifying cannabis extracts in the process of purification, filtration and crystallization. As seen with other concentrates, isolates are used as the base for many cannabis products, such as gummies.

There is also growing interest in CBG isolate, which is another non-psychoactive cannabinoid when consumed orally.

Live Resin

The cannabis concentrate live resin has taken the industry by storm over the past few years. Live resin is a form of extract that is originally sourced from freshly harvested and frozen cannabis plants. The primary selling point behind this extract is the fact that fresh flowers produce much more vibrant aromas and flavors than dried cannabis. Interestingly, this pungency is tied to the preservation of terpenes in live resin.

Just a few of the dozens of various products types on the market today.

To make live resin, producers “flash freeze” fresh cannabis plants immediately after harvest. Valuable cannabinoids and terpenes are then extracted from the fresh, frozen plant material using hydrocarbon solvents. This whole process is done at extremely cold temperatures, ensuring no thermal degradation to the precious and volatile terpenes.

In lieu of these intricate steps to preserve the flower and extracts, live resin has continuously gained popularity. Namely because vaping with live resin is the best way to sample fresh cannabis terpene profiles in its most authentic fashion

It is amazing to see how much cannabis extracts have grown and progressed with legalization. Due to such amazing advancements in standards, technology, and products, the concentrates category has exploded on the dispensary scene. In today’s market, flowers have been largely sidelined in favor of concentrate-based products like gummies. These products now adorn dispensary shelves in beautiful packaging replete with purity and testing specifications.

It’s an often-overlooked fact that the purity standards of the legal extracts have made reliable cannabis brands possible in the first place. You cannot develop a cannabis brand without consistent products that customers can rely on; all things considered, it can be said that advancements in extraction have not only stimulated the concentrate category but the entire industry as we know it today.

Cannabis Extracts for the Informed Consumer: Solvent or Solventless

By Nick J. Bucci
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Editor’s Note: Nick Bucci is a freelance cannabis writer. You can view his work here 


As cannabis markets continue to gain traction, inconsistent and largely unpredictable markets have left recreational consumers in an informational fog. Try as the industry may, or may not to inform consumers, the lack of knowledge was evident when an established Colorado hash company opened a second operation in California. Expecting high demand for their solventless concentrates, the demand for their solvent-based counterparts came as a surprise. Initially hoping to eliminate solvent extracts from their product line-up, the company was forced to devote about half their overall production to solvent extracts, until information spreads and attitudes start to change. Over the past year several companies have joined the solventless side of history, but consumer understanding remains largely stagnant. For those immediately overwhelmed by terminology, cannabis extracts, concentrates or hash are all interchangeable terms describing concentrated cannabis. Under these umbrella terms, two distinct categories emerge depending upon whether chemical solvents were or were not used to extract the hash. Hence: solvent or solventless. A brief overview of cannabis concentrates will help consumers to understand the evolution away from solvent extractions and toward a superior solventless future.

ecxtractionfig2
Science and economics merge when considering all the possible uses of concentrated compounds to final product formulations

Before regulated cannabis markets, cannabis extracts had long been in use. These old-world methods of cannabis extraction use very basic solventless techniques to create more potent, concentrated forms of cannabis. Dry sifting is easily the oldest form of cannabis extraction and a prime example of one solventless technique. Something as simple as shaking dried cannabis over metal screens and collecting the residue underneath creates a solventless product called keif. Dark brown bubble-hash, made popular decades ago, is another ancient technique using only ice and water to perform extractions without chemical solvents. After decades of stagnant and limited old-world methods, changes in legislation allowed cannabis sciences to flourish. These old-world hash methods were quickly forgotten, replaced by the astonishing progress of modern solvent extractions.

Tetrahydrocannabinol (THC), just one of hundreds of cannabinoids found in cannabis.

The emergence of solvent extracts revolutionized cannabis around 2011, creating new categories of cannabis products that exploded onto the scene. Not only did solvent extracts produce the most potent and cleanest forms of hash ever seen at this point, it also created new possibilities for hash-oil vape cartridges and cannabis extract infused edibles. These solvent extracts use butane, propane, or other hydrocarbon solvents to extract, or “blast” cannabinoids from the plant. By running solvents through cannabis and then purging or removing leftover, residual solvents, a super-potent, premium hash product is achieved. Regulated markets require testing to ensure only a safe level, if any, of the solvent used in the extraction process remains in the final product. This technology ushered in the first wave of concentrates to medical and recreational markets under the descriptive titles of wax, shatter and crumble. While these effective and affordable products can still be found today, far superior products have largely replaced wax and shatter. Distillation techniques can further purify and isolate THC-a, while removing harmful residual solvents. For a time, Solvent-free was used to describe this ultra-purified distillate, but the needless term has fallen out of use. Solvent-free is still a solvent extraction using chemical solvents, don’t be fooled. Distillation and CO2 extractions have fallen into general disfavor as they destroy the flavorful terpenes and valuable cannabinoids, that when present create an “entourage effect.” This “entourage effect” happens when the medicinal and recreational properties are most effective, pronounced, and impactful due to a full range of terpenes and cannabinoids being present in the final product. With companies manually reintroducing terpenes to their final extracts, it’s an attempt to restore what was lost during solvent extraction processes. Many brands claim to use cannabis derived or food-grade terpenes to infuse or reintroduce terpenes into their purified hash oils. While this adds flavor and taste, especially to distillate cartridges, it’s far from an ideal solution. Armed with this new information, the informed consumer looks for a full profile of terpenes and cannabinoids in their hash.

THC-A crumble, terpene-rich vape oil, THC sap (from left to right).

With terpene preservation a new priority, all aspects of hash making were reevaluated. By using fresh-frozen cannabis flower, solvent extractions quickly reached new heights. Using the same techniques as prior solvent extractions, the cannabis plant is frozen immediately upon harvesting, rather than trimming and drying the crop as usual. Freezing the plant preserves valuable terpenes helping to create a new category for hydrocarbon extracts under the general label of live resins. This live resin, containing vastly greater profiles of terpenes and cannabinoids than earlier waxes, shatters or crumbles is sold as live-resin sauce, sugar, badder, frosting, diamonds and more. Many versions of live resin re-use previous terms that describe consistencies. These live resin solvent extracts outperform the wax, crumble and shatters of old, and are priced accordingly. Some of the best solvent extracts available today use butane to extract hash oil, which forms THC-a crystals and diamonds seen in live resin sauces. Having learned the value of terpenes and cannabinoids, early efforts to purify THC were clearly misled. The industry defining use of fresh-frozen cannabis flowers greatly improved the quality of all extracts having realized the psychoactive effects are largely dependent on the various profiles of cannabinoids and terpenes. Pure THC-a crystals and isolates are easily achieved with solvent extractions but, produce inferior effects both medicinally and recreationally. Discovering the “entourage effect” as described earlier, these elements of cannabis allowed old-world solventless techniques to be re-inspired and reinvigorated with the benefit of healthy genetics and a hearty understanding of past mistakes.

Having gone full circle, solventless techniques are again at the forefront of the cannabis industry, having attained near perfection for our current understanding of cannabis anatomy.

figure1 extract
The increasingly finer mesh works to separate and extract microscopic trichomes

Using the lessons and tendencies of prior extractions, the solventless method, in all its final forms, begin with the same initial process to make ice-water hash oil. Often referred to as solventless hash oil (SHO), fresh-frozen flowers are submerged in ice and water, soaked and agitated before the water is filtered through mesh screens. As these mesh screens are measured by microns, the increasingly finer mesh works to separate and extract microscopic trichomes that break free from the cannabis plant. The 120- and 90-micron mesh screens usually collect pristine trichome heads. After scraping the remaining material from the screens, its sieved onto trays where the hash can dry using modern techniques of sublimation. The results are beyond phenomenal and are sure to shock even life-long cannabis consumers. This technique isolates only the most potent and psychoactive parts of the plant, to produce white to clear solventless ice water hash. When done with precision 6-star ice water hash is formed. The hash can be sold and consumed as is or undergo additional solventless techniques to produce hash-rosin. Not to be confused with live-resins, rosin uses pressure and slight heat to squeeze ice-water hash, into hash-rosin. Some companies have elected to whip their rosins into a solventless badder or allow their hash rosins to undergo a cold cure process that creates textures and varieties like hash rosin sauce. Regardless of the final solventless product, they all begin as ice water extractions. These simple, natural methods of extraction are quickly being adopted by companies known for live resin. As solventless extracts are safer, cleaner and superior in quality to solvent chemical extractions, the race is on as the industry shifts toward a solventless future.

While I’d be happy to never see another solvent extract again, without the miraculous breakthroughs and advances in all aspects of cannabis manufacturing and production we may have not yet arrived where we are today. When using solvents to extract, the trichomes, which contain the full spectrum of terpenes and cannabinoids, are dissolved by the solvent, which is then evaporated off, leaving behind dissolved trichomes. In solventless hash, these trichomes remain whole and are never dissolved or broken down. Instead they are broken free by agitation in ice and water, separating the trichome heads from their less-active stems. These valuable trichomes heads contain everything pertinent and are never destroyed, dissolved or melted like solvent-extractions are forced to do. The benefit of keeping the heads of these trichomes whole results in a far superior product expressing the full profile of terpenes and cannabinoids the way mother nature intended. This natural profile of trichomes lends itself directly to the entourage effect that solvent extracts were found to be missing.

Extraction techniques are not equal and depend upon whether quality or mass production is the aim. Solvent extracts have quickly begun to represent the old-guard of mass-produced cannabis concentrates, with the solventless new-guard focusing on quality, small batch, hash-rosin excellence.

Quality Assurance In The Field: Instruments For Growers & Processors

By Aaron G. Biros
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As the cannabis marketplace evolves, so does the technology. Cultivators are scaling up their production and commercial-scale operations are focusing more on quality. That greater attention to detail is leading growers, extractors and infused product manufacturers to use analytical chemistry as a quality control tool.

Previously, using analytical instrumentation, like mass spectrometry (MS) or gas chromatography (GC), required experience in the laboratory or with chromatography, a degree in chemistry or a deep understanding of analytical chemistry. This leaves the testing component to those that are competent enough and scientifically capable to use these complex instruments, like laboratory personnel, and that is still the case. As recent as less than two years ago, we began seeing instrument manufacturers making marketing claims that their instrument requires no experience in chromatography.

Instrument manufacturers are now competing in a new market: the instrument designed for quality assurance in the field. These instruments are more compact, lighter and easier to use than their counterparts in the lab. While they are no replacement for an accredited laboratory, manufacturers promise these instruments can give growers an accurate estimate for cannabinoid percentages. Let’s take a look at a few of these instruments designed and marketed for quality assurance in the field, specifically for cannabis producers.

Ellutia GC 200 Series

Shamanics, a cannabis extractor in Amsterdam, uses Ellutia’s 200 series for QA testing

Ellutia is an instrument manufacturer from the UK. They design and produce a range of gas chromatographs, GC accessories, software and consumables, most of which are designed for use in a laboratory. Andrew James, marketing director at Ellutia, says their instrument targeting this segment was originally designed for educational purposes. “The GC is compact in size and lightweight in stature with a full range of detectors,” says James. “This means not only is it portable and easy to access but also easy to use, which is why it was initially intended for the education market.”

Andrew James, marketing director at Ellutia

That original design for use in teaching, James says, is why cannabis producers might find it so user-friendly. “It offers equivalent performance to other GC’s meaning we can easily replace other GC’s performing the same analysis, but our customers can benefit from the lower space requirement, reduced energy bills, service costs and initial capital outlay,” says James. “This ensures the lowest possible cost of ownership, decreasing the cost per analysis and increasing profits on every sample analyzed.”

Shamanics, a cannabis oil extraction company based in Amsterdam, uses Ellutia’s 200 series for quality assurance in their products. According to Bart Roelfsema, co-founder of Shamanics, they have experienced a range of improvements in monitoring quality since they started using the 200 series. “It is very liberating to actually see what you are doing,” says Roelfsema. “If you are a grower, a manufacturer or a seller, it is always reassuring to see what you have and prove or improve on your quality.” Although testing isn’t commonplace in the Netherlands quite yet, the consumer demand is rising for tested products. “We also conduct terpene analysis and cannabinoid acid analysis,” says Roelfsema. “This is a very important aspect of the GC as now it is possible to methylate the sample and test for acids; and the 200 Series is very accurate, which is a huge benefit.” Roelfsema says being able to judge quality product and then relay that information to retail is helping them grow their business and stay ahead of the curve.

908 Devices G908 GC-HPMS

908 Devices, headquartered in Boston, is making a big splash in this new market with their modular G908 GC-HPMS. The company says they are “democratizing chemical analysis by way of mass spectrometry,” with their G908 device. That is a bold claim, but rather appropriate, given that MS used to be reserved strictly for the lab environment. According to Graham Shelver, Ph.D., commercial leader for Applied Markets at 908 Devices Inc., their company is making GC-HPMS readily available to users wanting to test cannabis products, who do not need to be trained analytical chemists.

The G908 device.

Shelver says they have made the hardware modular, letting the user service the device themselves. This, accompanied by simplified software, means you don’t need a Ph.D. to use it. “The “analyzer in a box” design philosophy behind the G908 GC-HPMS and the accompanying JetStream software has been to make using the entire system as straightforward as possible so that routine tasks such as mass axis calibration are reduced to simple single actions and sample injection to results reporting becomes a single button software operation,” says Shelver.

He also says while it is designed for use in the field, laboratories also use it to meet higher-than-usual demand. Both RM3 Labs in Colorado, and ProVerde in Massachusetts, use G908. “RM3’s main goal with the G908 is increased throughput and ProVerde has found it useful in adding an orthogonal and very rapid technique (GC-HPMS) to their suite of cannabis testing instruments,” says Shelver.

Orange Photonics LightLab Cannabis Analyzer

Orange Photonics’ LightLab Cannabis Analyzer

Dylan Wilks, a third generation spectroscopist, launched Orange Photonics with his team to produce analytical tools that are easy to use and can make data accessible where it has been historically absent, such as onsite testing within the cannabis space. According to Stephanie McArdle, president of Orange Photonics, the LightLab Cannabis Analyzer is based on the same principles as HPLC technology, combining liquid chromatography with spectroscopy. Unlike an HPLC however, LightLab is rugged, portable and they claim you do not need to be a chemist to use it.

“LightLab was developed to deliver accurate repeatable results for six primary cannabinoids, D9THC, THC-A, CBD, CBD-A, CBG-A and CBN,” says McArdle. “The sample prep is straightforward: Prepare a homogenous, representative sample, place a measured portion in the provided vial, introduce extraction solvent, input the sample into LightLab and eight minutes later you will have your potency information.” She says their goal is to ensure producers can get lab-grade results.

The hard plastic case is a unique feature of this instrument

McArdle also says the device is designed to test a wide range of samples, allowing growers, processors and infused product manufacturers to use it for quality assurance. “Extracts manufacturers use LightLab to limit loss- they accurately value trim purchases on the spot, they test throughout their extraction process including tests on spent material (raffinate) and of course the final product,” says McArdle. “Edibles manufacturers test the potency of their raw ingredients and check batch dosing. Cultivators use LightLab for strain selection, maturation monitoring, harvesting at peak and tinkering.”

Orange Photonics’ instrument also connects to devices via Wi-Fi and Bluetooth. McArdle says cannabis companies throughout the supply chain use it. “We aren’t trying to replace lab testing, but anyone making a cannabis product is shooting in the dark if they don’t have access to real time data about potency,” says McArdle.