Episode 9

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Published on:

16th Feb 2021

S1 E09 - Crystallization Of CBD Isolate

Luke Van Trieste of BR Instruments joins us to discuss CBD isolate crystallization. We get deep into the equipment, solvents, and SOPs used to crash out those crystals. We cover static and dynamic crystallization, as well as the continuous flow processes that are beginning to come online. In addition to the BR Instrument crystallization reactors, we discuss their patented spinning band distillation equipment.

EPISODE TRANSCRIPT:

Jason Showard - 00:00:10 

Hello and welcome to Episode nine of The Modern Extractor. This podcast focuses on the processes, equipment and science found in a cannabis extraction laboratory. I'm your host Jason Showard, and I work professionally in the cannabis extraction field. Here in season one, we're focusing on ethanol extraction and post processing, with each episode digging into a particular stage in that process. The shows are released in an order that follows the workflow through a lab as material makes its way from cultivar to concentrate. 

 

Jason Showard - 00:00:39 

Last week we had Jay Horton on the show. He's the founder of Genovations and the man that got me started distilling cannabis. We talked specific SOPs for wiped film and rolled film distillation. We went through how to push your machine to the absolute limit and get the maximum throughput out of a wiper. He hit us with a ton of distillation knowledge gained from his years of experience in the trenches cranking out liters, as well as his experience installing and training on Chemtech equipment. 

 

Jason Showard - 00:01:05 

Moving on to this week's show, let's catch back up with a work in progress. So far, we've performed a cold ethanol extraction in a centrifuge. We've cold filtered the resulting miscella through a lenticular filter. We ran the filtered miscella through a falling film evaporator to separate the oil and the ethanol. We decarboxylated the crude oil to convert the cannabinoids. We terp stripped, then we distilled the oil, creating some beautiful golden distillate. As I said last week, distillate is the end of the line for THC. 

 

Jason Showard - 00:01:34 

But today we'll take CBD distillate a step further in the purification process and crystallize it into 99.9% pure CBD isolate. Joining me on the show today is a man who has processed many a kilo of isolate. He's very well versed in the equipment, solvents and processes of CBD crystallization. He's usually found flying around the world installing and training on BR instrument crystallization reactors, as well as their patented spinning band distillation equipment. He certainly knows his way around a cannabis extraction laboratory. 

 

Jason Showard - 00:02:06 

Luke Van Trieste, welcome to The Modern Extractor. 

 

Luke Van Trieste - 00:02:09 

Hi, thanks for having me. 

 

Jason Showard - 00:02:10 

Absolutely. Where are you calling in from today? 

 

Luke Van Trieste - 00:02:13 

I live just outside Baltimore, Maryland. 

 

Jason Showard - 00:02:15 

Right on. You were telling me earlier it's a snowy day out there. It's a rainy day here in Los Angeles. 

 

Luke Van Trieste - 00:02:21 

Yeah, plenty of bad weather lately this winter. 

 

Jason Showard - 00:02:25 

So talk to me a little bit about your path to joining BR instruments. 

 

Luke Van Trieste - 00:02:31 

So this is actually my 10th year at BR Instrument. I basically started off in high school doing graphic design content and creating marketing materials. I worked there through most of high school and college, until I got my degree in chemistry. And then I transitioned into my role, into doing installations and trainings. So if you buy a piece of our equipment, there's a very good chance that I'll be the person that's actually there, you know, running you through the show. So, yeah, 10 years. It's exciting. 

 

Jason Showard - 00:03:08 

So give us a bird's eye view of BR instrument as a company. How'd its start? Where is it now? 

 

Luke Van Trieste - 00:03:14 

So we produce mostly spinning band distillation equipment, which is really useful for high purity applications or for difficult separations. So we see a lot of work in the petroleum, the pharmaceutical, environmental, analytical industries. And obviously, you know, cannabis and hemp has become a very big part of our company as well. So we really just, any kind of distillation is pretty much our wheelhouse. 

 

Jason Showard - 00:03:40 

All right. So are you guys primarily working right now in the cannabis and hemp industry or are you spread out amongst all of that currently? 

 

Luke Van Trieste - 00:03:50 

We're spread out amongst all of that currently. So we do a lot of international business as well, which probably represents about half of the total business for us. And at this point in time, at least, there's not a ton of cannabis and hemp, although it's starting to pick up around the world. But that may be another couple of years while other countries figure out, you know, imports and exports and stuff like that. 

 

Luke Van Trieste - 00:04:16 

So I'd say cannabis is about, domestic cannabis, is about half of it. And the international, that basically encompasses all the other things I mentioned. It's probably about the other half of it right now. 

 

Jason Showard - 00:04:28 

OK, I've been intrigued by your spinning band distillation for a while now. Last week on the show, we covered, actually the last couple of weeks on the show, we covered distillation of cannabinoids with a rolled film distillation unit. While this show is technically about CBD isolate and crystallization, I think while I've got you on the line here, it makes sense to go over spinning band a little bit. So tell me a little bit about spinning band. How does it work? 

 

Luke Van Trieste - 00:05:01 

So if you're familiar with the colloquial, short path distillation. So by that I mean a small flask with a short little column, and basically a very simple distillation model. And not in reference to a wiped film or a rolled film distillation with appropriate pressure. So like Lab Society or Summit or one of many other companies produce those short paths. It functions more similarly to that than a wiped film. 

 

Jason Showard - 00:05:33 

Yeah, I've on the show here previously. I've referred to those as a tabletop short path. While the rolled or the wiped film still technically a short path, I believe you're referring to the tabletop short path, correct? 

 

Luke Van Trieste - 00:05:45 

Correct. So basically we are a batch process where you're going to at the beginning of the run, fill up your flask with your starting material and then you're going to heat it up. And then by using different boiling points of the different compounds in there, we're going to slowly separate them out. And basically how we do that is, the way to separate a vapor from a liquid is to have them interact more. Strangely enough. And that's going to enrich both of those phases in their majority component. 

 

Luke Van Trieste - 00:06:19 

And so a spinning band. What we're doing is by highly agitating the column area, as vapors come off of the boiling flask that we've been heating, we're greatly agitating these vapors and making them slam into the liquid and along the wall of the column, and basically forcing tons of interactions with a very high refresh rate. 

 

Luke Van Trieste - 00:06:42 

And that gives you the highest purity out of fractional distillation. And so a comparable method would be, for like a tabletop short path, if you put in a packing substrate. And that basically gives you a surface area for the vapor liquid interaction. So a spinning band, it's a dynamic interaction where that surface is always being changed, it's constantly being refreshed. And there's definitely some other advantages too. Such as a spinning band is going to have generally a higher throughput for the purity that you get. Because as the cycle of boiling and condensing happens, the helix of the spinning bands pumps the rejected liquid that has been condensed back into the boiling flask to start the cycle over again. 

 

Luke Van Trieste - 00:07:32 

But vapors are basically able to travel relatively freely up the column because there's a large open space. It's just moving. So there's a couple of advantages. But purity is definitely the name of our game. 

 

Jason Showard - 00:07:48 

Yeah, I've basically from talking to you guys at the trade shows and reading on the Internet, the amount of theoretical plates that can be created with these is pretty impressive, but something that you really don't run into with a wiped or a rolled film unit. That would definitely be the upside. Now, I've heard some people in the industry say that a downside to a system like this or to your traditional short path is going to be something like residence time. What do you say to that? 

 

00:08:18  

I say that cannabinoids aren't as fragile as people like to make them out to be. I think that, you know, frequently people take maybe a little bit too much care. I think a lot of it has to do with the type of product that you're trying to make. I'd say that the maximum temperature is almost more important than your residence time. And basically the thought process behind that is a general rule of thumb for chemistry, is that by every 10 degrees Celsius you raise the temperature, you cause a reaction to happen twice as fast. 

 

Luke Van Trieste - 00:08:55 

So taking twice as long is effectively the same thing as doing something 10 degrees hotter, from a chemical reactions perspective. So I think, you know, if you're really concerned about residence time, I think maybe you should look at the maximum temperatures that you're incurring first instead. And as long as you're below 200, 190 Celsius, you're really not going to see a ton of stuff. 

 

Luke Van Trieste - 00:09:22 

The funky things start to happen at about 210 to 220 degrees Celsius, in my experience. That's where you'll start to see more and more rapid degradation. 

 

Jason Showard - 00:09:32 

OK, so with your style machine, also, the way that it functions, you're going to end up with the lighter stuff, which is typically more fragile, coming off first and getting out of there before the temperature rises anyway for the most part, right? 

 

Luke Van Trieste - 00:09:50 

Yeah, absolutely. We do a decent amount of terpene processing, too, as well. Which involves using virtually no heat and just vacuum. And so instead of heating something, we can just reduce the pressure which will cause us to distil over. And with terpenes, they tend to be quite low yielding, but for that very reason, you want to be very careful with them and very gentle with them. And those can be removed first in kind of a separate process, but still on the spinning band. 

 

Jason Showard - 00:10:18 

All right. Well, I'm glad we got a chance to kind of jump into that. I've wanted to talk to you guys about spinning band and had thought about reaching out regarding that. And then, you know, when it came up to reach out to you regarding crystallization, I figured it was a great opportunity to do that. So the reason that I reached out to you specifically about CBD crystallization is because of a blog post that you wrote back in early 2019 on the BR Instrument blog about creating CBD isolate. 

 

Jason Showard - 00:10:47 

It was full of equipment, knowledge and SOPs and just basically a really nice, informative package. In addition to the post afterwards, people started commenting and you were jumping right in there and responding to everybody's questions in the comments. I think that's great and really aligns with my approach here at The Modern Extractor, which is to kind of curate and release the best information possible to the audience. So because of that, I was excited to talk to you and I'd like to move on to the actual science behind the final stage in the process we've been covering this season, which is crystallization. 

 

Jason Showard - 00:11:20 

So let's talk a little bit about what we're trying to produce here. CBD isolate is purified, crystalized CBD. Let's break that down. So what is a crystal? 

 

Luke Van Trieste - 00:11:31 

So a basic overview of what a crystal is, is that it's going to be a solid that has its molecules in an organized long-range structure. And so I think it's important to talk about things that are not a crystal, so a very common example is a glass. Glass is clear, it's pretty. You can cut it into a crystal, but that doesn't make it structurally on the molecular level, a crystal. 

 

Luke Van Trieste - 00:11:58 

Another example is going to be like some kind of plastic or wax where, you know, these are very big molecules that kind of interact with each other in a much different way than a nice crystal lattice. I think it's also important to point out that a lot of natural substances are polycrystalline. And basically that's going to mean that you took a bunch of individual crystal structures, grew them together, and then they fused. So this is going to cover, you know, metals, some rocks or a ceramic, for example. 

 

Jason Showard - 00:12:30 

OK, so with those things that you were just talking about, for example, the metals, the rocks, the ceramic, that is, they were crystalline in nature prior to having a bunch of these crystalline structures formed together and then fused due to heat or some other environmental conditions? Pressure? 

 

Luke Van Trieste - 00:12:50 

Yes, you can almost think about the way they fused together as a joint. And so frequently that's where a weak spot in the crystal may form, is at the interface of two of these different sub crystals. And so you can call gold crystalline in some context, but you're not going to have a gold crystal, if that makes sense. It's going to be quite small, realistically. 

 

Jason Showard - 00:13:14 

OK, so solubility is an important concept when it comes to crystallization. Talk to us a little bit about the relationship between solubility and crystallization. 

 

Luke Van Trieste - 00:13:28 

So solubility is going to be in this case, how much CBD can we jam into a given solvent at a given temperature? And there's ways to change that. An important way is temperature. So as you increase the temperature of anything, it's going to become more soluble. And if you decrease the temperature, it's going to become less soluble. 

 

Luke Van Trieste - 00:13:54 

So we want to, our goal is to basically create a solution that has a lot of CBD in it and that's going to be called "saturated." So a saturated solution is when we get to the point where if you add more CBD, it doesn't dissolve anymore, it just kind of sinks to the bottom of the container. Then you can also have a supersaturated solution. 

 

Luke Van Trieste - 00:14:15 

So this is going to be a solution that has more CBD than it should technically be allowed to at that temperature. And how we create that is you elevate the temperature to dissolve a lot of CBD, but then through some controlled method, you reduce the temperature without crystalizing any of the CBD out of solution. Suddenly you have CBD that's just maybe a little bit thermodynamically unhappy to be there at this point, but it's not quite ready to crash out. 

 

Jason Showard - 00:14:44 

OK, well, before we get further down the road into the SOPs of crystallization and specific stuff about equipment, let's talk about solvents for a moment here. While you're talking about solvents, there's a variety of them that can be used for crystallization. Are you making solvent decisions based on solubility or is that more of a boiling point or regulation or a safety decision? 

 

Luke Van Trieste - 00:15:09 

So primarily the issue is solubility, because if it doesn't crash out at some point or you can't dissolve any of it, then that's just kind of a non-starter. So our solvent of choice really needs to have a couple characteristics regarding solubility. So the first one is that CBD needs to dissolve into our solvent well, at an elevated temperature like I mentioned. However, at decreased temperatures, when we start to cool our solution, CBD needs to become relatively insoluble. If it stays too soluble at a low temperature, then we're not going to get crystal formation. 

 

Luke Van Trieste - 00:15:49 

The final solubility consideration is what is our waste product consisting of? So if we have THC that needs to be removed from these CBD crystals so you can sell them internationally, then you need to make sure that your solvent of choice also carries THC quite well at low temperatures, not just high temperatures. Otherwise you're just going to end up with kind of a goo coating your crystals as it will crash out, but not really crystallize either. 

 

Jason Showard - 00:16:20 

Some CBD sauce. 

 

Luke Van Trieste - 00:16:22 

Yeah. So that's how you make your decision based on solubility, but in the real world, it's easier or harder to work with certain solvents. So I think it's important to cover the health and safety concerns of some of these solvents. 

 

Jason Showard - 00:16:39 

Definitely. 

 

Luke Van Trieste - 00:16:40 

For CBD crystallization, the primary group is going to be hydrocarbons. And so we're going to go from either pentane to hexane or to heptane. And so these are very similar to, you know, butane chemically, but they exist as liquids closer to room temperature. 

 

Luke Van Trieste - 00:17:00 

And these have a very good solubility at high temperatures and the correct solubility at the low temperatures for CBD as well, so it prevents a lot of waste. If you have a bad solvent of choice, then you're going to lose a lot of yield. So with these hydrocarbons, it's really important to discuss safety because none of these are great for you, the environment or your fire marshal. 

 

Luke Van Trieste - 00:17:30 

They can really present some serious hazards. So we'll go through them one by one, and basically, if you're down to the hydrocarbons at this point, then here's how you choose between the three. Pentane is going to be your lowest boiling one. That also makes it simultaneously the most dangerous in terms of explosions or flammability. So you're probably going to be looking at C1D1, C1D2 enclosures or regulations. Just for reference, the boiling point is 36 degrees Celsius or about 97 degrees Fahrenheit. 

 

Luke Van Trieste - 00:18:02 

So you could essentially boil it by holding it in your hands. That's kind of how volatile it can be. Then we move on to hexane, which is medium boiling, it's arguably the worst for your health. And so I think a lot of people tend to stray away from it a little bit because you need to be very careful about residual levels. You know, you need to be low on the PPMs if you're going to use hexane at all. 

 

Luke Van Trieste - 00:18:27 

Finally, that takes us to heptane which is the highest boiling. So that makes it relatively safe, but it also becomes much more difficult to purge from your final isolate product. So with a boiling point of about 100 degrees Celsius, you need to get water really, really boiling. 

 

Luke Van Trieste - 00:18:47 

So it's not just going to leave your crystals at room temperature without any kind of prompting. And as always, you need to just be very careful with all sources of ignition, so whether that means that you need to use some specialized tools, either wear some special jumpsuit to prevent static discharge, or you need to leave your phone in the other room. This is definitely up to your local jurisdictions, but you don't want to take any chances. You don't get a second chance to make that mistake. 

 

Jason Showard - 00:19:18 

Yeah. Yeah. So far this season, we've really only been dealing with ethanol, which is flammable in its own right, but not explosive, which some of these are. So definitely need to take the proper precautions when it comes to working with this stuff. So moving on from there, let's talk about the machines or vessels that you guys sell over there at BR, and how we can integrate them into our workflow for making these crystals. What is it that BR Instruments machines do to optimize the crystal growth and how do they work? 

 

Luke Van Trieste - 00:19:51 

So they're basically just a pretty simple jacketed vessel. And so through the jacket, you can pump your heating and cooling fluids. One of the key features is definitely agitation as opposed to kind of a static crystallization. So the agitation is very important because it's going to make your process much more rapid. And that's for a couple of reasons. The first reason being that agitation causes nucleation. 

 

Luke Van Trieste - 00:20:21 

And so nucleation is the start of crystal growth without the very first seed, so to speak, the rest of the crystals is not going to grow. And so basically by stirring, you create turbulence in the fluid and maybe cause some air bubbles to form or something. And basically at the change of those two phases where, you know, let's say an air bubble pops into your liquid, that's going to be an interface for nucleation. So it's going to promote crystal growth rapidly throughout your entire solution. 

 

Luke Van Trieste - 00:20:54 

If you were not to agitate it, then you'd probably see crystal growth start along the walls of your vessel and slowly work its way in and the center will remain kind of liquid. The other benefit of agitation is that when you have a static system like that, you are waiting for one CBD molecule to finally find the crystal and settle down. With agitation, you basically are giving it a little kick in the rear. You're trying to say, "Hey, everything is touching everything. There's constant contact between all our different phases." 

 

Luke Van Trieste - 00:21:26 

And so you just end up with a much more rapid crystallization process, regardless of the nucleation. You just basically help one CBD molecule find another CBD molecule all the way across the vessel or wherever it may be. 

 

Jason Showard - 00:21:39 

Gotcha. Yeah. So some of these original machines, or vessels rather that I was seeing for CBD crystallization were just very basic reactors with the temperature control on them and just an additional cold finger going down the middle. So it was doing exactly that, which was crystallizing on the walls. Nowadays, it seems like the agitation seems to be a little bit more of the way to go. With this, it does cause smaller crystals to grow, though. Is that correct? 

 

Luke Van Trieste - 00:22:10 

Yes, that's correct. I think for some people that's definitely desirable, though. 

 

Jason Showard - 00:22:15 

Agreed. 

 

Luke Van Trieste - 00:22:15 

Because for, let's say, a pharmaceutical purpose or a formulation purpose, you need to have a constant mill size. So you need to mill down. If you grow large crystals, that's great. They'll be nice, pure and pretty, but you're gonna have to grind them up at some point. And so with growing smaller crystals, it does a couple of things. 

 

Luke Van Trieste - 00:22:35 

The first is that you don't have to have a separate process where you mill a material that may still be laden with, again, an explosive, potentially explosive solvent. So that's not really super fun to do. So I think a lot of people tend to head towards the powder route because you can also wash the crystals or I guess I should say clean them up easier in the next step. Because they're already, there's tons of exposed surface area and it's much easier to handle than large chunky crystals, in my opinion. 

 

Jason Showard - 00:23:06 

Understood. Yeah, less trapped solvent as well. All right. So let's say that you've got 20 kilograms of an 85% CBD distillate. If you were to walk up to one of the BR instruments reactors that you used to crystallize, fire that thing up, what are your go to crystallization SOPs for CBD in regard to, you know, times, temps, pressures, all that? 

 

Luke Van Trieste - 00:23:28 

So just to walk you through how I do a pretty basic batch. So I think, you know, it's actually quite simple. But, you know, because there's a number of steps, it might seem a little bit more complicated. But like I said at the beginning, the basic rundown is that you're going to warm it up and you're going to cool it down and you're just going to be stirring it pretty much the whole time. That's the very basic level of it. 

 

Luke Van Trieste - 00:23:52 

So to dive into, again, some of the parameters, you're going to dissolve your CBD and whatever solvent you chose to use. And so what you basically want to do is probably heat the solvent close to its boiling point. And so for pentane, again, that's about 36. So heat your pentane up to just under boiling and that's going to let you dissolve the maximum amount of CBD or of distillate, I should say, that you can into this. 

 

Luke Van Trieste - 00:24:19 

It's very important at this stage to make sure that you have one homogenous solution at the end. And when I say solution, I mean fully dissolved. If you have some gunk or some goo or something that didn't dissolve in there. It may not work that well because, again, that stuff can kind of coat the surface of the crystals and inhibit crystallization. So it's very important to make sure that you have thoroughly mixed before you try to start this crystallization process. 

 

Jason Showard - 00:24:49 

And this is a time where it might not be a bad idea to mention the concept of oversaturating, because that can cause problems down the road, too right? 

 

Luke Van Trieste - 00:24:58 

So the level of saturation is going to vary a little bit based on your material. And so I think one of my most common answers to anybody regarding any question in this industry is, "it depends." Because there's such a wide variety of processing techniques, where you can be at this point, can kind of be a little bit up in the air. For a, let's say a first pass. Let's consider this a first pass crystallization. 

 

Luke Van Trieste - 00:25:26 

I'm probably going to start with it being a little bit more dilute, than saturated. But like I said, there is a balance between making it too saturated and too unsaturated. Because of it's too unsaturated, you'll never get crystal growth. And if it's too saturated, then again, you can run into problems such as you end up with weird viscosity issues and kind of funky problems. 

 

Luke Van Trieste - 00:25:52 

So a saturated solution is going to produce smaller crystals as well. And this has to do with the theory that crystallization is going to happen everywhere at the same time, because it can. If you consider that every point in the solution, again, that it is well mixed is going to be relatively equal to each other, then crystallization is just going to take place everywhere at the same time. So this leads to a lot more, but obviously smaller crystals. 

 

Jason Showard - 00:26:23 

Gotcha. So that said, for this example, we've got 20 kilograms of 85% CBD distillate. If you were to walk up to one of your BR instrument machines, one of your reactors and fire it up, what are your go to crystallization SOPs as far as times, temperatures, pressures, ratios, all that? 

 

Luke Van Trieste - 00:26:47 

So assuming that this is just from the start, we're going to go with, I prefer a ratio of about one to one. And this is by weight of my solvent to my distillate. And so by volume, that ends up being roughly two parts, pentane to one part distillate. But I think it's just easier to do it by weight. Because weight is going to be constant no matter what. 

 

Jason Showard - 00:27:11 

Mm hmm. 

 

Luke Van Trieste - 00:27:12 

So we're going to take our CBD, dissolve it into our starting material or starting solvent of choice. And this is going to involve a heating and mixing phase. What we really want is one homogenous liquid at the end. We don't want any separation of layers or any undissolved material floating around or sunk to the bottom of our container. 

 

Jason Showard - 00:27:35 

So for from an SOP standpoint, you're putting your solvent in first, I would imagine, and then putting your distillate in on top of that solvent. Is that accurate? 

 

Luke Van Trieste - 00:27:47 

Yes. If you do it the other way around, I find that you have a very hard time penetrating through all the distillate that's now sunk to the bottom of your reactor. And it can take quite a while to dissolve. For ease of use, I definitely recommend having pretty warmed your solvent, and then kind of maybe trickling in your distillate with stirring as you go from there. And so we even have a little hopper port essentially. So it's just basically a funnel with an open/close valve. So that way we can just turn upside down a little mason jar of distillate at a time or something as it warms up and mixes. And again, that definitely helps with the homogenization step. 

 

Jason Showard - 00:28:26 

OK, so now we've got our solvent in the reactor. We've added our warm distillate and it's been stirred around for a while to homogenize. Ballpark, what kind of times are we talking about? Like how long does it take, if you've pre-warmed your distillate, to really get a reasonable homogenization with that? 

 

Luke Van Trieste - 00:28:48 

Oh, you know, I might let it go for thirty minutes or an hour beyond the time that it's all in there. And that might even be a little excessive. Again, once you have a warm solvent, the pentane loves dissolving cannabinoids, whether it's THC or CBD. It's just some of the other stuff that might not be as enthusiastic about going into pentane like some of your residual fats and waxes, for example. 

 

Jason Showard - 00:29:14 

OK, so we've got it all dissolved. We let it wait for an hour to create a nice homogenized mixture. Now that we're confident that it is completely dissolved and everything is completely dissolved in there, what's the next step? 

 

Luke Van Trieste - 00:29:30 

So the next step is basically going to be to cool it. And it's kind of as simple as that. You know, you just take it, warm it up, get it all well mixed, and then we're going to start to cool it. I like to keep stirring, like we talked about dynamic versus, you know, kind of a static agitation. I definitely like to keep stirring. And that's just going to A, allow your solution to cool down faster because you have better heat transfer within your vessel. 

 

Luke Van Trieste - 00:29:57 

And B, it's going to, like we said, precipitate your crystals a little bit more quickly as well. And so I'll end up ramping, let's take the pentane situation from, let's say, 34 degrees Celsius and I'll ramp it down to about zero. And this is kind of where a detail that somebody else actually pointed out to me is that on your way down, at about eight degrees Celsius of your solution, you kind of tick back up for a second. 

 

Luke Van Trieste - 00:30:29 

So I might hit six degrees Celsius. And then as my crystals start to precipitate out of the solution, it actually increases the temperature of my vessel. And this is despite the fact that my chiller is still ramping down. So it's really interesting to see that these CBD crystals actually release a little bit of energy. And I interpret that as basically the CBD wants to be attached to another CBD molecule so much that it's actually able to release a little bit of energy instead of, for example, taking up a little bit of energy, which would involve some heating. 

 

Luke Van Trieste - 00:31:05 

And so I kind of use that as a rough gauge of to when I might be done crystallization. Because you can run vessels of all sizes, the times can really vary. And really your chiller size is definitely, and has an impact on the times you end up waiting. But, I'd say that I use that temperature as kind of a metric to when I maybe on the tail end of my crystallization. So once I tick back up from six degrees to eight degrees, once I start to go back down slowly, that's about when I think about what my yield needs to be for the day. 

 

Luke Van Trieste - 00:31:42 

You know, am I done? Should I push a little bit more? And generally my experiments have shown that it's a pretty good estimate. Like you can leave it overnight and your yield really won't improve that much. 

 

Jason Showard - 00:31:54 

OK. Is there anything, is there any reason not to leave it in there crystalizing for a little bit longer? I mean, if you're going to get, let's say you had nothing to do for the day and you might get a slight amount more out of the solution. Is there anything to be said for not doing it from the standpoint of creating any kind of purity problems or quality problems with your crystals? 

 

Luke Van Trieste - 00:32:17 

No, not particularly. You know, whenever, "When in doubt, you know, just wait it out." I think there can definitely be other problems preventing all of your crystals from crashing out. But there shouldn't. There's no problem with waiting. Giving it a little bit of extra time should not be a problem, though. 

 

Jason Showard - 00:32:36 

OK, so what kind of yield can you expect from a single crystallization, from a percentage perspective of your input material? 

 

Luke Van Trieste - 00:32:47 

So let's say, your example, you had 20 kg of CBD distillate. So if that test at 85% CBD, you're looking at about 17 kilograms of total available CBD in your solution at this point. So our yield from this point averages probably about 70%. That maybe a little bit higher, a little bit lower, depending on a ton of different factors, including your process and starting materials. But, so if you take 17 kilos with about a 70% yield, you're looking to get about 12 kilos of CBD out. And that's pretty reasonable. 

 

Jason Showard - 00:33:27 

OK, so a very common procedure at this point is to take those, let's say, 12 kilos that you got out, and re-dissolve and crystallize those in an effort to further purify. Can you speak to that? 

 

Luke Van Trieste - 00:33:41 

Yeah. So re-crystallization is more of a polishing step. You definitely see some diminishing returns from your first crystallization. So your first crystallization might take you from that 85% to the 98%. But the second crystallization is generally going to be when you go from your 98 to your 99.99 and you have your bleached white powder and it's a very high potency with almost no contaminants. 

 

Luke Van Trieste - 00:34:12 

One of the biggest problems with re-crystallization is it's a huge time sink and it has its losses. You know, you need to go through this whole crystallization process again. You need to use more solvent and you're going to leave even more CBD behind. 

 

Jason Showard - 00:34:28 

Yeah, actually, let's touch on that for a minute. What kind of loss do you think you can expect from let's say your 12 kilos that you've pulled out on your first crystallization? What do you think that turns into after you're finished with your re-dissolve and second crystallization? 

 

Luke Van Trieste - 00:34:44 

It probably translates to 10 to 20% of your CBD. So if you have 12 kilos, you know, you're looking at losing maybe a kilo of it. And when you're making hundreds of kilos, you know, the kind of, it really adds up. 

 

Jason Showard - 00:34:57 

Yeah. This is where you have to decide what's best for your business and what the market is asking for, and what you have a market for to make that decision. That said, circling back around to the first crystallization, if you can expect about 70% of your 17 kilos, let's talk about what happens to that other 30% of that 17 kilos that has to remain in the solvent. What are we doing with that? 

 

Luke Van Trieste - 00:35:26 

So that's a really good question. And I think that's a part of the market that is maybe even a little untapped. So the remaining solution is in the terms of the crystallization, our waste product. But as you said, it contains CBD as well as THC and some minor cannabinoids that have kind of been up until this point, more and more concentrated. 

 

Luke Van Trieste - 00:35:51 

And now that we've pushed out, you know, over half of the total volume, you know, think about it, we crashed out all the CBD. Now you really concentrate these minor cannabinoids. And so this leftover liquid is called the mother liquor. 

 

Luke Van Trieste - 00:36:10 

And I think it has fantastic properties that, again, are maybe a little bit unrealized at this point. And I'm sure there are some people that do chase that dragon. But it definitely may be a task for chromatography, for anybody out there who wants to look into that. 

 

Jason Showard - 00:36:26 

But let's talk about the common practices at the end of this. Now, you have crashed out your crystals, and you have solvent, a good amount of solvent, that is rich in the minor cannabinoids, has a little bit of THC, still has some CBD left. What do you do with the solvent after you have successfully crashed out the amount of CBD that you're trying to crash out of the solution? 

 

Luke Van Trieste - 00:36:52 

So you can take your residual mother liquor and you can put it through a solvent recovery process. And this is actually a pretty good task for a rotovap because you don't need to have super high temperatures or super high vacuum levels to pull it off. And also, generally, they're going to be a little bit, they're probably going to be a little bit safer to do this than another method. So, you know, I think a lot of people, it basically, once they recover their pentane let's say, they kind of just have barrels of it laying around. 

 

Luke Van Trieste - 00:37:25 

Like I said, I think there's an unrecognized potential for some of these materials because this is where you can get your CBD V or your THC V or, you know, some of these really kind of more rare cannabinoids that you can't just grow on the plant as of yet. 

 

Luke Van Trieste - 00:37:43 

So there's just hundreds of barrels laying around. And I've been to sites where they showed it to me. And it's like that, you know, that boggles my mind because you could really be doing some, I think, some interesting stuff. Whether you're just concentrating, let's say CBD V, or you're doing some synthetic chemistry, trying to modify some of these to do something else. I would be in line to do something with that if I had access. 

 

Jason Showard - 00:38:09 

Yeah, absolutely. It's amazing to me what this industry will call waste just because, you know, they're in the business of production of a particular material. And if it isn't that material, then it's waste. And there's just crazy things that have been called waste in front of me that just made my jaw drop. 

 

Jason Showard - 00:38:31 

So moving on from there. Let's talk a little bit about some of the things that can go wrong in your crystallization process. What are the most common reasons that you'll see somebody fail when they're going to crystallize CBD? 

 

Luke Van Trieste - 00:38:42 

So I probably most frequently get, "Hey, my yield is not where it's supposed to be." A lot of that has to do with, my first assumption is, go back to your distillate and check your winterization standard. 

 

Luke Van Trieste - 00:39:00 

How well was this winterized? And, you know, could we get more out? Fats and waxes tend to inhibit crystallization quite well. And, you know, I don't have necessarily a scientific reason for that. But if you think about it, when you make an edible, let's say, and you need to add some butter to make your oil in, the fat is basically the solvent. The fat in the butter or your MCT or whatever is your solvent. 

 

Luke Van Trieste - 00:39:29 

And so basically when you have, let's say, impurities such as these fats and waxes or terpenes, or even other cannabinoids, you can definitely inhibit crystal growth and that's really going to hurt your yield. 

 

Luke Van Trieste - 00:39:44 

The next most common one is probably the wrong ratio. So like I said, I start with one to one, but one of the benefits of doing this all in the reactor is let's say I had a bad day and I didn't get anything to crash out. Well, what I'll probably do is I'll just heat it back up. Maybe boil off some of my solvent and try again tomorrow with a more concentrated solution. So solvent ratio is really important and it's going to be highly material dependent as well, like I've been saying. 

 

Luke Van Trieste - 00:40:18 

Too concentrated, and you're going to get some goo that crashes out and it's going to be very viscous liquid. And you don't have those CBD molecules freely floating around trying to find each other. But on the other hand, if it's too dilute, nothing's ever going to happen. 

 

Jason Showard - 00:40:34 

OK, well, it's nice to know that you can try again tomorrow if it's not working out for you. Moving on from there, we've been talking all about the agitated batch crystallization today. I've been seeing some buzz about continuous flow crystallization lately. Talk to me a little bit about what that process looks like and how it works. 

 

Luke Van Trieste - 00:40:58 

So with a continuous process, one of the key components is having a constant feed stream. And so the more consistent your feed stream is, the better. I think that's one of the issues with Continuous that I'll bring up now is that, you know, every strain that you extract and every crop from every different farmer is going to be a little bit different. 

 

Luke Van Trieste - 00:41:25 

So with continuous that basically means that if you never turn this machine off and it's running all the time, that your composition is changing. And so your parameters need to change as well. But, to walk you through a basic continuous process, you're going to flow this premixed feedstock into a reactor. Generally, there's going to be several stages to the reactor. In the case of NiTech Solutions, they're a company out of Scotland, I believe. Basically, they stage temperature zones. So the first zone, I think, is that warmer one. 

 

Luke Van Trieste - 00:42:08 

So I think 15 to 20 degrees Celsius. And then the next zone is 10 degrees lower, and then the next zone is 10 degrees lower than that. And basically by, you know, having this continuous process, they can get very high purity with very little user input. And I think that's one of the attractive things about continuous processes, is that when they run, they don't stop. The spigot does not turn off. 

 

Jason Showard - 00:42:37 

So we've got staged temperature zones and different reactors. It just walks it all the way down to that same temperature zone that you would walk it down to in your batch reactor? 

 

Luke Van Trieste - 00:42:54 

Yeah, basically. And by staging it, you know, you can really, there's some energy advantages to staging it. And there's actually some purity advantage to staging it. So like I was saying, the higher temperatures, what kind of happens in the first stage is that some of your CBD does crash out in the first stage. But because your solvent is still room temperature, it's kind of at an equilibrium where it'll dissolve away a little bit, and then it'll kind of end up reforming at a little bit higher purity in the next stage, and so on and so on. 

 

Jason Showard - 00:43:28 

So do you collect the crystals from different stages, or are the crystals all collected together at the end? 

 

Luke Van Trieste - 00:43:34 

I believe they're collected all together at the end. As basically the final stage, you've been re-crystalized. So the first stage is crystallization and then the next two stages are essentially a re-crystallization. Or, your solution is at a higher potency by the time it's gotten to that point. I believe they're collected at the last stage. 

 

Jason Showard - 00:43:56 

Gotcha. OK, cool. It's such an interesting concept there with the continuous flow. So circling back around to you guys. BR made its name in the cannabis space with the spinning band distillation units. You guys were already an established company that kind of fell into the cannabis space because you had a machine that worked well for it, rather than designing one specifically for it. Since then, a bunch of other companies have popped up who are designing and marketing real hard directly into the cannabis market. So what are you guys doing to stay on top of your position there, and stay on top of the cannabis lab market with the new competition entering the space? 

 

Luke Van Trieste - 00:44:40 

So I'd say the first thing is always about scaling up. You know, five years ago, I don't think we pictured making spinning bands as big as we did. But, you know, we've kind of learned some lessons along the way. We've done some R&D. And I think things are only going to get bigger from here, whether it's CBD or THC. The demands for the average lab are only going to go up. And, you know, we'd like to stay relevant. So scaling up is probably our primary factor, but, you know, I like I said, I'm the person, I'm the boots on the ground, so to speak. So I'm there. I see what problems happen. 

 

Luke Van Trieste - 00:45:22 

People call me. I do a lot of the service, so I know what breaks when it breaks. And so we do a lot of R&D. And because at the end of the day, that makes my job easier. If I come up with a solution, then the customers are happier and I have less phone calls. So we've been doing a lot of R&D just to try to make our lives easier. And again, the customer doesn't want to be calling you either. You know, you have to consider that. 

 

Jason Showard - 00:45:45 

Yeah it makes everybody's life easier. 

 

Luke Van Trieste - 00:45:47 

Yeah. And the final thing is that we are just trying to offer more products to the cannabis space specifically. And so that's the function of this reactor. You know, the reactor isn't a super specialized piece of equipment, but it's something that we can offer. You know, we already buy tons of stainless steel and different vessels and stuff. So why aren't we selling one? You know, I've done crystallization. 

 

Jason Showard - 00:46:12 

I know how to crystallize, why am I not training people on them? So I think offering more products is definitely, you know, diversifying basically is definitely a goal as well. 

 

Jason Showard - 00:46:23 

Gotcha. Yeah. Do you guys have any new offerings scheduled to come out in 2021 one that we can look forward to? 

 

Luke Van Trieste - 00:46:30 

Yes, unfortunately I can't share a lot about them. But what I will say is, you know, one is a prototype that we will have finished building in March. And so by April we'll probably be selling some. You know, with a little bit of a lead time and then hopefully the lead time will go down from there. I can't say what it's for quite yet because of contracts and stuff like that, but do look forward to that if you're in the CBD/Hemp space. 

 

Jason Showard - 00:46:57 

Well definitely reach out to me and let me know when that does come out so I can go ahead and let all of our listeners know through the Instagram. 

 

Luke Van Trieste - 00:47:06 

Oh, yeah. And this other thing, if this works, I will be so excited and you may never hear from me again. If it works as well as I hope it do. Because I'll be retired on some island or something. But it's kind of so conceptual at this point. Again, one thing that I value, like I said with the reactor, is a multifaceted tool. Something that I can do more than one thing with, because in this industry, you need to stay flexible. You need to do what works. And so this would be more on the analytical side. 

 

Luke Van Trieste - 00:47:36 

But depending on what I can detect and the levels that I can detect with it. I don't mean to hype it up too much, but it really could be a game changer and it's quite exciting. But I just basically got my 30, 40 samples from my analytical lab back and tested. So it's still a little preliminary, but I'll be very excited if that goes through. 

 

Jason Showard - 00:47:59 

So some analytical machines as well. That'll be interesting. Now, the place that everybody usually drops all this new equipment and releases everything is Biz-Con. Everybody in the industry's favorite trip to Vegas to carry on with our peers. Unfortunately, we didn't get to do that this year because we were all in the middle of the pandemic. So what did you guys end up doing for the virtual Biz-Con that popped up this year? 

 

Luke Van Trieste - 00:48:26 

So honestly, we decided to sit this year out. I think we just felt like the virtual platform wasn't really going to do what we wanted it to. You know, I think, like you said a lot of Vegas is simply the networking. 

 

Luke Van Trieste - 00:48:41 

It's just being, everybody getting the same place, sitting down, doing these things. And I felt like that was maybe a little lost this year. So what I did instead is I asked my boss for the money that we got back because they held him up for the deposit. And I got to take some cool pictures of our equipment that I needed for the website and stuff. So I basically turned marketing into marketing, but we didn't participate in the virtual Biz-Con this year. 

 

Jason Showard - 00:49:05 

Understood. Yeah. I've seen some pictures of your lighting kit with some machines in front of it what not, on your website or maybe that was the blog. 

 

Luke Van Trieste - 00:49:13 

Oh yeah. That's me. That's my modeling career, if that ever takes off. 

 

Jason Showard - 00:49:18 

All right, cool. Yeah. That always helps with sales, having some good pics of the products. Hopefully you can get a couple of those over to me to help promote having you on the show on our Instagram. 

 

Luke Van Trieste - 00:49:29 

Yeah, absolutely. And if this is an appropriate time, I'd like to promote our Instagram as well. It's @BRInstrument. I believe it says mark.schmidt@brinstrument.com is like the title of it. But me and a couple other guys watch that. So if you anybody has any questions, you can reach out directly to us on Instagram, of course. 

 

Luke Van Trieste - 00:49:50 

And I think it's just, it's basically a portfolio of what we do. You know, I include a lot of cannabis and THC stuff, because that's where I spend most of my time. But, you know, you get to see some of the other side of things as well, like the petroleum and whatnot. 

 

Jason Showard - 00:50:02 

Yeah, I was about to circle around to the contact side of things, but before we get too far down that road, I do have a personal question for you. I like to ask everybody this. What is it that you are most excited about regarding the future of the extraction industry? 

 

Luke Van Trieste - 00:50:18 

I am most excited for maybe federal legalization, for a couple of reasons. I think the biggest thing is that right now I go to labs and they're killing it in one state and they have another lab in another state. Then they just can't replicate it. 

 

Luke Van Trieste - 00:50:37 

I really think this interstate competition will be beneficial to all labs ultimately. Because right now, you know, there's just so little information traveling across state lines, even between companies or, you know, different divisions of the same company. It's kind of crazy to me. You know, you should be able to send, you know, send your analytical sample here, there. So I'm excited for federal legalization because I think it'll definitely, it'll be a genesis for our industry. 

 

Luke Van Trieste - 00:51:07 

We're going to see a ton of new things dumped into it at the same time. And I think it'll definitely take a lot of people out at the same time. But, you know, it's definitely the next biggest step that we can hope for. 

 

Jason Showard - 00:51:21 

Yeah, I agree. There's going to be, there's certainly going to be some consolidations there and some big players entering the game. But as Jay, who was on last week said, you know, embrace change, it's going to bring a lot of advancements. It's going to bring a lot of interesting new stuff. And it's going to really see the industry that we enjoy being part of on a scientific side of things, have some real serious advancements when you can start sharing and working together instead of every man for himself. 

 

Luke Van Trieste - 00:51:53 

Yeah, and I think that it's really important to have this collaborative sense too, you know. Even when times make it a little bit tougher. I'm just a very big fan of free-flowing information. And I think that it's a way for maybe smaller guys like us or the individual lab to survive the big consolidation by Coca-Cola or whatever, is to, you know, be open and free in trading the stuff that they paid for in the eighties or whatever and been sitting on. They're sitting on ever since, you know. So I think it'll be a great opportunity. 

 

Jason Showard - 00:52:28 

You know, as people seem to be worried about this big giant corporate takeover that's coming. And, you know, look at the beer industry. There's plenty of craft breweries out there. There's always going to be a market for people that care for their craft, especially with the connoisseurs that exists in this industry. So I don't think any of us have too much to worry about in that respect. 

 

Luke Van Trieste - 00:52:51 

Yeah. And I think the other side of that is nobody wants to go buy Wal-Mart weed. You know, that doesn't have a nice ring to it, you know. So I think they're going to depend, maybe they'll buy you out. Because they're going to depend on your branding to change the perception of their products. 

 

Jason Showard - 00:53:06 

You know, I would go buy some Equate CBD, but I'm not going to go buy some Equate, you know, Bud, for example. Because that just does not sound you know, it'll be like their produce, just colorless and limp like. 

 

Luke Van Trieste - 00:53:22 

So, you know, I think there's two sides of that coin where they'll definitely have, they'll have all of us be on the scale and there's nothing we can do about that. But what we can do is stick together and share the information that we do know and advance ourselves to keep up with them. And again, like you said, there's tons of craft beer and wine out there now. So there's no reason that a product that started in the hands of the people can't stay in the hands of the people. 

 

Jason Showard - 00:53:49 

Absolutely. So you mentioned your Instagram a minute ago. Give that to us one more time and then any other methods of contact for you that are good. If people want to get a hold of you and see how either your knowledge or machinery can benefit them in their lab. 

 

Luke Van Trieste - 00:54:04 

So you can get a hold of us on Instagram at @BRInstrument. You can get a hold of us through our website. So that's brinstrument.com. You can use the contact button on there and ask for Luke, or you can get a hold of me directly through my email at luke.vantrieste@brinstrument.com. So that's luke.vantrieste@brinstrument.com with a dot between my first and last name. 

 

Jason Showard - 00:54:43 

Right on. Well I can attest to the fact that you're responsive. The fact that you are so responsive on that blog and watching that conversation unfold regarding the CBD crystallization is what made me want to have you on the show. So for the folks out there, he'll get back to you. And Luke, thank you so much for coming on the show. It was a pleasure to talk to you. I think it was a really informative episode of The Modern Extractor and a great person to wrap up the final episode of the season with. 

 

Luke Van Trieste - 00:55:12 

Well, thanks for having me and thanks for giving me a place to promote myself and my company. 

 

Jason Showard - 00:55:17 

Absolutely. Well, hopefully we'll talk to you again in the future. 

 

Luke Van Trieste - 00:55:19 

Thank you so much. 

 

Jason Showard - 00:55:21 

All right, thanks again to Luke for joining us on the show today. Those SOPs will have you crashing out crystals like a pro. If you want to get a hold of Luke, hit him up on Instagram @BRInstrument or email him directly, luke.vantrieste@brinstrument.com. He's a knowledgeable guy and he's always willing to help you improve your process. 

 

Jason Showard - 00:55:45 

As always, if you want to hear something specific on the show, let me know. Email me jason@modernextractor.com. 

 

Jason Showard - 00:55:53 

Make sure to follow the show on Instagram @The_Modern_Extractor. If you guys like the show, please subscribe and give us a rating. The more subscribers and better ratings we get, the better guests I can book for you here in the future. So congratulations, Modern Extractor listeners. We've made it all the way through an ethanol extraction lab. We've broken down each step of the process to take plant material all the way through to pure crystalized isolate. 

 

Jason Showard - 00:56:21 

As I said last week, the show's gotten some good traction. We're getting awesome guests and we've got people tuning in from all over the world. So I've decided to keep it rolling for another season. 

 

Jason Showard - 00:56:31 

After a short break, in season two, we're going to tackle hydrocarbon extraction and post processing. I'm really excited for it. And I've already been talking with some fantastic guests about joining us along the way. As I begin to flesh out the content for season two. I'd love your input. I want to know what you, the listeners want to know about. The floor is yours. Email me or drop me a line on Instagram to tell me what and who you want to hear. 

 

Jason Showard - 00:56:54 

Don't worry, I'm not going to leave you hanging too long. Between seasons, I'll be putting out bonus episodes to keep you all interested. If you're a subscriber to the show, that high tech gadget in your pocket will tell you when bonus episodes are released. Also, check in on the website for updates, www.modernextractor.com. 

 

Jason Showard - 00:57:12 

As usual, a big thanks to Yzaura Vanegas for handling business on the show's social Media. Thanks to Grind Life Republic for the care package, stickers, and the t-shirt. Thanks again to everybody for tuning into The Modern Extractor. Season two will be out before you know it. I'm Jason Showard, let's talk soon. 

 

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About the Podcast

The Modern Extractor
Professional extractors talk extraction!
The Modern Extractor is a podcast about the processes, equipment, and science found inside a cannabis extraction laboratory. Season one focuses on the process of ethanol extraction and post processing into either distillate or isolate. Season two focuses on hydrocarbon extraction and the craft concentrates that it can produce. Each episode digs deep into a particular stage in the extraction and finishing processes, and we discuss the various approaches with industry expert guests. Episodes are released in an order which follows the work flow through a lab, following material closely through the process from cultivar to concentrate.