Tek Solvent Extractions

[DieHard]

@SamuraiSam that stuff looks so good I can almost taste it!

 

[herbivore21]

I am still in learning / training mode and while I've had a hand in a a few runs here, I would not say "I've made it" unless I did every step start-to-finish, and I certainly haven't done that at this lab yet. I've mostly been doing labor for, and learning the process of ECC's head extractor as an 'intern' if you will. Due to the time it takes to process hydrocarbon extracts, I won't be completing anything solo until I come on board as a full time employee. I'll be sure to let ya know when that's happened, hopefully just a few more weeks.

Have any of ya watched Bill Nye's new show?

It's not magic, it's science!

No problem my friend. I respect your honesty man, that's one reason that I'm glad to have you here! Integrity in this sort of information is so important. I look forward to hearing about your first attempts at this on your own brother!

In the meantime, if you're able it'd be wonderful if you could let us know how this HTFSE and HCFSE are made?

Holy shit it has been a long time since I've run something with solvents. I wonder if I'll have to dust off the equipment one of these days and try this stuff?

Also I actually haven't seen Nye's new show, I am generally too busy doing my own science recently to watch much TV

 

[SamuraiSam]

Like I said, I dont make those trademarked five letter acronym products, Im working as a technician operating a closed loop extraction system. extractioneering has stated that the HTFSE and HCFSE are made with solvents "run to waste" aka not recovered for later use.

I haven't open blasted in a long time. So I'm doing some things differently than he is, and according to him, not producing the same products.

A really smart dude on Reddit had a comment regarding this topic, which I hadn't previously considered, and is worth discussing:

he has a point about not using recycled solvent though. There is quite a bit of speculation and some evidence that pesticide residue and other volatiles are retained in the solvent regardless of distilling it again.

Edit: http://cannabissafetyinstitute.org/wp-content/uploads/2015/06/CSI-Pesticides-White-Paper.pdf

"However, the observation that the mean level of pesticides appears to be roughly 10x higher in concentrates versus flowers is somewhat surprising, given that cannabinoids are only about 2-5x more concentrated in extracted products.
Several factors could be contributing to this phenomenon, including
(1) that some pesticides are more efficiently concentrated by these extraction techniques than cannabinoids are,
(2) that chronic contamination of equipment and solvents may lead to cross contamination of later products, and/or
(3) because it is a common practice to make concentrates from ‘trim’ which is left over after harvesting the quality buds and the ‘trim’ may be more heavily contaminated than the buds which are sold and analyzed separately."

 

[Killick]

Beautiful shots @SamuraiSam ! Thanks for sharing.

So slight off-topic, but solvent-extraction related-ish... Someone I know recently came into a couple of wierd things, including a 15 gallon still and 260 gallons of wine. They are hoping to not have any blasts whatsoever, but in the end should have a reasonable collection of extraction solvent. Does anyone have experience with that part of the 'solvent extraction' (and I admit this may not be the right thread for it) equation?

 

[SamuraiSam]

@SamuraiSam yes please! I've recently found a source for clean, solvent-grade propane and have been thinking about giving it a whirl. For the record I've never used any gases (nothing xxtane anyways). I did a couple of ISO washes when first starting, but didn't trust my purge tech enough and used it for topicals. So the short story is I want to learn how to use those techniques properly, even if I never try them IRL. People use what is available to them. I'd hate to see someone not make their own meds simply because they can't find the 'best' solvent available. Everything can be done safely.

The Mason jar method was a recent addition. I was wondering about storage and heard about canning and it seems to work dandy. It also worked well for the whole 'smush and fill with frozen EC' step yesterday. I'm always open to pointers, especially if I can make shatter as pretty as Herbies, as mine always comes up dark and sticky. I'm *finally* starting to realize this is because I'm washing too hard/long in all methods - bubble, solvent, etc. I've been trying to get everything first wash, which is fine for anything besides vaping. Next alcohol wash will be a 3 minute soak, 1 minute agitation, and fast filter. The herb will get another soak for FECO. Bubble, well, now I know there is more than 1 wash... I wonder if the stuff I put in the composter last fall could be cleaned up and run again? Or just start from fresh and be more gentle this time?

PS - now's likely a good time to thank @herbivore21 for all the kind assistance over the past few years. There are others, as well, but Herbie really goes out of his way to ensure we're doing things safely, and that has had a great impact on many of us, especially when we were first getting started. Now that I'm getting better with tech Herbie continues to provide great insight, and now I almost know what he's talking about - thanks Herbie - it's really appreciated :)

PS - I also have a High 5 rosin press. I wish it could hold an oz per squish, but it's pretty good for bubble :)

Beautiful shots @SamuraiSam ! Thanks for sharing.

So slight off-topic, but solvent-extraction related-ish... Someone I know recently came into a couple of wierd things, including a 15 gallon still and 260 gallons of wine. They are hoping to not have any blasts whatsoever, but in the end should have a reasonable collection of extraction solvent. Does anyone have experience with that part of the 'solvent extraction' (and I admit this may not be the right thread for it) equation?

Hey killick I'm sorry I didn't respond to your prior post. Regarding propane, it falls into the same classification as butane, in that it's a flammable gas and has to be handled and utilized safely. Propane has a much steeper pressure increase w regards to temperature.its working pressure is about 4 times greater than that of butane. For that reason not any butane closed loop system can be used to process with propane, the equipment manufacturer has to certify all the components of the system to handle the increased pressure vs n-butane or isobutane. IMO to make a quality solvent extract a closed loop system is required so that you can begin by distilling the solvent before it is put through the plant matter. There's a significant amount of residue left to clean off inside the collection pot after a distillation.

I have only tried the quick-wash ISO method two times and I didn't make anything worth consuming so that technique has been shelved for me, for quite some time. Alcohol is a highly polar solvent and will extract chlorophyll, waxes, vegetable oils, all those water-soluble components that are not touched by butane or propane.

With regards to run bubble material, I would throw it away. The plant matter has decomposed beyond a point worth running. if you 'washed' it again if any heads separated, they would be very green, and unpleasant to inhale. Once you obtain new material, unless you are running fresh frozen, be sure it is properly cured, then try multiple short washes, and keep washing until you don't yield resin worth collecting out of the bags.

 

[herbivore21]

Like I said, I dont make those trademarked five letter acronym products, Im working as a technician operating a closed loop extraction system. extractioneering has stated that the HTFSE and HCFSE are made with solvents "run to waste" aka not recovered for later use.

I haven't open blasted in a long time. So I'm doing some things differently than he is, and according to him, not producing the same products.

A really smart dude on Reddit had a comment regarding this topic, which I hadn't previously considered, and is worth discussing:


"However, the observation that the mean level of pesticides appears to be roughly 10x higher in concentrates versus flowers is somewhat surprising, given that cannabinoids are only about 2-5x more concentrated in extracted products.
Several factors could be contributing to this phenomenon, including
(1) that some pesticides are more efficiently concentrated by these extraction techniques than cannabinoids are,
(2) that chronic contamination of equipment and solvents may lead to cross contamination of later products, and/or
(3) because it is a common practice to make concentrates from ‘trim’ which is left over after harvesting the quality buds and the ‘trim’ may be more heavily contaminated than the buds which are sold and analyzed separately."

With regard to recovered solvents being used in subsequent extractions, I agree that there are definitely concerns as to contamination of the solvent especially with successive recovery. IMO, the solvent should be subject to testing for any relevant potential contamination if it is being reused. This is no doubt a consideration already in other manufacturing that involves similar organic solvent extractions across various industries.

I have been considering HTFSE and HCFSE a bit more now over the last week, and realize that to me, the most likely method being used is crystallization of a supersaturated solvent extract (BHO is the most likely initial extract being crystallized).

During a solvent purge in the right conditions, THCA crystals can be made to precipitate out of the solvent/solution, and start to grow into highly pure THCA crystals while the terps and other resin content remain dissolved in the solvent (this liquid fraction containing the solvent and remaining non-crystallized substances is called the 'mother liquor'). The crystals will contain mostly THCA, with some remaining 'mother liquor' trapped inside the crystals.

The crystals will not be completely pure and hence colorless, unless further washed/refined, and will retain some of the color of the solution due to residual mother liquor in the crystals. A colored, sugary, partially crystallized fraction, to my mind could be exactly what HCFSE is. The mother liquor remaining, when purged of residual solvent would be the HTFSE. Is this in the ballpark of what you are learning to do bro? I know that crystallization often makes use of a centrifuge to assist in separation of fractions which might explain extractioneering's use of one.

I have only tried the quick-wash ISO method two times and I didn't make anything worth consuming so that technique has been shelved for me, for quite some time. Alcohol is a highly polar solvent and will extract chlorophyll, waxes, vegetable oils, all those water-soluble components that are not touched by butane or propane.

I hope you've seen my iso extracts man, as iso was my primary extraction solvent. All of my solvent extract pics tend to be QWISO, and my QWISO was definitely more enjoyable to dab than run of the mill butane extractions at the time.

The properties of alcohol are greatly different, as you say. All this means is that to produce the best concentrates with iso vs other solvents, you need to adjust your flow speed, wash time and other relevant methods. I prefer iso to ethanol tbh, since the ISO I get has no sugars etc to impart into the final extract, unlike ethanol. I'd love to revisit my ISO tek with the greatly improved understanding that I have of cannabis resin now. One of these days, I'm sure it'll happen.

In my view, iso is very unforgiving at first and especially if you try to use it like other solvents (using similar wash times with iso as what you would use with ethanol/butane is gonna give you a very bad time!), but is a wonderful solvent to use if you can master it. Especially in a non-commercial home use scenario.

I have often lived in places where butane and propane extraction is entirely inappropriate and unsafe unless I had a fumehood ($$$). This is why I was forced to find a way with alcohol solvents that are viewed by most as impossible to use with worthwhile results.

 

[SamuraiSam]

https://www.reddit.com/r/CannabisEx...n_is_a_safe_and_green_way_to_extract/ddlan3h/

https://www.reddit.com/r/CannabisEx.../how_is_hcfse_high_cannabinoid_full_spectrum/

If extracted properly, crystallization occurs naturally in a purged solution of terpenes and cannabinoids. I've read a variety of different 'tricks' for 'seeding' crystal formation and have never tried any of them. As stated before extractioneering uses an n-butane/isobutane/n-propane mix to achieve their results.

My response to the 'pesticide solvent carry-over' was:

That's a really interesting hypothesis, thanks as always for sharing your knowledge. So it's possible that there is some tertiary reason beyond any stated by extrationeering for his reasoning to open blast. Th

e article linked showing higher levels detected in its sampling of concentrates does appear to be, as you stated, speculation and there are multiple hypothesis with no follow up studies performed such as comparing residual pesticide levels from different types of extracts such as a trim run vs nug run, BHO or mixed hydrocarbon versus CO2, versus rosin; testing the recovered, distilled solvent from a hydrocarbon extraction system for the presence of any of those pesticides that are suspected to be 'carried-over' in the solvent.
"Several factors could be contributing to this phenomenon, including
(1) that some pesticides are more efficiently concentrated by these extraction techniques than cannabinoids are,
(2) that chronic contamination of equipment and solvents may lead to cross contamination of later products, and/or
(3) because it is a common practice to make concentrates from ‘trim’ which is left over after harvesting the quality buds and the ‘trim’ may be more heavily contaminated than the buds which are sold and analyzed separately."

Sorry for the odd formatting, I've tried editing the post several times and no matter how many times I delete the extra quote brackets they keep coming back.

 

[herbivore21]

If extracted properly, crystallization occurs naturally in a purged solution of terpenes and cannabinoids. I've read a variety of different 'tricks' for 'seeding' crystal formation and have never tried any of them. As stated before extractioneering uses an n-butane/isobutane/n-propane mix to achieve their results.

I knew it! Knowing now what is being done to refine and create these products, I realize that holy shit, retailing those products must be profit heaven!

I'm quite familiar with relevant organic chem literature on crystallization and am happy to assist you with relevant theory if there's anything you'd like to try out (for example, using seed crystals to facilitate the reaction).

Yes, if left in the right conditions, crystallization will precipitate during a purge to some extent. Extractioneering is clearly not allowing crystallization to fully take its course. This would end in larger, more pure crystals of THCA with a slight color taint from residual mother liquor. Such relatively pure crystals would render the crystalline 'HCFSE' fraction too devoid of terps to be so enjoyable. It is also important not to too fully crystallize the THCA present, this is to ensure that some cannabinoids are present in the runny 'HTFSE' fraction.

BTW, aside from seeding, crystallization can be precipitated with vacuum or heat evaporation, scratching the glass in your vessel can also more readily precipitate crystallization at that point or by using different temps when dissolving the resin in your solvent in order to better achieve supersaturation (different temps with the same solvent = different solubility for the same solute).

It seems that we are in complete agreement on reusing solvents too bro lol! There are valid concerns about contamination, but we can simply test recovered solvent to ensure that these concerns are not born out in our meds

 

[DieHard]

Fuck! I love science!

 

[herbivore21]

Fuck! I love science!

Man ain't that the truth, I gotta make me some HTFSE one of these days lol

 

[Vicki]

A couple years ago, I started to get into vaping concentrates. I was getting it off the black market. The person making it wasn't purging it enough. I found out later that my BHO wasn't supposed to crackle and pop while vaping. I don't know if vaping that crap hurt me. I hope not. I was recently diagnosed with COPD, but can't be sure that contributed in any way because I did use to smoke cigarettes, but quit many years ago.

I wish I had more knowledge like this back then.

 

[herbivore21]

A couple years ago, I started to get into vaping concentrates. I was getting it off the black market. The person making it wasn't purging it enough. I found out later that my BHO wasn't supposed to crackle and pop while vaping. I don't know if vaping that crap hurt me. I hope not. I was recently diagnosed with COPD, but can't be sure that contributed in any way because I did use to smoke cigarettes, but quit many years ago.

I wish I had more knowledge like this back then.

I am sure I dabbed underpurged product in my very, very early QWISO attempts. I can only be glad that because I was seeking shatter at the time, I ended up if anything over-purging very quickly.

Do not buy black market solvent extracts is my advice. My bro @SamuraiSam is producing in a regulated and tested environment. They are by all accounts using proper equipment and this is the sort of vendor who can make safe solvent extracts. If you can get tested extracts from extract artists who take due diligence, provide test results and follow best manufacturing practices, solvent extracts can be affordable and in some cases, quite high quality!

I do not recommend that anybody try to DIY with solvent extractions these days. I've had a lot of PM's over the years from people asking me to help them with solvent extractions and holy shit do alarm bells go off in my mind reading what they are doing.

I've said it before and I'll say it again: MOST PEOPLE SHOULD NOT BE EXTRACTING WITH SOLVENTS. Leave it to the professionals, demand tests for their products and don't buy black market solvent extracts. If you want to DIY, check out rosin for equivalent yields and better results in a DIY home scenario. If you have a lot of flower/trim, try your hand at bubble tek or dry sifting to get your hands on the very best!

This thread and the great conversation we've been having here recently is a testament to the fact that solvent extractions are not dead, they've moved on to much bigger and better things in some cases. However, to make better solvent extractions than what you'll get from rosining the same material, you need considerably more lab know-how and equipment.

When I started with DIY solvent extracting, there was no rosin tek. I didn't have enough access to good quality flower to justify hash extraction methods. There was no other way to get into concentrates at the time. Now we only need to rosin our flower. Anyone can do that without hurting themselves or risking their home, family, pets and neighbors.

I truly hope that none of the COPD that you experience now has been as a result of those underpurged concentrates. You are right to say it is very difficult to isolate the extent to which cigarettes or other causes like underpurged extracts were responsible. All you can do now is take care of you.

It is so important to highlight that concentrates should not pop and sizzle when dabbed and that needs to go into the first post in this thread. I thank you for raising that here! It may seem to be assumed knowledge, but we need to communicate this stuff to everybody for their safety, whether they know much about extracts or not. I'm actually going to create new threads here for different kinds of solvent extracts soon enough. I need to attend to the Vape Safety section first as I know our friend @Ed's TnT has returned to finish going over his vape

There's no for the wicked it would seem!

 

[Ed's TnT]

There's no for the wicked it would seem!

I so feel you bro, seems we'll get that sleep when we die! Do what you do until you cant any longer!

 

[Baron23]

A couple years ago, I started to get into vaping concentrates. I was getting it off the black market. The person making it wasn't purging it enough. I found out later that my BHO wasn't supposed to crackle and pop while vaping. I don't know if vaping that crap hurt me. I hope not. I was recently diagnosed with COPD, but can't be sure that contributed in any way because I did use to smoke cigarettes, but quit many years ago.

I wish I had more knowledge like this back then.

Hi Vicki - of course @herbivore21 doesn't need me to validate his posts, but I agree completely about black market wax. Last time I bought some it was very dark in color, tasted like mowed grass, and although I had two grams of it, I would not vape it. Made it into brownies (and I'm not a big edibles fan).

Cheers

 

[momofthegoons]

Last time I bought some it was very dark in color, tasted like mowed grass, and although I had two grams of it, I would not vape it.

I've had this same thing happen recently with concentrate that I purchased at a dispensary. It left residue on the nail as well. I'm turning it into edibles too.

I'll be happy when all product sold at the dispensaries is tested. For now, I'll just sticking with extractionists that are tried and true.

 

[herbivore21]

I've had this same thing happen recently with concentrate that I purchased at a dispensary. It left residue on the nail as well. I'm turning it into edibles too.

I've found some frightening residues on my nails from extracts that I've made from flowers of unknown provenance. The scary thing is I'm talking residues that made it into full melt bubble hash that was produced by running it through gallons of water.

One thing that people need to appreciate is that some of the worst contaminants that get into extracts can come from the grower, not the extractor. There are for example, treatments that growers can apply for pests/mildew/mold that can impart oily substances that can get into the resin glands on both flowering and vegetative plants (sessile trichomes develop during veg on leaf matter, not just in flower on the nugs). There can be a variety of other problems in growing that can effect extracts like other pesticides, improper flushing and applications of systemic treatments of any kind.

 

[Killick]

I wasn't sure where to put this, but kinda thought Herbie might have some interest in it: https://skunkpharmresearch.com/2017/05/06/vacuum-pump-evaluation/

 

[herbivore21]

I wasn't sure where to put this, but kinda thought Herbie might have some interest in it: https://skunkpharmresearch.com/2017/05/06/vacuum-pump-evaluation/

This one may be better over in the Solvent Extracts thread, but this is a very interesting article! I have long said that diaphragm pumps are more appropriate for extraction purposes. Unfortunately, aside from the considerations mentioned by Skunk Pharm about needing to get the right diaphragm pump for the job, the cost of diaphragm pumps is generally greater than the rotary vane alternatives.

Man would I ever love to get my hands on a rotovap and a nice diaphragm pump

 

[DieHard]

Here are some more Unicorns! EXTSE (Extractioneering True Spectrum Extract) surrounded by HCFSE (High Cannabinoid Full Spectrum Extract) looking like vials of pure sunshine! This stuff tastes and smells closest to the respective strains than any other concentrate I have tried.

 

[SamuraiSam]

View attachment 312 Here are some more Unicorns! EXTSE (Extractioneering True Spectrum Extract) surrounded by HCFSE (High Cannabinoid Full Spectrum Extract) looking like vials of pure sunshine! This stuff tastes and smells closest to the respective strains than any other concentrate I have tried.

Such a shame he doesn't do business in Washington. I tried to get some goods last fall while in California but they were not in stock any where I visited. I'd particularly like to try the Sour Diesel.... mmmmm