Hexane Honey Oil extraction and alchemy

[bobblehead]

Good topic brother BH! As you may note, our process is different enough to not involve neutralizing with sodium bicarbonate.

As the lowly ancient equipment and process engineer in our scraggly group, I am going to encourage our bio-chemistry student, whom developed the process, to take a momentary break from class and adoration of his first new born son, to join this forum and provide the intimate details that you seek.

May I get back to you with his thoughts?

Thanks! I do recognize that we are using 2 different procedures... But they aren't that different. I've only had chem 131 & 132, so just enough to make me dangerous. Lol...

I'm also curious about your observations between the differences in isomerized but not acetylated, and acetylated. No pressurized hood?

I'll be around...

 

[Gray Wolf]

Thanks! I do recognize that we are using 2 different procedures... But they aren't that different. I've only had chem 131 & 132, so just enough to make me dangerous. Lol...

I'm also curious about your observations between the differences in isomerized but not acetylated, and acetylated. No pressurized hood?

I'll be around...

Yeah, I've forgotten enough of the chemistry I took over 50 years ago, to make me dangerous too.

My observations between isomerized and acetylated, is that isomerized was pretty ho hum, because there wasn't that much CBD to covert in the first place.

The acetate was a different story, and made a significant difference in uptake speed. Because it simply arrives, instead of coming on, it also put a couple extremely high tolerance, and over confident testers horizontal counting the clouds, where the plain oil and the isomerized oil have failed to phase them.

 

[G.O. Joe]

Yes but your oil may be both mostly isomerized and acetylated. The only answer can come from a lab that quantifies THC isomers, and figure out the acetate as well.

Some hints could be gleaned though from trying something different.

 

[bobblehead]

Yes but your oil may be both mostly isomerized and acetylated. The only answer can come from a lab that quantifies THC isomers, and figure out the acetate as well.

Some hints could be gleaned though from trying something different.

Exactly... Any cbd is going to be rotated to thc during the refluxing to achieve acetylation... The only reasons I didn't do acetylation were 1- b/c of the safety hazard, you're supposed to use a hood pressurized with nitrogen gas... And 2- anecdotal reports of acetylation not being all it's cracked up to be, b/c cannabis doesn't act on the brain in the same manner as opium.

I'm all ears though... B/c I'm no biochemist. I'm just on a quest to have the most potent concentrate available.

 

[G.O. Joe]

I'm still talking about isomerization of natural THC as I also referred to. The widely circulated methods using only sulfuric, hydrochloric, or tosic acids all take CBD to the wrong, thermodynamically stable isomer if at all. It's likely the same for the acetates.

A polarimeter can easily show the extent of isomerization of crude THC, but I have no idea about the acetate rotations.

 

[Gray Wolf]

The only reasons I didn't do acetylation were 1- b/c of the safety hazard, you're supposed to use a hood pressurized with nitrogen gas... And 2- anecdotal reports of acetylation not being all it's cracked up to be, b/c cannabis doesn't act on the brain in the same manner as opium.

Not sure why Stark tossed in the inert atmosphere chamber other than to discourage folks from trying it. Acetic Anhydride is nasty stuff, but no more corrosive than any number of other acids and no more flammable than hexane.

The local university didn't teach the need for an inert chamber, when they taught our biochemistry student how to make aspirin out of salicylic acid using Acetic Anhydride and we haven't used one when we've made cannabis acetate.

Here is the MSDS information on fire and toxicology.

Section 5: Fire and Explosion Data
Flammability of the Product: Flammable.
Auto-Ignition Temperature: 316°C (600.8°F)
Flash Points: CLOSED CUP: 49°C (120.2°F). OPEN CUP: 51°C (123.8°F).
Flammable Limits: LOWER: 2.7% UPPER: 10.3%
Products of Combustion: These products are carbon oxides (CO, CO2).
Fire Hazards in Presence of Various Substances: Flammable in presence of heat.
Explosion Hazards in Presence of Various Substances:
Risks of explosion of the product in presence of mechanical impact: Not available. Risks of explosion of the product in
presence of static discharge: Not available.
Fire Fighting Media and Instructions:
Flammable liquid. SMALL FIRE: Use DRY chemical powder. LARGE FIRE: Use alcohol foam, water spray or fog. Cool
containing vessels with water jet in order to prevent pressure build-up, autoignition or explosion.
Special Remarks on Fire Hazards: Not available.
Special Remarks on Explosion Hazards: Not available.

Section 11: Toxicological Information
Routes of Entry: Dermal contact. Eye contact. Inhalation. Ingestion.
Toxicity to Animals:
WARNING: THE LC50 VALUES HEREUNDER ARE ESTIMATED ON THE BASIS OF A 4-HOUR EXPOSURE. Acute oral
toxicity (LD50): 1780 mg/kg [Rat]. Acute dermal toxicity (LD50): 4000 mg/kg [Rabbit]. Acute toxicity of the vapor (LC50): 1000
4 hours [Rat].
Chronic Effects on Humans: Causes damage to the following organs: lungs, mucous membranes.
Other Toxic Effects on Humans:
Extremely hazardous in case of skin contact (irritant), of ingestion, . Very hazardous in case of skin contact (corrosive).
Hazardous in case of skin contact (permeator), of eye contact (corrosive), of inhalation (lung corrosive).
Special Remarks on Toxicity to Animals: Not available.
Special Remarks on Chronic Effects on Humans: Not available.
Special Remarks on other Toxic Effects on Humans: Not available.

 

[Grant]

Wow, this is really impressive. It seems to be a lot more complex than using simple butane or ISO. Anyway, thankyou very much for this valuable information on using hexane at a solvent.

 

[BennyBlanco]

I use hexane for all my ISO extractions......

This is it frozen so much easier to work with for more pics check my albums I'm on a mobile right now...

 

[squarepush3r]

Here's some straight acetone oil I just got the lab test results back, this is the highest I have received yet, 65% THC

 

[Druminfected]

I use hexane for both extraction and cannabis alchemy. Because it is relatively expensive, it is usually more cost effective to do the initial extraction with another less expensive solvent and use a lesser volume of hexane to polish it afterwards.

My friend did a iso wash first, since like you said hexane is expensive. He soaked material for 12 hours and then filtered, and then evaporated the iso and was left with the oil. He then put hexane in the bowl of oil from iso evap, but ran into a problem. The oil isn't dissolving fully, like it usually does. Later on he wants to salt water technique to remove unwanted materials, but first is trying to dissolve the rest of the oil in hexane.

I seen a previous post that you suggest to another member that made RS oil to redissolve in ethanol, but my friend was trying to follow what you were saying to use a less expensive solvent and evap and then use hexane, but it's not dissolving now into hexane.

Should he set aside all the oil that didn't dissolve, and strain the rest? Then take the stuff that didn't dissolve and put that in ethanol? not sure what to do, but any feedback is greatly appreciated.

 

[Gray Wolf]

My friend did a iso wash first, since like you said hexane is expensive. He soaked material for 12 hours and then filtered, and then evaporated the iso and was left with the oil. He then put hexane in the bowl of oil from iso evap, but ran into a problem. The oil isn't dissolving fully, like it usually does. Later on he wants to salt water technique to remove unwanted materials, but first is trying to dissolve the rest of the oil in hexane.

I seen a previous post that you suggest to another member that made RS oil to redissolve in ethanol, but my friend was trying to follow what you were saying to use a less expensive solvent and evap and then use hexane, but it's not dissolving now into hexane.

Should he set aside all the oil that didn't dissolve, and strain the rest? Then take the stuff that didn't dissolve and put that in ethanol? not sure what to do, but any feedback is greatly appreciated.

Heat the hexane up for best solvent action.

Everything that dissolved in alcohol, won't redissolve in hexane, but you are trying to get rid of that stuff anyway.

It is not necessary to evaporate off the alcohol first, so you can redissolve in alcohol and then mix that with equal parts hexane and salt water.

 

[Druminfected]

Heat the hexane up for best solvent action.

Everything that dissolved in alcohol, won't redissolve in hexane, but you are trying to get rid of that stuff anyway.

It is not necessary to evaporate off the alcohol first, so you can redissolve in alcohol and then mix that with equal parts hexane and salt water.

Thanks so much for the reply, I got him to stop everything and just wait until you replied so thanks again.

Right now he filtered the hexane used to dissolve some of the ISO Oil, and removed a bunch of unwanted material. He also took a little of the ISO Oil and put it in some Ethanol to see if it would dissolve but it didn't.

I think i got confused from the alcohol you were mentioning from ethanol and iso. What do you advise about all the ISO Oil that didn't dissolve? That Oil that didn't dissolve in Hexane is seperated on some parch paper for now. Did you say to throw that oil on paper into the filtered hexane and with the rest of the oil and heated up to dissolve you are saying?
You did say that, "Everything that dissolved in alcohol, won't redissolve in hexane, but you are trying to get rid of that stuff anyway." so you mean that all that iso oil that didn't redissolve in Hexane is garbage material and should just be thrown away?

Thanks again GW!

 

[Gray Wolf]

Thanks so much for the reply, I got him to stop everything and just wait until you replied so thanks again.

Right now he filtered the hexane used to dissolve some of the ISO Oil, and removed a bunch of unwanted material. He also took a little of the ISO Oil and put it in some Ethanol to see if it would dissolve but it didn't.

I think i got confused from the alcohol you were mentioning from ethanol and iso. What do you advise about all the ISO Oil that didn't dissolve? That Oil that didn't dissolve in Hexane is seperated on some parch paper for now. Did you say to throw that oil on paper into the filtered hexane and with the rest of the oil and heated up to dissolve you are saying?
You did say that, "Everything that dissolved in alcohol, won't redissolve in hexane, but you are trying to get rid of that stuff anyway." so you mean that all that iso oil that didn't redissolve in Hexane is garbage material and should just be thrown away?

Thanks again GW!

I would take the part that didn't dissolve in hexane, and put it in hexane that is near boiling. If it doesn't dissolve, then it is trash.

It doesn't matter whether you use Isopropyl, Methanol, or Ethanol as the alcohol, it still works the same in an alcohol/hexane/brine swap.

Cannabinoids are non polar, so they go to the non polar hexane, while the polar alcohol goes with the polar water and other polar constituets.

 

[Druminfected]

I would take the part that didn't dissolve in hexane, and put it in hexane that is near boiling. If it doesn't dissolve, then it is trash.

It doesn't matter whether you use Isopropyl, Methanol, or Ethanol as the alcohol, it still works the same in an alcohol/hexane/brine swap.

Cannabinoids are non polar, so they go to the non polar hexane, while the polar alcohol goes with the polar water and other polar constituets.

I'm pretty sure I understand now, this will prove if I understand now. That ISO Oil that didn't evaporate, he took a sample of it and put it in ethanol and heated it up, and it did not dissolve but the ethanol is now yellow. So the stuff that didn't redissolve is crap the throw away, and the stuff to keep would be what is left over after it's evaporated, correct?


Thanks again GW, just want to be super sure, but once it's cemented in the brain it won't forget!

 

[Gray Wolf]

I'm pretty sure I understand now, this will prove if I understand now. That ISO Oil that didn't evaporate, he took a sample of it and put it in ethanol and heated it up, and it did not dissolve but the ethanol is now yellow. So the stuff that didn't redissolve is crap the throw away, and the stuff to keep would be what is left over after it's evaporated, correct?


Thanks again GW, just want to be super sure, but once it's cemented in the brain it won't forget!

Yes, the stuff that won't dissolve is the waste. The stuff leftover after the alcohol evaporates is the good stuff.

 

[Druminfected]

Yes, the stuff that won't dissolve is the waste. The stuff leftover after the alcohol evaporates is the good stuff.

Awesome, I passed the test!

The left over hung of iso oil that wouldn't dissolve in hexane, was heated like you said to close to boiling point about 122F, and was heated for more than and hour.

It looks like the hunk of Iso Oil turned from black to this nice caramel looking color, but that is the stuff that Never dissolved.

It looks so yummy, but if you say it's crap and leftovers then I won't disagree one bit GW. I'll try and post before and after pics of the Iso Oil before and after pics as well.

after putting in the hunk of iso oil into heated hexane to redissolve, ( I took out the non dissolved stuff) is it even worth the trouble of doing a salt water bath mix with the remaining hexane or just skip this process, and after the hexane evaporation it's fine?

Thanks again GW.


Update: here's those pictures.

After Heated for more than a hour and this is what did NOT dissolve.

Here's another picture but over exposure added about +1,+2 (to bad didn't take pic of before Iso Oil)

Here's some magnified pictures of the leftover nondissolved material.

 

[Gray Wolf]

You don't have to do a brine wash. It is primarily to take out water solubles and to remove the hydrophilic coating on some of the plant proteins, so they also fall out.

You will most likely need to do some ethanol washes of the hexane extraction, to purge the hexane fully.

Here is a link with more details:

http://skunkpharmresearch.com/getting-the-green-and-waxes-out-afterwards/

PS: As the saying goes, "Put it in your pipe and smoke it." That should eliminate any doubt as to whether it has any value.

Hope you also share the results on the good stuff.

 

[Druminfected]

You don't have to do a brine wash. It is primarily to take out water solubles and to remove the hydrophilic coating on some of the plant proteins, so they also fall out.

You will most likely need to do some ethanol washes of the hexane extraction, to purge the hexane fully.

Here is a link with more details:

http://skunkpharmresearch.com/getting-the-green-and-waxes-out-afterwards/

PS: As the saying goes, "Put it in your pipe and smoke it." That should eliminate any doubt as to whether it has any value.

Hope you also share the results on the good stuff.

Thanks so much for that site of yours, it's so informal and educational, I feel that if everyone got this correct knowledge, more people would be doing it, but a lot of people just go for the butane way. So much information to soak up, but I love it and read itover and over thanks again Mr. GW

On the site for purging HHO, you say 10 to 1 ratio, but not sure if it's 10 parts HHO to 1 Part Ethanol or vise versa

 

[Gray Wolf]

The solvent to cannabis oil ratio should be at least 10:1.

IE: 10 gms cannabis oil, 100 grams of solvent.

 

[JColtrane]

The solvent to cannabis oil ratio should be at least 10:1.

IE: 10 gms cannabis oil, 100 grams of solvent.

Constantly droppin' knowledge on us GW! Thanks Bro ... you've made me such a better hash maker!