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ismokecrystals
#1 Posted : 1/8/2010 10:56:32 PM

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I'm looking for a way to extract THC from vegetative material (leaves,buds) to yield a 98%+ purity

I'm not a fan of BHO because butane is highly flammable and traces are left in the honey oil.

I have considered doing a cold, quick wash of plant material with 99% ISO (dried with anhydrous MgS04)

What about d-limonene? Would I be able to separate the THC from the limo?
- I hear limonene does not evaporate clearly
- Can the cannabinoids be salted?
 

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ismokecrystals
#2 Posted : 1/8/2010 11:25:14 PM

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I want my end result to be like
 
Buster
#3 Posted : 1/9/2010 1:26:47 AM

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hi i would be interested in this also.

however would redisolving the bho in %99ipa then evap be a way to clean any impurities left over
from the butane?

im no chemist, just a thought.
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ismokecrystals
#4 Posted : 1/9/2010 5:29:25 PM

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Buster wrote:
hi i would be interested in this also.

however would redisolving the bho in %99ipa then evap be a way to clean any impurities left over
from the butane?

im no chemist, just a thought.


For some reason (not a chemist here either) the butane still contaminates the BHO even when filtered under vacuum. I don't know how to further purify it. I've heard hexane works pretty well for doing this stuff.
 
MagikVenom
#5 Posted : 1/9/2010 7:06:01 PM

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ismokecrystals wrote:
I'm looking for a way to extract THC from vegetative material (leaves,buds) to yield a 98%+ purity

I'm not a fan of BHO because butane is highly flammable and traces are left in the honey oil.

I have considered doing a cold, quick wash of plant material with 99% ISO (dried with anhydrous MgS04)

What about d-limonene? Would I be able to separate the THC from the limo?
- I hear limonene does not evaporate clearly
- Can the cannabinoids be salted?


It is impossible for butane to leave traces in your oil. Butane boils at about 33F so if you extraction is at any temp above that for a brief pereoid of time it is impossible for your contams to be butane. It would still be boiling at any temp above 33f

THC is not a alkaloid you can not salt it out.

Many sativa cannabis strains contain limonene and such. When you have weed with a citrus flavor or a pine flavor or a mango smell these are similar compounds. They also enhance the effects of THC so no reason to get rid of them. They vaporize very close to the temp of THC. I posted a document on this is another thread yesterday.

No such thing as a 98percent THC extraction in the kitchen my guess would be around 90percent is the best you will get and that is pretty good. If you want 98 percent pure learn advanced chemestry and find your self a fully equipped lab with all the bells and whistles.

Standard butane oil is way to much for most people as it is. I used to run a little bead along the edge of a rolling paper and fold it over then roll one up. I would fire this up with ten people after the second hit they were waving it off they had enough and these peps were full time medical usersWink

Of course no one should use cannabis or its extracts without a legit medical reason. It is illegal in many places check your local laws.

Peace
MV
 
SnozzleBerry
#6 Posted : 1/9/2010 10:51:15 PM

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MagikVenom wrote:
It is impossible for butane to leave traces in your oil. Butane boils at about 33F so if you extraction is at any temp above that for a brief pereoid of time it is impossible for your contams to be butane. It would still be boiling at any temp above 33f

THC is not a alkaloid you can not salt it out.

Many sativa cannabis strains contain limonene and such. When you have weed with a citrus flavor or a pine flavor or a mango smell these are similar compounds. They also enhance the effects of THC so no reason to get rid of them. They vaporize very close to the temp of THC. I posted a document on this is another thread yesterday.

No such thing as a 98percent THC extraction in the kitchen my guess would be around 90percent is the best you will get and that is pretty good. If you want 98 percent pure learn advanced chemestry and find your self a fully equipped lab with all the bells and whistles.


Standard butane oil is way to much for most people as it is. I used to run a little bead along the edge of a rolling paper and fold it over then roll one up. I would fire this up with ten people after the second hit they were waving it off they had enough and these peps were full time medical usersWink

Of course no one should use cannabis or its extracts without a legit medical reason. It is illegal in many places check your local laws.

Peace
MV


Thanks for the bolded section especially MV, you're exactly correct in this post. If you want purity of that level make bubble hash or pressed kief hash using. If you truly want high percent thc oil with no risk of toxic contams use D-limonene. Soak your material in there for several days, filter, smoke, and prepare to be baked as all hell.
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Phlux-
#7 Posted : 1/10/2010 4:17:41 AM

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30 second hot naptha wash works well.
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SnozzleBerry
#8 Posted : 1/10/2010 4:53:21 AM

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Here's the section from "Run From the Cure: The Rick Simpson Story" that deals with making Hash Oil using Naptha. It's a great method for extracting, but not if you're looking for non-toxic tek.

The extraction is detailed starting at 1:50
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ismokecrystals
#9 Posted : 1/10/2010 5:09:36 AM

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Sam the Skunkman (breeder of Skunk) did a GC/MS on various BHO samples and all of them were said to be contaminated by Butane.

What contaminates exist in a kitchen extraction? Why can I not get a 98% pure sample with a NP solvent wash?
 
MagikVenom
#10 Posted : 1/10/2010 5:35:22 AM

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ismokecrystals wrote:
Sam the Skunkman (breeder of Skunk) did a GC/MS on various BHO samples and all of them were said to be contaminated by Butane.

What contaminates exist in a kitchen extraction? Why can I not get a 98% pure sample with a NP solvent wash?


They must not have been allowed to dry in a thin film in a large flat container. And even if they did contain small amounts of butane no big deal as butane will burn when you smoke it. Butane exist as a gas at atmospheric pressure at any temp above 33f so it would have to be a gas trapped in a solid ie the oil. It is very easy to separate gases from liquid solids.

If you are that concerned about butane better chuck that Bic lighter its contaminates everything you ignite with it.

I guarantee a naptha extract will contain far more contams than a butane extraction.

Just my tek but I will never be rinsing my clean butane oil with nastie naptha.

Of course if you run a GC/MS on anything you will find traces of everything that substance has been in contact with in trace amounts but the amounts are negligible.

I am telling you this not from theory but years of actual extractions and experiments on many many pounds of medicinal cannabis.

Look up the properties of pure THC it is unstable and can not be stored.

Oh yeah You should chill your butane and biomass as cold as you can get them before extraction. This locks up water soluble contams in the biomass as they freeze in place along with any small amount of water still present in plant material.

It also prevents your butane from boiling off when you are working with it. If you do not chill the butane it will boil off RAPIDLY until it cools the container it is in below the boiling point of butane.

Edit I was just looking at the pix you posted "I want mine to look like this" I can see the gas bubbles trapped inside perhaps that is the butane contam. Mine has no bubbles and is nearly completely clear slightly yellow but lighter than Honey not as dark as that and no gas bubbles.

Butane is also a natural part of every breath you take as it is always present in the air you breathe.

Good luck DudeSmile

Peace
MV
 
Touche Guevara
#11 Posted : 1/10/2010 6:35:50 PM
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ismokecrystals wrote:
Sam the Skunkman (breeder of Skunk) did a GC/MS on various BHO samples and all of them were said to be contaminated by Butane.

What contaminates exist in a kitchen extraction? Why can I not get a 98% pure sample with a NP solvent wash?

Got a source for this?

Butane combustion in the presence of oxygen (ie, ideal conditions) produces water and carbon dioxide. However, under limited oxygen conditions it will produce carbon monoxide, which of course is poisonous. Also, hash oil is often vaped and not burned, and vaporized butane in one's lungs can't be good, especially in the case of a medicinal user.

SWIM has seen videos wherein the producer will point the extraction tube into a vessel of hot water, which seems to instantly evaporate the butane. The oil floats on top and is scooped up and allowed to dry. This seems like a more reliable way to purge any and all butane, and I can't imagine it would take much longer to dry a bit of watery oil than it would to correctly evap BHO the normal way.
 
Oncewas
#12 Posted : 1/10/2010 10:10:40 PM
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Acetone and then some sort of binary solvent in a chromatography column, is the only way I can think of to get it that pure. Even BHO/ISO has other chemicals in it other than thc.
 
biopsylo
#13 Posted : 1/11/2010 1:47:12 AM

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proper ice water thc extraction is the biggest improvement in hashish making in 5000 years. there are many copy cats for this method.
To get to 98%, yes a solvent would need to be used. but you can get to 85-90%++ with just icewater and agitation + filtration. get rid of bulk vegetable matter first, and if it is good cannabis, this is prob as strong at u would need anyway.
I think the first guy in B.C. to make 98% "budder" used the finest bubble hash, then purified this further with ethanol. this way the product can remain Organic. (this is important for many clients of compassion clubs). maybe Fractal has come across some of this budder in vancouver/?? i havnt been there in a while, but i would love to try some!!
 
burnt
#14 Posted : 1/11/2010 6:26:44 PM

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Quote:
ismokecrystals wrote:
Sam the Skunkman (breeder of Skunk) did a GC/MS on various BHO samples and all of them were said to be contaminated by Butane.


A good way to solve this problem is redissolve the residue in another less toxic solvent like ethanol a reevaporate. This removes trace amounts of organic solvent that get trapped in the oil droplets of THC. Butane hexane naptha all these solvents are most likely retained in the hash oil unless removed this way or with extensive heating and stirring (which would cause degradation and is not recommended). Butane is actually the best though because its the most volatile.

Quote:
I guarantee a naptha extract will contain far more contams than a butane extraction.


It will extract more impurities. Butane is more selective. It depends on the naptha though if there are more aromatic hydrocarbons it will extract more then cannabinoids.

Quote:
Of course if you run a GC/MS on anything you will find traces of everything that substance has been in contact with in trace amounts but the amounts are negligible.


this depends totally on the quantity. but again butane is the best and least likely to contaminate compared to naptha hexane etc.

Quote:
What contaminates exist in a kitchen extraction? Why can I not get a 98% pure sample with a NP solvent wash?


You need to do chromatography or synthesis to get greater then 95% THC. Even with synthesis chromatographic clean up is needed. Anyone claiming they can get THC this pure without using chromatography has never analyzed their material.

All cannabis contains other cannabinoids which WILL always be present with THC unless some chromatographic separation is used. Depending on the cannabis these ratios can vary a lot. Most likely contaminants are cannabigerol, cannabichromene, cannabidiol, cannabinol (depending on freshness), tetrahydrocannabivarin and their corresponding acidic cannabinoids (again depending on freshness or if plant material was heated).





 
Oncewas
#15 Posted : 1/11/2010 8:21:53 PM
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What would be the binary solvent mixtures used for such chromatographic seperation?

This would certainly have my friend buying a column and practicing in the near future.
 
burnt
#16 Posted : 1/12/2010 9:04:19 AM

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combinations of hexane and lesser amounts of ethyl acetate over silica usually flash chromatography.
 
richierich_931
#17 Posted : 8/13/2010 3:09:17 PM

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SWIM made some cannabutter and was curious if anything was left in the material.
He filtered out plant material then added acetone and let sit.
The next morning there were crystalline floaties on top of the solution, as well as a separation of white (fats?) and green (chlorophyll?).

Floatie material is active...





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