Chloroform Extraction- First Attempt

atrumblood

atrumblood

Well-Known Member
I have been wanting to try extracts for a while now, and I have been doing a lot of reading on the topic.
While I would love to be able to do CO2 or butane extraction, I do not have the equipment needed to do that.

Ethanol, and Isopropyl Alcohol are the most common method of extracting cannabis, I have opted to try something different. Something that I don't think anyone here has tried before.

I am going to be doing the extraction using chloroform (Trichloromethane).
The chloroform I am using was made by my self and distilled to remove any impurities.

The reason I want to use chloroform is because of its properties as a solvent.
It has a low boiling point which will allow a thorough extract of the cannabis.
It has a low affinity towards chlorophyll and thus the extract will contain a lot less, which leads to a cleaner better tasting product.
It has a high vapor pressure which means it will not linger in the product, and will evaporate away.

The methods I will be using include refluxing via soxhlet extractor, distilling off the chloroform for reuse, then using a vacuum chamber to force any residual chloroform out of the product. Last I will be vacuum distilling the product to isolate the thc , waxes, and tannins using a short path distillation apparatus.

If all goes well, I should be left with a clear amber extract ready to smoke.

I will be posting my progress here.

I am thinking that this weekend I will begin the process.
 
atrumblood

atrumblood

Well-Known Member
I decided to make more chloroform last night to make sure I had enough to do this extraction.

I will be using about 26 grams of bud that I have ground up and decarbed. From what I have read on the net (correct me if I'm mistaken) I should be able to get about 10 grams from that 26 grams of starting material. Though it will most likely be closer to 5 grams

I should be able to begin the extraction tonight after work.

I will include pictures as well as temperatures and measurements for those who are curious.

20170309_193020.jpg
 
atrumblood

atrumblood

Well-Known Member
I just started the extraction a few hours ago. Sadly the claims that chloroform has a low affinity towards chlorophyll have been greatly exaggerated.

The extraction turned green instantly. Oh well, it was a chance I took. No harm done, just means the vacuum distillation afterwards is definitely going to be needed to remove all that chlorophyll.

20170312_222301.jpg 20170312_224802.jpg 20170312_230921.jpg
 
ttystikk

ttystikk

Well-Known Member
atrumblood said:
I have been wanting to try extracts for a while now, and I have been doing a lot of reading on the topic.
While I would love to be able to do CO2 or butane extraction, I do not have the equipment needed to do that.

Ethanol, and Isopropyl Alcohol are the most common method of extracting cannabis, I have opted to try something different. Something that I don't think anyone here has tried before.

I am going to be doing the extraction using chloroform (Trichloromethane).
The chloroform I am using was made by my self and distilled to remove any impurities.

The reason I want to use chloroform is because of its properties as a solvent.
It has a low boiling point which will allow a thorough extract of the cannabis.
It has a low affinity towards chlorophyll and thus the extract will contain a lot less, which leads to a cleaner better tasting product.
It has a high vapor pressure which means it will not linger in the product, and will evaporate away.

The methods I will be using include refluxing via soxhlet extractor, distilling off the chloroform for reuse, then using a vacuum chamber to force any residual chloroform out of the product. Last I will be vacuum distilling the product to isolate the thc , waxes, and tannins using a short path distillation apparatus.

If all goes well, I should be left with a clear amber extract ready to smoke.

I will be posting my progress here.

I am thinking that this weekend I will begin the process.
Click to expand...
Talk about putting you to sleep! Lol
 
Fadedawg

Fadedawg

Well-Known Member
atrumblood said:
I just started the extraction a few hours ago. Sadly the claims that chloroform has a low affinity towards chlorophyll have been greatly exaggerated.

The extraction turned green instantly. Oh well, it was a chance I took. No harm done, just means the vacuum distillation afterwards is definitely going to be needed to remove all that chlorophyll.

View attachment 3905178 View attachment 3905179 View attachment 3905180
Click to expand...
Oops! A perfect example of how practical experience trumps scholarly research and advice!

Good job! Thanks for sharing!
 
ttystikk

ttystikk

Well-Known Member
atrumblood said:
Just finished the extraction. It is a nice dark green. Almost black looking. The next step when I wake up will be distilling the chloroform out for reuse. Then I will setup for Vacuum distillation of the final product.View attachment 3905197
Click to expand...
To avoid excess chlorophyll extraction, those who use isopropyl alcohol as the solvent do a 'quick wash' to avoid letting the solvent sit too long on the material. Such an approach might be useful with this solvent as well.
 
MikeGanja

MikeGanja

Well-Known Member
atrumblood said:
I am a chemist as a hobby, and I am currently majoring in chemistry in college. Chloroform is about the easiest thing to make for me.
Click to expand...
How do you make the chloroform? As a non chemist I only know about the haloform reaction with acetone and bleach. Would that be good enough for extractions? Unfortunately you can not buy chloroform over the counter in my part of europe, so you have to make it yourself.

Looking forward to read more of your experiments!
 
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atrumblood

atrumblood

Well-Known Member
MikeGanja said:
How do you make the chloroform? As a non chemist I only know about the haloform reaction with acetone and bleach. Would that be good enough for extractions? Unfortunately you can not buy chloroform over the counter in my part of europe, so you have to make it yourself.

Looking forward to read more of your experiments!
Click to expand...
Yes that is how I make it. I use about 75mL of acetone for a bottle of bleach that is 8.25%. I shake it and let it sit for about a day to settle out, then I separate it.

Once separated, it should be distilled at least once to get rid of all the other stuff that may have been in your bleach and acetone.
 
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BobCajun

BobCajun

Well-Known Member
If you moisten the plant material somewhat, like half the weight in water, the solvent won't be able to either be absorbed by the material, wasting solvent, or get to the chlorophyll and other leaf crud. I did it using MEK, which doesn't mix with water, and it turned out well. There was some green, I did press on it to squeeze out the resin, but with no squeezing it should be lighter. The consistency was unlike BHO because it would flow at room temp like a thick paste. Maybe there was less wax than with BHO. Quite potent too. Anyway something to try sometime.
 
natureboygrower

natureboygrower

Well-Known Member
atrumblood said:
I just started the extraction a few hours ago. Sadly the claims that chloroform has a low affinity towards chlorophyll have been greatly exaggerated.

The extraction turned green instantly. Oh well, it was a chance I took. No harm done, just means the vacuum distillation afterwards is definitely going to be needed to remove all that chlorophyll.

View attachment 3905178 View attachment 3905179 View attachment 3905180
Click to expand...
were you able to fit all 26 grams of material into your soxhlet thimble?
 
atrumblood

atrumblood

Well-Known Member
BobCajun said:
If you moisten the plant material somewhat, like half the weight in water, the solvent won't be able to either be absorbed by the material, wasting solvent, or get to the chlorophyll and other leaf crud. I did it using MEK, which doesn't mix with water, and it turned out well. There was some green, I did press on it to squeeze out the resin, but with no squeezing it should be lighter. The consistency was unlike BHO because it would flow at room temp like a thick paste. Maybe there was less wax than with BHO. Quite potent too. Anyway something to try sometime.
Click to expand...

Thanks, I plan on giving this another try when I harvest my next grow. Last time I got around 3 oz of frosty trim. I think the extra volume will give me much more extract to work with. As it stands now, I only ended up with about 5g of crude product that I will need to refine. I probably won't be able to finish refining it until this next weekend when I receive my short path distillation apparatus.
 
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