Chloroform Extraction- First Attempt

cannabineer said:

Bing; that worked for me even with the stuff that wore a thin oily "condom" ... real bump beasts without the spinny thing

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In the undergrad labs we used to have to play musical chairs with the damn things. There was always one less than lab groups, sigh.

curious2garden said:

In the undergrad labs we used to have to play musical chairs with the damn things. There was always one less than lab groups, sigh.

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Grad lab was the land of milk and honey. i had my own BEAKERful of the things, including the compulsory big-ass cow magnet that is really a prank item. Spin one up and it'll stumble and head out the side of the flask.

cannabineer said:

Grad lab was the land of milk and honey. i had my own BEAKERful of the things, including the compulsory big-ass cow magnet that is really a prank item. Spin one up and it'll stumble and head out the side of the flask.

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Yeah I remember you guys, it's why we only RARELY invited you to parties.

curious2garden said:

Yeah I remember you guys, it's why we only RARELY invited you to parties.

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"Hey baby wanna be my electrophile?" That is a chemist asking for the old backside attack

cannabineer said:

"Hey baby wanna be my electrophile?" That is a chemist asking for the old backside attack

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Third string hun;
(1) Anesthesia residents,
(2) Pharmacology grad students,
(3) Chemists (we didn't even differentiate between types).

curious2garden said:

Third string hun;
(1) Anesthesia residents,
(2) Pharmacology grad students,
(3) Chemists (we didn't even differentiate between types).

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1) You won't feel this dear
2) you won't remember this dear
3) the physical chemists lie about getting physical

Ok, this did not go as planned.
The extract would not distill over, and I ended up charring it.
The theory is that there was not enough resin/terpenes to distill and what I had was mostly wax, fat, and chlorophyll.
I suspect this was due to the very poor quality of the weed I used.

All is not lost though. I feel like I can still recover something from this mess. Plus I learned something in the process.
I have redissolved the charred mess into more chloroform and added some water.
The plan is to distill off the chloroform, and then steam distill this to get the terpenes if any are there.
I have some more weed on the way and hopefully I will be trying this again very soon.

Pictures to follow.

Did you get it tested before distilling to see how potent it was?

I only have a small 500 ml soxhlet extractor that I use for chili and sometimes coffee but I must say I find this very interesting:

The idea of the initial extraction using the soxhlet is to extract nearly 100 % with minimal volume of solvent. The problem is that the process also extracts chlorophyll, waxes etcetera. Thats why you use the short path distillation in the second step to extract the THC from the nasty stuff. Is that correct?

MikeGanja said:

I only have a small 500 ml soxhlet extractor that I use for chili and sometimes coffee but I must say I find this very interesting:

The idea of the initial extraction using the soxhlet is to extract nearly 100 % with minimal volume of solvent. The problem is that the process also extracts chlorophyll, waxes etcetera. Thats why you use the short path distillation in the second step to extract the THC from the nasty stuff. Is that correct?

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Yes that is correct.

gwpharms said:

Did you get it tested before distilling to see how potent it was?

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I spaced completely. Must have been high or something.
I have a feeling that soxhleting would work if you had much more starting material.
I had my hot plate cranked at 550c for an hour and nothing came over. I started low and slowly cranked it up over the course of 2 hours.

plus.... it turned purple! WTF!!

atrumblood said:

I spaced completely. Must have been high or something.
I have a feeling that soxhleting would work if you had much more starting material.
I had my hot plate cranked at 550c for an hour and nothing came over I started low and slowly cranked it up over the course of 2 hours.

plus.... it turned purple! WTF!!

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What size of soxhlet would you say is reasonable to start with, how much plant material?

MikeGanja said:

What size of soxhlet would you say is reasonable to start with, how much plant material?

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I think that the 250mL one I used is fine for anything an ounce or lower. I am going to recommend not using the thimble though. The thimble made it so that the top of the weed was not getting submerged in the solvent. Tea bagging is the way to go since you can fill out the vessel while keeping things submerged.

atrumblood said:

I spaced completely. Must have been high or something.
I have a feeling that soxhleting would work if you had much more starting material.
I had my hot plate cranked at 550c for an hour and nothing came over I started low and slowly cranked it up over the course of 2 hours.

plus.... it turned purple! WTF!!

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What vacuum pressure we're you at?

MikeGanja said:

I only have a small 500 ml soxhlet extractor that I use for chili and sometimes coffee but I must say I find this very interesting:

The idea of the initial extraction using the soxhlet is to extract nearly 100 % with minimal volume of solvent. The problem is that the process also extracts chlorophyll, waxes etcetera. Thats why you use the short path distillation in the second step to extract the THC from the nasty stuff. Is that correct?

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Little to no fats or waxes with polar solvents. Just chlorophyll

gwpharms said:

What vacuum pressure we're you at?

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I don't have a guage. I will test it this week end by monitoring the temperature of water as I heat it under vacuum. I can figure out the max vacuum that way.

atrumblood said:

I don't have a guage. I will test it this week end by monitoring the temperature of water as I heat it under vacuum. I can figure out the max vacuum that way.

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You need to be able to measure the low Micron scale. And you will need to accurately Monitor and measure this. Very important. Short path of cannabis oil is very tricky and requires a lot of high end toys to be able to do it properly and efficiently. Like $3,000 vacuum pumps and $500 Micron gauges. A hot plate or water bath probably won't do the job either.
Next time if you are able to,
have your initial extract tested for potency so you know how much THC you're going after. There is other easier ways of purifying your extract if you just want pure THC. Maybe have terpenes tested and see if those are even worth going after and collecting in fractions. It sounds like a lot of work you are doing just to collect a few drops of terp Especially when you're doing small-scale. You should have had an initial extraction with little to no fat or wax and a lot of cannabinoids

gwpharms said:

You need to be able to measure the low Micron scale. And you will need to accurately Monitor and measure this. Very important. Short path of cannabis oil is very tricky and requires a lot of high end toys to be able to do it properly and efficiently. Like $3,000 vacuum pumps and $500 Micron gauges. A hot plate or water bath probably won't do the job either.

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Does the shortpath extraction process takes a lot of practicing before one master the method, or is it mostly a matter of investing in the right equipment to begin with?

MikeGanja said:

Does the shortpath extraction process takes a lot of practicing before one master the method, or is it mostly a matter of investing in the right equipment to begin with?

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Probably a little of both. Or a lot perhaps

I suppose its like anything,
Like say, you could paint your house with a rag on a stick and manage to get the job done but you'd be better off buying a quality brush and roller and even better with a sprayer.
And a well experienced craftsman would have more efficient technique and more tricks up his sleeve than a weekend do it yourselfer

gwpharms said:

You need to be able to measure the low Micron scale. And you will need to accurately Monitor and measure this. Very important. Short path of cannabis oil is very tricky and requires a lot of high end toys to be able to do it properly and efficiently. Like $3,000 vacuum pumps and $500 Micron gauges. A hot plate or water bath probably won't do the job either.
Next time if you are able to,
have your initial extract tested for potency so you know how much THC you're going after. There is other easier ways of purifying your extract if you just want pure THC. Maybe have terpenes tested and see if those are even worth going after and collecting in fractions. It sounds like a lot of work you are doing just to collect a few drops of terp Especially when you're doing small-scale. You should have had an initial extraction with little to no fat or wax and a lot of cannabinoids

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Yes, this is a lot of work for such a small amount. However, I am not doing this for profit. Right now I am exploring the science and trying to figure out the possibilities.
This is fun and exciting for me.

I may still be able to have this failed attempt tested. Since THC breaks down when heated strongly, I should in theory still be able to get a rough estimate of the starting levels of THC by quantitative analysis of the by products.

My plan for the next run will be pretty much the same. Only this time instead of trying to distill it in the short path. I will steam distill. This should bring over not only the terpenes, but also some of the other compounds that don't mix with water. Such as the cannabinoids. That may be an easy way to separate the compounds I want from things like chlorophyll.

As I continue to learn, and save up some cash, I will eventually have all the equipment I need to produce some good extracts. For now though, my goal is to research a way to efficiently extract small amounts. I may try to make Rosin and refine that.

Also here are those pictures I promised.



Here are some grow shots as well. About a month out. Probably longer.