Chloroform Extraction- First Attempt

gwpharms

gwpharms

Well-Known Member
20170317_215942.jpg
atrumblood said:
Your best bet is to use broken glass pieces, or you can even buy boiling stones from most laboratory supply websites.
Click to expand...
Careful under vacuum with boiling stones. Its debatable weather or not they work under reduced pressure. I say no.
But there kind of like a bunch of bb's or shrapnel. If the liquid does bump those boiling stones can possibly crack or chip your flask.
Stir is about all you can do. Or inert gas fine cappilary bubble works for me. I prefer only having fixed probes in my flask. Nothing that can smack the side wall
I just so happen to be dealing with this phenomenon right now. One probe is a thermometer and the other is creating the bubbles to break that surface area tension and prevent bumps. However It is inevitable bumps will happen no matter what you do as you can see by the splatter
 

Attachments

Last edited:
Fadedawg

Fadedawg

Well-Known Member
atrumblood said:
Bumping is when a liquid is heated past its boiling point and then suddenly boils all at once. It can cause the container to "bump" in the process and will likely splash some of the contents into your receiving flask, contaminating your distillate.
Click to expand...
What AB said. We also get it in the vacuum oven finishing off ethanol concentrates in a shallow casserole dish, so lay a sheet of glass over the top, to catch the splatter from the explosive bursts. It is easy to scrape off the glass, but makes "such a mess" in an unprotected oven.
 
atrumblood

atrumblood

Well-Known Member
gwpharms said:
View attachment 3912066
Careful under vacuum with boiling stones. Its debatable weather or not they work under reduced pressure. I say no.
But there kind of like a bunch of bb's or shrapnel. If the liquid does bump those boiling stones can possibly crack or chip your flask.
Stir is about all you can do. Or inert gas fine cappilary bubble works for me. I prefer only having fixed probes in my flask. Nothing that can smack the side wall
I just so happen to be dealing with this phenomenon right now. One probe is a thermometer and the other is creating the bubbles to break that surface area tension and prevent bumps. However It is inevitable bumps will happen no matter what you do as you can see by the splatter
Click to expand...

yeah, that is why I use glass beads. They are light enough that if they get thrown around they won't break anything. I wish I could afford such fancy equipment like a capillary tube. Or a heating mantle. I need to get a roto-vap eventually. That and a fraction collector.
 
gwpharms

gwpharms

Well-Known Member
atrumblood said:
yeah, that is why I use glass beads. They are light enough that if they get thrown around they won't break anything. I wish I could afford such fancy equipment like a capillary tube. Or a heating mantle. I need to get a roto-vap eventually. That and a fraction collector.
Click to expand...
You can make one out of a glass tube. Just heat to red hot and pull.
Heating mantle would be a good investment. A rotovap would be nice too but if your using it just to reclaim etoh, its way over kill.you can do that with a simple distillation setup for much cheaper
 
curious2garden

curious2garden

Well-Known Mod
Staff member
atrumblood said:
The advantage is for when you have high boiling points that you are trying to distill. The short path doesn't give the product time to solidify before reaching the receiving flask.

For example. The waxes and resins in cannabis are solid well above room temperature and in a normal distillation setup, they can clog the condenser and not even reach the receiving flask.

In addition to all of that, there will always be some mechanical losses when distilling. Some sticks to the sides of the condenser and distillation neck. The short path minimizes losses in that regard so that when working with small volumes like this, you don't lose as much product.
Click to expand...
@cannabineer
 
atrumblood

atrumblood

Well-Known Member
Its here! My precious!
20170324_200711.jpg

Finally I can finish this little project.
I will try to get it done over this weekend.

I have a friend with access to a gas chromatography mass spectrometer. I will be sending them a sample once I finish distilling the extract. Mainly I want to check cannabinoid content, as well as any residual chloroform.

If it checks out, I will be trying a hit.
 
cannabineer

cannabineer

Ursus marijanus
atrumblood said:
Its here! My precious!
View attachment 3912733

Finally I can finish this little project.
I will try to get it done over this weekend.

I have a friend with access to a gas chromatography mass spectrometer. I will be sending them a sample once I finish distilling the extract. Mainly I want to check cannabinoid content, as well as any residual chloroform.

If it checks out, I will be trying a hit.
Click to expand...
Find a way to run warm (40 to 50 C) condenser water. I don't think wax clogging will be an issue then, and your best cannabinoid fraction will be liquid enough at that temp. You will still need to do an alcoholic dewax step. Imagine my surprise when some of the wax codistilled. I argued with someone about that and got pwnt in my own field!
But ... wax does codistill. I am keen to try a fractional distillation of a large-enough amount of starting material.

I will go with magnetic stirring if I undertake that project. Boiling stones rely on having tiny gas-filled pores as nucleation sites. Glass beads have only promoted bumping in my experience. A mag stir bar beats bubbles into the still pot mix and ensures smooth ebullition.
 
atrumblood

atrumblood

Well-Known Member
cannabineer said:
Find a way to run warm (40 to 50 C) condenser water. I don't think wax clogging will be an issue then, and your best cannabinoid fraction will be liquid enough at that temp. You will still need to do an alcoholic dewax step. Imagine my surprise when some of the wax codistilled. I argued with someone about that and got pwnt in my own field!
But ... wax does codistill. I am keen to try a fractional distillation of a large-enough amount of starting material.

I will go with magnetic stirring if I undertake that project. Boiling stones rely on having tiny gas-filled pores as nucleation sites. Glass beads have only promoted bumping in my experience. A mag stir bar beats bubbles into the still pot mix and ensures smooth ebullition.
Click to expand...
These glass beads are not perfectly smooth, plus I add enough to cover the bottom of the flask.

So, when you talk about the dewax step. Are you talking about winterizing?
 
cannabineer

cannabineer

Ursus marijanus
atrumblood said:
These glass beads are not perfectly smooth, plus I add enough to cover the bottom of the flask.

So, when you talk about the dewax step. Are you talking about winterizing?
Click to expand...
I don't know about "winterizing". If it means what I think it does, then my dewax step does the job. I prefer more descriptive, less potentially concealing terms ... they stink to me of the sort of steganography that made chemists sit with other chemists and few others.
 
atrumblood

atrumblood

Well-Known Member
cannabineer said:
I don't know about "winterizing". If it means what I think it does, then my dewax step does the job. I prefer more descriptive, less potentially concealing terms ... they stink to me of the sort of steganography that made chemists sit with other chemists and few others.
Click to expand...

Yea I think it's the same thing.

Also about the running warm water through the condenser. I wonder if a fish tank heater would do the job
 
cannabineer

cannabineer

Ursus marijanus
atrumblood said:
Yea I think it's the same thing.

Also about the running warm water through the condenser. I wonder if a fish tank heater would do the job
Click to expand...
I don't think fish tank heaters go high enough. I'd use gravity flow system with warm water (from the house water heater) recirculating between a coupla coolers.
 
atrumblood

atrumblood

Well-Known Member
cannabineer said:
I don't think fish tank heaters go high enough. I'd use gravity flow system with warm water (from the house water heater) recirculating between a coupla coolers.
Click to expand...
Yea, I will try a few things. Worse case, I can just fill it with warm water and have both ends of the tubes held above the water line. The distillation should keep it plenty warm and insulated. Probably use a heat gun if I have to warm it a bit.

I'll figure it out. I will be doing it tonight if I get off work early enough.
 
cannabineer

cannabineer

Ursus marijanus
atrumblood said:
Yea, I will try a few things. Worse case, I can just fill it with warm water and have both ends of the tubes held above the water line. The distillation should keep it plenty warm and insulated. Probably use a heat gun if I have to warm it a bit.

I'll figure it out. I will be doing it tonight if I get off work early enough.
Click to expand...
The way i did it back in my lab days was by dropping the coolant flow. When i had it dialed in, I'd have a hot-water condenser and still got all the distillate condensed.
 
You must log in or register to reply here.
Top