Oil extraction

Good evening all,

I have a question for the chemistry geeks out there, or anyone with oil making experience...

I've been making green hash oil for a while now using a soxhlet extractor with allihson condenser. My patients have given it rave reviews, though I've thought about ways of making more potent stuff... My understanding of green oil is that it's not as potent as Butane Honey oil, but I haven't stepped up to Butane yet.

Instead, I've found a recipe for cold extraction... Run fresh, below freezing ethanol (I use only 191-proof everclear) over material in a strainer that's also been frozen, and don't allow it to soak. I have ~5 liters of everclear waiting for distillation which I'm currently doing, each with a beutiful amber color. And this is where my funny question comes into play:

Normally, making green oil, I put my flat bottomed boiler directly onto an electric stove element. This time around, however, I'm using the soxhlet as a distiller, and have the flask in a pot of near boiling water, 195-200F. But as the stuff boils down, it turns RED. Dark red, like blood. It's freaky.

I figured this means I've done something wrong, or it's what I should expect. I've read about red oil, and how it's precipitated out of a gas mixture using HCl and NaOH, (which I refuse to touch, I'm not putting nasty chemicals in my oil for patients), but I'm hoping I don't have an impurity or something that's changing the pH off or something?

Should I expect red stuff, should it be smokable, or should I just stick to my regular ethanol/green oil extraction method? I have no qualms throwing this batch out. I've only used 70g of trim leaf for this experiment, and have another pound and half to use.

Your suggestions are appreciated, or alternate forum suggestions.

Pictured, my setup: $13 electric hot plate, water pot, flat bottom boiling flask, 500ml Soxhlet extractor, alihson condensor, siphon tube through the middle, cooled from a 5gal bucket with an old dorm room fridge element, recircuilating pump to cool the condensor. 2x 6" fume vents off picture to the right.
m0015345.jpg
Pictured, ~4g of the 'red' oil final product (it's very thick). Should have another 12-16g on the way.
m0015350.jpg
 
I thought we harvested about on time... maybe we were late, not sure. It was our first. They were less than 50% amber, mostly cloudy/milky from what I remember. Unfortunately, most of the memories of that was all the time we spent trimming the ****ers :wall:
 

Buddreams

Active Member
i can't really comment on the original post, but I wanted to know what kind of collection procedure you used to collect the oil from the evaporation vessel and put into the small vial. I personally use the butane extraction and it produces a transparent liquid that can harden to a thick resin that even the sharpest razor blade has a hard time separating it from glass.
 
I use hot water for pouring my oils. Boil some water on the stove, and before it cools, stick your collection vessel into the hot water (obviously you don't want to get hot water into the vessel) and once it's heated up and softened, pour it into whatever other container you want.

It may be that I simply have lower-purity oils due to my extraction method (I would love to be able to tell THC content %), I'm not sure, but they seem to pour fine this way. If I don't, yeah, it's a pain to transfer, they typically thicken close to just below boiling. Room temp, the stuff in the vial isn't going anywhere unless I poke at it.... Hope that helps...
 

The Bushman

Member
Method #1

Hash Honey Oil Extraction With Supercritical Butane

For those of us who never quite got over the loss when fine-quality hash oil disappeared from the market, and for cannabis connoisseurs of all ages everywhere, it would be my honor to write up what has to be the easiest, highest-yielding and most selective cannabis oil extraction method available to date.

This method has its basis in a fascinating industrial extraction method known as Supercritical Fluid Extraction. It uses totally over-the-counter butane gas (8 oz can, camping supply store, ~US$4.50) as the extraction solvent, and requires nothing even remotely suspicious or difficult to purchase. The only other thing needed is about $2.00 worth of PVC pipe: a section 1.5 (one and a half) feet long and 1 & 3/4" diameter (outer diameter I believe), and two end caps. Threaded PVC is not necessary.

For reasons not yet clear to those of us investigating these things "unofficially," butane (and perhaps other gas/solvents with similar ultra-low-boiling properties) selectively solvate the desirable fraction(s) of cannabis oils, pulling out only a beautiful amber "honey oil" and leaving the undesirable vegetative oils, waxes, chlorophyll, etc. behind in the plant matter. Even unsmokable shade leaves produce a wonderfully clean and potent gold oil with this method. I have every reason to suspect that this would work splendidly to extract a super-strong and tasty oil from gross, unpalatable "schwag" commercial pot too, and of course, the better grade of herb you put it in, the better the resulting oil.

Method
Method
In one of the PVC end caps, drill a single small hole in the center. This hole should be correctly sized to snugly receive the little outlet nozzle of your butane can.

In the other end cap, drill a group of 5 or 6 small holes clustered in the center (like a pepper shaker).

After putting a piece of paper towel or coffee filter inside it for filtration, put the end cap with several holes on one end of the pipe. Push it on there real tight. This is the bottom.

Fill the pipe up with plant matter that has been pulverized into a coarse powder. You want it filled, but not packed down. (Full pipe estimated at 1.5 oz capacity, but this is a guess. I did not weigh it.)

Place the top end cap on the pipe. Again, push it on as securely as you can by hand.

Find a location outdoors with a decent breeze. You want these butane fumes to be quickly carried away. Seriously.

Mount the pipe (single hole-side up) over a vessel that can hold 300mL+. Beakers are perfect. A lab stand and clamp are ideal for the mounting, but a regular shop clamp or anything that can hold it sturdily is fine. (Avoid metal if you can, to reduce the chance of sparks.) Position the bottom end of the pipe immediately over (1-2") the receiving vessel to eliminate splatter loss.

Turn the butane gas can upside down and dispense the gas into the pipe via the single top hole. A whole 8-oz can takes about 10-12 seconds to evacuate. Be brave, swift, and careful. A spark at this moment would spell disaster since you have basically created an incendiary explosive device that is leaking.

When you've exhausted the can into the pipe, back off to a nice distance and let it do its thing.

The butane moves down the pipe, extracting the cannabis as it goes. When it gets to the bottom (~30 seconds after dispensing), it begins to drain into the receiving vessel. Notice the pale, glowing yellow-green-gold hue of the extract. It is obvious no chlorophyll was pulled out of the herb

Over approximately five to eight minutes, the butane extract will finish draining from the pipe to the receiving vessel. Maintain caution with the pipe, however, since there is a lot of residual butane still evaporating from within the pipe (notice the stream of fumes coming from the top hole). When it slows down to a drop every few seconds, you can tap on the top hole with your finger and it will help push the last of the liquid butane out (or one can gently blow into the top hole to do the same thing). Remember, NO SMOKING, unless you wish to immolate yourself in grand fashion.

Being very low-boiling and volatile, the collected butane will likely begin boiling at ambient temperature. The receiving vessel will gradually frost up as the butane cools it down, slowing down its rate of evaporation, but you can speed this up again simply by holding it in your hands. A better way is to set it in a saucepan containing a little bit of warm water. Watch the butane start bubbling madly with the increase in temperature and marvel at its low boiling point. Again, be doing this outdoors with a nice breeze! It takes about 20 minutes or so to allow the butane to evaporate, or quicker if you help it along. You are left with a deep amber, almost orange oil of amazing purity.

The best way to collect and store the oil is probably to let all of the butane evaporate off and then redissolve the oil in some anhydrous or high-% alcohol, and then pour this into a vial and let it sit out for a day or two to allow the alcohol to evaporate. Trying to transfer the oil into a small container while it is still solvated by the butane is too risky. I learned the hard way about this, thanks to the volatile temperament of butane. I had filled a vial almost all the way to the top and was preparing to drop those last couple drops in, so that cleverly, I could let the last of the butane evaporate from the vial and the oil would all be neatly contained. But when the last drop hit the mother lode in the vial, it changed the temperature of the solution in the vial upward by a hair and it all "superboiled" out of the vial and onto my fingers, which of course startled me and caused me to drop the vial. I suggest dissolving it in alcohol as I mentioned above. If you can get pure or 99% isopropanol (isopropyl), use it, because THC's photosensitivity reportedly does not occur in isopropanol.

The final product is a deep yellow-amber oil of the highest quality, incredibly pure and potent. I remember well some of the prime "honey oil" hash oils that hit the market in the late 1970s, and this stuff stands up to (if not exceeds) any of them. It's amazing how this method extracts only the good fraction and leaves the junk in the weed. But that's exactly what it does. Note also that this oil has a somewhat higher melt/vaporization point than traditional hash oils; the traditional dispensing method (dipping a needle or paper clip in, getting some goop on the end, and warming it with a flame to get it to drip off into your bowl) still works with this stuff, but it seems you have to be more careful with it because it doesn't heat to liquid state as quickly or in the same manner, and it can more easily be allowed to burn up on your needle. So be careful.

Those who prefer a tincture-like preparation can of course thin the product a little with a bit of warm high-percentage alcohol like Everclear or 90-whatever-% isopropyl, then drop it onto buds or let a joint absorb some, then let the alcohol evaporate. I also observed that unlike hash oil derived from traditional methods, this product is not immediately soluble in room-temp alcohol; it needed to be warmed before it dissolved fully.

Method #2

Extraction of THC Oil from Cannabis

"If you ever had to think twice about lighting up a joint for fear of someone smelling it. If you were ever forced to blow the smoke out a window and pray you don't reek of weed. If you ever had to sneak around and couldn't enjoy a good buzz..."

This article will describe, in detail, a technique of extracting the essential oils from hemp. The final product will be a dark, oily liquid that contains 70+% pure THC. The following steps require nothing more than simple, easy to find materials and a little time.

Advantages of THC oil:
Advantages of THC oil
• No hot, harsh smoke to irritate your lungs
• No tar to stain your teeth and fingers
• Very little smell
• 5 times as much THC in bloodstream
• No carcinogens to give you cancer


Materials you'll need for extraction:
Materials you will need for extraction
• A glass jar with a watertight lid (widemouth Mason jars work great)
• A metal measuring cup with handle (2 cup capacity recommended)
• Bottle of 190 proof grain alcohol (Everclear brand is perfect)
• Any quantity of pot, any strength (from a gram up to a few ounces)
• A 1' X 1' piece of sturdy cloth (t-shirt material works fine)
• An eye-dropper bottle (contact lens type bottles work great)
• The use of an ELECTRIC stove and its overhead fan

Step 1
Step 1
You'll need to chop up your weed and pick apart the buds until it looks like grass clippings. Remove any seeds, they have their own oils which we don't want. Dump the powdered pot into the mason jar and pour in just enough grain alcohol so the weed particles float freely in the mixture. Place the lid securely on the jar and shake a few times.

Let this mixture sit for a few hours, shaking it every once in a while. The alcohol should have turned a dark green color and when shaken should form colorful, oily bubbles on top.

Place the sturdy cloth over the metal container and press the cloth down to form a funnel. Carefully pour the contents of the mason jar onto the cloth which is in the metal cup. Make sure to get most of the weed particles out of the jar. Gather up the edges of the cloth and squeeze the remaining liquid out of the lump of weed into the metal cup.

Step 1a
Step 1a
You should now have a quantity of dark green liquid in your metal measuring cup. It is possible to extract more THC oil from the remaining pot. I recommend performing Step 1 a second time immediately after completing it the first time. No sense throwing away the good stuff. Dump the pot from the cloth back into the mason jar and repeat step 1. You now have twice as much liquid in your metal cup upon repeating the first step.

Step 2
Step 2
Be sure to use an electric stove in this step! (If you don't have one, read Step 2a)

Take the metal cup containing the green liquid over to the stove. Turn one of the electric eyes on LOW setting and place the metal cup on that burner. I highly suggest using the fan over the stove to remove the alcohol vapors during this entire step. Watch the liquid closely. It should only boil slightly, never raise the burner temperature above MEDIUM LOW. We need the liquid to cook down until it's slightly thick. This may take some time but be patient.

Once the liquid starts to thicken and turn darker, remove it from the heat. Never let it get too thick or it'll be too difficult to work with. If you do accidentally make it too thick, just add a small quantity of the grain alcohol to the metal cup and swirl it around till it's thinner.

Let it cool down to room temperature inside the metal cup. It should be runny enough to be poured into the eye-dropper bottle easily. You now have your final product: THC oil. It's necessary to have some grain alcohol left in the resulting liquid so it's easy to work with. This will not affect the potency of the oil.

Step 2a
Step 2a
This part is for the people with gas stoves. Do not use a gas stove to cook down alcohol! The vapors will explode! You'll have to have patience to complete this step. To get a final product just put the metal container in a place where it won't be disturbed. The alcohol will have to evaporate on its own. If at all possible keep it in a slightly warm area with decent ventilation. It may take days.

Once it's evaporated test to see if it's too thick. If it is, pour a small amount of grain alcohol in the metal cup and mix. Pour the liquid into your eye-dropper bottle.


Hope this helps.
 

MAc DRe

Well-Known Member
NEVER use PVC for oil extraction. The butane takes some of the chemicals out of the PVC and put it in your hash oil collection dish and those don't evaporate. In my opinion the only material for an extraction tube is glass or stainless steel. What I use to extract, the butane oil is a glass tube about three feet long and an inch thick glass( i got it at a headshop for like 100) it looks like a huge dildo and thats what you can say it is if you place ever gets raided, because just having an extraction device like that in California is a Felony. Also i have to say this about safety of making Butane hash oil, always do it outside or in a super well ventilated room or the butane will build up in the room and it take one spark to make that room a bomb. Hash oil is the best for of Medicine i have found, just always be smart and safe when making it. peace out:weed::weed:bongsmilie
 
Hi,

I'm not going to touch butane. I've decided to stick with Ethanol, after doing some reasearch. I'm getting more sugars because ethanol is is semi-polar, and can disolve both the sugars (chlorophyl, etc, polar) and the THC (non-polar). Even when cold, it was still extracting some sugars, though not as many. That said, I found I could use isopropyl, as it is less polar than ethanol, but still not truly non-polar. Butane, as the common solvent, is non-polar, and doesn't extract sugars, hence why it comes out so amber. I'd rather use food-grade items in the end.

FYI, butane extraction as listed is NOT super critical. The critical point for Butane is +152 deg. C, @ 37-something bar (http://encyclopedia.airliquide.com/encyclopedia.asp?GasID=8). It just boils at -0.5C at sea level, which causes the sugars to freeze and be really difficult to disolve.

That said, has anyone heard of non-supercritical CO2 extraction? CO2 is a very good, safe non-polar solvent, and you can get it liquid at ~250psi room temperature (my understanding). Saw a video of a guy extracting orange peel oil by putting dry ice on top of a chunk of peel in a pressure-capable vial, as the pressure built up, it turned to liquid and extracted oil. Ideas?

Cheers,
 

GreenThumbSucker

Well-Known Member
Method #1

Hash Honey Oil Extraction With Supercritical Butane

For those of us who never quite got over the loss when fine-quality hash oil disappeared from the market, and for cannabis connoisseurs of all ages everywhere, it would be my honor to write up what has to be the easiest, highest-yielding and most selective cannabis oil extraction method available to date.

This method has its basis in a fascinating industrial extraction method known as Supercritical Fluid Extraction. It uses totally over-the-counter butane gas (8 oz can, camping supply store, ~US$4.50) as the extraction solvent, and requires nothing even remotely suspicious or difficult to purchase. The only other thing needed is about $2.00 worth of PVC pipe: a section 1.5 (one and a half) feet long and 1 & 3/4" diameter (outer diameter I believe), and two end caps. Threaded PVC is not necessary.

For reasons not yet clear to those of us investigating these things "unofficially," butane (and perhaps other gas/solvents with similar ultra-low-boiling properties) selectively solvate the desirable fraction(s) of cannabis oils, pulling out only a beautiful amber "honey oil" and leaving the undesirable vegetative oils, waxes, chlorophyll, etc. behind in the plant matter. Even unsmokable shade leaves produce a wonderfully clean and potent gold oil with this method. I have every reason to suspect that this would work splendidly to extract a super-strong and tasty oil from gross, unpalatable "schwag" commercial pot too, and of course, the better grade of herb you put it in, the better the resulting oil.

Method
Method
In one of the PVC end caps, drill a single small hole in the center. This hole should be correctly sized to snugly receive the little outlet nozzle of your butane can.

In the other end cap, drill a group of 5 or 6 small holes clustered in the center (like a pepper shaker).

After putting a piece of paper towel or coffee filter inside it for filtration, put the end cap with several holes on one end of the pipe. Push it on there real tight. This is the bottom.

Fill the pipe up with plant matter that has been pulverized into a coarse powder. You want it filled, but not packed down. (Full pipe estimated at 1.5 oz capacity, but this is a guess. I did not weigh it.)

Place the top end cap on the pipe. Again, push it on as securely as you can by hand.

Find a location outdoors with a decent breeze. You want these butane fumes to be quickly carried away. Seriously.

Mount the pipe (single hole-side up) over a vessel that can hold 300mL+. Beakers are perfect. A lab stand and clamp are ideal for the mounting, but a regular shop clamp or anything that can hold it sturdily is fine. (Avoid metal if you can, to reduce the chance of sparks.) Position the bottom end of the pipe immediately over (1-2") the receiving vessel to eliminate splatter loss.

Turn the butane gas can upside down and dispense the gas into the pipe via the single top hole. A whole 8-oz can takes about 10-12 seconds to evacuate. Be brave, swift, and careful. A spark at this moment would spell disaster since you have basically created an incendiary explosive device that is leaking.

When you've exhausted the can into the pipe, back off to a nice distance and let it do its thing.

The butane moves down the pipe, extracting the cannabis as it goes. When it gets to the bottom (~30 seconds after dispensing), it begins to drain into the receiving vessel. Notice the pale, glowing yellow-green-gold hue of the extract. It is obvious no chlorophyll was pulled out of the herb

Over approximately five to eight minutes, the butane extract will finish draining from the pipe to the receiving vessel. Maintain caution with the pipe, however, since there is a lot of residual butane still evaporating from within the pipe (notice the stream of fumes coming from the top hole). When it slows down to a drop every few seconds, you can tap on the top hole with your finger and it will help push the last of the liquid butane out (or one can gently blow into the top hole to do the same thing). Remember, NO SMOKING, unless you wish to immolate yourself in grand fashion.

Being very low-boiling and volatile, the collected butane will likely begin boiling at ambient temperature. The receiving vessel will gradually frost up as the butane cools it down, slowing down its rate of evaporation, but you can speed this up again simply by holding it in your hands. A better way is to set it in a saucepan containing a little bit of warm water. Watch the butane start bubbling madly with the increase in temperature and marvel at its low boiling point. Again, be doing this outdoors with a nice breeze! It takes about 20 minutes or so to allow the butane to evaporate, or quicker if you help it along. You are left with a deep amber, almost orange oil of amazing purity.

The best way to collect and store the oil is probably to let all of the butane evaporate off and then redissolve the oil in some anhydrous or high-% alcohol, and then pour this into a vial and let it sit out for a day or two to allow the alcohol to evaporate. Trying to transfer the oil into a small container while it is still solvated by the butane is too risky. I learned the hard way about this, thanks to the volatile temperament of butane. I had filled a vial almost all the way to the top and was preparing to drop those last couple drops in, so that cleverly, I could let the last of the butane evaporate from the vial and the oil would all be neatly contained. But when the last drop hit the mother lode in the vial, it changed the temperature of the solution in the vial upward by a hair and it all "superboiled" out of the vial and onto my fingers, which of course startled me and caused me to drop the vial. I suggest dissolving it in alcohol as I mentioned above. If you can get pure or 99% isopropanol (isopropyl), use it, because THC's photosensitivity reportedly does not occur in isopropanol.

The final product is a deep yellow-amber oil of the highest quality, incredibly pure and potent. I remember well some of the prime "honey oil" hash oils that hit the market in the late 1970s, and this stuff stands up to (if not exceeds) any of them. It's amazing how this method extracts only the good fraction and leaves the junk in the weed. But that's exactly what it does. Note also that this oil has a somewhat higher melt/vaporization point than traditional hash oils; the traditional dispensing method (dipping a needle or paper clip in, getting some goop on the end, and warming it with a flame to get it to drip off into your bowl) still works with this stuff, but it seems you have to be more careful with it because it doesn't heat to liquid state as quickly or in the same manner, and it can more easily be allowed to burn up on your needle. So be careful.

Those who prefer a tincture-like preparation can of course thin the product a little with a bit of warm high-percentage alcohol like Everclear or 90-whatever-% isopropyl, then drop it onto buds or let a joint absorb some, then let the alcohol evaporate. I also observed that unlike hash oil derived from traditional methods, this product is not immediately soluble in room-temp alcohol; it needed to be warmed before it dissolved fully.

Method #2

Extraction of THC Oil from Cannabis

"If you ever had to think twice about lighting up a joint for fear of someone smelling it. If you were ever forced to blow the smoke out a window and pray you don't reek of weed. If you ever had to sneak around and couldn't enjoy a good buzz..."

This article will describe, in detail, a technique of extracting the essential oils from hemp. The final product will be a dark, oily liquid that contains 70+% pure THC. The following steps require nothing more than simple, easy to find materials and a little time.

Advantages of THC oil:
Advantages of THC oil
• No hot, harsh smoke to irritate your lungs
• No tar to stain your teeth and fingers
• Very little smell
• 5 times as much THC in bloodstream
• No carcinogens to give you cancer


Materials you'll need for extraction:
Materials you will need for extraction
• A glass jar with a watertight lid (widemouth Mason jars work great)
• A metal measuring cup with handle (2 cup capacity recommended)
• Bottle of 190 proof grain alcohol (Everclear brand is perfect)
• Any quantity of pot, any strength (from a gram up to a few ounces)
• A 1' X 1' piece of sturdy cloth (t-shirt material works fine)
• An eye-dropper bottle (contact lens type bottles work great)
• The use of an ELECTRIC stove and its overhead fan

Step 1
Step 1
You'll need to chop up your weed and pick apart the buds until it looks like grass clippings. Remove any seeds, they have their own oils which we don't want. Dump the powdered pot into the mason jar and pour in just enough grain alcohol so the weed particles float freely in the mixture. Place the lid securely on the jar and shake a few times.

Let this mixture sit for a few hours, shaking it every once in a while. The alcohol should have turned a dark green color and when shaken should form colorful, oily bubbles on top.

Place the sturdy cloth over the metal container and press the cloth down to form a funnel. Carefully pour the contents of the mason jar onto the cloth which is in the metal cup. Make sure to get most of the weed particles out of the jar. Gather up the edges of the cloth and squeeze the remaining liquid out of the lump of weed into the metal cup.

Step 1a
Step 1a
You should now have a quantity of dark green liquid in your metal measuring cup. It is possible to extract more THC oil from the remaining pot. I recommend performing Step 1 a second time immediately after completing it the first time. No sense throwing away the good stuff. Dump the pot from the cloth back into the mason jar and repeat step 1. You now have twice as much liquid in your metal cup upon repeating the first step.

Step 2
Step 2
Be sure to use an electric stove in this step! (If you don't have one, read Step 2a)

Take the metal cup containing the green liquid over to the stove. Turn one of the electric eyes on LOW setting and place the metal cup on that burner. I highly suggest using the fan over the stove to remove the alcohol vapors during this entire step. Watch the liquid closely. It should only boil slightly, never raise the burner temperature above MEDIUM LOW. We need the liquid to cook down until it's slightly thick. This may take some time but be patient.

Once the liquid starts to thicken and turn darker, remove it from the heat. Never let it get too thick or it'll be too difficult to work with. If you do accidentally make it too thick, just add a small quantity of the grain alcohol to the metal cup and swirl it around till it's thinner.

Let it cool down to room temperature inside the metal cup. It should be runny enough to be poured into the eye-dropper bottle easily. You now have your final product: THC oil. It's necessary to have some grain alcohol left in the resulting liquid so it's easy to work with. This will not affect the potency of the oil.

Step 2a
Step 2a
This part is for the people with gas stoves. Do not use a gas stove to cook down alcohol! The vapors will explode! You'll have to have patience to complete this step. To get a final product just put the metal container in a place where it won't be disturbed. The alcohol will have to evaporate on its own. If at all possible keep it in a slightly warm area with decent ventilation. It may take days.

Once it's evaporated test to see if it's too thick. If it is, pour a small amount of grain alcohol in the metal cup and mix. Pour the liquid into your eye-dropper bottle.


Hope this helps.
One thing. The kind of butane used for camping has additives. Use the kind sold for filling lighters, preferably 3x filtered or higher. Ive noticed that most asian owned grocery stores and gas stations sell it cheap. Lot of dollar stores sell it cheap too. Usually 2$-3$ per can.
 
Top