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Recovering Solvent When Making Oil

Old Salt

Member of the Month: Apr 2019
Pressing rosin leaves you with a product that still has to be decarbed, to get full potential. Fine if you smoke it, but less than optimum for edibles in it's raw stage.
So does RSO after the solvent has boiled off. That's why it's left on the heat for a while afterwards. Temperatures of 230°F / 110°C are needed for decarboxylation.

I put mine in capsules. The rosin and oil need to be warmed so they will flow easily. I heat the oil and rosin to 230°F / 110°C until decarb is complete, usually 15-20 minutes. I pour the oil into the rosin, mix it and let it cool to about 150°F, then use a syringe to load the capsules.
 

FeloniousPunk

Well-Known Member
Hi All,

This has been very educational. There are a couple of things that I'd like to know.

I will start with the IPA vs Ethyl discussion.

Because I'm in Canada, my perception regarding cost of alcohol is skewed (it can be very expensive and access can be very restricted too). As noted, 94% Alcool is $95 per litre. I have seen 99% Isopropyl Alcohol for about $8 per litre. This is a huge discrepancy in cost. While I come from the Ethynol is safer school of thought, I have made oil with both of these solvents. Nobody died from either batch. So I take the thoughts, observations and scientific arguements of Bush Doctor 77 as solid advice. We all are concerned about producing a quality product in a safe manor and so I look to history for some guidance.
I know oil has been available since I was a teen back in the 1970s. In all those years, how was it made? I am guessing, since Rick Simpson used Naphtha and has gone on record saying IPA is good too, that nobody was making it with Ethyl Alcohol. Maybe I'm being overly cautious. I suspect the IPA fumes are a much bigger threat to your health than the Isopropyl, if you are just boiling it off.

The other item is the water distiller that The Bard mentioned. I was looking at the Megahome MH-DA4B distiller. It had a disclaimer (on their website I think) that said:

"Please note: Please never use distiller to distil high concentrations alcohol or over 50%
isopropyl alcohol in order to avoid malfunction".

So I contacted them and this is what they said:

"The sealing degree of the Megahome distiller is only suitable for
the safety range of the general household use so this product
cannot extract and purify such a high concentration of alcohol".

Has anybody else run across this? The thought that this may leak has kept me from purchasing one. Does anyone know anymore about these devices?

Thanks,

FP. :peace:
 

Old Salt

Member of the Month: Apr 2019
Using a still to make your own ethanol has been illegal since the government started taxing alcohol, to protect that revenue stream. I think folks would have been tight lipped about using it as a solvent for cannabis. I did see a very few references to this in the '90s when the 'net took off. Most of the references were for the use of butane to extract the oil.

There are many references that show how to convert a gas engine to use alcohol as a fuel. All of these state that the seals in the fuel system needed to be changed to an alcohol proof material. The same appears to be true for the MH-DA4B. I found this on thewaterguy's storefront:
  • Using up to 60% isopropyl alcohol for extraction has been approved by testing against leaking seals. Using higher percentages may cause leaking in the main seal. Seals can be removed and let to dry out as they may have become saturated with alcohol.
  • We often receive emails regarding the uses and methods to produce many things.Certainly, the internet itself can provide much information on these subjects and there are many books out there with tried and true recipes and best practices help. Look for something a bit more than just an online recipe, try find a reputable author that has done their homework.
  • Another thing we get asked is about the legalities of producing Alcohol, Plant Extracts, Herbal Tinctures and Medical Marijuana Oils... these are local issues and one should familiarize oneself with what pertains to you in your area regardless of how ridiculous and archaic they may seem.
  • This is not a water distiller.
Brewhaus America sells a factory modified MH-DA4B called the 'EasyStill.' They say: "Our custom, chemical tolerant EasyFilter System with Distillery Grade Activated Carbon is included at no extra cost. This is in addition to the carbon filter for water that comes standard with the distiller. $14.95 value!"

If you read the instructions for the Brewhaus unit, you'll find:
"The EasyStill™ is a high quality, countertop distiller based on a very popular water distillation unit, but factory modified for the option of alcohol distillation*. The boiling vessel and cooling chamber are made of stainless steel. No cooling water is required, as the unit is fan cooled, making the distillation process virtually as simple as making coffee! A different heating element is used, and the chlorine release valve is omitted. This results in dramatically improved separation, and ultimately a very high quality finished product. For those in countries where alcohol distillation is legal, the unit can produce up to 60% abv product with virtually no off-tastes or smells on a single run. A second run can actually improve this to nearly 90%! "
 

Bush Doctor 77

Well-Known Member
The way I achieve complete decarb is to heat it until CO2 stops coming off. This is done at 220-230F in a pyrex dish in the oven, and decarb is complete when the extract stops degassing(frothing), and it takes a couple of hours. This also assures that there is absolutely no IPA left. IPA cannot exist as a liquid above 180F, just like liquid water cannot exist above 212F, unless it is under pressure. My bud with the dispensary does his IPA extraction on a commercial machine. He recovers his IPA through vacuum distillation, and doesn't need to heat the product during the IPA recovery.
 

Old Salt

Member of the Month: Apr 2019
The way I achieve complete decarb is to heat it until CO2 stops coming off. This is done at 220-230F in a pyrex dish in the oven, and decarb is complete when the extract stops degassing(frothing), and it takes a couple of hours. This also assures that there is absolutely no IPA left. IPA cannot exist as a liquid above 180F, just like liquid water cannot exist above 212F, unless it is under pressure. My bud with the dispensary does his IPA extraction on a commercial machine. He recovers his IPA through vacuum distillation, and doesn't need to heat the product during the IPA recovery.
IPA, or any solvent can exist as a liquid at temperatures higher than their boiling point at increased pressure. This increased pressure with rosin is created by its viscous nature. There are pockets of IPA trapped in the rosin. The anecdotal evidence was presented earlier:
However, I have also read anecdotal feedback from members here who have had their oil tested, and found traces of ISO/IPA remaining.
I have no problem with anyone using IPA or any other solvent. I want to ensure they are aware of any potential danger. After that, it's their choice. I'm not the government, and I very much disagree with their policies of protecting folks from themselves through laws banning certain activities.

Dangerous chemicals are present in the foods we eat. As an example, orange juice contains methanol in minute amounts that are measured in parts per million. We accept the risks, and live with the consequences of our choices.
 

Bush Doctor 77

Well-Known Member
IPA, or any solvent can exist as a liquid at temperatures higher than their boiling point at increased pressure. This increased pressure with rosin is created by its viscous nature.
True, but viscosity is reduced at higher temps, and thus so is pressure. My liquid extract at 220F is about as viscous as water.

Another indicator of the absence of IPA in my extract is when the temperature of the space above my extract in the still does not hold 180F any more. It cannot go above 180F if there is alcohol steam present, no matter how high the heat is turned up. The temp drops because there is no more IPA vapor being released. This is the same as steam never being hotter than 212F at sea level.

Phase changes are a really interesting phenomenon. It is critical in the study of intrusives, and the hunt for precious metals.
 

Old Salt

Member of the Month: Apr 2019
True, but viscosity is reduced at higher temps, and thus so is pressure. My liquid extract at 220F is about as viscous as water.

Another indicator of the absence of IPA in my extract is when the temperature of the space above my extract in the still does not hold 180F any more. It cannot go above 180F if there is alcohol steam present, no matter how high the heat is turned up. The temp drops because there is no more IPA vapor being released. This is the same as steam never being hotter than 212F at sea level.

Phase changes are a really interesting phenomenon. It is critical in the study of intrusives, and the hunt for precious metals.
Check the boiling point of various concentrations of alcohol in water. You'll find that it increases as the concentration of alcohol decreases. You'll also note that there is water present with the alcohol vapor, even at 180°F. You'll find that at 212° F alcohol is still present in the vapor.
 

FeloniousPunk

Well-Known Member
Using a still to make your own ethanol has been illegal since the government started taxing alcohol, to protect that revenue stream. I think folks would have been tight lipped about using it as a solvent for cannabis. I did see a very few references to this in the '90s when the 'net took off. Most of the references were for the use of butane to extract the oil.

There are many references that show how to convert a gas engine to use alcohol as a fuel. All of these state that the seals in the fuel system needed to be changed to an alcohol proof material. The same appears to be true for the MH-DA4B. I found this on thewaterguy's storefront:
  • Using up to 60% isopropyl alcohol for extraction has been approved by testing against leaking seals. Using higher percentages may cause leaking in the main seal. Seals can be removed and let to dry out as they may have become saturated with alcohol.
  • We often receive emails regarding the uses and methods to produce many things.Certainly, the internet itself can provide much information on these subjects and there are many books out there with tried and true recipes and best practices help. Look for something a bit more than just an online recipe, try find a reputable author that has done their homework.
  • Another thing we get asked is about the legalities of producing Alcohol, Plant Extracts, Herbal Tinctures and Medical Marijuana Oils... these are local issues and one should familiarize oneself with what pertains to you in your area regardless of how ridiculous and archaic they may seem.
  • This is not a water distiller.
Brewhaus America sells a factory modified MH-DA4B called the 'EasyStill.' They say: "Our custom, chemical tolerant EasyFilter System with Distillery Grade Activated Carbon is included at no extra cost. This is in addition to the carbon filter for water that comes standard with the distiller. $14.95 value!"

If you read the instructions for the Brewhaus unit, you'll find:
"The EasyStill™ is a high quality, countertop distiller based on a very popular water distillation unit, but factory modified for the option of alcohol distillation*. The boiling vessel and cooling chamber are made of stainless steel. No cooling water is required, as the unit is fan cooled, making the distillation process virtually as simple as making coffee! A different heating element is used, and the chlorine release valve is omitted. This results in dramatically improved separation, and ultimately a very high quality finished product. For those in countries where alcohol distillation is legal, the unit can produce up to 60% abv product with virtually no off-tastes or smells on a single run. A second run can actually improve this to nearly 90%! "
Good Morning Old Salt,

Thank you for this. In my search for a countertop distiller I did see the Brewhaus unit, but either didn't see what you posted from their instructions or I had forgotten it. Here in Canada the company has changed its name to Artizan Spiritz. The cost of the unit is $300.

Have you used the Brewhaus unit? I saw an oil making video with a similar unit that recovered about 60% of the alcohol. Is this because you can't boil off all the alcohol and are left with a couple cups of liquid that still needs to be boiled off?

FP. :peace:
 

Old Salt

Member of the Month: Apr 2019
Good Morning Old Salt,

Thank you for this. In my search for a countertop distiller I did see the Brewhaus unit, but either didn't see what you posted from their instructions or I had forgotten it. Here in Canada the company has changed its name to Artizan Spiritz. The cost of the unit is $300.

Have you used the Brewhaus unit? I saw an oil making video with a similar unit that recovered about 60% of the alcohol. Is this because you can't boil off all the alcohol and are left with a couple cups of liquid that still needs to be boiled off?

FP. :peace:
No, I haven't used any of the countertop models. We used a similar, but higher capacity unit on my parent's ranch where we raised chinchillas to distill water.

I made my own 'stills. The first was a new 20lb propane tank and condenser with heat supplied by a camp stove. That wasn't big enough so I used a forty gallon hot water heater, and condenser. That was problematic. I made hundreds of gallons of 90%+ ethanol and drank it with help from my friends. That's why I don't use ethanol, and press rosin today. The last 'still I made was an 80 gal Biodiesel reactor. Adding a condenser let me recover the unused methanol from the reaction. I have a picture of that:


80 US Gallon Biodiesel Reactor / Distiller (Used for Methanol Recovery)
 

Bush Doctor 77

Well-Known Member
Check the boiling point of various concentrations of alcohol in water. You'll find that it increases as the concentration of alcohol decreases. You'll also note that there is water present with the alcohol vapor, even at 180°F. You'll find that at 212° F alcohol is still present in the vapor.
I am well aware of how phase reactions can change with various solution concentrations. My whole point was that at 220-230F, there will be no alcohol or water present after a couple of hours.
 

FeloniousPunk

Well-Known Member
Good Morning,

So lets see that I understand...

If I decarbed the flower before making oil I would have a runny (ish) oil after boiling off the alcohol because of the water in the 95% alcohol?
So..., the bubbles in the boiling off are from the alcohol at around 172F. Once that is done, the temperature will rise to 212F to boil off the water and the bubbles at this temperature is the water boiling off. At around 230F is the decarb, and those bubbles are the carbon boiling off. Is this right?

If so, does that mean that oil, made with decarbed flower, washed with 100% alcohol, with the alcohol boiled off, would be more viscous than 95% alcohol done the same way?

We are experimenting with using glycerin in cleaning out the leftovers after drawing out the oil in syringes. Anybody else try this?

FP. :peace:
 

Bush Doctor 77

Well-Known Member
Good Morning,

So lets see that I understand...

If I decarbed the flower before making oil I would have a runny (ish) oil after boiling off the alcohol because of the water in the 95% alcohol?
So..., the bubbles in the boiling off are from the alcohol at around 172F. Once that is done, the temperature will rise to 212F to boil off the water and the bubbles at this temperature is the water boiling off. At around 230F is the decarb, and those bubbles are the carbon boiling off. Is this right?

If so, does that mean that oil, made with decarbed flower, washed with 100% alcohol, with the alcohol boiled off, would be more viscous than 95% alcohol done the same way?

We are experimenting with using glycerin in cleaning out the leftovers after drawing out the oil in syringes. Anybody else try this?

FP. :peace:
Why decarb twice? The first part of your statement is correct. As Old Salt mentioned, the alcohol/water mixture will have the boiling points different than pure water and pure IPA. My feeling is that it is insigificant for my method with IPA, as there is very little water present. The viscosity of the extract, minus IPA and alcohol, should be the same for either method, as you are measuring the viscosity of comparable extracts.
 

FeloniousPunk

Well-Known Member
Hello again,

Maybe I should have been more clear.

If we stop the process when the alcohol is boiled off, the oil made with a lower proof alcohol will be less viscous (thinner) than oil made with 200 proof alcohol, correct?

Will both solvents remove the same amount of cannabinoids from the flower, or does the water in lower proofs make the alcohol less effective?

I am trying to see if there is a way to extract the cannabinoids AND make them measurable for a "dose".

I know, I know, go to Sweet Sues oil page. LoL!

Thanks!

FP. :peace:
 

Old Salt

Member of the Month: Apr 2019
I am trying to see if there is a way to extract the cannabinoids AND make them measurable for a "dose".
Good questions.

So far I know that:
  • the cannabinoid content varies from plant to plant of a strain, and even from bud to bud on the same plant.
  • rosin, oil, diamonds, and sauce need to be tested for their cannabinoid content, which should be homogeneous
  • once tested, rosin, oil, diamonds and can be mixed and matched to achieve the desired bulk concentration
  • the bulk product can be divided into doses, accurate within a few percentage points

What I don't know:
  • whether rosin, oil, diamonds, and sauce can be tested at home as extracted.
  • whether mechanical separation (pressing) separates only the THC or the other cannabinoids are also extracted when pressing rosin through a 25 micron filter bag

I hope to be able to answer these question by next year. I need a cannabis test kit to determine this, and have to save up for one. Until then, I'll make a few test capsules to determine whether or not I got it right.
 

Old Salt

Member of the Month: Apr 2019
Oil made from low proof alcohol, because it has more water, should contain more chlorophyll. Not sure how that will impact viscosity. I may try one of our sponsors for my next solvent purchase.

Our Products - Extractohol
The chlorophyll can be removed by exposing the alcohol/oil mixture (before distilling) to sunlight for a few hours. A grow light may work as well.
 

Old Salt

Member of the Month: Apr 2019
Have you done that? Basically bleaching it. Interesting.
No, I don't use solvents. I did a lot of research into it before deciding to press rosin instead. Here's one of the sources I used (chlorophill removal is at about the 10 min 29 second mark):

 

TurboBucket

Photo of the Month: Jan 2019 - Plant of the Month: Feb 2019
I use 150 proof everclear because it's what's available. With a QWET you don't typically end up with a lot of chlorophyll, if you let it set for awhile you get more. Depends on what your trying to make I suppose. Extraction for dabs is different than extracting for medibles.
 
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