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Any one using the reflux method to make oil? What solvent are you using?

No Pain

Well-Known Member
I have been making oil for several years now mostly working with tric's now from dry ice extraction . Im looking to dive back into washing so to speak . I have come across multiple sources that talk about refluxing and it being a superior product and was wondering if anyone else was using this method . I am also looking to switch to a non polar solvent and doing several washes with ethyl alcohol and water . Three solvents have caught my eye Hexane , petroleum ether and chloroform ...the later two have superior extraction . All thoughts and opinions welcome .
 

Nunyabiz

Well-Known Member
I've only made oil a few times but will be making it much more soon.
I've recently bought a Extractcraft Source Turbo and have decided to make Concentrated Tincture.
I made one from a Honey Peach CBD 12%CBD 9%THC and it's quite nice.
I like concentrated Tinctures because they last pretty much indefinitely and my wife and I want to build up a nice supply to have immediately on hand in case one of us gets cancer so we could start the Rick Simpson protocol day one.

I use Extractahol which is food quality 200 proof alcohol and freeze it along with buds at -14 F pour the alchohol into cannabis and right back into freezer then shake lightly every 5 minutes for about 45 minutes and run that through a Buchner filter to remove most all impurities.
Makes a very potent Tincture.
 

No Pain

Well-Known Member
I've only made oil a few times but will be making it much more soon.
I've recently bought a Extractcraft Source Turbo and have decided to make Concentrated Tincture.
I made one from a Honey Peach CBD 12%CBD 9%THC and it's quite nice.
I like concentrated Tinctures because they last pretty much indefinitely and my wife and I want to build up a nice supply to have immediately on hand in case one of us gets cancer so we could start the Rick Simpson protocol day one.

I use Extractahol which is food quality 200 proof alcohol and freeze it along with buds at -14 F pour the alchohol into cannabis and right back into freezer then shake lightly every 5 minutes for about 45 minutes and run that through a Buchner filter to remove most all impurities.
Makes a very potent Tincture.
I am familiar with both items . Your solvent is equal to what I currently use . The method that is used with the turbo with the exception of applying a vacuum to boil solvents at a lower temp and recapture a good portion of it , is RS style or should I say his generic version , one the masses could easily follow . What I do now is not much different and its not that my oil is week by any means . Its just that I have come across several sources in regards to refluxing and it improving potency and healing powers as well as yields in comparison to any other method .
 

zeroday

Well-Known Member
I guess it depends on what you are trying to accomplish. If you don't mind me asking, what end product are you shooting for?
 

No Pain

Well-Known Member
I guess it depends on what you are trying to accomplish. If you don't mind me asking, what end product are you shooting for?
What I am looking for is to produce the best medicine that can possibly be produced through oil extraction . Like I Have stated prior is I have recently come across information that states Refluxing is the way to go to achieve this and you get an added benefit of increased yield .
 

zeroday

Well-Known Member
What I am looking for is to produce the best medicine that can possibly be produced through oil extraction . Like I Have stated prior is I have recently come across information that states Refluxing is the way to go to achieve this and you get an added benefit of increased yield .
I'd argue the better yield comments you see out there on the other forums. Folks go and use things like pentane, hexane, methane, etc.... and claim to get better yields. All they are really getting is more wax and lipids. If you were to take that crude oil and then refine it further, like with wiped film or short path distillation, you'd have to filter the hell out of your crude oil with things like celite, charcoal, carbon, etc. That and then you have to worry about color remediation. The most recent science I have seen on other forums states deep freezing your ETOH is better than using Hexane/Pentane/Methane. Reason is that deep frozen etoh precipitates the wax/lipids and crap, where as the other solvents only do a better job of stripping the wax/lipids.... Sure, you might get a bit more THC-A, but the amount of time, energy and money you'll spend in the filtering process negates any increased yield in my mind. If you aren't concerned with the percentage of wax/lips and don't mind dealing with the filtering, I guess this isn't such a big deal. I just find it very annoying to have to spend all the time filtering.

Also be aware that because you are vaporizing THC at normal environmental pressure with refluxing, the THC will be exposed to oxygen, and you'll lose some of the THC to oxidation. In most lab setups, they are doing the evaporation in a rotary evaporator that in under vaccum, and then take the resulting oil and run it through a short path still or something similar, also under vacuum. Having no oxygen present avoids degradation of the THC-A.

Lastly, unless you are going to test each and every single batch by a certified lab, you might want to reconsider using anything but etoh. I've seen lab test where the extractor thought he/she got all of the solvent out of their oil, but didn't. I'd hate to be the one consuming pentane and hexane.
 

No Pain

Well-Known Member
This is what I do only I made a distiller out of an electric tea kettle. Very easy and safe.

I use a very similar method one variant is I am working with product from dry ice extraction instead of plant material another is im using 200 proof food grade ethanol . I actually use the same distiller in the video . I will post a pic of my end product .

I'd argue the better yield comments you see out there on the other forums. Folks go and use things like pentane, hexane, methane, etc.... and claim to get better yields. All they are really getting is more wax and lipids. If you were to take that crude oil and then refine it further, like with wiped film or short path distillation, you'd have to filter the hell out of your crude oil with things like celite, charcoal, carbon, etc. That and then you have to worry about color remediation. The most recent science I have seen on other forums states deep freezing your ETOH is better than using Hexane/Pentane/Methane. Reason is that deep frozen etoh precipitates the wax/lipids and crap, where as the other solvents only do a better job of stripping the wax/lipids.... Sure, you might get a bit more THC-A, but the amount of time, energy and money you'll spend in the filtering process negates any increased yield in my mind. If you aren't concerned with the percentage of wax/lips and don't mind dealing with the filtering, I guess this isn't such a big deal. I just find it very annoying to have to spend all the time filtering.

Also be aware that because you are vaporizing THC at normal environmental pressure with refluxing, the THC will be exposed to oxygen, and you'll lose some of the THC to oxidation. In most lab setups, they are doing the evaporation in a rotary evaporator that in under vaccum, and then take the resulting oil and run it through a short path still or something similar, also under vacuum. Having no oxygen present avoids degradation of the THC-A.

Lastly, unless you are going to test each and every single batch by a certified lab, you might want to reconsider using anything but etoh. I've seen lab test where the extractor thought he/she got all of the solvent out of their oil, but didn't. I'd hate to be the one consuming pentane and hexane.
I am more concerned about the healing properties of the final product than i am about the quantity . If i was going to sacrifice something out of the quantity/quality equation in would be quantity .

In regards to solvents ethanol and methanol are superior to hexane here is a link to the study solvent testing . I have been very hesitant to this point of using anything but food grade ethanol because of what you stated about one feeling that they got all the solvent out and didn't . Thus my question about solvent that you are using . The top two for extraction are never food grade those two being chloroform and petroleum ether based on things i have come across along with the age only book Marijuana potency by Michael Starks go to page 112 here is the link . Now based on other things i have read about those to solvents is that you can successfully clean out all the residue using an ethanol / salt water bath then filtered through a separatory funnel . Th only reason i was asking about solvents and thinking of changing what i was doing was because i was looking into refluxing like is demonstrated in this video
I felt that if I used Ethanol that i would defiantly pull more chlorophyll out than i cared to have in the medicine produced. Here is a picture of the of some of what was left using my current methods to demonstrate color and what not .After some reading today thanks to a friend . Im thinking I should take my end product which would be considered crude oil and distill it .
IMG_6556.JPG
 

10gal

Well-Known Member
what do yo mean by reflux?

I can tell you the way i used to do it, but things change and reflux might not mean the same thing to you and me

but do a full run with a soxhlet extractor, retrieve your solvent, wash the solvent with water in a separation funnel to remove the polar elements extracted in your solvent, let it settle and separate, drain off the water, filter the solvent through a #2 filter paper(you will need suction) and evaporate off as normal.
you can also add a winterizing step to remove more waxes but at this stage you should be pretty good

but im english so it might be over kill... but it helps me sleep at night knowing i did shit right
 

zeroday

Well-Known Member
what do yo mean by reflux?

I can tell you the way i used to do it, but things change and reflux might not mean the same thing to you and me

but do a full run with a soxhlet extractor, retrieve your solvent, wash the solvent with water in a separation funnel to remove the polar elements extracted in your solvent, let it settle and separate, drain off the water, filter the solvent through a #2 filter paper(you will need suction) and evaporate off as normal.
you can also add a winterizing step to remove more waxes but at this stage you should be pretty good

but im english so it might be over kill... but it helps me sleep at night knowing i did shit right
Different apparatus. They are the same, except that a true Soxhlet has a permeable beaker between the hot bottom and the cold top, where as the Refluxing apparatus does not.
 

Nunyabiz

Well-Known Member
I cant imagine what could be better than super cold 200 proof alchohol.
And extract under vacuum, I get at least 95% of it back so only cost about $1 to extract from an oz of cannabis.
I leave a tiny amount of the alchohol in it to use as a Tincture.
It will last virtually forever preserved in alchohol and it starts coming on almost immediately.
I take 2 drops twice a day and I am medicated all day.

20191212_132730.jpg
 

No Pain

Well-Known Member
I cant imagine what could be better than super cold 200 proof alchohol.
And extract under vacuum, I get at least 95% of it back so only cost about $1 to extract from an oz of cannabis.
I leave a tiny amount of the alchohol in it to use as a Tincture.
It will last virtually forever preserved in alchohol and it starts coming on almost immediately.
I take 2 drops twice a day and I am medicated all day.

20191212_132730.jpg
well if by better you mean toxicity levels and hazards from the solvent and fumes ..there isn't one ..if you are referring to amount of cannabinoids extracted Chloroform and petroleum ether are at the top of the charts . I loose very little solvent in filtration ( love your vacuum filter unit) and I recapture 85-90 percent of my solvent when I distill it through a water distiller .
Im washing hash from dry ice extraction and my returns are quite good , that run that the pic of my beaker is from, I used around 40 grams of hash , washed it , then stuck it the freezer for a little over a day and cold filtered it the rest is history and I pulled 15 grams /15 ml of oil out . which is an excellent return in my book . Since I only make and use the hash for oil , the information about refluxing got me thinking about how much I could be leaving behind in my plant material as I stop sifting once anything but blonde hash appears . See I used 168 grams of flower for that 40 grams of blonde hash and that's a 24% return which is still good but im certain that more was left behind , I just don't know how much . In writing this the though came to me to wash the plant material in a completely separate wash and run just to see how much was truly left behind the next time I do an extraction .
 

No Pain

Well-Known Member
So you are getting 8% or so yield going from bud to the oil?
it actually comes out to a tad over 9%, what was left in the beaker wasn't weighed . Thus the question how much was truly left behind . Because 24% yield from flower to hash is good ..and 38% oil return from material weight is excellent . So if I did a wash of bud material and got say an extra 8% plus how much of that would actually be contaminants/impurities . With making oil from pure hash there is no chlorophyll or extra plant waxes to be concerned about . As I feel that I filter out the great majority of any waxes in my winterized filtration . I can truly state that since I started using straight hash to make oil the oil has come out way cleaner and is less viscus at room temperature not very difficult to squeeze out of the syringe as compared to when I did washes of bud material , when it cooled it was much like a plastic that need a little heat prior to trying to squeeze it out of the syringe . Now I will say that I have yet to preform a winterized wash of bud material as I was already washing hash by the time I came upon that information .
 

tslonige

Active Member
So you are getting 8% or so yield going from bud to the oil?
2 to 4 Grams per ounce of bud. Or around 15 to 25% approx. Depends on strain, grow conditions, drying method etc
That is using the method I posted in the video
Sorry if I responded inappropriately, I wasn't sure who the question was directed too.
 

zeroday

Well-Known Member
it actually comes out to a tad over 9%, what was left in the beaker wasn't weighed . Thus the question how much was truly left behind . Because 24% yield from flower to hash is good ..and 38% oil return from material weight is excellent . So if I did a wash of bud material and got say an extra 8% plus how much of that would actually be contaminants/impurities . With making oil from pure hash there is no chlorophyll or extra plant waxes to be concerned about . As I feel that I filter out the great majority of any waxes in my winterized filtration . I can truly state that since I started using straight hash to make oil the oil has come out way cleaner and is less viscus at room temperature not very difficult to squeeze out of the syringe as compared to when I did washes of bud material , when it cooled it was much like a plastic that need a little heat prior to trying to squeeze it out of the syringe . Now I will say that I have yet to preform a winterized wash of bud material as I was already washing hash by the time I came upon that information .
I'm getting 14% yield from bud to crude. From Bud to refined oil i'm getting about 7.5%, but I'm left with 3 separated parts: Garbage, THC oil, Terpenes.

Interesting that you are getting the thickness of the end product that you are getting. Both my crude and my refined oil is hard. Not as hard as plastic as you say, you can push your finger into it if you try, but you can tip the container upside down and it won't budge for a long time. Its essentially the same consistency as the concentrate I get from my dispensery.

Pic of what the end product looks like.

1E47F36D-5374-4E42-AC74-E41BF8CFD200.jpeg
 
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No Pain

Well-Known Member
I'm getting 14% yield from bud to crude. From Bud to refined oil i'm getting about 7.5%, but I'm left with 3 separated parts: Garbage, THC oil, Terpenes.

Interesting that you are getting the thickness of the end product that you are getting. Both my crude and my refined oil is hard. Not as hard as plastic as you say, you can push your finger into it if you try, but you can tip the container upside down and it won't budge for a long time. Its essentially the same consistency as the concentrate I get from my dispensery.

Pic of what the end product looks like.

1E47F36D-5374-4E42-AC74-E41BF8CFD200.jpeg
looks very nice . I need to get into making distillate !!!
Now don't think mine is over here just sloshing around as it is not . squeezing it out of a syringe would be somewhat comparable to you pushing your finger into your jar . I can hold that beaker upside down and it doesn't flow however I can easily put my finger into the build up and after removing my finger my finger print is clearly visible and several minutes later it is gone and only indentions are left .As you will see the two indentions I made are smooth .

No there really cannot be any terpenes in my weight/oil because i decrab my hash /oil i have done it both ways to see if there was any difference in the final product and so far i cannot say that there is . I decarb at 250 for 30-45 minutes .

In my opinion you could be dealing with wax as when you wash the plant material you are getting more than just the wax of the trichrome head where as the trichrome head is really all that i have to deal with working with hash. Im sure that you filter your wash , but do you cold filter and how many times ? Because aside from what you are washing i feel that would be the only difference ..i have less wax to deal with so i filter less . I.e say your getting 3 times as much wax in your crude as i am ...per weight you would have to (Cold) filter your wash 3 times as much. By the way i am only using coffee filters at the moment and i change them when they reduce to a drip if there is enough wash in the funnel where it should be flowing .

I plan on changing my filtration to vacuum filtration and a Buchner funnel i was looking at then early this week and a combo isn't really expensive . However the vacuum pump is a different story . I am the type of person that likes to spend wisely , meaning: Why get a cheep pump just for filtration if i plan to get into distillation ? I would rather spend my money one time and get one that with work for both . Thus me checking and asking about refluxing and solvents to help guide my way to a good destination for me .
IMG_6559.JPG
 

zeroday

Well-Known Member
looks very nice . I need to get into making distillate !!!
Now don't think mine is over here just sloshing around as it is not . squeezing it out of a syringe would be somewhat comparable to you pushing your finger into your jar . I can hold that beaker upside down and it doesn't flow however I can easily put my finger into the build up and after removing my finger my finger print is clearly visible and several minutes later it is gone and only indentions are left .As you will see the two indentions I made are smooth .
From the pic and your description, sounds like our consistencies are roughly the same.

No there really cannot be any terpenes in my weight/oil because i decrab my hash /oil i have done it both ways to see if there was any difference in the final product and so far i cannot say that there is . I decarb at 250 for 30-45 minutes .
If you are only going up to 250F, you're only going to boil off the B-caryophyllene. The other big ones, d-Limonene, Linalool, Pulegone, 1-8-cineole, a-pinene, a-terpineol and p-cymene all boil off between ~310F and ~440F. Then there are the Flavonoids: Apigenin, queretin, cannflavin A and B-sitosterol. Those all vaporize off ~270F to ~480F.

In my opinion you could be dealing with wax as when you wash the plant material you are getting more than just the wax of the trichrome head where as the trichrome head is really all that i have to deal with working with hash. Im sure that you filter your wash , but do you cold filter and how many times ? Because aside from what you are washing i feel that would be the only difference ..i have less wax to deal with so i filter less . I.e say your getting 3 times as much wax in your crude as i am ...per weight you would have to (Cold) filter your wash 3 times as much. By the way i am only using coffee filters at the moment and i change them when they reduce to a drip if there is enough wash in the funnel where it should be flowing .
I only do 2 filtrations. My ethanol is typically at -80c, so its more efficient and picks up significantly less wax/fats.

I plan on changing my filtration to vacuum filtration and a Buchner funnel i was looking at then early this week and a combo isn't really expensive . However the vacuum pump is a different story . I am the type of person that likes to spend wisely , meaning: Why get a cheep pump just for filtration if i plan to get into distillation ? I would rather spend my money one time and get one that with work for both . Thus me checking and asking about refluxing and solvents to help guide my way to a good destination for me .
I went with a cheap vacuum. I read allot of material that suggests that the fumes from the solvent will damage the pump. When I use my big dual vane pump on the SPD, the cold trap condenses any vapor that makes it anywhere close to the pump. Also, the pump has oil that will filter out anything that makes it past the cold trap. Even still, it is suggested that you change the oil after every run. So, I figured buying a cheap $20 hand held was the way to go. Its also a hell of allot quieter.

I am going to try out your method of evaping the solvent. The Source that I have been using has a 250ml crucible, when full takes 2 hours to run. So, when I'm running 4 liters of wash, it takes forever and a day. I was going to save up and build a DIY rotovap so I could just do the whole 4 liters at the same time, but for what you paid for your water distiller, I'm gonna give it a try, assuming I can figure it out, lol!
 

zeroday

Well-Known Member
I'd also add, that if your end goal is the best medicine, getting rid of the terpines might not be what you want anyway. Lots of science out there on how having all of natural elements present creates the "entourage effect". Now wouldn't that be interesting that the only way to get the medical benefits is to have all of the elements present, instead of isolating them.

When that info came out, the CBD Isolate market fell through the floor and broad-spectrum CBD went through the roof.
 

No Pain

Well-Known Member
From the pic and your description, sounds like our consistencies are roughly the same.



If you are only going up to 250F, you're only going to boil off the B-caryophyllene. The other big ones, d-Limonene, Linalool, Pulegone, 1-8-cineole, a-pinene, a-terpineol and p-cymene all boil off between ~310F and ~440F. Then there are the Flavonoids: Apigenin, queretin, cannflavin A and B-sitosterol. Those all vaporize off ~270F to ~480F.



I only do 2 filtrations. My ethanol is typically at -80c, so its more efficient and picks up significantly less wax/fats.



I went with a cheap vacuum. I read allot of material that suggests that the fumes from the solvent will damage the pump. When I use my big dual vane pump on the SPD, the cold trap condenses any vapor that makes it anywhere close to the pump. Also, the pump has oil that will filter out anything that makes it past the cold trap. Even still, it is suggested that you change the oil after every run. So, I figured buying a cheap $20 hand held was the way to go. Its also a hell of allot quieter.

I am going to try out your method of evaping the solvent. The Source that I have been using has a 250ml crucible, when full takes 2 hours to run. So, when I'm running 4 liters of wash, it takes forever and a day. I was going to save up and build a DIY rotovap so I could just do the whole 4 liters at the same time, but for what you paid for your water distiller, I'm gonna give it a try, assuming I can figure it out, lol!
As of right now with ,y methods im happy with the cosistancy I just feel that I could be better (its the over achiever in my I suppose , lol ) .

In regards to the terpenes based on the knowledge that you just bestowed up me , A better statement would have been that all the terpenes that are evaporated off during decarb are removed from my oil .

I have yet to do a cold wash , however it is on the list for sure i have been doing a lot of research and reading this past week and im still leading towards trying petroleum ether . There is just to much information that shows its a top shelf solvent , you just need to be extra careful because of its combustibility .Which i can do .

That water distiller is great , i wouldn't recommend finsihing the oil in it as it is a pain to remove. I tried it once and did not care for it . Since i put a mark on the decanter in regards to how much solvent Im putting in and pull the lid off and give it a quick check when its gets within 1/2"-1/4" of the marking . Once im satisfied i pour the remaining solvent in my beaker with a stir bar and put it on my prewarmed hotplate and do the final evaporation . The distiller will easily do a gallon of solvent within 1 1/2 hours . I'm certain that you will be happy with its performance .

I'd also add, that if your end goal is the best medicine, getting rid of the terpines might not be what you want anyway. Lots of science out there on how having all of natural elements present creates the "entourage effect". Now wouldn't that be interesting that the only way to get the medical benefits is to have all of the elements present, instead of isolating them.

When that info came out, the CBD Isolate market fell through the floor and broad-spectrum CBD went through the roof.
I agree and fully understand the synergistic effects of broad spectrum oil . That is the main reason i was also looking into steam distillation of essential oils . To first extract the essentials through steam distillation , re drying the material then doing a wash and making the crude and then reintroducing the essentials to the crude if im not doing spd by then if i am it would be after spd .
 
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