99.98% THCa Thc
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budchemist
Active Member
Great job!
budchemist
Active Member
What technique did you use?
Short path distillation?
Whatever the method it is clear you know what you are doing.
ander20n
Member
No distillation. Through recrystallization. Crystallization of course to start.
budchemist
Active Member
What solvent mix are you using to do that?
BobCajun
Well-Known Member
I recently found an easy way to get what seems to be fairly pure THCA. I dissolved some freezer made iso extract in a little iso, it was just an experiment so it was only about a gram in maybe 5-10 mls of iso. I put about an equal volume of baking soda in as the amount of extract. Then I gradually added deionized water with mixing until the soda was all dissolved, just enough to dissolve it. I filtered the solution and added more water, don't recall how much, just diluted it so it was mostly water, and then citric acid until a precipitate formed, and collected it in another filter, spraying pure water on at the end to wash the material of citric acid.
After drying the filter cake by laying the filter on a few sheets of paper towel, the precipitate could be removed from the paper in flakes by turning it upside down and plucking the flakes off with a knife tip, and then air dried. It's white chunks, which when heated fuse back into normal looking extract, pretty much exactly as it started out, same smell and everything, amber color though the flakes were white. Same as smoking normal extract but it's novel due to being white flakes before heated in a pipe. People can see you did some clean up work on it. I don't know how stable it is or anything. I didn't store it. I fused it back into a chunk of extract in the microwave.
After drying the filter cake by laying the filter on a few sheets of paper towel, the precipitate could be removed from the paper in flakes by turning it upside down and plucking the flakes off with a knife tip, and then air dried. It's white chunks, which when heated fuse back into normal looking extract, pretty much exactly as it started out, same smell and everything, amber color though the flakes were white. Same as smoking normal extract but it's novel due to being white flakes before heated in a pipe. People can see you did some clean up work on it. I don't know how stable it is or anything. I didn't store it. I fused it back into a chunk of extract in the microwave.
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budchemist
Active Member
Very interesting. The solid would likely be a lot more stable than the liquid, at least from my experience.
Curious what scale you did it on and what your yield was.
ander20n
Member
That is interesting. I honestly stay away from ISO, but in your instance you are washing it a few more times via h2o you can get all the iso out relatively easy. Id be curious to see your yield and a picture of what the product looked like. Ive heard of semi similar methods adjusting ph of water so that thca is soluble in it.
BobCajun
Well-Known Member
I was just doing the description based on memory. I may have diluted with a fair amount of water before the first filtering, rather than after, for instance. Didn't actually weigh for yields, but looked almost quantitative. I actually didn't expect it to work, so didn't put much detail into it. The thing here is that normally it's hard to get THCA to react with baking soda, because it's a rather weak base. I tried it a few times using camping fuel as solvent and it always failed. It also fails with no solvent at all, just water and soda, even if you heat it to liquefy the extract and mix it around well. Only a very slight amount reacts.
So I figured maybe if I dissolve the extract in iso and don't use immiscible solvents at all, and then add water little by little to dissolve the soda it might work better. Turned out I was right. It was as simple as that. Sodium carbonate might work even better, being more strongly basic than bicarbonate, or potassium carbonate, which is a lot more soluble. BTW, I doubt if vinegar would work, citric is the strongest organic carboxylic acid you can get. Fortunately, authorities would have trouble trying to restrict its sale, or baking soda.
So I figured maybe if I dissolve the extract in iso and don't use immiscible solvents at all, and then add water little by little to dissolve the soda it might work better. Turned out I was right. It was as simple as that. Sodium carbonate might work even better, being more strongly basic than bicarbonate, or potassium carbonate, which is a lot more soluble. BTW, I doubt if vinegar would work, citric is the strongest organic carboxylic acid you can get. Fortunately, authorities would have trouble trying to restrict its sale, or baking soda.
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ander20n
Member
I’ve seen this process. More people are using very high grade cold water hash filtered through 90-120 u, And then rosin press at temps low enough as to not hurt any mono terpenes through 90 u rosin filters. Purge shortly at low temps using a cold trap as to be sure they weren’t evaporating off any of the light end terps. Can’t reiterate how important the terpenes are here, there is no hydrocarbon assistance to help add viscousity to your extract, making it harder for THCa to move around freely. I’ve also seen extractors adding terpenes in with there rosin (some food grade, some marijuana terpenes, extractor dependent). Then go to jar tek method from there. Need to extract enough terpenes if you’re not adding any as these are the short chain hydrocarbons that make solventless hash a possibility. Some terpenes work better than others. Purity is a huge factor. Get your rosin up to 80-85% with heavy terpenes, and you’re in business.
BobCajun
Well-Known Member
I just made a batch up. Started with 10 g of extract. It's still drying so don't know the yield, looks pretty high though. There was just a little bit of sludge that got filtered out after reaction with the soda. After reaction and dilution, anything that doesn't dissolve is crud, or possibly THC but I'd say mostly useless sludge. It's a thin oil, light reddish brown. It will stick to a paper filter so can be removed that way, but the water goes through slow at the end. After filtering, I got a clear brown liquid, from which the white material precipitated.
You can see it fizzing during the soda reaction, so you know when it's getting done, not like vinegar and soda but noticeable bubbling. It's the method I described earlier, just scaled up some. I used probably about 30-40 mls of iso to dissolve the extract, with heating. Not easy to dissolve it all but eventually it goes. I used half its weight in soda, 5 g, theoretical is about 2.5 but I wanted some excess. I put it in the microwave to make sure it was all reacted after the bubbling died down, which was a long time, it reacts slowly at room temp. When I heated it, it bubbled more than before but it might just have been the soda bubbling from the heat.
This image shows what happens when you add the citric acid to precipitate the THCA. It forms an expanded muffin which floats on the top. You can spoon most of it out onto a filter. It gets a lot smaller as the water seeps out. You should always use at least 2 filters for this, because the particles can go through a single filter. With 2 or 3 the water comes out completely clear.
After filtering the whole cup and spraying quite a bit of pure water through to wash it, I broke the rocks up into smaller pebbles. It's still fairly crude, which is why it's tan colored. If I repeated the process again a time or more it would get purer each time but this should be good enough for now. It could appropriately be called "brown sugar" at this point. Should lighten up when dry though. It has a gritty feel by the way, kind of chalky. I tried a little piece, real smooth, good shit, melts right up when you put a flame to it, but will fizz if there's still water in it.
You can see it fizzing during the soda reaction, so you know when it's getting done, not like vinegar and soda but noticeable bubbling. It's the method I described earlier, just scaled up some. I used probably about 30-40 mls of iso to dissolve the extract, with heating. Not easy to dissolve it all but eventually it goes. I used half its weight in soda, 5 g, theoretical is about 2.5 but I wanted some excess. I put it in the microwave to make sure it was all reacted after the bubbling died down, which was a long time, it reacts slowly at room temp. When I heated it, it bubbled more than before but it might just have been the soda bubbling from the heat.
This image shows what happens when you add the citric acid to precipitate the THCA. It forms an expanded muffin which floats on the top. You can spoon most of it out onto a filter. It gets a lot smaller as the water seeps out. You should always use at least 2 filters for this, because the particles can go through a single filter. With 2 or 3 the water comes out completely clear.
After filtering the whole cup and spraying quite a bit of pure water through to wash it, I broke the rocks up into smaller pebbles. It's still fairly crude, which is why it's tan colored. If I repeated the process again a time or more it would get purer each time but this should be good enough for now. It could appropriately be called "brown sugar" at this point. Should lighten up when dry though. It has a gritty feel by the way, kind of chalky. I tried a little piece, real smooth, good shit, melts right up when you put a flame to it, but will fizz if there's still water in it.
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outliergenetix
Well-Known Member
I am not gonna go into great detail about that press tech for thca and why it is not true. I understand it can be made in a SIMILAR sounding way and it confuses ppl by making this way sound the same but it is not the same. those pores on that bag are not gonna cut the proverbial mustard. so you are 100% not getting thca with the equipment laid out by this tech. gopurepressure has that lame video on their rip off of a website and they can't even provide lab results. however they definitely did provide a disclaimer how this is not their claim yet they still used the vid on their site. I am sure ppl here will argue with me, but that is lipids etc... not pure thca sorry to say. you don't believe me go lab test your "thca". to be clear I am specifically talking about the re-pressing on a rosin press thru filtered bags etc.. totally bunk, not true, and most importantly it's not pure thca or even close to it
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BobCajun
Well-Known Member
Here's how it looks after overnight in a closed container with some calcium chloride pellets, which pulled a lot of water out, still a bit more to go judging by the weight. It actually looks lighter than this in real life, light tan or gold color. If you look at it with a magnifying glass you can see that it's like pumice, from the CO2 bubbles when the citric acid was added. It's kind of like "wax" but crisp instead of waxy and it's CO2 bubbles instead of butane. If you crush a piece between your fingers it powders instead of squishing.
BTW, I tried a larger hit and it's quite potent. I prefer it over crude extract, high-wise and smoothness-wise, not harsh at all. And the sludge I mentioned is obviously what the crystals are laying in with the acetone crystallization shown in this thread. You guys weren't actually smoking the sludge were ya? That must be what makes crude extract pliable, the sludge which is a fairly thin oil, like motor oil consistency. That's why extract only tests out to usually 60-80% THCA, the rest is sludge. Maybe the sludge has medicinal value though, who knows?
BTW, I tried a larger hit and it's quite potent. I prefer it over crude extract, high-wise and smoothness-wise, not harsh at all. And the sludge I mentioned is obviously what the crystals are laying in with the acetone crystallization shown in this thread. You guys weren't actually smoking the sludge were ya? That must be what makes crude extract pliable, the sludge which is a fairly thin oil, like motor oil consistency. That's why extract only tests out to usually 60-80% THCA, the rest is sludge. Maybe the sludge has medicinal value though, who knows?
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outliergenetix
Well-Known Member
it feels like wax because it is wax, aka lipids like i said in my previous post. it will get you high becasueit still has the thc in it and the high will be different because of allt he missing compounts that imo add to the high, but ic yu prefer that high whcih is fine, but really man you are basically pressing the lipids out if rosin if you are pressing it the way that video on gopurepressure doesHere's how it looks after overnight in a closed container with some calcium chloride pellets, which pulled a lot of water out, still a bit more to go judging by the weight. It actually looks lighter than this in real life, light tan or gold color. If you look at it with a magnifying glass you can see that it's like pumice, from the CO2 bubbles when the citric acid was added. It's kind of like "wax" but crisp instead of waxy and it's CO2 bubbles instead of butane. If you crush a piece between your fingers it powders instead of squishing.
BTW, I tried a larger hit and it's quite potent. I prefer it over crude extract, high-wise and smoothness-wise, not harsh at all. And the sludge I mentioned is obviously what the crystals are laying in with the acetone crystallization shown in this thread. You guys weren't actually smoking the sludge were ya? That must be what makes crude extract pliable, the sludge which is a fairly thin oil, like motor oil consistency. That's why extract only tests out to usually 60-80% THCA, the rest is sludge. Maybe the sludge has medicinal value though, who knows?
gwpharms
Well-Known Member
I think that's a urban legend. Started by guys that buy from China and sell in America. Same with cbd from China. I heard they grow hemp in fields contaminated with radiation and toxic metals so as to purify and decontaminate the soil.