Preparation of crystalline THCA

[SkyHighLer]

I've been avoiding this discussion since the product wasn't being personally put before me, things change... pics from the 3rd Annual Chalice California 'hash oil' festival yesterday.

I bought half a gram of the 'pure' THC-A crystals, and was given a half of the 95%. No taste or flavor with the first, and just a slight awareness of something flowery with the yellowish, sandy less pure stuff. No stand out effect after a couple of hits of each.

Sorry some of the pics are sideways, I didn't upload them that way... and yes they 'add terpenes' if you so desire to your pure THC-A crystals with that that there glass pipet thingee. They were even blowing out terpene holy water out their tent's mister system... gettin' them terpenes from somewhere/how..... ;-)

Such a slam down today hitting the crystals hard for the first time since I acquired this pure crystal 'stuff.' Full eyes shut at the mercy... where is it you guys want to go with other terpenes, THC alone delivers, I'm writing this without a desire to turn to my side and dab some oil, Tom Petty's singing out in the wide open.... Pandora rocks! Pounding! brother's and sisters, kudos to The Guild.

I'm fixing the previous post's sideways pics, seems to have been my bad, sorry.

So, in the pictures of my outing with my Health Stone sherlock and the crystals, the pic of the lid isn't legible, it reads, "EST. 2000 GUILD EXTRACTS where art meets science"

I have seen the lab test results, talk about how many 999's and zips, so I assume the extremely brief initial 'chemical smelling' impact is indeed just the THC saying good bye way too fast under the torch on the HS. The 'chemical smell' is instantaneous, and fully disappears, leaving you to experience the trip.

About 0.025g completely cleared in one hit was plenty for me.

 

[Digital Man]

Such a slam down today hitting the crystals hard for the first time since I acquired this pure crystal 'stuff.' Full eyes shut at the mercy... where is it you guys want to go with other terpenes, THC alone delivers, I'm writing this without a desire to turn to my side and dab some oil, Tom Petty's singing out in the wide open.... Pandora rocks! Pounding! brother's and sisters, kudos to The Guild.

I'm fixing the previous post's sideways pics, seems to have been my bad, sorry.

So, in the pictures of my outing with my Health Stone sherlock and the crystals, the pic of the lid isn't legible, it reads, "EST. 2000 GUILD EXTRACTS where art meets science"

I have seen the lab test results, talk about how many 999's and zips, so I assume the extremely brief initial 'chemical smelling' impact is indeed just the THC saying good bye way too fast under the torch on the HS. The 'chemical smell' is instantaneous, and fully disappears, leaving you to experience the trip.

About 0.025g completely cleared in one hit was plenty for me.

Looks like Crack ............. good luck explaining that one.

 

[Old Gold]

Looks like Crack ............. good luck explaining that one.

Sounds misinformed.
I've made sugar candy that you couldn't tell from the finest cocaine freebase.
The premise of your "it looks like crack" statement assumes that all things clear and crystalline follow the trend of crack cocaine. When in reality, crack cocaine follows similar trends as other crystalline substances.

And now, for relevance's sake, back to THCa....

 

[PoopGroup]

Nice post Old gold

 

[SkyHighLer]

I hadn't actually noticed how off white it is, contrasted against 'rock candy' (sugar crystals.) Never had any crack, wouldn't know... ;-)

 

[SkyHighLer]

My life revealed, laugh your ass off!!

Life was kind enough to provide me with this stuff, so I calibrated my soldering iron dab station, and checked out how this stuff behaves from 400F/204C to where I found it was sweet and stoney at 585F/307C, my new low end preset with the Hakko-FX888D.

A video at 400F/204C would be so much more a time sucker than just trusting me that the pictures showing a pool of oil just sitting there forever, really is just that, the oil right at about the lowest temp anyone would call a Bp at atmospheric. And the smell, almost like ammonia, better to get it over with at higher temps... in my nose's most humble opinion! But like I said in the previous paragraph, 585F/307C was as high as I needed to go, and after that is was obviously downhill with regard to smell. I've never thought that about any other oil, usually there is a broad higher range extending to my max preset of 710F/377C.

 

[SkyHighLer]

THC-A crystal pics via the little digital camera shown in the last post. The yellow globs in the crystal pics are the much larger pieces, same stuff.

 

[SkyHighLer]

Went out and spent more time with the crystals, I'm a THC addict, parfum terpenes are for wussies.

Spoons like snow, the rocks break up easily without mess, but the dust doesn't stick to your fingers - what clings is just a dry powder when you rub your fingers together. And when you do rub your fingers together firmly, putting some sweat and body oil into it, you can still feel 'grit.'

Btw, it oft times 'pops' depending on the size of the chunk and the temp, leaves flakes behind...

 

[SkyHighLer]

I much prefer the 99.99% crystals to even this 96% flake.

Doesn't take much to drag down the clarity of the high imo, you want to dream, add the terpenes back in.

 

[99.99 thca]

Do anyone could write the hole process again, ive got the part of the slow evaporative crystallization and the concept of Column Vacuum Chromatography as well, i can have access to all kind of machine, could anyone help me please?

 

[PoopGroup]

LOL the weed version of script kiddies

 

[SkyHighLer]

I went back and read this thread and weedaholic721's.

Two thoughts I held previously, and didn't see addressed;

I saw both fractional distillation and rotovaps being offered at Chalice...

You can't use heat obviously, and still have THC-A, but with all the interest in getting the biggest, baddest vacuum pump, scroll or whatever... is it practical to pull off the THC-A, at let's say, near room temperature or lower? If the Bp of THC is 70-160C @ .005 mm Hg, as the attachment indicates why wouldn't the THC-A crystals possibly pull out of solution? Check out my THC Bp under vacuum chart, hey I know it's off... but really, no one else is supplying solid data, huh!? ;-)) As you can see on the chart, .005 mm Hg is way, way down there, the bottom line is zero molecules, and is actually quite a distance from the second to last line as these are 'rough vacuum' numbers, those down to about .001 mm Hg. Dry scroll vacuum pumps can just about get you down to those levels.... 70C is 158F, not decarbing fast at that temp I assume as I haven't seen evidence of low temp decarbing under vacuum, decarbing is a temperature reaction, basically independent of vacuum, immho..... So, drop the temp down a little more, just until you still have a liquid solution of what you've previously isolated to primarily THC and THC-A, 120F or thereabouts, and then suck the life out of it. Use a decent micron meter. Pray for crystals. I know nothing... I just haven't heard that anyone's done it, and that nothing interesting was observed. Be suspicious of what should be known and isn't! This is new territory, do an online search for THC-A, ain't much.

Since isolation of a pure THC-A solution with some (hopefully reusable) filter material(s,) beads, or whatever seems to be the first obvious direction to check out,

GW, how about Joe's experiments there at SP? I remember you relating many moons ago he was figuring out the correct filter grades for a commercial product package we could experiment with.


Marijuana Red Oil Extraction: Page 11, "the Pyschedelic Guide to Preparation of the Eucharist in a few of its many guises" as edited by Robert E. Brown & Associates of the Neo American Church League for Spiritual Development & Ultimate Authority of the Clear Light, 4th edition, 1975

 

[DrNibs]

more questions then answers as always

 

[DrNibs]

anyway recrystallization is the essence of purification, first find a solvent that will dissolve the solid whilie hot, 2nd the same solvent should not dissolve it while cold, 3rd the cold solvent must keep impurities dissolved in it forever, otherwise your looking at a Mixed-solvent Recrystallization.

 

[G.O. Joe]

The 70-160° number is for "crude red oil". It's very active and full of crap. The full paragraph from the second reference seems off the topic but it's a lesson that shows what people who aren't really learned in the art tell everyone - the finer points are missed. It doesn't really matter since it seems that no one believes anything an Adams or Mechoulam says about anything, especially if someone in the business says something different.

Purified Red Oil.- The ethanol from 4 liters of ethanolic hemp extracts (25% solids) was removed by distillation. The residue was subjected to steam distillation to remove terpenes; after the collection of about 8 liters of distillate, the distillation was assumed to be complete. The water-insoluble residue was separated from the water, dissolved in petroleum ether (b. p. 30-60°) and the solution extracted three times with water. After evaporation of the solvent, the oil was distilled, b. p. 70-160° (5 X 10-3 mm.), with the temperature of the still varying from 180-250°. Care was taken in this and subsequent distillations to stop the distillation the moment gases appeared through the apparatus, indicating decomposition. About 300 g. of crude red oil resulted. This was dissolved in petroleum ether, washed with water, the solvent removed and again distilled through a heated carborundum-filled column (35 cm. long with outside diameter of column 23 mm. and of sidearm 12 mm.). Two fractions, about 30 g. each, were separated, one b. p. 70-130°, the second b. p. 130-150° (5 X 10-3 mm.) from which solid material crystallized on cooling (probably nonacosane). When all of the distillate from which solid crystallized had been removed, the fractionating column was replaced by a still head with sidearm of 15 mm. diameter and the material, b. p. 148-160° (5 X 10-3 mm.) (still temp. 180-230°), was collected. It was a clear, light red viscous oil weighing 200 g. and will be designated as "purified red oil."

Solid THCA has barriers to vaporization that THC doesn't, so THCA will have even less volatility than this mostly-CBD hemp oil. Presumably measurable in some way, so vacuum sublimation of a detectable amount should be possible after a long time, with the condensing surface right above the evaporating surface. Maybe a little air going through a porous surface finely coated with THCA, with the right collection unit? All of the available choices for summing it all up in a word are kind of negative, but I assume there are relevant patent claims.

 

[Chimera]

It doesn't really matter since it seems that no one believes anything an Adams or Mechoulam says about anything, especially if someone in the business says something different.

Believing almost anyone in the industry over Mechoulam, Adams, Brenneissen is a mistake!

 

[SkyHighLer]

The 70-160° number is for "crude red oil". It's very active and full of crap. The full paragraph from the second reference seems off the topic but it's a lesson that shows what people who aren't really learned in the art tell everyone - the finer points are missed. It doesn't really matter since it seems that no one believes anything an Adams or Mechoulam says about anything, especially if someone in the business says something different.

Purified Red Oil.- The ethanol from 4 liters of ethanolic hemp extracts (25% solids) was removed by distillation. The residue was subjected to steam distillation to remove terpenes; after the collection of about 8 liters of distillate, the distillation was assumed to be complete. The water-insoluble residue was separated from the water, dissolved in petroleum ether (b. p. 30-60°) and the solution extracted three times with water. After evaporation of the solvent, the oil was distilled, b. p. 70-160° (5 X 10-3 mm.), with the temperature of the still varying from 180-250°. Care was taken in this and subsequent distillations to stop the distillation the moment gases appeared through the apparatus, indicating decomposition. About 300 g. of crude red oil resulted. This was dissolved in petroleum ether, washed with water, the solvent removed and again distilled through a heated carborundum-filled column (35 cm. long with outside diameter of column 23 mm. and of sidearm 12 mm.). Two fractions, about 30 g. each, were separated, one b. p. 70-130°, the second b. p. 130-150° (5 X 10-3 mm.) from which solid material crystallized on cooling (probably nonacosane). When all of the distillate from which solid crystallized had been removed, the fractionating column was replaced by a still head with sidearm of 15 mm. diameter and the material, b. p. 148-160° (5 X 10-3 mm.) (still temp. 180-230°), was collected. It was a clear, light red viscous oil weighing 200 g. and will be designated as "purified red oil."

Solid THCA has barriers to vaporization that THC doesn't, so THCA will have even less volatility than this mostly-CBD hemp oil. Presumably measurable in some way, so vacuum sublimation of a detectable amount should be possible after a long time, with the condensing surface right above the evaporating surface. Maybe a little air going through a porous surface finely coated with THCA, with the right collection unit? All of the available choices for summing it all up in a word are kind of negative, but I assume there are relevant patent claims.

Thanks G.O. Joe... another conjecture to be disproved was raised recently, what happens when you put a liquid THC/THC-A solution in a centrifuge?

As to the wicked ass book I posted a scan from, I have nearly the entire book scanned and posted up at another forum, if anyone's interested I'd be glad to post it up here...

Cannabis related sections from the Psychedelic Guide to Preparation of the Eucharist,

http://www.tokecity.com/forums/show...rom-the-past&p=1316394&viewfull=1#post1316394

 

[G.O. Joe]

I have zero experience using a centrifuge and passed up buying a few used units because of a sinister smell inside.

So about those THC syntheses. This is the sort of thing I'm talking about - b.p. was my earlier reference exactly - the first synthesis from citral does not produce any d9 THC, more like 10% yield each of + and - trans- and cis-d8 THC as "a resin which was separated by preparative vpc" from other garbage. Wouldn't you like to know that? A person with scientist aspirations should be naturally disinclined to such shadiness.

There are no exact synthetic details in their first reference, so it's unclear where the numbers come from. An improvement was published in the same journal (6159, 1972) using 1% BF3, giving 35% +/- trans d9 THC and 15% +/- cis d9 THC.

There are a few different syntheses involving pulegone and olivetol but it's not clear where that second synthesis comes from or what it makes, but it's not (-)d9-trans-THC. A better place to start searching for the primary literature to actually use:
https://www.erowid.org/archive/rhodium/chemistry/psychedelicchemistry/chapter2.html

Another note on the volatility of THCA - someday the cartels will realize that dogs can't find THCA. THCA might be the next ice.

 

[SkyHighLer]

"Legal status
THCA is not scheduled by the United Nations' Convention on Psychotropic Substances.

United States
THCA is not scheduled at the federal level in the United States, but it is possible that THCA could legally be considered an analog of THC and sales or possession could potentially be prosecuted under the Federal Analogue Act.

There is also a practical legal issue of potential THC contamination of THCA which should be considered. As mentioned above, THCA decarboxylates to form THC, a Schedule I controlled substance. As such it is somewhat unlikely that any sample of THCA which may be analytically tested will not contain a quantifiable amount of THC, especially if the sampled product was retained at temperatures conducive to decarboxylation. This makes it likely that possession of THCA could get someone prosecuted for possession of THC due to contamination of the THCA with THC."
https://en.wikipedia.org/wiki/Tetrahydrocannabinolic_acid#Legal_status

My sample of 99.997% THC-A doesn't appear to be rapidly decarbing at 80F+ temps. Shouldn't the 'dust' in the jar be getting gooey and amber colored?

Thanks for taking a look at the synthesis formulas, I've never come across what I believed to be real synthetic THC, just assumed it must be too demanding in knowledge, resources, or patience. Interesting link brother, written by a water brother indeed, lol.

 

[G.O. Joe]

When I isolated THCA years ago by acid/base extraction, it was left on a plate next to a window for many weeks and if any THCA changed, it was to CBNA and some probably did. All of the federal and probably state laws that specifically name cannabinoids never mention the acidic forms. If it's natural acid it's marihuana though. And there is

tetrahydrocannabinols naturally contained in a plant of the genus Cannabis (cannabis plant), as well as synthetic equivalents of the substances contained in the cannabis plant, or in the resinous extractives of such plant, and/or synthetic substances, derivatives, and their isomers with similar chemical structure and pharmacological activity to those substances contained in the plant,

DEA has tried in sneaky ways to use that to make hemp illegal and also add new wording, they also tried to add cannabinol and cannabidiol by name as a new entry for extract in 2011. In other words a random judge would be likely to rule that synthetic THCA-A and B are tetrahydrocannabinols.

Stranger, more obscure, less interesting legal detail: hash and hash oil are not hash or hash oil, for the purposes of federal sentencing, unless either CBD or CBC is present.