Well, i start saying that im not a Ph D chemist. Soo dont judge me please haha. This is all test and dont consume and dont sell nothing to nobody.
I make some test adding after the extraction and before evaporation under vacuum at no more than 40 Celcius a little of Ascorbic Acid, in the first instans was a test for prevent oxidation of some elements and dont turn red the finish extraction. After evap i do a LLE with Dieth ether or Pentane to wash the acid . i like more the Diethyl , i think is more noble if something happen if i Smell accidently. I work in a fume but… never knows. a lot have afraid with the peroxides…i work no more than a liter and in years never have an issus…always fresh solvent. I have the teory that maybe some water soluble terps that the etoh carryer can migrate to the dieth. i do fresh frozen extraction in this form and have a really nice tranlucens yellow xtract that cristalizat easy whit a incredible smell. is too much work with eto and fresh frozen but…is good. And with dry material is still yellow the extract.
Details…After xtracted eto reach RT i add the acid, wait to dissolve and to the roto. When is finish the evaporation… i can see a precipitation…and separation, form a white milky water and and oil seperaration and more if is fresh frozen. I throw to the funnel add satured water shake as hell and add the Dieth. i do 3 wash in total. then i dry more with anhydrus sodium sulfate decant,filter evap fast or play with crystalization. The color and the smell in insane…the clarity …and crystalizat really fast. i dont use any media ,carbon bentonite nothing of this.
My doubt is if this procces can change the molecule of some terps or cannabinoids , or make something toxic or nasty, i never heat more than 40 celcius, i want to not pass the temp of the growing room in the procces for future extraction… if is can still doing the acid aproach.
maybe @Photon_noir can says me something, i know there are a lot of smart with a lot of chemitry up and more… but i dont want to bother all the brains here jeje.
I think you may be seeing an (for you) unanticipated benefit of using ascorbic acid. In addition to being an antioxidant, it is an acid, and as such forces the THCa to its protonated state.
Pretty sure there are patents describing the benefit of < 1% acetic acid in the butane.
Thanks for the reply, yes i read that text before and give me the impuls to try this. I know that state protonate the thca, but maybe something else can interact in a negative way, i dont have analytic to do. … is a weak acid and i dont apply heat , and wash rigurosly the ether layer… Thanks again
Hopefully not too much ascorbic acid ended up in the organic phase, but if so, the bulk of the crystalline material may still be THCa. An interesting solvent when dealing with THCa is reported in a “proto shatter” patent by Jeffrey Raber; MeCN or acetonitrile.
I found a paper studying the solubility of ascorbic acid in a range of solvents, among them MeCN; J Chem Eng Data v53, p1332 (2008)
Thankss friend, Can you tell me where i found that paper? I search a lot if the AA is soluble in ether or pentane but is aparently not, at last what i can read. The ether carryer more water than Pentane, i focus a lot to drying very well, if is still acid present after the wash and the ether is wet they will finish in the extract. Pentane is best for this reason but…
In the next batch i will do some tasty test …maybe …a little dab for science… we know
Start by googling j chem eng data. On the journal’s homepage, look for the all issues button. Find the right year and/or volume. Find the issue with the right page span.
The article you’re looking for is in that issue. Scroll until you find it, click on it. You are presented with the article data and look for a link that typically has doi.org in it. It’s usually a garbled-looking string of mostly numbers. That is the article’s Digital Object Identifier.
Publishers have started trying to hide the links, and for some journals you have to look for a citation button.
Copy the whole URL, if given, or just the link. Go to one of the Sci-Hub servers, sci-hub.se is almost always up, and there are several mirrors. Paste in your link.
It is really not clear what you are doing in the first extraction step.
if the material is dry, you have 8-10% water in biomass:
if it is fresh frozen you have about 76% water in biomass.
So the percent water in EtOH is variable.
When you get to the RoomTemp EtOH “add acid” step, Are you adding “Ascorbic Acid”
in the Acid Form or as a salt like Calcium Ascorbate. The difference is considerable concerning the pH of the resulting solution.
How much “ascorbic acid” do you add?
The pKa’s of the THCA and Ascorbic acid are about 3- 4. You are just going to end up buffering
you extract solution…but the predominate form will be in the ionized state COO-.
I have pointed this out in a number of discussions concerning butane extraction.
It is not that you can not do a butane biomass extraction or LLE into a nonpolar (some how it clearly works") which means the conceptual details of what is going on are flawed. I have proposed ion pairing or carboxylic acid dimerization as the mechanism. Also a number of monoterpenes may act as detergents. In this case you have added a considerable amount of Ascorbic acid which may result in a heterologous carboxylic acid dimer state
which extracts into the ether or pentane in addition to suppressing ionization.
Dr. Jerb, cyclopath, rioplek et al. need to think about this as well. It really involves a conceptual error in the foundation of thought concerning butane extractions.
The latter is off topic a bit, but when you add ascorbic and LLE into pentane we are talking the same conceptual problem.
One further question:
You rotovap, “throw to the funnel add satured water and shake”
do you mean: add water saturated with sodium chloride or do you mean presaturated with diethyl ether? Then you rextract that liquid emulsion with diethyl ether?
You are doing something VERY INTERESTING I am just trying to figure out what.
Hi thanks to you for the extend message really apreciate.
I extract whit grain alcohol 96% at -70 celcius. Always is some water present and from condensation . I do in “open air” the extraction.
Is Ascorbic acid pure not an ascorbate. My test i put 100 mg per liter of extracted eto. Yes i add satured sodium chloride water shake, and then the Dieth.
The oil out and floating in the milk. In the past whitout acid i make washes of low ph water to a pentane layer and the water out red/brown, was really nice but still finish orange red.
With acid , more clear solution with no reds/browns compared with my prior extractions, its more, in one test i pass the time of soak and the etoh warm a little more that i want and grab a litlle green but no red or dark finish in the extract, the xtract finish yellow and have a green reflect. so is the same principie i think but maybe with a plus, and maybe is for this reason that crystalization to me go more fluid and faster compared with… again… my prior extractions.
Is knowing that ascorbic acid prevent browning in some juice and drink industries and act as a redu agent. MaybeThe alcohol in the moment that reach RT is start same oxidation, is what i add the acid inmediatly make the filtration of the extraction when is still really cold ,one time i put the acid befor make the extraction at -20c, and then LLE pentane and finish with yellow gold.
Playing and a little with my common sens, i imagine that maybe i can do the low ph wash and at the same time prevent oxidation of elements in the solution and preserv the most terp posibles switching to Dieth.
When i can i will like to do a more rigorous comparation in real time with 2 extractions and strict some parameters.All this was made “in the air”
Now i switch to the cellphone i show some photos
Is not my native lenguaje english i efford to make me understand for more traductor that i use
Thanks to you for “help” to deduct this crazy ideas. Like i says… iam not a “real” chemist. Maybe just was coincidence in some parameters and is a ilusion, like i says, was all in the air . But for me something help, for sure a wash ph low always help and if is that really help for more clear non oxidation and fast crystalization…i love to do análisis for view all de detalis.
I forget to put some fotos…
This was with out ascorbic acid in the etoh. This was pentane , washes with citric acid at ph 3 and then ph 9 with sodium hidrox
And this is adding the ascorbic acid before the extraction and do at -20 or - 40 celcius dont remember well, then switch to pentane…this have a bentonite scrub too . ( But i dont think help in nothing i dont like uses of clays )
And what if i heat the ethyl acetate near to the boiling point and satured with sugar, and then slow down the temp in 16 hs at RT? I imagine what maybe can happen… I want to try this with turpentine to.
Edit- the turpentine not to the boiling point…of course
