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CASW (bye bye acetic, hello to citric)

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dooby

dooby

Rising Star
Hello,

I'd like to share my observations regarding the use of citric acid saturated water for the back-salting of, in this case, toluene pulls...

I have around 400 ml of toluene from final pulls on 180 gr of mhrb...

I made a citric acid saturated solution which took a lot of time as water can dissolve a lot of citric acid and it's a slow reaction...

I started with 75 ml of demineralised water and ended up with 150 ml of a rather viscous liquid...

A first salting of the toluene was done with 50 ml of CASW...

After separation and decanting of the toluene, the CASW is a golden/orange "tea"...

A second salting with 25 ml of CASW didn't seem to be of much use, the colour of the CASW barely changed...

For now, I have only 75 ml to evap - I'm saving the toluene in case I want to try a third salting later on...

Since freebasing is the final goal I don't mind the expected gooyness of the dmt-citrate (and other alkaloid-citrates) - I'm mostly really happy about having much less to evap than when salting with vinegar...

I will post updates as they become available...

Fingers crossed ;)
 
he dooby,

Why did you use a saturated solution? Since there is a maximum of say 2 grams of spice in there. Just adding 2 or 3 grams of citric acid to a 50 ml of water would do the trick as well.
 
Yeah, I already figured that there would be a large excess of citric acid - but everything I've read so far about back-salting mentions saturated solutions (except vinegar which I think cannot be saturated?)... So I didn't want to take any changes ;)

I also didn't have any numbers on dmt-citrate solubility or how much dmt can be salted with a given amount of citric acid - hence my "experiment"...

I could've washed the toluene with much less CASW perhaps, like only a few ml's, but then the changes of the citrate molecules "finding" dmt to bond with would become much smaller?
I remember having to use an equal (absurd) amount of vinegar as the nps to be salted and how long it takes to evap which may have contributed to my decision to saturate the solution...

I was already wondering though if citric acid evaporates with the water, if not, there'll be a ton of excess citric acid left over after evaporation ;) - but not to worry, the final goal is to freebase anyhow...

It's a learning process - I like to experiment a little as long as I feel confident that any "mistakes" I make can be corrected at a later stage - especially if I can't seem to find any hard data...

But thank you very much for your info... I should have put more effort into calculating how much citric acid would be needed to salt a given amount of dmt, but I got confused when reading about 1 M and 1 N solutions and I seriously lack in math skills (I studied languages and only had 2 hrs of very basic math each week - 20 years ago)

Thanks again, I feel a little bit smarter now ;)
 
So...

Evapping always takes a long time :(

I also think evapping might not be the best thing to do as I suspect that some or most of the citric acid will not evaporate but perhaps crystallize?

I am currently wondering if this tek:

Fumarates to Freebase Conversion TEK - DMT-Nexus Wiki

wiki.dmt-nexus.me wiki.dmt-nexus.me
could be modified in order to work on my CASW solution (keeping in mind that it's a full-spectrum yield that I'm after - but if this is not possible I'll settle for dmt-only and go for full-spectrum on another occasion)...

Any help would be greatly appreciated ;)
 
dooby said:
So...

Evapping always takes a long time :(

I also think evapping might not be the best thing to do as I suspect that some or most of the citric acid will not evaporate but perhaps crystallize?

I am currently wondering if this tek:

Fumarates to Freebase Conversion TEK - DMT-Nexus Wiki

wiki.dmt-nexus.me wiki.dmt-nexus.me
could be modified in order to work on my CASW solution (keeping in mind that it's a full-spectrum yield that I'm after - but if this is not possible I'll settle for dmt-only and go for full-spectrum on another occasion)...

Any help would be greatly appreciated ;)
Click to expand...

The citric acid will definitely cristalize, after evaporating you will have a mixture of DMT citrate and citric acid, I would re-base it and pull with naphtha then freeze precipitate if you have the chemicals.
 
Maybe I should...It's a saturated solution ;)

I'll rebase with NaOH, pull with toluene again, redo the citric acid wash again with a non-saturated solution, perhaps 3 x 25 ml of an 8% solution?

And thank you ymer ;)

ps I don't have a freezer yet and my only means of salting the alks out of the toluene are citric and acetic (fumaric is on its way but taking quite long to get here)
 
This is cool...

I made a 250 ml solution of water and 30 gr of NaOH...

I added this slowly to my CASW while swirling the reaction vessel...

At a certain point, clouds would form then disappear again, then form again when new NaOH-solution was added, and so on for quite a while (I added only little bits at a time)...

This was very cool to watch happening ;) lol

Now I'll add some more until the cloudiness persists...

Hands-on learning, never thought it would be so much fun ;)

ps the amount of naoh was "calculated" based on how much citric acid I "calculated" to be in solution ;)
 
i have never heard of base precipitating DMT.
i see no reason why it couldn't be done (given that freebase is insoluble in water), so it will be interesting to see how it turns out (assuming benz doesn't come in and spoil all the fun :d )
 
I could pull from this now milky solution, but according to one of the "fumarate to freebase" conversion teks a "water crystallisation" should be possible...

So my reaction vessel is now sitting in the fridge so I can see if anything happens...

I can pull with an nps at any time, so why not give this a try first, right?

I will also check into sodium acetate as I suspect that this will be formed as well as freebase dmt... Solubility data of sodium acetate should indicate whether or not I can expect any sodium acetate to precipitate or not, or am I mistaken? Wouldn't the equation be dmt-citrate + sodium hydroxide = dmt-freebase + sodium citrate?

I can understand quite a bit of the chemistry I'm trying to study, unfortunately I have not been sufficiently educated in mathematics to apply most of what I've learned so far... Math 101 is on my agenda for the coming weeks ;)

edit - sodium citrate is a food additive, so my "milk" should be good to go as-is (after adjusting pH to consumable levels?) lol... anyway, there are three forms of sodium citrate, apparently the trisodium citrate is most common and it's solubility data suggest that none should precipitate out of this solution of mine ;)
 
After 10 hrs in the fridge...a sight to be seen...

Keeping in mind that this "water crystallisation" is a slow process ;) ...

Bottom: a few millimeters of clear liquid

Middle: two distinct "layers", both milky/white, though with a minor difference in transparency

Top: a thin layer of presumably freebase alkaloids...tilting the reaction vessel makes some of the substance stick to the sides of the container...

There are also little "clumps" forming that are suspended in the solution...

Now, should I add some NaCl to help push the alks out of solution or will this create dmt-hydrochloride as well as dmt-freebase and sodium citrate? And if so, would that be an indication not to add NaCl?

Also, if this water crystallisation works, wouldn't it be possible to precipitate freebase alkaloids out of the basic soup during an extraction, provided that the organic material is filtered out, thus making the use of a non polar solvent redundant? Or maybe this would allow evaporation of acidic solutions that were used for back-salting to be omitted (thus being a serious time-saver)?

I guess someone will come up with some reasons why this wouldn't work - otherwise people would probably be doing it already, no?

I do need to find a stainless steel mesh "filter" that is finer than my tea sieve though, or imagine another way of recovering the alks as I want to avoid having to use a coffee filter...

For now, I'm pretty happy with the way things are going - having everything work perfectly wouldn't be half the challenge/adventure/fun that I'm having by having to solve all the "mistakes" I seem to keep making (lol)...and it makes me appreciate it that much more when things do seem to work perfectly ;)

PLUR

edit - I just found out that I have quite a bit of reading to do regarding this subject, as there are several "old" threads about it...
 
Update...

After sitting in the fridge for about 32 hours the solution was filtered through a steel pipe screen (brand new, cleaned with acetone then water)... The solution is practically clear but there are still some goodies in there... I combined a second batch with the filtered solution and that will be left in there for about 36 hours as well...

The water-precipitated crystals are now drying for weighing purposes then they will be cleaned up further although they already look very nice ;)

As long as it's freebase one is after there seems to be no reason to dehydrate epsom salts or to dry acetone/IPA - no need to saturate either in the case of citric acid...

I don't think I could be any happier with the way things are going ;)

I'm sure my enthusiasm will backfire sooner or later - why hasn't anything gone wrong yet? lol
 
Some observations about the water crystallisation process...

So far, I get the distinct impression that this happens in two stages...

Stage 1: crystals rise to the surface, some are suspended in the solution, a layer of clear liquid may be seen at the bottom of the jar...The transparency of the solution decreases from bottom to top...

Stage 2: most of the crystals are suspended in the solution, some stick to the sides of the container, the transparency of the solution is more uniform...

However little dmt can be dissolved in water, it will be less as the waters temperature decreases...

This got me thinking - could the water crystallisation process benefit from placing the container in as cold as possible a batch while keeping the upper part at room-temperature
in order to "force" more dmt into the warmer upper layer of the solution? By very gradually adding ice to the bath one could start freezing from the bottom up until only a small amount of liquid is left on top hopefully with all the alkaloids in or on it? This might speed up the overall process, as well as facilitating the recovery of the alkaloids?

I'm also going to look into what ways there are to increase the density of the solution without adding any chemicals that would be detrimental to yield or purity...

But my conclusion remains: nps pulls, citric acid salting, add NaOH then water crystallise - big smiles ;)
 
Apart from what is mentioned in my previous posts...

So far I have 1.35 gr of crystals - not completely dry yet though...

The looked very white but upon scraping them together they did get a golden tinge...

This is coming from pulls 4 and 5 with toluene on 180 g of mhrb...
Pull three is still trapped in acetate goo ;)
Pulls one and two were done with warm naphtha and yielded 1 g in the fridge (spice that wasn't precipitated out in the fridge is transferred to next extraction)

What I yielded so far from the water crystallisation was filtered out after 32 hours in the fridge - the filtered solution was combined with a fresh batch of basified citric acid (from pull 6, toluene)...

The really convenient thing (as is the case with fumaric, I presume) is that you have confirmation of having pulled something practically immediately - no need to freeze or evap - as soon as the base is added to the acidic solution you'll see if anything is in there and whether or not doing another pull is worth the effort...

Btw - the tek I followed (until the toluene pulls) was more or less Cybs hybrid salt tek...
 
Have you tried the product to check potency? (aka it's only dmt and no other sub products from the basing)
 
Well, I haven't yet completed the cleanup process...

I was warned that my crystals would be contaminated with base so I did a recrystallisation on the first crystals I retrieved and they were indeed (quite heavily) contaminated with lye...This may be due to the process itself or to my choice of reagents or the amounts of reagents I used... Perhaps a simple water wash (pinch of sodium carb or bicarb?) would have also been okay...

At that point there were still a lot of alkaloids left in the solution - knowing that they wouldn't come out clean anyway I decided to pull them from solution with an nps...

I did a few naphtha pulls and the solution became much clearer...

I then noticed that something reddish was floating on the water but not being pulled by naphtha... I did some toluene pulls until the red was gone and evaporated those...

The naphtha are in the fridge until my new freezer arrives...

The evaporated toluene pulls smell much nicer than regular dmt and have a golden orange colour... I know my toluene evaps clean but I might do an acetone re-x nonetheless to make sure there's no traces of toluene (or base) in my final product...

I have a small batch of water-crystallising dmt in the fridge - after 5 days the solution is practically clear so I'll filter out the crystals and compare to previous results as this batch was done with sodium carbonate and the first attempt was with NaOH...

PLUR
 
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