im doing a 200 g extract using vovins formula

vovin calls for 100 ml per pull x 3 for a 50 g extract 600 ml total if you have to split your acid extract

using this much solvent i end up with under saturated solvent, as i dont like to evaporate solvent im wondering two things...

what would the ideal volume of solvent be per pull on a 200 g extract using vovins a/b method?

can i instead of cutting down on solvent use, salt my dmt by mixing my solvent with an hcl solution. discard my NPS, basify my acid and do small pulls with NPS until i know ive extracted all the goods...?

please help this is kind of an urgent issue as i dont have much time to finish and i would like to know whether i should evaporate my solvent or just salt it out like i said.

40-50ml solvent is about right for a 50g bark xtract. If you have a lot of solvent already pulled. You can evap it down (with a fan) until its around 50-80ml and then freeze.

on a 200g bark...80-100ml would be OK per pull...the less there is ...the more it saturates.

I wouldn't bother salting...the goods are in the solvent..you just got to freeze them out.
Just keep pulling till nothing precips anymore...then youre done..

i dont like to evaporate my solvent. klean strip brand vm&p naptha. as i find it becomes discolored after heavy reductions. im not trying to concentrate the impurities. ive tried 100 ml pulls which do work, and i can freeze precipitate. but i like the idea of salting my dmt out of the naptha then using smaller pulls on a concentrated basic solution. has anyone tried this? any reason it wont work?

It should work...but if you've already A/B 'd then, effectively...you are just doing it again.
You could always split the mix and try it on half...experiment.

The colouration of the product can be remedied later with a Re-x..

edit: most peeps are asleep right now..so it may be a while before a definitive answer comes.

yes, i realize its kind of a round about way to get there. but it allows me to use large volume of solvent on my initial pulls to guarantee ive pulled everything out. and ive assumed that if im working with just solvent and clean solutions i cant shake the shit out of my funnnel and i wont form emulsions. so it should go rather quickly. kinda like solvent washes

The addition of regular salt into the basic mix will increase the ionic strength and negate any emulsions...also increases yield in the first few pulls....if that's any help

no, im saying i dont think it would be a very long or involved thing to do because the separations will occur so quickly. will probably take less time than evapping half my solvent. im worried that if i reduce and rex, the contaminants from the reduced solvent will stick to my xtals then during my heptane rex the oils will pool and condense but could also contaminate my goods. i get beautiful white crystals from freeze precip when i dont reduce but when i do they turn more yellow.

yeah sure it should work to salt out with an acidic solution, base and pull with small amount of warm solution.

In any case the solvent becoming "discolored" during reduction should not be any problem, you freeze and it will probably come out pretty clean because most impurities will stay in the solvent even at freeze temperatures. And even if not, you can always re-x later on.

But yeah you can do as you planned.

thank you, endlessness. i figured it would work, i just needed some confirmation. but i guess people do similar things when working with wider spectrum solvents like xylene. as long as i dont lose a big chunk of my dimethyl i think this is a nice solution for people with too much solvent. you could collect the solvent from a few extracts do a mini a/b, then have one big collected freeze precip container. which has always seemed attractive to me .

so is there any chance that my aqueous solution could become too concentrated to basify. when i basify my acid solution lots of chunks form. usually they go away. is there some chance that there isnt enough room for the reaction to fully occur if i concentrate my acid too much? currently looking at at a few inches of freebase chunks sitting at the bottom of my 2000 ml sep funnel. uhhhh

what base and acid did you use?

Could be some less soluble organic salts, could be some dmt freebase precipitating. In any case if you mix with a non-polar, DMT should dissolve in it and other salts shouldn't. Maybe do it warm by heating with a water bath (no fires on!) to help the alkaloids dissolving in the solvent

i've used lab grade HCl 33% dilute to pH my water to 4 for the acid extract. then i used lab grade NaOH to basify my water to about 13.5... mixed my acid solution with my basic water and tons of big white chunks precipitated and fell to the bottom of my funnel. unfortunately i've filled up my 2000 ml sep funnel without getting the pH above 12.5 so i will need to split the volume up to add more base and the NPS. if i remove some of the basic water and add more base will these chunks go away or are they going to chill in there until i start pulling with NPS. this question also relates to my idea to salt dmt out of naphtha... if i end up with a super concentrated acid solution with grams of dmt in it will i be able to convert all the salts to freebase. by adding an equal volume of base to the acid? or will i need more "room" maybe split my acid into three or four batches... basify and do small pulls until i've exhausted my solution

either way it was quite a show watching those chunks fall to the bottom of my funnel.

should i split it up and add more base? will the chunks go away? or is it nbd if there are solids hanging around before your first NPS pull?

don't worry about it

What are the impurities? Are they in the yellow?

Is there another way besides freeze precipitation to remove them?

Necrobump alert! Double AA was replying to a nearly 11-year-old thread. OP should have resolved issue by now...

Darn. I am sorry about that.
This thread just came up as new when I was pondering the very question it covers.
I will go ahead and ask questions if I may, and will delete my post if need be. let let me know.

Since most or all the beginners instructions out there use Naptha, and since klean strip is the one you always see, it's likely that many extractions are using it. It's also likely that many people are evaporating since the freezer method can get smells in your food.

First. Does it matter, evaporating? Is it really something to worry about?

Is there any other way to clean up Naptha extracted/evaporated DMT? If you pull into water and then pull off that to clean up, does that have any effect? Is there a further water wash you could do once evaporation is done?

Does re-xing and precipitating with the same type Naptha clean it up? What if you used a very small amount of Naptha to do that? Would it clean up? Has anyone used an ice bath successfully to do that?

Let me know if I should delete this addition to the necro thread.

It's fine to continue when you've relevant matters to consider

Re-xing from the same solvent is fine (assuming the solvent evaporates cleanly), as long as you understand that recrystallisation in the true sense of the term involves only the differential solubilty over a temperature range. Redissolving material in naphtha and then evaporating it all does not count as recrystallisation! You clearly already appreciate this given your question abou ice baths, which I can answer in the affirmative - it will work, although in my case I was experimenting with aqueous ethanol as the solvent. To that end, you could in principle use vodka if you can make a decent freezing mixture, like crushed ice with calcium chloride hexahydrate for example.

What I did find with vodka is that the redissolution temperature is quite near to the usual minimum temperature of a domestic freezer, so it's necessary to drain the solvent off as quickly as possible and preferably somewhere as cold as possible.

Another clean-up method is the mini A/B - this should be self-explanatory but it is described in various places around the forum and wiki.

OK. Thanks so much.

I do have another question, a bit off topic. I can't seem to find the answer to this one.

In a straight to base you would pull the sludge 3-5 times.
If you then let it sit overnight, possibly adding more lye, would things degrade? Does the extremely basic solution break down the desirable stuff? So, could you just do 3 (or so) pulls a day until you reached diminishing returns?