Need Help water layer came through Lime-tec with Limonene

[plumsmooth]

My Friend went to try and finish up an old in-completed extraction which was bascially a lb of MHRB with Lime and Limonene Soaking. When he decanted a thin water layer appeared and settled to bottom of quart mason jar. He made mistake of not getting rid of the water I believe.

During FASI water layer appeared to grow; and although huge clouds formed, they quickly dissapated leaving rather clear Limonene. However the bottom layer got darker. More FASI was added and more clouds formed and once again disapated. There is a light coating around jar of spice but not nearly enough to account for what should have been.

Conclusion: 80% or more of spice is now in the bottom layer of water and possibly IPA. Since he read that one can clean limonene-FASI with water -- this is why it is believed that the FASI is moving to the bottom with the water carrying the spice that would have otherwise precipitated upon FASI drops.

Trying to figure out best way to retrieve and clean up the lost spice.

One Idea: Decant Limonene, collect what is on jar sides, then add more water to make sure any spice still traped in Limonene moves together with FASI/Water/spice layer.

Then separate in separatory funnel and evaporate water/FASI/SPICE layer.

Then should have spice and fumaric acid and some impurities carried over from MHRB through the water.

Unsure at this point.
Please help...
Thanks for your time knowledgable ones...

 

[endlessness]

Your plan sounds good. Separate layers, wash with more water, evap water to have dirty fumarates, and proceed to clean up (for example, freebasing it and doing FASA or FASI to get cleaner fumarates, or recrystallizing with warm IPA or acetone)

 

[plumsmooth]

I had thought to add water before separation in hopes that would encourage anything (fumarates) left in the Limonene to move out.

So would your FB Water crystalization be an acceptable move with the dry dirty fumarates.

Or since Clean Fumarate Salts are my final hope could I simply redissolve dirty fumarates into clean limonene.
OOooops i guess it will not dissolve, ha ha that's the whole point of FASI.

So it looks like I have to go back to FB HUH?

Then back to Fumarates.

Any recomendation as not to lose as much as is lost with the Water Crystalization technique.

That is the only one tried thus-far in my friends experiments.

 

[endlessness]

I think better not do the water crystallization now. Making paste with sodium carb or calcium hydroxide and pulling with acetone or IPA and adding FASA or FASI is better I think, to clean up the fumarates. Whatever you try in the end, you can try with half your product in two different ways to compare and let us know!

 

[plumsmooth]

Got it thanks a lot!

I'm sure I'll find the paste method in the tec department.

Thanks again!

P.S. Do you think the water was simply from TOO much of it in the Lime phase?

I'm wondering if the Fumaric Acid will alter the paste making process.

I'm wondering if there isn't a way to pull the spice away from the Fumaric Acid by disolving into something that isn't welcoming of the Fumaric.

 

[plumsmooth]

Trying to figure out how exactly one can actually lose the excess Fumaric Acid at this point.

Since it is soluble in IPA it seems pointless to try to convert to freebase using Sodium Carbonate becasue the fumaric will just come back with the spice?

Read a tec suggesting water washing but I believe that Fumaric Acid IS solable in water so I am confused about that option.

Purification of Spice Fumarate Product - DMT-Nexus Wiki

wiki.dmt-nexus.me

Anyway my friend will proceed to lose the lower possibly water/dirty spice layer.

IT is further confusing because it doesn't appear that all the IPAFumaric Acid has necessarily mixed with the bottom layer either.

 

[endlessness]

Separate the layer, and do a couple of further pure water washes. Get all the water together, evap. Add sodium carbonate and a bit of water (or add before its totally evapped and keep drying at low temperature), mix well, and let it dry, under 80c, till its totally dry. Pull with dry IPA, which should pull alkaloids but not sodium acetate (which will have formed in the mixture of excess sodium carb to fumaric acid). Then add FASI to it to precipitate purer alkaloids.

 

[plumsmooth]

Ah Ha I had just started searching which I should have done before the questions.

I found reference to that Sodium Fumarate situation.

And I also see a freeze precipitation IPA technique: Do you see any place for this with the clean-up attempt...

OR is this something only to employ without Sodium Carbonate.
MEaning sodium acetate and Freeze precipitation is contradicted some how.

One thing, when you say add FASI after pulling with IPA I'm not sure what you mean.

Do you mean redissolve in Limonene then FASI...

Thanks again...

P.S. It almost looks as though could dry then go straight for a Freeze Precipitation with the Boiling IPA tec?

 

[endlessness]

Ive had mixed experiences with the recrystallization... I've had once where the fumarates would hardly dissolve on warm IPA and I had to add a lot of it, and then when freeze precipitating, only very little came out. Other people had more experience.

When I say add FASI after pulling with IPA, no there's no limonene involved. You have only your evaporated water pulls which yield crude fumarates, then freebase that as a paste with sodium carb, pull 3x with warm IPA and put it together, and add FASI to the IPA pulls, and your cleaner fumarates should crash out

 

[plumsmooth]

Got it, I guess then it is not necessary for the IPA to be fully saturated with Fumaric Acid for this technique to be effective.

one more thing if I may:
being that no more clouds are forming in the Limonene upon droplets of FASI,

then wouldn't it be safe to assume that there is no spice left in the limonene and that all of what didn't precipitate (and at least a gram did out of an lb of MHRB) is in (if any) the bottom dark water layer.

So thinking why add more water and pull any excess fumaric acid and IPA left in the Limonene>

Thinking just separate and dry?

 

[plumsmooth]

So may I ask is the final process to simply FASI the IPA and the same effect will happen as Limonene being added to?

In other words will the crystals stick to jar and be collected in the same fashion.

Thanks...