Question 1) I can't seem to find an explanation for the reason that Sodium Hydroxide (Lye) and Potassium Hydroxide cannot be used for basing when pulling with d-Limonene, Xylene or Toluene for FASX. What would happen if you do and why?

Source: https://wiki.dmt-nexus.m.../Lime_A/B_Extraction_Tek

Question 2) The official statement is that if your NP solvent precipitates out Fumaric Acid, it cannot be used for FASX. But what would happen when you do a mini A/B on a Naptha pull using water acidified with Fumaric acid, then seperate and evaporate the water? Won't the DMT travel down from the NP into the acidic solution just like it does when an other acid is used for a mini A/B cleanup?

It should work with lye, I see no reason why it wouldn't.. But, you'll have a very caustic sludge you'll be dealing with, that is potentially dangerous for spills, stuff going into your skin/eyes, etc, so if you use lye you should be specially careful.

Lye would not work if the solvent used was a vegetable oil since it would saponify, but thats not the case with limo/xylene/toluene.


As for the fumaric acid suggestion, yes you can most definitely do that, it's called FASW. If you read BLAB tek, at the end in the salting part you can see it's explained.

The fumaric acid precipitation which can occur with certain solvents can be worked around by spiking the solvent with some anhydrous acetone before adding the FASA. This is an experimental technique, the proportion of acetone required is up to you to determine.

Lime teks rely on the low solubility of calcium hydroxide to form a thick paste. Lye is highly soluble thus this paste, which is crucial to the technique for ease of handling, will not be formed when using lye.

endlessness, my thoughts too, but some people think different about using lye and I wondered why.
downwardsfromzero, I've never heard of a thick paste crucial for easy handling. Could you give more detail?

I've just back-salted DMT-Fumerate with FASW on some limo that precipitated FA (during a FASA precip test).
So for me no big deal if limo precips FA or not, FASW works.

Looking back the precip of FA probably occurred because I've added FASA too quickly. I'm no expert, but I think adding FASA slowly keeps the FA better dissolved in the acetone which dissolves in the limo. Adding quickly separates the FA from the acetone too much, after which some organic limo impurities dissolve into the acetone, locking the FA out out of the acetone into the limo where is can't dissolve and thus crashes out. The more impurities the limo contains, the worse this gets. To the point that adding FASA slowly doesn't even help. Explaining the difference between limo brands. This is just my theory so please correct me if I'm wrong.

You mentioned adding some acetone to the limo prior FASA. This makes sense as it probably creates a buffer of additional acetone for the FA to dissolve. If so, why are we saturating acetone with FA instead of staying below saturation point (eg. 3-4mg FA instead of 6mg FA per 1ml acetone)? Won't this give better results for FASA on limo in general?

Update:

1) Took 20ml Limo
2) Added 20ml FASA: precipitation (Limo not usable for FASA)

1) Took 20ml Limo
2) Added 5ml Aceton: dissolved
3) Added 20ml FASA: clear, no precipitation

1) Took 10ml FASA
2) Added 10ml Aceton: dissolved
3) Added 20 Limo: clear, no precipitation

Conclusion: Adding 1/4 acetone to 1 limo prior adding fasa works. Also, using a concentration of 3mg/ml FA/Acetone instead of the usual saturation at 6mg/ml works as well. I didn't go testing down to find the limit.

Thats the good news. The bad news is after the test I couldn't clean the Limo with water. When I added water the limo went cloudy and stayed cloudy. Dont get why the FA is not dissolving properly into the water. Might have to wait some longer for it to settle.

If this works for Limo, it could work with Naphta. Though I don't see the direct benefit of doing FASA on Naptha vs freezing it.

Great that you tried some experiments, some one. Limo tends to form emulsions a bit, especially when slightly oxidised. Also, acetone is completely miscible with both water and limo so your clouding is likely colloidal aqueous acetone. You will have to write off your 60mL of limo as the price of the experiment.

The extra lesson would be to use smaller amounts of materials for such tests (hint: consider the size of a test tube ) but I would guess you were limited by the resolution of your volumetric equipment.


A thick paste allows for mixing between the limo and the aqueous phase without the particulates of dried material or the emulsions of a more liquid preparation. Granted, a certain amount of limo becomes trapped in the paste but this is of negligible significance if multiple portions of limo are used.


You may have/want to FASA from naphtha if:

ø your naphtha is not sufficiently saturated to freeze precip and you don't want to evap it
ø your naphtha contains a significant proportion of aromatic hydrocarbons thus precluding the use of freeze precip
ø you want to store your product as the fumarate and fancy trying a short cut ( )

Thanks.


Wasting 60ml limo on experimentation didn't seem like a big deal


So are you saying that Calcium Hydroxide is more prone to form emulsions compared to Sodium Carbonate? I did get an emulsion using Calcium Hydroxide on Limo..


I could try the do the experiment again with IPA and FASI to see if that works better for cleaning. If not, only way is distillation I guess. But I'm not going that route.

No, I'm saying that if you use calcium hydroxide your aqueous phase should be a thick paste. If it was a liquid with suspended particles of calcium hydroxide then there's little wonder that you experienced problems with emulsions. Other useful terms for optimal limetek consistency - putty, dough, clay, plasticine.

This dough should remain stuck together as you mash limo through it.

Late reply, haven't posted in a while.

Ok I see what you mean downwardsfromzero.

Update on the limo: I did a FASA and a FASI extraction with the aceton treated limo. The extractions went fine, but when I tried to clean the limo from excess acetone and fumaric acid by adding water and mixing, the limo went cloudy and I couldn't get it clean again. Did several batches of clean water, filtering in a separatory funnel. Let it settle for weeks.

Adding IPA to the cloudy limo made it go clear. But after adding water it went cloudy again. Letting it settle for a long time resulted in a less transparent layer on the bottom of the limo above the water. Tried discarding water and repeating etc. No luck....

Seems like the excess fumaric acid was trapped inside the limo after the acetone (or IPA) were pulled down into the water below. Odd..

Nice to be reminded of old posts

You could clean it up by swirling with solid caustic soda but only if you've only used IPA. I wouldn't want to do that if there was a significant amount of acetone present. For acetone, you could try bisulphite as solid or solution. I've pulled MEK denaturant out of bio-ethanol using solid bisulphite. (It forms a complex with ketones, rather handy.)

All told, I've found working with limonene engenders its own subset of special problems (to put it nicely!)