Need help with 69ron mesc extraction please

[windoze9x]

Hello,

Someone I know has been doing the 69ron d-limonene mescaline extraction for a long time now with some pretty good results. He has one recurring issue that he's not sure how to solve though. Maybe you guys could point him in a direction. When extracting and putting the d-limonene/vinegar in the separatory funnel he end up with this bubbly layer between the d-limonene and the vinegar. It does slowly dissipate but it seems it never completely goes away. Sometimes it's a little worse than others. It is slowing him down quite a while and leaves him with that stuff he's not sure what to do with. I'm not sure if he can put it in his tray and evaporate it or if i should discard it or what. Here is a pic of what it looks like (it is less or worse sometimes):

 

[Infundibulum]

This white layer is called emulsion, a dreaded suspension of the non-polar solvent and the water. It is nothing to worry about if it is as small as in the picture shown. And given that one salts out of each limo pull 3-4 times there'll be little if anything trapped in this emulsion layer.

Emulsions are caused by moderate to violent mixing of the two layers. Often emulsions go away with time, gentle rubbing, vibrations, sonication, centrifugation, increase in the ionic strength of the solution etc. Some other times an emulsion is so hard and thick that you can hardly do anything. Such emulsions are called emulsions from hell and they are a major headache. Learning to avoid emulsions is a true art.

 

[futura]

Hot water baths(around 140 degrees F) will break most emulsions and shouldnt affect mesc alkaloids at all...

 

[dg]

you'll find the emulsion and limo filter out of the water nicely


i like the ever high tech funnel and cotton ball(let it filter until just before the limo starts to go thru the filter)

 

[Virola78]

dude you got more than one french press?

ow, about the emulsion, did you shake it like hell?

 

[odawg]

I always get that exact same emulsion. I usually just ignore it and leave it in the limo between vinegar pulls. By the time you've done a few pulls with the vinegar, the impact should be quite small. I also usually do a rough decanting for each pull, collecting the vinegar layers together in a jar, and then use a sep. funnel after so that I have very little limo in the funnel.

DG's suggestion is great also when you suspect that some limo may have gotten through. A quick run through a funnel/cotton ball will clear out trace limo that can cause the final evaporated product to be gunky.

 

[windoze9x]

Thanks for all the suggestions guys!

dude you got more than one french press?

ow, about the emulsion, did you shake it like hell?

Yes he often does more than 100g of cactus at a time and needs a couple french presses to do multiple batches at once.

DG's suggestion is great also when you suspect that some limo may have gotten through. A quick run through a funnel/cotton ball will clear out trace limo that can cause the final evaporated product to be gunky

He sometimes does get gunky results even though he tries to be really careful. The cotton ball thing sounds good but wouldn't it absorb a bit of vinegar too. He'd hate to lose yield. It might be worth a small loss for a cleaner result though.

ow, about the emulsion, did you shake it like hell?

When I was looking up this problem I ran into the dmt problem about emulsions. My friend used to just stir pretty vigorously with a fork but his first yields were truly terrible. He never started getting good yields until he shook the vinegar/d-limo. He tried last night using an electric mixer instead and the emulsion layer was still really bad and maybe even worse .

 

[Virola78]

Fairly good results are possible without vigorous shaking/stirring.
Salting of mesc can take some time.

Just leave the fluids in contact for few hours with occasional (and gentle) swirl.
Then separate the salting solution, and repeat.

I think basifying is one of most crucial step in the process.
How long do you basify?

 

[windoze9x]

hi,
when swim gets emulsion he saves it and in the end of the process he dilutes with acetic solution, stirs and hot bathes it and waits a couple of hours to separate, and retrieve the vinagar..minimizing any possible loss.dont polute your stuff with emulsion or d limonene.swim finds a magnetic stirrer to be a great investment.

My friend was actually looking into a magnetic stirrer! At least then he could just set it and forget it and experiment with speeds/time. Btw he switched from vinegar (acetate) to hydrochloric adic (hcl) and the difference in the result is amazing. Now all he has to do is learn to clean this stuff up for ultimate purity. Does the person you know find the magnetic stirrer does a good job minimizing emulsion?

 

[bluntmuffin]

Figured I'd re-use this topic for my post:

Some alley cats were found by me to be performing 69ron's extraction in an alley (because that's where the cats live). And they meowed concern that their mixing of the 90g~ of cactus powder + 22g~ of Calcium hydroxide + 300mL of water seemed strange. The texture was found to be quite squishy (is that correct, sort of like a cake dough), and it appears some of the lime has fallen to the bottom of the beaker - where it remains stubborn and stuck to the sides. Should the alley cats attempt to stir this into the green mass? They're trying, but much more force and the stirring rod is in danger of smashing. I can request those alley cats to provide photos within minutes if required.

While watching from my window through binoculars, I have seen the alley cats pour in 300mL of d-Limonene and begin stirring. It appears that the d-Limonene has taken on a light green colour, and the cactus powder has begun clinging together in small balls. The alley cats appear to be stirring this now.

 

[Virola78]

^ good, you corrected for the calcium hydroxide. So why didnt you correct for the water?

weight of cactus powder X 0.25 = weight of calciumhydroxide
weight of cactus powder X 3 = weight water = volume water

did you break up lumps of lime before you added water?
did you thoroughly mix the cactus powder and the calciumhydroxide before adding the water?
did you add the water slowly while stirring with a wooden stick?

 

[bluntmuffin]

I figured that this cactus was extra mucous-like in consistency, and I felt that more water was needed to have a stirrable consistency.
The way it was anyway, it was still hard to stir.

I had extremely finely powdered lime, finer than talc I'd have to guess. It only lumped after water was added.

...That would be the problem then. I just added the water in 3-4 large splashes. Next time I'll mix the lime and powdered cactus more thoroughly, and will add water very slowly.

The next problem is that I'm trying to remove the d-Limonene from the stock. Can't find my sieve. Wish I bought an el cheapo coffee plunger now. :S


UPDATE:

I'm having problems drying what may or may not be aqueous mesc. HCl. I've got a small amount in a pyrex dish with a fan blowing cold air over it. It's not really evaporating. Would I be ruining it by using an oven at a low temperature?

 

[windoze9x]

yes for acetete stiring is better than shaking, not for carbonate.Dont know about hcl.Anyway look for a used mag. stirrer or a new HAMA hi 190m, good price and quality.it feels more systematic and tidy, more of a pro feel.
swim is so satisfied with acetate (using 5% glacial acetic acid solution) that has not bothered yet to do hcl mesc. though he has hcl at hand.He gets 1.8-2% yields of full spectrum and 1.5% o washed mesc.(one time cold mek) every time.Nice crystals!!! Check a post in this forum called "the goo factor" swim would like to know how swiy made hcl, concentrartion etc...

the highland spirit likes this :

SWIM prepared his HCL by buying muriatic acid (33% hydrochloric acid solution) and then diluting it with 2 parts water which gave me approx 11% solution. Then SWIM did 9 drops of water into 200mL of solution per the suggestion of someone else correcting the original 69ron tek which seems to call for too much acidity pulling too much junk. SWIM doesn't have a ph meter yet to test the ph so his extractions vary slightly in color probably due to not being 100% accurate with the solution.

The next problem is that I'm trying to remove the d-Limonene from the stock. Can't find my sieve. Wish I bought an el cheapo coffee plunger now. :S


UPDATE:

I'm having problems drying what may or may not be aqueous mesc. HCl. I've got a small amount in a pyrex dish with a fan blowing cold air over it. It's not really evaporating. Would I be ruining it by using an oven at a low temperature?

SWIM puts his hydrochloric acid (or vinegar) with his alkaloids in a pyrex dish and places the top of one of them round food dehydrators over it. Even at the lowest temp (like 90 degrees) it should evaporate everything in 4-8 hours probably depending on how much liquid. He often turns it up to 150-160 degrees while there is lots of liquid and then turn it down later to avoid burning drying materials. If you use the larger pyrex baking dishes it probably will evaporate faster due to more surface area.