Soulfood,

SWIM suggest the following process : dissolve extract is as few acetone as possible (go drop by drop).

Btw, Warrensaged, 5 ml for 25 mg is way too much. Even for 250 mg, that would be too much. SWIM perfectly dissolved 250 mg in 2 ml of acetone.

So the extract is dissolved in a small glass (a tube is better). Naphta is added drop by drop. Wait few minutes every few drops. The naphta layer becomes very cloudy but some brown precipitate will appear in the acetone. This is not immediate, that's why SWIM suggest to wait a bit between naphta adds.
When this happend, carefully pour off the liquid in a second jar and keep the solids for further purifications (or use it).
You can continue to add slowly some naphta in the second jar and slowy agitate the jar. When nothing new seems happening, wait 30 min, separate the acetone layer (on the bottom) and evaporate it. What you will get is cleaner than the initial extract. There should be not that much goodies in the naphta layer.
SWIM did not find any ratio acetone:naphta. It depends on the purity of the extract. With cleaner extract, less naphta is required, but SWIM used until 3:1 naphta:acetone.

However, SWIM prefer the following : dissolve the crude extract in a bit of MEK (as few as possible again), than add some xylene, shake, then add some ammonia, shake, wait, and keep the ammonia layer and evaporate it.
Ex, for 250 mg, 0.5 ml of MEK and 5 ml of xylene, then 5-7 ml of ammonia (does'nt really matter, it's just longer to evaporate with more).
The idea is that MEK and xylene are miscible, so the bufo is 'spreaded' in the xylene but not dissolved. When adding ammonia, some of the bufo is catched by the ammonia (maybe just fall down). Ammonia stinks but is less toxic than xylene and SWIM feel more comfortable about it. And pure ammonia leaves 0% residue.
There are no scientific facts about the idea above, but practice showed that the ammonia layer keep something, while the xylene layer 'lose' some colors.
The evaporated extract from the ammonia layer is dry, less dark than the initial extract and smell nothing (while the initial extract smells like toasted peanuts).

Ah cool!

Cheers Garulfo. It's really good to see other ways of purifying.

What advantages does MEK have over acetone?

For what we were doing that's actually what it took.
That's including the solvent needed to rinse the beaker & dropper out too BTW.

The idea was to saturate the joint with it.
Not just to liquefy the bufo & drop it, to stick on the outside of the paper, but to get the Bufo to soak into the paper & into the herb completely.
I tried less acetone at first, but the acetone would soak into the paper/herb & leave the bufo stuck to the outside of the paper, like a filter.
We also had to keep letting it dry out before adding more, or it would saturate with bufo-tone & start unglueing the rolling paper because it wouldn't soak in anymore liquid.

Like I said, the joint was already rolled (my buddy brought the J with him when he came over]), or I probably would have saturated the herb itself, before rolling it up or something.

...mother of invention...

Should have explained that better, I guess.


Cheers,

WS

Ok, weird result.

From disolving 200mg crude bufotenine in vinegar with excess zinc, stirring, filtering then evaporating the vinegar I got 2g's of flaky solids?

That's higher by 2x of the bufotenine and zinc combined. So huh?

Weird.

Freebased the stuff and washed with IPA (out of acetone )... now evapping.


Also I'm not sure I understand the whole drytek thing. When first doing dryteks I follwed the instructions and got good results. But just recently I've been checking ph's before drying and the pH never seems to be anywhere near high enough. But after drying then wetting a small amount of material the pH is where it should be.

Is there an accurate way of predicting the pH of this stuff before it dries?

Ah yes, makes sense indeed. SWIM should try that way because freebasing hurts lungs.

Soulfood,

MEK is miscible with naphta or xylene, while acetone is not (or partialy ?) that's why I guess that MEK can 'convey' (?) things to the naphta/xylene.

SWIM tried 25 mg of his MEK->xylene->ammnonia extract in sublingual form. It was definitivly bufo effects but pretty weak. SWIM will try 50 next time.

Have you tried the whole progressive toasting thing where you burn it, then filter out the goods more than once?

If so what's the weight-loss : purity you can expect on the second toasting compared to the first?

Also have you tried toasting before the initial limonene wash?

SWIM's biggest annoyance with himself is, he doesn't think. Can someone put me out of my misery and confirm for me what I am now a victim of due to stupidity.

Sodium carbonate is soluble in IPA isn't it?

Them sure don't look like bufotenine crystals.

I'm in the process of doing it now.

I toasted the seeds @ 350F degrees for 30 minutes after they stopped jumping.
I pre-washed the ground seeds in acetone, using THP before basifying & got a whole lot of dark yellow colored acetone out of it.
I did the rest of the extraction, doing one D-Limo wash, then dried it out & toasted the precipitate @ 350 for 30 minutes, before scraping it up.
I let the dish cool, scraped up the burnt-black extract & dissolved it in acetone & filtered out the solids, then filtered the liquid 2 more times before evaporating & scraping up the drier, cleaner extract.
I then did another D-Limo wash, dried it, scraped it up, dissolved the darker powder (??) in acetone for filtering & I'm waiting for it to evap right now.

When its finished drying, I'm not sure if I want to do the whole toasting/filtering process on it a 2nd time, or just try smoking a little, it's really pretty clean already.

Notes:
**When I did the acetone pre-wash, I was in a bit of a hurry, & I didn't have a whole lot of acetone either, so I only washed it 2 times, pouring 200ml of acetone through THP 5 times, each.
To be honest, I have not really noticed any difference in the amount of impurities or stickiness of the extract throughout the process. However, it did clean out a lot of yellow stuff. to make sure there was no Bufo pulled out with it, I poured some FASA into it & nothing at all precipitated!!
So I think I'll do it again next time, but I'll use a lot more acetone & keep washing it until the color starts getting lighter in color.

**A lot of stuff was burned out of the extract during the 2nd toasting. It pretty much cut my yield in half, after filtering the burnt solids out & doing a 2nd D-Limo wash on it!! That is just fine with me though, as long as it's crap being burnt off & not Bufo & that is what seems to be going on.

I attached some pics of the first D-Limo boil I did for those new to the process to check out.
I numbered them, so they are in chronological order.
I'll add a pic of the cleaned extract to, after its finished drying & I scrape it up.

Cheers!

WS

Here are some pics of the angled precipitation dish & the D-Limo pooled in the corner cooling.
Also a few of what the D-Limo looks like after letting it sit for a 1/2 hour or so & all the Bufo has dropped out, but not all of the unwanted oils.

Still drying the final last evap.

Cheers

Whaow, thanks for all that photos.
So you initially washed your seeds with acetone, not acidified acetone ?

The Bufo in the seeds are already a salt so it's naturally acidic.
And that's the whole idea, the acidic bufo will not migrate to the acetone, because it's not soluble in acetone when its an acid, but some of the other oils & fats are, so they migrate to the acetone during the wash.
That way, when you then basify the seeds & do the acetone percolation again, the bufo migrates over to the acetone, without those oils & fats that were already pulled out!!


Cheers!

WS

Has anyone noticed some sparkly substance just after mixing the base with the ground seeds?

It looks very glassy and crystal clear. Almost needle-like.

Here are some pics of "Before & After" doing the D-Limo wash, re-toasting the dried extract, Acetone filtering, 2 more D-Limo washes & a bunch of Acetone washes:

I did not end up doing anymore toasting this time, I want to actually have enough to try vaporizing a larger dose this time.
In all my past attempts, I've ended up loosing most of my yield to a screw up, near the end of the process.
I've actually got some nice looking extract here & I want to try some of it now.

After the 2nd toasting, dissolving in acetone, filtering it, drying, & 2 more D-Limo washes, I just did a number of acetone washes, over & over.
I would dissolve the dry Bufo extract in about 10-15ml of acetone & stir it for 2-4 minutes.
Then I filtered out any solids (impurities) using a small filter paper, that I folded into a fluted cone & put into a small funnel. I poured the liquid into the filter paper a little at a time, allowing it to drip into a small beaker below. Then I filtered the liquid Bufo-tone 2 more times through cotton stuffed into the neck of the small funnel. The 3rd time, it was dripped from the filter into a large glass dish, to be evaporated.
Once dry, It would scrape it up & do that same filtering process again.
I did this I think, about 5 times, catching less & less solids each time the extract was scraped up & passed through the fluted filter paper again.

This resulted in a very fine, tan colored powder, have not weighed it yet, but I'm guessing it's about 300-400mg.

I wish my camera would take close up pics with better resolution!!
The extract always looks a bit darker that it actually is in my pictures.

I'm going to extract 75g of seeds soon & after doing the first D-Limo cleaning & toasting, I'm going to split the resulting extract in 2 & experiment with doing a 2nd FASA conversion again, to try getting rid of any residual oils & impurities.
The other half, I'm going to keep doing D-Limo washing, re-toasting & acetone filtering a number of times, trying to clean off all the impurities etc...


Cheers!!

WS

Hmm, Warren, no offense but that seems a lot of work for such brown thing
I wonder if the toasting is really efficient.

Yeah...it is.

Although, my shitty camera makes it look much darker than it really is, it's more of a light tan.
But still, lots of work...period!!

Also, this stuff oxidizes & gets darker very quickly after it drys!!
That is getting a bit old too!!
It's nice & light tan after scraping it up & then after an hour, in a sealed jar, its 2-3 shades darker!!
WTF!!!

Anyway, gonna smoke some tonight & see if it was worth it at all.

Cheers,

WS

Did you get there yet?

SWIM tried toasting his extract in the drying step after the fumerate to base conversion. It made his kitchen smell like bad breath and much filtering later he had a dark amber solution.

I know this is probably not a saturated solution but would it be a good idea for SWIM to add naphtha gradually to the mix if he evaps down a little before hand to change the polarity of the solvent for a little purifying?

Or would it be best to evap all the way, scrape up and then re-dissolve?

Or should SWIM proceed with the limo clean? He'd like to save that until last in the hope of only one limo wash to gain a suitable potency with a slight orangey taste and minimal orange residue.

Toasting during the basification was probably not a real great idea.
There is already one chemical reaction happening & heating something during a chem reaction usually effects the reaction. (Right?)

That sounds absolutely nothing like what I've experienced when re-toasting after the 1st D-Limo wash.
When I've done this, there is not any smell, other than maybe a bit of orangey scent.
Although, I've been using the "High Purity" D-Limonene, which doesn't have as much of the orange smell anyway.

I did test some of my last extract the other night, same thing as the others, just a nice body buzz...not much by way of visuals...but a nice, warm body buzz.


WS

I got some CEV's off of some brown muck that were pretty cool, but I only had 100mg to play with and the rest was lost to experimentation.

I'm pretty adament if you want it bad enough you can keep this stuff down as long as it's been cleaned a little.

The next batch is going onto leaf though

My understanding is if you toast the basified material one of the toxins should boil off so I wasn't too surprised.

Ok just went ahead and evapped using heat.

At one very end of the dish there's a little bit of dark amber but the rest of the material is sandy brown. Vaporized 8mg and it's defo bufotenine and it seems to be ok, it was still harsh but only caused containable diaphragm contractions. There's definately a little peripheral weirdness going on.

Haven't even done a single D-limo boil yet.

I think I'm going to do the sandy stuff and the darker stuff seperately. This is the first time I've got this stuff to sparkle at me.

Needless to say... I'm excited