• Members of the previous forum can retrieve their temporary password here, (login and check your PM).

Phosphoric acid test - RESULTS IN

Migrated topic.

Viracocha

..still lc..
Some aya brews have been known to use Phosphoric Acid in place of citric, acetic, or other. Multiple sources state that it produces a more full experience of greater intensity. There have been suggestion that it may help pull the dark alkaloids as well as the dmt from MHRB into the brew but this is mere speculation at this point (unless someone knows different?) - although it does add an further aspect of interest

I have yet to see an extraction tek use phosphoric acid,
so i thought we should give this a go

I passed on the request to the mad scientist on the moon and he will soon get back to me with the results.

The test will use Acacia Obtusifolia bark and the following process:

1: Acid cook in dilute phosphoric acid (pH4)
2: Exhaust plant material and discard
3: Basify liquid to pH12 using NaOH
4: Extract with Shellite

-- at this point the shellite will be halved
- the first half will go straight into the freezer for freeze precip
- the second half will proceed to step 5

5: Wash Shellite with dilute phosphoric acid (pH4), discard shellite
6: Basify liquid to pH12 using NaOH
7: Extract with Shellite and freeze precipitate

* Steps 5-7 is the purification technique from the LexTek, however I am beginning to think that perhaps the double AB is in some way affecting the final result, putting the molecule through more stress than necessary. It would be interesting to compare the products from Step 4 to Step 7. The Step 4 product will be left in tact as is, no cleaning whatsoever, we want to see just what exactly those oils do contribute

** A further step will be done:
** 4.5: Do a Xylene pull and evaporate, clean with hot Shelite

To see if there are any dark alkaloids present in Acacia Material


Updates soon!
 
Alright, just two comments:

1. When the pH4 dilute phosphoric acid was added to the bark, it began to bubble a little. Like some kind of reaction was already starting. Also, after the cooks the liquid was a thick brown, definitely NOT red like acetic or HCl tends to produce.

Two four litre cooks were done (1Kg of bark used) and combined and reduced. After reduction there is about 2L - was it taken too far? It should be ok...


2. When it came to add NaOH, to the solution still hot from reduction, about two teaspoons was initially added. Surprisingly the solution turned milky white almost instantly. On closer inspection it was actually a precipitate.

Note that this is suspected to be high content bark, so perhaps this would make sense

At the moment the vessel is too hot to add more NaOH (scary stuff) so it'll be left to cool for the moment. More will be added later. Perhaps some Shellite will be added first so the precipitate has somewhere to sit before proceeding to add more NaOH
 
Solution was allowed to cool, then 250mL of Shellite was added as well as NaOH at a slow rate until the black liquid formed. Approximately 50grams of NaOH was used. The precipitate which formed was still present but after mixing the solution two distinct layers formed as per usual (black on bottom, clear on top)

Proceeded to separate the layers and combine 3 x 250mL Shellite pulls
Proceeded to then do a single 250mL Xylene pull

Below you can see the Shellite pull to the left and the Xylene to the right

img0639fi6.jpg


Note that the Xylene pull is orange (kind of). Yellow plus red makes orange right? So if the Xylene is evaporated and the residue is repeatedly washed with Shellite perhaps a red oil will be obtained? We'll see in time

Also note that the Shellite layer has a lot stronger yellow colour than seen in the LexTek which uses acetic acid. In time the result of this will be seen
 
As mentioned in the first post, the initial round of Shellite pulls will be split into two; one half will go straight into the freezer (the yellow liquid to the left in post 3), and the other half will be given a second round of A/B for purification purposes

Here you can see the resultant Shellite from the second A/B
Note that it is completely deviod of any hint of yellow. It will be interesting to compare both products qualitatively

img0641ov0.jpg
 
Ooooh! but the one on the left looks greenish..!?

- just wondering - if you do or don't pre-dissolve the lye in a strong solution..? Or do you just add the lye as a solid.? It's a little less exothermically 'explosive' if you add it as solution...
 
Yeah clear indeed, but certainly contains the goods
About 12 more hours in freeze precipitate before the solvent will be decanted and the results weighed for comparison

Here's a sneak preview:

img0644gm2.jpg


img0645ak4.jpg



El Ka Bong,
The Lye is usually added as a solid but you make a point, in future your suggestion will be put into practice
 
That's seems to be the case
Take a look at the initial shellite extraction from the LexTek which uses acetic acid

lexfirstxu2.jpg


Clearly not as yellow as the phosphoric result; different bark was used however which could contribute to the effect (although both were using acacia obtusifolia - the phosphoric tests are done on a far older specimen)

Conversely, the second A/B really helped in removing the yellow pigment (however we're yet to see whether that's a good thing or not). Nonetheless, the double A/B is no doubt an effective purification technique, but one has to wonder if the salt to freebase to salt to freebase could carry with it some unwanted reactions. Perhaps a sample of both final products should be sent for some kind of component analysis
 
Total time in freeze precipitate was +30 hours
Here are the final products (each from 500 grams of acacia obtusifolia bark):

From the yellow jar:
Yield: 0.78%

img0655cd3.jpg



From the clear jar:
Yield: 0.67%

img0653fd5.jpg


As expected the clear jar has a slightly lower yield, but consider the lack of yellow (oil) plus the added losses of the extra A/B

For a combined yield of 0.73%, that's not too bad for good old acacia bark!

It was interesting to see that the product of the yellow jar didn't contain a large amount of oil as expected (due to previous experiments using acetic acid). For the higher yield I'd say the second A/B isn't needed unless an ultra pure product is required (for purposes such as producing snortable/other'able salts)

Experience comparison to come..
 
.73% sounds good for acacia's. how does the phosphoric result compare to acetic acid or HCL in terms of yeild? I see when acetic was used in the lextek the yeilds were much lower..

also was a defat done on this extraction?
 
The reason we are looking away from acetic acid is that there has been some mention of acetate salts breaking down in concentrated pH solution - like when reducing the liquid from the two or three initial acid cooks. I'm not sure if dmt.acetate is in this weak category, but best to stay clear for the moment

HCl salts can withstand these conditions, as can phosphoric by the looks of it

No traditional defatting was done. By traditional, i mean performing multiple Shellite pulls on the acidic solution. The more yellow spice was a basic Acid -> Base -> Pull -> Precip and the whiter spice was done with Acid -> Base -> Pull -> Acid -> Base -> Pull -> Precip; the second A/B acts as a defat in this regard

The next test in the coming months will be to do side-by-side extractions using:
Phosphoric Acid
Hydrochloric Acid
Acetic Acid

In my mind, acetic acid shall be shunned for all things dmt related (god knows how much was lost over time..), but the test will be done for referrence purposes

Keep in mind that different bark was used between the making of the LexTek and the phosphoric extraction you see here. The key factor is the age of the bark (+10 years difference)

Regardless, phosphoric is looking pretty good so far
 
Coschi you're the man, thanks for the interesting experimental data.

I'd be interested to see how Ascorbic acid (Vitamin C) fairs in one of these test runs, it has become SWIMs acid of choice for DMT extraction.
 
My pleasure sippyj, but realistically all we've established is that phosphoric acid works.
what if that bark is massively loaded like 1.5% and there's still a better choice out there?
and we're yet to see how the experience differs with the use of phosphoric acid..
 
Well, it definitely works
The LexTek will be released as version 2, using phosphoric acid

The yield was substantially high (not sure how much i'd attribute that to the phosphoric)

Most definitely more of the yellow came through (two attemps using phosphoric this has been the case, and never in the past, i'd say for sure that phosphoric helps bring across the colour, but i bet other acids would do similar things)

Now,
you may have heard me rave on about this first batch of dmt i tried, how it was the business, everything you could want; entities, unimaginable worlds of colour and morphing stuff i'm not even going to try to explain. Everything since this batch has been substandard

There have been other batches, took me to different places, different beings, but nothing compared to this first

Important thought 1:
Since i've extracted spice myself and made my own leaf blends, i found that 90% of breakthroughs would actually result in no entities. Just patterns, strange and interesting things (dancing trees, seemingly random dialog, etc..) BUT no entities which got to me. Always the method was double A/B using acetic acid to yield a pure white product (ala LexTek v1). To be honest, i'd say the majority of the blends I made during this time were equal to (or slightly better than) the substandard ones i mention above. DMT of course can never be called substandard, but when i use that first ultimate batch as a reference.. well, you see what i mean

and, I suspect that when entities were present, they were introduced from the leaf blends rather than the dmt itself. Brugmansia always gave black women and children..


Important thought 2:
This time, single A/B using phoshoric
More yellow, more oils, MORE PLANT

No cleaning, yellow oily crystals deposited straight onto carrier leaf (3 parts pau d'arco, 1 part blue lotus, 1 part white lotus)

GLORY FUCKING GLORY

she's back, morphing able to invert pippy-longstockings girl (from the first batch)

I didn't get to do too much yet, but even just this first time was enough to know i'm a hell of a lot closer to where i want to be than previously.

All that lovely stuff is right back where it should be, and my mind wasn't hectically trying to keep up with it either (as was with all the previous batches using ultra clean acetic product). I could just stare in awe at the whole thing without a single thought in my head, just appreciating


Preliminary Conclusion:

Well, the main reason of the test was to check clean crystal (double A/B) vs dirty yellow crystal (single A/B, no recrystallisation)

The oils, from the plant..
DMT is a multi-dimensional gateway, and the plant matter is the pointer

Brug would introduce those south american native looking people, full of earthy tones like green brown black clay mud swamp

The acacia oils introduce an electronic vibe, synthetic yet purely natural. I think the entities of the dmt containing plant are the ones to keep in play, but then again it all depends on what you're looking for. How about dirty dmt laced onto dried shrooms?

Have i made myself clear?

From now on, i'll be cleaning the crystals only for the purposes of crystal growing and snorting, salting etc.. for the purpose of smoking, enhancing leaf, introducing people to dmt etc.. I want that stuff as dirty as can be. It didn't make the slightest bit difference to the harshness, and all the things previously lacking in the experience are now back. The only thing left is to being back those purples...
 
Very interesting. So you are saying that the leaf mixture along with oils from the plant make more of a difference in the experience than the acid used or the pH it was pulled at? I guess that makes some sense.

Very interesting reading. BTW I am using phosphoric acid exclusively in my extractions now. It is easier to handle than HCL and seems to pull more spice than vinegar.

I have not had the problem with oils coming through though...quite the opposite..I have had much fewer oils than any other tek used. This may be because I am not pulling the spice with hot NP but waiting until everything is room temperature before pulling.

Do you feel that the pau d'arco makes a big difference? I mean have you tried just using blue/white lotus leaf?
 
Back
Top Bottom